SEMS-RM DOCID # 1163861

317 E. Main Street Ventura, CA 93001 Tel: (805) 585‐2110 Fax: (805) 585‐2111

MONTHLY MONITORING REPORT MAY 2016

DATE: July 8, 2016 (revised Jan 4, 2017 to correct groundwater gradient to southeasterly - see Section 2.0, 3rd line)

PREPARED FOR: Rose Marie Caraway, Remedial Project Manager/Environmental Scientist U.S. Environmental Protection Agency, Region 9 75 Hawthorne Street, SFD 7‐2 San Francisco, California 94105

PREPARED BY: Max Ramos, E.I.T., Staff Environmental Engineer, OTIE John Wingate, P.E., Project Manager, OTIE Lindsey Larsen, Environmental Scientist, OTIE

RE: May 2016 Plant Influent and Effluent Sampling Results for the Pemaco Superfund Site Treatment Plant, Maywood, California

1.0 INTRODUCTION The United States Environmental Protection Agency (U.S. EPA) is currently implementing the Long‐Term Response Action (LTRA) at the Pemaco Superfund Site in Maywood, California. Oneida Total Integrated Enterprises, LLC. (OTIE) performs monthly monitoring work for the U.S. EPA under contract by the United States Army Corps of Engineers (USACE), Los Angeles District Contract Number W912PL 13‐D‐0017, Task Order 0002. OTIE prepared this Report to summarize the results of monthly influent and effluent water and vapor sampling performed on May 12, 2016 at the Pemaco Superfund Site Treatment Plant (Plant). The influent and effluent water samples (SP‐201 and SP‐209, respectively), and influent and effluent vapor samples (SP‐104 and SP‐106, respectively) were analyzed for volatile organic compounds (VOCs) and 1,4‐dioxane. Samples were analyzed in accordance with the Final Sampling and Analysis Plan, (Field Sampling Plan and Quality Assurance Project Plan), Long‐Term Response Action for the Pemaco Remedial Action (OTIE, 2015). Monthly water and vapor sampling is performed to demonstrate compliance with Los Angeles County Sanitation District (LACSD) limits and South Coast Air Quality Management District (SCAQMD) guidance; confirm liquid phase granular activated carbon (LGAC) and vapor phase granular activated carbon (VGAC) effectiveness; and summarize data trends necessary for evaluation of remedial progress. The metric for “mass removal” is evaluated in the Quarterly Operations and Maintenance Report. The groundwater treatment system (GTS) and vapor treatment system (VTS) achieved operational uptimes of approximately 97% and 39%, respectively, during May 2016. The VTS was not operated from

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May 23 to May 31 in accordance with the “pulsed” operational schedule. Additional treatment system shutdowns occurred as follows:  The VTS was not operated from May 1 to May 9 due to a motor failure fault on the variable frequency drive for blower B‐101;

 The VTS was not operated on the morning of May 10 to accommodate changeout of VGAC for vessel T‐301 and cooling fan timer repair; and  The GTS operation was temporarily suspended on May 15 and 22 because the filter bags were full. Operation resumed the following day subsequent to replacement of the filter bags. Additional operational details are available in the most recent Operations Summary and the May weekly Quality Control Reports located on the Pemaco SharePoint website. Plant operational details will be summarized in the 2016 Second Quarter Operation and Maintenance Report. 2.0 ‘A’ ZONE GROUNDWATER LEVEL GAUGING Groundwater elevations and analytical data suggest an off‐site contaminant source is located northwest of Maywood Riverfront Park, with significant trichloroethene (TCE) concentrations in the Exposition Aquifer ‘A’ Zone (OTIE, 2016). Groundwater extraction from the ‘A’ Zone may promote a southeasterly migration of contaminants from northwest of the Park toward the former electrical resistive heating (ERH) area. In order to protect the ERH remedy area and discourage migration of the off‐site source, the ‘A’ Zone wells were shut down on April 28, 2016 following stakeholder discussion and U.S. EPA approval. Groundwater levels in the ‘A’ Zone will be gauged monthly to monitor gradient changes while the ‘A’ Zone extraction wells remain inactive. The May 26, 2016 ‘A’ Zone groundwater gauging event was the first groundwater level monitoring task performed since shutdown of ‘A’ Zone extraction wells in April 2016. Groundwater elevation data for the May 2016 gauging event is provided in Attachment 1. May 2016 groundwater elevations are compared to the most recent groundwater elevation data from the December 2015 semiannual groundwater monitoring event. ‘A’ Zone groundwater elevation changes at individual well locations include both increases and decreases compared to December 2015 values. The wells with the greatest change in groundwater elevation were DA‐12 (2.95‐foot decrease) and DA‐01 (2.09‐foot decrease). Evaluation of the overall ‘A’ Zone groundwater elevation trends will be included in future monthly monitoring reports, following sufficient rounds of monthly gauging. 3.0 PLANT WATER SAMPLING RESULTS Influent and effluent water grab samples were collected on May 12, 2016 and the detected analytical results are summarized in Table 1. The laboratory analysis was performed by Eurofins CalScience, Inc. The laboratory report containing the full list of analytes is provided in Attachment 2. The influent sample results represent a composite of flow from the following active wells screened in the Perched and Exposition Zones:

 Perched Zone (dual‐phase extraction [DPE]): PB‐01, PB‐02, PB‐03, PB‐05, PC‐06, PD‐04, PD‐05, PD‐06, and PD‐07; and  Exposition Zones (groundwater only [GW]): DB‐01, DB‐03, DB‐04, DB‐05, DB‐07, and DB‐09.

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Table 1 Monthly Summary of Detected VOCs in influent / Effluent Water Samples

Sample Locations SP‐201 (Influent) SP‐201 (Effluent) Sample ID SP‐201‐20160512 SP‐201‐20160512 Sample Date 5/12/2016 5/12/2016 Analyte Method SSRL Unit Results Results 1,1‐Dichloroethane SW8260B 5 μg/L <0.28 1.1** 1,4‐Dioxane (P‐Dioxane) SW8260SIM 1* μg/L 7.9 J 8.6** Chloroform SW8260B 80 μg/L <0.46 0.92 J** cis‐1,2‐Dichloroethene SW8260B 6 μg/L 9.9 5 Trichloroethene SW8260B 5 μg/L 84 0.40 J Notes: 1. * ‐ Indicates value is a "California Notification Level" which is less than the SSRL of 3.0, listed in the ROD (U.S. EPA, 2005). 2. ** ‐ Indicates effluent sample concentration was higher than influent concentration as a result of preferential desorption. 3. Bold indicates a sample detection. 4. ID = identification; SSRL = site‐specific remediation level; μg/L = micrograms per liter; < = indicates compound was not detected above the method detection limit. 5. Effluent water quality complied with the LACSD permit limit of 1,000 μg/L for total VOCs.

3.1 PROCESS WATER INFLUENT (SP‐201) DISCUSSION The following VOCs are associated with groundwater plumes being monitored as part of the semiannual groundwater monitoring program. Analytical results for samples collected during the May 2016 event for these VOCs are summarized below:

 Cis‐1,2‐dichloroethene (cis‐1,2‐DCE) was detected at a concentration of 9.9 μg/L for the month of May (Figure 1). The cis‐1,2‐DCE concentration in process water influent shows some variation between monthly samples, although samples from the previous 24 months have not exceeded 17 μg/L. The overall cis‐1,2‐DCE concentration trend is slightly increasing for the previous 24 months.

 TCE was detected at a concentration of 84 μg/L, higher than the previous process water influent sample (64 μg/L) but within the typical range for influent TCE concentrations (Figure 2). The TCE concentration in process water influent samples from the previous 24 months shows significant variation between monthly samples, with a generally constant trend over time.

 1,4‐Dioxane was detected at a concentration of 7.9 µg/L, slightly higher than the previous process water influent sample (6.9 μg/L) (Figure 3). The 1,4‐dioxane concentration in process water influent from the previous 24 months shows some variation between monthly samples, with a generally constant trend.

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Figure 1 Historical Concentrations of cis‐1,2‐Dichloroethene in Influent Water Historical Concentrations of cis‐1,2‐DCE 18 1/19/15 2/12/16 16 12/2/14 3/5/15 9/3/15 14

(µg/L) 5/15/15 11/3/14 12 8/11/15 6/4/14 2/12/15 10/23/15 3/8/16 5/12/16 10 7/23/15 1/5/16 4/6/16 8 Concentration 9/3/14 6 10/1/14 Influent 4 12/2/15 GTS 2 8/6/14 0 Jun‐14 Sep‐14 Dec‐14 Mar‐15 Jul‐15 Oct‐15 Jan‐16 May‐16 Sample Date (Plant Water)

Figure 2 Historical Concentrations of Trichloroethene in Influent Water Historical Concentrations of TCE 300

1/19/15 250 (µg/L) 4/14/15 9/3/15 2/12/16 200 12/2/14 5/15/15 2/12/15 6/1/15 3/5/15 8/11/15 150 6/4/14 11/3/14 8/11/15 Concentration 1/5/16 100 5/12/16 7/23/15 3/8/16 Influent 4/6/16 50 GTS 9/3/14 10/1/14 8/6/14 12/2/15 0 Jun‐14 Aug‐14 Nov‐14 Jan‐15 Apr‐15 Jul‐15 Sep‐15 Dec‐15 Mar‐16 May‐16 Sample Date (Plant Water)

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Figure 3 Historical Concentrations of 1,4‐Dioxane in Influent Water Historical Concentrations of 1,4‐Dioxane 20 5/15/15 18 3/5/15

16 1/19/15 6/1/15 1/5/16

(µg/L) 2/12/15 14 4/14/15 9/3/15 12 6/4/14 8/6/14 8/11/15 10/23/15 2/12/16 10 7/23/15 12/2/15 5/12/16 8 Concentration

10/1/14 6 11/3/14 4/6/16 12/2/14 3/8/16 4 9/3/14 Influent 2 0 Jun‐14 Sep‐14 Dec‐14 Mar‐15 Jul‐15 Oct‐15 Jan‐16 May‐16 Sample Date (Plant Water)

Notes for Figures 1, 2, and 3: 1. Data collected over a 24 month period beginning in June 2014. Concentration values reflected on the figure represent samples collected during monthly monitoring events. 2. Values that were below the laboratory detection limit are expressed as concentrations of zero. 3. Plant influent water was not analyzed in July 2014 and November 2015. 4. The trend line represents a linear regression of 22 data points from samples collected during monthly monitoring events. The trend line is a best‐fit representation of the data and serves as a forecasting tool; it is not intended to represent the mean value of all samples collected.

3.2 PROCESS WATER EFFLUENT (SP‐209) DISCUSSION The water effluent quality satisfied the LACSD permit limit for total VOCs of 1,000 μg/L. VOC concentrations in plant effluent were below their respective SSRLs, with the exception of 1,4‐dioxane (8.6 μg/L), which has low LGAC adsorptive capacity. The LGAC performance is satisfactory because the LACSD permit limits were satisfied and filter vessels continue to operate with acceptable head loss. 4.0 PLANT VAPOR SAMPLING RESULTS The influent and effluent vapor samples were collected in 1‐liter SUMMA® canisters on May 12, 2016. The analytical results for this event are summarized in Table 2. The laboratory analysis was performed by ALS Environmental and the laboratory report is provided as Attachment 3. The May 2016 influent vapor sample represents a composite of concentrations from active DPE wells (PB‐01, PB‐02, PB‐03, PB‐05, PC‐06, PD‐04, PD‐05, PD‐06, and PD‐07), all screened in the Perched Zone.

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Table 2 Summary of Detected VOCs in Influent and Effluent Vapor Samples

Sample Location SP‐104 (Influent) SP‐106 (Effluent) Sample ID SP‐104‐20160512 SP‐106‐20160512 Sample Date 5/12/2016 5/12/2016 Analyte Method Unit Result Result 1,1,1‐Trichloroethane TO15 μg/m3 2.2 <0.58 1,1‐Dichloroethane TO15 μg/m3 5.5 <0.55 1,1‐Dichloroethene TO15 μg/m3 25 <0.58 1,2,4‐Trimethylbenzene TO15 μg/m3 0.80 J <0.51 2‐Butanone TO15 μg/m3 3.5 J 2.1 J 2‐Propanol TO15 μg/m3 1.5 J 1.7 J TO15 μg/m3 46 8.3 J Benzene TO15 μg/m3 13 1.0 J Chloroform TO15 μg/m3 13 <0.58 cis‐1,2‐Dichloroethene TO15 μg/m3 38 <0.55 Cumene TO15 μg/m3 0.61 J <0.51 Cyclohexane TO15 μg/m3 120 <0.99 Ethanol TO15 μg/m3 36 280* Ethylbenzene TO15 μg/m3 1.1 J <0.55 Isopropylbenzene TO15 μg/m3 0.61 J <0.51 Methylene chloride TO15 μg/m3 0.92 J 0.74 J N‐Heptane TO15 μg/m3 48 <0.58 N‐Hexane TO15 μg/m3 190 1.3 J N‐Nonane TO15 μg/m3 0.68 J <0.51 N‐Octane TO15 μg/m3 8.9 <0.62 Propene TO15 μg/m3 <0.48 0.74 J* Tetrachloroethene TO15 μg/m3 160 <0.48 Tetrahydrofuran TO15 μg/m3 3.2 <0.69 Toluene TO15 μg/m3 1.6 J 2.6* trans‐1,2‐Dichloroethene TO15 μg/m3 2.1 <0.65 Trichloroethene TO15 μg/m3 530 3 Trichlorofluoromethane TO15 μg/m3 1.5 J <0.58 Vinyl Chloride TO15 μg/m3 1.7 <0.58 m,p‐Xylenes TO15 μg/m3 1.3 J <1.0 Notes: 1. * ‐ Indicates effluent sample concentration was higher than influent sample concentration as a result of preferential desorption. 2. Bold indicates sample detection. 3. ID = identification; J = estimated value; μg/m3 = micrograms per cubic meter; < = indicates compound was not detected above the method detection limits. 4. A complete listing of analytes is found in the laboratory report (Attachment 3).

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4.1 PROCESS VAPOR INFLUENT (SP‐204) DISCUSSION Influent vapor concentrations over the previous 24 months are presented in Figure 4. The sum of VOCs detected in plant vapor influent shows a decreasing trend. The trend is influenced by the high VOC concentrations detected during the months of January and February 2015. This concentration spike was associated with prolonged shutdown of the VTS system from December 4, 2014 to January 16, 2015 to facilitate removal of the Flameless Thermal Oxidizer. Influent vapor VOC concentrations since the June 2015 sampling event have been consistent with influent vapor VOC concentrations prior to the VTS shutdown. The COCs with highest concentrations in the vapor influent were: TCE (530 μg/m3), n‐hexane (190 μg/m3), tetrachloroethene (PCE) (160 μg/m3), cyclohexane (120 μg/m3), n‐heptane (48 μg/m3), and acetone (46 μg/m3). Figure 4 Historical Influent VOC Concentrations in Vapor

Historical Influent VOC Concentrations 70000

60000 1/21/15 (µg/L)

50000 2/12/15 40000 Concentration 30000 3/5/15 4/14/15

Influent 20000

5/15/15 VTS 6/1/15 10000 7/23/15 6/4/14 9/3/14 12/3/16 8/11/15 1/5/16 3/14/16 8/6/14 11/3/14 10/23/15 0 10/1/14 9/3/15 5/12/16 Jun‐14 Sep‐14 Dec‐14 Mar‐15 Jul‐15 Oct‐15 Jan‐16 May‐16 Sample Date (Plant Vapor)

Notes: 1. Monthly data collected over a 24 month period beginning in June 2014. Concentration values reflected on the figure represent samples collected during monthly monitoring events. 2. Plant influent vapor was not analyzed in July 2014 and November 2015. 3. The trend line represents a linear regression of 22 data points from samples collected during monthly monitoring events. The trend line is a best‐fit representation of the data and serves as a forecasting tool; it is not intended to represent the mean value of all samples collected.

4.2 PROCESS VAPOR EFFLUENT (SP‐208) DISCUSSION Plant air effluent is not formally permitted but does comply with the 2007 SCAQMD permit guidance for health risk that was prescribed for the Pemaco plant. Using the 2007 SCAQMD protocols, a Tier 2 Air Screening Risk Assessment (Attachment 4) was performed for the purpose of calculating the maximum

Oneida Total Integrated Enterprises Page 7 of 9 Monthly Monitoring Report May 2016 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California incremental cancer risk (MICR), the chronic hazard index (HIc), and acute hazard index (HIa) (SCAQMD, 2005). A summary of the results from the Tier 2 Air Screening Risk Assessment is presented in Table 3. Table 3 Summary of Tier 2 Air Screening Risk Assessment for Toxic Air Contaminants (TACs) to Nearest Receptor (75 Meters from Stack) Maximum Individual Chronic Hazard Acute Hazard Cancer Risk1 (MICR) Index1 (HIc) Index1 (HIa) Toxic Air Contaminants2 5.43E‐10 4.76E‐07 7.85E‐11 (including carcinogens and non‐carcinogens) Notes: 1. Cancer Risk and Chronic and Acute Hazard Index to nearest receptor at approximately 75 meters from stack. In June 2015 new risk assessment procedures were introduced by SCAQMD that contain updated risk assessment methodologies. An update to the present Tier 2 Air Screening Risk Assessment is in process for the Pemaco LTRA. 2. Refer to California Health and Safety Code 39655. "Toxic Air Contaminant" means an air pollutant which may cause or contribute to an increase in mortality or in serious illness, or which may pose a present or potential hazard to human health. A substance that is listed as a hazardous air pollutant pursuant to subsection (b) of Section 112 of the Federal Act (42 U.S.C. Sec. 7412 [b]) is a toxic air contaminant. As shown in Table 3, the MICR associated with potential exposure to the toxic air contaminants (TACs) at a distance of 75 meters from the stack is roughly four orders of magnitude less than “one in a million” (1 x 10‐6). Both the acute and chronic hazard indexes from potential exposure to TACs are less than one. Plant vapor emissions comply with the 2007 SCAQMD permit regulations. Destruction removal efficiency (DRE) is typically calculated to evaluate the performance of the VGAC and the vapor conditioning package. The DRE equals the mass difference between the influent and effluent divided by the total mass in the influent. The sum of VOCs detected in the influent was 1257 μg/m3; the sum of VOCs detected in the effluent was 302 μg/m3. The resulting DRE of 76% for May 2016 is satisfactory and represents a return to typical operational values following abnormally low DRE values for the months of March and April (‐315% and ‐38%, respectively). The increased DRE value is a response to VGAC changeout that was performed on May 10, 2016. OTIE oversaw replacement of spent carbon in one of the 4,000‐pound VGAC vessels (T‐301) by subcontractor Prominent Systems. The work was documented in Weekly Quality Control Field Report #379 and will be discussed further in the Second Quarter Operations and Maintenance Report. 5.0 CONCLUSIONS  During the month of May, the GTS achieved an uptime of 97% and the VTS achieved an uptime of 39%;

 ‘A’ Zone groundwater elevation measurements were collected approximately one month following shutdown of the ‘A’ Zone groundwater extraction wells. Elevation trends will be evaluated following additional rounds of monthly gauging;

 Results of the May 2016 plant water and vapor sampling conducted on May 12, 2016 confirmed compliance with LACSD permit limits and 2007 SCAQMD permit guidance;  Concentrations of VOCs in influent water and vapor samples were generally within the range of typical concentrations detected during previous monthly sampling events;

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 The LGAC performance is satisfactory because the LACSD permit limits were satisfied and filter vessels continue to operate with acceptable head loss; and  Vapor effluent VOC concentrations and DRE values returned to satisfactory levels during the May monthly sampling event following changeout of the VGAC on May 10, 2016. 6.0 REFERENCES Oneida Total Integrated Enterprises (OTIE). 2015. Final Sampling and Analysis Plan (Field Sampling Plan and Quality Assurance Project Plan), Long‐Term Response Action for the Pemaco Remedial Action. September.

_____. 2016. Draft Semiannual Groundwater Monitoring Report, December 2015 Monitoring Event for the Pemaco Superfund Site Treatment Plant, Maywood, California. April.

South Coast Air Quality Management District (SCAQMD). 2005. Risk Assessment Procedures for Rules 1401 and 212 Version 7.0, Permit Application Package “L” Rules 1401 and 212 Version 7.0. July 1.

United States Environmental Protection Agency (U.S. EPA). 2005. Record of Decision, Pemaco Maywood Superfund Site, Maywood, California. EPA ID: CAD980737092. January 13.

ATTACHMENTS Attachment 1 May 2016 ‘A’ Zone Groundwater Gauging Results Attachment 2 Lab Report from Eurofins CalScience, Inc. Attachment 3 Lab Report from ALS Environmental Attachment 4 Tier 2 Air Screening Risk Assessment for VOCs to Nearest Receptor, Approximately 75 Meters from Stack, Pemaco Superfund Site, Maywood, California

Oneida Total Integrated Enterprises Page 9 of 9 ATTACHMENT 1

May 2016 'A' Zone Groundwater Gauging Results Attachment 1 May 2016 'A' Zone Groundwater Gauging Results Pemaco Superfund Site, Maywood, California

December 4, 20151 May 26, 20161 Change in Screen Depth to Groundwater Depth to Groundwater Groundwater Interval Water Elevation Water Elevation Elevation Well ID Well Type (ft btoc) (ft btoc) (ft amsl) (ft btoc) (ft amsl) (ft) 1MW‐01‐80 Monitoring 59 ‐ 79 75.48 73.08 75.53 73.03 ‐0.05 2MW‐03‐70 Monitoring 60 ‐ 70 Dry Dry Dry Dry ‐‐ 3MW‐04‐75 Monitoring 65 ‐ 75 70.75 75.32 70.68 75.39 0.07 4MW‐07‐75 Monitoring 65 ‐ 75 64.11 75.21 64.89 74.43 ‐0.78 5MW‐08‐70 Monitoring 63 ‐ 68 Dry Dry Dry Dry ‐‐ 6MW‐09‐70 Monitoring 65 ‐ 70 Dry Dry Dry Dry ‐‐ 7MW‐10‐75 Monitoring 68 ‐ 73 67.73 72.89 * ‐‐ ‐‐ 8MW‐12‐70 Monitoring 65 ‐ 70 Dry Dry Dry Dry ‐‐ 9MW‐14‐80 Monitoring 76 ‐ 81 75.67 73.88 75.41 74.14 0.26 10 MW‐19‐70 Monitoring 62 ‐ 67 Dry Dry Dry Dry ‐‐ 11 MW‐20‐70 Monitoring 63 ‐ 68 Dry Dry Dry Dry ‐‐ 12 MW‐21‐80 Monitoring 68 ‐ 78 74.16 74.23 74.19 74.20 ‐0.03 13 MW‐22‐75 Monitoring 69 ‐ 74 Dry Dry Dry Dry ‐‐ 14 MW‐26‐75 Monitoring 65 ‐ 75 Dry Dry 73.82 72.28 ‐‐ 15 MW‐27‐70 Monitoring 60 ‐ 70 Dry Dry Dry Dry ‐‐ 16 RW‐01‐70 Monitoring 55 ‐ 70 Dry Dry Dry Dry ‐‐ 17 WW‐MW‐30A Monitoring 61 ‐ 66 NM ‐‐ 65.72 75.12 ‐‐ 18 MW‐36‐80 Monitoring 67.5 ‐ 77.5 69.15 74.83 69.25 74.73 ‐0.1 19 MW‐37‐80 Monitoring 68 ‐ 78 69.83 72.61 69.82 72.60 0.01 20 MW‐38‐80 Monitoring 67.5 ‐ 77.5 69.51 73.02 69.63 72.90 ‐0.12 21 DA‐01 Extraction 61 ‐ 76 68.11 72.60 70.20 70.51 ‐2.09 22 DA‐02 Extraction 72 ‐ 82 67.48 71.22 67.41 71.29 0.07 23 DA‐03 Extraction 74 ‐ 84 67.85 71.07 67.64 71.28 0.21 24 DA‐04 Extraction 56 ‐ 66 Dry Dry Dry Dry ‐‐ 25 DA‐05 Extraction 68 ‐ 78 * ‐‐ 69.81 71.50 ‐‐ 26 DA‐06 Extraction 60 ‐ 70 Dry Dry Dry Dry ‐‐ 27 DA‐07 Extraction 61 ‐ 71 Dry Dry 65.93 79.34 ‐‐ 28 DA‐08 Extraction 65 ‐ 75 * ‐‐ 66.89 73.74 ‐‐ 29 DA‐09 Extraction 66 ‐ 76 Dry Dry Dry Dry ‐‐ 20 DA‐10 Extraction 66 ‐ 76 Dry Dry Dry Dry ‐‐ 21 DA‐11 Extraction 64 ‐ 74 NM ‐‐ Dry Dry ‐‐ 32 DA‐12 Extraction 66 ‐ 76 65.58 78.04 68.53 75.09 ‐2.95 Notes: 1) Gauging data from the December 2015 semiannual groundwater monitoring event under dynamic (pumping) conditions. 2) Gauging data from May 26, 2016 under static (non‐pumping) conditions. 'A' Zone groundwater extraction wells were shut down on April 28,2016. 3) "*" indicates the water level could not be determined due to the presence of an in‐well pump. Acronyms: amsl = above mean sea level; btoc = below top of casing; ft = feet; NM = not measured; "‐‐" = not available.

OTIE Page 1 of 1 ATTACHMENT 2

Lab Report from Eurofins CalScience, Inc. Page 1 of 29

WORK ORDER NUMBER: 16-05-0912

AIR SOIL WATER MARINE CHEMISTRY

Analytical Report For Client: OTIE Client Project Name: Pemaco / 2014166 Attention: Orval Osborne 317 East Main Street Ventura, CA 93001-2624

Approved for release on 05/27/2016 by: Virendra Patel Project Manager

Eurofins Calscience, Inc. (Calscience) certifies that the test results provided in this report meet all NELAC requirements for parameters for which accreditation is required or available. Any exceptions to NELAC requirements are noted in the case narrative. The original report of subcontracted analyses, if any, is attached to this report. The results in this report are limited to the sample(s) tested and any reproduction thereof must be made in its entirety. The client or recipient of this report is specifically prohibited from making material changes to said report and, to the extent that such changes are made, Calscience is not responsible, legally or otherwise. The client or recipient agrees to indemnify Calscience for any defense to any litigation which may arise. Page 2 of 29

Contents Client Project Name: Pemaco / 2014166 Work Order Number: 16-05-0912

1 Work Order Narrative...... 3

2 Sample Summary...... 4

3 QC Association Summary...... 5

4 Detections Summary...... 6

5 Client Sample Data...... 7 5.1 EPA 8260 SIM 1,4-Dioxane (Aqueous)...... 7 5.2 EPA 8260B Volatile Organics (Aqueous)...... 8

6 Quality Control Sample Data...... 14 6.1 MS/MSD...... 14 6.2 LCS/LCSD...... 20

7 Sample Analysis Summary...... 26

8 Glossary of Terms and Qualifiers...... 27

9 Chain-of-Custody/Sample Receipt Form...... 28

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Work Order Narrative

Work Order: 16-05-0912 Page 1 of 1

Condition Upon Receipt: Samples were received under Chain-of-Custody (COC) on 05/12/16. They were assigned to Work Order 16-05-0912. Unless otherwise noted on the Sample Receiving forms all samples were received in good condition and within the recommended EPA temperature criteria for the methods noted on the COC. The COC and Sample Receiving Documents are integral elements of the analytical report and are presented at the back of the report. Holding Times: All samples were analyzed within prescribed holding times (HT) and/or in accordance with the Calscience Sample Acceptance Policy unless otherwise noted in the analytical report and/or comprehensive case narrative, if required. Any parameter identified in 40CFR Part 136.3 Table II that is designated as "analyze immediately" with a holding time of <= 15 minutes (40CFR-136.3 Table II, footnote 4), is considered a "field" test and the reported results will be qualified as being received outside of the stated holding time unless received at the laboratory within 15 minutes of the collection time. Quality Control: All quality control parameters (QC) were within established control limits except where noted in the QC summary forms or described further within this report. Subcontractor Information: Return to Contents Unless otherwise noted below (or on the subcontract form), no samples were subcontracted. Additional Comments: Air - Sorbent-extracted air methods (EPA TO-4A, EPA TO-10, EPA TO-13A, EPA TO-17): Analytical results are converted from mass/sample basis to mass/volume basis using client-supplied air volumes. Solid - Unless otherwise indicated, solid sample data is reported on a wet weight basis, not corrected for % moisture. All QC results are always reported on a wet weight basis.

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Sample Summary

Client: OTIE Work Order: 16-05-0912 317 East Main Street Project Name: Pemaco / 2014166 Ventura, CA 93001-2624 PO Number: 2014166 Date/Time 05/12/16 12:22 Received: Number of 20 Containers: Attn: Orval Osborne

Sample Identification Lab Number Collection Date and Time Number of Matrix Containers SP-201-20160512 16-05-0912-1 05/12/16 08:00 10 Aqueous SP-209-20160512 16-05-0912-2 05/12/16 07:30 10 Aqueous Return to Contents

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QC Association Summary

Work Order: 16-05-0912 Page 1 of 1

Client Sample ID Method Name Type Ext Name Instrument MS/MSD/SDP LCS/LCSD SP-201-20160512 EPA 8260 SIM 1,4-Dioxane EPA 5030C GC/MS M 160518S009 160518L043 SP-201-20160512 EPA 8260B Volatile Organics EPA 5030C GC/MS V V 160512S020 160512L053 SP-209-20160512 EPA 8260 SIM 1,4-Dioxane EPA 5030C GC/MS M 160517S011 160517L038 SP-209-20160512 EPA 8260B Volatile Organics EPA 5030C GC/MS V V 160512S020 160512L053 Return to Contents

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Detections Summary

Client: OTIE Work Order: 16-05-0912 317 East Main Street Project Name: Pemaco / 2014166 Ventura, CA 93001-2624 Received: 05/12/16 Attn: Orval Osborne Page 1 of 1

Client SampleID Analyte Result Qualifiers RL Units Method Extraction

SP-201-20160512 (16-05-0912-1) 1,4-Dioxane 7.9 J 3.5* ug/L EPA 8260 SIM EPA 5030C c-1,2-Dichloroethene 9.9 1.0 ug/L EPA 8260B EPA 5030C Trichloroethene 84 1.0 ug/L EPA 8260B EPA 5030C SP-209-20160512 (16-05-0912-2) 1,4-Dioxane 8.6 1.0 ug/L EPA 8260 SIM EPA 5030C Chloroform 0.92 J 0.46* ug/L EPA 8260B EPA 5030C 1,1-Dichloroethane 1.1 1.0 ug/L EPA 8260B EPA 5030C c-1,2-Dichloroethene 5.0 1.0 ug/L EPA 8260B EPA 5030C Trichloroethene 0.40 J 0.37* ug/L EPA 8260B EPA 5030C

Subcontracted analyses, if any, are not included in this summary. Return to Contents

* MDL is shown

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Units: ug/L Project: Pemaco / 2014166 Page 1 of 1

Client Sample Number Lab Sample Date/Time Matrix Instrument Date Date/Time QC Batch ID Number Collected Prepared Analyzed SP-201-20160512 16-05-0912-1-H 05/12/16 Aqueous GC/MS M 05/18/16 05/18/16 160518L043 08:00 15:46 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers 1,4-Dioxane 7.9 10 3.5 10.0 J

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Dichlorobutane 91 80-120

SP-209-20160512 16-05-0912-2-G 05/12/16 Aqueous GC/MS M 05/17/16 05/17/16 160517L038 07:30 21:36 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers 1,4-Dioxane 8.6 1.0 0.35 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Dichlorobutane 107 80-120 Return to Contents

Method Blank 099-16-536-68 N/A Aqueous GC/MS M 05/17/16 05/17/16 160517L038 12:24 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers 1,4-Dioxane ND 1.0 0.35 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Dichlorobutane 116 80-120

Method Blank 099-16-536-69 N/A Aqueous GC/MS M 05/18/16 05/18/16 160518L043 11:25 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers 1,4-Dioxane ND 1.0 0.35 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Dichlorobutane 104 80-120

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 1 of 6

Client Sample Number Lab Sample Date/Time Matrix Instrument Date Date/Time QC Batch ID Number Collected Prepared Analyzed SP-201-20160512 16-05-0912-1-A 05/12/16 Aqueous GC/MS V V 05/12/16 05/13/16 160512L053 08:00 11:16 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers Acetone ND 20 10 1.00 Benzene ND 0.50 0.14 1.00 Bromobenzene ND 1.0 0.30 1.00 Bromochloromethane ND 1.0 0.48 1.00 Bromodichloromethane ND 1.0 0.21 1.00 Bromoform ND 1.0 0.50 1.00 Bromomethane ND 10 3.9 1.00 2-Butanone ND 10 4.4 1.00 n-Butylbenzene ND 1.0 0.23 1.00 sec-Butylbenzene ND 1.0 0.25 1.00 tert-Butylbenzene ND 1.0 0.28 1.00 Carbon Disulfide ND 10 4.1 1.00 Carbon Tetrachloride ND 0.50 0.23 1.00 Return to Contents Chlorobenzene ND 1.0 0.17 1.00 Chloroethane ND 5.0 2.3 1.00 Chloroform ND 1.0 0.46 1.00 Chloromethane ND 10 3.5 1.00 2-Chlorotoluene ND 1.0 0.24 1.00 4-Chlorotoluene ND 1.0 0.13 1.00 Dibromochloromethane ND 1.0 0.25 1.00 1,2-Dibromo-3-Chloropropane ND 5.0 1.2 1.00 1,2-Dibromoethane ND 1.0 0.36 1.00 Dibromomethane ND 1.0 0.46 1.00 1,2-Dichlorobenzene ND 1.0 0.46 1.00 1,3-Dichlorobenzene ND 1.0 0.40 1.00 1,4-Dichlorobenzene ND 1.0 0.43 1.00 Dichlorodifluoromethane ND 1.0 0.46 1.00 1,1-Dichloroethane ND 1.0 0.28 1.00 1,2-Dichloroethane ND 0.50 0.24 1.00 1,1-Dichloroethene ND 1.0 0.43 1.00 c-1,2-Dichloroethene 9.9 1.0 0.48 1.00 t-1,2-Dichloroethene ND 1.0 0.37 1.00 1,2-Dichloropropane ND 1.0 0.42 1.00 1,3-Dichloropropane ND 1.0 0.30 1.00

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 2 of 6

Parameter Result RL MDL DF Qualifiers 2,2-Dichloropropane ND 1.0 0.36 1.00 1,1-Dichloropropene ND 1.0 0.46 1.00 c-1,3-Dichloropropene ND 0.50 0.25 1.00 t-1,3-Dichloropropene ND 0.50 0.25 1.00 Ethylbenzene ND 1.0 0.14 1.00 2-Hexanone ND 10 4.2 1.00 Isopropylbenzene ND 1.0 0.58 1.00 p-Isopropyltoluene ND 1.0 0.16 1.00 Methylene Chloride ND 10 3.8 1.00 4-Methyl-2-Pentanone ND 10 4.4 1.00 Naphthalene ND 10 5.0 1.00 n-Propylbenzene ND 1.0 0.17 1.00 Styrene ND 1.0 0.17 1.00 1,1,1,2-Tetrachloroethane ND 1.0 0.40 1.00 1,1,2,2-Tetrachloroethane ND 1.0 0.41 1.00 Tetrachloroethene ND 1.0 0.39 1.00

Toluene ND 1.0 0.24 1.00 Return to Contents 1,2,3-Trichlorobenzene ND 1.0 0.51 1.00 1,2,4-Trichlorobenzene ND 1.0 0.50 1.00 1,1,1-Trichloroethane ND 1.0 0.30 1.00 1,1,2-Trichloro-1,2,2-Trifluoroethane ND 10 3.9 1.00 1,1,2-Trichloroethane ND 1.0 0.38 1.00 Trichloroethene 84 1.0 0.37 1.00 Trichlorofluoromethane ND 10 3.3 1.00 1,2,3-Trichloropropane ND 5.0 0.64 1.00 1,2,4-Trimethylbenzene ND 1.0 0.36 1.00 1,3,5-Trimethylbenzene ND 1.0 0.28 1.00 Vinyl Acetate ND 10 5.6 1.00 Vinyl Chloride ND 0.50 0.30 1.00 p/m-Xylene ND 1.0 0.30 1.00 o-Xylene ND 1.0 0.23 1.00 Methyl-t-Butyl Ether (MTBE) ND 1.0 0.31 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Bromofluorobenzene 88 80-120 Dibromofluoromethane 115 78-126 1,2-Dichloroethane-d4 104 75-135 Toluene-d8 110 80-120

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 3 of 6

Client Sample Number Lab Sample Date/Time Matrix Instrument Date Date/Time QC Batch ID Number Collected Prepared Analyzed SP-209-20160512 16-05-0912-2-A 05/12/16 Aqueous GC/MS V V 05/12/16 05/13/16 160512L053 07:30 07:36 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers Acetone ND 20 10 1.00 Benzene ND 0.50 0.14 1.00 Bromobenzene ND 1.0 0.30 1.00 Bromochloromethane ND 1.0 0.48 1.00 Bromodichloromethane ND 1.0 0.21 1.00 Bromoform ND 1.0 0.50 1.00 Bromomethane ND 10 3.9 1.00 2-Butanone ND 10 4.4 1.00 n-Butylbenzene ND 1.0 0.23 1.00 sec-Butylbenzene ND 1.0 0.25 1.00 tert-Butylbenzene ND 1.0 0.28 1.00 Carbon Disulfide ND 10 4.1 1.00 Carbon Tetrachloride ND 0.50 0.23 1.00 Return to Contents Chlorobenzene ND 1.0 0.17 1.00 Chloroethane ND 5.0 2.3 1.00 Chloroform 0.92 1.0 0.46 1.00 J Chloromethane ND 10 3.5 1.00 2-Chlorotoluene ND 1.0 0.24 1.00 4-Chlorotoluene ND 1.0 0.13 1.00 Dibromochloromethane ND 1.0 0.25 1.00 1,2-Dibromo-3-Chloropropane ND 5.0 1.2 1.00 1,2-Dibromoethane ND 1.0 0.36 1.00 Dibromomethane ND 1.0 0.46 1.00 1,2-Dichlorobenzene ND 1.0 0.46 1.00 1,3-Dichlorobenzene ND 1.0 0.40 1.00 1,4-Dichlorobenzene ND 1.0 0.43 1.00 Dichlorodifluoromethane ND 1.0 0.46 1.00 1,1-Dichloroethane 1.1 1.0 0.28 1.00 1,2-Dichloroethane ND 0.50 0.24 1.00 1,1-Dichloroethene ND 1.0 0.43 1.00 c-1,2-Dichloroethene 5.0 1.0 0.48 1.00 t-1,2-Dichloroethene ND 1.0 0.37 1.00 1,2-Dichloropropane ND 1.0 0.42 1.00 1,3-Dichloropropane ND 1.0 0.30 1.00

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 4 of 6

Parameter Result RL MDL DF Qualifiers 2,2-Dichloropropane ND 1.0 0.36 1.00 1,1-Dichloropropene ND 1.0 0.46 1.00 c-1,3-Dichloropropene ND 0.50 0.25 1.00 t-1,3-Dichloropropene ND 0.50 0.25 1.00 Ethylbenzene ND 1.0 0.14 1.00 2-Hexanone ND 10 4.2 1.00 Isopropylbenzene ND 1.0 0.58 1.00 p-Isopropyltoluene ND 1.0 0.16 1.00 Methylene Chloride ND 10 3.8 1.00 4-Methyl-2-Pentanone ND 10 4.4 1.00 Naphthalene ND 10 5.0 1.00 n-Propylbenzene ND 1.0 0.17 1.00 Styrene ND 1.0 0.17 1.00 1,1,1,2-Tetrachloroethane ND 1.0 0.40 1.00 1,1,2,2-Tetrachloroethane ND 1.0 0.41 1.00 Tetrachloroethene ND 1.0 0.39 1.00

Toluene ND 1.0 0.24 1.00 Return to Contents 1,2,3-Trichlorobenzene ND 1.0 0.51 1.00 1,2,4-Trichlorobenzene ND 1.0 0.50 1.00 1,1,1-Trichloroethane ND 1.0 0.30 1.00 1,1,2-Trichloro-1,2,2-Trifluoroethane ND 10 3.9 1.00 1,1,2-Trichloroethane ND 1.0 0.38 1.00 Trichloroethene 0.40 1.0 0.37 1.00 J Trichlorofluoromethane ND 10 3.3 1.00 1,2,3-Trichloropropane ND 5.0 0.64 1.00 1,2,4-Trimethylbenzene ND 1.0 0.36 1.00 1,3,5-Trimethylbenzene ND 1.0 0.28 1.00 Vinyl Acetate ND 10 5.6 1.00 Vinyl Chloride ND 0.50 0.30 1.00 p/m-Xylene ND 1.0 0.30 1.00 o-Xylene ND 1.0 0.23 1.00 Methyl-t-Butyl Ether (MTBE) ND 1.0 0.31 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Bromofluorobenzene 100 80-120 Dibromofluoromethane 111 78-126 1,2-Dichloroethane-d4 103 75-135 Toluene-d8 97 80-120

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 5 of 6

Client Sample Number Lab Sample Date/Time Matrix Instrument Date Date/Time QC Batch ID Number Collected Prepared Analyzed Method Blank 099-14-001-20328 N/A Aqueous GC/MS V V 05/12/16 05/13/16 160512L053 04:51 Comment(s): - Results were evaluated to the MDL (DL), concentrations >= to the MDL (DL) but < RL (LOQ), if found, are qualified with a "J" flag. Parameter Result RL MDL DF Qualifiers Acetone ND 20 10 1.00 Benzene ND 0.50 0.14 1.00 Bromobenzene ND 1.0 0.30 1.00 Bromochloromethane ND 1.0 0.48 1.00 Bromodichloromethane ND 1.0 0.21 1.00 Bromoform ND 1.0 0.50 1.00 Bromomethane ND 10 3.9 1.00 2-Butanone ND 10 4.4 1.00 n-Butylbenzene ND 1.0 0.23 1.00 sec-Butylbenzene ND 1.0 0.25 1.00 tert-Butylbenzene ND 1.0 0.28 1.00 Carbon Disulfide ND 10 4.1 1.00 Carbon Tetrachloride ND 0.50 0.23 1.00 Return to Contents Chlorobenzene ND 1.0 0.17 1.00 Chloroethane ND 5.0 2.3 1.00 Chloroform ND 1.0 0.46 1.00 Chloromethane ND 10 3.5 1.00 2-Chlorotoluene ND 1.0 0.24 1.00 4-Chlorotoluene ND 1.0 0.13 1.00 Dibromochloromethane ND 1.0 0.25 1.00 1,2-Dibromo-3-Chloropropane ND 5.0 1.2 1.00 1,2-Dibromoethane ND 1.0 0.36 1.00 Dibromomethane ND 1.0 0.46 1.00 1,2-Dichlorobenzene ND 1.0 0.46 1.00 1,3-Dichlorobenzene ND 1.0 0.40 1.00 1,4-Dichlorobenzene ND 1.0 0.43 1.00 Dichlorodifluoromethane ND 1.0 0.46 1.00 1,1-Dichloroethane ND 1.0 0.28 1.00 1,2-Dichloroethane ND 0.50 0.24 1.00 1,1-Dichloroethene ND 1.0 0.43 1.00 c-1,2-Dichloroethene ND 1.0 0.48 1.00 t-1,2-Dichloroethene ND 1.0 0.37 1.00 1,2-Dichloropropane ND 1.0 0.42 1.00 1,3-Dichloropropane ND 1.0 0.30 1.00

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Analytical Report

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Units: ug/L Project: Pemaco / 2014166 Page 6 of 6

Parameter Result RL MDL DF Qualifiers 2,2-Dichloropropane ND 1.0 0.36 1.00 1,1-Dichloropropene ND 1.0 0.46 1.00 c-1,3-Dichloropropene ND 0.50 0.25 1.00 t-1,3-Dichloropropene ND 0.50 0.25 1.00 Ethylbenzene ND 1.0 0.14 1.00 2-Hexanone ND 10 4.2 1.00 Isopropylbenzene ND 1.0 0.58 1.00 p-Isopropyltoluene ND 1.0 0.16 1.00 Methylene Chloride ND 10 3.8 1.00 4-Methyl-2-Pentanone ND 10 4.4 1.00 Naphthalene ND 10 5.0 1.00 n-Propylbenzene ND 1.0 0.17 1.00 Styrene ND 1.0 0.17 1.00 1,1,1,2-Tetrachloroethane ND 1.0 0.40 1.00 1,1,2,2-Tetrachloroethane ND 1.0 0.41 1.00 Tetrachloroethene ND 1.0 0.39 1.00

Toluene ND 1.0 0.24 1.00 Return to Contents 1,2,3-Trichlorobenzene ND 1.0 0.51 1.00 1,2,4-Trichlorobenzene ND 1.0 0.50 1.00 1,1,1-Trichloroethane ND 1.0 0.30 1.00 1,1,2-Trichloro-1,2,2-Trifluoroethane ND 10 3.9 1.00 1,1,2-Trichloroethane ND 1.0 0.38 1.00 Trichloroethene ND 1.0 0.37 1.00 Trichlorofluoromethane ND 10 3.3 1.00 1,2,3-Trichloropropane ND 5.0 0.64 1.00 1,2,4-Trimethylbenzene ND 1.0 0.36 1.00 1,3,5-Trimethylbenzene ND 1.0 0.28 1.00 Vinyl Acetate ND 10 5.6 1.00 Vinyl Chloride ND 0.50 0.30 1.00 p/m-Xylene ND 1.0 0.30 1.00 o-Xylene ND 1.0 0.23 1.00 Methyl-t-Butyl Ether (MTBE) ND 1.0 0.31 1.00

Surrogate Rec. (%) Control Limits Qualifiers 1,4-Bromofluorobenzene 105 80-120 Dibromofluoromethane 102 78-126 1,2-Dichloroethane-d4 107 75-135 Toluene-d8 97 80-120

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Quality Control - Spike/Spike Duplicate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 1 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-0923-1 Sample Aqueous GC/MS M 05/17/16 05/17/16 12:53 160517S011 16-05-0923-1 Matrix Spike Aqueous GC/MS M 05/17/16 05/17/16 14:49 160517S011 16-05-0923-1 Matrix Spike Duplicate Aqueous GC/MS M 05/17/16 05/17/16 15:18 160517S011 Parameter Sample Spike MS MS MSD MSD %Rec. CL RPD RPD CL Qualifiers Conc. Added Conc. %Rec. Conc. %Rec. 1,4-Dioxane ND 20.00 17.55 88 21.00 105 80-120 18 0-20 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

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Spike/Spike Duplicate - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 2 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-0923-1 Sample Aqueous GC/MS M 05/17/16 05/17/16 12:53 160517S011 16-05-0923-1 Matrix Spike Aqueous GC/MS M 05/17/16 05/17/16 14:49 160517S011 16-05-0923-1 Matrix Spike Duplicate Aqueous GC/MS M 05/17/16 05/17/16 15:18 160517S011 Parameter Spike Added MS Conc. MS %Rec. MSD Conc. MSD %Rec. %Rec. CL Qualifiers 1,4-Dichlorobutane 8.000 9.512 119 11.71 146 80-120 2 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

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Quality Control - Spike/Spike Duplicate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 3 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-1051-4 Sample Aqueous GC/MS M 05/18/16 05/18/16 11:54 160518S009 16-05-1051-4 Matrix Spike Aqueous GC/MS M 05/18/16 05/18/16 13:50 160518S009 16-05-1051-4 Matrix Spike Duplicate Aqueous GC/MS M 05/18/16 05/18/16 14:19 160518S009 Parameter Sample Spike MS MS MSD MSD %Rec. CL RPD RPD CL Qualifiers Conc. Added Conc. %Rec. Conc. %Rec. 1,4-Dioxane 22.45 20.00 41.99 98 45.07 113 80-120 7 0-20 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

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Spike/Spike Duplicate - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 4 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-1051-4 Sample Aqueous GC/MS M 05/18/16 05/18/16 11:54 160518S009 16-05-1051-4 Matrix Spike Aqueous GC/MS M 05/18/16 05/18/16 13:50 160518S009 16-05-1051-4 Matrix Spike Duplicate Aqueous GC/MS M 05/18/16 05/18/16 14:19 160518S009 Parameter Spike Added MS Conc. MS %Rec. MSD Conc. MSD %Rec. %Rec. CL Qualifiers 1,4-Dichlorobutane 8.000 9.192 115 8.939 112 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

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Quality Control - Spike/Spike Duplicate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Project: Pemaco / 2014166 Page 5 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-0902-2 Sample Aqueous GC/MS V V 05/12/16 05/13/16 05:46 160512S020 16-05-0902-2 Matrix Spike Aqueous GC/MS V V 05/12/16 05/13/16 03:29 160512S020 16-05-0902-2 Matrix Spike Duplicate Aqueous GC/MS V V 05/12/16 05/13/16 03:56 160512S020 Parameter Sample Spike MS MS MSD MSD %Rec. CL RPD RPD CL Qualifiers Conc. Added Conc. %Rec. Conc. %Rec. Benzene ND 50.00 54.32 109 55.54 111 74-122 2 0-21 Carbon Tetrachloride ND 50.00 61.64 123 66.68 133 60-144 8 0-21 Chlorobenzene ND 50.00 57.01 114 49.48 99 73-120 14 0-22 1,2-Dibromoethane ND 50.00 55.04 110 52.15 104 80-122 5 0-20 1,2-Dichlorobenzene ND 50.00 52.45 105 52.62 105 70-120 0 0-26 1,2-Dichloroethane ND 50.00 52.65 105 52.63 105 64-142 0 0-20 1,1-Dichloroethene ND 50.00 51.06 102 52.70 105 52-136 3 0-21 Ethylbenzene ND 50.00 58.71 117 56.86 114 77-125 3 0-24 Toluene ND 50.00 57.44 115 53.90 108 72-126 6 0-23 Trichloroethene ND 50.00 53.01 106 52.14 104 74-128 2 0-22 Vinyl Chloride ND 50.00 46.64 93 49.91 100 67-133 7 0-20 p/m-Xylene ND 100.0 113.3 113 104.7 105 63-129 8 0-25 o-Xylene ND 50.00 60.03 120 55.61 111 62-128 8 0-24 Return to Contents Methyl-t-Butyl Ether (MTBE) ND 50.00 60.69 121 61.24 122 68-134 1 0-21

RPD: Relative Percent Difference. CL: Control Limits

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Spike/Spike Duplicate - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Project: Pemaco / 2014166 Page 6 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number 16-05-0902-2 Sample Aqueous GC/MS V V 05/12/16 05/13/16 05:46 160512S020 16-05-0902-2 Matrix Spike Aqueous GC/MS V V 05/12/16 05/13/16 03:29 160512S020 16-05-0902-2 Matrix Spike Duplicate Aqueous GC/MS V V 05/12/16 05/13/16 03:56 160512S020 Parameter Spike Added MS Conc. MS %Rec. MSD Conc. MSD %Rec. %Rec. CL Qualifiers 1,4-Bromofluorobenzene 50.00 52.78 106 50.22 100 80-120 Dibromofluoromethane 50.00 52.15 104 49.55 99 78-126 1,2-Dichloroethane-d4 50.00 47.89 96 50.78 102 75-135 Toluene-d8 50.00 49.85 100 47.70 95 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

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Quality Control - LCS

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 1 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-16-536-68 LCS Aqueous GC/MS M 05/17/16 05/17/16 11:26 160517L038 Parameter Spike Added Conc. Recovered LCS %Rec. %Rec. CL Qualifiers 1,4-Dioxane 20.00 19.57 98 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 21 of 29

LCS Only - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 2 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-16-536-68 LCS Aqueous GC/MS M 05/17/16 05/17/16 11:26 160517L038 Parameter Spike Added LCS Conc. LCS %Rec. %Rec. CL Qualifiers 1,4-Dichlorobutane 8.000 8.284 104 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 22 of 29

Quality Control - LCS

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 3 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-16-536-69 LCS Aqueous GC/MS M 05/18/16 05/18/16 10:25 160518L043 Parameter Spike Added Conc. Recovered LCS %Rec. %Rec. CL Qualifiers 1,4-Dioxane 20.00 18.22 91 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 23 of 29

LCS Only - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260 SIM Project: Pemaco / 2014166 Page 4 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-16-536-69 LCS Aqueous GC/MS M 05/18/16 05/18/16 10:25 160518L043 Parameter Spike Added LCS Conc. LCS %Rec. %Rec. CL Qualifiers 1,4-Dichlorobutane 8.000 6.666 83 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 24 of 29

Quality Control - LCS

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Project: Pemaco / 2014166 Page 5 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-14-001-20328 LCS Aqueous GC/MS V V 05/12/16 05/13/16 03:01 160512L053 Parameter Spike Added Conc. Recovered LCS %Rec. %Rec. CL ME CL Qualifiers Benzene 50.00 51.50 103 80-120 73-127 Carbon Tetrachloride 50.00 60.83 122 67-139 55-151 Chlorobenzene 50.00 54.27 109 78-120 71-127 1,2-Dibromoethane 50.00 53.73 107 80-120 73-127 1,2-Dichlorobenzene 50.00 50.77 102 63-129 52-140 1,2-Dichloroethane 50.00 50.21 100 70-130 60-140 1,1-Dichloroethene 50.00 48.20 96 66-126 56-136 Ethylbenzene 50.00 52.21 104 80-123 73-130 Toluene 50.00 49.85 100 80-120 73-127 Trichloroethene 50.00 49.98 100 80-122 73-129 Vinyl Chloride 50.00 43.09 86 70-130 60-140 p/m-Xylene 100.0 109.2 109 75-123 67-131 o-Xylene 50.00 56.90 114 74-122 66-130 Methyl-t-Butyl Ether (MTBE) 50.00 60.75 122 69-129 59-139

Total number of LCS compounds: 14 Return to Contents Total number of ME compounds: 0 Total number of ME compounds allowed: 1 LCS ME CL validation result: Pass

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 25 of 29

LCS Only - Surrogate

OTIE Date Received: 05/12/16 317 East Main Street Work Order: 16-05-0912 Ventura, CA 93001-2624 Preparation: EPA 5030C Method: EPA 8260B Project: Pemaco / 2014166 Page 6 of 6

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number 099-14-001-20328 LCS Aqueous GC/MS V V 05/12/16 05/13/16 03:01 160512L053 Parameter Spike Added LCS Conc. LCS %Rec. %Rec. CL Qualifiers 1,4-Bromofluorobenzene 50.00 52.90 106 80-120 Dibromofluoromethane 50.00 49.62 99 78-126 1,2-Dichloroethane-d4 50.00 49.82 100 75-135 Toluene-d8 50.00 49.72 99 80-120 Return to Contents

RPD: Relative Percent Difference. CL: Control Limits

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 26 of 29

Sample Analysis Summary Report

Work Order: 16-05-0912 Page 1 of 1

Method Extraction Chemist ID Instrument Analytical Location EPA 8260 SIM EPA 5030C 486 GC/MS M 2 EPA 8260B EPA 5030C 1073 GC/MS V V 2 Return to Contents

Location 2: 7445 Lampson Avenue, Garden Grove, CA 92841

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Page 27 of 29

Glossary of Terms and Qualifiers

Work Order: 16-05-0912 Page 1 of 1

Qualifiers Definition * See applicable analysis comment. < Less than the indicated value. > Greater than the indicated value. 1 Surrogate compound recovery was out of control due to a required sample dilution. Therefore, the sample data was reported without further clarification. 2 Surrogate compound recovery was out of control due to matrix interference. The associated method blank surrogate spike compound was in control and, therefore, the sample data was reported without further clarification. 3 Recovery of the Matrix Spike (MS) or Matrix Spike Duplicate (MSD) compound was out of control due to suspected matrix interference. The associated LCS recovery was in control. 4 The MS/MSD RPD was out of control due to suspected matrix interference. 5 The PDS/PDSD or PES/PESD associated with this batch of samples was out of control due to suspected matrix interference. 6 Surrogate recovery below the acceptance limit. 7 Surrogate recovery above the acceptance limit. B Analyte was present in the associated method blank. BU Sample analyzed after holding time expired. BV Sample received after holding time expired. CI See case narrative. E Concentration exceeds the calibration range. ET Sample was extracted past end of recommended max. holding time. HD The chromatographic pattern was inconsistent with the profile of the reference fuel standard. HDH The sample chromatographic pattern for TPH matches the chromatographic pattern of the specified standard but heavier hydrocarbons were also present (or detected). HDL The sample chromatographic pattern for TPH matches the chromatographic pattern of the specified standard but lighter hydrocarbons were also present (or detected). J Analyte was detected at a concentration below the reporting limit and above the laboratory method detection limit. Reported value is Return to Contents estimated. JA Analyte positively identified but quantitation is an estimate. ME LCS Recovery Percentage is within Marginal Exceedance (ME) Control Limit range (+/- 4 SD from the mean). ND Parameter not detected at the indicated reporting limit. Q Spike recovery and RPD control limits do not apply resulting from the parameter concentration in the sample exceeding the spike concentration by a factor of four or greater. SG The sample extract was subjected to Silica Gel treatment prior to analysis. X % Recovery and/or RPD out-of-range. Z Analyte presence was not confirmed by second column or GC/MS analysis. Solid - Unless otherwise indicated, solid sample data is reported on a wet weight basis, not corrected for % moisture. All QC results are reported on a wet weight basis. Any parameter identified in 40CFR Part 136.3 Table II that is designated as "analyze immediately" with a holding time of <= 15 minutes (40CFR-136.3 Table II, footnote 4), is considered a "field" test and the reported results will be qualified as being received outside of the stated holding time unless received at the laboratory within 15 minutes of the collection time. A calculated total result (Example: Total Pesticides) is the summation of each component concentration and/or, if "J" flags are reported, estimated concentration. Component concentrations showing not detected (ND) are summed into the calculated total result as zero concentrations.

