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Contract Rwbtr DAAK11-B3-IH)007 Talk Nuabir 0004 Dalitarjr Ordir Hi»b«r 000)
NUT ?HCIMIA ORDNANCE WORKS ENVIROHMEHTAL SURVEY UnUNCBD tfPENDICIS SDPKKTINC DATA ITEMS A003 ADD A004
WVIIOmB!TAL SCIENCE AND INCINEEKING, INC. ;j P.O. Boi E8E CiiotivilU, FU. 32602
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Diitribution liaittd to U.S. Covtrmint Aftnciii only for pro tic t ion of privil«|td info nit ion tvtluttini »ooth«r conand: Noviibtr 1984. KtqiMiti for thii docuMnt auit bt rcfirrtd to: Comandir, U.S. Any Toxic and Hatatdoui Matiriali Agtncy, Abirdttn Proving Ground. Md. 21010-3401.
Frtpartd for: U.S. ARMY TOXIC AND HAZARDOUS HATERIALS AGENCY AitniMnti Diviiion Abardttn Provini Ground, Md. 21010-5401 BR3QI007 TABLE OF CONTENTS APPENDIX A--ESE FIELD LABORATORY AND QUALITY ASSURANCE PLAN APPENDIX B—DATA MANAGEMENT PLAN APPENDIX C--ESE ANALYTICAL LABORATORY SAFETY PLAN
AR30I008 o
o APPENDIX A
ESE FIELD LABORATORY QUALITY ASSURANCE PUN
(Reviled 11/07/84)
r•**y/ AR30I00„•„.•• 9 QA.l/QAPLAN/TUC.l 11/07/84
TABLE OF CONTENTS
Page INTRODUCTION A-l 2.0 RESPONSIBILITIES FOR QA A-2 2.1 OVERALL PLAN FUNCTION A-2 2.2 QA/QC RESPONSIBILITIES A-4 2.2.1 USATHAMA CENTRAL LABORATORY A-4 , QA COORDINATOR A-6 2.2.2 ESE PROJECT QA SUPERVISOR 2.2.3 ESE SITE MANAGER A-7 ' 2.2.4 CHEMICAL ANALYSIS SUPERVISOR A-8 2.2.5 ESE ANALYTICAL OR FIELD TEAM LEADER A-8 2.2.6 ESE ANALYSTS AND SAMPLING PERSONNEL A-S 3.0 ANALYTICAL SYSTEMS CONTROLS A-9 3.1 SAMPLE MANAGEMENT A-9 3.2 SAMPLING A-n 3.2.1 VOLATILES A-15 3.2.2 GROUND HATER A-15 3.2.3 SURFACE HATER A-17 3.2.4 AIR •A-18 3.2.5 SOIL A-18 3.2.6 SEDIMENTS A-19 3.3 SAMPLE PRESERVATION A-21 3.4 SAMPLE PREPARATION A-21 3.4.1 WATEK SAMPLES A-27 3.4.2 SOIL SAMPLES A-27 3.4.3 SEDIMENT SAMPLES A-2B 3.4.4 STANDARD SAMPLES A-28 3.5 8UBSAMPLIN6 A-28 3.6 CONTROL SAMPLES A-29 3.7 REFERENCE MATERIALS A-29 3.8 ANALYTICAL METHODS AND CERTIFICATION A-29 3.8.1 RATIONALE A-29 3.8.2 METHOD CERTIFICATION A-30 3,9 ANALYST CERTIFICATION
A-i (Red).