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501 Chain of Custody Report To: Bill To: Shaded Areas For Internal Use Only 1 of 1 Contact: Orval Osborne Contact Accounts Payable Lab Lot# Company: OTIE Company: OTIE

I· _._f>_a__ ·:·.··.t_•-••.- .·.·_l ... Address: 317 East Main Street Address: 1033 N. Mayfair Road, Ste 200 L 5· 0 ···.

Project Name: Pemaco - Project Number: 2014166 2014166

Project Location: 5973 S. District Date Requested: NTAT M G . $afoptet~t,>eis.ahdcoo Agree ··.··-· Blvd Marn.,ood CA 90270 t r X a Yes< No cqonatpres~nr_· · Lab PM: Virendra Patel, CalScience b 714-895-5494 - 0 ~ :ii (!) N 0(/)x- Q() MS Sampling # of ·-oo ' LabClratory Client ' co 0 0 ·10 MSD Sample ID Date Time Cont. ~-" Additional Analyses I Remarks I SP-201-20160512 05/12/16 0800 10 w X X X pH grab sample measured at 0730 SP-209-20160512 05/12/16 0730 10 w X X X = 7.46 from SP-209

I I I RELINQUISHED BY}.. J / J COMPANY TIME RECjjV EO BY COMPANY ~tTE_ J TIME DATE os:(/2 {& l 'J,,tb-..J t-1owl/ At'JI... 0·71~ ..VA ' b-1 S"! / 2-lk I 'L-~ RELINOUISHEO BY COMPANY DATE TIME V COMPANY DATE t TIME Page 28of29 Matrix Key Container Key Preservative Key COMMENTS: WW = Wastewater SE = Sediment 1. Plastic 1. HCI, Cool lo 4' All samples are HCI preserved 40ml VOAs Date Received W = Water SO = Solid 2. VOA Vial 2. H2S04 , Cool l o 4' OTIE-soecific EDDs needed S = Soil DS = Drum Solid 3. Sterile Pla~tic 3. HN03 , Cool l o 4' Level 3 data packaqe Courier: Hand Delivered~ SL = Sludge DL = Drum Liquid 4. Amber Glass 4. NaOH. Cool to 4' Reoort to MDLs (J-flao) MS = Mlscellaneous L = Leachate 5. Widemouth Glass 5. NaOH/Zn Acetate, Cool to 4" OL = Oil WI = Wipe 6. Other 6. Cool to 4' Bill of Lading: (~ A =Air O= ___ _ _ 7. None

Return to Contents .. :::: CLIENT: •"- TEMPERATURE: Cooler Chain-of-Custody CUSTODY Sample(s) Thermometer Ambient Proper COC Sampler's Sample Samples Sufficient Sample SAMPLE D Proper D Container(s) CONTAINER Solid: T Air: Aqueous: Pr D Co ed es Sample(s) 125PBznna 500PB ntainer: D D D D Aqueous Unpreserved D D 9'Volatile D euro lar T D ervative Sample(s) Sample(s) document(s) No Sampling Volatile pH Ca ™ D containers p container(s) container ed!a re r Temperature: __ analysis 4ozCGJ received bag(s) bon CONDITION: volume/mass A= D D name serv D SEAL: : f .. r™ samples b s for VOA Residual received tns 1AGB Organics Dioxide Organics Amber, ID: 0--=-l_l TYPE: D D = = ation date D H buffer certain outside outside fr aq Present Present indicated D SC2A 2 requested ee (COC) label(s) (Criteria: 250AGB for S0 within received D u ¢ Canister chemical(s) eo int of D B 4 8ozCGJ (2_--_. e for analyses V~h . D (SM · , Calscience Chlorine at d D u ac = u co 1AGBna , analysis for (CF: s temperature temperature Sampling D D f Bottle ce holding = ambient and and document{s) Air t nd sample ------'----- = consistent on 4500) ult and analyses rtain Total Diss 0.0°C filtered complete D e ra 0.0°C); D Intact Intact D nsation COG D , D - 250CGB D in reque C pur 2 o Sorbent VOAna analyses Not free noted Filter D time Metals lved ( = 16ozCGJ good temperature; - , s) D e, time D C h Dissolved 6.0°C, ...... lear, received znna relinquished requested Temperature 1A = s with Ferrous criteria criteria of Gases SAMPLE ted received ...... HCI ···· on 2 condition ...... GB D D headspa Tube D D E D COC 0 · received = Present , COG Present but ··· D s noltrozen = n 250CGBs ... Matrix Z D 1 Dissolved but (PM/APM Env · n( = {RSK-175) OOPJ for ...... Iron ·· Sulfide C Sleeve{ HN0 D · placed with ..... and/or ..... · 1PB H ce e received · certain PUF · lope 3C . (SM ··· (w/o but .. .. D within 3 . . D 02 , D RECEIPT ...... samples . ·· . . , na No except .... D Number ) G Not Not _ ...... D on 1 . Metals ... 2 D 3500) contacted sa CF): . . D OOPJna . . . .. = + ana = 1PBna ...... relinquished 250PB mple _ . .... Dissolved on 15-minut ...... D ice _ Na Na G ...... Intact Intact ...... la ...... Dissolved lyses OH, ...... ) O ice/chilled sediment/tissue) _ for ...... lf .. ss .. H D ... container ...... of D 2 , . .. . _ ...... transport . . . . J na D .5 ...... Hydrogen Sulfide Hydrogen 2 D containers by: EnC . . D 1 D = e ...... CHECKLIST 2 ...... Oxygen Jar ...... holding = WORK . . Other 50 .. . 25 . date o Na . . . .. Oxygen , res . . . . on PBn °C ...... A ...... P .. . .. 2 . GB S . ® = . . by . . same (w/ 2 ...... L__) Matrix( ...... P 0 . (Trip D time ...... last courier ...... ORDER 3 . ... . D ) . . , . . D CF): .. ... D No (SM p ...... 500A ...... i . c, day 125AGBh . . . . = ...... Blank . . .. relinquished . . . .. H and _ .. . . (Hac ...... 4500) ...... 3 ...... 'f ...... D of P G ...... _ ...... 04 .. O B Z NUMBER: ...... Terra sampling . - h) Lot . . , = D D .. ___ S ...... Ziploc/Resealable ...... NIA NIA ...... D . . Cores® 500AGJ D Number: L ...... abe ...... 125AGBp . . °C; time ...... DATE: ...... ): ...... COOLER . . led . D . . . . D ...... D . 16-05- L__) Revie Yes /Checked __ Checked Checked Checked Ji Blank y{' .12('. .0 ~ ::: D D ~ ~ ___ 05 500AGJs Page 29of D w D _ Bag e / 12 2 ~mple _j_ __ D d 0 /J- 15 No by: by:\ by: 5PB D D D D D D by: by D D D D D D D D D D ___ __ D - 04 ~ : fl __ OF - l _ 0 10 / O q Sib __ ~b 2016 \, Re !': \1 _j_ N/A _

/2._ D D D D D rr D vi _ s

) i o · n

t

Return to Contents ATTACHMENT 3

Lab Report from ALS Environmental 2655 Park Center Dr., Suite A Simi Valley, CA 93065 T: +1 805 526 7161 F: +1 805 526 7270 www.alsglobal.com

LABORATORY REPORT

June 1, 2016

Orval Osborne Oneida Total Integrated Enterprises (OTIE) 317 E. Main St. Ventura, CA 93001

RE: Pemaco - Plant Vapor Monitoring

Dear Orval:

Enclosed are the results of the samples submitted to our laboratory on May 12, 2016. For your reference, these analyses have been assigned our service request number P1602483.

All analyses were performed according to our laboratory’s NELAP and DoD-ELAP-approved quality assurance program. The test results meet requirements of the current NELAP and DoD-ELAP standards, where applicable, and except as noted in the laboratory case narrative provided. For a specific list of NELAP and DoD-ELAP-accredited analytes, refer to the certifications section at www.alsglobal.com. Results are intended to be considered in their entirety and apply only to the samples analyzed and reported herein.

If you have any questions, please call me at (805) 526-7161.

Respectfully submitted,

ALS | Environmental

Kelly Horiuchi Laboratory Director

RIGHT SOLUTIONS | RIGHT PARTNER

1 of 156 2655 Park Center Dr., Suite A Simi Valley, CA 93065 T: +1 805 526 7161 F: +1 805 526 7270 www.alsglobal.com

Client: Oneida Total Integrated Enterprises (OTIE) Service Request No: P1602483 Project: Pemaco - Plant Vapor Monitoring ______

CASE NARRATIVE

The samples were received intact under chain of custody on May 12, 2016 and were stored in accordance with the analytical method requirements. Please refer to the sample acceptance check form for additional information. The results reported herein are applicable only to the condition of the samples at the time of sample receipt.

Volatile Organic Compound Analysis

The samples were analyzed for volatile organic compounds in accordance with EPA Method TO- 15 from the Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air, Second Edition (EPA/625/R-96/010b), January, 1999. This procedure is described in laboratory SOP VOA-TO15. The analytical system was comprised of a gas chromatograph / mass spectrometer (GC/MS) interfaced to a whole-air preconcentrator. This method is included on the laboratory’s NELAP and DoD-ELAP scope of accreditation, however it is not part of the AIHA-LAP accreditation. Any analytes flagged with an X are not included on the NELAP or DoD- ELAP accreditation.

The containers were cleaned, prior to sampling, down to the method reporting limit (MRL) reported for this project. Please note, projects which require reporting below the MRL could have results between the MRL and method detection limit (MDL) that are biased high. ______

The results of analyses are given in the attached laboratory report. All results are intended to be considered in their entirety, and ALS Environmental (ALS) is not responsible for utilization of less than the complete report.

Use of ALS Environmental (ALS)’s Name. Client shall not use ALS’s name or trademark in any marketing or reporting materials, press releases or in any other manner (“Materials”) whatsoever and shall not attribute to ALS any test result, tolerance or specification derived from ALS’s data (“Attribution”) without ALS’s prior written consent, which may be withheld by ALS for any reason in its sole discretion. To request ALS’s consent, Client shall provide copies of the proposed Materials or Attribution and describe in writing Client’s proposed use of such Materials or Attribution. If ALS has not provided written approval of the Materials or Attribution within ten (10) days of receipt from Client, Client’s request to use ALS’s name or trademark in any Materials or Attribution shall be deemed denied. ALS may, in its discretion, reasonably charge Client for its time in reviewing Materials or Attribution requests. Client acknowledges and agrees that the unauthorized use of ALS’s name or trademark may cause ALS to incur irreparable harm for which the recovery of money damages will be inadequate. Accordingly, Client acknowledges and agrees that a violation shall justify preliminary injunctive relief. For questions contact the laboratory.

RIGHT SOLUTIONS | RIGHT PARTNER

2 of 156 2655 Park Center Dr., Suite A Simi Valley, CA 93065 T: +1 805 526 7161 F: +1 805 526 7270 www.alsglobal.com

ALS Environmental – Simi Valley

CERTIFICATIONS, ACCREDITATIONS, AND REGISTRATIONS

Agency Web Site Number

AIHA http://www.aihaaccreditedlabs.org 101661

Arizona DHS http://www.azdhs.gov/lab/license/env.htm AZ0694

DoD ELAP http://www.pjlabs.com/search-accredited-labs L15-398 Florida DOH http://www.doh.state.fl.us/lab/EnvLabCert/WaterCert.htm E871020 (NELAP) http://www.maine.gov/dhhs/mecdc/environmental-health/water/dwp- Maine DHHS 2014025 services/labcert/labcert.htm Minnesota DOH http://www.health.state.mn.us/accreditation 977273 (NELAP) New Jersey DEP http://www.nj.gov/dep/oqa/ CA009 (NELAP) New York DOH http://www.wadsworth.org/labcert/elap/elap.html 11221 (NELAP) Oregon PHD http://public.health.oregon.gov/LaboratoryServices/EnvironmentalLaborat 4068-003 (NELAP) oryAccreditation/Pages/index.aspx 68-03307 Pennsylvania DEP http://www.depweb.state.pa.us/labs (Registration) Texas CEQ T104704413- http://www.tceq.texas.gov/field/qa/env_lab_accreditation.html (NELAP) 15-6 Utah DOH CA01627201 http://www.health.utah.gov/lab/labimp/certification/index.html (NELAP) 5-5 Washington DOE http://www.ecy.wa.gov/programs/eap/labs/lab-accreditation.html C946 Analyses were performed according to our laboratory’s NELAP and DoD-ELAP approved quality assurance program. A complete listing of specific NELAP and DoD-ELAP certified analytes can be found in the certifications section at www.alsglobal.com, or at the accreditation body’s website.

Each of the certifications listed above have an explicit Scope of Accreditation that applies to specific matrices/methods/analytes; therefore, please contact the laboratory for information corresponding to a particular certification.

RIGHT SOLUTIONS | RIGHT PARTNER

3 of 156 ALS ENVIRONMENTAL

DETAIL SUMMARY REPORT Client: Oneida Total Integrated Enterprises (OTIE) Service Request: P1602483 Project ID: Pemaco - Plant Vapor Monitoring

Date Received: 5/12/2016 Time Received: 12:40

Date Time Container Pi1 Pf1

Client Sample ID Lab Code Matrix Collected Collected ID (psig) (psig) TO-15 VOC - Cans SP-106-20160512 P1602483-001 Air 5/12/2016 09:00 1BV06394 -0.18 5.16 X SP-104-20160512 P1602483-002 Air 5/12/2016 09:45 1BV06389 -0.09 5.18 X

4 of 156 P1602483_Detail Summary_1605261501_RB.xls - DETAIL SUMMARY ,:::::.: ,.;::::::::;:., TYPE RECORD RECORD Titne: ::::::::., Tlmo: T.ma: 2014166 1BV06394 18V06389 AINcR ..... ·.·.· 5/12/2016 5/12/2016 I,(,, I CON!' Bottle BotUe ...... · P,0.NO.: ;;~::;.:::::::;:!::;:;;;;;:i;.:;- ·~101aoat ·~101aoat •:•: CUSTODY CUSTODY S/" b oaic: 0 Dale: OF CODE oolloctad DD LOG wai, T DAlE: CHAIN ANALYSIS ¢5 COEL Somplo DD '1 /Z.. tlL3aiftt SP-108. /1<,, to b ... REQUESTED :s-( lri 6P·10a r Monitorina from ,a f po,t Vapor 'S"m ""'"Pie ..#7 i:,,- l•g Plant • lvl th• (SIGH6.TIJRE) . CONTACT: Osborn& A t-w.n,lrnn chon!jOd ) PRO£CT SN~Pt.ER(S): " X X "S" :& e .. > 0 0 Pemaco Orval A~Bn x1·t. which {Signsh,re) (Si9ow.t"e} '/ . 1 1 COll'J. l'tO.vr b)': :,i,y; T..:302, DAYS X '"'' air air , MAlRI 10 Re~ttd ·= ..--- T-3011<> { (iJ 11111£ 9:00 from 9:45 !J..~D 50AYS ooG"orne,,..,..tie.oom ooG"orne,,..,..tie.oom $.4,Mf>l.fNO cl>Mged DATE E-f,'\6.11. D 05/12/16 05112/16 se1, .. b v f D 93001 Street - ~nd Nani~ CA mg/m3 ro../ 072HR Jl11 Ollt OTIE Main )1 .. Point and • ii APPLY) E. 52li-7220 A, I SP-106 SP-104 806.fi85.2111 F1e1d '4'.Y A 48HR ~mmge • Ventura T-301. i.J 317 ppmv F".oJ(: (8!>5) . \lapor V8por n D 'j Su;lo cos1e carbon both FAX: !. I Ve:tS&I J in Orlvt, ;a~et" 9306$ » GAC -30.09 ·30.11 r PO (AO.Om::titAL ' at at CA EDDs 024HR 52&-7161. : Conti!, tampli> .. tffll.KM'tt SAMPLE Environmental Environmental IUE {Si9nft.H'8) cy19~) cS19nahn) J Part< (80$) Vall•y. cue the started started report - Dy: ,:,,,: by: Vapor REOUIRE/r'EHTS 805.585.4313 INSTRUCTIONS ALS TEL: io1;5 Simi SP-106,20160512 108 SP·104-20100S12 1st from ' ; , ... VNN"oROin.u SP- SP-104 Please , LA80RA,._., ADORES$; TEL: D SPECW.. 0SAME0AY ~PECb\L Rell~\.ished ,,.J ,ntrni i~i R111!i"lqu18l\ed RellnQuiahe

5 of 156 ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Note: This form is used for all samples received by ALS. The use of this form for custody seals is strictly meant to indicate presence/absence and not as an indication of compliance or nonconformity. Thermal preservation and pH will only be evaluated either at the request of the client and/or as required by the method/SOP. Yes No N/A 1 Were sample containers properly marked with client sample ID?    2 Did sample containers arrive in good condition?    3 Were chain-of-custody papers used and filled out?    4 Did sample container labels and/or tags agree with custody papers?    5 Was sample volume received adequate for analysis?    6 Are samples within specified holding times?    7 Was proper temperature (thermal preservation) of cooler at receipt adhered to?   

8 Were custody seals on outside of cooler/Box/Container?    Location of seal(s)? Sealing Lid?    Were signature and date included?    Were seals intact?    9 Do containers have appropriate preservation, according to method/SOP or Client specified information?    Is there a client indication that the submitted samples are pH preserved?    Were VOA vials checked for presence/absence of air bubbles?    Does the client/method/SOP require that the analyst check the sample pH and if necessary alter it?    10 Tubes: Are the tubes capped and intact?    11 Badges: Are the badges properly capped and intact?    Are dual bed badges separated and individually capped and intact?   

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

6 of 156 P1602483-001.01__.xls - Page 1 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

7 of 156 P1602483-001.01__.xls - Page 2 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

8 of 156 P1602483-001.01__.xls - Page 3 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

9 of 156 P1602483-001.01__.xls - Page 4 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

10 of 156 P1602483-001.01__.xls - Page 5 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4) 11 of 156 P1602483-001.01__.xls - Page 6 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

12 of 156 P1602483-001.01__.xls - Page 7 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

13 of 156 P1602483-001.01__.xls - Page 8 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

14 of 156 P1602483-001.01__.xls - Page 9 of 10 6/1/16 8:55 AM ALS Environmental Sample Acceptance Check Form Client: Work order: P1602483-001.01 Project: Sample(s) received on: Date opened: by:

Lab Sample ID Container Required Received Adjusted VOA Headspace Receipt / Preservation Description pH * pH pH (Presence/Absence) Comments

Explain any discrepancies: (include lab sample ID numbers):

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

15 of 156 P1602483-001.01__.xls - Page 10 of 10 6/1/16 8:55 AM ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-106-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-001

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: Container ID: 1BV06394

Initial Pressure (psig): -0.18 Final Pressure (psig): 5.16

Canister Dilution Factor: 1.37

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 115-07-1 Propene 0.74 1.7 0.48 0.43 1.0 0.28 J 75-71-8 Dichlorodifluoromethane (CFC 12) ND 1.7 0.58 ND 0.35 0.12 74-87-3 Chloromethane ND 1.7 0.51 ND 0.83 0.25 1,2-Dichloro-1,1,2,2- 76-14-2 ND 1.7 0.65 ND 0.25 tetrafluoroethane (CFC 114) 0.093 75-01-4 Vinyl Chloride ND 1.7 0.58 ND 0.67 0.23 106-99-0 1,3-Butadiene ND 1.7 0.75 ND 0.77 0.34 74-83-9 Bromomethane ND 1.7 0.65 ND 0.44 0.17 75-00-3 Chloroethane ND 1.7 0.58 ND 0.65 0.22 64-17-5 280 17 2.7 150 9.1 1.5 75-05-8 Acetonitrile ND 1.7 0.62 ND 1.0 0.37 107-02-8 Acrolein ND 6.9 0.58 ND 3.0 0.25 67-64-1 Acetone 8.3 17 2.6 3.5 7.2 1.1 J 75-69-4 Trichlorofluoromethane ND 1.7 0.58 ND 0.30 0.10 67-63-0 2-Propanol (Isopropyl Alcohol) 1.7 17 1.4 0.69 7.0 0.59 J 107-13-1 Acrylonitrile ND 1.7 0.58 ND 0.79 0.27 75-35-4 1,1-Dichloroethene ND 1.7 0.58 ND 0.43 0.15 75-09-2 Methylene Chloride 0.74 1.7 0.58 0.21 0.49 0.17 J 107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 1.7 0.55 ND 0.55 0.18 76-13-1 Trichlorotrifluoroethane ND 1.7 0.58 ND 0.22 0.076 75-15-0 Carbon Disulfide ND 17 0.51 ND 5.5 0.17 156-60-5 trans-1,2-Dichloroethene ND 1.7 0.65 ND 0.43 0.16 75-34-3 1,1-Dichloroethane ND 1.7 0.55 ND 0.42 0.14 1634-04-4 Methyl tert-Butyl Ether ND 1.7 0.58 ND 0.48 0.16 108-05-4 Vinyl Acetate ND 17 2.2 ND 4.9 0.63 78-93-3 2-Butanone (MEK) 2.1 17 0.72 0.73 5.8 0.24 J

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method. J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.

16 of 156 P1602483_TO15_1605261228_SC.xls - Sample TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 2 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-106-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-001

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: Container ID: 1BV06394

Initial Pressure (psig): -0.18 Final Pressure (psig): 5.16

Canister Dilution Factor: 1.37

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 156-59-2 cis-1,2-Dichloroethene ND 1.7 0.55 ND 0.43 0.14 141-78-6 Ethyl Acetate ND 3.4 1.2 ND 0.95 0.33 110-54-3 n-Hexane 1.3 1.7 0.51 0.37 0.49 0.15 J 67-66-3 Chloroform ND 1.7 0.58 ND 0.35 0.12 109-99-9 Tetrahydrofuran (THF) ND 1.7 0.69 ND 0.58 0.23 107-06-2 1,2-Dichloroethane ND 1.7 0.55 ND 0.42 0.14 71-55-6 1,1,1-Trichloroethane ND 1.7 0.58 ND 0.31 0.11 71-43-2 Benzene 1.0 1.7 0.55 0.32 0.54 0.17 J 56-23-5 Carbon Tetrachloride ND 1.7 0.51 ND 0.27 0.082 110-82-7 Cyclohexane ND 3.4 0.99 ND 1.0 0.29 78-87-5 1,2-Dichloropropane ND 1.7 0.55 ND 0.37 0.12 75-27-4 Bromodichloromethane ND 1.7 0.51 ND 0.26 0.077 79-01-6 Trichloroethene 3.0 1.7 0.48 0.57 0.32 0.089 123-91-1 1,4-Dioxane ND 1.7 0.55 ND 0.48 0.15 80-62-6 Methyl Methacrylate ND 3.4 1.1 ND 0.84 0.26 142-82-5 n-Heptane ND 1.7 0.58 ND 0.42 0.14 10061-01-5 cis-1,3-Dichloropropene ND 1.7 0.48 ND 0.38 0.11 108-10-1 4-Methyl-2-pentanone ND 1.7 0.55 ND 0.42 0.13 10061-02-6 trans-1,3-Dichloropropene ND 1.7 0.55 ND 0.38 0.12 79-00-5 1,1,2-Trichloroethane ND 1.7 0.55 ND 0.31 0.10 108-88-3 Toluene 2.6 1.7 0.58 0.68 0.45 0.15 591-78-6 2-Hexanone ND 1.7 0.55 ND 0.42 0.13 124-48-1 Dibromochloromethane ND 1.7 0.55 ND 0.20 0.064 106-93-4 1,2-Dibromoethane ND 1.7 0.55 ND 0.22 0.071 123-86-4 n-Butyl Acetate ND 1.7 0.55 ND 0.36 0.12

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method. J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.

17 of 156 P1602483_TO15_1605261228_SC.xls - Sample TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 3 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-106-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-001

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: Container ID: 1BV06394

Initial Pressure (psig): -0.18 Final Pressure (psig): 5.16

Canister Dilution Factor: 1.37

Result MRL MDL Result MRL MDL Data CAS # Compound µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 111-65-9 n-Octane ND 1.7 0.62 ND 0.37 0.13 127-18-4 Tetrachloroethene ND 1.7 0.48 ND 0.25 0.071 108-90-7 Chlorobenzene ND 1.7 0.55 ND 0.37 0.12 100-41-4 Ethylbenzene ND 1.7 0.55 ND 0.39 0.13 179601-23-1 m,p-Xylenes ND 3.4 1.0 ND 0.79 0.24 75-25-2 Bromoform ND 1.7 0.51 ND 0.17 0.050 100-42-5 Styrene ND 1.7 0.51 ND 0.40 0.12 95-47-6 o-Xylene ND 1.7 0.51 ND 0.39 0.12 111-84-2 n-Nonane ND 1.7 0.51 ND 0.33 0.098 79-34-5 1,1,2,2-Tetrachloroethane ND 1.7 0.51 ND 0.25 0.075 98-82-8 Cumene ND 1.7 0.51 ND 0.35 0.10 80-56-8 alpha-Pinene ND 1.7 0.48 ND 0.31 0.086 103-65-1 n-Propylbenzene ND 1.7 0.55 ND 0.35 0.11 622-96-8 4-Ethyltoluene ND 1.7 0.55 ND 0.35 0.11 108-67-8 1,3,5-Trimethylbenzene ND 1.7 0.55 ND 0.35 0.11 95-63-6 1,2,4-Trimethylbenzene ND 1.7 0.51 ND 0.35 0.10 100-44-7 Benzyl Chloride ND 1.7 0.38 ND 0.33 0.073 541-73-1 1,3-Dichlorobenzene ND 1.7 0.51 ND 0.28 0.085 106-46-7 1,4-Dichlorobenzene ND 1.7 0.48 ND 0.28 0.080 95-50-1 1,2-Dichlorobenzene ND 1.7 0.51 ND 0.28 0.085 5989-27-5 d-Limonene ND 1.7 0.48 ND 0.31 0.086 96-12-8 1,2-Dibromo-3-chloropropane ND 1.7 0.34 ND 0.18 0.035 120-82-1 1,2,4-Trichlorobenzene ND 1.7 0.55 ND 0.23 0.074 91-20-3 Naphthalene ND 1.7 0.62 ND 0.33 0.12 87-68-3 Hexachlorobutadiene ND 1.7 0.48 ND 0.16 0.045

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

18 of 156 P1602483_TO15_1605261228_SC.xls - Sample TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-104-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-002

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: 0.040 Liter(s) Container ID: 1BV06389

Initial Pressure (psig): -0.09 Final Pressure (psig): 5.18

Canister Dilution Factor: 1.36

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 115-07-1 Propene ND 1.7 0.48 ND 0.99 0.28 75-71-8 Dichlorodifluoromethane (CFC 12) ND 1.7 0.58 ND 0.34 0.12 74-87-3 Chloromethane ND 1.7 0.51 ND 0.82 0.25 1,2-Dichloro-1,1,2,2- 76-14-2 ND 1.7 0.65 ND 0.24 tetrafluoroethane (CFC 114) 0.092 75-01-4 Vinyl Chloride 1.7 1.7 0.58 0.67 0.67 0.23 106-99-0 1,3-Butadiene ND 1.7 0.75 ND 0.77 0.34 74-83-9 Bromomethane ND 1.7 0.65 ND 0.44 0.17 75-00-3 Chloroethane ND 1.7 0.58 ND 0.64 0.22 64-17-5 Ethanol 36 17 2.7 19 9.0 1.4 75-05-8 Acetonitrile ND 1.7 0.61 ND 1.0 0.36 107-02-8 Acrolein ND 6.8 0.58 ND 3.0 0.25 67-64-1 Acetone 46 17 2.6 19 7.2 1.1 75-69-4 Trichlorofluoromethane 1.5 1.7 0.58 0.28 0.30 0.10 J 67-63-0 2-Propanol (Isopropyl Alcohol) 1.5 17 1.4 0.63 6.9 0.58 J 107-13-1 Acrylonitrile ND 1.7 0.58 ND 0.78 0.27 75-35-4 1,1-Dichloroethene 25 1.7 0.58 6.3 0.43 0.15 75-09-2 Methylene Chloride 0.92 1.7 0.58 0.26 0.49 0.17 J 107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 1.7 0.54 ND 0.54 0.17 76-13-1 Trichlorotrifluoroethane ND 1.7 0.58 ND 0.22 0.075 75-15-0 Carbon Disulfide ND 17 0.51 ND 5.5 0.16 156-60-5 trans-1,2-Dichloroethene 2.1 1.7 0.65 0.53 0.43 0.16 75-34-3 1,1-Dichloroethane 5.5 1.7 0.54 1.4 0.42 0.13 1634-04-4 Methyl tert-Butyl Ether ND 1.7 0.58 ND 0.47 0.16 108-05-4 Vinyl Acetate ND 17 2.2 ND 4.8 0.63 78-93-3 2-Butanone (MEK) 3.5 17 0.71 1.2 5.8 0.24 J

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method. J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.

19 of 156 P1602483_TO15_1605261228_SC.xls - Sample (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 2 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-104-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-002

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: 0.040 Liter(s) Container ID: 1BV06389

Initial Pressure (psig): -0.09 Final Pressure (psig): 5.18

Canister Dilution Factor: 1.36

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 156-59-2 cis-1,2-Dichloroethene 38 1.7 0.54 9.6 0.43 0.14 141-78-6 Ethyl Acetate ND 3.4 1.2 ND 0.94 0.33 110-54-3 n-Hexane 190 1.7 0.51 54 0.48 0.14 67-66-3 Chloroform 13 1.7 0.58 2.7 0.35 0.12 109-99-9 Tetrahydrofuran (THF) 3.2 1.7 0.68 1.1 0.58 0.23 107-06-2 1,2-Dichloroethane ND 1.7 0.54 ND 0.42 0.13 71-55-6 1,1,1-Trichloroethane 2.2 1.7 0.58 0.40 0.31 0.11 71-43-2 Benzene 13 1.7 0.54 4.0 0.53 0.17 56-23-5 Carbon Tetrachloride ND 1.7 0.51 ND 0.27 0.081 110-82-7 Cyclohexane 120 3.4 0.99 36 0.99 0.29 78-87-5 1,2-Dichloropropane ND 1.7 0.54 ND 0.37 0.12 75-27-4 Bromodichloromethane ND 1.7 0.51 ND 0.25 0.076 79-01-6 Trichloroethene 530 17 4.8 98 3.2 0.89 D 123-91-1 1,4-Dioxane ND 1.7 0.54 ND 0.47 0.15 80-62-6 Methyl Methacrylate ND 3.4 1.1 ND 0.83 0.26 142-82-5 n-Heptane 48 1.7 0.58 12 0.41 0.14 10061-01-5 cis-1,3-Dichloropropene ND 1.7 0.48 ND 0.37 0.10 108-10-1 4-Methyl-2-pentanone ND 1.7 0.54 ND 0.41 0.13 10061-02-6 trans-1,3-Dichloropropene ND 1.7 0.54 ND 0.37 0.12 79-00-5 1,1,2-Trichloroethane ND 1.7 0.54 ND 0.31 0.10 108-88-3 Toluene 1.6 1.7 0.58 0.43 0.45 0.15 J 591-78-6 2-Hexanone ND 1.7 0.54 ND 0.42 0.13 124-48-1 Dibromochloromethane ND 1.7 0.54 ND 0.20 0.064 106-93-4 1,2-Dibromoethane ND 1.7 0.54 ND 0.22 0.071 123-86-4 n-Butyl Acetate ND 1.7 0.54 ND 0.36 0.11

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method. J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL. D = The reported result is from a dilution.

20 of 156 P1602483_TO15_1605261228_SC.xls - Sample (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 3 of 3 Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: SP-104-20160512 ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P1602483-002

Test Code: EPA TO-15 Modified Date Collected: 5/12/16 Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 5/12/16 Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.40 Liter(s) Test Notes: 0.040 Liter(s) Container ID: 1BV06389

Initial Pressure (psig): -0.09 Final Pressure (psig): 5.18

Canister Dilution Factor: 1.36

Result MRL MDL Result MRL MDL Data CAS # Compound µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 111-65-9 n-Octane 8.9 1.7 0.61 1.9 0.36 0.13 127-18-4 Tetrachloroethene 160 1.7 0.48 24 0.25 0.070 108-90-7 Chlorobenzene ND 1.7 0.54 ND 0.37 0.12 100-41-4 Ethylbenzene 1.1 1.7 0.54 0.25 0.39 0.13 J 179601-23-1 m,p-Xylenes 1.3 3.4 1.0 0.30 0.78 0.23 J 75-25-2 Bromoform ND 1.7 0.51 ND 0.16 0.049 100-42-5 Styrene ND 1.7 0.51 ND 0.40 0.12 95-47-6 o-Xylene ND 1.7 0.51 ND 0.39 0.12 111-84-2 n-Nonane 0.68 1.7 0.51 0.13 0.32 0.097 J 79-34-5 1,1,2,2-Tetrachloroethane ND 1.7 0.51 ND 0.25 0.074 98-82-8 Cumene 0.61 1.7 0.51 0.12 0.35 0.10 J 80-56-8 alpha-Pinene ND 1.7 0.48 ND 0.31 0.085 103-65-1 n-Propylbenzene ND 1.7 0.54 ND 0.35 0.11 622-96-8 4-Ethyltoluene ND 1.7 0.54 ND 0.35 0.11 108-67-8 1,3,5-Trimethylbenzene ND 1.7 0.54 ND 0.35 0.11 95-63-6 1,2,4-Trimethylbenzene 0.80 1.7 0.51 0.16 0.35 0.10 J 100-44-7 Benzyl Chloride ND 1.7 0.37 ND 0.33 0.072 541-73-1 1,3-Dichlorobenzene ND 1.7 0.51 ND 0.28 0.085 106-46-7 1,4-Dichlorobenzene ND 1.7 0.48 ND 0.28 0.079 95-50-1 1,2-Dichlorobenzene ND 1.7 0.51 ND 0.28 0.085 5989-27-5 d-Limonene ND 1.7 0.48 ND 0.31 0.085 96-12-8 1,2-Dibromo-3-chloropropane ND 1.7 0.34 ND 0.18 0.035 120-82-1 1,2,4-Trichlorobenzene ND 1.7 0.54 ND 0.23 0.073 91-20-3 Naphthalene ND 1.7 0.61 ND 0.32 0.12 87-68-3 Hexachlorobutadiene ND 1.7 0.48 ND 0.16 0.045

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method. J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.

21 of 156 P1602483_TO15_1605261228_SC.xls - Sample (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 115-07-1 Propene ND 0.50 0.14 ND 0.29 0.081 75-71-8 Dichlorodifluoromethane (CFC 12) ND 0.50 0.17 ND 0.10 0.034 74-87-3 Chloromethane ND 0.50 0.15 ND 0.24 0.073 1,2-Dichloro-1,1,2,2- 76-14-2 ND 0.50 0.19 ND 0.072 tetrafluoroethane (CFC 114) 0.027 75-01-4 Vinyl Chloride ND 0.50 0.17 ND 0.20 0.067 106-99-0 1,3-Butadiene ND 0.50 0.22 ND 0.23 0.099 74-83-9 Bromomethane ND 0.50 0.19 ND 0.13 0.049 75-00-3 Chloroethane ND 0.50 0.17 ND 0.19 0.064 64-17-5 Ethanol ND 5.0 0.80 ND 2.7 0.42 75-05-8 Acetonitrile ND 0.50 0.18 ND 0.30 0.11 107-02-8 Acrolein ND 2.0 0.17 ND 0.87 0.074 67-64-1 Acetone ND 5.0 0.77 ND 2.1 0.32 75-69-4 Trichlorofluoromethane ND 0.50 0.17 ND 0.089 0.030 67-63-0 2-Propanol (Isopropyl Alcohol) ND 5.0 0.42 ND 2.0 0.17 107-13-1 Acrylonitrile ND 0.50 0.17 ND 0.23 0.078 75-35-4 1,1-Dichloroethene ND 0.50 0.17 ND 0.13 0.043 75-09-2 Methylene Chloride ND 0.50 0.17 ND 0.14 0.049 107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 0.50 0.16 ND 0.16 0.051 76-13-1 Trichlorotrifluoroethane ND 0.50 0.17 ND 0.065 0.022 75-15-0 Carbon Disulfide ND 5.0 0.15 ND 1.6 0.048 156-60-5 trans-1,2-Dichloroethene ND 0.50 0.19 ND 0.13 0.048 75-34-3 1,1-Dichloroethane ND 0.50 0.16 ND 0.12 0.040 1634-04-4 Methyl tert-Butyl Ether ND 0.50 0.17 ND 0.14 0.047 108-05-4 Vinyl Acetate ND 5.0 0.65 ND 1.4 0.18 78-93-3 2-Butanone (MEK) ND 5.0 0.21 ND 1.7 0.071

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

22 of 156 P1602483_TO15_1605261228_SC.xls - MBlank TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 2 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 156-59-2 cis-1,2-Dichloroethene ND 0.50 0.16 ND 0.13 0.040 141-78-6 Ethyl Acetate ND 1.0 0.35 ND 0.28 0.097 110-54-3 n-Hexane ND 0.50 0.15 ND 0.14 0.043 67-66-3 Chloroform ND 0.50 0.17 ND 0.10 0.035 109-99-9 Tetrahydrofuran (THF) ND 0.50 0.20 ND 0.17 0.068 107-06-2 1,2-Dichloroethane ND 0.50 0.16 ND 0.12 0.040 71-55-6 1,1,1-Trichloroethane ND 0.50 0.17 ND 0.092 0.031 71-43-2 Benzene ND 0.50 0.16 ND 0.16 0.050 56-23-5 Carbon Tetrachloride ND 0.50 0.15 ND 0.080 0.024 110-82-7 Cyclohexane ND 1.0 0.29 ND 0.29 0.084 78-87-5 1,2-Dichloropropane ND 0.50 0.16 ND 0.11 0.035 75-27-4 Bromodichloromethane ND 0.50 0.15 ND 0.075 0.022 79-01-6 Trichloroethene ND 0.50 0.14 ND 0.093 0.026 123-91-1 1,4-Dioxane ND 0.50 0.16 ND 0.14 0.044 80-62-6 Methyl Methacrylate ND 1.0 0.31 ND 0.24 0.076 142-82-5 n-Heptane ND 0.50 0.17 ND 0.12 0.041 10061-01-5 cis-1,3-Dichloropropene ND 0.50 0.14 ND 0.11 0.031 108-10-1 4-Methyl-2-pentanone ND 0.50 0.16 ND 0.12 0.039 10061-02-6 trans-1,3-Dichloropropene ND 0.50 0.16 ND 0.11 0.035 79-00-5 1,1,2-Trichloroethane ND 0.50 0.16 ND 0.092 0.029 108-88-3 Toluene ND 0.50 0.17 ND 0.13 0.045 591-78-6 2-Hexanone ND 0.50 0.16 ND 0.12 0.039 124-48-1 Dibromochloromethane ND 0.50 0.16 ND 0.059 0.019 106-93-4 1,2-Dibromoethane ND 0.50 0.16 ND 0.065 0.021 123-86-4 n-Butyl Acetate ND 0.50 0.16 ND 0.11 0.034

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

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RESULTS OF ANALYSIS Page 3 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

Result MRL MDL Result MRL MDL Data CAS # Compound µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 111-65-9 n-Octane ND 0.50 0.18 ND 0.11 0.039 127-18-4 Tetrachloroethene ND 0.50 0.14 ND 0.074 0.021 108-90-7 Chlorobenzene ND 0.50 0.16 ND 0.11 0.035 100-41-4 Ethylbenzene ND 0.50 0.16 ND 0.12 0.037 179601-23-1 m,p-Xylenes ND 1.0 0.30 ND 0.23 0.069 75-25-2 Bromoform ND 0.50 0.15 ND 0.048 0.015 100-42-5 Styrene ND 0.50 0.15 ND 0.12 0.035 95-47-6 o-Xylene ND 0.50 0.15 ND 0.12 0.035 111-84-2 n-Nonane ND 0.50 0.15 ND 0.095 0.029 79-34-5 1,1,2,2-Tetrachloroethane ND 0.50 0.15 ND 0.073 0.022 98-82-8 Cumene ND 0.50 0.15 ND 0.10 0.031 80-56-8 alpha-Pinene ND 0.50 0.14 ND 0.090 0.025 103-65-1 n-Propylbenzene ND 0.50 0.16 ND 0.10 0.033 622-96-8 4-Ethyltoluene ND 0.50 0.16 ND 0.10 0.033 108-67-8 1,3,5-Trimethylbenzene ND 0.50 0.16 ND 0.10 0.033 95-63-6 1,2,4-Trimethylbenzene ND 0.50 0.15 ND 0.10 0.031 100-44-7 Benzyl Chloride ND 0.50 0.11 ND 0.097 0.021 541-73-1 1,3-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025 106-46-7 1,4-Dichlorobenzene ND 0.50 0.14 ND 0.083 0.023 95-50-1 1,2-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025 5989-27-5 d-Limonene ND 0.50 0.14 ND 0.090 0.025 96-12-8 1,2-Dibromo-3-chloropropane ND 0.50 0.099 ND 0.052 0.010 120-82-1 1,2,4-Trichlorobenzene ND 0.50 0.16 ND 0.067 0.022 91-20-3 Naphthalene ND 0.50 0.18 ND 0.095 0.034 87-68-3 Hexachlorobutadiene ND 0.50 0.14 ND 0.047 0.013

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

24 of 156 P1602483_TO15_1605261228_SC.xls - MBlank TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 115-07-1 Propene ND 0.50 0.14 ND 0.29 0.081 75-71-8 Dichlorodifluoromethane (CFC 12) ND 0.50 0.17 ND 0.10 0.034 74-87-3 Chloromethane ND 0.50 0.15 ND 0.24 0.073 1,2-Dichloro-1,1,2,2- 76-14-2 ND 0.50 0.19 ND 0.072 tetrafluoroethane (CFC 114) 0.027 75-01-4 Vinyl Chloride ND 0.50 0.17 ND 0.20 0.067 106-99-0 1,3-Butadiene ND 0.50 0.22 ND 0.23 0.099 74-83-9 Bromomethane ND 0.50 0.19 ND 0.13 0.049 75-00-3 Chloroethane ND 0.50 0.17 ND 0.19 0.064 64-17-5 Ethanol ND 5.0 0.80 ND 2.7 0.42 75-05-8 Acetonitrile ND 0.50 0.18 ND 0.30 0.11 107-02-8 Acrolein ND 2.0 0.17 ND 0.87 0.074 67-64-1 Acetone ND 5.0 0.77 ND 2.1 0.32 75-69-4 Trichlorofluoromethane ND 0.50 0.17 ND 0.089 0.030 67-63-0 2-Propanol (Isopropyl Alcohol) ND 5.0 0.42 ND 2.0 0.17 107-13-1 Acrylonitrile ND 0.50 0.17 ND 0.23 0.078 75-35-4 1,1-Dichloroethene ND 0.50 0.17 ND 0.13 0.043 75-09-2 Methylene Chloride ND 0.50 0.17 ND 0.14 0.049 107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 0.50 0.16 ND 0.16 0.051 76-13-1 Trichlorotrifluoroethane ND 0.50 0.17 ND 0.065 0.022 75-15-0 Carbon Disulfide ND 5.0 0.15 ND 1.6 0.048 156-60-5 trans-1,2-Dichloroethene ND 0.50 0.19 ND 0.13 0.048 75-34-3 1,1-Dichloroethane ND 0.50 0.16 ND 0.12 0.040 1634-04-4 Methyl tert-Butyl Ether ND 0.50 0.17 ND 0.14 0.047 108-05-4 Vinyl Acetate ND 5.0 0.65 ND 1.4 0.18 78-93-3 2-Butanone (MEK) ND 5.0 0.21 ND 1.7 0.071

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

25 of 156 P1602483_TO15_1605261228_SC.xls - MBlank (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 2 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

CAS # Compound Result MRL MDL Result MRL MDL Data µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 156-59-2 cis-1,2-Dichloroethene ND 0.50 0.16 ND 0.13 0.040 141-78-6 Ethyl Acetate ND 1.0 0.35 ND 0.28 0.097 110-54-3 n-Hexane ND 0.50 0.15 ND 0.14 0.043 67-66-3 Chloroform ND 0.50 0.17 ND 0.10 0.035 109-99-9 Tetrahydrofuran (THF) ND 0.50 0.20 ND 0.17 0.068 107-06-2 1,2-Dichloroethane ND 0.50 0.16 ND 0.12 0.040 71-55-6 1,1,1-Trichloroethane ND 0.50 0.17 ND 0.092 0.031 71-43-2 Benzene ND 0.50 0.16 ND 0.16 0.050 56-23-5 Carbon Tetrachloride ND 0.50 0.15 ND 0.080 0.024 110-82-7 Cyclohexane ND 1.0 0.29 ND 0.29 0.084 78-87-5 1,2-Dichloropropane ND 0.50 0.16 ND 0.11 0.035 75-27-4 Bromodichloromethane ND 0.50 0.15 ND 0.075 0.022 79-01-6 Trichloroethene ND 0.50 0.14 ND 0.093 0.026 123-91-1 1,4-Dioxane ND 0.50 0.16 ND 0.14 0.044 80-62-6 Methyl Methacrylate ND 1.0 0.31 ND 0.24 0.076 142-82-5 n-Heptane ND 0.50 0.17 ND 0.12 0.041 10061-01-5 cis-1,3-Dichloropropene ND 0.50 0.14 ND 0.11 0.031 108-10-1 4-Methyl-2-pentanone ND 0.50 0.16 ND 0.12 0.039 10061-02-6 trans-1,3-Dichloropropene ND 0.50 0.16 ND 0.11 0.035 79-00-5 1,1,2-Trichloroethane ND 0.50 0.16 ND 0.092 0.029 108-88-3 Toluene ND 0.50 0.17 ND 0.13 0.045 591-78-6 2-Hexanone ND 0.50 0.16 ND 0.12 0.039 124-48-1 Dibromochloromethane ND 0.50 0.16 ND 0.059 0.019 106-93-4 1,2-Dibromoethane ND 0.50 0.16 ND 0.065 0.021 123-86-4 n-Butyl Acetate ND 0.50 0.16 ND 0.11 0.034

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

26 of 156 P1602483_TO15_1605261228_SC.xls - MBlank (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 3 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Method Blank ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-MB

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s) Test Notes:

Canister Dilution Factor: 1.00

Result MRL MDL Result MRL MDL Data CAS # Compound µg/m³ µg/m³ µg/m³ ppbV ppbV ppbV Qualifier 111-65-9 n-Octane ND 0.50 0.18 ND 0.11 0.039 127-18-4 Tetrachloroethene ND 0.50 0.14 ND 0.074 0.021 108-90-7 Chlorobenzene ND 0.50 0.16 ND 0.11 0.035 100-41-4 Ethylbenzene ND 0.50 0.16 ND 0.12 0.037 179601-23-1 m,p-Xylenes ND 1.0 0.30 ND 0.23 0.069 75-25-2 Bromoform ND 0.50 0.15 ND 0.048 0.015 100-42-5 Styrene ND 0.50 0.15 ND 0.12 0.035 95-47-6 o-Xylene ND 0.50 0.15 ND 0.12 0.035 111-84-2 n-Nonane ND 0.50 0.15 ND 0.095 0.029 79-34-5 1,1,2,2-Tetrachloroethane ND 0.50 0.15 ND 0.073 0.022 98-82-8 Cumene ND 0.50 0.15 ND 0.10 0.031 80-56-8 alpha-Pinene ND 0.50 0.14 ND 0.090 0.025 103-65-1 n-Propylbenzene ND 0.50 0.16 ND 0.10 0.033 622-96-8 4-Ethyltoluene ND 0.50 0.16 ND 0.10 0.033 108-67-8 1,3,5-Trimethylbenzene ND 0.50 0.16 ND 0.10 0.033 95-63-6 1,2,4-Trimethylbenzene ND 0.50 0.15 ND 0.10 0.031 100-44-7 Benzyl Chloride ND 0.50 0.11 ND 0.097 0.021 541-73-1 1,3-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025 106-46-7 1,4-Dichlorobenzene ND 0.50 0.14 ND 0.083 0.023 95-50-1 1,2-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025 5989-27-5 d-Limonene ND 0.50 0.14 ND 0.090 0.025 96-12-8 1,2-Dibromo-3-chloropropane ND 0.50 0.099 ND 0.052 0.010 120-82-1 1,2,4-Trichlorobenzene ND 0.50 0.16 ND 0.067 0.022 91-20-3 Naphthalene ND 0.50 0.18 ND 0.095 0.034 87-68-3 Hexachlorobutadiene ND 0.50 0.14 ND 0.047 0.013

ND = Compound was analyzed for, but not detected above the laboratory detection limit. MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.

27 of 156 P1602483_TO15_1605261228_SC.xls - MBlank (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

SURROGATE SPIKE RECOVERY RESULTS Page 1 of 1

Client: Oneida Total Integrated Enterprises (OTIE) Client Project ID: Pemaco - Plant Vapor Monitoring ALS Project ID: P1602483

Test Code: EPA TO-15 Modified Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date(s) Collected: 5/12/16 Analyst: Wida Ang Date(s) Received: 5/12/16 Sample Type: 1.0 L Bottle-Vac™(s) Date(s) Analyzed: 5/25/16 Test Notes:

1,2-Dichloroethane-d4 Toluene-d8 Bromofluorobenzene Client Sample ID ALS Sample ID Percent Percent Percent Acceptance Data Recovered Recovered Recovered Limits Qualifier Method Blank P160525-MB 100 100 109 70-130 Method Blank P160525-MB 95 100 112 70-130 Lab Control Sample P160525-LCS 98 99 113 70-130 Lab Control Sample P160525-LCS 94 98 115 70-130 SP-106-20160512 P1602483-001 97 97 113 70-130 SP-104-20160512 P1602483-002 99 97 114 70-130

Surrogate percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly from the on-column percent recovery.

28 of 156 P1602483_TO15_1605261228_SC.xls - Surrogates TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 115-07-1 Propene 196 161 82 49-131 75-71-8 Dichlorodifluoromethane (CFC 12) 188 158 84 65-117 74-87-3 Chloromethane 200 154 77 48-132 1,2-Dichloro-1,1,2,2- 76-14-2 84 65-122 tetrafluoroethane (CFC 114) 204 172 75-01-4 Vinyl Chloride 200 161 81 65-128 106-99-0 1,3-Butadiene 206 246 119 62-143 74-83-9 Bromomethane 202 179 89 65-130 75-00-3 Chloroethane 200 176 88 69-126 64-17-5 Ethanol 998 951 95 57-126 75-05-8 Acetonitrile 212 165 78 51-134 107-02-8 Acrolein 214 176 82 55-146 67-64-1 Acetone 1,080 820 76 57-120 75-69-4 Trichlorofluoromethane 216 166 77 59-139 67-63-0 2-Propanol (Isopropyl Alcohol) 418 353 84 59-129 107-13-1 Acrylonitrile 212 175 83 64-136 75-35-4 1,1-Dichloroethene 216 187 87 72-123 75-09-2 Methylene Chloride 222 157 71 63-117 107-05-1 3-Chloro-1-propene (Allyl Chloride) 218 175 80 50-141 76-13-1 Trichlorotrifluoroethane 220 187 85 68-118 75-15-0 Carbon Disulfide 210 164 78 55-143 156-60-5 trans-1,2-Dichloroethene 210 183 87 69-129 75-34-3 1,1-Dichloroethane 212 170 80 66-122 1634-04-4 Methyl tert-Butyl Ether 216 179 83 55-128 108-05-4 Vinyl Acetate 1,040 969 93 66-140 78-93-3 2-Butanone (MEK) 220 194 88 62-127

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

29 of 156 P1602483_TO15_1605261228_SC.xls - LCS TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 2 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 156-59-2 cis-1,2-Dichloroethene 218 182 83 65-125 141-78-6 Ethyl Acetate 428 372 87 64-132 110-54-3 n-Hexane 212 161 76 58-126 67-66-3 Chloroform 224 185 83 68-117 109-99-9 Tetrahydrofuran (THF) 220 173 79 64-123 107-06-2 1,2-Dichloroethane 214 188 88 63-124 71-55-6 1,1,1-Trichloroethane 210 188 90 68-120 71-43-2 Benzene 226 164 73 61-110 56-23-5 Carbon Tetrachloride 230 198 86 65-137 110-82-7 Cyclohexane 424 351 83 68-122 78-87-5 1,2-Dichloropropane 216 178 82 67-122 75-27-4 Bromodichloromethane 218 194 89 71-124 79-01-6 Trichloroethene 216 188 87 71-121 123-91-1 1,4-Dioxane 210 216 103 67-122 80-62-6 Methyl Methacrylate 422 398 94 76-130 142-82-5 n-Heptane 216 177 82 67-125 10061-01-5 cis-1,3-Dichloropropene 208 192 92 73-131 108-10-1 4-Methyl-2-pentanone 220 196 89 66-132 10061-02-6 trans-1,3-Dichloropropene 210 191 91 76-135 79-00-5 1,1,2-Trichloroethane 216 194 90 73-121 108-88-3 Toluene 218 178 82 67-117 591-78-6 2-Hexanone 220 213 97 59-128 124-48-1 Dibromochloromethane 220 208 95 73-132 106-93-4 1,2-Dibromoethane 218 205 94 73-128 123-86-4 n-Butyl Acetate 226 207 92 61-136

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

30 of 156 P1602483_TO15_1605261228_SC.xls - LCS TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 3 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 111-65-9 n-Octane 210 168 80 67-124 127-18-4 Tetrachloroethene 202 189 94 65-126 108-90-7 Chlorobenzene 220 192 87 68-120 100-41-4 Ethylbenzene 218 191 88 69-123 179601-23-1 m,p-Xylenes 428 378 88 67-125 75-25-2 Bromoform 228 211 93 68-153 100-42-5 Styrene 222 209 94 68-132 95-47-6 o-Xylene 210 184 88 67-124 111-84-2 n-Nonane 204 165 81 60-130 79-34-5 1,1,2,2-Tetrachloroethane 210 188 90 72-128 98-82-8 Cumene 208 185 89 67-124 80-56-8 alpha-Pinene 212 190 90 67-129 103-65-1 n-Propylbenzene 204 182 89 67-125 622-96-8 4-Ethyltoluene 214 192 90 66-128 108-67-8 1,3,5-Trimethylbenzene 214 194 91 65-125 95-63-6 1,2,4-Trimethylbenzene 218 204 94 62-134 100-44-7 Benzyl Chloride 220 200 91 74-145 541-73-1 1,3-Dichlorobenzene 228 227 100 63-133 106-46-7 1,4-Dichlorobenzene 208 220 106 62-129 95-50-1 1,2-Dichlorobenzene 220 222 101 62-134 5989-27-5 d-Limonene 210 196 93 66-137 96-12-8 1,2-Dibromo-3-chloropropane 218 198 91 71-147 120-82-1 1,2,4-Trichlorobenzene 230 200 87 60-145 91-20-3 Naphthalene 218 191 88 56-158 87-68-3 Hexachlorobutadiene 230 238 103 56-139

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

31 of 156 P1602483_TO15_1605261228_SC.xls - LCS TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 115-07-1 Propene 196 152 78 49-131 75-71-8 Dichlorodifluoromethane (CFC 12) 188 150 80 65-117 74-87-3 Chloromethane 200 150 75 48-132 1,2-Dichloro-1,1,2,2- 76-14-2 83 65-122 tetrafluoroethane (CFC 114) 204 170 75-01-4 Vinyl Chloride 200 159 80 65-128 106-99-0 1,3-Butadiene 206 245 119 62-143 74-83-9 Bromomethane 202 178 88 65-130 75-00-3 Chloroethane 200 175 88 69-126 64-17-5 Ethanol 998 921 92 57-126 75-05-8 Acetonitrile 212 159 75 51-134 107-02-8 Acrolein 214 172 80 55-146 67-64-1 Acetone 1,080 801 74 57-120 75-69-4 Trichlorofluoromethane 216 159 74 59-139 67-63-0 2-Propanol (Isopropyl Alcohol) 418 339 81 59-129 107-13-1 Acrylonitrile 212 170 80 64-136 75-35-4 1,1-Dichloroethene 216 185 86 72-123 75-09-2 Methylene Chloride 222 154 69 63-117 107-05-1 3-Chloro-1-propene (Allyl Chloride) 218 168 77 50-141 76-13-1 Trichlorotrifluoroethane 220 186 85 68-118 75-15-0 Carbon Disulfide 210 161 77 55-143 156-60-5 trans-1,2-Dichloroethene 210 178 85 69-129 75-34-3 1,1-Dichloroethane 212 165 78 66-122 1634-04-4 Methyl tert-Butyl Ether 216 173 80 55-128 108-05-4 Vinyl Acetate 1,040 953 92 66-140 78-93-3 2-Butanone (MEK) 220 190 86 62-127

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

32 of 156 P1602483_TO15_1605261228_SC.xls - LCS (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 2 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 156-59-2 cis-1,2-Dichloroethene 218 176 81 65-125 141-78-6 Ethyl Acetate 428 364 85 64-132 110-54-3 n-Hexane 212 157 74 58-126 67-66-3 Chloroform 224 176 79 68-117 109-99-9 Tetrahydrofuran (THF) 220 168 76 64-123 107-06-2 1,2-Dichloroethane 214 176 82 63-124 71-55-6 1,1,1-Trichloroethane 210 180 86 68-120 71-43-2 Benzene 226 160 71 61-110 56-23-5 Carbon Tetrachloride 230 187 81 65-137 110-82-7 Cyclohexane 424 343 81 68-122 78-87-5 1,2-Dichloropropane 216 172 80 67-122 75-27-4 Bromodichloromethane 218 184 84 71-124 79-01-6 Trichloroethene 216 184 85 71-121 123-91-1 1,4-Dioxane 210 208 99 67-122 80-62-6 Methyl Methacrylate 422 392 93 76-130 142-82-5 n-Heptane 216 171 79 67-125 10061-01-5 cis-1,3-Dichloropropene 208 184 88 73-131 108-10-1 4-Methyl-2-pentanone 220 187 85 66-132 10061-02-6 trans-1,3-Dichloropropene 210 183 87 76-135 79-00-5 1,1,2-Trichloroethane 216 187 87 73-121 108-88-3 Toluene 218 172 79 67-117 591-78-6 2-Hexanone 220 200 91 59-128 124-48-1 Dibromochloromethane 220 200 91 73-132 106-93-4 1,2-Dibromoethane 218 198 91 73-128 123-86-4 n-Butyl Acetate 226 196 87 61-136

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

33 of 156 P1602483_TO15_1605261228_SC.xls - LCS (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARY Page 3 of 3

Client: Oneida Total Integrated Enterprises (OTIE) Client Sample ID: Lab Control Sample ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring ALS Sample ID: P160525-LCS

Test Code: EPA TO-15 Modified Date Collected: NA Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NA Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.125 Liter(s) Test Notes:

ALS CAS # Compound Spike Amount Result % Recovery Acceptance Data µg/m³ µg/m³ Limits Qualifier 111-65-9 n-Octane 210 160 76 67-124 127-18-4 Tetrachloroethene 202 183 91 65-126 108-90-7 Chlorobenzene 220 185 84 68-120 100-41-4 Ethylbenzene 218 184 84 69-123 179601-23-1 m,p-Xylenes 428 363 85 67-125 75-25-2 Bromoform 228 203 89 68-153 100-42-5 Styrene 222 202 91 68-132 95-47-6 o-Xylene 210 176 84 67-124 111-84-2 n-Nonane 204 156 76 60-130 79-34-5 1,1,2,2-Tetrachloroethane 210 180 86 72-128 98-82-8 Cumene 208 177 85 67-124 80-56-8 alpha-Pinene 212 181 85 67-129 103-65-1 n-Propylbenzene 204 173 85 67-125 622-96-8 4-Ethyltoluene 214 183 86 66-128 108-67-8 1,3,5-Trimethylbenzene 214 185 86 65-125 95-63-6 1,2,4-Trimethylbenzene 218 194 89 62-134 100-44-7 Benzyl Chloride 220 191 87 74-145 541-73-1 1,3-Dichlorobenzene 228 217 95 63-133 106-46-7 1,4-Dichlorobenzene 208 209 100 62-129 95-50-1 1,2-Dichlorobenzene 220 211 96 62-134 5989-27-5 d-Limonene 210 185 88 66-137 96-12-8 1,2-Dibromo-3-chloropropane 218 188 86 71-147 120-82-1 1,2,4-Trichlorobenzene 230 190 83 60-145 91-20-3 Naphthalene 218 181 83 56-158 87-68-3 Hexachlorobutadiene 230 225 98 56-139

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result. Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

34 of 156 P1602483_TO15_1605261228_SC.xls - LCS (2) TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 1

Client: Oneida Total Integrated Enterprises (OTIE) ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring

Internal Standard Area and RT Summary

Test Code: EPA TO-15 Modified Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Lab File ID: 05251601.D Analyst: Wida Ang Date Analyzed: 5/24/16 Sample Type: 1.0 L Bottle-Vac™(s) Time Analyzed: 23:11 Test Notes:

IS1 (BCM) IS2 (DFB) IS3 (CBZ) AREA # RT # AREA # RT # AREA # RT # 24 Hour Standard 99860 8.90 517535 10.88 218283 15.22 Upper Limit 139804 9.23 724549 11.21 305596 15.55 Lower Limit 59916 8.57 310521 10.55 130970 14.89

Client Sample ID 01 Method Blank 94179 8.89 491956 10.87 208053 15.22 02 Lab Control Sample 101579 8.91 518098 10.88 222485 15.23 03 SP-106-20160512 102043 8.89 531215 10.87 231182 15.22 04 SP-104-20160512 99127 8.89 521581 10.88 227680 15.23 05 06 07 08 09 10 11 12 13 14 15 16 17 18 19 20 IS1 (BCM) = Bromochloromethane IS2 (DFB) = 1,4-Difluorobenzene IS3 (CBZ) = Chlorobenzene-d5 AREA UPPER LIMIT = 140% of internal standard area AREA LOWER LIMIT = 60% of internal standard area RT UPPER LIMIT = 0.33 minutes of internal standard RT RT LOWER LIMIT = 0.33 minutes of internal standard RT # Column used to flag values outside QC limits with an I. I = Internal standard not within the specified limits.

35 of 156 P1602483_TO15_1605261228_SC.xls - ISS TO15SCAN.XLS - 75 Compounds - PageNo.: ALS ENVIRONMENTAL

RESULTS OF ANALYSIS Page 1 of 1

Client: Oneida Total Integrated Enterprises (OTIE) ALS Project ID: P1602483 Client Project ID: Pemaco - Plant Vapor Monitoring

Internal Standard Area and RT Summary

Test Code: EPA TO-15 Modified Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Lab File ID: 05251625.D Analyst: Wida Ang Date Analyzed: 5/25/16 Sample Type: 1.0 L Bottle-Vac™(s) Time Analyzed: 16:52 Test Notes:

IS1 (BCM) IS2 (DFB) IS3 (CBZ) AREA # RT # AREA # RT # AREA # RT # 24 Hour Standard 110473 8.92 566557 10.89 249800 15.23 Upper Limit 154662 9.25 793180 11.22 349720 15.56 Lower Limit 66284 8.59 339934 10.56 149880 14.90

Client Sample ID 01 Method Blank 105451 8.89 551714 10.87 232857 15.22 02 Lab Control Sample 115023 8.92 591634 10.88 253986 15.23 03 SP-104-20160512 (Dilution) 112265 8.89 586691 10.87 247730 15.22 04 05 06 07 08 09 10 11 12 13 14 15 16 17 18 19 20 IS1 (BCM) = Bromochloromethane IS2 (DFB) = 1,4-Difluorobenzene IS3 (CBZ) = Chlorobenzene-d5 AREA UPPER LIMIT = 140% of internal standard area AREA LOWER LIMIT = 60% of internal standard area RT UPPER LIMIT = 0.33 minutes of internal standard RT RT LOWER LIMIT = 0.33 minutes of internal standard RT # Column used to flag values outside QC limits with an I. I = Internal standard not within the specified limits.

36 of 156 P1602483_TO15_1605261228_SC.xls - ISS (2) TO15SCAN.XLS - 75 Compounds - PageNo.: Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251623.D Vial: 5 Acq On : 25 May 2016 15:44 Operator: WA Sample : P1602483-001 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:14:21 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 102043 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 531215 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 231182 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 161943 12.170 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.36% 57) Toluene-d8 (SS2) 13.31 98 530236 12.187 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.52% 73) Bromofluorobenzene (SS3) 16.84 174 202975 14.122 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 112.96%

Target Compounds Qvalue 2) Propene 3.71 42 3334 0.216 ng # 74 3) Dichlorodifluoromethan... 3.81 85 3432 0.114 ng # 92 4) Chloromethane 4.01 50 2009 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 4.16 135 1116 N.D. 6) Vinyl Chloride 4.28 62 1368 N.D. 7) 1,3-Butadiene 4.46 54 867 N.D. 8) Bromomethane 4.75 94 919 N.D. 9) Chloroethane 4.97 64 678 N.D. 10) Ethanol 5.18 45 804494 81.471 ng 99 11) Acetonitrile 5.36 41 1628 N.D. 12) Acrolein 5.51 56 1328 0.161 ng 97 13) Acetone 5.64 58 28127 2.430 ng 95 14) Trichlorofluoromethane 5.80 101 3013 0.124 ng 94 15) 2-Propanol (Isopropanol) 5.98 45 18268 0.492 ng 96 16) Acrylonitrile 6.16 53 742 N.D. 17) 1,1-Dichloroethene 6.50 96 698 N.D. 18) 2-Methyl-2-Propanol (t... 0.00 59 0 N.D. d 19) Methylene Chloride 6.63 84 3620 0.217 ng 98 20) 3-Chloro-1-propene (Al... 6.76 41 899 N.D. 21) Trichlorotrifluoroethane 6.95 151 1100 0.097 ng 96 22) Carbon Disulfide 6.93 76 3334 N.D. 23) trans-1,2-Dichloroethene 7.65 61 799 N.D. 24) 1,1-Dichloroethane 7.85 63 1832 N.D. 25) Methyl tert-Butyl Ether 7.97 73 3085 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 8.29 72 5738 0.626 ng # 86 28) cis-1,2-Dichloroethene 8.73 61 1463 N.D. 29) Diisopropyl Ether 0.00 87 0 N.D. d 30) Ethyl Acetate 9.00 61 1327 0.256 ng 87 31) n-Hexane 8.98 57 9666 0.383 ng 99 32) Chloroform 9.03 83 1819 N.D. 34) Tetrahydrofuran (THF) 9.48 72 1297 0.129 ng # 50 35) Ethyl tert-Butyl Ether 9.55 87 869 N.D. 36) 1,2-Dichloroethane 9.78 62 1115 N.D. 38) 1,1,1-Trichloroethane 10.05 97 1423 N.D. 39) Isopropyl Acetate 10.46 61 1009 0.113 ng # 1 40) 1-Butanol 0.00 56 0 N.D. d 41) Benzene 10.51 78 18802 0.298 ng 99 42) Carbon Tetrachloride 10.67 117 1228 N.D. 43) Cyclohexane 10.79 84 6427 0.287 ng 98 44) tert-Amyl Methyl Ether 11.14 73 2164 N.D. 45) 1,2-Dichloropropane 11.33 63 1008 N.D. 46) Bromodichloromethane 11.52 83 1497 N.D. 47) Trichloroethene 11.57 130 13452 0.890 ng 99 48) 1,4-Dioxane 11.60 88 679 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. d 50) Methyl Methacrylate 11.77 100 470 N.D. 37 of 156 R9042116.M Thu May 26 11:15:57 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251623.D Vial: 5 Acq On : 25 May 2016 15:44 Operator: WA Sample : P1602483-001 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:14:21 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 11.90 71 2029 0.137 ng 96 52) cis-1,3-Dichloropropene 12.43 75 976 N.D. 53) 4-Methyl-2-pentanone 12.48 58 905 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 13.12 97 767 N.D. 58) Toluene 13.42 91 47126 0.753 ng 97 59) 2-Hexanone 13.69 43 3368 0.113 ng 77 60) Dibromochloromethane 13.83 129 871 N.D. 61) 1,2-Dibromoethane 14.08 107 513 N.D. 62) n-Butyl Acetate 14.32 43 2309 N.D. 63) n-Octane 14.44 57 1229 N.D. 64) Tetrachloroethene 14.57 166 1184 N.D. 65) Chlorobenzene 15.27 112 2293 N.D. 66) Ethylbenzene 15.68 91 6494 0.098 ng 94 67) m- & p-Xylenes 15.86 91 10782 0.204 ng 95 68) Bromoform 15.93 173 462 N.D. 69) Styrene 16.25 104 3443 0.090 ng 88 70) o-Xylene 16.37 91 5203 0.095 ng 96 71) n-Nonane 16.61 43 2823 N.D. 72) 1,1,2,2-Tetrachloroethane 16.34 83 1386 N.D. 74) Cumene 16.99 105 5413 N.D. 75) alpha-Pinene 17.39 93 1539 N.D. 76) n-Propylbenzene 17.52 91 5721 N.D. 77) 3-Ethyltoluene 17.63 105 5325 N.D. 78) 4-Ethyltoluene 17.68 105 4637 N.D. 79) 1,3,5-Trimethylbenzene 17.75 105 4368 N.D. 80) alpha-Methylstyrene 17.92 118 2389 N.D. 81) 2-Ethyltoluene 17.96 105 4795 N.D. 82) 1,2,4-Trimethylbenzene 18.19 105 4731 N.D. 83) n-Decane 0.00 57 0 N.D. d 84) Benzyl Chloride 18.32 91 518 N.D. 85) 1,3-Dichlorobenzene 18.35 146 1279 N.D. 86) 1,4-Dichlorobenzene 18.41 146 1338 N.D. 87) sec-Butylbenzene 18.48 105 4784 N.D. 88) 4-Isopropyltoluene (p-... 18.64 119 4853 N.D. 89) 1,2,3-Trimethylbenzene 18.64 105 4102 N.D. 90) 1,2-Dichlorobenzene 18.77 146 1603 N.D. 91) d-Limonene 18.80 68 1973 N.D. 92) 1,2-Dibromo-3-Chloropr... 19.23 157 405 N.D. 93) n-Undecane 0.00 57 0 N.D. d 94) 1,2,4-Trichlorobenzene 20.59 180 839 N.D. 95) Naphthalene 20.71 128 4635 N.D. 96) n-Dodecane 0.00 57 0 N.D. d 97) Hexachlorobutadiene 21.07 225 940 N.D. 98) Cyclohexanone 0.00 55 0 N.D. d 99) tert-Butylbenzene 18.18 119 3865 N.D. 100) n-Butylbenzene 19.09 91 4436 N.D. ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

38 of 156 R9042116.M Thu May 26 11:15:57 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251623.D Vial: 5 Acq On : 25 May 2016 15:44 Operator: WA Sample : P1602483-001 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:14:21 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251623.D\data.ms 800000

750000

700000

650000 Chlorobenzene-d5 (IS3),IR Toluene-d8 (SS2),S

600000 Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR 550000

500000 Ethanol,T

450000

400000

350000

300000

250000 Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

200000

150000

100000 Acetone,T Toluene,T Trichloroethene,T n-Hexane,T Benzene,T Ethyl Acetate,T Propene,T Isopropyl Acetate,T Cyclohexane,T 2-Butanone (MEK),T

50000 Methylene Chloride,T m- & p-Xylenes,T 2-Propanol (Isopropanol),T n-Heptane,T o-Xylene,T Dichlorodifluoromethane (CFC 12),T Ethylbenzene,T Styrene,T Tetrahydrofuran (THF),T Trichlorofluoromethane,T Trichlorotrifluoroethane,T 2-Hexanone,T Acrolein,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0039 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:15:58 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251623.D Vial: 5 Acq On : 25 May 2016 15:44 Operator: WA Sample : P1602483-001 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:14:21 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 102043 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 531215 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 231182 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 161943 12.170 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.36% 57) Toluene-d8 (SS2) 13.31 98 530236 12.187 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.52% 73) Bromofluorobenzene (SS3) 16.84 174 202975 14.122 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 112.96%

Target Compounds Qvalue 2) Propene 3.71 42 3334 0.216 ng # 74 3) Dichlorodifluoromethan... 3.81 85 3432 0.114 ng # 92 10) Ethanol 5.18 45 804494 81.471 ng 99 12) Acrolein 5.51 56 1328 0.161 ng 97 13) Acetone 5.64 58 28127 2.430 ng 95 14) Trichlorofluoromethane 5.80 101 3013 0.124 ng 94 15) 2-Propanol (Isopropanol) 5.98 45 18268 0.492 ng 96 19) Methylene Chloride 6.63 84 3620 0.217 ng 98 21) Trichlorotrifluoroethane 6.95 151 1100 0.097 ng 96 27) 2-Butanone (MEK) 8.29 72 5738 0.626 ng # 86 30) Ethyl Acetate 9.00 61 1327 0.256 ng 87 31) n-Hexane 8.98 57 9666 0.383 ng 99 34) Tetrahydrofuran (THF) 9.48 72 1297 0.129 ng # 50 39) Isopropyl Acetate 10.46 61 1009 0.113 ng # 1 41) Benzene 10.51 78 18802 0.298 ng 99 43) Cyclohexane 10.79 84 6427 0.287 ng 98 47) Trichloroethene 11.57 130 13452 0.890 ng 99 51) n-Heptane 11.90 71 2029 0.137 ng 96 58) Toluene 13.42 91 47126 0.753 ng 97 59) 2-Hexanone 13.69 43 3368 0.113 ng 77 66) Ethylbenzene 15.68 91 6494 0.098 ng 94 67) m- & p-Xylenes 15.86 91 10782 0.204 ng 95 69) Styrene 16.25 104 3443 0.090 ng 88 70) o-Xylene 16.37 91 5203 0.095 ng 96 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

40 of 156 R9042116.M Thu May 26 11:15:33 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251623.D Vial: 5 Acq On : 25 May 2016 15:44 Operator: WA Sample : P1602483-001 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:14:21 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251623.D\data.ms 800000

750000

700000

650000 Chlorobenzene-d5 (IS3),IR Toluene-d8 (SS2),S

600000 Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR 550000

500000 Ethanol,T

450000

400000

350000

300000

250000 Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

200000

150000

100000 Acetone,T Toluene,T Trichloroethene,T n-Hexane,T Benzene,T Ethyl Acetate,T Propene,T Isopropyl Acetate,T Cyclohexane,T 2-Butanone (MEK),T

50000 Methylene Chloride,T m- & p-Xylenes,T 2-Propanol (Isopropanol),T n-Heptane,T o-Xylene,T Dichlorodifluoromethane (CFC 12),T Ethylbenzene,T Styrene,T Tetrahydrofuran (THF),T Trichlorofluoromethane,T Trichlorotrifluoroethane,T 2-Hexanone,T Acrolein,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0041 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:15:33 2016 Page: 2 Abundance Scan 53 (3.672 min): 04211627.D\data.ms (-44) (-) #2 41 Propene Concen: 0.22 ng RT: 3.71 min Scan# 60 Ref 50 Delta R.T. 0.027 min Lab File: 05251623.D 38 Acq: 25 May 2016 15:44 32 60 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 Tgt Ion: 42 Resp: 3334 Abundance Scan 60 (3.711 min): 05251623.D\data.ms Ion Ratio Lower Upper 29 42 100 39 138.3 83.4 123.4# 41 41 176.7 130.1 170.1# 44 Raw 50 32 Abundance 51 38 3000 60 67 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 Abundance Scan 60 (3.711 min): 05251623.D\data.ms (-9) (-) 2000 41 3.711

Sub 1000 50 51 38 32 60 67 0 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 Time--> 3.65 3.70 3.75

Abundance Scan 72 (3.776 min): 04211627.D\data.ms (-63) (-) #3 85 Dichlorodifluoromethane (CFC 12) Concen: 0.11 ng RT: 3.81 min Scan# 78 Ref 50 Delta R.T. 0.022 min Lab File: 05251623.D 50 101 Acq: 25 May 2016 15:44 35 4266 74 122 0 m/z--> 20 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 85 Resp: 3432 Abundance Scan 78 (3.809 min): 05251623.D\data.ms Ion Ratio Lower Upper 85 85 100 32 87 31.1 12.1 52.1 101 0.0 0.0 28.9 Raw 50 103 0.0 0.0 25.7 Abundance 3.809 44 101 2000 0 m/z--> 20 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 78 (3.809 min): 05251623.D\data.ms (-28) (-) 1500 85 1000 Sub 50 500 32 50 101 0 0 m/z--> 20 30 40 50 60 70 80 90 100 110 120 130 Time--> 3.75 3.80 3.85

42 of 156 05251623.D R9042116.M Thu May 26 11:15:34 2016 Page 3 Abundance Scan 337 (5.197 min): 04211627.D\data.ms (-318) (-) #10 45 Ethanol Concen: 81.47 ng RT: 5.18 min Scan# 333 Ref 50 Delta R.T. -0.077 min Lab File: 05251623.D 43 Acq: 25 May 2016 15:44 33 41 47 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Tgt Ion: 45 Resp: 804494 Abundance Scan 333 (5.176 min): 05251623.D\data.ms Ion Ratio Lower Upper 45 45 100 46 36.5 16.8 56.8

Raw 50 Abundance 43 250000 5.176 33 41 47 0 200000 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Abundance Scan 333 (5.176 min): 05251623.D\data.ms (-280) (-) 45 150000

Sub 100000 50 50000 43 33 41 47 0 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Time--> 5.00 5.20 5.40 5.60

Abundance Scan 394 (5.491 min): 04211627.D\data.ms (-380) (-) #12 56 Acrolein Concen: 0.16 ng RT: 5.51 min Scan# 397 Ref 50 Delta R.T. -0.011 min Lab File: 05251623.D Acq: 25 May 2016 15:44 37 53 39 58 0 m/z--> 30 35 40 45 50 55 60 65 Tgt Ion: 56 Resp: 1328 Abundance Scan 397 (5.507 min): 05251623.D\data.ms Ion Ratio Lower Upper 56 56 100 55 66.6 48.8 88.8 40 45 Raw 50 Abundance 5.507 400 0 m/z--> 30 35 40 45 50 55 60 65 Abundance Scan 397 (5.507 min): 05251623.D\data.ms (-351) (-) 300 56 200 Sub 50 41 100

0 0 m/z--> 30 35 40 45 50 55 60 65 Time--> 5.45 5.50 5.55

43 of 156 05251623.D R9042116.M Thu May 26 11:15:34 2016 Page 4 Abundance Scan 423 (5.640 min): 04211627.D\data.ms (-408) (-) #13 43 Acetone Concen: 2.43 ng RT: 5.64 min Scan# 422 Ref 50 Delta R.T. -0.041 min 58 Lab File: 05251623.D Acq: 25 May 2016 15:44 3739 41 45 52 54 56 60 0 m/z--> 30 35 40 45 50 55 60 65 Tgt Ion: 58 Resp: 28127 Abundance Scan 422 (5.635 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 58 100 43 293.6 255.0 315.0

Raw 50 58 Abundance 30000 37 3941 4553 55 0 m/z--> 30 35 40 45 50 55 60 65 Abundance Scan 422 (5.635 min): 05251623.D\data.ms (-382) (-) 20000 43

Sub 5.635 50 10000 58

37 3941 53 55 0 0 m/z--> 30 35 40 45 50 55 60 65 Time--> 5.60 5.70

Abundance Scan 453 (5.795 min): 04211627.D\data.ms (-440) (-) #14 101 Trichlorofluoromethane Concen: 0.12 ng RT: 5.80 min Scan# 453 Ref 50 Delta R.T. -0.010 min Lab File: 05251623.D Acq: 25 May 2016 15:44 4735 66 74 82 117 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion:101 Resp: 3013 Abundance Scan 453 (5.795 min): 05251623.D\data.ms Ion Ratio Lower Upper 101 101 100 103 59.5 44.5 84.5

Raw 50 Abundance 43 5.795 58 1500 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 453 (5.795 min): 05251623.D\data.ms (-407) (-) 1000 101

Sub 50 500 43 58 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 5.75 5.80 5.85

44 of 156 05251623.D R9042116.M Thu May 26 11:15:35 2016 Page 5 Abundance Scan 488 (5.976 min): 04211627.D\data.ms (-469) (-) #15 45 2-Propanol (Isopropanol) Concen: 0.49 ng RT: 5.98 min Scan# 488 Ref 50 Delta R.T. -0.046 min Lab File: 05251623.D Acq: 25 May 2016 15:44 33 59 207 0 m/z--> 40 60 80 100 120 140 160 180 200 Tgt Ion: 45 Resp: 18268 Abundance Scan 488 (5.976 min): 05251623.D\data.ms Ion Ratio Lower Upper 45 45 100 43 18.7 0.0 37.0

Raw 50 Abundance 5.976 59 0 m/z--> 40 60 80 100 120 140 160 180 200 4000 Abundance Scan 488 (5.976 min): 05251623.D\data.ms (-449) (-) 45

Sub 2000 50

59 0 0 m/z--> 40 60 80 100 120 140 160 180 200 Time--> 5.80 5.90 6.00 6.10 6.20

Abundance Scan 619 (6.651 min): 04211627.D\data.ms (-603) (-) #19 49 84 Methylene Chloride Concen: 0.22 ng RT: 6.63 min Scan# 615 Ref 50 Delta R.T. -0.041 min Lab File: 05251623.D 59 Acq: 25 May 2016 15:44 4135 88 38 5345 7073 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Tgt Ion: 84 Resp: 3620 Abundance Scan 615 (6.631 min): 05251623.D\data.ms Ion Ratio Lower Upper 59 84 100 49 126.0 99.2 149.2 49 84 Raw 50 Abundance 43 35 39 88 0 6.631 1500 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Abundance Scan 615 (6.631 min): 05251623.D\data.ms (-575) (-) 59 1000 49 Sub 84 50 500 43 35 39 88 0 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Time--> 6.55 6.60 6.65 6.70

45 of 156 05251623.D R9042116.M Thu May 26 11:15:35 2016 Page 6 Abundance Scan 675 (6.940 min): 04211627.D\data.ms (-659) (-) #21 101 Trichlorotrifluoroethane 151 Concen: 0.10 ng RT: 6.95 min Scan# 676 Ref 50 85 Delta R.T. -0.010 min Lab File: 05251623.D 66 Acq: 25 May 2016 15:44 47 116 35 132 171 0 m/z--> 40 60 80 100 120 140 160 Tgt Ion:151 Resp: 1100 Abundance Scan 676 (6.945 min): 05251623.D\data.ms Ion Ratio Lower Upper 76101 151 151 100 101 131.0 106.1 146.1

Raw 50 Abundance 40 6.945 600 0 m/z--> 40 60 80 100 120 140 160 Abundance Scan 676 (6.945 min): 05251623.D\data.ms (-630) (-) 400 76101 151

Sub 50 200 40

0 0 m/z--> 40 60 80 100 120 140 160 Time--> 6.90 6.95

Abundance Scan 937 (8.291 min): 04211627.D\data.ms (-925) (-) #27 43 2-Butanone (MEK) Concen: 0.63 ng RT: 8.29 min Scan# 937 Ref 50 Delta R.T. -0.031 min 72 Lab File: 05251623.D Acq: 25 May 2016 15:44 57 53 69 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 Tgt Ion: 72 Resp: 5738 Abundance Scan 937 (8.291 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 72 100 43 349.1 362.0 402.0#

Raw 50 Abundance 72 57 8000 39 51 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 6000 Abundance Scan 937 (8.291 min): 05251623.D\data.ms (-895) (-) 72 4000 43 Sub 50 8.291 2000

51 57 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 Time--> 8.25 8.30 8.35 8.40

46 of 156 05251623.D R9042116.M Thu May 26 11:15:35 2016 Page 7 Abundance Scan 1073 (8.992 min): 04211627.D\data.ms (-1060) (-) #30 43 Ethyl Acetate Concen: 0.26 ng RT: 9.00 min Scan# 1074 Ref 50 Delta R.T. -0.021 min 57 Lab File: 05251623.D 70 87 Acq: 25 May 2016 15:44 101 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 61 Resp: 1327 Abundance Scan 1074 (8.998 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 61 100 70 68.0 59.0 99.0

Raw 50 57 Abundance 600 8.998 130 70 87 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1074 (8.998 min): 05251623.D\data.ms (-1030) (-) 400 43

Sub 200 50 57

130 70 87 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 8.95 9.00 9.05

Abundance Scan 1072 (8.987 min): 04211627.D\data.ms (-1058) (-) #31 43 n-Hexane Concen: 0.38 ng RT: 8.98 min Scan# 1071 Ref 50 Delta R.T. -0.015 min 57 Lab File: 05251623.D Acq: 25 May 2016 15:44 70 87 78 101 120 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 57 Resp: 9666 Abundance Scan 1071 (8.982 min): 05251623.D\data.ms Ion Ratio Lower Upper 5743 57 100 56 50.5 40.9 61.3 86 15.0 11.4 17.2 Raw 50 Abundance 8.982 86 130 71 95 4000 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1071 (8.982 min): 05251623.D\data.ms (-1026) (-) 3000 5743 2000 Sub 50 1000 86 130 70 95 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 8.90 8.95 9.00 9.05

47 of 156 05251623.D R9042116.M Thu May 26 11:15:36 2016 Page 8 Abundance Scan 1160 (9.441 min): 04211627.D\data.ms (-1149) (-) #34 42 Tetrahydrofuran (THF) Concen: 0.13 ng RT: 9.48 min Scan# 1167 Ref 50 72 Delta R.T. 0.026 min Lab File: 05251623.D 39 Acq: 25 May 2016 15:44 3545 49 52 55 68 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Tgt Ion: 72 Resp: 1297 Abundance Scan 1167 (9.477 min): 05251623.D\data.ms Ion Ratio Lower Upper 42 72 100 71 98.1 76.2 116.2 42 342.9 206.6 246.6# Raw 50 72 Abundance 39 1500 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Abundance Scan 1167 (9.477 min): 05251623.D\data.ms (-1114) (-) 42 1000 9.477 Sub 50 72 500 39

0 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Time--> 9.45 9.50

Abundance Scan 1354 (10.441 min): 04211627.D\data.ms (-1342) (-) #39 43 Isopropyl Acetate Concen: 0.11 ng RT: 10.46 min Scan# 1357 Ref 50 Delta R.T. -0.000 min Lab File: 05251623.D 61 87 Acq: 25 May 2016 15:44 33 49 55 73 101 0 m/z--> 30 40 50 60 70 80 90 100 110 Tgt Ion: 61 Resp: 1009 Abundance Scan 1357 (10.457 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 56 61 100 87 54.8 31.6 71.6 43 1771.5 501.6 541.6# Raw 50 Abundance 5000 87 0 m/z--> 30 40 50 60 70 80 90 100 110 4000 Abundance Scan 1357 (10.457 min): 05251623.D\data.ms (-1309) (-) 43 56 3000

Sub 2000 50 1000 10.457 87 0 0 m/z--> 30 40 50 60 70 80 90 100 110 Time--> 10.40 10.45 10.50

48 of 156 05251623.D R9042116.M Thu May 26 11:15:36 2016 Page 9 Abundance Scan 1370 (10.524 min): 04211627.D\data.ms (-1356) (-) #41 78 Benzene Concen: 0.30 ng RT: 10.51 min Scan# 1368 Ref 50 Delta R.T. -0.026 min Lab File: 05251623.D 52 Acq: 25 May 2016 15:44 37 49 63 74 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Tgt Ion: 78 Resp: 18802 Abundance Scan 1368 (10.514 min): 05251623.D\data.ms Ion Ratio Lower Upper 78 78 100 77 23.2 3.9 43.9

Raw 50 Abundance 56 41 52 8000 10.514 3844 49 63 74 84 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 6000 Abundance Scan 1368 (10.514 min): 05251623.D\data.ms (-1325) (-) 78 4000 Sub 50 2000 56 41 52 3844 49 63 74 84 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Time--> 10.50 10.60

Abundance Scan 1424 (10.802 min): 04211627.D\data.ms (-1410) (-) #43 56 84 Cyclohexane Concen: 0.29 ng RT: 10.79 min Scan# 1422 41 Ref 50 Delta R.T. -0.021 min 69 Lab File: 05251623.D Acq: 25 May 2016 15:44 38 445053 6063 66 74 79 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Tgt Ion: 84 Resp: 6427 Abundance Scan 1422 (10.792 min): 05251623.D\data.ms Ion Ratio Lower Upper 56 84 100 84 69 39.0 17.1 57.1 56 122.0 100.6 140.6 41 Raw 50 69 Abundance

53 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 4000 Abundance Scan 1422 (10.792 min): 05251623.D\data.ms (-1378) (-) 56 84 10.792

Sub 41 2000 50 69

53 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Time--> 10.70 10.75 10.80 10.85

49 of 156 05251623.D R9042116.M Thu May 26 11:15:36 2016 Page 10 Abundance Scan 1575 (11.581 min): 04211627.D\data.ms (-1558) (-) #47 95 130 Trichloroethene Concen: 0.89 ng RT: 11.57 min Scan# 1573 Ref 50 60 Delta R.T. -0.021 min Lab File: 05251623.D Acq: 25 May 2016 15:44 35 47 68 82 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Tgt Ion:130 Resp: 13452 Abundance Scan 1573 (11.571 min): 05251623.D\data.ms Ion Ratio Lower Upper 95 130 130 100 132 94.6 75.8 115.8

Raw 50 60 Abundance 6000 11.571 35 47 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Abundance Scan 1573 (11.571 min): 05251623.D\data.ms (-1529) (-) 4000 95 130

Sub 2000 50 60

35 47 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Time--> 11.50 11.55 11.60 11.65

Abundance Scan 1637 (11.900 min): 04211627.D\data.ms (-1626) (-) #51 43 n-Heptane Concen: 0.14 ng 71 RT: 11.90 min Scan# 1636 Ref 50 Delta R.T. -0.015 min Lab File: 05251623.D 100 Acq: 25 May 2016 15:44 281 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Tgt Ion: 71 Resp: 2029 Abundance Scan 1636 (11.896 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 71 100 57 97.2 72.3 112.3 71 100 26.6 6.1 46.1 Raw 50 Abundance 100 11.896 1000 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 800 Abundance Scan 1636 (11.896 min): 05251623.D\data.ms (-1591) (-) 43 600 71 Sub 400 50 100 200

0 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Time--> 11.85 11.90

50 of 156 05251623.D R9042116.M Thu May 26 11:15:37 2016 Page 11 Abundance Scan 1932 (13.422 min): 04211627.D\data.ms (-1919) (-) #58 91 Toluene Concen: 0.75 ng RT: 13.42 min Scan# 1931 Ref 50 Delta R.T. -0.010 min Lab File: 05251623.D Acq: 25 May 2016 15:44 39 65 45 51 8574 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 91 Resp: 47126 Abundance Scan 1931 (13.417 min): 05251623.D\data.ms Ion Ratio Lower Upper 91 91 100 92 56.5 38.5 78.5

Raw 50 Abundance 13.417 39 65 4551 57 74 85 98 20000 0 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 1931 (13.417 min): 05251623.D\data.ms (-1885) (-) 15000 91 10000 Sub 50 5000

39 65 4551 57 74 85 98 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 13.40 13.50

Abundance Scan 1979 (13.664 min): 04211627.D\data.ms (-1967) (-) #59 43 2-Hexanone Concen: 0.11 ng 58 RT: 13.69 min Scan# 1984 Ref 50 Delta R.T. 0.015 min Lab File: 05251623.D Acq: 25 May 2016 15:44 71 85 100 37 50 65 77 91 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 43 Resp: 3368 Abundance Scan 1984 (13.690 min): 05251623.D\data.ms Ion Ratio Lower Upper 43 43 100 58 41.8 39.4 79.4

Raw 50 58 Abundance 13.690

0 1000 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 1984 (13.690 min): 05251623.D\data.ms (-1933) (-) 43

Sub 58 500 50

0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 13.60 13.65 13.70 13.75

51 of 156 05251623.D R9042116.M Thu May 26 11:15:37 2016 Page 12 Abundance Scan 2369 (15.675 min): 04211627.D\data.ms (-2357) (-) #66 91 Ethylbenzene Concen: 0.10 ng RT: 15.68 min Scan# 2369 Ref 50 Delta R.T. -0.005 min 106 Lab File: 05251623.D Acq: 25 May 2016 15:44 5165 77 39 84 97 0 m/z--> 30 40 50 60 70 80 90 100 110 Tgt Ion: 91 Resp: 6494 Abundance Scan 2369 (15.675 min): 05251623.D\data.ms Ion Ratio Lower Upper 91 91 100 106 28.8 11.9 51.9

Raw 50 106 Abundance 15.675 3000 40 5165 77 0 m/z--> 30 40 50 60 70 80 90 100 110 Abundance Scan 2369 (15.675 min): 05251623.D\data.ms (-2322) (-) 2000 91

Sub 50 1000 106

40 51 65 77 0 0 m/z--> 30 40 50 60 70 80 90 100 110 Time--> 15.60 15.65 15.70 15.75

Abundance Scan 2407 (15.871 min): 04211627.D\data.ms (-2393) (-) #67 91 m- & p-Xylenes Concen: 0.20 ng RT: 15.86 min Scan# 2405 106 Ref 50 Delta R.T. -0.021 min Lab File: 05251623.D 77 Acq: 25 May 2016 15:44 39 51 65 84 97 0 m/z--> 30 40 50 60 70 80 90 100 110 Tgt Ion: 91 Resp: 10782 Abundance Scan 2405 (15.861 min): 05251623.D\data.ms Ion Ratio Lower Upper 91 91 100 106 52.9 29.4 69.4 106 Raw 50 Abundance 15.861 77 39 51 65 0 3000 m/z--> 30 40 50 60 70 80 90 100 110 Abundance Scan 2405 (15.861 min): 05251623.D\data.ms (-2361) (-) 91 2000

Sub 106 50 1000

77 39 51 65 0 0 m/z--> 30 40 50 60 70 80 90 100 110 Time--> 15.80 15.90

52 of 156 05251623.D R9042116.M Thu May 26 11:15:37 2016 Page 13 Abundance Scan 2480 (16.248 min): 04211627.D\data.ms (-2469) (-) #69 104 Styrene Concen: 0.09 ng RT: 16.25 min Scan# 2481 Ref 50 78 Delta R.T. -0.000 min 51 Lab File: 05251623.D Acq: 25 May 2016 15:44 39 63 89 98 0 m/z--> 30 40 50 60 70 80 90 100 110 Tgt Ion:104 Resp: 3443 Abundance Scan 2481 (16.253 min): 05251623.D\data.ms Ion Ratio Lower Upper 104 104 100 78 31.5 20.7 60.7 103 41.1 27.9 67.9 Raw 50 78 Abundance 44 51 16.253 57 70 1500 0 m/z--> 30 40 50 60 70 80 90 100 110 Abundance Scan 2481 (16.253 min): 05251623.D\data.ms (-2433) (-) 1000 104

Sub 50 500 78 51 39 0 0 m/z--> 30 40 50 60 70 80 90 100 110 Time--> 16.20 16.25 16.30

Abundance Scan 2503 (16.366 min): 04211627.D\data.ms (-2493) (-) #70 91 o-Xylene Concen: 0.09 ng RT: 16.37 min Scan# 2503 Ref 50 106 Delta R.T. -0.010 min Lab File: 05251623.D 77 Acq: 25 May 2016 15:44 39 51 65 98 0 m/z--> 30 40 50 60 70 80 90 100 110 Tgt Ion: 91 Resp: 5203 Abundance Scan 2503 (16.366 min): 05251623.D\data.ms Ion Ratio Lower Upper 91 91 100 106 45.8 28.3 68.3

Raw 50 106 Abundance 16.366 39 51 61 77 2500 0 m/z--> 30 40 50 60 70 80 90 100 110 2000 Abundance Scan 2503 (16.366 min): 05251623.D\data.ms (-2457) (-) 91 1500

Sub 1000 50 106 500 3951 61 77 0 0 m/z--> 30 40 50 60 70 80 90 100 110 Time--> 16.30 16.35 16.40

53 of 156 05251623.D R9042116.M Thu May 26 11:15:38 2016 Page 14 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:51:14 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 99127 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.88 114 521581 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 227680 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 160406 12.409 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.28% 57) Toluene-d8 (SS2) 13.32 98 520612 12.150 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.20% 73) Bromofluorobenzene (SS3) 16.84 174 201024 14.202 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 113.60%

Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. d 3) Dichlorodifluoromethan... 0.00 85 0 N.D. d 4) Chloromethane 4.01 50 2634 0.107 ng 93 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 4.29 62 10505 0.502 ng 97 7) 1,3-Butadiene 0.00 54 0 N.D. d 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.15 45 100712 10.499 ng 98 11) Acetonitrile 5.41 41 2380 N.D. 12) Acrolein 0.00 56 0 N.D. d 13) Acetone 5.61 58 150516m 13.384 ng 14) Trichlorofluoromethane 5.81 101 10726 0.455 ng 99 15) 2-Propanol (Isopropanol) 5.95 45 16343 0.454 ng # 61 16) Acrylonitrile 6.11 53 251 N.D. 17) 1,1-Dichloroethene 6.50 96 95864 7.389 ng 99 18) 2-Methyl-2-Propanol (t... 0.00 59 0 N.D. d 19) Methylene Chloride 6.62 84 4374 0.270 ng 97 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. d 21) Trichlorotrifluoroethane 6.96 151 1411 0.128 ng 83 22) Carbon Disulfide 6.92 76 2136 N.D. 23) trans-1,2-Dichloroethene 7.65 61 11782 0.618 ng 99 24) 1,1-Dichloroethane 7.86 63 41960 1.623 ng 99 25) Methyl tert-Butyl Ether 7.90 73 811 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 8.30 72 9177 1.031 ng 97 28) cis-1,2-Dichloroethene 8.73 61 208820 11.171 ng 100 29) Diisopropyl Ether 0.00 87 0 N.D. d 30) Ethyl Acetate 0.00 61 0 N.D. d 31) n-Hexane 9.00 57 1364580 55.679 ng 100 32) Chloroform 9.04 83 91227 3.913 ng 93 34) Tetrahydrofuran (THF) 9.46 72 9271 0.947 ng 91 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. d 38) 1,1,1-Trichloroethane 10.06 97 13138 0.649 ng 98 39) Isopropyl Acetate 0.00 61 0 N.D. d 40) 1-Butanol 0.00 56 0 N.D. d 41) Benzene 10.52 78 229911 3.710 ng 99 42) Carbon Tetrachloride 10.67 117 1274 N.D. 43) Cyclohexane 10.81 84 806262 36.648 ng 99 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 11.24 63 800 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. d 47) Trichloroethene 11.58 130 2779295 187.203 ng 100 48) 1,4-Dioxane 0.00 88 0 N.D. d 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. d 50) Methyl Methacrylate 0.00 100 0 N.D. d 54 of 156 R9042116.M Thu May 26 11:52:45 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:51:14 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 11.90 71 205364 14.128 ng 100 52) cis-1,3-Dichloropropene 12.56 75 515 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. d 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. d 58) Toluene 13.42 91 29434 0.478 ng 99 59) 2-Hexanone 0.00 43 0 N.D. d 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. d 63) n-Octane 14.44 57 35570 2.629 ng 98 64) Tetrachloroethene 14.57 166 764660 47.839 ng 100 65) Chlorobenzene 0.00 112 0 N.D. d 66) Ethylbenzene 15.68 91 20703 0.318 ng 98 67) m- & p-Xylenes 15.86 91 19892 0.382 ng 99 68) Bromoform 0.00 173 0 N.D. 69) Styrene 16.25 104 950 N.D. 70) o-Xylene 16.37 91 6920 0.128 ng 90 71) n-Nonane 16.61 43 6306 0.201 ng 82 72) 1,1,2,2-Tetrachloroethane 16.37 83 845 N.D. 74) Cumene 16.98 105 12031 0.178 ng 98 75) alpha-Pinene 17.40 93 1375 N.D. 76) n-Propylbenzene 17.52 91 11517 0.138 ng 79 77) 3-Ethyltoluene 17.63 105 3635 N.D. 78) 4-Ethyltoluene 17.67 105 3159 N.D. 79) 1,3,5-Trimethylbenzene 17.76 105 3146 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. d 81) 2-Ethyltoluene 17.95 105 2684 N.D. 82) 1,2,4-Trimethylbenzene 18.19 105 12408 0.236 ng 87 83) n-Decane 0.00 57 0 N.D. d 84) Benzyl Chloride 18.35 91 1524 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. d 88) 4-Isopropyltoluene (p-... 18.64 119 2402 N.D. 89) 1,2,3-Trimethylbenzene 18.64 105 3929 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. d 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. d 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.71 128 6450 N.D. 96) n-Dodecane 0.00 57 0 N.D. d 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. d 99) tert-Butylbenzene 18.19 119 2601 N.D. 100) n-Butylbenzene 19.08 91 3904 N.D. ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

55 of 156 R9042116.M Thu May 26 11:52:45 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:51:14 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251624.D\data.ms 2.1e+07

2e+07

1.9e+07

1.8e+07

1.7e+07

1.6e+07

1.5e+07

1.4e+07

1.3e+07

1.2e+07

1.1e+07

1e+07

9000000

8000000 Trichloroethene,T

7000000

6000000

5000000

4000000 n-Hexane,T 3000000 Tetrachloroethene,T Cyclohexane,T

2000000 n-Heptane,T Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR Acetone,T cis-1,2-Dichloroethene,T Bromochloromethane (IS1),IR Benzene,T 1,1-Dichloroethene,T 1,2-Dichloroethane-d4(SS1),S n-Octane,T Chloroform,T 1,2,4-Trimethylbenzene,T Cumene,T Ethylbenzene,T Toluene,T o-Xylene,T Vinyl Chloride,T Ethanol,T n-Propylbenzene,T m- & p-Xylenes,T n-Nonane,T 1,1-Dichloroethane,T Tetrahydrofuran (THF),T 1,1,1-Trichloroethane,T 2-Butanone (MEK),T Trichlorofluoromethane,T Chloromethane,T trans-1,2-Dichloroethene,T 2-Propanol (Isopropanol),T Methylene Chloride,T 1000000 Trichlorotrifluoroethane,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0056 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:52:46 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:51:14 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 99127 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.88 114 521581 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 227680 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 160406 12.409 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.28% 57) Toluene-d8 (SS2) 13.32 98 520612 12.150 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.20% 73) Bromofluorobenzene (SS3) 16.84 174 201024 14.202 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 113.60%

Target Compounds Qvalue 4) Chloromethane 4.01 50 2634 0.107 ng 93 6) Vinyl Chloride 4.29 62 10505 0.502 ng 97 10) Ethanol 5.15 45 100712 10.499 ng 98 13) Acetone 5.61 58 150516m 13.384 ng 14) Trichlorofluoromethane 5.81 101 10726 0.455 ng 99 15) 2-Propanol (Isopropanol) 5.95 45 16343 0.454 ng # 61 17) 1,1-Dichloroethene 6.50 96 95864 7.389 ng 99 19) Methylene Chloride 6.62 84 4374 0.270 ng 97 21) Trichlorotrifluoroethane 6.96 151 1411 0.128 ng 83 23) trans-1,2-Dichloroethene 7.65 61 11782 0.618 ng 99 24) 1,1-Dichloroethane 7.86 63 41960 1.623 ng 99 27) 2-Butanone (MEK) 8.30 72 9177 1.031 ng 97 28) cis-1,2-Dichloroethene 8.73 61 208820 11.171 ng 100 31) n-Hexane 9.00 57 1364580 55.679 ng 100 32) Chloroform 9.04 83 91227 3.913 ng 93 34) Tetrahydrofuran (THF) 9.46 72 9271 0.947 ng 91 38) 1,1,1-Trichloroethane 10.06 97 13138 0.649 ng 98 41) Benzene 10.52 78 229911 3.710 ng 99 43) Cyclohexane 10.81 84 806262 36.648 ng 99 47) Trichloroethene 11.58 130 2779295 187.203 ng 100 51) n-Heptane 11.90 71 205364 14.128 ng 100 58) Toluene 13.42 91 29434 0.478 ng 99 63) n-Octane 14.44 57 35570 2.629 ng 98 64) Tetrachloroethene 14.57 166 764660 47.839 ng 100 66) Ethylbenzene 15.68 91 20703 0.318 ng 98 67) m- & p-Xylenes 15.86 91 19892 0.382 ng 99 70) o-Xylene 16.37 91 6920 0.128 ng 90 71) n-Nonane 16.61 43 6306 0.201 ng 82 74) Cumene 16.98 105 12031 0.178 ng 98 76) n-Propylbenzene 17.52 91 11517 0.138 ng 79 82) 1,2,4-Trimethylbenzene 18.19 105 12408 0.236 ng 87 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

57 of 156 R9042116.M Thu May 26 11:52:07 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:51:14 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251624.D\data.ms 2.1e+07

2e+07

1.9e+07

1.8e+07

1.7e+07

1.6e+07

1.5e+07

1.4e+07

1.3e+07

1.2e+07

1.1e+07

1e+07

9000000

8000000 Trichloroethene,T

7000000

6000000

5000000

4000000 n-Hexane,T 3000000 Tetrachloroethene,T Cyclohexane,T

2000000 n-Heptane,T Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR Acetone,T cis-1,2-Dichloroethene,T Bromochloromethane (IS1),IR Benzene,T 1,1-Dichloroethene,T 1,2-Dichloroethane-d4(SS1),S n-Octane,T Chloroform,T 1,2,4-Trimethylbenzene,T Cumene,T Ethylbenzene,T Toluene,T o-Xylene,T Vinyl Chloride,T Ethanol,T n-Propylbenzene,T m- & p-Xylenes,T n-Nonane,T 1,1-Dichloroethane,T Tetrahydrofuran (THF),T 1,1,1-Trichloroethane,T 2-Butanone (MEK),T Trichlorofluoromethane,T Chloromethane,T trans-1,2-Dichloroethene,T 2-Propanol (Isopropanol),T Methylene Chloride,T 1000000 Trichlorotrifluoroethane,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0058 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:52:08 2016 Page: 2 Abundance Scan 108 (3.974 min): 04211627.D\data.ms (-98) (-) #4 50 Chloromethane Concen: 0.11 ng RT: 4.01 min Scan# 114 Ref 50 Delta R.T. 0.016 min Lab File: 05251624.D Acq: 25 May 2016 16:18 2935 39 44 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 Tgt Ion: 50 Resp: 2634 Abundance Scan 114 (4.007 min): 05251624.D\data.ms Ion Ratio Lower Upper 29 50 100 52 28.9 12.8 52.8

Raw 50 45 50 Abundance 41 65 4.007 37 85 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 1000 Abundance Scan 114 (4.007 min): 05251624.D\data.ms (-65) (-) 32 50

Sub 500 50 65

85 0 0 m/z--> 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 Time--> 3.95 4.00 4.05

Abundance Scan 158 (4.248 min): 04211627.D\data.ms (-148) (-) #6 62 Vinyl Chloride Concen: 0.50 ng RT: 4.29 min Scan# 165 Ref 50 Delta R.T. 0.022 min Lab File: 05251624.D Acq: 25 May 2016 16:18 35 48 0 m/z--> 20 40 60 80 100 120 140 160 180 200 Tgt Ion: 62 Resp: 10505 Abundance Scan 165 (4.287 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 62 100 29 64 30.5 12.1 52.1 62 Raw 50 Abundance 6000 4.287 207 0 m/z--> 20 40 60 80 100 120 140 160 180 200 Abundance Scan 165 (4.287 min): 05251624.D\data.ms (-115) (-) 4000 43 62 Sub 29 50 2000

207 0 0 m/z--> 20 40 60 80 100 120 140 160 180 200 Time--> 4.20 4.25 4.30 4.35

59 of 156 05251624.D R9042116.M Thu May 26 11:52:08 2016 Page 3 Abundance Scan 337 (5.197 min): 04211627.D\data.ms (-318) (-) #10 45 Ethanol Concen: 10.50 ng RT: 5.15 min Scan# 328 Ref 50 Delta R.T. -0.103 min Lab File: 05251624.D 43 Acq: 25 May 2016 16:18 33 41 47 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Tgt Ion: 45 Resp: 100712 Abundance Scan 328 (5.151 min): 05251624.D\data.ms Ion Ratio Lower Upper 45 45 100 46 35.7 16.8 56.8

Raw 50 Abundance 43 5.151 41 47 30000 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Abundance Scan 328 (5.151 min): 05251624.D\data.ms (-280) (-) 45 20000

Sub 50 10000

43 41 47 0 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Time--> 5.00 5.20 5.40

Abundance Scan 423 (5.640 min): 04211627.D\data.ms (-408) (-) #13 43 Acetone Concen: 13.38 ng m RT: 5.61 min Scan# 417 Ref 50 Delta R.T. -0.067 min 58 Lab File: 05251624.D Acq: 25 May 2016 16:18 36 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Tgt Ion: 58 Resp: 150516 Abundance Scan 417 (5.609 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 58 100 43 3194.8 255.0 315.0#

Raw 50 58 Abundance 2000000

36 67 85 117 0 m/z--> 30 40 50 60 70 80 90 100 110 120 1500000 Abundance Scan 417 (5.609 min): 05251624.D\data.ms (-382) (-) 43 1000000 Sub 50 58 500000

5.609 36 67 85 117 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Time--> 5.55 5.60 5.65

60 of 156 05251624.D R9042116.M Thu May 26 11:52:09 2016 Page 4 Abundance Scan 453 (5.795 min): 04211627.D\data.ms (-440) (-) #14 101 Trichlorofluoromethane Concen: 0.46 ng RT: 5.81 min Scan# 456 Ref 50 Delta R.T. 0.005 min Lab File: 05251624.D Acq: 25 May 2016 16:18 4735 66 74 82 117 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion:101 Resp: 10726 Abundance Scan 456 (5.811 min): 05251624.D\data.ms Ion Ratio Lower Upper 101 101 100 103 63.9 44.5 84.5

Raw 50 43 Abundance 5000 5.811 57 66 35 82 119 0 4000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 456 (5.811 min): 05251624.D\data.ms (-407) (-) 101 3000