*JiJA.l/QAPLA«/TOC.A 2 11/07/B4
O TABLE OF CONTENTS
Pagt ANALYSIS OF SAMPLES A-36 4.1 LABORATORY INSTRUMENT QC CONTROLS A-36 4.2 CONTROL SAMPLESA-38 5.0 INSTRUMENT CALIBRATION AND MAINTENANCE A-41 5.1 FIELD INSTRUMENT CALIBRATION A-42 5.2 ANALYTICAL NOTEBOOKS AND INSTRUMENT LOGBOOKS A-43 5.3 SPECIFIC ANALYTICAL SYSTEMS CONTROL • A-45 5.3.1 METALS SYSTEM CONTROL A-45 5.3.2 NITRITE PLUS NITRATE, SULFATE, AND PHOSPHATE ANALYSES A-46 5.3.3 GC A-46 5.3.4 GC/MS ANALYSIS A-47 6.0 AUDITING AND REPORTING OF Dili .A-48 6.1 SEMIQUAHIITATIVE ANALYSES A-48 6.2 QUANTITATIVE ANALYSES A-50
BIBLIOGRAPHY A-52
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A-ii IJA.l/QAPLAN/LOTF.l 11/07/84
LIST OF TABLES
TabIt Page 3.3-1 Container!, Prtiarvation, and Holding Tinea A-22 3.3-2 Saaple Container Cleaning Procedurei A-25 4.1-1 Suoaary of Inacrunental Syitena Control A-37 Kequiranenti 4.2-1 QC tequirenenta by Saople Lot A-39
LIST OF FIGURES Figure Page 2.1-1 Laboratory QA/QC Organization and Function A-3 2.1-2 Field QA/QC Plan Organization and Function A-5 3.2-1 Field Sampling Audit Checkliit A-12 3.2-2 Surface Soil Corapoaite Sampling Method A-20 3,9-1 Typical Certification Audit Page A-34 6.1-1 Arny Data Review Form A-49
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A-iii ^A.l/tfAPLAN/1.1 09/20/84 0- 1.0 INTRODUCTION
Thii document ia the overall ESE Project Quality Control (QC) Plan for aampling and analyiei performed on taaka and contracta for USATHAMA which require compliance with the U.S. Army Toxic and Hasardou* Materiala Agency (USATHAMA) Quality Aiiurance (QA) Program of April 1982. This plan it baaed on and complies with thia USATHAMA QA Program. Specific detaila and deviationa from thia general plan, if any, for a certain talk or lurvey will be deicribed in detail in the Taak Sampling and Analysis Plan or teit plana. Becauie of the detailed nature of the USATHAMA QA Program Plan, thii Project QC Plan includes aectiona that are very limilar to those in the USATHAMA QA Program Plan.
' The specific objectivei of thia plan are to describe in general detail the processes for controlling the validity of the data generated in the aaupling and analyiia efforts; the raecnoda and criteria for detection of } out-of-control situations; steps to be taken to provide timely • corrective action; and how auch actions will be reported and documented. The Project QA Plan alao supports the Dita Management Plan by providing documentation of the limit! of precision, accuracy, and sensitivity ot all analytical systems generating data and by providing mechanisms for documentation of the validity of all reported data,
Some environmental surveys and other tasks assigned under this contract may require the development and documentation of certain lemiquanti- tative and quantitative analytical methods for all phases of the project. The analytical aystems controls and data validation procedures deicribed in this QC Plan will be employed to ensure valid, properly formatted data defining the precision, accuracy, and sensitivity of each method.
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2.0 RESPONSIBILITIES FOR QA
The QC Plan functiona according to the USATHAMA central-laboratory/ field-laboratory concept, Environmental Science and Engineering, Inc. (ESE) acta ai the field laboratory, which is monitored by the USATHAMA Central Laboratory QA Coordinator, The overall QA/QC organisation to provide valid data to the Commander of USATHAMA is shown in Fig, 2,1-1, The function of the plan and QA responsibilities of each of the project participants are outlined in the following subsectioni,
2.1 OVERALL PLAN FUNCTION Fig. 2,1-1 depicts the nanner in which the ESE Project QA Supervisor monitors the conduct of the,sampling and analytical effort. In thii poaition, the QA Supervisor is not directly subordinate to anyone reaponsible for sampling and analysis; the supervisor reports to the ESE Project Manager, Within the flow of the project scheme, the QA Superviior monitors the receipt of samples and the organization of samples into analytical lots and ensures that appropriate QC samples are included, The specific responsibilities of the QA Superviior are detailed in Par, 2,2,2.