Sub 2000 50 43 1000 57 66 35 82 119 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 5.75 5.80 5.85

Abundance Scan 488 (5.976 min): 04211627.D\data.ms (-469) (-) #15 45 2-Propanol (Isopropanol) Concen: 0.45 ng RT: 5.95 min Scan# 484 Ref 50 Delta R.T. -0.067 min Lab File: 05251624.D Acq: 25 May 2016 16:18 33 59 207 0 m/z--> 40 60 80 100 120 140 160 180 200 Tgt Ion: 45 Resp: 16343 Abundance Scan 484 (5.955 min): 05251624.D\data.ms Ion Ratio Lower Upper 45 45 100 43 0.0 0.0 37.0

Raw 50 Abundance 5.955 81 59 5000 0 m/z--> 40 60 80 100 120 140 160 180 200 4000 Abundance Scan 484 (5.955 min): 05251624.D\data.ms (-449) (-) 45 3000

Sub 2000 50 1000 81 59 0 0 m/z--> 40 60 80 100 120 140 160 180 200 Time--> 5.90 6.00

61 of 156 05251624.D R9042116.M Thu May 26 11:52:09 2016 Page 5 Abundance Scan 586 (6.481 min): 04211627.D\data.ms (-574) (-) #17 61 1,1-Dichloroethene Concen: 7.39 ng 96 RT: 6.50 min Scan# 589 Ref 50 Delta R.T. -0.000 min Lab File: 05251624.D Acq: 25 May 2016 16:18 35 47 70 82 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 96 Resp: 95864 Abundance Scan 589 (6.496 min): 05251624.D\data.ms Ion Ratio Lower Upper 61 96 100 61 155.1 136.0 176.0 96 Raw 50 Abundance

60000 35 47 84 0 m/z--> 30 40 50 60 70 80 90 100 6.496 Abundance Scan 589 (6.496 min): 05251624.D\data.ms (-541) (-) 40000 61 96 Sub 50 20000

35 47 82 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 6.40 6.45 6.50 6.55 6.60

Abundance Scan 619 (6.651 min): 04211627.D\data.ms (-603) (-) #19 49 84 Methylene Chloride Concen: 0.27 ng RT: 6.62 min Scan# 613 Ref 50 Delta R.T. -0.052 min Lab File: 05251624.D 59 Acq: 25 May 2016 16:18 4135 88 38 5345 7073 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Tgt Ion: 84 Resp: 4374 Abundance Scan 613 (6.620 min): 05251624.D\data.ms Ion Ratio Lower Upper 5949 84 100 84 49 121.0 99.2 149.2

Raw 50 43 Abundance 2500 35 39 88 6.620 0 2000 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Abundance Scan 613 (6.620 min): 05251624.D\data.ms (-575) (-) 1500 5949 84 1000 Sub 50 43 500 35 39 88 0 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Time--> 6.55 6.60 6.65

62 of 156 05251624.D R9042116.M Thu May 26 11:52:09 2016 Page 6 Abundance Scan 675 (6.940 min): 04211627.D\data.ms (-659) (-) #21 101 Trichlorotrifluoroethane 151 Concen: 0.13 ng RT: 6.96 min Scan# 678 Ref 50 85 Delta R.T. -0.000 min Lab File: 05251624.D 66 Acq: 25 May 2016 16:18 47 116 35 132 171 0 m/z--> 40 60 80 100 120 140 160 Tgt Ion:151 Resp: 1411 Abundance Scan 678 (6.955 min): 05251624.D\data.ms Ion Ratio Lower Upper 101 151 151 100 101 145.8 106.1 146.1

Raw 50 44 85 Abundance 800 0 6.955 m/z--> 40 60 80 100 120 140 160 600 Abundance Scan 678 (6.955 min): 05251624.D\data.ms (-630) (-) 101 151 400 Sub 50 200 85 44 0 0 m/z--> 40 60 80 100 120 140 160 Time--> 6.90 6.95 7.00

Abundance Scan 815 (7.662 min): 04211627.D\data.ms (-800) (-) #23 61 trans-1,2-Dichloroethene 96 Concen: 0.62 ng RT: 7.65 min Scan# 813 Ref 50 Delta R.T. -0.026 min Lab File: 05251624.D Acq: 25 May 2016 16:18 35 47 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 61 Resp: 11782 Abundance Scan 813 (7.651 min): 05251624.D\data.ms Ion Ratio Lower Upper 61 61 100 96 69.6 50.6 90.6 96 Raw 50 Abundance 5000 7.651 40 47 0 4000 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 813 (7.651 min): 05251624.D\data.ms (-770) (-) 61 3000

96 2000 Sub 50 1000

47 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 7.55 7.60 7.65 7.70

63 of 156 05251624.D R9042116.M Thu May 26 11:52:10 2016 Page 7 Abundance Scan 857 (7.878 min): 04211627.D\data.ms (-837) (-) #24 63 1,1-Dichloroethane Concen: 1.62 ng RT: 7.86 min Scan# 853 Ref 50 Delta R.T. -0.041 min Lab File: 05251624.D 83 Acq: 25 May 2016 16:18 35 47 70 98 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 63 Resp: 41960 Abundance Scan 853 (7.858 min): 05251624.D\data.ms Ion Ratio Lower Upper 63 63 100 65 32.9 12.3 52.3

Raw 50 Abundance 7.858 83 35 47 75 98 15000 0 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 853 (7.858 min): 05251624.D\data.ms (-813) (-) 63 10000

Sub 50 5000

83 35 4475 100 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 7.80 7.85 7.90

Abundance Scan 937 (8.291 min): 04211627.D\data.ms (-925) (-) #27 43 2-Butanone (MEK) Concen: 1.03 ng RT: 8.30 min Scan# 938 Ref 50 Delta R.T. -0.026 min 72 Lab File: 05251624.D Acq: 25 May 2016 16:18 57 53 0 m/z--> -5 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 Tgt Ion: 72 Resp: 9177 Abundance Scan 938 (8.296 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 72 100 43 374.9 362.0 402.0

Raw 50 Abundance 72 57 39 51 0 m/z--> -5 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 10000 Abundance Scan 938 (8.296 min): 05251624.D\data.ms (-895) (-)

Sub 5000 50 8.296

0 0 m/z--> -5 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 Time--> 8.20 8.25 8.30 8.35 8.40

64 of 156 05251624.D R9042116.M Thu May 26 11:52:10 2016 Page 8 Abundance Scan 1026 (8.750 min): 04211627.D\data.ms (-1013) (-) #28 61 cis-1,2-Dichloroethene 96 Concen: 11.17 ng RT: 8.73 min Scan# 1022 Ref 50 Delta R.T. -0.041 min Lab File: 05251624.D Acq: 25 May 2016 16:18 35 47 70 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 61 Resp: 208820 Abundance Scan 1022 (8.729 min): 05251624.D\data.ms Ion Ratio Lower Upper 61 61 100 96 96 78.6 58.7 98.7

Raw 50 Abundance 8.729 80000 35 47 70 0 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 1022 (8.729 min): 05251624.D\data.ms (-982) (-) 60000 61 96 40000 Sub 50 20000

35 47 70 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 8.60 8.70 8.80 8.90

Abundance Scan 1072 (8.987 min): 04211627.D\data.ms (-1058) (-) #31 43 n-Hexane Concen: 55.68 ng RT: 9.00 min Scan# 1074 Ref 50 Delta R.T. -0.000 min 57 Lab File: 05251624.D Acq: 25 May 2016 16:18 70 87 78 101 120 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 57 Resp: 1364580 Abundance Scan 1074 (8.997 min): 05251624.D\data.ms Ion Ratio Lower Upper 57 57 100 56 51.4 40.9 61.3 41 86 14.4 11.4 17.2 Raw 50 Abundance 600000 8.997 86 71 49 128 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1074 (8.997 min): 05251624.D\data.ms (-1026) (-) 400000 57 41 Sub 200000 50

86 71 50 130 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 8.90 9.00 9.10 9.20

65 of 156 05251624.D R9042116.M Thu May 26 11:52:10 2016 Page 9 Abundance Scan 1086 (9.059 min): 04211627.D\data.ms (-1071) (-) #32 83 Chloroform Concen: 3.91 ng RT: 9.04 min Scan# 1082 Ref 50 Delta R.T. -0.052 min Lab File: 05251624.D 47 Acq: 25 May 2016 16:18 35 58 119 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 83 Resp: 91227 Abundance Scan 1082 (9.039 min): 05251624.D\data.ms Ion Ratio Lower Upper 83 83 100 85 70.4 45.1 85.1

Raw 50 57 Abundance 41 40000 9.039 48 71 117 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 30000 Abundance Scan 1082 (9.039 min): 05251624.D\data.ms (-1044) (-) 83 20000 Sub 50 57 10000 41 48 71 119 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 9.00 9.10

Abundance Scan 1160 (9.441 min): 04211627.D\data.ms (-1149) (-) #34 42 Tetrahydrofuran (THF) Concen: 0.95 ng RT: 9.46 min Scan# 1163 Ref 50 72 Delta R.T. 0.005 min Lab File: 05251624.D 39 Acq: 25 May 2016 16:18 3545 49 52 55 68 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Tgt Ion: 72 Resp: 9271 Abundance Scan 1163 (9.456 min): 05251624.D\data.ms Ion Ratio Lower Upper 42 72 100 71 94.3 76.2 116.2 42 245.2 206.6 246.6 Raw 50 72 Abundance 39 45 8000 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Abundance Scan 1163 (9.456 min): 05251624.D\data.ms (-1114) (-) 6000 42 4000 9.456 Sub 50 72 2000 39 45 0 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 Time--> 9.40 9.45 9.50 9.55

66 of 156 05251624.D R9042116.M Thu May 26 11:52:11 2016 Page 10 Abundance Scan 1281 (10.065 min): 04211627.D\data.ms (-1268) (-) #38 97 1,1,1-Trichloroethane Concen: 0.65 ng RT: 10.06 min Scan# 1280 Ref 50 61 Delta R.T. -0.021 min Lab File: 05251624.D 117 Acq: 25 May 2016 16:18 35 47 70 82 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 97 Resp: 13138 Abundance Scan 1280 (10.060 min): 05251624.D\data.ms Ion Ratio Lower Upper 97 97 100 99 65.8 44.4 84.4 61 41.0 20.1 60.1 Raw 50 61 Abundance 43 6000 10.060 85 117 35 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1280 (10.060 min): 05251624.D\data.ms (-1236) (-) 4000 97

Sub 2000 50 61 119 35 47 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 10.00 10.05 10.10

Abundance Scan 1370 (10.524 min): 04211627.D\data.ms (-1356) (-) #41 78 Benzene Concen: 3.71 ng RT: 10.52 min Scan# 1369 Ref 50 Delta R.T. -0.021 min Lab File: 05251624.D 52 Acq: 25 May 2016 16:18 37 49 63 74 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Tgt Ion: 78 Resp: 229911 Abundance Scan 1369 (10.519 min): 05251624.D\data.ms Ion Ratio Lower Upper 78 78 100 77 23.4 3.9 43.9

Raw 50 Abundance 100000 10.519 51 39 36 43 48 56 60 63 74 0 80000 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Abundance Scan 1369 (10.519 min): 05251624.D\data.ms (-1325) (-) 78 60000

40000 Sub 50 20000 52 39 36 43 49 56 60 63 74 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Time--> 10.40 10.50 10.60

67 of 156 05251624.D R9042116.M Thu May 26 11:52:11 2016 Page 11 Abundance Scan 1424 (10.802 min): 04211627.D\data.ms (-1410) (-) #43 56 84 Cyclohexane Concen: 36.65 ng RT: 10.81 min Scan# 1425 41 Ref 50 Delta R.T. -0.005 min 69 Lab File: 05251624.D Acq: 25 May 2016 16:18 38 44 5053 6063 66 74 79 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Tgt Ion: 84 Resp: 806262 Abundance Scan 1425 (10.807 min): 05251624.D\data.ms Ion Ratio Lower Upper 56 84 100 84 69 37.0 17.1 57.1 56 119.0 100.6 140.6 41 Raw 50 69 Abundance 400000 10.807 3844 5053 6366 73 77 81 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 300000 Abundance Scan 1425 (10.807 min): 05251624.D\data.ms (-1378) (-) 56 84 200000

Sub 41 50 69 100000

38 44 5053 6366 73 7780 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Time--> 10.70 10.80 10.90

Abundance Scan 1575 (11.581 min): 04211627.D\data.ms (-1558) (-) #47 95 130 Trichloroethene Concen: 187.20 ng RT: 11.58 min Scan# 1574 Ref 50 60 Delta R.T. -0.016 min Lab File: 05251624.D Acq: 25 May 2016 16:18 35 47 68 82 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Tgt Ion:130 Resp: 2779295 Abundance Scan 1574 (11.576 min): 05251624.D\data.ms Ion Ratio Lower Upper 95 130 130 100 132 95.5 75.8 115.8

Raw 50 60 Abundance 11.576 35 47 70 82 0 1000000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Abundance Scan 1574 (11.576 min): 05251624.D\data.ms (-1529) (-) 95 130

Sub 500000 50 60

35 47 70 82 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Time--> 11.40 11.60 11.80

68 of 156 05251624.D R9042116.M Thu May 26 11:52:11 2016 Page 12 Abundance Scan 1637 (11.900 min): 04211627.D\data.ms (-1626) (-) #51 43 n-Heptane Concen: 14.13 ng 71 RT: 11.90 min Scan# 1637 Ref 50 Delta R.T. -0.011 min Lab File: 05251624.D 100 Acq: 25 May 2016 16:18 281 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Tgt Ion: 71 Resp: 205364 Abundance Scan 1637 (11.901 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 71 100 57 92.4 72.3 112.3 71 100 26.3 6.1 46.1 Raw 50 Abundance 100000 11.901 100

0 80000 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Abundance Scan 1637 (11.901 min): 05251624.D\data.ms (-1591) (-) 43 60000

Sub 71 40000 50 20000 100 0 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Time--> 11.80 11.90 12.00

Abundance Scan 1932 (13.422 min): 04211627.D\data.ms (-1919) (-) #58 91 Toluene Concen: 0.48 ng RT: 13.42 min Scan# 1931 Ref 50 Delta R.T. -0.011 min Lab File: 05251624.D Acq: 25 May 2016 16:18 39 65 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Tgt Ion: 91 Resp: 29434 Abundance Scan 1931 (13.417 min): 05251624.D\data.ms Ion Ratio Lower Upper 91 91 100 92 58.0 38.5 78.5 43 Raw 50 71 Abundance 13.417 281 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 10000 Abundance Scan 1931 (13.417 min): 05251624.D\data.ms (-1885) (-) 91

Sub 43 5000 50 71

281 0 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Time--> 13.35 13.40 13.45 13.50

69 of 156 05251624.D R9042116.M Thu May 26 11:52:12 2016 Page 13 Abundance Scan 2130 (14.443 min): 04211627.D\data.ms (-2118) (-) #63 43 n-Octane Concen: 2.63 ng RT: 14.44 min Scan# 2129 Ref 50 57 85 Delta R.T. -0.011 min 71 Lab File: 05251624.D Acq: 25 May 2016 16:18 98 114 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 Tgt Ion: 57 Resp: 35570 Abundance Scan 2129 (14.438 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 57 100 85 107.5 88.2 132.2 71 69.4 55.8 83.8 Raw 50 57 85 Abundance 71 14.438 114 166 0 15000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 Abundance Scan 2129 (14.438 min): 05251624.D\data.ms (-2083) (-) 43 10000 Sub 50 85 57 5000 71

114 166 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 Time--> 14.35 14.40 14.45 14.50

Abundance Scan 2155 (14.572 min): 04211627.D\data.ms (-2144) (-) #64 166 Tetrachloroethene 129 Concen: 47.84 ng RT: 14.57 min Scan# 2155 Ref 50 94 Delta R.T. -0.005 min Lab File: 05251624.D 47 59 Acq: 25 May 2016 16:18 35 82 70 117 0 m/z--> 40 60 80 100 120 140 160 Tgt Ion:166 Resp: 764660 Abundance Scan 2155 (14.572 min): 05251624.D\data.ms Ion Ratio Lower Upper 166 166 100 129 164 78.2 58.4 98.4

Raw 50 94 Abundance 14.572 47 59 35 84 69 117 0 300000 m/z--> 40 60 80 100 120 140 160 Abundance Scan 2155 (14.572 min): 05251624.D\data.ms (-2108) (-) 166 200000 129 Sub 50 94 100000

47 59 35 82 69 117 0 0 m/z--> 40 60 80 100 120 140 160 Time--> 14.50 14.60 14.70

70 of 156 05251624.D R9042116.M Thu May 26 11:52:12 2016 Page 14 Abundance Scan 2369 (15.675 min): 04211627.D\data.ms (-2357) (-) #66 91 Ethylbenzene Concen: 0.32 ng RT: 15.68 min Scan# 2369 Ref 50 Delta R.T. -0.005 min 106 Lab File: 05251624.D Acq: 25 May 2016 16:18 51 65 77 39 84 98 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 91 Resp: 20703 Abundance Scan 2369 (15.675 min): 05251624.D\data.ms Ion Ratio Lower Upper 91 91 100 106 30.6 11.9 51.9 55 Raw 50 69 41 84 106 Abundance 10000 15.675 77 98 126 0 8000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 2369 (15.675 min): 05251624.D\data.ms (-2322) (-) 91 6000

Sub 4000 50 106 2000

50 63 78 98 125 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 15.60 15.65 15.70 15.75

Abundance Scan 2407 (15.871 min): 04211627.D\data.ms (-2393) (-) #67 91 m- & p-Xylenes Concen: 0.38 ng RT: 15.86 min Scan# 2404 106 Ref 50 Delta R.T. -0.026 min Lab File: 05251624.D 77 Acq: 25 May 2016 16:18 39 51 65 84 98 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 91 Resp: 19892 Abundance Scan 2404 (15.856 min): 05251624.D\data.ms Ion Ratio Lower Upper 91 91 100 43 57 106 48.8 29.4 69.4

Raw 50 106 Abundance 70 84 6000 15.856 77 98 50 126 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 2404 (15.856 min): 05251624.D\data.ms (-2361) (-) 4000 91

57 Sub 43 50 106 2000

65 77 50 98 126 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 15.80 15.90

71 of 156 05251624.D R9042116.M Thu May 26 11:52:12 2016 Page 15 Abundance Scan 2503 (16.366 min): 04211627.D\data.ms (-2493) (-) #70 91 o-Xylene Concen: 0.13 ng RT: 16.37 min Scan# 2503 Ref 50 106 Delta R.T. -0.011 min Lab File: 05251624.D 77 Acq: 25 May 2016 16:18 39 51 65 98 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 91 Resp: 6920 Abundance Scan 2503 (16.366 min): 05251624.D\data.ms Ion Ratio Lower Upper 69 111 91 100 55 106 41.3 28.3 68.3 Raw 50 41 91 Abundance 126 84 16.366 77 98 0 3000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 2503 (16.366 min): 05251624.D\data.ms (-2457) (-) 69 111 2000 55 Sub 50 91 1000 41 126

77 84 98 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 16.30 16.35 16.40

Abundance Scan 2551 (16.614 min): 04211627.D\data.ms (-2534) (-) #71 43 57 n-Nonane Concen: 0.20 ng RT: 16.61 min Scan# 2551 Ref 50 Delta R.T. -0.005 min 85 71 Lab File: 05251624.D Acq: 25 May 2016 16:18 99 36 50 112 128 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 43 Resp: 6306 Abundance Scan 2551 (16.614 min): 05251624.D\data.ms Ion Ratio Lower Upper 43 57 43 100 69 57 107.2 72.5 112.5 85 48.8 14.1 54.1 Raw 50 83 111 Abundance 125 97

0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 10000 Abundance Scan 2551 (16.614 min): 05251624.D\data.ms (-2504) (-) 5743

Sub 5000 16.614 50 85 125 71 99 110 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 16.60 16.65

72 of 156 05251624.D R9042116.M Thu May 26 11:52:13 2016 Page 16 Abundance Scan 2624 (16.990 min): 04211627.D\data.ms (-2607) (-) #74 105 Cumene Concen: 0.18 ng RT: 16.98 min Scan# 2623 Ref 50 Delta R.T. -0.011 min 120 Lab File: 05251624.D 77 Acq: 25 May 2016 16:18 51 91 39 63 7098 113 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Tgt Ion:105 Resp: 12031 Abundance Scan 2623 (16.985 min): 05251624.D\data.ms Ion Ratio Lower Upper 105 100 57 105 43 97 120 25.6 6.8 46.8

Raw 50 69 Abundance 85 120 16.985 77 50 6000 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Abundance Scan 2623 (16.985 min): 05251624.D\data.ms (-2577) (-) 57 105 4000

Sub 43 97 50 2000 120 77 85 50 65 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Time--> 16.90 16.95 17.00 17.05

Abundance Scan 2727 (17.521 min): 04211627.D\data.ms (-2713) (-) #76 91 n-Propylbenzene Concen: 0.14 ng RT: 17.52 min Scan# 2727 Ref 50 Delta R.T. -0.005 min 120 Lab File: 05251624.D 65 Acq: 25 May 2016 16:18 39 5178 105 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Tgt Ion: 91 Resp: 11517 Abundance Scan 2727 (17.521 min): 05251624.D\data.ms Ion Ratio Lower Upper 91 91 100 120 18.5 3.1 43.1 55 65 27.3 0.0 29.5 Raw 69 50 41 81 Abundance 120 6000 17.521 110 138 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Abundance Scan 2727 (17.521 min): 05251624.D\data.ms (-2680) (-) 4000 91

Sub 2000 50 120 6550 78 105 138 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Time--> 17.45 17.50 17.55 17.60

73 of 156 05251624.D R9042116.M Thu May 26 11:52:13 2016 Page 17 Abundance Scan 2856 (18.186 min): 04211627.D\data.ms (-2843) (-) #82 105 1,2,4-Trimethylbenzene Concen: 0.24 ng RT: 18.19 min Scan# 2856 Ref 50 Delta R.T. -0.011 min Lab File: 05251624.D 77 134 41 Acq: 25 May 2016 16:18 58 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Tgt Ion:105 Resp: 12408 Abundance Scan 2856 (18.186 min): 05251624.D\data.ms Ion Ratio Lower Upper 55 105 100 97 120 45.9 35.2 75.2

Raw 50 Abundance 18.186 120 140 281 77 38 191 6000 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Abundance Scan 2856 (18.186 min): 05251624.D\data.ms (-2810) (-) 55 97 4000

Sub 50 2000

120 140 281 3877 191 0 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Time--> 18.10 18.15 18.20 18.25

74 of 156 05251624.D R9042116.M Thu May 26 11:52:13 2016 Page 18 Quantitation Report (Qedit)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 25 17:03:02 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance Ion 58.00 (57.70 to 58.70): 05251624.D\data.ms 3000000 Ion 43.00 (42.70 to 43.70): 05251624.D\data.ms

2500000

| 2000000

| 1500000 | 1000000 |

500000 |

5.666 | 2d 1| | 0

Time--> 4.70 4.80 4.90 5.00 5.10 5.20 5.30 5.40 5.50 5.60 5.70 5.80 5.90 6.00 6.10 6.20 6.30 6.40 6.50 6.60 6.70 Abundance Scan 428 (5.666 min): 05251624.D\data.ms 2000000 424341 57

1000000 39 56 55 72 3738 40 4445495051525354 5859 60 62 63 666765 69 71 73 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 72 74 76 78 80 82 Abundance Scan 423 (5.640 min): 04211627.D\data.ms (-408) (-) 43

5000 58

42 3738394041 45 5253 55 56 59 60 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 72 74 76 78 80 82

TIC: 05251624.D\data.ms

(13) Acetone (T)

5.666min (-0.011) 15.35ng

response 172642

Ion Exp% Act%

58.00 100 100

43.00 285.00 2785.39#

0.00 0.00 0.00

0.00 0.00 0.00

75 of 156 R9042116.M Thu May 26 11:17:41 2016 Page: 1 Quantitation Report (Qedit)

Data File : I:\MS09\Data\2016_05\25\05251624.D Vial: 6 Acq On : 25 May 2016 16:18 Operator: WA Sample : P1602483-002 (400mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 25 17:03:02 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance Ion 58.00 (57.70 to 58.70): 05251624.D\data.ms 3000000 Ion 43.00 (42.70 to 43.70): 05251624.D\data.ms

2500000

| 2000000

| 1500000 | 1000000 |

500000 |

| 5.6092d 1| | 0

Time--> 4.60 4.70 4.80 4.90 5.00 5.10 5.20 5.30 5.40 5.50 5.60 5.70 5.80 5.90 6.00 6.10 6.20 6.30 6.40 6.50 6.60 Abundance Scan 417 (5.609 min): 05251624.D\data.ms 43 150000

100000 58 50000 3639 53 67 85 117 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 Abundance Scan 423 (5.640 min): 04211627.D\data.ms (-408) (-) 43

5000 58

36 39 53 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125

TIC: 05251624.D\data.ms

(13) Acetone (T)

5.609min (-0.067) 13.38ng m

response 150516

Ion Exp% Act%

58.00 100 100

43.00 285.00 3194.84#

0.00 0.00 0.00

0.00 0.00 0.00

76 of 156 R9042116.M Thu May 26 11:18:04 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251629.D Vial: 6 Acq On : 25 May 2016 19:07 Operator: WA Sample : P1602483-002dil (40mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:25:33 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 112265 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 586691 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 247730 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 174057 11.889 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 95.12% 57) Toluene-d8 (SS2) 13.31 98 582156 12.486 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 73) Bromofluorobenzene (SS3) 16.84 174 220748 14.333 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 114.64%

Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. d 3) Dichlorodifluoromethan... 3.80 85 1668 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 4.27 62 847 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. d 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.16 45 10299 0.948 ng 91 11) Acetonitrile 0.00 41 0 N.D. 12) Acrolein 0.00 56 0 N.D. d 13) Acetone 0.00 58 0 N.D. d 14) Trichlorofluoromethane 5.79 101 973 N.D. 15) 2-Propanol (Isopropanol) 5.99 45 1900 N.D. 16) Acrylonitrile 0.00 53 0 N.D. d 17) 1,1-Dichloroethene 6.48 96 9017 0.614 ng 97 18) 2-Methyl-2-Propanol (t... 6.66 59 1692 N.D. 19) Methylene Chloride 6.63 84 2253 0.123 ng 93 20) 3-Chloro-1-propene (Al... 6.69 41 433 N.D. 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 6.91 76 415 N.D. 23) trans-1,2-Dichloroethene 7.65 61 622 N.D. 24) 1,1-Dichloroethane 7.85 63 4132 0.141 ng 96 25) Methyl tert-Butyl Ether 0.00 73 0 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 0.00 72 0 N.D. d 28) cis-1,2-Dichloroethene 8.73 61 18724 0.884 ng 97 29) Diisopropyl Ether 0.00 87 0 N.D. d 30) Ethyl Acetate 0.00 61 0 N.D. 31) n-Hexane 8.99 57 133382 4.805 ng 99 32) Chloroform 9.03 83 8713 0.330 ng 91 34) Tetrahydrofuran (THF) 9.48 72 953 N.D. 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. 38) 1,1,1-Trichloroethane 10.05 97 1400 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 0.00 56 0 N.D. d 41) Benzene 10.52 78 22654 0.325 ng 99 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 10.80 84 77146 3.117 ng 98 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. d 47) Trichloroethene 11.57 130 259863 15.561 ng 100 48) 1,4-Dioxane 11.59 88 644 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. d 50) Methyl Methacrylate 0.00 100 0 N.D. d 77 of 156 R9042116.M Thu May 26 11:26:06 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251629.D Vial: 6 Acq On : 25 May 2016 19:07 Operator: WA Sample : P1602483-002dil (40mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:25:33 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 11.90 71 20010 1.224 ng 99 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 13.03 97 679 N.D. 58) Toluene 13.41 91 4208 N.D. 59) 2-Hexanone 0.00 43 0 N.D. d 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 14.31 43 499 N.D. 63) n-Octane 14.44 57 3579 0.243 ng 94 64) Tetrachloroethene 14.57 166 71207 4.094 ng 99 65) Chlorobenzene 15.30 112 3343 N.D. 66) Ethylbenzene 15.68 91 2755 N.D. 67) m- & p-Xylenes 15.86 91 3256 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 16.37 91 1237 N.D. 71) n-Nonane 16.61 43 1178 N.D. 72) 1,1,2,2-Tetrachloroethane 16.29 83 1562 N.D. 74) Cumene 17.00 105 1514 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 17.52 91 1832 N.D. 77) 3-Ethyltoluene 17.63 105 1597 N.D. 78) 4-Ethyltoluene 17.68 105 1351 N.D. 79) 1,3,5-Trimethylbenzene 17.76 105 985 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. d 81) 2-Ethyltoluene 17.95 105 908 N.D. 82) 1,2,4-Trimethylbenzene 18.19 105 1799 N.D. 83) n-Decane 0.00 57 0 N.D. d 84) Benzyl Chloride 18.42 91 453 N.D. 85) 1,3-Dichlorobenzene 18.42 146 458 N.D. 86) 1,4-Dichlorobenzene 18.42 146 458 N.D. 87) sec-Butylbenzene 18.48 105 1065 N.D. 88) 4-Isopropyltoluene (p-... 18.64 119 724 N.D. 89) 1,2,3-Trimethylbenzene 18.64 105 736 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 18.78 68 496 N.D. 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. d 94) 1,2,4-Trichlorobenzene 20.59 180 599 N.D. 95) Naphthalene 20.71 128 4629 N.D. 96) n-Dodecane 0.00 57 0 N.D. d 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 16.05 55 1495 N.D. 99) tert-Butylbenzene 18.19 119 612 N.D. 100) n-Butylbenzene 19.09 91 879 N.D. ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

78 of 156 R9042116.M Thu May 26 11:26:06 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251629.D Vial: 6 Acq On : 25 May 2016 19:07 Operator: WA Sample : P1602483-002dil (40mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:25:33 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251629.D\data.ms

9500000

9000000

8500000

8000000

7500000

7000000

6500000

6000000

5500000

5000000

4500000

4000000

3500000

3000000

2500000

2000000

1500000 Toluene-d8 (SS2),S Trichloroethene,T Chlorobenzene-d5 (IS3),IR Bromofluorobenzene (SS3),S 1000000 1,4-Difluorobenzene (IS2),IR n-Hexane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S Tetrachloroethene,T Cyclohexane,T n-Heptane,T cis-1,2-Dichloroethene,T Benzene,T 1,1-Dichloroethene,T

500000 n-Octane,T Chloroform,T Ethanol,T Methylene Chloride,T 1,1-Dichloroethane,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0079 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:26:06 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251629.D Vial: 6 Acq On : 25 May 2016 19:07 Operator: WA Sample : P1602483-002dil (40mL) Inst : MS09 Misc : S29-04191601

Quant Time: May 26 11:25:33 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 112265 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 586691 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 247730 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 174057 11.889 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 95.12% 57) Toluene-d8 (SS2) 13.31 98 582156 12.486 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 73) Bromofluorobenzene (SS3) 16.84 174 220748 14.333 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 114.64%

Target Compounds Qvalue 10) Ethanol 5.16 45 10299 0.948 ng 91 17) 1,1-Dichloroethene 6.48 96 9017 0.614 ng 97 19) Methylene Chloride 6.63 84 2253 0.123 ng 93 24) 1,1-Dichloroethane 7.85 63 4132 0.141 ng 96 28) cis-1,2-Dichloroethene 8.73 61 18724 0.884 ng 97 31) n-Hexane 8.99 57 133382 4.805 ng 99 32) Chloroform 9.03 83 8713 0.330 ng 91 41) Benzene 10.52 78 22654 0.325 ng 99 43) Cyclohexane 10.80 84 77146 3.117 ng 98 47) Trichloroethene 11.57 130 259863 15.561 ng 100 51) n-Heptane 11.90 71 20010 1.224 ng 99 63) n-Octane 14.44 57 3579 0.243 ng 94 64) Tetrachloroethene 14.57 166 71207 4.094 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

80 of 156 R9042116.M Thu May 26 11:25:48 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251629.D Vial: 6 Acq On : 25 May 2016 19:07 Operator: WA Sample : P1602483-002dil (40mL) Inst : MS09 Misc : S29-04191601 Quant Time: May 26 11:25:33 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251629.D\data.ms

9500000

9000000

8500000

8000000

7500000

7000000

6500000

6000000

5500000

5000000

4500000

4000000

3500000

3000000

2500000

2000000

1500000 Toluene-d8 (SS2),S Trichloroethene,T Chlorobenzene-d5 (IS3),IR Bromofluorobenzene (SS3),S 1000000 1,4-Difluorobenzene (IS2),IR n-Hexane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S Tetrachloroethene,T Cyclohexane,T n-Heptane,T cis-1,2-Dichloroethene,T Benzene,T 1,1-Dichloroethene,T

500000 n-Octane,T Chloroform,T Ethanol,T Methylene Chloride,T 1,1-Dichloroethane,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0081 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 11:25:49 2016 Page: 2 Abundance Scan 337 (5.197 min): 04211627.D\data.ms (-318) (-) #10 45 Ethanol Concen: 0.95 ng RT: 5.16 min Scan# 330 Ref 50 Delta R.T. -0.093 min Lab File: 05251629.D 43 Acq: 25 May 2016 19:07 33 41 47 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Tgt Ion: 45 Resp: 10299 Abundance Scan 330 (5.161 min): 05251629.D\data.ms Ion Ratio Lower Upper 45 45 100 46 31.5 16.8 56.8

Raw 50 Abundance 43 5.161 40 2000 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Abundance Scan 330 (5.161 min): 05251629.D\data.ms (-280) (-) 1500 45 1000 Sub 50 500 43 40 0 0 m/z--> 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 Time--> 5.10 5.20 5.30

Abundance Scan 586 (6.481 min): 04211627.D\data.ms (-574) (-) #17 61 1,1-Dichloroethene Concen: 0.61 ng 96 RT: 6.48 min Scan# 586 Ref 50 Delta R.T. -0.016 min Lab File: 05251629.D Acq: 25 May 2016 19:07 35 47 70 82 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 96 Resp: 9017 Abundance Scan 586 (6.481 min): 05251629.D\data.ms Ion Ratio Lower Upper 61 96 100 61 152.0 136.0 176.0 96

Raw 50 Abundance 6000 35 47 0 m/z--> 30 40 50 60 70 80 90 100 6.481 Abundance Scan 586 (6.481 min): 05251629.D\data.ms (-541) (-) 4000 61 96 Sub 2000 50

35 47 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 6.40 6.45 6.50 6.55

82 of 156 05251629.D R9042116.M Thu May 26 11:25:50 2016 Page 3 Abundance Scan 619 (6.651 min): 04211627.D\data.ms (-603) (-) #19 49 84 Methylene Chloride Concen: 0.12 ng RT: 6.63 min Scan# 614 Ref 50 Delta R.T. -0.047 min Lab File: 05251629.D 59 Acq: 25 May 2016 19:07 4135 88 38 5345 7073 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Tgt Ion: 84 Resp: 2253 Abundance Scan 614 (6.625 min): 05251629.D\data.ms Ion Ratio Lower Upper 49 84 84 100 49 116.8 99.2 149.2

Raw 50 Abundance 6.625 1000 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 800 Abundance Scan 614 (6.625 min): 05251629.D\data.ms (-575) (-) 49 84 600

Sub 400 50 200

0 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 Time--> 6.55 6.60 6.65 6.70

Abundance Scan 857 (7.878 min): 04211627.D\data.ms (-837) (-) #24 63 1,1-Dichloroethane Concen: 0.14 ng RT: 7.85 min Scan# 852 Ref 50 Delta R.T. -0.047 min Lab File: 05251629.D 83 Acq: 25 May 2016 19:07 35 47 70 98 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 63 Resp: 4132 Abundance Scan 852 (7.853 min): 05251629.D\data.ms Ion Ratio Lower Upper 63 63 100 65 34.5 12.3 52.3

Raw 50 Abundance 7.853 40 83 0 1500 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 852 (7.853 min): 05251629.D\data.ms (-813) (-) 63 1000

Sub 50 500

83 40 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 7.80 7.85 7.90

83 of 156 05251629.D R9042116.M Thu May 26 11:25:50 2016 Page 4 Abundance Scan 1026 (8.750 min): 04211627.D\data.ms (-1013) (-) #28 61 cis-1,2-Dichloroethene 96 Concen: 0.88 ng RT: 8.73 min Scan# 1022 Ref 50 Delta R.T. -0.041 min Lab File: 05251629.D Acq: 25 May 2016 19:07 35 47 70 0 m/z--> 30 40 50 60 70 80 90 100 Tgt Ion: 61 Resp: 18724 Abundance Scan 1022 (8.729 min): 05251629.D\data.ms Ion Ratio Lower Upper 61 61 100 96 96 81.4 58.7 98.7

Raw 50 Abundance 8.729 35 48 0 6000 m/z--> 30 40 50 60 70 80 90 100 Abundance Scan 1022 (8.729 min): 05251629.D\data.ms (-982) (-) 61 96 4000

Sub 50 2000

35 47 0 0 m/z--> 30 40 50 60 70 80 90 100 Time--> 8.70 8.80

Abundance Scan 1072 (8.987 min): 04211627.D\data.ms (-1058) (-) #31 43 n-Hexane Concen: 4.81 ng RT: 8.99 min Scan# 1072 Ref 50 Delta R.T. -0.010 min 57 Lab File: 05251629.D Acq: 25 May 2016 19:07 70 87 78 101 120 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 57 Resp: 133382 Abundance Scan 1072 (8.987 min): 05251629.D\data.ms Ion Ratio Lower Upper 57 57 100 56 50.2 40.9 61.3 41 86 14.3 11.4 17.2 Raw 50 Abundance 8.987 86 60000 71 49 79 95 130 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1072 (8.987 min): 05251629.D\data.ms (-1026) (-) 40000 57 41 Sub 50 20000

86 71 49 79 95 130 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 8.90 9.00 9.10

84 of 156 05251629.D R9042116.M Thu May 26 11:25:50 2016 Page 5 Abundance Scan 1086 (9.059 min): 04211627.D\data.ms (-1071) (-) #32 83 Chloroform Concen: 0.33 ng RT: 9.03 min Scan# 1081 Ref 50 Delta R.T. -0.057 min Lab File: 05251629.D 47 Acq: 25 May 2016 19:07 35 58 119 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Tgt Ion: 83 Resp: 8713 Abundance Scan 1081 (9.034 min): 05251629.D\data.ms Ion Ratio Lower Upper 83 83 100 85 72.5 45.1 85.1

Raw 50 Abundance 47 9.034 57 130 35 93 0 3000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Abundance Scan 1081 (9.034 min): 05251629.D\data.ms (-1044) (-) 83 2000

Sub 50 1000 47 57 35 93 130 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 Time--> 8.95 9.00 9.05 9.10

Abundance Scan 1370 (10.524 min): 04211627.D\data.ms (-1356) (-) #41 78 Benzene Concen: 0.32 ng RT: 10.52 min Scan# 1369 Ref 50 Delta R.T. -0.021 min Lab File: 05251629.D 52 Acq: 25 May 2016 19:07 37 49 63 74 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Tgt Ion: 78 Resp: 22654 Abundance Scan 1369 (10.519 min): 05251629.D\data.ms Ion Ratio Lower Upper 78 78 100 77 24.2 3.9 43.9

Raw 50 Abundance 10000 10.519 39 51 43 56 63 74 0 8000 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Abundance Scan 1369 (10.519 min): 05251629.D\data.ms (-1325) (-) 78 6000

4000 Sub 50 2000 39 51 43 56 63 74 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 Time--> 10.45 10.50 10.55 10.60

85 of 156 05251629.D R9042116.M Thu May 26 11:25:51 2016 Page 6 Abundance Scan 1424 (10.802 min): 04211627.D\data.ms (-1410) (-) #43 56 84 Cyclohexane Concen: 3.12 ng RT: 10.80 min Scan# 1423 41 Ref 50 Delta R.T. -0.016 min 69 Lab File: 05251629.D Acq: 25 May 2016 19:07 38 445053 6063 66 74 79 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Tgt Ion: 84 Resp: 77146 Abundance Scan 1423 (10.797 min): 05251629.D\data.ms Ion Ratio Lower Upper 56 84 84 100 69 36.4 17.1 57.1 56 117.8 100.6 140.6 41 Raw 50 69 Abundance 40000 10.797 38 445053 6366 77 81 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 30000 Abundance Scan 1423 (10.797 min): 05251629.D\data.ms (-1378) (-) 56 84 20000

Sub 41 50 10000 69

38 445053 6366 77 81 0 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 Time--> 10.70 10.80

Abundance Scan 1575 (11.581 min): 04211627.D\data.ms (-1558) (-) #47 95 130 Trichloroethene Concen: 15.56 ng RT: 11.57 min Scan# 1573 Ref 50 60 Delta R.T. -0.021 min Lab File: 05251629.D Acq: 25 May 2016 19:07 35 47 68 82 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Tgt Ion:130 Resp: 259863 Abundance Scan 1573 (11.571 min): 05251629.D\data.ms Ion Ratio Lower Upper 95 130 130 100 132 95.7 75.8 115.8

Raw 50 60 Abundance 11.571 35 47 70 82 0 100000 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Abundance Scan 1573 (11.571 min): 05251629.D\data.ms (-1529) (-) 95 130

50000 Sub 50 60

35 47 70 82 0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 130 140 Time--> 11.50 11.60 11.70

86 of 156 05251629.D R9042116.M Thu May 26 11:25:51 2016 Page 7 Abundance Scan 1637 (11.900 min): 04211627.D\data.ms (-1626) (-) #51 43 n-Heptane Concen: 1.22 ng 71 RT: 11.90 min Scan# 1636 Ref 50 Delta R.T. -0.016 min Lab File: 05251629.D 100 Acq: 25 May 2016 19:07 281 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Tgt Ion: 71 Resp: 20010 Abundance Scan 1636 (11.896 min): 05251629.D\data.ms Ion Ratio Lower Upper 43 71 100 57 91.4 72.3 112.3 71 100 26.0 6.1 46.1 Raw 50 Abundance 100 10000 11.896

0 8000 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Abundance Scan 1636 (11.896 min): 05251629.D\data.ms (-1591) (-) 43 6000

71 Sub 4000 50 2000 100

0 0 m/z--> 40 60 80 100 120 140 160 180 200 220 240 260 280 Time--> 11.85 11.90 11.95

Abundance Scan 2130 (14.443 min): 04211627.D\data.ms (-2118) (-) #63 43 n-Octane Concen: 0.24 ng RT: 14.44 min Scan# 2129 Ref 50 57 85 Delta R.T. -0.010 min 71 Lab File: 05251629.D Acq: 25 May 2016 19:07 5037 78 98 114 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Tgt Ion: 57 Resp: 3579 Abundance Scan 2129 (14.438 min): 05251629.D\data.ms Ion Ratio Lower Upper 43 57 100 85 106.2 88.2 132.2 71 62.8 55.8 83.8 Raw 50 57 85 Abundance 71 2000 14.438 0 1500 m/z--> 30 40 50 60 70 80 90 100 110 120 Abundance Scan 2129 (14.438 min): 05251629.D\data.ms (-2083) (-) 43 1000 Sub 50 85 57 500 71

0 0 m/z--> 30 40 50 60 70 80 90 100 110 120 Time--> 14.40 14.45 14.50

87 of 156 05251629.D R9042116.M Thu May 26 11:25:51 2016 Page 8 Abundance Scan 2155 (14.572 min): 04211627.D\data.ms (-2144) (-) #64 166 Tetrachloroethene 129 Concen: 4.09 ng RT: 14.57 min Scan# 2155 Ref 50 94 Delta R.T. -0.005 min Lab File: 05251629.D 47 59 Acq: 25 May 2016 19:07 35 82 70 117 0 m/z--> 40 60 80 100 120 140 160 Tgt Ion:166 Resp: 71207 Abundance Scan 2155 (14.572 min): 05251629.D\data.ms Ion Ratio Lower Upper 166 166 100 164 77.8 58.4 98.4 129

Raw 50 94 Abundance 47 14.572 59 82 35 70 117 30000 0 m/z--> 40 60 80 100 120 140 160 Abundance Scan 2155 (14.572 min): 05251629.D\data.ms (-2108) (-) 166 20000 129 Sub 50 10000 94 47 59 84 35 69 117 0 0 m/z--> 40 60 80 100 120 140 160 Time--> 14.50 14.55 14.60 14.65

88 of 156 05251629.D R9042116.M Thu May 26 11:25:51 2016 Page 9 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251603.D Acq On : 25 May 2016 00:18 Operator: WA Sample : MB R9052516_1000mL Misc : S29-04191601(AC00463) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:28 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 94179 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 491956 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 208053 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 153414 12.492 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 57) Toluene-d8 (SS2) 13.31 98 488981 12.488 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 73) Bromofluorobenzene (SS3) 16.84 174 176020 13.608 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 108.88%

Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. 3) Dichlorodifluoromethan... 0.00 85 0 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 0.00 62 0 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.22 45 46 N.D. 11) Acetonitrile 0.00 41 0 N.D. 12) Acrolein 0.00 56 0 N.D. 13) Acetone 5.68 58 1846 0.173 ng 95 14) Trichlorofluoromethane 0.00 101 0 N.D. 15) 2-Propanol (Isopropanol) 0.00 45 0 N.D. 16) Acrylonitrile 0.00 53 0 N.D. 17) 1,1-Dichloroethene 0.00 96 0 N.D. 18) 2-Methyl-2-Propanol (t... 0.00 59 0 N.D. 19) Methylene Chloride 6.64 84 1544 0.100 ng 99 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 0.00 76 0 N.D. 23) trans-1,2-Dichloroethene 0.00 61 0 N.D. 24) 1,1-Dichloroethane 0.00 63 0 N.D. 25) Methyl tert-Butyl Ether 0.00 73 0 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. 27) 2-Butanone (MEK) 0.00 72 0 N.D. 28) cis-1,2-Dichloroethene 0.00 61 0 N.D. 29) Diisopropyl Ether 0.00 87 0 N.D. 30) Ethyl Acetate 0.00 61 0 N.D. 31) n-Hexane 0.00 57 0 N.D. 32) Chloroform 0.00 83 0 N.D. 34) Tetrahydrofuran (THF) 0.00 72 0 N.D. 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. 38) 1,1,1-Trichloroethane 0.00 97 0 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 0.00 56 0 N.D. 41) Benzene 10.51 78 796 N.D. 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 0.00 84 0 N.D. 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. 47) Trichloroethene 0.00 130 0 N.D. 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. 89 of 156 R9042116.M Wed May 25 17:19:07 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251603.D Acq On : 25 May 2016 00:18 Operator: WA Sample : MB R9052516_1000mL Misc : S29-04191601(AC00463) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:28 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 0.00 100 0 N.D. 51) n-Heptane 0.00 71 0 N.D. 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. 58) Toluene 13.42 91 2138 N.D. 59) 2-Hexanone 0.00 43 0 N.D. 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. 63) n-Octane 0.00 57 0 N.D. 64) Tetrachloroethene 0.00 166 0 N.D. 65) Chlorobenzene 0.00 112 0 N.D. 66) Ethylbenzene 0.00 91 0 N.D. 67) m- & p-Xylenes 0.00 91 0 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 0.00 91 0 N.D. 71) n-Nonane 0.00 43 0 N.D. 72) 1,1,2,2-Tetrachloroethane 0.00 83 0 N.D. 74) Cumene 0.00 105 0 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 0.00 91 0 N.D. 77) 3-Ethyltoluene 0.00 105 0 N.D. 78) 4-Ethyltoluene 0.00 105 0 N.D. 79) 1,3,5-Trimethylbenzene 0.00 105 0 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. 81) 2-Ethyltoluene 0.00 105 0 N.D. 82) 1,2,4-Trimethylbenzene 0.00 105 0 N.D. 83) n-Decane 0.00 57 0 N.D. 84) Benzyl Chloride 0.00 91 0 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. 88) 4-Isopropyltoluene (p-... 0.00 119 0 N.D. 89) 1,2,3-Trimethylbenzene 0.00 105 0 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 19.52 57 478 N.D. 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.75 128 743 N.D. 96) n-Dodecane 0.00 57 0 N.D. 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. 99) tert-Butylbenzene 0.00 119 0 N.D. 100) n-Butylbenzene 0.00 91 0 N.D. ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

90 of 156 R9042116.M Wed May 25 17:19:07 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251603.D Acq On : 25 May 2016 00:18 Operator: WA Sample : MB R9052516_1000mL Misc : S29-04191601(AC00463) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:28 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251603.D\data.ms 750000

700000

650000

600000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR 550000 1,4-Difluorobenzene (IS2),IR Bromofluorobenzene (SS3),S 500000

450000

400000

350000

300000

250000 Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S 200000

150000

100000

50000 Acetone,T Methylene Chloride,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0091 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Wed May 25 17:19:08 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251627.D Vial: 2 Acq On : 25 May 2016 18:00 Operator: WA Sample : MB2 R9052516_1000mL Inst : MS09 Misc : S29-04191601(AC00463)

Quant Time: May 26 07:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 105451 12.500 ng -0.05 37) 1,4-Difluorobenzene (IS2) 10.87 114 551714 12.500 ng -0.03 56) Chlorobenzene-d5 (IS3) 15.22 82 232857 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 163399 11.883 ng -0.04 Spiked Amount 12.500 Range 70 - 130 Recovery = 95.04% 57) Toluene-d8 (SS2) 13.31 98 547581 12.495 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 73) Bromofluorobenzene (SS3) 16.84 174 202299 13.974 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 111.76%

Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. 3) Dichlorodifluoromethan... 0.00 85 0 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 0.00 62 0 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.21 45 1182 0.116 ng # 52 11) Acetonitrile 5.43 41 95 N.D. 12) Acrolein 0.00 56 0 N.D. 13) Acetone 5.69 58 2166 0.181 ng # 75 14) Trichlorofluoromethane 0.00 101 0 N.D. 15) 2-Propanol (Isopropanol) 6.01 45 332 N.D. 16) Acrylonitrile 0.00 53 0 N.D. 17) 1,1-Dichloroethene 0.00 96 0 N.D. 18) 2-Methyl-2-Propanol (t... 6.69 59 62 N.D. 19) Methylene Chloride 6.64 84 1808 0.105 ng 93 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 0.00 76 0 N.D. 23) trans-1,2-Dichloroethene 0.00 61 0 N.D. 24) 1,1-Dichloroethane 0.00 63 0 N.D. 25) Methyl tert-Butyl Ether 0.00 73 0 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. 27) 2-Butanone (MEK) 0.00 72 0 N.D. 28) cis-1,2-Dichloroethene 0.00 61 0 N.D. 29) Diisopropyl Ether 0.00 87 0 N.D. 30) Ethyl Acetate 0.00 61 0 N.D. 31) n-Hexane 0.00 57 0 N.D. 32) Chloroform 0.00 83 0 N.D. 34) Tetrahydrofuran (THF) 0.00 72 0 N.D. 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. 38) 1,1,1-Trichloroethane 0.00 97 0 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 10.52 56 609 N.D. 41) Benzene 10.51 78 3196 N.D. 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 0.00 84 0 N.D. 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. 47) Trichloroethene 0.00 130 0 N.D. 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. 50) Methyl Methacrylate 0.00 100 0 N.D. 92 of 156 R9042116.M Thu May 26 10:05:50 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251627.D Vial: 2 Acq On : 25 May 2016 18:00 Operator: WA Sample : MB2 R9052516_1000mL Inst : MS09 Misc : S29-04191601(AC00463)

Quant Time: May 26 07:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 0.00 71 0 N.D. 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. 58) Toluene 13.41 91 2559 N.D. 59) 2-Hexanone 0.00 43 0 N.D. 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. 63) n-Octane 0.00 57 0 N.D. 64) Tetrachloroethene 0.00 166 0 N.D. 65) Chlorobenzene 0.00 112 0 N.D. 66) Ethylbenzene 0.00 91 0 N.D. 67) m- & p-Xylenes 0.00 91 0 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 0.00 91 0 N.D. 71) n-Nonane 0.00 43 0 N.D. 72) 1,1,2,2-Tetrachloroethane 0.00 83 0 N.D. 74) Cumene 0.00 105 0 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 0.00 91 0 N.D. 77) 3-Ethyltoluene 17.50 105 558 N.D. 78) 4-Ethyltoluene 17.50 105 558 N.D. 79) 1,3,5-Trimethylbenzene 0.00 105 0 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. 81) 2-Ethyltoluene 0.00 105 0 N.D. 82) 1,2,4-Trimethylbenzene 0.00 105 0 N.D. 83) n-Decane 0.00 57 0 N.D. 84) Benzyl Chloride 0.00 91 0 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. 88) 4-Isopropyltoluene (p-... 0.00 119 0 N.D. 89) 1,2,3-Trimethylbenzene 0.00 105 0 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 19.52 57 500 N.D. 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.73 128 2234 N.D. 96) n-Dodecane 0.00 57 0 N.D. 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. 99) tert-Butylbenzene 0.00 119 0 N.D. 100) n-Butylbenzene 0.00 91 0 N.D. ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

93 of 156 R9042116.M Thu May 26 10:05:50 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251627.D Vial: 2 Acq On : 25 May 2016 18:00 Operator: WA Sample : MB2 R9052516_1000mL Inst : MS09 Misc : S29-04191601(AC00463) Quant Time: May 26 07:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251627.D\data.ms

800000

750000

700000

650000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR

600000 Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR

550000

500000

450000

400000

350000

300000

250000 1,2-Dichloroethane-d4(SS1),S Bromochloromethane (IS1),IR

200000

150000

100000

50000 Methylene Chloride,T Acetone,T Ethanol,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0094 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 10:05:51 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251604.D Acq On : 25 May 2016 00:52 Operator: WA Sample : LCS R9052516_25ng Misc : S29-04191601/S29-05101606 (6/8) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:30 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.91 130 101579 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.88 114 518098 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 222485 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.69 65 161898 12.222 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 97.76% 57) Toluene-d8 (SS2) 13.32 98 517149 12.351 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 98.80% 73) Bromofluorobenzene (SS3) 16.84 174 195722 14.150 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 113.20%

Target Compounds Qvalue 2) Propene 3.67 42 309202 20.111 ng 99 3) Dichlorodifluoromethan... 3.78 85 595722 19.805 ng 100 4) Chloromethane 3.97 50 488512 19.286 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.13 135 322167 21.551 ng 100 6) Vinyl Chloride 4.25 62 431461 20.120 ng 100 7) 1,3-Butadiene 4.42 54 332828 30.688 ng 97 8) Bromomethane 4.72 94 283812 22.394 ng 100 9) Chloroethane 4.93 64 228278 21.961 ng 99 10) Ethanol 5.20 45 1168751 118.900 ng 100 11) Acetonitrile 5.38 41 573182 20.610 ng 99 12) Acrolein 5.49 56 180906 21.995 ng 98 13) Acetone 5.64 58 1180786 102.464 ng 96 14) Trichlorofluoromethane 5.79 101 502124 20.802 ng 100 15) 2-Propanol (Isopropanol) 5.97 45 1630363 44.151 ng 98 16) Acrylonitrile 6.16 53 423286 21.915 ng 99 17) 1,1-Dichloroethene 6.48 96 311319 23.416 ng 98 18) 2-Methyl-2-Propanol (t... 6.61 59 1663682 45.716 ng 99 19) Methylene Chloride 6.65 84 325263 19.588 ng 96 20) 3-Chloro-1-propene (Al... 6.76 41 454805 21.919 ng 100 21) Trichlorotrifluoroethane 6.94 151 265460 23.431 ng 100 22) Carbon Disulfide 6.90 76 1076004 20.513 ng 100 23) trans-1,2-Dichloroethene 7.66 61 445591 22.815 ng 97 24) 1,1-Dichloroethane 7.88 63 561640 21.201 ng 100 25) Methyl tert-Butyl Ether 7.93 73 959439 22.313 ng 99 26) Vinyl Acetate 8.06 86 357709 121.109 ng # 95 27) 2-Butanone (MEK) 8.29 72 220961 24.233 ng 99 28) cis-1,2-Dichloroethene 8.75 61 435657 22.743 ng 98 29) Diisopropyl Ether 8.99 87 258345 22.177 ng 99 30) Ethyl Acetate 8.99 61 239784 46.532 ng 97 31) n-Hexane 8.99 57 504526 20.089 ng 99 32) Chloroform 9.06 83 553449 23.168 ng 100 34) Tetrahydrofuran (THF) 9.44 72 216386 21.566 ng 97 35) Ethyl tert-Butyl Ether 9.53 87 381746 22.766 ng 99 36) 1,2-Dichloroethane 9.80 62 386720 23.440 ng 100 38) 1,1,1-Trichloroethane 10.06 97 473408 23.538 ng 100 39) Isopropyl Acetate 10.44 61 409087 46.873 ng 97 40) 1-Butanol 10.46 56 684928 52.208 ng 99 41) Benzene 10.52 78 1265524 20.556 ng 100 42) Carbon Tetrachloride 10.67 117 407601 24.729 ng 100 43) Cyclohexane 10.80 84 958624 43.867 ng 99 44) tert-Amyl Methyl Ether 11.13 73 920227 22.336 ng 100 45) 1,2-Dichloropropane 11.34 63 327857 22.277 ng 99 46) Bromodichloromethane 11.52 83 443570 24.293 ng 100 47) Trichloroethene 11.58 130 345742 23.445 ng 100 48) 1,4-Dioxane 11.55 88 281169 26.962 ng 98 49) 2,2,4-Trimethylpentane... 11.64 57 1356246 20.869 ng 99 95 of 156 R9042116.M Wed May 25 17:19:29 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251604.D Acq On : 25 May 2016 00:52 Operator: WA Sample : LCS R9052516_25ng Misc : S29-04191601/S29-05101606 (6/8) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:30 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 263098 49.726 ng 99 51) n-Heptane 11.90 71 319686 22.141 ng 99 52) cis-1,3-Dichloropropene 12.43 75 501336 24.034 ng 99 53) 4-Methyl-2-pentanone 12.46 58 317064 24.494 ng 100 54) trans-1,3-Dichloropropene 12.95 75 454754 23.847 ng 100 55) 1,1,2-Trichloroethane 13.12 97 324299 24.198 ng 99 58) Toluene 13.42 91 1340706 22.263 ng 100 59) 2-Hexanone 13.66 43 761837 26.612 ng 99 60) Dibromochloromethane 13.83 129 376383 25.968 ng 100 61) 1,2-Dibromoethane 14.08 107 370554 25.622 ng 99 62) n-Butyl Acetate 14.31 43 850232 25.916 ng 99 63) n-Octane 14.44 57 277629 21.001 ng 98 64) Tetrachloroethene 14.57 166 368098 23.567 ng 100 65) Chlorobenzene 15.27 112 876009 23.956 ng 100 66) Ethylbenzene 15.68 91 1519947 23.876 ng 100 67) m- & p-Xylenes 15.87 91 2402948 47.254 ng 100 68) Bromoform 15.93 173 323413 26.393 ng 99 69) Styrene 16.25 104 957885 26.088 ng 100 70) o-Xylene 16.37 91 1210196 22.948 ng 100 71) n-Nonane 16.61 43 632008 20.604 ng 99 72) 1,1,2,2-Tetrachloroethane 16.34 83 584574 23.515 ng 100 74) Cumene 16.98 105 1520701 23.072 ng 100 75) alpha-Pinene 17.40 93 788859 23.723 ng 99 76) n-Propylbenzene 17.52 91 1851995 22.760 ng 100 77) 3-Ethyltoluene 17.63 105 1556169 24.586 ng 100 78) 4-Ethyltoluene 17.68 105 1452244 23.959 ng 100 79) 1,3,5-Trimethylbenzene 17.76 105 1262376 24.203 ng 100 80) alpha-Methylstyrene 17.91 118 707300 26.367 ng 100 81) 2-Ethyltoluene 17.95 105 1479560 24.089 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 1314046 25.526 ng 99 83) n-Decane 18.31 57 688776 22.135 ng 99 84) Benzyl Chloride 18.32 91 1118091 24.954 ng 100 85) 1,3-Dichlorobenzene 18.34 146 763678 28.409 ng 100 86) 1,4-Dichlorobenzene 18.41 146 755737 27.445 ng 100 87) sec-Butylbenzene 18.48 105 1711966 24.770 ng 100 88) 4-Isopropyltoluene (p-... 18.64 119 1575168 24.816 ng 100 89) 1,2,3-Trimethylbenzene 18.63 105 1354829 25.551 ng 100 90) 1,2-Dichlorobenzene 18.77 146 731475 27.688 ng 100 91) d-Limonene 18.79 68 524108 24.536 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.23 157 265162 24.692 ng 99 93) n-Undecane 19.65 57 715222 23.344 ng 100 94) 1,2,4-Trichlorobenzene 20.59 180 524936 24.992 ng 99 95) Naphthalene 20.70 128 1693210 23.820 ng 100 96) n-Dodecane 20.74 57 689576 21.717 ng 100 97) Hexachlorobutadiene 21.07 225 334804 29.706 ng 100 98) Cyclohexanone 16.02 55 526864 29.807 ng 99 99) tert-Butylbenzene 18.19 119 1249734 24.766 ng 100 100) n-Butylbenzene 19.08 91 1406634 26.111 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

96 of 156 R9042116.M Wed May 25 17:19:29 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251604.D Acq On : 25 May 2016 00:52 Operator: WA Sample : LCS R9052516_25ng Misc : S29-04191601/S29-05101606 (6/8) ALS Vial : 2 Sample Multiplier: 1

Quant Time: May 25 06:28:30 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251604.D\data.ms

5000000

4800000

4600000

4400000 1,2,3-Trimethylbenzene,T 4200000

4000000 4-Isopropyltoluene (p-Cymene),T 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T

3800000

3600000

3400000

3200000 n-Decane,T Diisopropyln-Hexane,T Ether,T 3000000 Benzyl Chloride,T Ethyl Acetate,T

2800000

2600000 n-Butylbenzene,T d-Limonene,T sec-Butylbenzene,T 4-Ethyltoluene,T n-Dodecane,T

2400000 2-Ethyltoluene,T Naphthalene,T Isopropyl Acetate,T n-Propylbenzene,T n-Undecane,T 3-Ethyltoluene,T m- & p-Xylenes,T Cyclohexane,T alpha-Methylstyrene,T 1,3,5-Trimethylbenzene,T Vinyl Acetate,T

2200000 Cumene,T 1-Butanol,T 1,2-Dichlorobenzene,T 1,3-Dichlorobenzene,T o-Xylene,T

2000000 Acetone,T Hexachlorobutadiene,T Ethylbenzene,T alpha-Pinene,T 1,4-Dichlorobenzene,T Styrene,T 1,2,4-Trichlorobenzene,T 1800000 n-Nonane,T Methyl Methacrylate,T Toluene,T

1600000 n-Octane,T Chlorobenzene,T 2,2,4-Trimethylpentane (Isooctane),T Benzene,T

1400000 n-Heptane,T 1,1,2,2-Tetrachloroethane,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T n-Butyl Acetate,T Tetrachloroethene,T Cyclohexanone,T 4-Methyl-2-pentanone,T 2-Hexanone,T

1200000 tert-Amyl Methyl Ether,T 2-Propanol (Isopropanol),T Propene,T Ethyl tert-Butyl Ether,T Trichloroethene,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 1,2-Dibromo-3-Chloropropane,T 1,1,2-Trichloroethane,T Dichlorodifluoromethane (CFC 12),T

1000000 cis-1,3-Dichloropropene,T Methyl tert-Butyl Ether,T 1,3-Butadiene,T 1,2-Dichloropropane,T trans-1,3-Dichloropropene,T Toluene-d8 (SS2),S Trichlorotrifluoroethane,T Tetrahydrofuran (THF),T Bromodichloromethane,T Carbon Disulfide,T 1,1-Dichloroethene,T cis-1,2-Dichloroethene,T 1,1,1-Trichloroethane,T Chloroform,T Chlorobenzene-d5 (IS3),IR Ethanol,T Dibromochloromethane,T trans-1,2-Dichloroethene,T Carbon Tetrachloride,T Bromofluorobenzene (SS3),S

800000 1,4-Dioxane,T 2-Butanone (MEK),T Methylene Chloride,T 1,4-Difluorobenzene (IS2),IR Trichlorofluoromethane,T Bromoform,T Chloromethane,T 3-Chloro-1-propene (Allyl Chloride),T 1,2-Dibromoethane,T 1,1-Dichloroethane,T 1,2-Dichloroethane,T Vinyl Chloride,T Acrylonitrile,T Bromomethane,T 600000 Acetonitrile,T Chloroethane,T Bromochloromethane (IS1),IR 400000 1,2-Dichloroethane-d4(SS1),S Acrolein,T

200000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.0097 of 14.00156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Wed May 25 17:19:29 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251628.D Vial: 2 Acq On : 25 May 2016 18:33 Operator: WA Sample : LCS2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05101606 (6/8)

Quant Time: May 26 07:04:01 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.92 130 115023 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.88 114 591634 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 253986 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.69 65 176449 11.764 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 94.08% 57) Toluene-d8 (SS2) 13.32 98 585400 12.247 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 98.00% 73) Bromofluorobenzene (SS3) 16.84 174 226788 14.362 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 114.88%

Target Compounds Qvalue 2) Propene 3.67 42 331397 19.035 ng 99 3) Dichlorodifluoromethan... 3.78 85 638430 18.744 ng 99 4) Chloromethane 3.97 50 536280 18.698 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.13 135 358666 21.188 ng 100 6) Vinyl Chloride 4.25 62 481594 19.833 ng 99 7) 1,3-Butadiene 4.42 54 376666 30.671 ng 99 8) Bromomethane 4.72 94 319835 22.286 ng 99 9) Chloroethane 4.93 64 257424 21.870 ng 99 10) Ethanol 5.20 45 1281717 115.151 ng 99 11) Acetonitrile 5.38 41 625704 19.869 ng 100 12) Acrolein 5.49 56 200548 21.533 ng 98 13) Acetone 5.64 58 1305955 100.080 ng 99 14) Trichlorofluoromethane 5.80 101 542979 19.865 ng 100 15) 2-Propanol (Isopropanol) 5.98 45 1773026 42.403 ng 99 16) Acrylonitrile 6.17 53 465234 21.271 ng 99 17) 1,1-Dichloroethene 6.48 96 347640 23.091 ng 95 18) 2-Methyl-2-Propanol (t... 6.61 59 1820097 44.169 ng 99 19) Methylene Chloride 6.65 84 362404 19.274 ng 94 20) 3-Chloro-1-propene (Al... 6.76 41 493091 20.987 ng 98 21) Trichlorotrifluoroethane 6.94 151 297813 23.215 ng 98 22) Carbon Disulfide 6.90 76 1196372 20.142 ng 100 23) trans-1,2-Dichloroethene 7.66 61 492394 22.265 ng 97 24) 1,1-Dichloroethane 7.88 63 617116 20.573 ng 100 25) Methyl tert-Butyl Ether 7.94 73 1054990 21.667 ng 99 26) Vinyl Acetate 8.06 86 398572 119.172 ng # 88 27) 2-Butanone (MEK) 8.29 72 245427 23.770 ng 95 28) cis-1,2-Dichloroethene 8.75 61 476889 21.986 ng 97 29) Diisopropyl Ether 8.99 87 287614 21.804 ng # 94 30) Ethyl Acetate 8.99 61 265319 45.470 ng 99 31) n-Hexane 8.99 57 559425 19.672 ng 100 32) Chloroform 9.06 83 596477 22.050 ng 99 34) Tetrahydrofuran (THF) 9.44 72 238853 21.023 ng 95 35) Ethyl tert-Butyl Ether 9.53 87 422069 22.229 ng 98 36) 1,2-Dichloroethane 9.80 62 411505 22.027 ng 99 38) 1,1,1-Trichloroethane 10.07 97 515396 22.441 ng 99 39) Isopropyl Acetate 10.44 61 452293 45.383 ng 98 40) 1-Butanol 10.46 56 758525 50.632 ng 99 41) Benzene 10.52 78 1408538 20.035 ng 100 42) Carbon Tetrachloride 10.68 117 441097 23.435 ng 100 43) Cyclohexane 10.80 84 1068747 42.827 ng 97 44) tert-Amyl Methyl Ether 11.13 73 1014026 21.554 ng 99 45) 1,2-Dichloropropane 11.34 63 361447 21.507 ng 99 46) Bromodichloromethane 11.52 83 480405 23.041 ng 99 47) Trichloroethene 11.58 130 386428 22.946 ng 99 48) 1,4-Dioxane 11.55 88 309329 25.976 ng 97 49) 2,2,4-Trimethylpentane... 11.64 57 1485468 20.016 ng 100 50) Methyl Methacrylate 11.77 100 295710 48.943 ng 96 98 of 156 R9042116.M Thu May 26 10:06:05 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251628.D Vial: 2 Acq On : 25 May 2016 18:33 Operator: WA Sample : LCS2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05101606 (6/8)

Quant Time: May 26 07:04:01 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 11.90 71 353343 21.430 ng 98 52) cis-1,3-Dichloropropene 12.43 75 548962 23.046 ng 100 53) 4-Methyl-2-pentanone 12.46 58 346394 23.434 ng 99 54) trans-1,3-Dichloropropene 12.95 75 498870 22.909 ng 100 55) 1,1,2-Trichloroethane 13.12 97 357307 23.347 ng 99 58) Toluene 13.42 91 1476898 21.483 ng 100 59) 2-Hexanone 13.66 43 819039 25.062 ng 99 60) Dibromochloromethane 13.83 129 412965 24.958 ng 100 61) 1,2-Dibromoethane 14.08 107 408303 24.730 ng 100 62) n-Butyl Acetate 14.31 43 915426 24.443 ng 100 63) n-Octane 14.44 57 302725 20.059 ng 97 64) Tetrachloroethene 14.57 166 407379 22.847 ng 100 65) Chlorobenzene 15.27 112 967340 23.173 ng 100 66) Ethylbenzene 15.68 91 1669449 22.972 ng 100 67) m- & p-Xylenes 15.87 91 2633344 45.362 ng 100 68) Bromoform 15.93 173 355007 25.378 ng 99 69) Styrene 16.25 104 1058133 25.244 ng 100 70) o-Xylene 16.37 91 1325424 22.016 ng 100 71) n-Nonane 16.61 43 681637 19.466 ng 99 72) 1,1,2,2-Tetrachloroethane 16.34 83 638760 22.508 ng 100 74) Cumene 16.99 105 1661065 22.076 ng 100 75) alpha-Pinene 17.40 93 860762 22.675 ng 99 76) n-Propylbenzene 17.52 91 2011474 21.654 ng 100 77) 3-Ethyltoluene 17.63 105 1702421 23.561 ng 100 78) 4-Ethyltoluene 17.68 105 1583553 22.885 ng 100 79) 1,3,5-Trimethylbenzene 17.75 105 1379673 23.172 ng 100 80) alpha-Methylstyrene 17.91 118 766203 25.020 ng 99 81) 2-Ethyltoluene 17.95 105 1605816 22.902 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 1425882 24.264 ng 100 83) n-Decane 18.31 57 744137 20.948 ng 99 84) Benzyl Chloride 18.32 91 1218553 23.824 ng 100 85) 1,3-Dichlorobenzene 18.34 146 833936 27.175 ng 100 86) 1,4-Dichlorobenzene 18.41 146 823196 26.187 ng 100 87) sec-Butylbenzene 18.48 105 1854483 23.504 ng 100 88) 4-Isopropyltoluene (p-... 18.64 119 1702891 23.501 ng 100 89) 1,2,3-Trimethylbenzene 18.64 105 1463305 24.174 ng 100 90) 1,2-Dichlorobenzene 18.77 146 793759 26.319 ng 100 91) d-Limonene 18.80 68 562924 23.085 ng 98 92) 1,2-Dibromo-3-Chloropr... 19.23 157 288286 23.515 ng 97 93) n-Undecane 19.65 57 763466 21.828 ng 99 94) 1,2,4-Trichlorobenzene 20.59 180 569959 23.770 ng 99 95) Naphthalene 20.70 128 1837787 22.647 ng 100 96) n-Dodecane 20.74 57 746057 20.582 ng 99 97) Hexachlorobutadiene 21.07 225 362107 28.144 ng 99 98) Cyclohexanone 16.02 55 572573 28.375 ng 99 99) tert-Butylbenzene 18.19 119 1350820 23.449 ng 100 100) n-Butylbenzene 19.08 91 1509755 24.549 ng 100 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

99 of 156 R9042116.M Thu May 26 10:06:05 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251628.D Vial: 2 Acq On : 25 May 2016 18:33 Operator: WA Sample : LCS2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05101606 (6/8) Quant Time: May 26 07:04:01 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251628.D\data.ms 5600000

5400000

5200000

5000000

4800000

4600000 1,2,3-Trimethylbenzene,T

4400000 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T 4200000 4-Isopropyltoluene (p-Cymene),T

4000000

3800000

3600000

3400000 n-Decane,T Diisopropyln-Hexane,T Ether,T Benzyl Chloride,T 3200000 Ethyl Acetate,T

3000000

2800000 n-Butylbenzene,T d-Limonene,T sec-Butylbenzene,T 4-Ethyltoluene,T n-Dodecane,T

2600000 Naphthalene,T 3-Ethyltoluene,T n-Propylbenzene,T m- & p-Xylenes,T 2-Ethyltoluene,T Cyclohexane,T Isopropyl Acetate,T n-Undecane,T 1,3,5-Trimethylbenzene,T alpha-Methylstyrene,T Vinyl Acetate,T

2400000 1-Butanol,T Cumene,T 1,2-Dichlorobenzene,T 1,3-Dichlorobenzene,T 2200000 o-Xylene,T Ethylbenzene,T Acetone,T alpha-Pinene,T Hexachlorobutadiene,T 1,4-Dichlorobenzene,T

2000000 Styrene,T n-Nonane,T 1,2,4-Trichlorobenzene,T Methyl Methacrylate,T Toluene,T 1800000 n-Octane,T Chlorobenzene,T 1600000 2,2,4-Trimethylpentane (Isooctane),T Benzene,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T n-Heptane,T 1,1,2,2-Tetrachloroethane,T 1400000 n-Butyl Acetate,T Tetrachloroethene,T Cyclohexanone,T 2-Hexanone,T 4-Methyl-2-pentanone,T tert-Amyl Methyl Ether,T 2-Propanol (Isopropanol),T Trichloroethene,T Ethyl tert-Butyl Ether,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 1200000 Propene,T 1,1,2-Trichloroethane,T 1,2-Dibromo-3-Chloropropane,T cis-1,3-Dichloropropene,T Dichlorodifluoromethane (CFC 12),T Methyl tert-Butyl Ether,T 1,3-Butadiene,T 1,2-Dichloropropane,T Toluene-d8 (SS2),S

1000000 trans-1,3-Dichloropropene,T Trichlorotrifluoroethane,T Carbon Disulfide,T Tetrahydrofuran (THF),T Chlorobenzene-d5 (IS3),IR cis-1,2-Dichloroethene,T 1,1-Dichloroethene,T Bromodichloromethane,T 1,1,1-Trichloroethane,T Chloroform,T Bromofluorobenzene (SS3),S Ethanol,T Methylene Chloride,T Dibromochloromethane,T trans-1,2-Dichloroethene,T Carbon Tetrachloride,T 1,4-Dioxane,T 1,4-Difluorobenzene (IS2),IR 2-Butanone (MEK),T Bromoform,T 800000 Trichlorofluoromethane,T Chloromethane,T 1,2-Dibromoethane,T 1,1-Dichloroethane,T 3-Chloro-1-propene (Allyl Chloride),T Vinyl Chloride,T 1,2-Dichloroethane,T Bromomethane,T Acrylonitrile,T 600000 Acetonitrile,T Chloroethane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

400000 Acrolein,T

200000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00100 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 10:06:06 2016 Page: 3 Response Factor Report MS09

Method Path : I:\MS09\Methods\ Method File : R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) 4/22/16 Last Update : Fri Apr 22 10:14:32 2016 Response Via : Initial Calibration

Calibration Files 0.08=04211621.D 0.10=04211622.D 0.20=04211623.D 0.40=04211624.D 1.0 =04211625.D 5.0 =04211626.D 25 =04211627.D 50 =04211628.D 100 =04211629.D

Compound 0.08 0.10 0.20 0.40 1.0 5.0 25 50 100 Avg %RSD ------

1) IR Bromochloromethane... ------ISTD------2) T Propene 2.106 1.826 1.681 1.893 1.795 1.726 2.117 1.958 1.925 1.892 8.11 3) T Dichlorodifluo... 3.567 3.515 3.417 3.856 3.634 3.677 4.149 3.868 3.628 3.701 6.01 4) T Chloromethane 3.029 3.051 2.760 3.280 3.091 3.078 3.548 3.265 2.952 3.117 7.20 5) T 1,2-Dichloro-1... 1.819 1.716 1.741 1.866 1.780 1.779 2.016 1.938 1.900 1.840 5.36 6) T Vinyl Chloride 2.442 2.468 2.197 2.683 2.586 2.608 3.034 2.895 2.837 2.639 9.75 7) T 1,3-Butadiene 0.893 1.130 1.093 1.156 1.676 1.677 1.716 1.335 25.72 8) T Bromomethane 1.421 1.328 1.394 1.583 1.531 1.538 1.826 1.746 1.671 1.560 10.63 9) T Chloroethane 1.338 1.363 1.243 1.262 1.200 1.202 1.365 1.296 1.244 1.279 5.04 10) T Ethanol 1.138 0.992 1.074 1.234 1.481 1.166 1.604 1.161 1.036 1.210 16.92 11) T Acetonitrile 3.490 3.246 3.257 3.468 3.643 2.954 3.996 3.748 2.999 3.422 10.06 12) T Acrolein 0.805 0.768 0.722 0.990 1.013 1.091 1.334 1.232 1.154 1.012 21.12 13) T Acetone 1.522 1.471 1.331 1.504 1.359 1.371 1.531 1.414 1.260 1.418 6.69 14) of 156 101 T Trichlorofluor... 3.101 2.804 2.686 3.068 2.916 2.883 3.223 3.076 2.976 2.970 5.59 15) T 2-Propanol (Is... 4.042 4.207 3.866 4.501 4.870 4.848 5.287 4.905 4.371 4.544 10.26 16) T Acrylonitrile 1.286 2.356 2.408 2.501 2.827 2.676 2.584 2.377 21.33 17) T 1,1-Dichloroet... 1.571 1.305 1.524 1.692 1.616 1.600 1.884 1.796 1.737 1.636 10.33 18) T 2-Methyl-2-Pro... 4.115 4.094 3.917 4.592 4.624 4.687 5.164 4.848 4.264 4.478 9.09 19) T Methylene Chlo... 2.650 2.293 1.919 1.786 1.982 1.878 1.796 2.043 15.52 20) T 3-Chloro-1-pro... 2.229 2.065 2.307 2.639 2.458 2.830 2.986 2.800 2.667 2.553 12.05 21) T Trichlorotrifl... 1.403 1.305 1.269 1.463 1.374 1.329 1.520 1.463 1.422 1.394 5.91 22) T Carbon Disulfide 5.098 5.583 5.384 6.277 6.303 6.672 7.916 7.599 7.263 6.455 15.44 23) T trans-1,2-Dich... 1.997 1.984 1.895 2.340 2.466 2.559 2.931 2.788 2.670 2.403 15.63 24) T 1,1-Dichloroet... 3.074 3.188 2.957 3.359 3.238 3.217 3.609 3.410 3.286 3.260 5.83 25) T Methyl tert-Bu... 5.009 5.089 4.723 5.419 5.170 5.227 5.939 5.633 5.415 5.291 6.78 26) T Vinyl Acetate 0.241 0.275 0.330 0.371 0.462 0.442 0.423 0.363 23.44 27) T 2-Butanone (MEK) 0.841 0.951 0.978 1.153 1.139 1.171 1.347 1.279 1.240 1.122 14.84 28) T cis-1,2-Dichlo... 2.113 2.242 2.060 2.387 2.300 2.389 2.711 2.553 2.459 2.357 8.75 29) T Diisopropyl Ether 1.480 0.817 1.580 1.760 1.419 1.389 1.577 1.487 1.393 1.434 18.09 30) T Ethyl Acetate 0.500 0.523 0.548 0.658 0.684 0.677 0.767 0.711 0.640 0.634 14.35 31) T n-Hexane 3.126 3.285 2.983 3.403 3.087 3.018 3.217 2.998 2.697 3.090 6.60 32) T Chloroform 3.036 2.767 2.635 2.957 2.843 2.873 3.264 3.092 2.990 2.940 6.32 33) S 1,2-Dichloroet... 1.631 1.631 1.626 1.690 1.624 1.635 1.613 1.613 1.606 1.630 1.51 34) T Tetrahydrofura... 1.288 1.217 1.153 1.239 1.215 1.194 1.326 1.257 1.225 1.235 4.11 35) T Ethyl tert-But... 2.044 1.783 1.759 2.134 2.019 2.056 2.349 2.251 2.176 2.063 9.50 36) T 1,2-Dichloroet... 1.794 1.765 1.826 2.150 2.064 2.055 2.323 2.190 2.103 2.030 9.55

37) IR 1,4-Difluorobenzen... ------ISTD------38) T 1,1,1-Trichlor... 0.436 0.417 0.440 0.495 0.488 0.493 0.555 0.533 0.509 0.485 9.50 39) T Isopropyl Acetate 0.197 0.198 0.176 0.211 0.215 0.219 0.242 0.228 0.208 0.211 9.09 40) T 1-Butanol 0.199 0.224 0.363 0.373 0.379 0.354 0.324 0.317 23.43 41) T Benzene 1.825 1.682 1.495 1.626 1.333 1.321 1.429 1.361 1.297 1.485 12.56 42) T Carbon Tetrach... 0.366 0.365 0.338 0.387 0.392 0.402 0.459 0.443 0.428 0.398 10.00 R9042116.M Fri Apr 22 10:42:46 2016 Page: 1 Response Factor Report MS09

Method Path : I:\MS09\Methods\ Method File : R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) 43) T Cyclohexane 0.522 0.507 0.473 0.542 0.520 0.524 0.585 0.557 0.515 0.527 6.02 44) T tert-Amyl Meth... 0.961 0.924 0.892 0.977 0.977 0.994 1.126 1.075 1.021 0.994 7.26 45) T 1,2-Dichloropr... 0.342 0.315 0.324 0.360 0.360 0.355 0.397 0.379 0.363 0.355 7.15 46) T Bromodichlorom... 0.405 0.374 0.383 0.436 0.428 0.450 0.517 0.496 0.474 0.441 11.13 47) T Trichloroethene 0.320 0.324 0.317 0.355 0.354 0.362 0.403 0.390 0.377 0.356 8.70 48) T 1,4-Dioxane 0.184 0.227 0.203 0.228 0.260 0.272 0.308 0.297 0.286 0.252 17.22 49) T 2,2,4-Trimethy... 1.574 1.579 1.428 1.550 1.546 1.556 1.740 1.632 1.508 1.568 5.42 50) T Methyl Methacr... 0.097 0.100 0.107 0.124 0.132 0.138 0.156 0.150 0.144 0.128 17.14 51) T n-Heptane 0.332 0.336 0.329 0.373 0.342 0.340 0.378 0.362 0.344 0.348 5.16 52) T cis-1,3-Dichlo... 0.400 0.400 0.383 0.473 0.521 0.546 0.627 0.603 0.576 0.503 18.51 53) T 4-Methyl-2-pen... 0.256 0.270 0.255 0.309 0.328 0.334 0.373 0.353 0.332 0.312 13.72 54) T trans-1,3-Dich... 0.296 0.381 0.439 0.480 0.563 0.543 0.519 0.460 20.77 55) T 1,1,2-Trichlor... 0.282 0.283 0.280 0.308 0.330 0.334 0.379 0.364 0.350 0.323 11.55

56) IR Chlorobenzene-d5 (... ------ISTD------57) S Toluene-d8 (SS2) 2.343 2.369 2.372 2.366 2.358 2.349 2.326 2.340 2.350 2.353 0.64 58) T Toluene 3.572 3.398 3.095 3.323 3.302 3.267 3.663 3.499 3.332 3.383 5.09 59) T 2-Hexanone 1.299 1.298 1.288 1.551 1.768 1.815 1.933 1.817 1.707 1.608 15.93 60) T Dibromochlorom... 0.655 0.724 0.680 0.741 0.809 0.846 0.991 0.953 0.931 0.814 15.17 61) T 1,2-Dibromoethane 0.613 0.673 0.670 0.762 0.831 0.860 0.997 0.967 0.941 0.813 17.37 62) T n-Butyl Acetate 1.599 1.475 1.508 1.729 1.983 2.043 2.216 2.086 1.949 1.843 14.72 63) T n-Octane 0.725 0.733 0.664 0.740 0.750 0.728 0.823 0.783 0.739 0.743 5.81 64) T Tetrachloroethene 0.789 0.813 0.749 0.827 0.875 0.881 1.008 0.982 0.974 0.878 10.54 65) of 156 102 T Chlorobenzene 1.977 1.928 1.797 1.970 2.063 2.052 2.324 2.227 2.153 2.054 7.84 66) T Ethylbenzene 3.368 3.211 3.068 3.406 3.599 3.673 4.157 3.961 3.748 3.577 9.83 67) T m- & p-Xylenes 2.635 2.587 2.397 2.750 2.895 2.932 3.326 3.182 3.008 2.857 10.36 68) T Bromoform 0.520 0.527 0.548 0.604 0.671 0.721 0.879 0.862 0.864 0.688 21.77 69) T Styrene 1.724 1.636 1.679 1.868 2.140 2.203 2.537 2.433 2.345 2.063 16.70 70) T o-Xylene 2.834 2.738 2.610 2.751 2.971 2.973 3.416 3.264 3.110 2.963 8.88 71) T n-Nonane 1.668 1.744 1.556 1.718 1.741 1.746 1.937 1.792 1.609 1.723 6.35 72) T 1,1,2,2-Tetrac... 1.159 1.114 1.100 1.218 1.454 1.495 1.749 1.676 1.606 1.397 18.16 73) S Bromofluoroben... 0.768 0.773 0.773 0.769 0.777 0.782 0.781 0.780 0.790 0.777 0.91 74) T Cumene 3.437 3.383 3.168 3.598 3.738 3.766 4.298 4.090 3.850 3.703 9.55 75) T alpha-Pinene 1.772 1.645 1.622 1.803 1.809 1.878 2.195 2.093 1.997 1.868 10.39 76) T n-Propylbenzene 4.193 4.146 3.861 4.326 4.709 4.781 5.370 5.059 4.702 4.572 10.51 77) T 3-Ethyltoluene 3.462 3.186 2.843 3.293 3.554 3.658 4.279 3.952 3.779 3.556 12.02 78) T 4-Ethyltoluene 3.018 2.947 2.930 3.231 3.541 3.598 3.953 3.857 3.573 3.405 11.40 79) T 1,3,5-Trimethy... 2.704 2.560 2.458 2.711 3.016 3.052 3.449 3.294 3.129 2.930 11.59 80) T alpha-Methylst... 1.166 1.196 1.088 1.333 1.626 1.703 1.895 1.815 1.742 1.507 20.61 81) T 2-Ethyltoluene 3.209 3.025 2.951 3.204 3.567 3.566 4.032 3.862 3.641 3.451 10.85 82) T 1,2,4-Trimethy... 2.592 2.553 2.322 2.520 3.006 3.072 3.546 3.357 3.063 2.892 14.40 83) T n-Decane 1.687 1.553 1.557 1.606 1.853 1.866 2.095 1.911 1.607 1.748 10.90 84) T Benzyl Chloride 1.387 2.152 2.521 3.161 3.048 2.835 2.517 26.39 85) T 1,3-Dichlorobe... 1.127 1.210 1.123 1.257 1.612 1.653 1.939 1.876 1.798 1.510 22.00 86) T 1,4-Dichlorobe... 1.166 1.191 1.104 1.322 1.668 1.726 1.980 1.912 1.855 1.547 22.64 87) T sec-Butylbenzene 3.372 3.424 3.376 3.610 4.035 4.089 4.632 4.365 4.044 3.883 11.83 88) T 4-Isopropyltol... 3.127 3.026 2.958 3.272 3.798 3.827 4.372 4.086 3.630 3.566 13.97 89) T 1,2,3-Trimethy... 2.610 2.554 2.379 2.653 3.128 3.184 3.661 3.488 3.154 2.979 15.02 90) T 1,2-Dichlorobe... 1.135 1.189 1.105 1.243 1.611 1.642 1.886 1.812 1.736 1.484 21.09 91) T d-Limonene 0.986 1.058 1.011 1.102 1.268 1.311 1.444 1.377 1.244 1.200 13.84 92) T 1,2-Dibromo-3-... 0.372 0.535 0.596 0.722 0.702 0.694 0.603 22.24 93) T n-Undecane 1.499 1.416 1.229 1.389 1.966 1.976 2.176 2.032 1.809 1.721 19.82 94) T 1,2,4-Trichlor... 0.623 1.152 1.221 1.381 1.356 1.348 1.180 24.35 R9042116.M Fri Apr 22 10:42:46 2016 Page: 2 Response Factor Report MS09

Method Path : I:\MS09\Methods\ Method File : R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) 95) T Naphthalene 1.968 4.144 4.382 4.728 4.509 4.232 3.994 25.38 96) T n-Dodecane 1.003 1.925 2.019 2.076 1.949 1.730 1.784 22.42 97) T Hexachlorobuta... 0.462 0.438 0.490 0.494 0.666 0.695 0.821 0.812 0.819 0.633 25.85 98) T Cyclohexanone 0.818 0.838 0.752 0.887 1.119 1.152 1.173 1.122 1.077 0.993 16.75 99) T tert-Butylbenzene 2.643 2.551 2.398 2.688 2.871 2.940 3.374 3.173 2.878 2.835 10.79 100) T n-Butylbenzene 2.592 2.447 2.409 2.698 3.263 3.314 3.734 3.529 3.255 3.027 16.34 ------(#) = Out of Range 103 of 156 103

R9042116.M Fri Apr 22 10:42:46 2016 Page: 3 Primary Source Standards Concentrations (Working & Initial Calibration) 1ng/L Std. ID: 4ng/L Std. ID: S29-04201403 20ng/L Std. ID: S29-04131608

200ng/L Std. ID: S29-04131603 Working STD Dilution Factors: 5 50 250 1000 Conc.(ng/L): 4444 20 20 200 200 200 Source Std. Primary Working Standards Injection (L): 0.020 0.025 0.050 0.100 0.050 0.25 0.125 0.25 0.50 Compounds mg/m3 200ng/L 20ng/L 4ng/L 1ng/L ICAL Points: 0.08ng 0.1ng 0.2ng 0.4ng 1ng 5ng 25ng 50ng 100ng Propene 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Dichlorodifluoromethane 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 Chloromethane 0.98 196 19.6 3.92 0.98 0.0784 0.098 0.196 0.392 0.98 4.90 24.50 49.0 98 Freon-114 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Vinyl Chloride 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 1,3-Butadiene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106 Bromomethane 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 Chloroethane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101 Ethanol 5.06 1012 101.2 20.24 5.06 0.4048 0.506 1.012 2.024 5.06 25.30 126.50 253.0 506 Acetonitrile 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102 Acrolein 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Acetone 5.37 1074 107.4 21.48 5.37 0.4296 0.537 1.074 2.148 5.37 26.85 134.25 268.5 537 Trichlorofluoromethane 0.99 198 19.8 3.96 0.99 0.0792 0.099 0.198 0.396 0.99 4.95 24.75 49.5 99 Isopropanol 2.09 418 41.8 8.36 2.09 0.1672 0.209 0.418 0.836 2.09 10.45 52.25 104.5 209 Acrylonitrile 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 1,1-Dichloroethene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 tert-Butanol 2.09 418 41.8 8.36 2.09 0.1672 0.209 0.418 0.836 2.09 10.45 52.25 104.5 209 Methylene Chloride 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Allyl Chloride 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Trichlorotrifluoroethane 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Carbon Disulfide 0.98 196 19.6 3.92 0.98 0.0784 0.098 0.196 0.392 0.98 4.90 24.50 49.0 98 trans-1,2-Dichloroethene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106 1,1-Dichloroethane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 104 of 156 104 Methyl tert-Butyl Ether 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 Vinyl Acetate 5.07 1014 101.4 20.28 5.07 0.4056 0.507 1.014 2.028 5.07 25.35 126.75 253.5 507 2-Butanone 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 cis-1,2-Dichloroethene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Diisopropyl Ether 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Ethyl Acetate 2.12 424 42.4 8.48 2.12 0.1696 0.212 0.424 0.848 2.12 10.60 53.00 106.0 212 n-Hexane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 Chloroform 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Tetrahydrofuran 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102 Ethyl tert-Butyl Ether 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 1,2-Dichloroethane 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 1,1,1-Trichloroethane 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Isopropyl Acetate 2.21 442 44.2 8.84 2.21 0.1768 0.221 0.442 0.884 2.21 11.05 55.25 110.5 221 1-Butanol 2.26 452 45.2 9.04 2.26 0.1808 0.226 0.452 0.904 2.26 11.30 56.50 113.0 226 Benzene 1.11 222 22.2 4.44 1.11 0.0888 0.111 0.222 0.444 1.11 5.55 27.75 55.5 111 Carbon Tetrachloride 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Cyclohexane 2.09 418 41.8 8.36 2.09 0.1672 0.209 0.418 0.836 2.09 10.45 52.25 104.5 209 tert-Amyl Methyl Ether 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 1,2-Dichloropropane 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 Bromodichloromethane 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Trichloroethene 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 1,4-Dioxane 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 Isooctane 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Methyl Methacrylate 2.08 416 41.6 8.32 2.08 0.1664 0.208 0.416 0.832 2.08 10.40 52.00 104.0 208 n-Heptane 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 cis-1,3-Dichloropropene 1.12 224 22.4 4.48 1.12 0.0896 0.112 0.224 0.448 1.12 5.60 28.00 56.0 112

1 of 2 Date Updated: 07/14/15 Q:\TO15 Std. Concentrations\MS09 Std. Conc\2016\R9042116\ICAL Conc. (Primary Source) Version: 0 Primary Source Standards Concentrations (Working & Initial Calibration) 1ng/L Std. ID: 4ng/L Std. ID: S29-04201403 20ng/L Std. ID: S29-04131608

200ng/L Std. ID: S29-04131603 Working STD Dilution Factors: 5 50 250 1000 Conc.(ng/L): 4444 20 20 200 200 200 Source Std. Primary Working Standards Injection (L): 0.020 0.025 0.050 0.100 0.050 0.25 0.125 0.25 0.50 Compounds mg/m3 200ng/L 20ng/L 4ng/L 1ng/L ICAL Points: 0.08ng 0.1ng 0.2ng 0.4ng 1ng 5ng 25ng 50ng 100ng 4-Methyl-2-pentanone 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 trans-1,3-Dichloropropene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 1,1,2-Trichloroethane 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 Toluene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 2-Hexanone 1.11 222 22.2 4.44 1.11 0.0888 0.111 0.222 0.444 1.11 5.55 27.75 55.5 111 Dibromochloromethane 1.10 220 22.0 4.40 1.10 0.0880 0.110 0.220 0.440 1.10 5.50 27.50 55.0 110 1,2-Dibromoethane 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 n-Butyl Acetate 1.11 222 22.2 4.44 1.11 0.0888 0.111 0.222 0.444 1.11 5.55 27.75 55.5 111 n-Octane 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Tetrachloroethene 0.99 198 19.8 3.96 0.99 0.0792 0.099 0.198 0.396 0.99 4.95 24.75 49.5 99 Chlorobenzene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Ethylbenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 m-&p-Xylene 2.08 416 41.6 8.32 2.08 0.1664 0.208 0.416 0.832 2.08 10.40 52.00 104.0 208 Bromoform 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Styrene 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 o-Xylene 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102 n-Nonane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101 1,1,2,2-Tetrachloroethane 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 Cumene 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101 alpha-Pinene 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 n-Propylbenzene 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 3-Ethyltoluene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 4-Ethyltoluene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 105 of 156 105 1,3,5-Trimethylbenzene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 alpha-Methylstyrene 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 2-Ethyltoluene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 1,2,4-Trimethylbenzene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 n-Decane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101 Benzyl Chloride 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 1,3-Dichlorobenzene 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108 1,4-Dichlorobenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 sec-Butylbenzene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106 p-Isopropyltoluene 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 1,2,3-Trimethylbenzene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 1,2-Dichlorobenzene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 d-Limonene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 1,2-Dibromo-3-chloropropane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 n-Undecane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101 1,2,4-Trichlorobenzene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 Naphthalene 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100 n-Dodecane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104 Hexachloro-1,3-butadiene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107 Methacrylonitrile 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103 Cyclohexanone 1.12 224 22.4 4.48 1.12 0.0896 0.112 0.224 0.448 1.12 5.60 28.00 56.0 112 tert-Butylbenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105 n-Butylbenzene 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108

2 of 2 Date Updated: 07/14/15 Q:\TO15 Std. Concentrations\MS09 Std. Conc\2016\R9042116\ICAL Conc. (Primary Source) Version: 0 Calibration Status Report MS09

Method : I:\MS09\Methods\R9042116.M (RTE Integrator) Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration

# ID Conc ISTD Path\File Conc ------1 0.08 0 13 I:\MS09\Data\2016_04\21\04211621.D 2 0.10 0 13 I:\MS09\Data\2016_04\21\04211622.D 3 0.20 0 13 I:\MS09\Data\2016_04\21\04211623.D 4 0.40 0 13 I:\MS09\Data\2016_04\21\04211624.D 5 1.0 1 13 I:\MS09\Data\2016_04\21\04211625.D 6 5.0 5 13 I:\MS09\Data\2016_04\21\04211626.D 7 25 26 13 I:\MS09\Data\2016_04\21\04211627.D 8 50 52 13 I:\MS09\Data\2016_04\21\04211628.D 9 100 103 13 I:\MS09\Data\2016_04\21\04211629.D

# ID Update Time Quant Time Acquisition Time ------1 0.08 Apr 22 10:12 2016 Apr 22 10:06 2016 21 Apr 2016 23:06 2 0.10 Apr 22 10:12 2016 Apr 22 10:03 2016 21 Apr 2016 23:40 3 0.20 Apr 22 10:12 2016 Apr 22 10:01 2016 22 Apr 2016 00:14 4 0.40 Apr 22 10:13 2016 Apr 22 10:00 2016 22 Apr 2016 00:48 5 1.0 Apr 22 10:13 2016 Apr 22 09:59 2016 22 Apr 2016 1:22 6 5.0 Apr 22 10:13 2016 Apr 22 09:58 2016 22 Apr 2016 1:56 7 25 Apr 22 10:13 2016 Apr 22 09:55 2016 22 Apr 2016 2:30 8 50 Apr 22 10:14 2016 Apr 22 10:08 2016 22 Apr 2016 3:04 9 100 Apr 22 10:14 2016 Apr 22 10:09 2016 22 Apr 2016 3:37

R9042116.M Fri Apr 22 10:59:42 2016

106 of 156 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211621.D Acq On : 21 Apr 2016 23:06 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:06:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 126819 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.87 114 661613 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 283935 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 206844 12.731 ng -0.03 Spiked Amount 12.500 Range 70 - 130 Recovery = 101.84% 57) Toluene-d8 (SS2) 13.31 98 665303 12.459 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.68% 73) Bromofluorobenzene (SS3) 16.84 174 218104 11.395 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 91.12%

Target Compounds Qvalue 2) Propene 3.72 42 1761 0.156 ng 99 3) Dichlorodifluoromethan... 3.81 85 2895 0.124 ng # 93 4) Chloromethane 4.01 50 2409 0.172 ng 97 5) 1,2-Dichloro-1,1,2,2-t... 4.16 135 1521 0.157 ng 92 6) Vinyl Chloride 4.28 62 1982 0.132 ng 94 7) 1,3-Butadiene 4.46 54 840 0.121 ng 89 8) Bromomethane 4.75 94 1153 0.115 ng 97 9) Chloroethane 4.96 64 1097 0.127 ng # 43 10) Ethanol 5.18 45 4674 0.447 ng 74 11) Acetonitrile 5.41 41 2889 0.110 ng # 1 12) Acrolein 5.52 56 699 0.097 ng 87 13) Acetone 5.65 58 6634 0.600 ng 98 14) Trichlorofluoromethane 5.81 101 2492 0.148 ng 91 15) 2-Propanol (Isopropanol) 6.00 45 6856 0.180 ng 96 16) Acrylonitrile 6.19 53 807 N.D. 17) 1,1-Dichloroethene 6.49 96 1364 0.127 ng 97 18) 2-Methyl-2-Propanol (t... 6.67 59 6980 0.203 ng 89 19) Methylene Chloride 6.63 84 3924 0.291 ng 91 20) 3-Chloro-1-propene (Al... 6.76 41 1954 0.130 ng 78 21) Trichlorotrifluoroethane 6.95 151 1230m 0.133 ng 22) Carbon Disulfide 6.92 76 4055 0.095 ng # 74 23) trans-1,2-Dichloroethene 7.65 61 1718 0.090 ng 92 24) 1,1-Dichloroethane 7.85 63 2595 0.105 ng 94 25) Methyl tert-Butyl Ether 7.98 73 4269 0.106 ng 96 26) Vinyl Acetate 8.06 86 796 0.326 ng # 1 27) 2-Butanone (MEK) 8.32 72 730 0.078 ng # 28 28) cis-1,2-Dichloroethene 8.72 61 1835 0.106 ng 96 29) Diisopropyl Ether 9.01 87 1297 0.106 ng # 94 30) Ethyl Acetate 9.01 61 860 0.167 ng 92 31) n-Hexane 8.99 57 2639 0.108 ng # 87 32) Chloroform 9.03 83 2637 0.116 ng 91 34) Tetrahydrofuran (THF) 9.48 72 1066 0.108 ng # 76 35) Ethyl tert-Butyl Ether 9.55 87 1742 0.110 ng 98 36) 1,2-Dichloroethane 9.79 62 1529 0.097 ng 97 38) 1,1,1-Trichloroethane 10.05 97 1902 0.096 ng 96 39) Isopropyl Acetate 10.45 61 1847 0.224 ng # 88 40) 1-Butanol 10.49 56 2157 0.150 ng 85 41) Benzene 10.51 78 8576 0.155 ng 97 42) Carbon Tetrachloride 10.67 117 1673 0.115 ng 87 43) Cyclohexane 10.79 84 4616 0.221 ng 94 44) tert-Amyl Methyl Ether 11.14 73 4230 0.109 ng 97 45) 1,2-Dichloropropane 11.33 63 1520 0.104 ng 98 46) Bromodichloromethane 11.51 83 1835 0.107 ng 86 47) Trichloroethene 11.57 130 1397 0.086 ng 95 48) 1,4-Dioxane 11.59 88 842 0.074 ng 90 49) 2,2,4-Trimethylpentane... 11.63 57 6865 0.110 ng 96 107 of 156 R9042116.M Fri Apr 22 10:07:38 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211621.D Acq On : 21 Apr 2016 23:06 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:06:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.79 100 856 0.149 ng # 69 51) n-Heptane 11.90 71 1505 0.107 ng # 85 52) cis-1,3-Dichloropropene 12.43 75 1896 0.085 ng # 43 53) 4-Methyl-2-pentanone 12.49 58 1171 0.086 ng # 79 54) trans-1,3-Dichloropropene 12.95 75 1153 0.061 ng # 43 55) 1,1,2-Trichloroethane 13.11 97 1252 0.092 ng 95 58) Toluene 13.41 91 6816 0.104 ng 100 59) 2-Hexanone 13.68 43 2620 0.091 ng 97 60) Dibromochloromethane 13.82 129 1309 0.087 ng 90 61) 1,2-Dibromoethane 14.08 107 1191 0.080 ng 94 62) n-Butyl Acetate 14.32 43 3226 0.099 ng # 87 63) n-Octane 14.44 57 1357 0.105 ng 96 64) Tetrachloroethene 14.57 166 1419 0.088 ng 98 65) Chlorobenzene 15.27 112 3845 0.105 ng 97 66) Ethylbenzene 15.67 91 6427 0.101 ng 96 67) m- & p-Xylenes 15.86 91 9960 0.187 ng 99 68) Bromoform 15.92 173 1011 0.078 ng # 28 69) Styrene 16.25 104 3383 0.095 ng 95 70) o-Xylene 16.36 91 5253 0.099 ng 89 71) n-Nonane 16.61 43 3062 0.104 ng 97 72) 1,1,2,2-Tetrachloroethane 16.34 83 2106 0.092 ng 95 74) Cumene 16.99 105 6309 0.094 ng 99 75) alpha-Pinene 17.40 93 3317 0.104 ng # 58 76) n-Propylbenzene 17.52 91 7619 0.092 ng 96 77) 3-Ethyltoluene 17.63 105 6542 0.099 ng 90 78) 4-Ethyltoluene 17.68 105 5759 0.091 ng 99 79) 1,3,5-Trimethylbenzene 17.76 105 5110 0.092 ng 98 80) alpha-Methylstyrene 17.91 118 2183 0.081 ng 97 81) 2-Ethyltoluene 17.95 105 6064 0.094 ng 97 82) 1,2,4-Trimethylbenzene 18.19 105 4899 0.088 ng 94 83) n-Decane 18.31 57 3096 0.097 ng 95 84) Benzyl Chloride 18.32 91 2371 0.059 ng # 55 85) 1,3-Dichlorobenzene 18.34 146 2211 0.076 ng 97 86) 1,4-Dichlorobenzene 18.41 146 2224 0.072 ng 98 87) sec-Butylbenzene 18.47 105 6496 0.088 ng 98 88) 4-Isopropyltoluene (p-... 18.64 119 5682 0.082 ng 92 89) 1,2,3-Trimethylbenzene 18.64 105 4933 0.086 ng 98 90) 1,2-Dichlorobenzene 18.77 146 2207 0.074 ng 97 91) d-Limonene 18.80 68 1863 0.086 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.23 157 445 N.D. 93) n-Undecane 19.65 57 2752 0.080 ng 90 94) 1,2,4-Trichlorobenzene 20.59 180 978 N.D. 95) Naphthalene 20.71 128 3121 N.D. 96) n-Dodecane 20.74 57 2216 0.071 ng 85 97) Hexachlorobutadiene 21.07 225 899 0.061 ng 100 98) Cyclohexanone 16.03 55 1665 0.090 ng # 90 99) tert-Butylbenzene 18.18 119 5043 0.094 ng 96 100) n-Butylbenzene 19.08 91 5087 0.087 ng 96 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

108 of 156 R9042116.M Fri Apr 22 10:07:38 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211621.D Acq On : 21 Apr 2016 23:06 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:06:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211621.D\data.ms

1000000

950000

900000

850000

800000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR 750000 1,4-Difluorobenzene (IS2),IR

700000 Bromofluorobenzene (SS3),S

650000

600000

550000

500000

450000

400000

350000 Bromochloromethane (IS1),IR

300000 1,2-Dichloroethane-d4(SS1),S

250000

200000

150000

100000 n-Hexane,T tert-Butylbenzene,T 1,2,4-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T 1,2,3-Trimethylbenzene,T EthylDiisopropyl Acetate,T Ether,T Acetone,T Cyclohexane,T Benzene,T n-Decane,T Chlorobenzene,T m- & p-Xylenes,T sec-Butylbenzene,T n-Butylbenzene,T Cumene,T 3-Ethyltoluene,T 2-Ethyltoluene,T d-Limonene,T n-Propylbenzene,T Propene,T 4-Ethyltoluene,T Toluene,T o-Xylene,T Methylene Chloride,T alpha-Pinene,T n-Nonane,T Chloroform,T n-Octane,T Isopropyl Acetate,T n-Undecane,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 1,3,5-Trimethylbenzene,T 1-Butanol,T 2,2,4-Trimethylpentane (Isooctane),T alpha-Methylstyrene,T Benzyl Chloride,T n-Dodecane,T Dichlorodifluoromethane (CFC 12),T Ethylbenzene,T Vinyl Acetate,T n-Heptane,T 1,3-Dichlorobenzene,T Styrene,T Ethyl tert-Butyl Ether,T 1,2-Dichlorobenzene,T Hexachlorobutadiene,T Vinyl Chloride,T Tetrachloroethene,T tert-Amyl Methyl Ether,T Methyl Methacrylate,T Tetrahydrofuran (THF),T Chloromethane,T 1,4-Dichlorobenzene,T n-Butyl Acetate,T 1,3-Butadiene,T Methyl tert-Butyl Ether,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Trichloroethene,T Carbon Disulfide,T Trichlorotrifluoroethane,T Cyclohexanone,T 1,1,2,2-Tetrachloroethane,T 4-Methyl-2-pentanone,T 1,2-Dichloroethane,T 1,1-Dichloroethene,T Trichlorofluoromethane,T 1,2-Dichloropropane,T 1,1,2-Trichloroethane,T 2-Propanol (Isopropanol),T 2-Hexanone,T cis-1,3-Dichloropropene,T 1,1,1-Trichloroethane,T 1,4-Dioxane,T 2-Butanone (MEK),T cis-1,2-Dichloroethene,T Bromomethane,T 1,1-Dichloroethane,T trans-1,2-Dichloroethene,T Carbon Tetrachloride,T 3-Chloro-1-propene (Allyl Chloride),T Ethanol,T Dibromochloromethane,T Bromodichloromethane,T Chloroethane,T 1,2-Dibromoethane,T Acrolein,T Bromoform,T trans-1,3-Dichloropropene,T 50000 Acetonitrile,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00109 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:07:40 2016 Page: 3 Quantitation Report (Qedit)

Data File: I:\MS09\Data\2016_04\21\04211621.D Acq On : 21 Apr 2016 23:06 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:05:23 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance Ion 150.90 (150.60 to 151.60): 04211621.D\data.ms Ion 100.90 (100.60 to 101.60): 04211621.D\data.ms 1000

800 |

600 6.935|

| 400 |

200 | | | | | | | | 0

Time--> 6.00 6.10 6.20 6.30 6.40 6.50 6.60 6.70 6.80 6.90 7.00 7.10 7.20 7.30 7.40 7.50 7.60 7.70 7.80 7.90 Abundance Scan 674 (6.935 min): 04211621.D\data.ms 76

1000

800

101 600 151

400

85 44 200

0 m/z--> 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 TIC: 04211621.D\data.ms

(21) Trichlorotrifluoroethane (T)

6.935min (-0.005) 0.07ng

response 608

Ion Exp% Act%

150.90 100 100

100.90 126.10 245.72#

0.00 0.00 0.00

0.00 0.00 0.00

110 of 156 R9042116.M Fri Apr 22 10:06:01 2016 Page: 1 Quantitation Report (Qedit)

Data File: I:\MS09\Data\2016_04\21\04211621.D Acq On : 21 Apr 2016 23:06 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:05:23 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance Ion 150.90 (150.60 to 151.60): 04211621.D\data.ms Ion 100.90 (100.60 to 101.60): 04211621.D\data.ms 1000

800 |

600 6.945|

| 400 |

200 | | | | | | | | 0

Time--> 6.00 6.10 6.20 6.30 6.40 6.50 6.60 6.70 6.80 6.90 7.00 7.10 7.20 7.30 7.40 7.50 7.60 7.70 7.80 7.90 Abundance Scan 676 (6.945 min): 04211621.D\data.ms 700 76 101 600 151

500

400

300 85

200 44

100

0 m/z--> 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 TIC: 04211621.D\data.ms

(21) Trichlorotrifluoroethane (T)

6.945min (+0.005) 0.13ng m

response 1230

Ion Exp% Act%

150.90 100 100

100.90 126.10 121.46

0.00 0.00 0.00

0.00 0.00 0.00

111 of 156 R9042116.M Fri Apr 22 10:06:10 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211622.D Acq On : 21 Apr 2016 23:40 Operator: SC Sample : 0.10ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.88 130 125303 12.500 ng -0.04 37) 1,4-Difluorobenzene (IS2) 10.87 114 654697 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 277954 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 204410 12.733 ng -0.03 Spiked Amount 12.500 Range 70 - 130 Recovery = 101.84% 57) Toluene-d8 (SS2) 13.31 98 658562 12.598 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.80% 73) Bromofluorobenzene (SS3) 16.84 174 214886 11.468 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 91.76%

Target Compounds Qvalue 2) Propene 3.71 42 1885 0.169 ng 94 3) Dichlorodifluoromethan... 3.81 85 3524 0.152 ng # 93 4) Chloromethane 4.01 50 2997 0.217 ng 95 5) 1,2-Dichloro-1,1,2,2-t... 4.16 135 1772 0.185 ng 96 6) Vinyl Chloride 4.28 62 2474 0.167 ng 95 7) 1,3-Butadiene 4.45 54 911 0.133 ng # 83 8) Bromomethane 4.74 94 1331 0.135 ng 85 9) Chloroethane 4.96 64 1380 0.161 ng # 43 10) Ethanol 5.16 45 5032 0.487 ng 83 11) Acetonitrile 5.41 41 3319 0.128 ng # 21 12) Acrolein 5.51 56 824 0.116 ng # 64 13) Acetone 5.65 58 7921 0.725 ng 95 14) Trichlorofluoromethane 5.80 101 2783 0.168 ng 97 15) 2-Propanol (Isopropanol) 5.99 45 8814 0.234 ng 96 16) Acrylonitrile 6.15 53 1163 0.067 ng # 56 17) 1,1-Dichloroethene 6.49 96 1400 0.132 ng # 69 18) 2-Methyl-2-Propanol (t... 6.65 59 8577 0.252 ng 93 19) Methylene Chloride 6.62 84 4061 0.305 ng 98 20) 3-Chloro-1-propene (Al... 6.75 41 2236 0.151 ng 88 21) Trichlorotrifluoroethane 6.95 151 1413 0.155 ng 97 22) Carbon Disulfide 6.91 76 5485 0.130 ng # 74 23) trans-1,2-Dichloroethene 7.64 61 2108 0.111 ng # 56 24) 1,1-Dichloroethane 7.85 63 3324 0.136 ng 96 25) Methyl tert-Butyl Ether 7.97 73 5356 0.135 ng 97 26) Vinyl Acetate 8.04 86 1193 0.495 ng # 92 27) 2-Butanone (MEK) 8.31 72 1020 0.111 ng # 56 28) cis-1,2-Dichloroethene 8.73 61 2405 0.140 ng 86 29) Diisopropyl Ether 8.99 87 884 0.073 ng # 1 30) Ethyl Acetate 9.00 61 1111 0.218 ng 93 31) n-Hexane 8.98 57 3425 0.142 ng # 88 32) Chloroform 9.03 83 2968 0.132 ng 96 34) Tetrahydrofuran (THF) 9.48 72 1244 0.128 ng # 78 35) Ethyl tert-Butyl Ether 9.55 87 1877 0.120 ng # 78 36) 1,2-Dichloroethane 9.79 62 1858 0.119 ng 98 38) 1,1,1-Trichloroethane 10.05 97 2249 0.115 ng 94 39) Isopropyl Acetate 10.45 61 2295 0.281 ng 95 40) 1-Butanol 10.49 56 2718 0.191 ng # 68 41) Benzene 10.51 78 9778 0.178 ng 99 42) Carbon Tetrachloride 10.66 117 2063 0.143 ng 97 43) Cyclohexane 10.80 84 5551 0.268 ng 99 44) tert-Amyl Methyl Ether 11.14 73 5031 0.130 ng 96 45) 1,2-Dichloropropane 11.34 63 1734 0.119 ng 96 46) Bromodichloromethane 11.52 83 2098 0.123 ng 98 47) Trichloroethene 11.56 130 1748 0.109 ng 98 48) 1,4-Dioxane 11.59 88 1283 0.114 ng 86 49) 2,2,4-Trimethylpentane... 11.64 57 8516 0.138 ng 96 112 of 156 R9042116.M Fri Apr 22 10:05:05 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211622.D Acq On : 21 Apr 2016 23:40 Operator: SC Sample : 0.10ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 1088 0.192 ng # 86 51) n-Heptane 11.90 71 1883 0.136 ng # 88 52) cis-1,3-Dichloropropene 12.43 75 2348 0.106 ng 94 53) 4-Methyl-2-pentanone 12.47 58 1527 0.113 ng # 82 54) trans-1,3-Dichloropropene 12.95 75 1470 0.079 ng # 43 55) 1,1,2-Trichloroethane 13.12 97 1556 0.115 ng 96 58) Toluene 13.41 91 7933 0.124 ng 97 59) 2-Hexanone 13.68 43 3204 0.114 ng 95 60) Dibromochloromethane 13.83 129 1771 0.121 ng 94 61) 1,2-Dibromoethane 14.08 107 1602 0.110 ng 95 62) n-Butyl Acetate 14.32 43 3640 0.115 ng 99 63) n-Octane 14.44 57 1679 0.132 ng # 85 64) Tetrachloroethene 14.57 166 1790 0.113 ng 91 65) Chlorobenzene 15.26 112 4587 0.128 ng 96 66) Ethylbenzene 15.68 91 7497 0.120 ng 97 67) m- & p-Xylenes 15.86 91 11965 0.229 ng 100 68) Bromoform 15.93 173 1255 0.099 ng 81 69) Styrene 16.25 104 3930 0.113 ng 99 70) o-Xylene 16.37 91 6211 0.119 ng 96 71) n-Nonane 16.61 43 3916 0.135 ng 94 72) 1,1,2,2-Tetrachloroethane 16.34 83 2478 0.110 ng 97 74) Cumene 16.99 105 7598 0.115 ng 98 75) alpha-Pinene 17.40 93 3768 0.121 ng # 24 76) n-Propylbenzene 17.52 91 9219 0.113 ng 97 77) 3-Ethyltoluene 17.63 105 7367 0.114 ng 98 78) 4-Ethyltoluene 17.67 105 6880 0.112 ng 96 79) 1,3,5-Trimethylbenzene 17.75 105 5921 0.109 ng 96 80) alpha-Methylstyrene 17.92 118 2739 0.103 ng 96 81) 2-Ethyltoluene 17.95 105 6995 0.110 ng 99 82) 1,2,4-Trimethylbenzene 18.19 105 5903 0.109 ng 96 83) n-Decane 18.31 57 3487 0.111 ng 94 84) Benzyl Chloride 18.32 91 2838 0.073 ng 91 85) 1,3-Dichlorobenzene 18.34 146 2905 0.103 ng 99 86) 1,4-Dichlorobenzene 18.41 146 2781 0.092 ng 97 87) sec-Butylbenzene 18.48 105 8070 0.112 ng 99 88) 4-Isopropyltoluene (p-... 18.64 119 6728 0.099 ng 93 89) 1,2,3-Trimethylbenzene 18.64 105 5907 0.105 ng 99 90) 1,2-Dichlorobenzene 18.77 146 2830 0.097 ng 97 91) d-Limonene 18.80 68 2447 0.115 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.24 157 696 0.068 ng # 79 93) n-Undecane 19.65 57 3181 0.094 ng 92 94) 1,2,4-Trichlorobenzene 20.59 180 1410 0.067 ng # 86 95) Naphthalene 20.71 128 3837 0.052 ng # 71 96) n-Dodecane 20.74 57 2528 0.082 ng 90 97) Hexachlorobutadiene 21.07 225 1042 0.072 ng 99 98) Cyclohexanone 16.03 55 2088 0.115 ng 94 99) tert-Butylbenzene 18.18 119 5957 0.113 ng 99 100) n-Butylbenzene 19.08 91 5877 0.103 ng 98 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

113 of 156 R9042116.M Fri Apr 22 10:05:05 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211622.D Acq On : 21 Apr 2016 23:40 Operator: SC Sample : 0.10ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:03:59 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211622.D\data.ms

1000000

950000

900000

850000

800000 Toluene-d8 (SS2),S

750000 Chlorobenzene-d5 (IS3),IR 1,4-Difluorobenzene (IS2),IR

700000 Bromofluorobenzene (SS3),S 650000

600000

550000

500000

450000

400000

350000 Bromochloromethane (IS1),IR 300000 1,2-Dichloroethane-d4(SS1),S

250000

200000

150000

100000 n-Hexane,T Diisopropyl Ether,T 1,2,4-Trimethylbenzene,T Chlorobenzene,T 4-Isopropyltoluene (p-Cymene),T Ethyl Acetate,T tert-Butylbenzene,T 1,2,3-Trimethylbenzene,T Acetone,T Cyclohexane,T Benzene,T m- & p-Xylenes,T n-Decane,T d-Limonene,T Cumene,T n-Butylbenzene,T 4-Ethyltoluene,T 1,3,5-Trimethylbenzene,T n-Undecane,T n-Propylbenzene,T 3-Ethyltoluene,T n-Nonane,T alpha-Pinene,T sec-Butylbenzene,T Propene,T 2-Ethyltoluene,T Isopropyl Acetate,T Toluene,T n-Octane,T o-Xylene,T 2,2,4-Trimethylpentane (Isooctane),T Ethylbenzene,T 1-Butanol,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Methylene Chloride,T n-Heptane,T Benzyl Chloride,T n-Dodecane,T Methyl Methacrylate,T alpha-Methylstyrene,T Vinyl Acetate,T Chloroform,T Dichlorodifluoromethane (CFC 12),T 1,3-Dichlorobenzene,T Styrene,T tert-Amyl Methyl Ether,T 1,2-Dichlorobenzene,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Hexachlorobutadiene,T Ethyl tert-Butyl Ether,T 1,4-Dichlorobenzene,T 4-Methyl-2-pentanone,T Tetrachloroethene,T Vinyl Chloride,T Naphthalene,T 1,3-Butadiene,T n-Butyl Acetate,T Chloromethane,T Tetrahydrofuran (THF),T Methyl tert-Butyl Ether,T Trichloroethene,T 1,1,2,2-Tetrachloroethane,T Trichlorotrifluoroethane,T Cyclohexanone,T 1,1,2-Trichloroethane,T 2-Hexanone,T cis-1,2-Dichloroethene,T 1,1-Dichloroethene,T Carbon Tetrachloride,T Trichlorofluoromethane,T 1,2-Dichloroethane,T 1,1-Dichloroethane,T 2-Propanol (Isopropanol),T 1,2-Dichloropropane,T cis-1,3-Dichloropropene,T 1,1,1-Trichloroethane,T 2-Butanone (MEK),T 1,2,4-Trichlorobenzene,T 3-Chloro-1-propene (Allyl Chloride),T Carbon Disulfide,T trans-1,2-Dichloroethene,T Bromomethane,T 1,2-Dibromo-3-Chloropropane,T Ethanol,T 1,2-Dibromoethane,T Bromodichloromethane,T Dibromochloromethane,T Bromoform,T 1,4-Dioxane,T trans-1,3-Dichloropropene,T Chloroethane,T Acrolein,T Acetonitrile,T 50000 Acrylonitrile,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00114 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:05:06 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211623.D Acq On : 22 Apr 2016 00:14 Operator: SC Sample : 0.20ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:01:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 125959 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.87 114 655466 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 276866 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 204866 12.695 ng -0.03 Spiked Amount 12.500 Range 70 - 130 Recovery = 101.60% 57) Toluene-d8 (SS2) 13.31 98 656602 12.610 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.88% 73) Bromofluorobenzene (SS3) 16.84 174 213941 11.463 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 91.68%

Target Compounds Qvalue 2) Propene 3.71 42 3489 0.310 ng 97 3) Dichlorodifluoromethan... 3.80 85 6887 0.296 ng # 96 4) Chloromethane 4.00 50 5451 0.393 ng 96 5) 1,2-Dichloro-1,1,2,2-t... 4.16 135 3615 0.376 ng 95 6) Vinyl Chloride 4.27 62 4427 0.297 ng 99 7) 1,3-Butadiene 4.44 54 1907 0.276 ng 94 8) Bromomethane 4.74 94 2810 0.283 ng 96 9) Chloroethane 4.95 64 2530 0.294 ng 93 10) Ethanol 5.15 45 10954 1.055 ng 96 11) Acetonitrile 5.38 41 6696 0.257 ng # 53 12) Acrolein 5.49 56 1556 0.218 ng 100 13) Acetone 5.64 58 14407 1.311 ng 96 14) Trichlorofluoromethane 5.80 101 5359 0.321 ng 99 15) 2-Propanol (Isopropanol) 5.97 45 16284 0.430 ng 98 16) Acrylonitrile 6.14 53 2669 0.154 ng 92 17) 1,1-Dichloroethene 6.49 96 3286 0.309 ng 96 18) 2-Methyl-2-Propanol (t... 6.65 59 16498 0.483 ng 96 19) Methylene Chloride 6.62 84 5767 0.431 ng 96 20) 3-Chloro-1-propene (Al... 6.76 41 5021 0.337 ng 87 21) Trichlorotrifluoroethane 6.95 151 2762 0.301 ng 97 22) Carbon Disulfide 6.91 76 10634 0.250 ng 94 23) trans-1,2-Dichloroethene 7.65 61 4048 0.212 ng 99 24) 1,1-Dichloroethane 7.85 63 6198 0.251 ng 98 25) Methyl tert-Butyl Ether 7.96 73 9994 0.250 ng 100 26) Vinyl Acetate 8.04 86 2461 1.016 ng # 90 27) 2-Butanone (MEK) 8.30 72 2109 0.228 ng # 81 28) cis-1,2-Dichloroethene 8.73 61 4443 0.258 ng 94 29) Diisopropyl Ether 8.99 87 3440 0.284 ng # 68 30) Ethyl Acetate 8.99 61 2342 0.457 ng 93 31) n-Hexane 8.98 57 6253 0.257 ng 98 32) Chloroform 9.03 83 5683 0.251 ng 100 34) Tetrahydrofuran (THF) 9.47 72 2371 0.243 ng 90 35) Ethyl tert-Butyl Ether 9.54 87 3723 0.236 ng # 88 36) 1,2-Dichloroethane 9.79 62 3865 0.246 ng 98 38) 1,1,1-Trichloroethane 10.05 97 4757 0.243 ng 98 39) Isopropyl Acetate 10.45 61 4083 0.500 ng # 91 40) 1-Butanol 10.48 56 4727 0.333 ng # 66 41) Benzene 10.51 78 17409 0.317 ng 100 42) Carbon Tetrachloride 10.66 117 3825 0.265 ng 97 43) Cyclohexane 10.79 84 10367 0.500 ng 97 44) tert-Amyl Methyl Ether 11.13 73 9727 0.252 ng 97 45) 1,2-Dichloropropane 11.33 63 3570 0.245 ng 99 46) Bromodichloromethane 11.51 83 4303 0.252 ng 99 47) Trichloroethene 11.58 130 3424 0.213 ng 96 48) 1,4-Dioxane 11.58 88 2294 0.204 ng 97 49) 2,2,4-Trimethylpentane... 11.64 57 15423 0.249 ng 100 115 of 156 R9042116.M Fri Apr 22 10:03:01 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211623.D Acq On : 22 Apr 2016 00:14 Operator: SC Sample : 0.20ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:01:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 2344 0.413 ng 99 51) n-Heptane 11.90 71 3688 0.265 ng 97 52) cis-1,3-Dichloropropene 12.43 75 4499 0.203 ng 100 53) 4-Methyl-2-pentanone 12.48 58 2892 0.214 ng 90 54) trans-1,3-Dichloropropene 12.96 75 3322 0.178 ng 96 55) 1,1,2-Trichloroethane 13.12 97 3083 0.228 ng 98 58) Toluene 13.41 91 14397 0.226 ng 100 59) 2-Hexanone 13.68 43 6332 0.225 ng 98 60) Dibromochloromethane 13.82 129 3314 0.227 ng 99 61) 1,2-Dibromoethane 14.08 107 3174 0.218 ng 99 62) n-Butyl Acetate 14.32 43 7417 0.234 ng 96 63) n-Octane 14.44 57 3031 0.240 ng 96 64) Tetrachloroethene 14.57 166 3284 0.208 ng 97 65) Chlorobenzene 15.27 112 8516 0.238 ng 99 66) Ethylbenzene 15.67 91 14270 0.230 ng 99 67) m- & p-Xylenes 15.86 91 22090 0.425 ng 99 68) Bromoform 15.92 173 2598 0.207 ng 94 69) Styrene 16.25 104 8035 0.232 ng 100 70) o-Xylene 16.36 91 11792 0.227 ng 97 71) n-Nonane 16.61 43 6962 0.241 ng 97 72) 1,1,2,2-Tetrachloroethane 16.34 83 4872 0.217 ng 98 74) Cumene 16.99 105 14175 0.216 ng 97 75) alpha-Pinene 17.40 93 7399 0.238 ng 85 76) n-Propylbenzene 17.52 91 17102 0.211 ng 97 77) 3-Ethyltoluene 17.63 105 13099 0.204 ng 97 78) 4-Ethyltoluene 17.67 105 13627 0.222 ng 97 79) 1,3,5-Trimethylbenzene 17.75 105 11323 0.209 ng 100 80) alpha-Methylstyrene 17.92 118 4963 0.188 ng 96 81) 2-Ethyltoluene 17.95 105 13596 0.215 ng 99 82) 1,2,4-Trimethylbenzene 18.19 105 10699 0.198 ng 99 83) n-Decane 18.31 57 6968 0.223 ng 94 84) Benzyl Chloride 18.32 91 5612 0.144 ng 98 85) 1,3-Dichlorobenzene 18.34 146 5371 0.190 ng 99 86) 1,4-Dichlorobenzene 18.41 146 5135 0.171 ng 98 87) sec-Butylbenzene 18.47 105 15853 0.221 ng 98 88) 4-Isopropyltoluene (p-... 18.64 119 13103 0.193 ng 94 89) 1,2,3-Trimethylbenzene 18.64 105 10959 0.195 ng 94 90) 1,2-Dichlorobenzene 18.77 146 5236 0.180 ng 99 91) d-Limonene 18.79 68 4660 0.219 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.23 157 1445 0.142 ng 93 93) n-Undecane 19.65 57 5499 0.163 ng 98 94) 1,2,4-Trichlorobenzene 20.59 180 2507 0.120 ng # 95 95) Naphthalene 20.71 128 7870 0.108 ng 97 96) n-Dodecane 20.74 57 4494 0.147 ng 90 97) Hexachlorobutadiene 21.07 225 2324 0.161 ng 86 98) Cyclohexanone 16.03 55 3729 0.207 ng 96 99) tert-Butylbenzene 18.18 119 11154 0.212 ng 100 100) n-Butylbenzene 19.08 91 11524 0.203 ng 95 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

116 of 156 R9042116.M Fri Apr 22 10:03:01 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211623.D Acq On : 22 Apr 2016 00:14 Operator: SC Sample : 0.20ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:01:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211623.D\data.ms

1000000

950000

900000

850000

800000 Toluene-d8 (SS2),S

750000 Chlorobenzene-d5 (IS3),IR 1,4-Difluorobenzene (IS2),IR 700000 Bromofluorobenzene (SS3),S

650000

600000

550000

500000

450000

400000

350000 Bromochloromethane (IS1),IR 300000 1,2-Dichloroethane-d4(SS1),S

250000

200000

150000

100000 EthylDiisopropyl Acetate,T Ether,T tert-Butylbenzene,T 1,2,4-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T 1,2,3-Trimethylbenzene,T n-Hexane,T Acetone,T Cyclohexane,T 3-Ethyltoluene,T n-Decane,T sec-Butylbenzene,T Benzene,T m- & p-Xylenes,T 1,3,5-Trimethylbenzene,T d-Limonene,T 2-Ethyltoluene,T n-Propylbenzene,T n-Butylbenzene,T Chlorobenzene,T o-Xylene,T 4-Ethyltoluene,T Cumene,T n-Nonane,T alpha-Pinene,T Isopropyl Acetate,T Toluene,T n-Undecane,T Ethylbenzene,T Benzyl Chloride,T Vinyl Acetate,T 2,2,4-Trimethylpentane (Isooctane),T n-Octane,T alpha-Methylstyrene,T n-Heptane,T Methyl Methacrylate,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T n-Dodecane,T Propene,T 1,3-Dichlorobenzene,T Styrene,T 1,2-Dichlorobenzene,T Hexachlorobutadiene,T Dichlorodifluoromethane (CFC 12),T Methylene Chloride,T tert-Amyl Methyl Ether,T Chloroform,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Ethyl tert-Butyl Ether,T 1,4-Dichlorobenzene,T 1,1,2,2-Tetrachloroethane,T 1-Butanol,T Tetrachloroethene,T Methyl tert-Butyl Ether,T 1,4-Dioxane,TTrichloroethene,T 4-Methyl-2-pentanone,T n-Butyl Acetate,T Naphthalene,T 2-Hexanone,T 1,2-Dichloropropane,T Tetrahydrofuran (THF),T Cyclohexanone,T Trichlorotrifluoroethane,T Chloromethane,T 1,1-Dichloroethene,T Vinyl Chloride,T 1,1,2-Trichloroethane,T 1,2,4-Trichlorobenzene,T Carbon Disulfide,T 1,1,1-Trichloroethane,T Trichlorofluoromethane,T 2-Butanone (MEK),T 1,3-Butadiene,T 3-Chloro-1-propene (Allyl Chloride),T cis-1,2-Dichloroethene,T cis-1,3-Dichloropropene,T Carbon Tetrachloride,T 2-Propanol (Isopropanol),T 1,1-Dichloroethane,T 1,2-Dichloroethane,T Bromodichloromethane,T trans-1,2-Dichloroethene,T Dibromochloromethane,T 1,2-Dibromo-3-Chloropropane,T Ethanol,T Bromomethane,T Bromoform,T trans-1,3-Dichloropropene,T Chloroethane,T 1,2-Dibromoethane,T Acetonitrile,T Acrolein,T 50000 Acrylonitrile,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00117 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:03:02 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211624.D Acq On : 22 Apr 2016 00:48 Operator: SC Sample : 0.40ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:00:36 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 110297 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.87 114 590009 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 251046 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.67 65 186434 13.193 ng -0.03 Spiked Amount 12.500 Range 70 - 130 Recovery = 105.52% 57) Toluene-d8 (SS2) 13.31 98 593929 12.579 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.64% 73) Bromofluorobenzene (SS3) 16.84 174 193068 11.408 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 91.28%

Target Compounds Qvalue 2) Propene 3.69 42 6882 0.699 ng 96 3) Dichlorodifluoromethan... 3.80 85 13611 0.668 ng 99 4) Chloromethane 4.00 50 11344 0.933 ng 96 5) 1,2-Dichloro-1,1,2,2-t... 4.15 135 6782 0.806 ng 97 6) Vinyl Chloride 4.26 62 9469 0.725 ng 98 7) 1,3-Butadiene 4.43 54 4227 0.698 ng 89 8) Bromomethane 4.73 94 5586 0.642 ng 95 9) Chloroethane 4.94 64 4498 0.597 ng 99 10) Ethanol 5.14 45 22039 2.424 ng 92 11) Acetonitrile 5.36 41 12485 0.546 ng # 70 12) Acrolein 5.49 56 3740 0.600 ng 92 13) Acetone 5.62 58 28508 2.963 ng 97 14) Trichlorofluoromethane 5.80 101 10720 0.734 ng 98 15) 2-Propanol (Isopropanol) 5.94 45 33199 1.001 ng 98 16) Acrylonitrile 6.14 53 8566 0.563 ng 97 17) 1,1-Dichloroethene 6.48 96 6389 0.686 ng 95 18) 2-Methyl-2-Propanol (t... 6.65 59 33876 1.132 ng 96 19) Methylene Chloride 6.62 84 8740 0.746 ng 90 20) 3-Chloro-1-propene (Al... 6.75 41 10058 0.772 ng 86 21) Trichlorotrifluoroethane 6.93 151 5575 0.693 ng 100 22) Carbon Disulfide 6.90 76 21710 0.584 ng 98 23) trans-1,2-Dichloroethene 7.64 61 8756 0.525 ng 95 24) 1,1-Dichloroethane 7.85 63 12330 0.571 ng 98 25) Methyl tert-Butyl Ether 7.96 73 20083 0.575 ng 99 26) Vinyl Acetate 8.04 86 4919 2.318 ng # 77 27) 2-Butanone (MEK) 8.29 72 4354 0.537 ng # 79 28) cis-1,2-Dichloroethene 8.72 61 9015 0.597 ng 98 29) Diisopropyl Ether 8.99 87 6709 0.632 ng # 76 30) Ethyl Acetate 8.99 61 4921 1.096 ng 96 31) n-Hexane 8.98 57 12491 0.587 ng 98 32) Chloroform 9.03 83 11166 0.564 ng 97 34) Tetrahydrofuran (THF) 9.46 72 4460 0.521 ng 92 35) Ethyl tert-Butyl Ether 9.54 87 7909 0.573 ng 94 36) 1,2-Dichloroethane 9.79 62 7969 0.579 ng 99 38) 1,1,1-Trichloroethane 10.05 97 9629 0.546 ng 98 39) Isopropyl Acetate 10.44 61 8823 1.200 ng 97 40) 1-Butanol 10.48 56 9542 0.746 ng # 42 41) Benzene 10.51 78 34086 0.689 ng 99 42) Carbon Tetrachloride 10.66 117 7882 0.606 ng 99 43) Cyclohexane 10.79 84 21368 1.145 ng 99 44) tert-Amyl Methyl Ether 11.13 73 19192 0.552 ng 98 45) 1,2-Dichloropropane 11.33 63 7134 0.545 ng 98 46) Bromodichloromethane 11.51 83 8804 0.573 ng 98 47) Trichloroethene 11.57 130 6908 0.477 ng 96 48) 1,4-Dioxane 11.58 88 4658 0.461 ng 97 49) 2,2,4-Trimethylpentane... 11.63 57 30145 0.541 ng 98 118 of 156 R9042116.M Fri Apr 22 10:01:37 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211624.D Acq On : 22 Apr 2016 00:48 Operator: SC Sample : 0.40ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:00:36 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 4870 0.953 ng 94 51) n-Heptane 11.90 71 7536 0.603 ng 97 52) cis-1,3-Dichloropropene 12.42 75 9997 0.500 ng 97 53) 4-Methyl-2-pentanone 12.47 58 6305 0.518 ng 94 54) trans-1,3-Dichloropropene 12.95 75 7701 0.459 ng 95 55) 1,1,2-Trichloroethane 13.12 97 6114 0.502 ng 97 58) Toluene 13.41 91 28031 0.485 ng 98 59) 2-Hexanone 13.67 43 13827 0.542 ng 92 60) Dibromochloromethane 13.82 129 6544 0.494 ng 98 61) 1,2-Dibromoethane 14.08 107 6547 0.497 ng 98 62) n-Butyl Acetate 14.32 43 15419 0.538 ng 97 63) n-Octane 14.43 57 6121 0.535 ng 93 64) Tetrachloroethene 14.57 166 6578 0.459 ng 98 65) Chlorobenzene 15.27 112 16934 0.521 ng 100 66) Ethylbenzene 15.68 91 28732 0.511 ng 98 67) m- & p-Xylenes 15.86 91 45951 0.975 ng 99 68) Bromoform 15.93 173 5189 0.455 ng 99 69) Styrene 16.25 104 16208 0.517 ng 98 70) o-Xylene 16.36 91 22544 0.479 ng 98 71) n-Nonane 16.61 43 13936 0.533 ng 98 72) 1,1,2,2-Tetrachloroethane 16.34 83 9784 0.482 ng 99 74) Cumene 16.99 105 29194 0.491 ng 99 75) alpha-Pinene 17.40 93 14922 0.529 ng 96 76) n-Propylbenzene 17.52 91 34749 0.473 ng 98 77) 3-Ethyltoluene 17.63 105 27513 0.473 ng 98 78) 4-Ethyltoluene 17.68 105 27254 0.490 ng 100 79) 1,3,5-Trimethylbenzene 17.75 105 22649 0.462 ng 100 80) alpha-Methylstyrene 17.91 118 11033 0.460 ng 97 81) 2-Ethyltoluene 17.95 105 26765 0.467 ng 98 82) 1,2,4-Trimethylbenzene 18.19 105 21051 0.430 ng 100 83) n-Decane 18.31 57 13027 0.460 ng 97 84) Benzyl Chloride 18.32 91 12037 0.341 ng 93 85) 1,3-Dichlorobenzene 18.34 146 10903 0.426 ng 98 86) 1,4-Dichlorobenzene 18.41 146 11148 0.411 ng 99 87) sec-Butylbenzene 18.47 105 30745 0.472 ng 98 88) 4-Isopropyltoluene (p-... 18.64 119 26288 0.427 ng 96 89) 1,2,3-Trimethylbenzene 18.64 105 22166 0.435 ng 98 90) 1,2-Dichlorobenzene 18.77 146 10684 0.405 ng 99 91) d-Limonene 18.80 68 9207 0.478 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.24 157 3111 0.337 ng 88 93) n-Undecane 19.65 57 11267 0.368 ng 99 94) 1,2,4-Trichlorobenzene 20.59 180 5202 0.275 ng 99 95) Naphthalene 20.70 128 15810 0.239 ng 99 96) n-Dodecane 20.74 57 8384 0.302 ng 97 97) Hexachlorobutadiene 21.07 225 4245 0.325 ng 98 98) Cyclohexanone 16.02 55 7978 0.488 ng 96 99) tert-Butylbenzene 18.18 119 22672 0.476 ng 100 100) n-Butylbenzene 19.08 91 23411 0.455 ng 97 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

119 of 156 R9042116.M Fri Apr 22 10:01:37 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211624.D Acq On : 22 Apr 2016 00:48 Operator: SC Sample : 0.40ng TO-15 ICAL STD Misc : S29-04191601/S29-04201603 (5/19) ALS Vial : 5 Sample Multiplier: 1

Quant Time: Apr 22 10:00:36 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211624.D\data.ms 900000

850000

800000

750000

700000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR

650000 1,4-Difluorobenzene (IS2),IR

600000 Bromofluorobenzene (SS3),S

550000

500000

450000

400000

350000

300000 Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

250000

200000

150000 1,2,3-Trimethylbenzene,T tert-Butylbenzene,T 1,2,4-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T EthylDiisopropyl Acetate,T Ether,T n-Hexane,T

100000 Acetone,T Cyclohexane,T n-Decane,T sec-Butylbenzene,T 3-Ethyltoluene,T n-Butylbenzene,T m- & p-Xylenes,T 2-Ethyltoluene,T n-Propylbenzene,T 4-Ethyltoluene,T 1,3,5-Trimethylbenzene,T Cumene,T d-Limonene,T Benzene,T Benzyl Chloride,T alpha-Pinene,T o-Xylene,T n-Nonane,T Vinyl Acetate,T Isopropyl Acetate,T n-Undecane,T Toluene,T alpha-Methylstyrene,T Ethylbenzene,T Chlorobenzene,T 1,2-Dichlorobenzene,T 2,2,4-Trimethylpentane (Isooctane),T n-Octane,T Methyl Methacrylate,T 1,3-Dichlorobenzene,T n-Heptane,T n-Dodecane,T Styrene,T Propene,T Hexachlorobutadiene,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Methylene Chloride,T Trichloroethene,T 1,4-Dichlorobenzene,T Ethyl tert-Butyl Ether,T tert-Amyl Methyl Ether,T Dichlorodifluoromethane (CFC 12),T 1,4-Dioxane,T Naphthalene,T 4-Methyl-2-pentanone,T Tetrachloroethene,T n-Butyl Acetate,T Methyl tert-Butyl Ether,T 1-Butanol,T Trichlorotrifluoroethane,T 1,1,2,2-Tetrachloroethane,T Chloroform,T 1,1,2-Trichloroethane,T 2-Hexanone,T 1,2,4-Trichlorobenzene,T 1,2-Dichloropropane,T Cyclohexanone,T 1,1-Dichloroethene,T 1,1,1-Trichloroethane,T Tetrahydrofuran (THF),T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Chloromethane,T cis-1,2-Dichloroethene,T Trichlorofluoromethane,T cis-1,3-Dichloropropene,T 2-Butanone (MEK),T Vinyl Chloride,T 1,3-Butadiene,T 3-Chloro-1-propene (Allyl Chloride),T Carbon Tetrachloride,T trans-1,2-Dichloroethene,T Carbon Disulfide,T 2-Propanol (Isopropanol),T Bromodichloromethane,T 1,1-Dichloroethane,T Ethanol,T 1,2-Dichloroethane,T 1,2-Dibromo-3-Chloropropane,T Bromoform,T Dibromochloromethane,T trans-1,3-Dichloropropene,T Bromomethane,T 1,2-Dibromoethane,T

50000 Acrylonitrile,T Acetonitrile,T Acrolein,T Chloroethane,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00120 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:01:39 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211625.D Acq On : 22 Apr 2016 1:22 Operator: SC Sample : 1.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:59:22 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.89 130 124410 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.87 114 641002 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 273526 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 202040 12.676 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 101.44% 57) Toluene-d8 (SS2) 13.31 98 645089 12.540 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.32% 73) Bromofluorobenzene (SS3) 16.84 174 212655 11.533 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 92.24%

Target Compounds Qvalue 2) Propene 3.69 42 18405 1.658 ng 99 3) Dichlorodifluoromethan... 3.79 85 36168 1.573 ng 99 4) Chloromethane 3.98 50 30144 2.198 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.14 135 18244 1.922 ng 99 6) Vinyl Chloride 4.26 62 25742 1.748 ng 100 7) 1,3-Butadiene 4.43 54 11535 1.690 ng 99 8) Bromomethane 4.73 94 15240 1.553 ng 99 9) Chloroethane 4.94 64 12065 1.420 ng 99 10) Ethanol 5.14 45 74590 7.275 ng 100 11) Acetonitrile 5.35 41 36987 1.435 ng 93 12) Acrolein 5.48 56 10790 1.534 ng 95 13) Acetone 5.62 58 72619 6.691 ng 96 14) Trichlorofluoromethane 5.80 101 28728 1.745 ng 100 15) 2-Propanol (Isopropanol) 5.93 45 101312 2.708 ng 97 16) Acrylonitrile 6.14 53 24689 1.438 ng 100 17) 1,1-Dichloroethene 6.48 96 17208 1.637 ng 97 18) 2-Methyl-2-Propanol (t... 6.57 59 96186 2.850 ng 99 19) Methylene Chloride 6.62 84 20628 1.562 ng 97 20) 3-Chloro-1-propene (Al... 6.75 41 26416 1.797 ng 91 21) Trichlorotrifluoroethane 6.94 151 14771 1.628 ng 97 22) Carbon Disulfide 6.90 76 61479 1.465 ng 100 23) trans-1,2-Dichloroethene 7.64 61 26019 1.383 ng 97 24) 1,1-Dichloroethane 7.85 63 33515 1.377 ng 98 25) Methyl tert-Butyl Ether 7.95 73 54026 1.371 ng 98 26) Vinyl Acetate 8.04 86 16661 6.961 ng # 73 27) 2-Butanone (MEK) 8.29 72 12132 1.327 ng 93 28) cis-1,2-Dichloroethene 8.73 61 24497 1.438 ng 99 29) Diisopropyl Ether 8.98 87 15255 1.275 ng # 88 30) Ethyl Acetate 8.98 61 14438 2.851 ng 96 31) n-Hexane 8.98 57 31953 1.331 ng 99 32) Chloroform 9.03 83 30278 1.357 ng 100 34) Tetrahydrofuran (THF) 9.45 72 12332 1.277 ng 99 35) Ethyl tert-Butyl Ether 9.53 87 21100 1.354 ng 94 36) 1,2-Dichloroethane 9.79 62 21569 1.388 ng 99 38) 1,1,1-Trichloroethane 10.05 97 25774 1.346 ng 98 39) Isopropyl Acetate 10.44 61 24355 3.049 ng # 91 40) 1-Butanol 10.46 56 42056 3.026 ng 99 41) Benzene 10.51 78 75848 1.412 ng 99 42) Carbon Tetrachloride 10.66 117 21704 1.537 ng 100 43) Cyclohexane 10.79 84 55745 2.750 ng 97 44) tert-Amyl Methyl Ether 11.13 73 52098 1.380 ng 99 45) 1,2-Dichloropropane 11.33 63 19397 1.364 ng 99 46) Bromodichloromethane 11.51 83 23511 1.409 ng 99 47) Trichloroethene 11.57 130 18695 1.188 ng 100 48) 1,4-Dioxane 11.56 88 14376 1.309 ng 93 49) 2,2,4-Trimethylpentane... 11.64 57 81653 1.349 ng 100 121 of 156 R9042116.M Fri Apr 22 10:00:19 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211625.D Acq On : 22 Apr 2016 1:22 Operator: SC Sample : 1.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:59:22 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 14107 2.541 ng 93 51) n-Heptane 11.89 71 18758 1.381 ng 98 52) cis-1,3-Dichloropropene 12.43 75 29937 1.379 ng 97 53) 4-Methyl-2-pentanone 12.46 58 18144 1.371 ng 98 54) trans-1,3-Dichloropropene 12.95 75 24097 1.322 ng 99 55) 1,1,2-Trichloroethane 13.12 97 17751 1.342 ng 99 58) Toluene 13.42 91 75868 1.205 ng 99 59) 2-Hexanone 13.67 43 42938 1.546 ng 96 60) Dibromochloromethane 13.82 129 19470 1.348 ng 100 61) 1,2-Dibromoethane 14.08 107 19456 1.355 ng 99 62) n-Butyl Acetate 14.31 43 48163 1.541 ng 98 63) n-Octane 14.44 57 16907 1.356 ng 97 64) Tetrachloroethene 14.57 166 18953 1.215 ng 100 65) Chlorobenzene 15.27 112 48296 1.364 ng 100 66) Ethylbenzene 15.68 91 82683 1.350 ng 100 67) m- & p-Xylenes 15.87 91 131762 2.566 ng 99 68) Bromoform 15.92 173 15709 1.264 ng 100 69) Styrene 16.24 104 50578 1.480 ng 98 70) o-Xylene 16.36 91 66306 1.292 ng 99 71) n-Nonane 16.61 43 38467 1.350 ng 98 72) 1,1,2,2-Tetrachloroethane 16.34 83 31823 1.438 ng 99 74) Cumene 16.99 105 82611 1.275 ng 99 75) alpha-Pinene 17.40 93 40776 1.326 ng 96 76) n-Propylbenzene 17.52 91 103036 1.286 ng 99 77) 3-Ethyltoluene 17.63 105 80884 1.277 ng 100 78) 4-Ethyltoluene 17.67 105 81367 1.342 ng 99 79) 1,3,5-Trimethylbenzene 17.75 105 68630 1.285 ng 98 80) alpha-Methylstyrene 17.91 118 36655 1.403 ng 99 81) 2-Ethyltoluene 17.95 105 81183 1.301 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 68404 1.282 ng 100 83) n-Decane 18.31 57 40961 1.329 ng 99 84) Benzyl Chloride 18.32 91 50861 1.322 ng 98 85) 1,3-Dichlorobenzene 18.34 146 38088 1.366 ng 100 86) 1,4-Dichlorobenzene 18.41 146 38332 1.296 ng 99 87) sec-Butylbenzene 18.47 105 93594 1.318 ng 98 88) 4-Isopropyltoluene (p-... 18.64 119 83107 1.239 ng 98 89) 1,2,3-Trimethylbenzene 18.64 105 71187 1.284 ng 99 90) 1,2-Dichlorobenzene 18.77 146 37726 1.311 ng 99 91) d-Limonene 18.80 68 28863 1.376 ng 98 92) 1,2-Dibromo-3-Chloropr... 19.23 157 12168 1.210 ng 90 93) n-Undecane 19.65 57 43449 1.304 ng 98 94) 1,2,4-Trichlorobenzene 20.59 180 26216 1.274 ng 99 95) Naphthalene 20.70 128 90672 1.260 ng 99 96) n-Dodecane 20.74 57 43810 1.451 ng 99 97) Hexachlorobutadiene 21.07 225 15601 1.095 ng 97 98) Cyclohexanone 16.02 55 27425 1.538 ng 97 99) tert-Butylbenzene 18.18 119 65964 1.272 ng 100 100) n-Butylbenzene 19.08 91 77111 1.376 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

122 of 156 R9042116.M Fri Apr 22 10:00:19 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211625.D Acq On : 22 Apr 2016 1:22 Operator: SC Sample : 1.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:59:22 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211625.D\data.ms 1000000

950000

900000

850000

800000

750000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR

700000 1,4-Difluorobenzene (IS2),IR Bromofluorobenzene (SS3),S

650000

600000

550000

500000

450000

400000

350000 Bromochloromethane (IS1),IR

300000 1,2-Dichloroethane-d4(SS1),S 1,2,3-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T 1,2,4-Trimethylbenzene,T tert-Butylbenzene,T 250000 n-Hexane,TEthylDiisopropyl Acetate,T Ether,T

200000 n-Decane,T Acetone,T n-Dodecane,T n-Butylbenzene,T Benzyl Chloride,T Cyclohexane,T n-Undecane,T sec-Butylbenzene,T d-Limonene,T n-Propylbenzene,T 4-Ethyltoluene,T 3-Ethyltoluene,T 2-Ethyltoluene,T m- & p-Xylenes,T 1,3,5-Trimethylbenzene,T Isopropyl Acetate,T Naphthalene,T Cumene,T alpha-Methylstyrene,T o-Xylene,T 150000 Vinyl Acetate,T 1,3-Dichlorobenzene,T n-Nonane,T Ethylbenzene,T alpha-Pinene,T 1,2-Dichlorobenzene,T Hexachlorobutadiene,T Toluene,T 1,4-Dichlorobenzene,T Methyl Methacrylate,T Styrene,T n-Octane,T Benzene,T 1,2,4-Trichlorobenzene,T 2,2,4-Trimethylpentane (Isooctane),T Chlorobenzene,T 1-Butanol,T n-Heptane,T Trichloroethene,T Propene,T 1,4-Dioxane,T Ethyl tert-Butyl Ether,T tert-Amyl Methyl Ether,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T n-Butyl Acetate,T 1,1,2,2-Tetrachloroethane,T 100000 4-Methyl-2-pentanone,T Tetrachloroethene,T Cyclohexanone,T 2-Hexanone,T Dichlorodifluoromethane (CFC 12),T Methylene Chloride,T Methyl tert-Butyl Ether,T 1,1,2-Trichloroethane,T cis-1,3-Dichloropropene,T 2-Propanol (Isopropanol),T 1,2-Dichloropropane,T 1,2-Dibromo-3-Chloropropane,T Trichlorotrifluoroethane,T Ethanol,T 1,1-Dichloroethene,T Chloroform,T Tetrahydrofuran (THF),T cis-1,2-Dichloroethene,T trans-1,2-Dichloroethene,T 1,1,1-Trichloroethane,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T 2-Butanone (MEK),T 3-Chloro-1-propene (Allyl Chloride),T Trichlorofluoromethane,T trans-1,3-Dichloropropene,T Carbon Disulfide,T Bromodichloromethane,T Dibromochloromethane,T Carbon Tetrachloride,T Chloromethane,T 1,1-Dichloroethane,T Bromoform,T Vinyl Chloride,T 1,3-Butadiene,T 1,2-Dichloroethane,T 1,2-Dibromoethane,T Bromomethane,T Acrylonitrile,T Acetonitrile,T Chloroethane,T 50000 Acrolein,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00123 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:00:21 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211626.D Acq On : 22 Apr 2016 1:56 Operator: SC Sample : 5.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:58:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.90 130 112991 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.88 114 579489 12.500 ng -0.01 56) Chlorobenzene-d5 (IS3) 15.23 82 247560 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 184723 12.761 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 102.08% 57) Toluene-d8 (SS2) 13.31 98 581431 12.488 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.92% 73) Bromofluorobenzene (SS3) 16.84 174 193670 11.605 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 92.88%

Target Compounds Qvalue 2) Propene 3.68 42 80345 7.969 ng 100 3) Dichlorodifluoromethan... 3.78 85 166194 7.959 ng 100 4) Chloromethane 3.97 50 136333 10.947 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.14 135 82833 9.610 ng 99 6) Vinyl Chloride 4.24 62 117892 8.817 ng 98 7) 1,3-Butadiene 4.42 54 55403 8.937 ng 97 8) Bromomethane 4.72 94 69501 7.796 ng 100 9) Chloroethane 4.93 64 54852 7.109 ng 99 10) Ethanol 5.16 45 266674 28.637 ng 98 11) Acetonitrile 5.35 41 136188 5.819 ng 98 12) Acrolein 5.48 56 52762 8.259 ng 96 13) Acetone 5.62 58 332675 33.750 ng 97 14) Trichlorofluoromethane 5.79 101 129018 8.627 ng 99 15) 2-Propanol (Isopropanol) 5.94 45 457914 13.477 ng 99 16) Acrylonitrile 6.14 53 116438 7.467 ng 100 17) 1,1-Dichloroethene 6.48 96 77391 8.107 ng 97 18) 2-Methyl-2-Propanol (t... 6.58 59 442692 14.444 ng 98 19) Methylene Chloride 6.63 84 87183 7.268 ng 100 20) 3-Chloro-1-propene (Al... 6.75 41 138141 10.347 ng 89 21) Trichlorotrifluoroethane 6.94 151 64850 7.872 ng 95 22) Carbon Disulfide 6.89 76 295518 7.756 ng 100 23) trans-1,2-Dichloroethene 7.64 61 122614 7.175 ng 98 24) 1,1-Dichloroethane 7.86 63 151229 6.841 ng 99 25) Methyl tert-Butyl Ether 7.94 73 248044 6.928 ng 98 26) Vinyl Acetate 8.04 86 84949 39.081 ng # 81 27) 2-Butanone (MEK) 8.28 72 56645 6.823 ng # 88 28) cis-1,2-Dichloroethene 8.74 61 115553 7.469 ng 97 29) Diisopropyl Ether 8.98 87 67812 6.240 ng # 84 30) Ethyl Acetate 8.99 61 64878 14.107 ng 98 31) n-Hexane 8.98 57 141863 6.507 ng 99 32) Chloroform 9.04 83 138928 6.854 ng 100 34) Tetrahydrofuran (THF) 9.44 72 55054 6.277 ng 98 35) Ethyl tert-Butyl Ether 9.53 87 97560 6.895 ng 95 36) 1,2-Dichloroethane 9.79 62 97542 6.913 ng 100 38) 1,1,1-Trichloroethane 10.05 97 117765 6.803 ng 99 39) Isopropyl Acetate 10.44 61 112022 15.511 ng # 93 40) 1-Butanol 10.45 56 195582 15.567 ng 99 41) Benzene 10.51 78 339811 6.996 ng 99 42) Carbon Tetrachloride 10.67 117 100641 7.881 ng 99 43) Cyclohexane 10.80 84 254000 13.861 ng 98 44) tert-Amyl Methyl Ether 11.12 73 239622 7.021 ng 99 45) 1,2-Dichloropropane 11.34 63 86402 6.719 ng 100 46) Bromodichloromethane 11.52 83 111730 7.409 ng 100 47) Trichloroethene 11.57 130 86442 6.077 ng 100 48) 1,4-Dioxane 11.55 88 67997 6.849 ng 98 49) 2,2,4-Trimethylpentane... 11.64 57 371567 6.788 ng 100 124 of 156 R9042116.M Fri Apr 22 09:59:03 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211626.D Acq On : 22 Apr 2016 1:56 Operator: SC Sample : 5.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:58:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 66471 13.243 ng 95 51) n-Heptane 11.90 71 84376 6.871 ng 98 52) cis-1,3-Dichloropropene 12.43 75 141769 7.225 ng 99 53) 4-Methyl-2-pentanone 12.46 58 83630 6.989 ng 96 54) trans-1,3-Dichloropropene 12.95 75 118980 7.218 ng 98 55) 1,1,2-Trichloroethane 13.12 97 81236 6.791 ng 100 58) Toluene 13.42 91 339639 5.962 ng 100 59) 2-Hexanone 13.66 43 199543 7.937 ng 97 60) Dibromochloromethane 13.82 129 92128 7.046 ng 99 61) 1,2-Dibromoethane 14.08 107 91096 7.011 ng 99 62) n-Butyl Acetate 14.31 43 224591 7.940 ng 97 63) n-Octane 14.44 57 74230 6.577 ng 98 64) Tetrachloroethene 14.57 166 86368 6.116 ng 98 65) Chlorobenzene 15.27 112 217432 6.787 ng 99 66) Ethylbenzene 15.67 91 381883 6.890 ng 99 67) m- & p-Xylenes 15.87 91 603984 12.997 ng 99 68) Bromoform 15.92 173 76418 6.793 ng 99 69) Styrene 16.25 104 235613 7.619 ng 99 70) o-Xylene 16.36 91 300241 6.464 ng 99 71) n-Nonane 16.61 43 174651 6.772 ng 97 72) 1,1,2,2-Tetrachloroethane 16.34 83 148031 7.389 ng 99 74) Cumene 16.99 105 376613 6.424 ng 99 75) alpha-Pinene 17.40 93 191534 6.880 ng 100 76) n-Propylbenzene 17.52 91 473422 6.530 ng 98 77) 3-Ethyltoluene 17.63 105 376675 6.569 ng 99 78) 4-Ethyltoluene 17.68 105 374109 6.815 ng 99 79) 1,3,5-Trimethylbenzene 17.75 105 314361 6.503 ng 99 80) alpha-Methylstyrene 17.91 118 173710 7.348 ng 99 81) 2-Ethyltoluene 17.95 105 367261 6.504 ng 99 82) 1,2,4-Trimethylbenzene 18.19 105 316332 6.551 ng 99 83) n-Decane 18.31 57 186659 6.689 ng 98 84) Benzyl Chloride 18.32 91 269579 7.744 ng 98 85) 1,3-Dichlorobenzene 18.34 146 176745 7.003 ng 99 86) 1,4-Dichlorobenzene 18.41 146 179490 6.703 ng 100 87) sec-Butylbenzene 18.47 105 429189 6.679 ng 99 88) 4-Isopropyltoluene (p-... 18.64 119 379002 6.244 ng 100 89) 1,2,3-Trimethylbenzene 18.64 105 327915 6.533 ng 99 90) 1,2-Dichlorobenzene 18.77 146 173935 6.680 ng 99 91) d-Limonene 18.80 68 134979 7.107 ng 97 92) 1,2-Dibromo-3-Chloropr... 19.23 157 61340 6.737 ng 95 93) n-Undecane 19.65 57 197655 6.554 ng 98 94) 1,2,4-Trichlorobenzene 20.59 180 125699 6.747 ng 99 95) Naphthalene 20.70 128 433936 6.662 ng 99 96) n-Dodecane 20.74 57 207938 7.608 ng 98 97) Hexachlorobutadiene 21.07 225 73637 5.711 ng 99 98) Cyclohexanone 16.01 55 127787 7.920 ng 98 99) tert-Butylbenzene 18.18 119 305697 6.513 ng 98 100) n-Butylbenzene 19.08 91 354412 6.990 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

125 of 156 R9042116.M Fri Apr 22 09:59:03 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211626.D Acq On : 22 Apr 2016 1:56 Operator: SC Sample : 5.0ng TO-15 ICAL STD Misc : S29-04191601/S29-04131608 (5/12) ALS Vial : 6 Sample Multiplier: 1

Quant Time: Apr 22 09:58:06 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211626.D\data.ms

1200000

1150000

1100000

1050000

1000000

950000 tert-Butylbenzene,T1,2,4-Trimethylbenzene,T 1,2,3-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T

900000 Diisopropyln-Hexane,T Ether,T

850000 n-Decane,T Ethyl Acetate,T Benzyl Chloride,T

800000 Toluene-d8 (SS2),S

750000 n-Dodecane,T

700000 Chlorobenzene-d5 (IS3),IR Acetone,T 1,4-Difluorobenzene (IS2),IR Isopropyl Acetate,T n-Butylbenzene,T

650000 1-Butanol,T n-Undecane,T Cyclohexane,T Bromofluorobenzene (SS3),S Vinyl Acetate,T sec-Butylbenzene,T d-Limonene,T Naphthalene,T 600000 3-Ethyltoluene,T m- & p-Xylenes,T 4-Ethyltoluene,T n-Propylbenzene,T 2-Ethyltoluene,T 1,3,5-Trimethylbenzene,T alpha-Methylstyrene,T

550000 Cumene,T o-Xylene,T 500000 Ethylbenzene,T n-Nonane,T alpha-Pinene,T 1,2-Dichlorobenzene,T 1,3-Dichlorobenzene,T Methyl Methacrylate,T 450000 1,4-Dichlorobenzene,T Hexachlorobutadiene,T Toluene,T 1,2,4-Trichlorobenzene,T Styrene,T n-Octane,T

400000 2,2,4-Trimethylpentane (Isooctane),T Benzene,T Chlorobenzene,T n-Heptane,T 350000 n-Butyl Acetate,T Bromochloromethane (IS1),IR 1,1,2,2-Tetrachloroethane,T 4-Methyl-2-pentanone,T tert-Amyl Methyl Ether,T Trichloroethene,T 2-Hexanone,T Ethyl tert-Butyl Ether,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 1,2-Dichloroethane-d4(SS1),S

300000 Cyclohexanone,T Propene,T Tetrachloroethene,T Dichlorodifluoromethane (CFC 12),T 1,1,2-Trichloroethane,T Methyl tert-Butyl Ether,T 2-Propanol (Isopropanol),T cis-1,3-Dichloropropene,T 1,2-Dibromo-3-Chloropropane,T 250000 Methylene Chloride,T 1,2-Dichloropropane,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T trans-1,3-Dichloropropene,T 1,1-Dichloroethene,T trans-1,2-Dichloroethene,T cis-1,2-Dichloroethene,T Trichlorotrifluoroethane,T Chloroform,T Carbon Disulfide,T Tetrahydrofuran (THF),T 1,1,1-Trichloroethane,T 1,4-Dioxane,T 3-Chloro-1-propene (Allyl Chloride),T 2-Butanone (MEK),T Bromodichloromethane,T Trichlorofluoromethane,T 200000 Carbon Tetrachloride,T Dibromochloromethane,T Chloromethane,T Bromoform,T Ethanol,T 1,1-Dichloroethane,T 1,3-Butadiene,T Vinyl Chloride,T Acrylonitrile,T 1,2-Dichloroethane,T 1,2-Dibromoethane,T Bromomethane,T 150000 Acetonitrile,T Chloroethane,T

100000 Acrolein,T

50000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00126 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 09:59:05 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211627.D Acq On : 22 Apr 2016 2:30 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 09:55:09 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Apr 12 09:51:38 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.92 130 112535 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.89 114 582115 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 248231 12.500 ng -0.02

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.70 65 181572 12.594 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.72% 57) Toluene-d8 (SS2) 13.32 98 577303 12.366 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 98.96% 73) Bromofluorobenzene (SS3) 16.84 174 193914 11.588 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 92.72%

Target Compounds Qvalue 2) Propene 3.67 42 490866 48.885 ng 100 3) Dichlorodifluoromethan... 3.78 85 933913 44.906 ng 99 4) Chloromethane 3.97 50 782478 63.083 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.13 135 467455 54.452 ng 100 6) Vinyl Chloride 4.25 62 682884 51.278 ng 100 7) 1,3-Butadiene 4.42 54 399966 64.776 ng 97 8) Bromomethane 4.73 94 410868 46.277 ng 99 9) Chloroethane 4.93 64 310190 40.365 ng 100 10) Ethanol 5.20 45 1826639 196.951 ng 99 11) Acetonitrile 5.38 41 917479 39.361 ng 100 12) Acrolein 5.49 56 321367 50.507 ng 100 13) Acetone 5.64 58 1849964 188.442 ng 100 14) Trichlorofluoromethane 5.80 101 718169 48.217 ng 100 15) 2-Propanol (Isopropanol) 5.98 45 2487220 73.501 ng 99 16) Acrylonitrile 6.16 53 655337 42.193 ng 99 17) 1,1-Dichloroethene 6.48 96 453775 47.728 ng 98 18) 2-Methyl-2-Propanol (t... 6.61 59 2428903 79.571 ng 99 19) Methylene Chloride 6.65 84 481850 40.331 ng 99 20) 3-Chloro-1-propene (Al... 6.76 41 725714 54.575 ng 96 21) Trichlorotrifluoroethane 6.94 151 369369 45.020 ng 95 22) Carbon Disulfide 6.90 76 1745999 46.010 ng 100 23) trans-1,2-Dichloroethene 7.66 61 699229 41.081 ng 99 24) 1,1-Dichloroethane 7.88 63 844817 38.369 ng 100 25) Methyl tert-Butyl Ether 7.94 73 1403509 39.362 ng 98 26) Vinyl Acetate 8.06 86 527173 243.508 ng # 95 27) 2-Butanone (MEK) 8.29 72 324272 39.216 ng 96 28) cis-1,2-Dichloroethene 8.75 61 652924 42.372 ng 98 29) Diisopropyl Ether 8.99 87 383276 35.414 ng # 95 30) Ethyl Acetate 8.99 61 365766 79.856 ng 98 31) n-Hexane 8.99 57 752998 34.679 ng 100 32) Chloroform 9.06 83 786005 38.933 ng 100 34) Tetrahydrofuran (THF) 9.44 72 304311 34.839 ng 97 35) Ethyl tert-Butyl Ether 9.54 87 555008 39.386 ng 96 36) 1,2-Dichloroethane 9.81 62 549095 39.074 ng 99 38) 1,1,1-Trichloroethane 10.06 97 665959 38.296 ng 99 39) Isopropyl Acetate 10.44 61 623801 85.983 ng 99 40) 1-Butanol 10.46 56 996237 78.937 ng 98 41) Benzene 10.52 78 1846632 37.847 ng 100 42) Carbon Tetrachloride 10.68 117 577384 45.010 ng 100 43) Cyclohexane 10.80 84 1424407 77.378 ng 98 44) tert-Amyl Methyl Ether 11.13 73 1363222 39.762 ng 99 45) 1,2-Dichloropropane 11.34 63 485208 37.560 ng 99 46) Bromodichloromethane 11.52 83 643972 42.510 ng 99 47) Trichloroethene 11.58 130 483720 33.854 ng 100 48) 1,4-Dioxane 11.55 88 387067 38.812 ng 98 49) 2,2,4-Trimethylpentane... 11.64 57 2086009 37.939 ng 100 127 of 156 R9042116.M Fri Apr 22 09:56:31 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211627.D Acq On : 22 Apr 2016 2:30 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 09:55:09 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Apr 12 09:51:38 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 378366 75.040 ng 97 51) n-Heptane 11.90 71 470371 38.129 ng 99 52) cis-1,3-Dichloropropene 12.43 75 817557 41.476 ng 100 53) 4-Methyl-2-pentanone 12.46 58 469530 39.061 ng 99 54) trans-1,3-Dichloropropene 12.95 75 700978 42.336 ng 100 55) 1,1,2-Trichloroethane 13.12 97 463680 38.590 ng 98 58) Toluene 13.42 91 1909641 33.429 ng 100 59) 2-Hexanone 13.66 43 1065362 42.261 ng 99 60) Dibromochloromethane 13.83 129 540922 41.260 ng 100 61) 1,2-Dibromoethane 14.08 107 529513 40.644 ng 99 62) n-Butyl Acetate 14.31 43 1221073 43.050 ng 99 63) n-Octane 14.44 57 420764 37.178 ng 99 64) Tetrachloroethene 14.57 166 495447 34.987 ng 100 65) Chlorobenzene 15.27 112 1234372 38.426 ng 100 66) Ethylbenzene 15.68 91 2166877 38.990 ng 99 67) m- & p-Xylenes 15.87 91 3434858 73.713 ng 99 68) Bromoform 15.93 173 466707 41.377 ng 99 69) Styrene 16.25 104 1360453 43.876 ng 99 70) o-Xylene 16.37 91 1729648 37.136 ng 99 71) n-Nonane 16.61 43 971232 37.558 ng 99 72) 1,1,2,2-Tetrachloroethane 16.34 83 868228 43.223 ng 99 74) Cumene 16.99 105 2155247 36.661 ng 99 75) alpha-Pinene 17.40 93 1122471 40.211 ng 99 76) n-Propylbenzene 17.52 91 2666111 36.677 ng 99 77) 3-Ethyltoluene 17.63 105 2209175 38.425 ng 100 78) 4-Ethyltoluene 17.68 105 2060870 37.441 ng 100 79) 1,3,5-Trimethylbenzene 17.76 105 1781007 36.743 ng 99 80) alpha-Methylstyrene 17.92 118 969010 40.878 ng 100 81) 2-Ethyltoluene 17.95 105 2081839 36.769 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 1830947 37.816 ng 99 83) n-Decane 18.31 57 1050391 37.540 ng 99 84) Benzyl Chloride 18.32 91 1694995 48.562 ng 99 85) 1,3-Dichlorobenzene 18.34 146 1039645 41.082 ng 100 86) 1,4-Dichlorobenzene 18.41 146 1032075 38.436 ng 100 87) sec-Butylbenzene 18.48 105 2437687 37.835 ng 99 88) 4-Isopropyltoluene (p-... 18.64 119 2170488 35.664 ng 99 89) 1,2,3-Trimethylbenzene 18.64 105 1890140 37.556 ng 100 90) 1,2-Dichlorobenzene 18.77 146 1001878 38.374 ng 100 91) d-Limonene 18.79 68 745462 39.147 ng 98 92) 1,2-Dibromo-3-Chloropr... 19.23 157 372607 40.812 ng 97 93) n-Undecane 19.65 57 1091222 36.087 ng 99 94) 1,2,4-Trichlorobenzene 20.59 180 712816 38.156 ng 99 95) Naphthalene 20.70 128 2347119 35.939 ng 100 96) n-Dodecane 20.74 57 1071983 39.114 ng 99 97) Hexachlorobutadiene 21.07 225 436363 33.752 ng 99 98) Cyclohexanone 16.02 55 652421 40.327 ng 99 99) tert-Butylbenzene 18.19 119 1758882 37.374 ng 100 100) n-Butylbenzene 19.09 91 2002303 39.385 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

128 of 156 R9042116.M Fri Apr 22 09:56:31 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211627.D Acq On : 22 Apr 2016 2:30 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 09:55:09 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Apr 12 09:51:38 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211627.D\data.ms

7000000

6500000

6000000 1,2,3-Trimethylbenzene,T

5500000 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T 4-Isopropyltoluene (p-Cymene),T

5000000 n-Decane,T Benzyl Chloride,T Diisopropyln-Hexane,T Ether,T 4500000 Ethyl Acetate,T

4000000 n-Butylbenzene,T n-Dodecane,T sec-Butylbenzene,T n-Undecane,T

3500000 d-Limonene,T Cyclohexane,T Vinyl Acetate,T 4-Ethyltoluene,T Isopropyl Acetate,T Naphthalene,T n-Propylbenzene,T 3-Ethyltoluene,T 2-Ethyltoluene,T m- & p-Xylenes,T 1,3,5-Trimethylbenzene,T 1-Butanol,T alpha-Methylstyrene,T Cumene,T

3000000 Acetone,T 1,3-Dichlorobenzene,T o-Xylene,T 1,2-Dichlorobenzene,T Ethylbenzene,T alpha-Pinene,T n-Nonane,T Styrene,T 1,4-Dichlorobenzene,T Methyl Methacrylate,T 1,2,4-Trichlorobenzene,T Hexachlorobutadiene,T

2500000 Toluene,T n-Octane,T 2,2,4-Trimethylpentane (Isooctane),T Chlorobenzene,T Benzene,T 2000000 n-Heptane,T 1,1,2,2-Tetrachloroethane,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Propene,T n-Butyl Acetate,T tert-Amyl Methyl Ether,T 4-Methyl-2-pentanone,T 2-Propanol (Isopropanol),T Tetrachloroethene,T 2-Hexanone,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Ethyl tert-Butyl Ether,T Trichloroethene,T Cyclohexanone,T 1,2-Dibromo-3-Chloropropane,T cis-1,3-Dichloropropene,T 1,1,2-Trichloroethane,T 1500000 Dichlorodifluoromethane (CFC 12),T Methyl tert-Butyl Ether,T trans-1,3-Dichloropropene,T 1,2-Dichloropropane,T Carbon Disulfide,T Trichlorotrifluoroethane,T 1,1-Dichloroethene,T Ethanol,T cis-1,2-Dichloroethene,T Tetrahydrofuran (THF),T Bromodichloromethane,T trans-1,2-Dichloroethene,T 1,3-Butadiene,T 1,1,1-Trichloroethane,T Chloroform,T Dibromochloromethane,T 2-Butanone (MEK),T Methylene Chloride,T Carbon Tetrachloride,T 1,4-Dioxane,T Bromoform,T Trichlorofluoromethane,T Toluene-d8 (SS2),S Chloromethane,T

1000000 3-Chloro-1-propene (Allyl Chloride),T 1,1-Dichloroethane,T Chlorobenzene-d5 (IS3),IR Vinyl Chloride,T 1,2-Dibromoethane,T 1,2-Dichloroethane,T Acrylonitrile,T Acetonitrile,T 1,4-Difluorobenzene (IS2),IR Bromofluorobenzene (SS3),S Bromomethane,T Chloroethane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S 500000 Acrolein,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00129 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 09:56:35 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211628.D Acq On : 22 Apr 2016 3:04 Operator: SC Sample : 50ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:08:27 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.93 130 115660 12.500 ng 0.00 37) 1,4-Difluorobenzene (IS2) 10.89 114 596797 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.23 82 254042 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.70 65 186531 12.588 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.72% 57) Toluene-d8 (SS2) 13.32 98 594510 12.443 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.52% 73) Bromofluorobenzene (SS3) 16.84 174 198148 11.570 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 92.56%

Target Compounds Qvalue 2) Propene 3.67 42 933259 90.432 ng 100 3) Dichlorodifluoromethan... 3.78 85 1789504 83.720 ng 99 4) Chloromethane 3.97 50 1480336 116.120 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.13 135 923595 104.679 ng 99 6) Vinyl Chloride 4.25 62 1339210 97.844 ng 100 7) 1,3-Butadiene 4.42 54 822468 129.604 ng 98 8) Bromomethane 4.73 94 807617 88.506 ng 100 9) Chloroethane 4.94 64 605674 76.686 ng 99 10) Ethanol 5.22 45 2717994 285.140 ng 98 11) Acetonitrile 5.39 41 1768422 73.818 ng 100 12) Acrolein 5.50 56 609630 93.222 ng 100 13) Acetone 5.65 58 3512163 348.092 ng 98 14) Trichlorofluoromethane 5.80 101 1408733 92.025 ng 100 15) 2-Propanol (Isopropanol) 6.00 45 4742762 136.368 ng 100 16) Acrylonitrile 6.18 53 1275138 79.881 ng 99 17) 1,1-Dichloroethene 6.49 96 888954 90.974 ng 100 18) 2-Methyl-2-Propanol (t... 6.63 59 4687518 149.414 ng 99 19) Methylene Chloride 6.66 84 938506 76.430 ng 100 20) 3-Chloro-1-propene (Al... 6.77 41 1398962 102.362 ng 98 21) Trichlorotrifluoroethane 6.95 151 731216 86.715 ng 96 22) Carbon Disulfide 6.90 76 3445190 88.334 ng 100 23) trans-1,2-Dichloroethene 7.67 61 1367217 78.156 ng 100 24) 1,1-Dichloroethane 7.88 63 1640611 72.498 ng 100 25) Methyl tert-Butyl Ether 7.95 73 2736314 74.668 ng 99 26) Vinyl Acetate 8.07 86 1037867 466.452 ng # 93 27) 2-Butanone (MEK) 8.30 72 633115 74.497 ng 98 28) cis-1,2-Dichloroethene 8.76 61 1263577 79.786 ng 100 29) Diisopropyl Ether 8.99 87 743086 66.805 ng # 95 30) Ethyl Acetate 9.00 61 697283 148.121 ng 98 31) n-Hexane 8.99 57 1442265 64.628 ng 100 32) Chloroform 9.07 83 1530410 73.757 ng 100 34) Tetrahydrofuran (THF) 9.44 72 592952 66.049 ng 99 35) Ethyl tert-Butyl Ether 9.54 87 1093473 75.501 ng 98 36) 1,2-Dichloroethane 9.81 62 1063756 73.653 ng 99 38) 1,1,1-Trichloroethane 10.07 97 1309580 73.454 ng 100 39) Isopropyl Acetate 10.45 61 1204087 161.884 ng 95 40) 1-Butanol 10.47 56 1907268 147.404 ng 100 41) Benzene 10.53 78 3605353 72.073 ng 100 42) Carbon Tetrachloride 10.68 117 1143178 86.925 ng 100 43) Cyclohexane 10.81 84 2779506 147.276 ng 99 44) tert-Amyl Methyl Ether 11.13 73 2667755 75.898 ng 100 45) 1,2-Dichloropropane 11.35 63 950869 71.797 ng 100 46) Bromodichloromethane 11.53 83 1267521 81.613 ng 100 47) Trichloroethene 11.59 130 957828 65.386 ng 100 48) 1,4-Dioxane 11.56 88 765957 74.914 ng 99 49) 2,2,4-Trimethylpentane... 11.65 57 4011711 71.167 ng 100 130 of 156 R9042116.M Fri Apr 22 10:09:32 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211628.D Acq On : 22 Apr 2016 3:04 Operator: SC Sample : 50ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:08:27 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.78 100 745384 144.192 ng 98 51) n-Heptane 11.90 71 924987 73.136 ng 100 52) cis-1,3-Dichloropropene 12.43 75 1612602 79.797 ng 100 53) 4-Methyl-2-pentanone 12.47 58 909431 73.795 ng 99 54) trans-1,3-Dichloropropene 12.95 75 1387262 81.723 ng 100 55) 1,1,2-Trichloroethane 13.13 97 913621 74.165 ng 99 58) Toluene 13.42 91 3733116 63.855 ng 100 59) 2-Hexanone 13.67 43 2049725 79.449 ng 100 60) Dibromochloromethane 13.83 129 1065339 79.403 ng 99 61) 1,2-Dibromoethane 14.09 107 1051511 78.865 ng 100 62) n-Butyl Acetate 14.31 43 2352834 81.053 ng 100 63) n-Octane 14.44 57 819424 70.747 ng 99 64) Tetrachloroethene 14.58 166 987888 68.167 ng 100 65) Chlorobenzene 15.27 112 2421596 73.660 ng 100 66) Ethylbenzene 15.68 91 4225772 74.298 ng 100 67) m- & p-Xylenes 15.88 91 6726304 141.047 ng 100 68) Bromoform 15.93 173 937563 81.221 ng 100 69) Styrene 16.25 104 2670574 84.158 ng 99 70) o-Xylene 16.37 91 3382864 70.969 ng 100 71) n-Nonane 16.61 43 1839513 69.508 ng 100 72) 1,1,2,2-Tetrachloroethane 16.34 83 1702962 82.840 ng 100 74) Cumene 16.99 105 4197207 69.763 ng 100 75) alpha-Pinene 17.40 93 2190622 76.681 ng 100 76) n-Propylbenzene 17.52 91 5140799 69.103 ng 100 77) 3-Ethyltoluene 17.63 105 4176989 70.990 ng 100 78) 4-Ethyltoluene 17.68 105 4115709 73.062 ng 100 79) 1,3,5-Trimethylbenzene 17.76 105 3481174 70.175 ng 100 80) alpha-Methylstyrene 17.92 118 1899474 78.297 ng 99 81) 2-Ethyltoluene 17.96 105 4081789 70.442 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 3547713 71.597 ng 99 83) n-Decane 18.32 57 1961665 68.504 ng 99 84) Benzyl Chloride 18.33 91 3344740 93.636 ng 100 85) 1,3-Dichlorobenzene 18.35 146 2058612 79.486 ng 100 86) 1,4-Dichlorobenzene 18.41 146 2039597 74.220 ng 100 87) sec-Butylbenzene 18.48 105 4702054 71.310 ng 99 88) 4-Isopropyltoluene (p-... 18.65 119 4151770 66.658 ng 99 89) 1,2,3-Trimethylbenzene 18.64 105 3686637 71.575 ng 99 90) 1,2-Dichlorobenzene 18.77 146 1969969 73.728 ng 100 91) d-Limonene 18.80 68 1454962 74.657 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.24 157 741467 79.355 ng 98 93) n-Undecane 19.65 57 2085003 67.374 ng 100 94) 1,2,4-Trichlorobenzene 20.59 180 1433391 74.972 ng 99 95) Naphthalene 20.70 128 4581909 68.554 ng 99 96) n-Dodecane 20.74 57 2060072 73.447 ng 99 97) Hexachlorobutadiene 21.07 225 883291 66.758 ng 100 98) Cyclohexanone 16.02 55 1276586 77.103 ng 99 99) tert-Butylbenzene 18.19 119 3385895 70.300 ng 100 100) n-Butylbenzene 19.09 91 3872422 74.427 ng 100 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

131 of 156 R9042116.M Fri Apr 22 10:09:32 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211628.D Acq On : 22 Apr 2016 3:04 Operator: SC Sample : 50ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:08:27 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211628.D\data.ms

1.3e+07

1.25e+07

1.2e+07

1.15e+07

1.1e+07

1.05e+07 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T 1e+07 1,2,3-Trimethylbenzene,T4-Isopropyltoluene (p-Cymene),T

9500000

9000000 n-Decane,T

8500000 Benzyl Chloride,T 8000000 Diisopropyln-Hexane,T Ether,T 7500000 n-Butylbenzene,T Ethyl Acetate,T 7000000 n-Dodecane,T sec-Butylbenzene,T Cyclohexane,T Naphthalene,T n-Undecane,T

6500000 m- & p-Xylenes,T 3-Ethyltoluene,T 4-Ethyltoluene,T 1,3,5-Trimethylbenzene,T d-Limonene,T n-Propylbenzene,T 2-Ethyltoluene,T alpha-Methylstyrene,T Cumene,T

6000000 Vinyl Acetate,T Isopropyl Acetate,T o-Xylene,T 1,2-Dichlorobenzene,T 5500000 1,3-Dichlorobenzene,T alpha-Pinene,T Ethylbenzene,T 1,4-Dichlorobenzene,T Hexachlorobutadiene,T 1-Butanol,T Acetone,T n-Nonane,T 1,2,4-Trichlorobenzene,T 5000000 Styrene,T Methyl Methacrylate,T Toluene,T

4500000 n-Octane,T 2,2,4-Trimethylpentane (Isooctane),T Chlorobenzene,T

4000000 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Benzene,T n-Heptane,T

3500000 1,1,2,2-Tetrachloroethane,T n-Butyl Acetate,T 4-Methyl-2-pentanone,T tert-Amyl Methyl Ether,T Tetrachloroethene,T 2-Hexanone,T 2-Propanol (Isopropanol),T Propene,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Ethyl tert-Butyl Ether,T Cyclohexanone,T 3000000 Trichloroethene,T 1,1,2-Trichloroethane,T cis-1,3-Dichloropropene,T 1,2-Dibromo-3-Chloropropane,T Dichlorodifluoromethane (CFC 12),T trans-1,3-Dichloropropene,T Methyl tert-Butyl Ether,T 1,2-Dichloropropane,T Carbon Disulfide,T

2500000 Methylene Chloride,T Bromodichloromethane,T cis-1,2-Dichloroethene,T 1,1-Dichloroethene,T 1,3-Butadiene,T Trichlorotrifluoroethane,T Tetrahydrofuran (THF),T 1,1,1-Trichloroethane,T Dibromochloromethane,T trans-1,2-Dichloroethene,T 1,4-Dioxane,T Chloroform,T 2-Butanone (MEK),T Carbon Tetrachloride,T Bromoform,T

2000000 Trichlorofluoromethane,T Ethanol,T Chloromethane,T 1,2-Dibromoethane,T 3-Chloro-1-propene (Allyl Chloride),T 1,2-Dichloroethane,T 1,1-Dichloroethane,T Vinyl Chloride,T Acrylonitrile,T Acetonitrile,T Bromomethane,T 1500000 Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR Chloroethane,T 1,4-Difluorobenzene (IS2),IR Bromofluorobenzene (SS3),S

1000000 Acrolein,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

500000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00132 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:09:34 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211629.D Acq On : 22 Apr 2016 3:37 Operator: SC Sample : 100ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:09:50 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.94 130 119131 12.500 ng 0.02 37) 1,4-Difluorobenzene (IS2) 10.90 114 620652 12.500 ng 0.01 56) Chlorobenzene-d5 (IS3) 15.23 82 260628 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.71 65 191360 12.538 ng 0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.32% 57) Toluene-d8 (SS2) 13.32 98 612534 12.497 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.00% 73) Bromofluorobenzene (SS3) 16.84 174 205940 11.722 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 93.76%

Target Compounds Qvalue 2) Propene 3.68 42 1889394 177.746 ng 100 3) Dichlorodifluoromethan... 3.79 85 3458021 157.067 ng 99 4) Chloromethane 3.99 50 2757538 210.003 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.14 135 1865112 205.230 ng 99 6) Vinyl Chloride 4.26 62 2703477 191.764 ng 100 7) 1,3-Butadiene 4.44 54 1734010 265.282 ng 98 8) Bromomethane 4.74 94 1592430 169.429 ng 100 9) Chloroethane 4.95 64 1197213 147.166 ng 100 10) Ethanol 5.25 45 4996237 508.874 ng 99 11) Acetonitrile 5.42 41 2915213 118.143 ng 99 12) Acrolein 5.52 56 1176781 174.705 ng 93 13) Acetone 5.68 58 6450021 620.639 ng 95 14) Trichlorofluoromethane 5.81 101 2808355 178.109 ng 100 15) 2-Propanol (Isopropanol) 6.02 45 8706466 243.042 ng 99 16) Acrylonitrile 6.20 53 2536225 154.252 ng 99 17) 1,1-Dichloroethene 6.50 96 1771414 176.001 ng 98 18) 2-Methyl-2-Propanol (t... 6.66 59 8493580 262.843 ng 98 19) Methylene Chloride 6.67 84 1848102 146.120 ng 97 20) 3-Chloro-1-propene (Al... 6.78 41 2745082 195.005 ng 99 21) Trichlorotrifluoroethane 6.96 151 1463373 168.486 ng 97 22) Carbon Disulfide 6.91 76 6783177 168.852 ng 100 23) trans-1,2-Dichloroethene 7.68 61 2697301 149.697 ng 99 24) 1,1-Dichloroethane 7.90 63 3256768 139.722 ng 100 25) Methyl tert-Butyl Ether 7.96 73 5418379 143.548 ng 99 26) Vinyl Acetate 8.09 86 2044543 892.112 ng # 73 27) 2-Butanone (MEK) 8.32 72 1264650 144.472 ng 99 28) cis-1,2-Dichloroethene 8.77 61 2507771 153.734 ng 99 29) Diisopropyl Ether 9.00 87 1433297 125.103 ng # 80 30) Ethyl Acetate 9.02 61 1292718 266.606 ng 99 31) n-Hexane 9.00 57 2672953 116.285 ng 99 32) Chloroform 9.09 83 3049388 142.682 ng 99 34) Tetrahydrofuran (THF) 9.45 72 1190712 128.770 ng 98 35) Ethyl tert-Butyl Ether 9.55 87 2177152 145.946 ng 99 36) 1,2-Dichloroethane 9.82 62 2104595 141.473 ng 99 38) 1,1,1-Trichloroethane 10.08 97 2605515 140.526 ng 100 39) Isopropyl Acetate 10.46 61 2277592 294.443 ng # 89 40) 1-Butanol 10.49 56 3637969 270.356 ng 98 41) Benzene 10.54 78 7147147 137.385 ng 99 42) Carbon Tetrachloride 10.69 117 2293827 167.714 ng 99 43) Cyclohexane 10.81 84 5345292 272.342 ng 98 44) tert-Amyl Methyl Ether 11.14 73 5272913 144.250 ng 100 45) 1,2-Dichloropropane 11.35 63 1892517 137.404 ng 100 46) Bromodichloromethane 11.54 83 2517954 155.894 ng 99 47) Trichloroethene 11.59 130 1926723 126.472 ng 100 48) 1,4-Dioxane 11.57 88 1535457 144.402 ng 100 49) 2,2,4-Trimethylpentane... 11.65 57 7710333 131.523 ng 99 133 of 156 R9042116.M Fri Apr 22 10:11:20 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211629.D Acq On : 22 Apr 2016 3:37 Operator: SC Sample : 100ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:09:50 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.79 100 1485772 276.370 ng 98 51) n-Heptane 11.91 71 1825301 138.774 ng 100 52) cis-1,3-Dichloropropene 12.44 75 3203628 152.433 ng 100 53) 4-Methyl-2-pentanone 12.48 58 1782409 139.073 ng 97 54) trans-1,3-Dichloropropene 12.96 75 2755335 156.077 ng 100 55) 1,1,2-Trichloroethane 13.13 97 1824432 142.410 ng 99 58) Toluene 13.43 91 7295187 121.632 ng 99 59) 2-Hexanone 13.67 43 3949879 149.231 ng 99 60) Dibromochloromethane 13.83 129 2135917 155.174 ng 99 61) 1,2-Dibromoethane 14.09 107 2099906 153.517 ng 100 62) n-Butyl Acetate 14.32 43 4511266 151.483 ng 99 63) n-Octane 14.45 57 1586598 133.521 ng 99 64) Tetrachloroethene 14.58 166 2010804 135.244 ng 99 65) Chlorobenzene 15.28 112 4802623 142.394 ng 99 66) Ethylbenzene 15.68 91 8205117 140.617 ng 99 67) m- & p-Xylenes 15.88 91 13043919 266.611 ng 100 68) Bromoform 15.93 173 1927400 162.750 ng 100 69) Styrene 16.25 104 5279963 162.184 ng 99 70) o-Xylene 16.38 91 6614096 135.250 ng 100 71) n-Nonane 16.62 43 3388311 124.796 ng 97 72) 1,1,2,2-Tetrachloroethane 16.35 83 3347571 158.726 ng 100 74) Cumene 17.00 105 8108646 131.370 ng 99 75) alpha-Pinene 17.40 93 4288544 146.324 ng 100 76) n-Propylbenzene 17.53 91 9804183 128.459 ng 98 77) 3-Ethyltoluene 17.64 105 8194115 135.744 ng 99 78) 4-Ethyltoluene 17.68 105 7822507 135.356 ng 99 79) 1,3,5-Trimethylbenzene 17.76 105 6784316 133.304 ng 100 80) alpha-Methylstyrene 17.92 118 3740239 150.277 ng 98 81) 2-Ethyltoluene 17.96 105 7894768 132.802 ng 99 82) 1,2,4-Trimethylbenzene 18.20 105 6640905 130.635 ng 99 83) n-Decane 18.32 57 3383097 115.157 ng 95 84) Benzyl Chloride 18.33 91 6383399 174.188 ng 98 85) 1,3-Dichlorobenzene 18.35 146 4048371 152.363 ng 99 86) 1,4-Dichlorobenzene 18.42 146 4061977 144.078 ng 100 87) sec-Butylbenzene 18.48 105 8937623 132.120 ng 98 88) 4-Isopropyltoluene (p-... 18.65 119 7569454 118.459 ng 97 89) 1,2,3-Trimethylbenzene 18.65 105 6838836 129.419 ng 98 90) 1,2-Dichlorobenzene 18.78 146 3872743 141.279 ng 100 91) d-Limonene 18.80 68 2697627 134.924 ng 97 92) 1,2-Dibromo-3-Chloropr... 19.24 157 1505315 157.034 ng 99 93) n-Undecane 19.65 57 3808731 119.965 ng 97 94) 1,2,4-Trichlorobenzene 20.59 180 2924099 149.077 ng 99 95) Naphthalene 20.71 128 8823537 128.681 ng 98 96) n-Dodecane 20.74 57 3752388 130.402 ng 97 97) Hexachlorobutadiene 21.07 225 1828151 134.677 ng 100 98) Cyclohexanone 16.03 55 2514679 148.044 ng 99 99) tert-Butylbenzene 18.20 119 6299769 127.494 ng 98 100) n-Butylbenzene 19.09 91 7328682 137.296 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

134 of 156 R9042116.M Fri Apr 22 10:11:20 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211629.D Acq On : 22 Apr 2016 3:37 Operator: SC Sample : 100ng TO-15 ICAL STD Misc : S29-04191601/S29-04131603 (5/12) ALS Vial : 7 Sample Multiplier: 1

Quant Time: Apr 22 10:09:50 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 09:57:48 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211629.D\data.ms

2.3e+07

2.2e+07

2.1e+07

2e+07 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T

1.9e+07

1.8e+07 1,2,3-Trimethylbenzene,T4-Isopropyltoluene (p-Cymene),T

1.7e+07

1.6e+07

1.5e+07 Benzyl Chloride,T

1.4e+07 n-Butylbenzene,T n-Decane,T

1.3e+07 d-Limonene,T sec-Butylbenzene,T 4-Ethyltoluene,T Naphthalene,T n-Dodecane,T m- & p-Xylenes,T 1,3,5-Trimethylbenzene,T 3-Ethyltoluene,T n-Propylbenzene,T alpha-Methylstyrene,T 1.2e+07 2-Ethyltoluene,T Diisopropyl Ether,T n-Undecane,T Cyclohexane,T Cumene,T n-Hexane,T 1.1e+07 1,2-Dichlorobenzene,T o-Xylene,T 1,3-Dichlorobenzene,T Hexachlorobutadiene,T Ethyl Acetate,T 1,4-Dichlorobenzene,T alpha-Pinene,T 1e+07 Ethylbenzene,T 1,2,4-Trichlorobenzene,T Styrene,T n-Nonane,T Vinyl Acetate,T Toluene,T Isopropyl Acetate,T

9000000 Methyl Methacrylate,T n-Octane,T Acetone,T Chlorobenzene,T

8000000 2,2,4-Trimethylpentane (Isooctane),T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T n-Heptane,T Benzene,T

7000000 1,1,2,2-Tetrachloroethane,T Tetrachloroethene,T n-Butyl Acetate,T 1-Butanol,T tert-Amyl Methyl Ether,T 4-Methyl-2-pentanone,T Methylene Chloride,T 2-Hexanone,T Propene,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Cyclohexanone,T 6000000 Trichloroethene,T 1,2-Dibromo-3-Chloropropane,T Ethyl tert-Butyl Ether,T 1,1,2-Trichloroethane,T 2-Propanol (Isopropanol),T cis-1,3-Dichloropropene,T Dichlorodifluoromethane (CFC 12),T trans-1,3-Dichloropropene,T

5000000 1,2-Dichloropropane,T Carbon Disulfide,T Methyl tert-Butyl Ether,T 1,4-Dioxane,T Bromodichloromethane,T Trichlorotrifluoroethane,T cis-1,2-Dichloroethene,T 1,1-Dichloroethene,T 1,3-Butadiene,T Dibromochloromethane,T 1,1,1-Trichloroethane,T Tetrahydrofuran (THF),T Bromoform,T trans-1,2-Dichloroethene,T Carbon Tetrachloride,T Chloroform,T 4000000 2-Butanone (MEK),T Trichlorofluoromethane,T 1,2-Dibromoethane,T 1,2-Dichloroethane,T 3-Chloro-1-propene (Allyl Chloride),T 1,1-Dichloroethane,T Vinyl Chloride,T Ethanol,T Chloromethane,T Acrylonitrile,T 3000000 Bromomethane,T Acetonitrile,T

2000000 Chloroethane,T Toluene-d8 (SS2),S Chlorobenzene-d5 (IS3),IR 1,4-Difluorobenzene (IS2),IR Acrolein,T Bromofluorobenzene (SS3),S Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S 1000000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00135 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:11:23 2016 Page: 3 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211632.D Acq On : 22 Apr 2016 5:19 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-04191601/S29-04141603 (5/12) ALS Vial : 2 Sample Multiplier: 1

Quant Time: Apr 22 10:44:26 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.92 130 126707 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.88 114 651221 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.23 82 272477 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.70 65 197885 11.976 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 95.84% 57) Toluene-d8 (SS2) 13.32 98 645755 12.592 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 100.72% 73) Bromofluorobenzene (SS3) 16.84 174 219280 12.945 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 103.52%

Target Compounds Qvalue 2) Propene 3.67 42 484698 25.273 ng 100 3) Dichlorodifluoromethan... 3.78 85 883224 23.540 ng 99 4) Chloromethane 3.97 50 792324 25.077 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.13 135 486162 26.072 ng 99 6) Vinyl Chloride 4.25 62 687280 25.694 ng 100 7) 1,3-Butadiene 4.42 54 445820 32.954 ng 98 8) Bromomethane 4.72 94 441129 27.904 ng 99 9) Chloroethane 4.93 64 335653 25.887 ng 99 10) Ethanol 5.20 45 1910801 155.839 ng 100 11) Acetonitrile 5.38 41 953494 27.485 ng 100 12) Acrolein 5.49 56 305930 29.819 ng 99 13) Acetone 5.64 58 1925320 133.938 ng 97 14) Trichlorofluoromethane 5.79 101 734984 24.410 ng 100 15) 2-Propanol (Isopropanol) 5.98 45 2608832 56.638 ng 100 16) Acrylonitrile 6.16 53 692867 28.758 ng 100 17) 1,1-Dichloroethene 6.48 96 480532 28.975 ng 99 18) 2-Methyl-2-Propanol (t... 6.61 59 2601582 57.312 ng 99 19) Methylene Chloride 6.65 84 512201 24.729 ng 99 20) 3-Chloro-1-propene (Al... 6.76 41 730018 28.206 ng 99 21) Trichlorotrifluoroethane 6.94 151 397464 28.125 ng 97 22) Carbon Disulfide 6.90 76 1711905 26.164 ng 100 23) trans-1,2-Dichloroethene 7.66 61 710226 29.153 ng 98 24) 1,1-Dichloroethane 7.88 63 891410 26.977 ng 100 25) Methyl tert-Butyl Ether 7.94 73 1498735 27.942 ng 99 26) Vinyl Acetate 8.06 86 578824 157.108 ng 98 27) 2-Butanone (MEK) 8.29 72 350099 30.781 ng 100 28) cis-1,2-Dichloroethene 8.76 61 689007 28.835 ng 99 29) Diisopropyl Ether 8.99 87 407360 28.034 ng 98 30) Ethyl Acetate 8.99 61 390994 60.828 ng 99 31) n-Hexane 8.99 57 815497 26.032 ng 100 32) Chloroform 9.06 83 844249 28.332 ng 99 34) Tetrahydrofuran (THF) 9.44 72 344182 27.500 ng 100 35) Ethyl tert-Butyl Ether 9.53 87 598910 28.634 ng 99 36) 1,2-Dichloroethane 9.81 62 581922 28.277 ng 100 38) 1,1,1-Trichloroethane 10.06 97 712568 28.187 ng 100 39) Isopropyl Acetate 10.44 61 670415 61.114 ng 98 40) 1-Butanol 10.46 56 1104289 66.967 ng 99 41) Benzene 10.52 78 2005506 25.917 ng 100 42) Carbon Tetrachloride 10.67 117 608410 29.366 ng 99 43) Cyclohexane 10.80 84 1524811 55.512 ng 99 44) tert-Amyl Methyl Ether 11.13 73 1471359 28.413 ng 99 45) 1,2-Dichloropropane 11.34 63 525535 28.409 ng 99 46) Bromodichloromethane 11.52 83 676110 29.460 ng 100 47) Trichloroethene 11.58 130 521587 28.138 ng 99 48) 1,4-Dioxane 11.55 88 434204 33.126 ng 100 49) 2,2,4-Trimethylpentane... 11.64 57 2200143 26.934 ng 99 136 of 156 R9042116.M Fri Apr 22 10:45:22 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211632.D Acq On : 22 Apr 2016 5:19 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-04191601/S29-04141603 (5/12) ALS Vial : 2 Sample Multiplier: 1

Quant Time: Apr 22 10:44:26 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 415336 62.452 ng 99 51) n-Heptane 11.90 71 505627 27.860 ng 99 52) cis-1,3-Dichloropropene 12.43 75 793822 30.277 ng 100 53) 4-Methyl-2-pentanone 12.46 58 502752 30.899 ng 99 54) trans-1,3-Dichloropropene 12.95 75 718404 29.972 ng 100 55) 1,1,2-Trichloroethane 13.12 97 502396 29.824 ng 100 58) Toluene 13.42 91 2085241 28.273 ng 100 59) 2-Hexanone 13.66 43 1159286 33.065 ng 100 60) Dibromochloromethane 13.83 129 566952 31.939 ng 100 61) 1,2-Dibromoethane 14.08 107 570584 32.214 ng 99 62) n-Butyl Acetate 14.31 43 1319893 32.851 ng 100 63) n-Octane 14.44 57 446883 27.602 ng 99 64) Tetrachloroethene 14.57 166 540098 28.235 ng 100 65) Chlorobenzene 15.27 112 1348259 30.106 ng 100 66) Ethylbenzene 15.68 91 2352009 30.167 ng 100 67) m- & p-Xylenes 15.87 91 3721514 59.757 ng 100 68) Bromoform 15.93 173 483831 32.240 ng 99 69) Styrene 16.25 104 1490426 33.144 ng 100 70) o-Xylene 16.37 91 1868316 28.928 ng 99 71) n-Nonane 16.61 43 1016576 27.060 ng 100 72) 1,1,2,2-Tetrachloroethane 16.34 83 927775 30.473 ng 100 74) Cumene 16.99 105 2320942 28.752 ng 100 75) alpha-Pinene 17.40 93 1218318 29.916 ng 99 76) n-Propylbenzene 17.52 91 2844716 28.545 ng 100 77) 3-Ethyltoluene 17.63 105 2380204 30.705 ng 100 78) 4-Ethyltoluene 17.68 105 2231530 30.061 ng 100 79) 1,3,5-Trimethylbenzene 17.76 105 1933112 30.263 ng 99 80) alpha-Methylstyrene 17.91 118 1067842 32.504 ng 100 81) 2-Ethyltoluene 17.95 105 2255089 29.980 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 2007445 31.842 ng 99 83) n-Decane 18.31 57 1109521 29.114 ng 100 84) Benzyl Chloride 18.32 91 1862393 33.940 ng 100 85) 1,3-Dichlorobenzene 18.34 146 1161376 35.277 ng 100 86) 1,4-Dichlorobenzene 18.41 146 1143242 33.900 ng 100 87) sec-Butylbenzene 18.48 105 2596976 30.681 ng 100 88) 4-Isopropyltoluene (p-... 18.64 119 2353038 30.269 ng 99 89) 1,2,3-Trimethylbenzene 18.64 105 2062575 31.762 ng 99 90) 1,2-Dichlorobenzene 18.77 146 1104502 34.137 ng 100 91) d-Limonene 18.80 68 815683 31.180 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.23 157 409317 31.122 ng 98 93) n-Undecane 19.65 57 1170281 31.189 ng 100 94) 1,2,4-Trichlorobenzene 20.59 180 869329 33.795 ng 100 95) Naphthalene 20.70 128 2914650 33.480 ng 100 96) n-Dodecane 20.74 57 1229587 31.620 ng 100 97) Hexachlorobutadiene 21.07 225 486474 35.244 ng 100 98) Cyclohexanone 16.02 55 721930 33.349 ng 99 99) tert-Butylbenzene 18.19 119 1873904 30.322 ng 100 100) n-Butylbenzene 19.09 91 2160581 32.747 ng 100 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

137 of 156 R9042116.M Fri Apr 22 10:45:22 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_04\21\04211632.D Acq On : 22 Apr 2016 5:19 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-04191601/S29-04141603 (5/12) ALS Vial : 2 Sample Multiplier: 1

Quant Time: Apr 22 10:44:26 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 04211632.D\data.ms

7500000

7000000

6500000 1,2,3-Trimethylbenzene,T

6000000 4-Isopropyltoluene (p-Cymene),T 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T

5500000

5000000 n-Decane,T Benzyl Chloride,T Diisopropyln-Hexane,T Ether,T Ethyl Acetate,T

4500000 Naphthalene,T n-Dodecane,T 4000000 n-Butylbenzene,T d-Limonene,T n-Undecane,T sec-Butylbenzene,T Cyclohexane,T 4-Ethyltoluene,T Isopropyl Acetate,T Vinyl Acetate,T 2-Ethyltoluene,T m- & p-Xylenes,T n-Propylbenzene,T 3-Ethyltoluene,T 1,3,5-Trimethylbenzene,T

3500000 alpha-Methylstyrene,T 1-Butanol,T Cumene,T 1,3-Dichlorobenzene,T 1,2-Dichlorobenzene,T o-Xylene,T Acetone,T Ethylbenzene,T 1,2,4-Trichlorobenzene,T

3000000 alpha-Pinene,T 1,4-Dichlorobenzene,T Hexachlorobutadiene,T n-Nonane,T Styrene,T Methyl Methacrylate,T Toluene,T

2500000 n-Octane,T 2,2,4-Trimethylpentane (Isooctane),T Chlorobenzene,T Benzene,T n-Heptane,T

2000000 2-Methyl-2-Propanol (tert-Butyl Alcohol,T n-Butyl Acetate,T 4-Methyl-2-pentanone,T 1,1,2,2-Tetrachloroethane,T tert-Amyl Methyl Ether,T 2-Hexanone,T Tetrachloroethene,T 2-Propanol (Isopropanol),T Propene,T Ethyl tert-Butyl Ether,T Trichloroethene,T Cyclohexanone,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 1,2-Dibromo-3-Chloropropane,T 1,1,2-Trichloroethane,T

1500000 cis-1,3-Dichloropropene,T Methyl tert-Butyl Ether,T Dichlorodifluoromethane (CFC 12),T 1,2-Dichloropropane,T trans-1,3-Dichloropropene,T Tetrahydrofuran (THF),T cis-1,2-Dichloroethene,T Carbon Disulfide,T Trichlorotrifluoroethane,T Ethanol,T 1,1-Dichloroethene,T 1,3-Butadiene,T Methylene Chloride,T Bromodichloromethane,T 1,1,1-Trichloroethane,T Chloroform,T trans-1,2-Dichloroethene,T 2-Butanone (MEK),T Dibromochloromethane,T 1,4-Dioxane,T Toluene-d8 (SS2),S Carbon Tetrachloride,T Bromoform,T Trichlorofluoromethane,T Chloromethane,T Chlorobenzene-d5 (IS3),IR 3-Chloro-1-propene (Allyl Chloride),T 1,1-Dichloroethane,T 1,2-Dibromoethane,T 1,4-Difluorobenzene (IS2),IR Vinyl Chloride,T 1,2-Dichloroethane,T Bromofluorobenzene (SS3),S

1000000 Acrylonitrile,T Acetonitrile,T Bromomethane,T Chloroethane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S 500000 Acrolein,T

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00138 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Fri Apr 22 10:45:24 2016 Page: 3 INITIAL CALIBRATION VERIFICATION CHECK SHEET

Data File Name: 04211632.D Acq. Method File: TO15.M Data File Path: I:\MS09\Data\2016_04\21\ Sample Name: 25ng TO-15 ICV STD Operator: SC Misc Info: S29-04191601/S29-04141603 ( Date Acquired: 4/22/16 5:19 Instrument Name: MS09

Compound Ret. Amt. Spike % Lower Upper * OR # Name Time (ng) Amt.(ng) Rec. Limit Limit Fail 2) Propene 3.67 25.3 24.50 103 70 130 * 3) Dichlorodifluoromethane (CFC 12 3.78 23.5 23.50 100 70 130 * 4) Chloromethane 3.97 25.1 25.00 100 70 130 * 5) 1,2-Dichloro-1,1,2,2-tetrafluoroeth 4.13 26.1 25.50 102 70 130 * 6) Vinyl Chloride 4.25 25.7 25.00 103 70 130 * 7) 1,3-Butadiene 4.42 33.0 25.75 128 70 130 * 8) Bromomethane 4.72 27.9 25.25 110 70 130 * 9) Chloroethane 4.93 25.9 25.00 104 70 130 * 10) Ethanol 5.20 156 124.75 125 70 130 * 11) Acetonitrile 5.38 27.5 26.50 104 70 130 * 12) Acrolein 5.49 29.8 26.75 111 70 130 * 13) Acetone 5.64 134 134.75 99 70 130 * 14) Trichlorofluoromethane 5.79 24.4 27.00 90 70 130 * 15) 2-Propanol (Isopropanol) 5.98 56.6 52.25 108 70 130 * 16) Acrylonitrile 6.16 28.8 26.50 109 70 130 * 17) 1,1-Dichloroethene 6.48 29.0 27.00 107 70 130 * 18) 2-Methyl-2-Propanol (tert-Butyl Alco 6.61 57.3 50.00 115 70 130 * 19) Methylene Chloride 6.65 24.7 27.75 89 70 130 * 20) 3-Chloro-1-propene (Allyl Chlorid 6.76 28.2 27.25 103 70 130 * 21) Trichlorotrifluoroethane 6.94 28.1 27.50 102 70 130 * 22) Carbon Disulfide 6.90 26.2 26.25 100 70 130 * 23) trans-1,2-Dichloroethene 7.66 29.2 26.25 111 70 130 * 24) 1,1-Dichloroethane 7.88 27.0 26.50 102 70 130 * 25) Methyl tert-Butyl Ether 7.94 27.9 27.00 103 70 130 * 26) Vinyl Acetate 8.06 157 129.75 121 70 130 * 27) 2-Butanone (MEK) 8.29 30.8 27.50 112 70 130 * 28) cis-1,2-Dichloroethene 8.76 28.8 27.25 106 70 130 * 29) Diisopropyl Ether 8.99 28.0 27.00 104 70 130 * 30) Ethyl Acetate 8.99 60.8 53.50 114 70 130 * 31) n-Hexane 8.99 26.0 26.50 98 70 130 * 32) Chloroform 9.06 28.3 28.00 101 70 130 * 34) Tetrahydrofuran (THF) 9.44 27.5 27.50 100 70 130 * 35) Ethyl tert-Butyl Ether 9.53 28.6 26.75 107 70 130 * 36) 1,2-Dichloroethane 9.81 28.3 26.75 106 70 130 * 38) 1,1,1-Trichloroethane 10.06 28.2 26.25 107 70 130 * 39) Isopropyl Acetate 10.44 61.1 57.25 107 70 130 * 40) 1-Butanol 10.46 67.0 51.25 131 70 130 FAIL 41) Benzene 10.52 25.9 28.25 92 70 130 * 42) Carbon Tetrachloride 10.67 29.4 28.75 102 70 130 * 43) Cyclohexane 10.80 55.5 53.00 105 70 130 * 44) tert-Amyl Methyl Ether 11.13 28.4 26.75 106 70 130 * 45) 1,2-Dichloropropane 11.34 28.4 27.00 105 70 130 * 46) Bromodichloromethane 11.52 29.5 27.25 108 70 130 * 47) Trichloroethene 11.58 28.1 27.00 104 70 130 * 48) 1,4-Dioxane 11.55 33.1 26.25 126 70 130 * 49) 2,2,4-Trimethylpentane (Isooctane) 11.64 26.9 26.75 101 70 130 *

Page 1 of 2 I:\MS09\0-Instrument Info\0-Security Certificates\ICV_07141501.CRT 4/22/16 10:46 AM 139 of 156 INITIAL CALIBRATION VERIFICATION CHECK SHEET

Data File Name: 04211632.D Acq. Method File: TO15.M Data File Path: I:\MS09\Data\2016_04\21\ Sample Name: 25ng TO-15 ICV STD Operator: SC Misc Info: S29-04191601/S29-04141603 ( Date Acquired: 4/22/16 5:19 Instrument Name: MS09 Compound Ret. Amt. Spike % Lower Upper * OR # Name Time (ng) Amt.(ng) Rec. Limit Limit Fail 50) Methyl Methacrylate 11.77 62.5 52.75 118 70 130 * 51) n-Heptane 11.90 27.9 27.00 103 70 130 * 52) cis-1,3-Dichloropropene 12.43 30.3 26.00 117 70 130 * 53) 4-Methyl-2-pentanone 12.46 30.9 27.50 112 70 130 * 54) trans-1,3-Dichloropropene 12.95 30.0 26.25 114 70 130 * 55) 1,1,2-Trichloroethane 13.12 29.8 27.00 110 70 130 * 58) Toluene 13.42 28.3 27.25 104 70 130 * 59) 2-Hexanone 13.66 33.1 27.50 120 70 130 * 60) Dibromochloromethane 13.83 31.9 27.50 116 70 130 * 61) 1,2-Dibromoethane 14.08 32.2 27.25 118 70 130 * 62) n-Butyl Acetate 14.31 32.9 28.25 116 70 130 * 63) n-Octane 14.44 27.6 26.25 105 70 130 * 64) Tetrachloroethene 14.57 28.2 25.25 112 70 130 * 65) Chlorobenzene 15.27 30.1 27.50 109 70 130 * 66) Ethylbenzene 15.68 30.2 27.25 111 70 130 * 67) m- & p-Xylenes 15.87 59.8 53.50 112 70 130 * 68) Bromoform 15.93 32.2 28.50 113 70 130 * 69) Styrene 16.25 33.1 27.75 119 70 130 * 70) o-Xylene 16.37 28.9 26.25 110 70 130 * 71) n-Nonane 16.61 27.1 25.50 106 70 130 * 72) 1,1,2,2-Tetrachloroethane 16.34 30.5 26.25 116 70 130 * 74) Cumene 16.99 28.8 26.00 111 70 130 * 75) alpha-Pinene 17.40 29.9 26.50 113 70 130 * 76) n-Propylbenzene 17.52 28.5 25.50 112 70 130 * 77) 3-Ethyltoluene 17.63 30.7 26.75 115 70 130 * 78) 4-Ethyltoluene 17.68 30.1 26.75 113 70 130 * 79) 1,3,5-Trimethylbenzene 17.76 30.3 26.75 113 70 130 * 80) alpha-Methylstyrene 17.91 32.5 26.25 124 70 130 * 81) 2-Ethyltoluene 17.95 30.0 26.75 112 70 130 * 82) 1,2,4-Trimethylbenzene 18.19 31.8 27.25 117 70 130 * 83) n-Decane 18.31 29.1 26.25 111 70 130 * 84) Benzyl Chloride 18.32 33.9 27.50 123 70 130 * 85) 1,3-Dichlorobenzene 18.34 35.3 28.50 124 70 130 * 86) 1,4-Dichlorobenzene 18.41 33.9 26.00 130 70 130 * 87) sec-Butylbenzene 18.48 30.7 27.25 113 70 130 * 88) 4-Isopropyltoluene (p-Cymene) 18.64 30.3 26.00 117 70 130 * 89) 1,2,3-Trimethylbenzene 18.64 31.8 26.50 120 70 130 * 90) 1,2-Dichlorobenzene 18.77 34.1 27.50 124 70 130 * 91) d-Limonene 18.80 31.2 26.25 119 70 130 * 92) 1,2-Dibromo-3-Chloropropane 19.23 31.1 27.25 114 70 130 * 93) n-Undecane 19.65 31.2 25.25 124 70 130 * 94) 1,2,4-Trichlorobenzene 20.59 33.8 28.75 118 70 130 * 95) Naphthalene 20.70 33.5 27.25 123 70 130 * 96) n-Dodecane 20.74 31.6 27.25 116 70 130 * 97) Hexachlorobutadiene 21.07 35.2 28.75 122 70 130 * 98) Cyclohexanone 16.02 33.3 27.50 121 70 130 * 99) tert-Butylbenzene 18.19 30.3 26.75 113 70 130 * 100) n-Butylbenzene 19.09 32.7 28.00 117 70 130 * Bold = 75 Compound List * = Pass Page 2 of 2 I:\MS09\0-Instrument Info\0-Security Certificates\ICV_07141501.CRT 4/22/16 10:47 AM 140 of 156 Evaluate Continuing Calibration Report

Data File: I:\MS09\Data\2016_05\25\05251601.D Acq On : 24 May 2016 23:11 Operator: WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1

Quant Time: May 25 06:28:24 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200%

Compound AvgRF CCRF %Dev Area% Dev(min) ------1 IR Bromochloromethane (IS1) 1.000 1.000 0.0 88 -0.04 2 T Propene 1.892 1.533 19.0 78 0.00 3 T Dichlorodifluoromethane (CF 3.701 3.273 11.6 79 0.00 4 T Chloromethane 3.117 2.474 20.6 71 -0.02 5 T 1,2-Dichloro-1,1,2,2-tetraf 1.840 1.609 12.6 80 0.00 6 T Vinyl Chloride 2.639 2.211 16.2 75 -0.02 7 T 1,3-Butadiene 1.335 1.591 -19.2 122 -0.02 8 T Bromomethane 1.560 1.519 2.6 87 -0.03 9 T Chloroethane 1.279 1.178 7.9 87 -0.02 10 T Ethanol 1.210 1.185 2.1 90 -0.10 11 T Acetonitrile 3.422 2.806 18.0 84 -0.07 12 T Acrolein 1.012 0.946 6.5 77 -0.04 13 T Acetone 1.418 1.114 21.4 72 -0.06 14 T Trichlorofluoromethane 2.970 2.654 10.6 81 -0.02 15 T 2-Propanol (Isopropanol) 4.544 3.889 14.4 71 -0.08 16 T Acrylonitrile 2.377 2.009 15.5 71 -0.06 17 T 1,1-Dichloroethene 1.636 1.453 11.2 80 -0.02 18 T 2-Methyl-2-Propanol (tert-B 4.478 3.915 12.6 74 -0.08 19 T Methylene Chloride 2.043 1.523 25.5 75 -0.05 20 T 3-Chloro-1-propene (Allyl C 2.553 2.003 21.5 63 -0.03 21 T Trichlorotrifluoroethane 1.394 1.227 12.0 82 -0.02 22 T Carbon Disulfide 6.455 5.822 9.8 77 -0.02 23 T trans-1,2-Dichloroethene 2.403 2.101 12.6 73 -0.03 24 T 1,1-Dichloroethane 3.260 2.702 17.1 74 -0.04 25 T Methyl tert-Butyl Ether 5.291 4.548 14.0 77 -0.03 26 T Vinyl Acetate 0.363 0.330 9.1 79 -0.05 27 T 2-Butanone (MEK) 1.122 0.995 11.3 75 -0.05 28 T cis-1,2-Dichloroethene 2.357 1.997 15.3 74 -0.03 29 T Diisopropyl Ether 1.434 1.220 14.9 78 -0.03 30 T Ethyl Acetate 0.634 0.554 12.6 72 -0.04 31 T n-Hexane 3.090 2.576 16.6 75 -0.02 32 T Chloroform 2.940 2.565 12.8 79 -0.05 33 S 1,2-Dichloroethane-d4(SS1) 1.630 1.605 1.5 87 -0.03 34 T Tetrahydrofuran (THF) 1.235 0.999 19.1 74 -0.02 35 T Ethyl tert-Butyl Ether 2.063 1.803 12.6 78 -0.02 36 T 1,2-Dichloroethane 2.030 1.820 10.3 78 -0.03

37 IR 1,4-Difluorobenzene (IS2) 1.000 1.000 0.0 89 -0.02 38 T 1,1,1-Trichloroethane 0.485 0.438 9.7 79 -0.03 39 T Isopropyl Acetate 0.211 0.177 16.1 72 -0.02 40 T 1-Butanol 0.317 0.282 11.0 68 -0.05 41 T Benzene 1.485 1.104 25.7 75 -0.03 42 T Carbon Tetrachloride 0.398 0.356 10.6 79 -0.02 43 T Cyclohexane 0.527 0.450 14.6 77 -0.02 44 T tert-Amyl Methyl Ether 0.994 0.863 13.2 78 -0.02 45 T 1,2-Dichloropropane 0.355 0.296 16.6 74 -0.02 46 T Bromodichloromethane 0.441 0.387 12.2 77 -0.02 47 T Trichloroethene 0.356 0.322 9.6 79 -0.02 48 T 1,4-Dioxane 0.252 0.235 6.7 77 -0.02 49 T 2,2,4-Trimethylpentane (Iso 1.568 1.285 18.0 74 -0.02 50 T Methyl Methacrylate 0.128 0.119 7.0 77 -0.02 51 T n-Heptane 0.348 0.292 16.1 77 -0.02 52 T cis-1,3-Dichloropropene 0.503 0.460 8.5 75 -0.01 53 T 4-Methyl-2-pentanone 0.312 0.270 13.5 72 -0.02 54 T trans-1,3-Dichloropropene 0.460 0.396 13.9 74 -0.01 141 of 156 R9042116.M Wed May 25 17:18:36 2016 Page: 1 Evaluate Continuing Calibration Report

Data File: I:\MS09\Data\2016_05\25\05251601.D Acq On : 24 May 2016 23:11 Operator: WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1

Quant Time: May 25 06:28:24 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200%

Compound AvgRF CCRF %Dev Area% Dev(min) ------55 T 1,1,2-Trichloroethane 0.323 0.288 10.8 77 -0.02

56 IR Chlorobenzene-d5 (IS3) 1.000 1.000 0.0 88 -0.01 57 S Toluene-d8 (SS2) 2.353 2.345 0.3 88 -0.01 58 T Toluene 3.383 2.892 14.5 78 -0.01 59 T 2-Hexanone 1.608 1.461 9.1 71 -0.01 60 T Dibromochloromethane 0.814 0.768 5.7 80 -0.01 61 T 1,2-Dibromoethane 0.813 0.757 6.9 78 -0.01 62 T n-Butyl Acetate 1.843 1.619 12.2 70 -0.01 63 T n-Octane 0.743 0.617 17.0 75 -0.01 64 T Tetrachloroethene 0.878 0.835 4.9 84 0.00 65 T Chlorobenzene 2.054 1.840 10.4 79 -0.01 66 T Ethylbenzene 3.577 3.227 9.8 77 0.00 67 T m- & p-Xylenes 2.857 2.601 9.0 78 -0.02 68 T Bromoform 0.688 0.665 3.3 81 -0.01 69 T Styrene 2.063 1.938 6.1 78 -0.01 70 T o-Xylene 2.963 2.674 9.8 79 -0.02 71 T n-Nonane 1.723 1.448 16.0 73 -0.01 72 T 1,1,2,2-Tetrachloroethane 1.397 1.307 6.4 77 -0.01 73 S Bromofluorobenzene (SS3) 0.777 0.879 -13.1 99 0.00 74 T Cumene 3.703 3.404 8.1 80 -0.01 75 T alpha-Pinene 1.868 1.688 9.6 79 0.00 76 T n-Propylbenzene 4.572 4.193 8.3 77 0.00 77 T 3-Ethyltoluene 3.556 3.258 8.4 79 -0.01 78 T 4-Ethyltoluene 3.405 3.181 6.6 78 0.00 79 T 1,3,5-Trimethylbenzene 2.930 2.709 7.5 78 -0.01 80 T alpha-Methylstyrene 1.507 1.441 4.4 75 -0.01 81 T 2-Ethyltoluene 3.451 3.217 6.8 80 -0.02 82 T 1,2,4-Trimethylbenzene 2.892 2.744 5.1 79 -0.01 83 T n-Decane 1.748 1.563 10.6 74 0.00 84 T Benzyl Chloride 2.517 2.075 17.6 73 -0.02 85 T 1,3-Dichlorobenzene 1.510 1.519 -0.6 81 -0.02 86 T 1,4-Dichlorobenzene 1.547 1.563 -1.0 80 -0.01 87 T sec-Butylbenzene 3.883 3.666 5.6 79 -0.01 88 T 4-Isopropyltoluene (p-Cymen 3.566 3.439 3.6 79 -0.01 89 T 1,2,3-Trimethylbenzene 2.979 2.858 4.1 79 -0.01 90 T 1,2-Dichlorobenzene 1.484 1.508 -1.6 81 -0.01 91 T d-Limonene 1.200 1.071 10.8 72 0.00 92 T 1,2-Dibromo-3-Chloropropane 0.603 0.544 9.8 81 0.00 93 T n-Undecane 1.721 1.637 4.9 73 0.00 94 T 1,2,4-Trichlorobenzene 1.180 1.096 7.1 79 0.00 95 T Naphthalene 3.994 3.801 4.8 76 0.00 96 T n-Dodecane 1.784 1.564 12.3 68 0.00 97 T Hexachlorobutadiene 0.633 0.653 -3.2 83 0.00 98 T Cyclohexanone 0.993 0.907 8.7 69 -0.02 99 T tert-Butylbenzene 2.835 2.666 6.0 80 -0.02 100 T n-Butylbenzene 3.027 2.910 3.9 77 -0.01 ------

(#) = Out of Range SPCC's out = 0 CCC's out = 0

142 of 156 R9042116.M Wed May 25 17:18:36 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251601.D Acq On : 24 May 2016 23:11 Operator: WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1

Quant Time: May 25 06:28:24 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.90 130 99860 12.500 ng -0.04 37) 1,4-Difluorobenzene (IS2) 10.88 114 517535 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.22 82 218283 12.500 ng -0.01

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.68 65 160247 12.306 ng -0.03 Spiked Amount 12.500 Range 70 - 130 Recovery = 98.48% 57) Toluene-d8 (SS2) 13.31 98 511801 12.458 ng -0.01 Spiked Amount 12.500 Range 70 - 130 Recovery = 99.68% 73) Bromofluorobenzene (SS3) 16.84 174 191972 14.146 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 113.20%

Target Compounds Qvalue 2) Propene 3.68 42 63052 4.172 ng 98 3) Dichlorodifluoromethan... 3.78 85 130720 4.421 ng 100 4) Chloromethane 3.97 50 96830 3.889 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.14 135 66211 4.505 ng 100 6) Vinyl Chloride 4.25 62 88311 4.189 ng 99 7) 1,3-Butadiene 4.42 54 67374 6.319 ng 97 8) Bromomethane 4.72 94 60662 4.869 ng 97 9) Chloroethane 4.93 64 47521 4.650 ng 100 10) Ethanol 5.16 45 239605 24.795 ng 98 11) Acetonitrile 5.35 41 114335 4.182 ng 97 12) Acrolein 5.48 56 40418 4.999 ng 96 13) Acetone 5.61 58 239002 21.097 ng 95 14) Trichlorofluoromethane 5.79 101 104958 4.423 ng 100 15) 2-Propanol (Isopropanol) 5.94 45 324647 8.943 ng 97 16) Acrylonitrile 6.14 53 82635 4.352 ng 100 17) 1,1-Dichloroethene 6.48 96 62115 4.752 ng 99 18) 2-Methyl-2-Propanol (t... 6.58 59 326797 9.135 ng 99 19) Methylene Chloride 6.63 84 65690 4.024 ng 96 20) 3-Chloro-1-propene (Al... 6.75 41 86410 4.236 ng 100 21) Trichlorotrifluoroethane 6.93 151 52947 4.754 ng 99 22) Carbon Disulfide 6.90 76 227922 4.420 ng 100 23) trans-1,2-Dichloroethene 7.65 61 88951 4.633 ng 97 24) 1,1-Dichloroethane 7.86 63 112240 4.310 ng 99 25) Methyl tert-Butyl Ether 7.93 73 190759 4.513 ng 99 26) Vinyl Acetate 8.04 86 66790 23.002 ng # 95 27) 2-Butanone (MEK) 8.28 72 42525 4.744 ng 99 28) cis-1,2-Dichloroethene 8.74 61 85345 4.532 ng 98 29) Diisopropyl Ether 8.98 87 52615 4.594 ng 98 30) Ethyl Acetate 8.98 61 46930 9.264 ng 98 31) n-Hexane 8.98 57 107014 4.334 ng 98 32) Chloroform 9.04 83 109632 4.668 ng 99 34) Tetrahydrofuran (THF) 9.44 72 40696 4.126 ng 98 35) Ethyl tert-Butyl Ether 9.53 87 75614 4.587 ng 98 36) 1,2-Dichloroethane 9.79 62 76343 4.707 ng 100 38) 1,1,1-Trichloroethane 10.05 97 93491 4.654 ng 100 39) Isopropyl Acetate 10.44 61 81169 9.311 ng 94 40) 1-Butanol 10.45 56 132040 10.076 ng 97 41) Benzene 10.51 78 253588 4.124 ng 98 42) Carbon Tetrachloride 10.67 117 79584 4.834 ng 100 43) Cyclohexane 10.80 84 194486 8.909 ng 99 44) tert-Amyl Methyl Ether 11.12 73 185799 4.515 ng 100 45) 1,2-Dichloropropane 11.33 63 64304 4.374 ng 99 46) Bromodichloromethane 11.52 83 85791 4.704 ng 99 47) Trichloroethene 11.57 130 68643 4.660 ng 99 48) 1,4-Dioxane 11.55 88 52533 5.043 ng 98 49) 2,2,4-Trimethylpentane... 11.64 57 273939 4.220 ng 100 143 of 156 R9042116.M Wed May 25 17:18:16 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251601.D Acq On : 24 May 2016 23:11 Operator: WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1

Quant Time: May 25 06:28:24 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------50) Methyl Methacrylate 11.77 100 51282 9.703 ng 98 51) n-Heptane 11.90 71 64583 4.478 ng 100 52) cis-1,3-Dichloropropene 12.43 75 106574 5.115 ng 98 53) 4-Methyl-2-pentanone 12.46 58 60466 4.676 ng 98 54) trans-1,3-Dichloropropene 12.95 75 87631 4.600 ng 100 55) 1,1,2-Trichloroethane 13.12 97 62661 4.681 ng 98 58) Toluene 13.42 91 265107 4.487 ng 99 59) 2-Hexanone 13.66 43 141616 5.042 ng 98 60) Dibromochloromethane 13.82 129 73737 5.185 ng 99 61) 1,2-Dibromoethane 14.08 107 70681 4.981 ng 99 62) n-Butyl Acetate 14.31 43 156922 4.875 ng 98 63) n-Octane 14.44 57 55508 4.280 ng 98 64) Tetrachloroethene 14.57 166 72198 4.711 ng 99 65) Chlorobenzene 15.27 112 171921 4.792 ng 99 66) Ethylbenzene 15.68 91 295861 4.737 ng 99 67) m- & p-Xylenes 15.87 91 472358 9.468 ng 99 68) Bromoform 15.92 173 62168 5.171 ng 99 69) Styrene 16.24 104 182745 5.073 ng 99 70) o-Xylene 16.36 91 238162 4.603 ng 99 71) n-Nonane 16.61 43 127710 4.244 ng 99 72) 1,1,2,2-Tetrachloroethane 16.34 83 114125 4.679 ng 98 74) Cumene 16.99 105 300152 4.641 ng 99 75) alpha-Pinene 17.40 93 151792 4.653 ng 100 76) n-Propylbenzene 17.52 91 366125 4.586 ng 99 77) 3-Ethyltoluene 17.63 105 295817 4.764 ng 100 78) 4-Ethyltoluene 17.68 105 291656 4.904 ng 100 79) 1,3,5-Trimethylbenzene 17.75 105 246034 4.808 ng 100 80) alpha-Methylstyrene 17.91 118 129566 4.923 ng 99 81) 2-Ethyltoluene 17.95 105 292113 4.848 ng 99 82) 1,2,4-Trimethylbenzene 18.19 105 249142 4.933 ng 100 83) n-Decane 18.31 57 137816 4.514 ng 99 84) Benzyl Chloride 18.32 91 195626 4.450 ng 99 85) 1,3-Dichlorobenzene 18.34 146 143270 5.432 ng 99 86) 1,4-Dichlorobenzene 18.41 146 143327 5.305 ng 100 87) sec-Butylbenzene 18.47 105 339299 5.004 ng 99 88) 4-Isopropyltoluene (p-... 18.64 119 300298 4.822 ng 99 89) 1,2,3-Trimethylbenzene 18.64 105 259567 4.990 ng 100 90) 1,2-Dichlorobenzene 18.77 146 140921 5.437 ng 100 91) d-Limonene 18.80 68 97236 4.640 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.23 157 49416 4.690 ng 99 93) n-Undecane 19.65 57 144368 4.803 ng 99 94) 1,2,4-Trichlorobenzene 20.59 180 99534 4.830 ng 99 95) Naphthalene 20.70 128 331877 4.759 ng 99 96) n-Dodecane 20.74 57 141985 4.558 ng 99 97) Hexachlorobutadiene 21.07 225 60984 5.515 ng 99 98) Cyclohexanone 16.01 55 88728 5.116 ng 98 99) tert-Butylbenzene 18.18 119 244451 4.937 ng 100 100) n-Butylbenzene 19.08 91 274434 5.192 ng 99 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

144 of 156 R9042116.M Wed May 25 17:18:16 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2016_05\25\05251601.D Acq On : 24 May 2016 23:11 Operator: WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1

Quant Time: May 25 06:28:24 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251601.D\data.ms

950000

900000

850000

800000

750000 1,2,3-Trimethylbenzene,T 4-Isopropyltoluene (p-Cymene),T tert-Butylbenzene,T1,2,4-Trimethylbenzene,T

700000 Toluene-d8 (SS2),S

650000 n-Hexane,TEthyl Acetate,T Diisopropyl Ether,T n-Decane,T Chlorobenzene-d5 (IS3),IR

600000 Benzyl Chloride,T Bromofluorobenzene (SS3),S 1,4-Difluorobenzene (IS2),IR 550000 Isopropyl Acetate,T 500000 n-Butylbenzene,T sec-Butylbenzene,T Acetone,T n-Dodecane,T n-Undecane,T Cyclohexane,T 3-Ethyltoluene,T n-Propylbenzene,T 2-Ethyltoluene,T 1-Butanol,T d-Limonene,T Vinyl Acetate,T m- & p-Xylenes,T

450000 1,3,5-Trimethylbenzene,T 4-Ethyltoluene,T Cumene,T Naphthalene,T alpha-Methylstyrene,T 1,3-Dichlorobenzene,T 400000 o-Xylene,T alpha-Pinene,T Ethylbenzene,T 1,2-Dichlorobenzene,T Hexachlorobutadiene,T n-Nonane,T

350000 1,4-Dichlorobenzene,T Methyl Methacrylate,T Toluene,T Styrene,T 1,2,4-Trichlorobenzene,T n-Octane,T

300000 2,2,4-Trimethylpentane (Isooctane),T Chlorobenzene,T Benzene,T n-Heptane,T Bromochloromethane (IS1),IR 1,1,2,2-Tetrachloroethane,T 250000 1,2-Dichloroethane-d4(SS1),S Trichloroethene,T tert-Amyl Methyl Ether,T Tetrachloroethene,T 4-Methyl-2-pentanone,T Ethyl tert-Butyl Ether,T n-Butyl Acetate,T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T Propene,T 2-Hexanone,T 2-Propanol (Isopropanol),T Cyclohexanone,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T Dichlorodifluoromethane (CFC 12),T 1,1,2-Trichloroethane,T 1,2-Dibromo-3-Chloropropane,T 200000 Methyl tert-Butyl Ether,T cis-1,3-Dichloropropene,T 1,3-Butadiene,T Methylene Chloride,T Trichlorotrifluoroethane,T 1,2-Dichloropropane,T Ethanol,T 1,1-Dichloroethene,T trans-1,3-Dichloropropene,T cis-1,2-Dichloroethene,T trans-1,2-Dichloroethene,T Chloroform,T Carbon Disulfide,T 1,1,1-Trichloroethane,T Trichlorofluoromethane,T Tetrahydrofuran (THF),T 1,4-Dioxane,T Bromodichloromethane,T Carbon Tetrachloride,T Dibromochloromethane,T 2-Butanone (MEK),T

150000 Bromoform,T 3-Chloro-1-propene (Allyl Chloride),T 1,1-Dichloroethane,T Chloromethane,T Vinyl Chloride,T 1,2-Dibromoethane,T 1,2-Dichloroethane,T Bromomethane,T Acrylonitrile,T Acetonitrile,T

100000 Chloroethane,T Acrolein,T

50000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00145 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Wed May 25 17:18:17 2016 Page: 3 Evaluate Continuing Calibration Report

Data File : I:\MS09\Data\2016_05\25\05251625.D Vial: 16 Acq On : 25 May 2016 16:52 Operator: WA Sample : CCV2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05111605 (6/9)

Quant Time: May 26 07:03:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200%

Compound AvgRF CCRF %Dev Area% Dev(min) ------1 IR Bromochloromethane (IS1) 1.000 1.000 0.0 98 -0.02 2 T Propene 1.892 1.406 25.7 65 -0.01 3 T Dichlorodifluoromethane (CF 3.701 2.972 19.7 70 0.00 4 T Chloromethane 3.117 2.315 25.7 64 -0.01 5 T 1,2-Dichloro-1,1,2,2-tetraf 1.840 1.596 13.3 78 0.00 6 T Vinyl Chloride 2.639 2.169 17.8 70 -0.01 7 T 1,3-Butadiene 1.335 1.611 -20.7 94 -0.01 8 T Bromomethane 1.560 1.480 5.1 80 -0.02 9 T Chloroethane 1.279 1.136 11.2 82 -0.02 10 T Ethanol 1.210 1.120 7.4 69 -0.05 11 T Acetonitrile 3.422 2.747 19.7 67 -0.04 12 T Acrolein 1.012 0.928 8.3 68 -0.02 13 T Acetone 1.418 1.071 24.5 69 -0.04 14 T Trichlorofluoromethane 2.970 2.499 15.9 76 0.00 15 T 2-Propanol (Isopropanol) 4.544 3.762 17.2 70 -0.05 16 T Acrylonitrile 2.377 2.015 15.2 70 -0.03 17 T 1,1-Dichloroethene 1.636 1.430 12.6 74 -0.01 18 T 2-Methyl-2-Propanol (tert-B 4.478 3.858 13.8 73 -0.04 19 T Methylene Chloride 2.043 1.471 28.0 73 -0.02 20 T 3-Chloro-1-propene (Allyl C 2.553 2.042 20.0 67 -0.01 21 T Trichlorotrifluoroethane 1.394 1.220 12.5 79 -0.01 22 T Carbon Disulfide 6.455 5.833 9.6 72 0.00 23 T trans-1,2-Dichloroethene 2.403 2.114 12.0 71 -0.02 24 T 1,1-Dichloroethane 3.260 2.642 19.0 72 -0.02 25 T Methyl tert-Butyl Ether 5.291 4.486 15.2 74 -0.02 26 T Vinyl Acetate 0.363 0.350 3.6 74 -0.03 27 T 2-Butanone (MEK) 1.122 0.995 11.3 73 -0.03 28 T cis-1,2-Dichloroethene 2.357 1.961 16.8 71 -0.02 29 T Diisopropyl Ether 1.434 1.211 15.6 75 -0.02 30 T Ethyl Acetate 0.634 0.556 12.3 71 -0.03 31 T n-Hexane 3.090 2.439 21.1 74 0.00 32 T Chloroform 2.940 2.476 15.8 74 -0.03 33 S 1,2-Dichloroethane-d4(SS1) 1.630 1.544 5.3 94 -0.02 34 T Tetrahydrofuran (THF) 1.235 0.982 20.5 73 -0.01 35 T Ethyl tert-Butyl Ether 2.063 1.801 12.7 75 -0.01 36 T 1,2-Dichloroethane 2.030 1.750 13.8 74 -0.02

37 IR 1,4-Difluorobenzene (IS2) 1.000 1.000 0.0 97 -0.01 38 T 1,1,1-Trichloroethane 0.485 0.433 10.7 76 -0.01 39 T Isopropyl Acetate 0.211 0.178 15.6 72 -0.02 40 T 1-Butanol 0.317 0.292 7.9 75 -0.04 41 T Benzene 1.485 1.093 26.4 74 -0.02 42 T Carbon Tetrachloride 0.398 0.359 9.8 76 -0.01 43 T Cyclohexane 0.527 0.447 15.2 74 -0.01 44 T tert-Amyl Methyl Ether 0.994 0.853 14.2 74 -0.01 45 T 1,2-Dichloropropane 0.355 0.295 16.9 72 -0.01 46 T Bromodichloromethane 0.441 0.392 11.1 74 -0.02 47 T Trichloroethene 0.356 0.324 9.0 78 -0.01 48 T 1,4-Dioxane 0.252 0.239 5.2 76 -0.02 49 T 2,2,4-Trimethylpentane (Iso 1.568 1.256 19.9 70 -0.01 50 T Methyl Methacrylate 0.128 0.123 3.9 76 -0.02 51 T n-Heptane 0.348 0.292 16.1 75 -0.01 52 T cis-1,3-Dichloropropene 0.503 0.471 6.4 73 0.00 53 T 4-Methyl-2-pentanone 0.312 0.278 10.9 72 -0.01 54 T trans-1,3-Dichloropropene 0.460 0.423 8.0 73 -0.01 55 T 1,1,2-Trichloroethane 0.323 0.294 9.0 75 -0.01 146 of 156 R9042116.M Thu May 26 10:05:10 2016 Page: 1 Evaluate Continuing Calibration Report

Data File : I:\MS09\Data\2016_05\25\05251625.D Vial: 16 Acq On : 25 May 2016 16:52 Operator: WA Sample : CCV2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05111605 (6/9)

Quant Time: May 26 07:03:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200%

Compound AvgRF CCRF %Dev Area% Dev(min) ------

56 IR Chlorobenzene-d5 (IS3) 1.000 1.000 0.0 101 0.00 57 S Toluene-d8 (SS2) 2.353 2.269 3.6 98 0.00 58 T Toluene 3.383 2.747 18.8 75 0.00 59 T 2-Hexanone 1.608 1.393 13.4 73 -0.01 60 T Dibromochloromethane 0.814 0.749 8.0 76 0.00 61 T 1,2-Dibromoethane 0.813 0.750 7.7 76 -0.01 62 T n-Butyl Acetate 1.843 1.572 14.7 71 0.00 63 T n-Octane 0.743 0.588 20.9 72 0.00 64 T Tetrachloroethene 0.878 0.811 7.6 81 0.00 65 T Chlorobenzene 2.054 1.765 14.1 76 0.00 66 T Ethylbenzene 3.577 3.107 13.1 75 0.00 67 T m- & p-Xylenes 2.857 2.487 13.0 75 -0.01 68 T Bromoform 0.688 0.685 0.4 78 0.00 69 T Styrene 2.063 1.898 8.0 75 0.00 70 T o-Xylene 2.963 2.540 14.3 75 -0.01 71 T n-Nonane 1.723 1.346 21.9 70 0.00 72 T 1,1,2,2-Tetrachloroethane 1.397 1.273 8.9 73 0.00 73 S Bromofluorobenzene (SS3) 0.777 0.894 -15.1 115 0.00 74 T Cumene 3.703 3.246 12.3 76 0.00 75 T alpha-Pinene 1.868 1.631 12.7 75 0.00 76 T n-Propylbenzene 4.572 3.970 13.2 74 0.00 77 T 3-Ethyltoluene 3.556 3.200 10.0 75 -0.01 78 T 4-Ethyltoluene 3.405 2.969 12.8 76 0.00 79 T 1,3,5-Trimethylbenzene 2.930 2.600 11.3 76 0.00 80 T alpha-Methylstyrene 1.507 1.417 6.0 75 0.00 81 T 2-Ethyltoluene 3.451 3.036 12.0 76 -0.01 82 T 1,2,4-Trimethylbenzene 2.892 2.649 8.4 75 -0.01 83 T n-Decane 1.748 1.473 15.7 71 0.00 84 T Benzyl Chloride 2.517 2.274 9.7 72 -0.01 85 T 1,3-Dichlorobenzene 1.510 1.485 1.7 77 -0.01 86 T 1,4-Dichlorobenzene 1.547 1.530 1.1 78 0.00 87 T sec-Butylbenzene 3.883 3.443 11.3 75 0.00 88 T 4-Isopropyltoluene (p-Cymen 3.566 3.307 7.3 76 -0.01 89 T 1,2,3-Trimethylbenzene 2.979 2.740 8.0 75 -0.01 90 T 1,2-Dichlorobenzene 1.484 1.448 2.4 77 0.00 91 T d-Limonene 1.200 1.047 12.8 73 0.00 92 T 1,2-Dibromo-3-Chloropropane 0.603 0.553 8.3 77 0.00 93 T n-Undecane 1.721 1.537 10.7 71 0.00 94 T 1,2,4-Trichlorobenzene 1.180 1.089 7.7 79 0.00 95 T Naphthalene 3.994 3.711 7.1 79 0.00 96 T n-Dodecane 1.784 1.486 16.7 72 0.00 97 T Hexachlorobutadiene 0.633 0.651 -2.8 80 0.00 98 T Cyclohexanone 0.993 0.896 9.8 77 -0.01 99 T tert-Butylbenzene 2.835 2.542 10.3 76 -0.01 100 T n-Butylbenzene 3.027 2.758 8.9 74 0.00 ------

(#) = Out of Range SPCC's out = 0 CCC's out = 0

147 of 156 R9042116.M Thu May 26 10:05:10 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251625.D Vial: 16 Acq On : 25 May 2016 16:52 Operator: WA Sample : CCV2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05111605 (6/9)

Quant Time: May 26 07:03:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------1) Bromochloromethane (IS1) 8.92 130 110473 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.89 114 566557 12.500 ng -0.01 56) Chlorobenzene-d5 (IS3) 15.23 82 249800 12.500 ng 0.00

System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.70 65 170621 11.844 ng -0.02 Spiked Amount 12.500 Range 70 - 130 Recovery = 94.72% 57) Toluene-d8 (SS2) 13.32 98 566736 12.055 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 96.40% 73) Bromofluorobenzene (SS3) 16.84 174 223425 14.387 ng 0.00 Spiked Amount 12.500 Range 70 - 130 Recovery = 115.12%

Target Compounds Qvalue 2) Propene 3.67 42 320013 19.138 ng 98 3) Dichlorodifluoromethan... 3.78 85 656695 20.075 ng 100 4) Chloromethane 3.98 50 501238 18.196 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.14 135 363290 22.345 ng 99 6) Vinyl Chloride 4.25 62 479235 20.549 ng 100 7) 1,3-Butadiene 4.43 54 377234 31.982 ng 98 8) Bromomethane 4.73 94 326951 23.721 ng 100 9) Chloroethane 4.94 64 253411 22.416 ng 99 10) Ethanol 5.20 45 1252621 117.172 ng 100 11) Acetonitrile 5.38 41 619019 20.466 ng 100 12) Acrolein 5.50 56 219317 24.518 ng 99 13) Acetone 5.64 58 1270300 101.357 ng 99 14) Trichlorofluoromethane 5.80 101 546697 20.825 ng 100 15) 2-Propanol (Isopropanol) 5.98 45 1737194 43.257 ng 99 16) Acrylonitrile 6.17 53 458658 21.834 ng 100 17) 1,1-Dichloroethene 6.49 96 337997 23.376 ng 96 18) 2-Methyl-2-Propanol (t... 6.61 59 1781731 45.019 ng 99 19) Methylene Chloride 6.65 84 350925 19.432 ng 95 20) 3-Chloro-1-propene (Al... 6.77 41 487274 21.593 ng 98 21) Trichlorotrifluoroethane 6.94 151 291204 23.634 ng 99 22) Carbon Disulfide 6.91 76 1262925 22.138 ng 100 23) trans-1,2-Dichloroethene 7.66 61 495190 23.313 ng 96 24) 1,1-Dichloroethane 7.88 63 607000 21.069 ng 100 25) Methyl tert-Butyl Ether 7.94 73 1040640 22.253 ng 99 26) Vinyl Acetate 8.06 86 391679 121.934 ng # 90 27) 2-Butanone (MEK) 8.29 72 235313 23.729 ng 97 28) cis-1,2-Dichloroethene 8.75 61 463597 22.253 ng 96 29) Diisopropyl Ether 8.99 87 288900 22.803 ng # 91 30) Ethyl Acetate 8.99 61 260407 46.466 ng 99 31) n-Hexane 8.99 57 560368 20.516 ng 99 32) Chloroform 9.06 83 585444 22.534 ng 100 34) Tetrahydrofuran (THF) 9.44 72 221240 20.274 ng 97 35) Ethyl tert-Butyl Ether 9.54 87 417784 22.910 ng 99 36) 1,2-Dichloroethane 9.81 62 405884 22.621 ng 100 38) 1,1,1-Trichloroethane 10.07 97 505414 22.980 ng 99 39) Isopropyl Acetate 10.44 61 446929 46.829 ng 98 40) 1-Butanol 10.46 56 748513 52.175 ng 99 41) Benzene 10.52 78 1374149 20.411 ng 100 42) Carbon Tetrachloride 10.68 117 439891 24.405 ng 100 43) Cyclohexane 10.80 84 1058533 44.295 ng 98 44) tert-Amyl Methyl Ether 11.13 73 1005415 22.317 ng 99 45) 1,2-Dichloropropane 11.34 63 351059 21.813 ng 99 46) Bromodichloromethane 11.52 83 475098 23.795 ng 100 47) Trichloroethene 11.58 130 377662 23.419 ng 99 48) 1,4-Dioxane 11.55 88 292814 25.677 ng 98 49) 2,2,4-Trimethylpentane... 11.64 57 1466424 20.634 ng 100 50) Methyl Methacrylate 11.77 100 289409 50.020 ng 98 148 of 156 R9042116.M Thu May 26 09:57:25 2016 Page: 1 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251625.D Vial: 16 Acq On : 25 May 2016 16:52 Operator: WA Sample : CCV2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05111605 (6/9)

Quant Time: May 26 07:03:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Internal Standards R.T. QIon Response Conc Units Dev(Min) ------51) n-Heptane 11.90 71 353521 22.390 ng 99 52) cis-1,3-Dichloropropene 12.43 75 597722 26.204 ng 99 53) 4-Methyl-2-pentanone 12.47 58 340098 24.026 ng 98 54) trans-1,3-Dichloropropene 12.95 75 512500 24.577 ng 100 55) 1,1,2-Trichloroethane 13.12 97 349606 23.855 ng 99 58) Toluene 13.42 91 1440874 21.310 ng 100 59) 2-Hexanone 13.66 43 772425 24.031 ng 100 60) Dibromochloromethane 13.83 129 411733 25.300 ng 100 61) 1,2-Dibromoethane 14.08 107 400831 24.685 ng 99 62) n-Butyl Acetate 14.31 43 871739 23.666 ng 100 63) n-Octane 14.44 57 302379 20.372 ng 98 64) Tetrachloroethene 14.57 166 401120 22.873 ng 99 65) Chlorobenzene 15.27 112 943291 22.975 ng 100 66) Ethylbenzene 15.68 91 1630094 22.806 ng 100 67) m- & p-Xylenes 15.87 91 2584136 45.261 ng 100 68) Bromoform 15.93 173 366160 26.614 ng 99 69) Styrene 16.25 104 1023899 24.836 ng 100 70) o-Xylene 16.37 91 1294579 21.864 ng 100 71) n-Nonane 16.61 43 679402 19.727 ng 99 72) 1,1,2,2-Tetrachloroethane 16.34 83 636014 22.786 ng 100 74) Cumene 16.99 105 1637760 22.131 ng 100 75) alpha-Pinene 17.40 93 839430 22.483 ng 100 76) n-Propylbenzene 17.52 91 1983356 21.709 ng 100 77) 3-Ethyltoluene 17.63 105 1662601 23.395 ng 100 78) 4-Ethyltoluene 17.68 105 1557440 22.885 ng 100 79) 1,3,5-Trimethylbenzene 17.76 105 1350695 23.065 ng 100 80) alpha-Methylstyrene 17.92 118 729062 24.206 ng 99 81) 2-Ethyltoluene 17.95 105 1577660 22.878 ng 100 82) 1,2,4-Trimethylbenzene 18.19 105 1376300 23.812 ng 100 83) n-Decane 18.31 57 743518 21.281 ng 99 84) Benzyl Chloride 18.32 91 1226917 24.389 ng 100 85) 1,3-Dichlorobenzene 18.34 146 801190 26.546 ng 100 86) 1,4-Dichlorobenzene 18.41 146 802396 25.953 ng 100 87) sec-Butylbenzene 18.48 105 1823124 23.494 ng 100 88) 4-Isopropyltoluene (p-... 18.64 119 1652130 23.182 ng 100 89) 1,2,3-Trimethylbenzene 18.64 105 1423410 23.909 ng 100 90) 1,2-Dichlorobenzene 18.77 146 774075 26.096 ng 100 91) d-Limonene 18.79 68 544206 22.691 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.23 157 287488 23.843 ng 98 93) n-Undecane 19.65 57 775636 22.548 ng 99 94) 1,2,4-Trichlorobenzene 20.59 180 566024 24.001 ng 100 95) Naphthalene 20.70 128 1854014 23.230 ng 100 96) n-Dodecane 20.74 57 772172 21.660 ng 99 97) Hexachlorobutadiene 21.07 225 348057 27.505 ng 100 98) Cyclohexanone 16.02 55 501514 25.270 ng 99 99) tert-Butylbenzene 18.19 119 1333470 23.536 ng 100 100) n-Butylbenzene 19.09 91 1488064 24.602 ng 100 ------

(#) = qualifier out of range (m) = manual integration (+) = signals summed

149 of 156 R9042116.M Thu May 26 09:57:25 2016 Page: 2 Quantitation Report (QT Reviewed)

Data File : I:\MS09\Data\2016_05\25\05251625.D Vial: 16 Acq On : 25 May 2016 16:52 Operator: WA Sample : CCV2 R9052516_25ng Inst : MS09 Misc : S29-04191601/S29-05111605 (6/9) Quant Time: May 26 07:03:55 2016 Quant Method : I:\MS09\Methods\R9042116.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Fri Apr 22 10:14:32 2016 Response via : Initial Calibration DataAcq Meth:TO15.M

Abundance TIC: 05251625.D\data.ms 5400000

5200000

5000000

4800000

4600000

4400000 1,2,3-Trimethylbenzene,T

4200000 4-Isopropyltoluene (p-Cymene),T 1,2,4-Trimethylbenzene,Ttert-Butylbenzene,T 4000000

3800000

3600000

3400000 n-Decane,T n-Hexane,TEthyl Acetate,T Benzyl Chloride,T

3200000 Diisopropyl Ether,T

3000000

2800000 n-Butylbenzene,T n-Dodecane,T sec-Butylbenzene,T

2600000 Naphthalene,T d-Limonene,T 4-Ethyltoluene,T 3-Ethyltoluene,T m- & p-Xylenes,T 2-Ethyltoluene,T n-Undecane,T n-Propylbenzene,T Cyclohexane,T Vinyl Acetate,T 1,3,5-Trimethylbenzene,T 1-Butanol,T 2400000 Isopropyl Acetate,T Cumene,T alpha-Methylstyrene,T 1,3-Dichlorobenzene,T 1,2-Dichlorobenzene,T 2200000 o-Xylene,T Acetone,T Ethylbenzene,T alpha-Pinene,T 2000000 1,4-Dichlorobenzene,T 1,2,4-Trichlorobenzene,T Hexachlorobutadiene,T Styrene,T n-Nonane,T Methyl Methacrylate,T Toluene,T 1800000 n-Octane,T Chlorobenzene,T 1600000 2,2,4-Trimethylpentane (Isooctane),T n-Heptane,T Benzene,T 2-Methyl-2-Propanol (tert-Butyl Alcohol,T

1400000 1,1,2,2-Tetrachloroethane,T Tetrachloroethene,T n-Butyl Acetate,T tert-Amyl Methyl Ether,T 4-Methyl-2-pentanone,T 2-Propanol (Isopropanol),T 1,2-Dichloro-1,1,2,2-tetrafluoroethane ,T 2-Hexanone,T Trichloroethene,T Ethyl tert-Butyl Ether,T 1200000 Cyclohexanone,T Propene,T 1,2-Dibromo-3-Chloropropane,T cis-1,3-Dichloropropene,T 1,1,2-Trichloroethane,T Dichlorodifluoromethane (CFC 12),T 1,3-Butadiene,T Methyl tert-Butyl Ether,T trans-1,3-Dichloropropene,T

1000000 1,2-Dichloropropane,T Toluene-d8 (SS2),S Carbon Disulfide,T Trichlorotrifluoroethane,T cis-1,2-Dichloroethene,T 1,1-Dichloroethene,T Chlorobenzene-d5 (IS3),IR 1,1,1-Trichloroethane,T Bromodichloromethane,T Bromofluorobenzene (SS3),S Ethanol,T Tetrahydrofuran (THF),T Dibromochloromethane,T trans-1,2-Dichloroethene,T Chloroform,T Carbon Tetrachloride,T Bromoform,T Methylene Chloride,T 1,4-Difluorobenzene (IS2),IR 1,4-Dioxane,T 2-Butanone (MEK),T 800000 Trichlorofluoromethane,T 3-Chloro-1-propene (Allyl Chloride),T 1,2-Dibromoethane,T 1,1-Dichloroethane,T Vinyl Chloride,T 1,2-Dichloroethane,T Chloromethane,T Bromomethane,T Acrylonitrile,T 600000 Acetonitrile,T Chloroethane,T Bromochloromethane (IS1),IR 1,2-Dichloroethane-d4(SS1),S

400000 Acrolein,T

200000

0 Time--> 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00150 13.00 of 14.00 156 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.00 R9042116.M Thu May 26 09:57:26 2016 Page: 3 BFB

Data Path : I:\MS09\Data\2016_04\21\ Data File : 04211620.D Acq On : 21 Apr 2016 22:32 Operator : SC Sample : 12.5ng TO-15 BFB STD Misc : S29-04191601 ALS Vial : 2 Sample Multiplier: 1 Integration File: LSCINT.P Method : I:\MS09\Methods\R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Fri Apr 22 09:57:48 2016

Abundance TIC: 04211620.D\data.ms

2000000

1500000

1000000

500000

0 Time--> 15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 Abundance Average of 16.830 to 16.841 min.: 04211620.D\data.ms (-) 95 120000

174 100000

80000

60000 75

40000

20000 50 69 37 61 87 45 56 81 104117 128 135 143 148 157 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185

AutoFind: Scans 2593, 2594, 2595; Background Corrected with Scan 2584 | Target | Rel. to | Lower | Upper | Rel. | Raw | Result | | Mass | Mass | Limit% | Limit% | Abn% | Abn | Pass/Fail | ------| 50 | 95 | 8 | 40 | 16.1 | 19379 | PASS | | 75 | 95 | 30 | 66 | 43.8 | 52816 | PASS | | 95 | 95 | 100 | 100 | 100.0 | 120637 | PASS | | 96 | 95 | 5 | 9 | 6.6 | 7938 | PASS | | 173 | 174 | 0.00 | 2 | 0.0 | 0 | PASS | | 174 | 95 | 50 | 120 | 85.6 | 103323 | PASS | | 175 | 174 | 4 | 9 | 7.9 | 8164 | PASS | | 176 | 174 | 93 | 101 | 97.3 | 100579 | PASS | | 177 | 176 | 5 | 9 | 6.4 | 6393 | PASS | ------

151 of 156 R9042116.M Fri Apr 22 10:08:06 2016 Page: 1 BFB

Data Path : I:\MS09\Data\2016_05\25\ Data File : 05251601.D Acq On : 24 May 2016 23:11 Operator : WA Sample : CCV R9052516_5.0ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1 Integration File: LSCINT.P Method : I:\MS09\Methods\R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Fri Apr 22 10:14:32 2016

Abundance TIC: 05251601.D\data.ms 800000

700000

600000

500000

400000

300000

200000

100000

0 Time--> 15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 Abundance Average of 16.830 to 16.841 min.: 05251601.D\data.ms (-) 95 100000 174

80000

60000

75 40000

20000 50 69 37 61 87 45 56 81 104 117 128 137 143 148 155 0 m/z--> 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185

AutoFind: Scans 2593, 2594, 2595; Background Corrected with Scan 2584 | Target | Rel. to | Lower | Upper | Rel. | Raw | Result | | Mass | Mass | Limit% | Limit% | Abn% | Abn | Pass/Fail | ------| 50 | 95 | 8 | 40 | 15.6 | 16508 | PASS | | 75 | 95 | 30 | 66 | 44.3 | 46827 | PASS | | 95 | 95 | 100 | 100 | 100.0 | 105672 | PASS | | 96 | 95 | 5 | 9 | 6.4 | 6800 | PASS | | 173 | 174 | 0.00 | 2 | 0.0 | 0 | PASS | | 174 | 95 | 50 | 120 | 93.0 | 98293 | PASS | | 175 | 174 | 4 | 9 | 7.9 | 7794 | PASS | | 176 | 174 | 93 | 101 | 96.9 | 95205 | PASS | | 177 | 176 | 5 | 9 | 6.6 | 6287 | PASS | ------

152 of 156 R9042116.M Wed May 25 17:18:02 2016 Page: 1 BFB

Data Path : I:\MS09\Data\2016_05\25\ Data File : 05251625.D Acq On : 25 May 2016 16:52 Operator : WA Sample : CCV2 R9052516_25ng Misc : S29-04191601/S29-05111605 (6/9) ALS Vial : 16 Sample Multiplier: 1 Integration File: LSCINT.P Method : I:\MS09\Methods\R9042116.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Fri Apr 22 10:14:32 2016

Abundance TIC: 05251625.D\data.ms

4000000

3000000

2000000

1000000

0 Time--> 15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 Abundance Average of 16.830 to 16.841 min.: 05251625.D\data.ms (-) 95 120000 174

100000

80000

60000 75

40000

20000 50 69 37 61 87 45 56 81 106 111 117 130135143 148 155 161 0 m/z--> 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 185

AutoFind: Scans 2593, 2594, 2595; Background Corrected with Scan 2584 | Target | Rel. to | Lower | Upper | Rel. | Raw | Result | | Mass | Mass | Limit% | Limit% | Abn% | Abn | Pass/Fail | ------| 50 | 95 | 8 | 40 | 15.3 | 19080 | PASS | | 75 | 95 | 30 | 66 | 43.1 | 53736 | PASS | | 95 | 95 | 100 | 100 | 100.0 | 124620 | PASS | | 96 | 95 | 5 | 9 | 6.4 | 7974 | PASS | | 173 | 174 | 0.00 | 2 | 0.0 | 0 | PASS | | 174 | 95 | 50 | 120 | 92.2 | 114864 | PASS | | 175 | 174 | 4 | 9 | 8.1 | 9347 | PASS | | 176 | 174 | 93 | 101 | 96.7 | 111051 | PASS | | 177 | 176 | 5 | 9 | 6.7 | 7434 | PASS | ------

153 of 156 R9042116.M Thu May 26 10:05:24 2016 Page: 1 Injection Log Directory: J:\MS09\Data\2016_04\21\ Date/Time File Name Sample ID Misc Info Operator Vial Comment 20 4/21/16 22:32 04211620.D 12.5ng TO-15 BFB STD S29-04191601 SC 2 21 4/21/16 23:06 04211621.D 0.08ng TO-15 ICAL STD S29-04191601/S29-04201603 (5/19) SC 5 22 4/21/16 23:40 04211622.D 0.10ng TO-15 ICAL STD S29-04191601/S29-04201603 (5/19) SC 5 23 4/22/16 0:14 04211623.D 0.20ng TO-15 ICAL STD S29-04191601/S29-04201603 (5/19) SC 5 24 4/22/16 0:48 04211624.D 0.40ng TO-15 ICAL STD S29-04191601/S29-04201603 (5/19) SC 5 25 4/22/16 1:22 04211625.D 1.0ng TO-15 ICAL STD S29-04191601/S29-04131608 (5/12) SC 6 26 4/22/16 1:56 04211626.D 5.0ng TO-15 ICAL STD S29-04191601/S29-04131608 (5/12) SC 6 27 4/22/16 2:30 04211627.D 25ng TO-15 ICAL STD S29-04191601/S29-04131603 (5/12) SC 7 28 4/22/16 3:04 04211628.D 50ng TO-15 ICAL STD S29-04191601/S29-04131603 (5/12) SC 7 29 4/22/16 3:37 04211629.D 100ng TO-15 ICAL STD S29-04191601/S29-04131603 (5/12) SC 7 30 4/22/16 4:11 04211630.D Blank (100mL) S29-04191601 SC 2 31 4/22/16 4:45 04211631.D 25ng TO-15 ICV STD S29-04191601/S29-04141603 (5/12) SC 2 cf 32 4/22/16 5:19 04211632.D 25ng TO-15 ICV STD S29-04191601/S29-04141603 (5/12) SC 2 pass 33 34 35 36 37 38 39 40 41 42 43 44 45 pass 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61

Page 1 of 1 154 of 156 Injection Log Directory: I:\MS09\Data\2016_05\25\ Date/Time File Name Sample ID Misc Info Operator Vial Comment

1 5/24/16 23:11 05251601.D CCV R9052516_5.0ng S29-04191601/S29-05111605 (6/9) WA 16 Passed

2 5/24/16 23:45 05251602.D CCV R9052416_5.0ng S29-04191601/S29-05121603 (6/10) WA 15

3 5/25/16 0:18 05251603.D MB R9052516_1000mL S29-04191601(AC00463) WA 2 Passed

4 5/25/16 0:52 05251604.D LCS R9052516_25ng S29-04191601/S29-05101606 (6/8) WA 2 Passed

5 5/25/16 1:26 05251605.D P1602642-005 (1000mL) S29-04191601 WA 7

6 5/25/16 2:00 05251606.D P1602642-006 (1000mL) S29-04191601 WA 8

7 5/25/16 2:34 05251607.D P1602642-007 (1000mL) S29-04191601 WA 13

8 5/25/16 3:09 05251608.D P1602642-008 (1000mL) S29-04191601 WA 1

9 5/25/16 7:09 05251609.D J1603422-001 (1000mL) S29-04191601 WA 1

10 5/25/16 7:43 05251610.D J1603423-001 (1000mL) S29-04191601 WA 3

11 5/25/16 8:17 05251611.D J1603423-001dil (100mL) S29-04191601 WA 3

12 5/25/16 8:50 05251612.D J1603424-001 (1000mL) S29-04191601 WA 4

13 5/25/16 9:31 05251613.D J1603424-001dil (200mL) S29-04191601 WA 4

14 5/25/16 10:05 05251614.D P1602479-001 (400mL) S29-04191601 WA 5

15 5/25/16 10:39 05251615.D P1602480-001 (400mL) S29-04191601 WA 6

16 5/25/16 11:12 05251616.D P1602481-001 (25mL) S29-04191601 WA 7 rerun higher

17 5/25/16 11:46 05251617.D P1602482-001 (400mL) S29-04191601 WA 8

18 5/25/16 12:20 05251618.D P1602481-001 (200mL) S29-04191601 WA 7

19 5/25/16 12:54 05251619.D J1603422-001dup (1000mL) S29-04191601 WA 1

20 5/25/16 13:28 05251620.D P1602666-001 (0.5mL) S29-04191601 WA 1 not used

21 5/25/16 14:06 05251621.D P1602666-001 (0.3mL) S29-04191601 WA 1

22 5/25/16 14:40 05251622.D P1602666-002 (0.6mL) S29-04191601 WA 1

23 5/25/16 15:44 05251623.D P1602483-001 (400mL) S29-04191601 WA 5

24 5/25/16 16:18 05251624.D P1602483-002 (400mL) S29-04191601 WA 6

155 of 156 J:\EXCEL\REPORT\TO15\Msd09\MS09day\2016\05\D09052516 Page 1 of 1 Injection Log Directory: I:\MS09\Data\2016_05\25\ Date/Time File Name Sample ID Misc Info Operator Vial Comment

1 5/25/16 16:52 05251625.D CCV2 R9052516_25ng S29-04191601/S29-05111605 (6/9) WA 16 Pass

2 5/25/16 17:26 05251626.D CCV2 R9052516_5.0ng S29-04191601/S29-05121603 (6/10) WA 15 Not Used

3 5/25/16 18:00 05251627.D MB2 R9052516_1000mL S29-04191601(AC00463) WA 2 Pass

4 5/25/16 18:33 05251628.D LCS2 R9052516_25ng S29-04191601/S29-05101606 (6/8) WA 2 Pass

5 5/25/16 19:07 05251629.D P1602483-002dil (40mL) S29-04191601 WA 6

6 5/25/16 19:41 05251630.D P1602669-001 (1000mL) S29-04191601 WA 3

7 5/25/16 20:15 05251631.D P1602669-002 (1000mL) S29-04191601 WA 4

8 5/25/16 20:49 05251632.D P1602669-003 (1000mL) S29-04191601 WA 7

9 5/25/16 21:23 05251633.D P1602669-004 (1000mL) S29-04191601 WA 8

10 5/25/16 21:57 05251634.D P1602669-005 (1000mL) S29-04191601 WA 9

11 5/25/16 22:31 05251635.D LCSD2 R9052516_25ng S29-04191601/S29-05101606 (6/8) WA 2 Pass

12 5/25/16 23:05 05251636.D P1602669-006 (1000mL) S29-04191601 WA 10

13 5/25/16 23:39 05251637.D P1602669-007 (1000mL) S29-04191601 WA 13

14 5/26/16 0:13 05251638.D P1602669-008 (1000mL) S29-04191601 WA 14

15 5/26/16 0:47 05251639.D P1602492-001 (1000mL) S29-04191601 WA 11

16 5/26/16 1:25 05251640.D P1602492-001dup (1000mL) S29-04191601 WA 11 Pass for Dup

17 5/26/16 1:59 05251641.D P1602492-002 (1000mL) S29-04191601 WA 12

18 5/26/16 2:33 05251642.D P1602492-002dil (100mL) S29-04191601 WA 12

156 of 156 I:\EXCEL\REPORT\TO15\Msd09\MS09day\2016\05\D09052516_2 Page 1 of 1 ATTACHMENT 4

Tier 2 Air Screening Risk Assessment for VOCs to Nearest Receptor, Approximately 75 Meters from Stack, Pemaco Superfund Site, Maywood, California Attachment 4 Tier 2 Screening Risk Assessment for VOCs to Nearest Receptor Approximately 75 Meters from Stack Pemaco Superfund Site, Maywood California

Results for vapor sample collected at SP‐106 (final effluent) on 5/12/2016 (TO‐15SIM method)

Average Air Cancer Maximum Individual Chronic Reference Chronic Hazard Acute Reference Acute Hazard Effluent 1 Mass flow rate2 Concentration3 Predicted Inhalation Dose Potency4 Cancer Risk Exposure Level Index Exposure Level4 Index4

Compound Concentration Qlbs Qton Cair Concentrations DI CP MICR RELC HIC RELA HIA 3 3 ‐1 3 ug/m lbs/yr ton/yr mg/m ppmv mg/kg/day (mg/kg‐day) ug/m 1,1,1‐Trichloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 1000 0.00E+00 3900 0.0E+00 1,1,2,2‐Tetrachloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.0E‐01 0.0E+00 NR NA NR NA 1,1,2‐Trichloro‐1,2,2‐Trifluoroethane (Freon 113) 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,1,2‐Trichloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,1‐Dichloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 5.7E‐03 0.0E+00 NR NA NR NA 1,1‐Dichloroethene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 70 0.00E+00 NR NA 1,2,4‐Trichlorobenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,2,4‐Trimethylbenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,2‐Dibromoethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.5E‐01 0.0E+00 0.8 0.00E+00 NR NA 1,2‐Dichlorobenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,2‐Dichloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 7.2E‐02 0.0E+00 400 0.00E+00 NR NA 1,2‐Dichloropropane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,2‐Dichlorotetrafluoroethane (Freon 114) 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,3,5‐Trimethylbenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA 1,3‐Dichlorobenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA 3900 0.0E+00 1,4‐Dichlorobenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 4.0E‐02 0.0E+00 800 0.00E+00 NR NA 1,4‐Dioxane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.7E‐02 0.0E+00 3000 0.00E+00 3000 0.0E+00 2‐Butanone (Methyl ethyl ketone) 2.1 9.5E‐03 4.73E‐06 3.2E‐05 0.0000000110 9.4E‐09 NR NA NR NA 13000 1.0E‐11 Acetone 8.3 3.7E‐02 1.87E‐05 1.3E‐04 0.0000000195 3.7E‐08 NR NA NR NA NR NA Benzene 1.0 4.5E‐03 2.25E‐06 1.5E‐05 0.0000000048 4.5E‐09 1.0E‐01 4.5E‐10 60 2.58E‐07 1300 4.9E‐11 Bromomethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 5 0.00E+00 NR NA Carbon Disulfide 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 800 0.00E+00 6200 0.0E+00 Carbon tetrachloride 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.5E‐01 0.0E+00 40 0.00E+00 NR NA Chlorobenzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 1000 0.00E+00 1900 0.0E+00 Chloroethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 30000 0.00E+00 NR NA Chloroform 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.9E‐02 0.0E+00 300 0.00E+00 NR NA Chloromethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA cis‐1,2‐Dichloroethene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA cis‐1,3‐Dichloropropene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Cyclohexane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Dichlorodifluoromethane (Freon 12) 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Dimethyl octane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Ethyl benzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 8.7E‐03 0.0E+00 2000 0.00E+00 NR NA Hexachloro‐1,3‐Butadiene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Isopropanol 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 7000 0.00E+00 150 0.0E+00 m/p Xylene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00 Methyl ethyl benzene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Methylene chloride 0.74 3.3E‐03 1.67E‐06 1.1E‐05 0.0000000033 3.3E‐09 NR NA 30000 3.81E‐10 3200 1.5E‐11 N‐Hexane 1.3 5.9E‐03 2.93E‐06 2.0E‐05 0.0000000057 5.8E‐09 NR NA 7000 2.87E‐09 NR NA o‐Xylene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00 Propylene 0.74 3.3E‐03 1.67E‐06 1.1E‐05 0.0000000066 3.3E‐09 NR NA 3000 3.81E‐09 NR NA Styrene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 900 0.00E+00 21000 0.0E+00 Tert‐Butyl Methyl Ether (MTBE) 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.8E‐03 0.0E+00 8000 0.00E+00 NR NA Tetrachloroethene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.1E‐02 0.0E+00 35 0.00E+00 NR NA Toluene 2.6 1.2E‐02 5.86E‐06 4.0E‐05 0.0000000107 1.2E‐08 NR NA 300 1.34E‐07 37000 4.5E‐12 trans‐1,2‐Dichloroethene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA trans‐1,3‐Dichloropropene 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Trichloroethene 3.0 1.4E‐02 6.76E‐06 4.6E‐05 0.0000000086 1.3E‐08 7.0E‐03 9.4E‐11 600 7.73E‐08 NR NA Trichlorofluoromethane 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA Vinyl Chloride 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.7E‐01 0.0E+00 NR NA 180000 0.0E+00 Xylenes (total) 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00

Total 0.0000000703 5.43E‐10 4.76E‐07 7.85E‐11 Source: Earth Tech, Inc. 2007. SCAQMD ‐ Tier 2 Toxic Air Contaminant Emissions Modeling, Pemaco Superfund Site, 5050 East Saluson Avenue, Maywood, California. February.

Notes: 1. Mass flux rate is based on a volumetric flow rate of 137.3 standard cubic feet per minute (scfm). 5. Blue results indicate positive detection. 2. Average air concentration and dispersion factor at nearest receptor approximately 75 meters from stack. 6. Zero was used for the non‐detected results. 3. Cancer Risk and Chronic Hazard Index to nearest receptor approximately 75 meters from stack. 7. NA = not applicable; NR = not reported. 4. South Coast Air Quality Management District, July 1, 2005 Risk Assessment Procedures for Rules 1401 and 212 Version 8. The following COCs were detected in plant vapor effluent during the May 2016 sampling event, but were not included in the original Tier 2 Screening Risk Assessment 7.0, Permit Application Package "L" Rules 1401 and 212 Version 7.0 model: 2‐Propanol (1.7J ug/m3) and Ethanol (280 ug/m3). Detected concentration of these COCs in plant vapor effluent was assessed using the highest Cancer Potency factor from the original model (2.7E‐01, for Vinyl Chloride). The resulting total Maximum Individual Cancer Risk (approximately 3.42E‐7) remains below the one‐in‐a‐million (1.0E‐6) threshold.

Attachment 4 Tier 2 Screening Risk Assessment for VOCs to Nearest Receptor OTIE Page 1 of 1