The analyst performs the analyses of samples and control simples and submits results to the Analytical Team Leaders for approval, The Data Assistant enters the data into the ESE data handling system, where preprogrammed QC checks are run and a printout is generated. The QA Supervisor monitors the QC results, approves results which are in control, and updates QC criteria and control charts, At this point, any analytical problems and out-of-control situations are identified by the QA Superviior and corrective action is recommended, Subsequently, data are reviewed by the ESE Project Manager within the overall context of the sampling and analysis program. If questions are encountered, they are resolved before further data processing, AR30IOU
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Approved data are transcribed into the U,S, Army format and entered at Level 1, The Project QA Superviior validates the Level 1 data by verifying the accuracy of the analysis and transcription of a data subiample, Thia ia repreaented in Fig. 2.1-1 by the dotted linea pasting back from the validation step to the sample,
The nanner in which the Project QA Superviior monitor a the field effort it shown in Fig, 2,1-2, Thii figure shows that the Project QA Super- viior monitors the logging-in of samples, checks copies of field notebook entries and logiheeti, and reports any inconaiatenciei and/or omiisioni to the Field Team Leader. The QA Superviior also monitors the QC and calibration data submitted to tupport field teati and analysis.
The field data will consist of three types of data files: (1) the field drilling: file, (2) the ground water stabilized file, and (3) the map file. In addition, certain field sampling information must be collected and entered into the chemical data files. ,-;J7v '-^X Field data which have passed the QC checks are passed to the Data Assistant for direct entry to the U.S. Army system. Validation of field data is performed by the QA Supervisor in the same manner as for laboratory results,
2,2 QA/QC RESPONSIBILITIES 2.2,1 USATHAMA CENTRAL LABORATORY QA COORDINATOR The Central QA Laboratory will monitor the QA/QC activiti.es of the field laboratory to enaure the quality of the generated data, The USATHAMA Central Laboratory QA Coordinator therefore has the following responsibilities in fulfilling this objective: 1, Provide technical evaluations of QC plans submitted by performers, as required. QC plans are to be developed according to this USATHAMA QA Program. 2. Provide technical evaluations of laboratory facilitiea and capabilities, as required. AR3•••••••-0 1016 . Q
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3. Manage the QA activities required for the preparation of standards and the evaluation of methods, 4. Maintain the analytical reference material repository. 5, Provide analytical reference miterials with supporting documentation to field laboratories. 6. Notify the Field Laboratory Chief, USATHAMA Project Officer, and Analytical Branch when a situation exists at a field laboratory that precludes atatiitical control of remits. 7, Provide a lyitematic review of how the USATHAMA QA Program ii being implemented at each field laboratory by conducting viaits to the field laboratory and reporting the findings to the USATHAMA Analytical Branch and Project Officer. 8. Provide QC samples and data analysis program tapes to field laboratories.
2.2.2 ESE PROJECT QA SUPERVISOR The ESE Project QA Supervisor ii responsible for monitoring and docu- menting the quality of all data reported to USATHAMA. The supervisor's specific responsibilities are: 1. To provide an independent overview of the QC practices of the Project Team from the beginning of the project through acceptance of the final report, to ensure that the team completes all QC requirements of the project plan; 2. To maintain and review all QC records, including control charts, and to provide copies of QC records to USATHAMA on a weekly basis: 3, To prepare those lections of all interim and final project reporta dealing with QC data; 4. To establish teiting lots (batches) in coordination with the Analytical Team Leader and/or Site Manager and to ensure the introduction of appropriate control samples in each lot; 5. To monitor the logging-in of samples, as well as sample preservation, handling, sub sampling, and transport UippughoiitQ the project; AR30IO[b
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6. To audit data files for correct entry of all data and approve all data before tranamittal to Level 2; 7, To obtain and maintain records on Standard Analytical Reference Material (SARM) or interim reference materials; 8. To establiih and maintain liaison between the ESE Project Team and the USATHAMA Central QA Coordinator; 9. To maintain a vigil of the entire laboratory and field operation to detect conditions which might jeopardize control of the varioui analytical and aampling systems; 10. To ensure by field visits that appropriate sampling, field teiting, and field analysis procedurei are followed and that correct QC checks are being aide; 11, To inform the ESE project management and the USATHAMA Central QA Coordinator concerning nonconformance with the QA program and provide documentation of aaid nonconformance, to recommend the corrective actions that are to be taken, and to document their completion; 12. To maintain and update records of the qualifications of the analysts and field team members; and 13, To update QA/QC procedures as new developments occur. This includes new developments in the QA/QC field and specifically any proposed changes in the project QA Plan. Any proposed revisions will be approved by both ESE project management and the USATHAMA Analytical Branch and Project Officer.
2.2.3 ESE SITE MANAGER The ESE Site Manager is responsible for effective day-to-day management of the total project staff, as well as direct communication and liaison with the USATHAMA Project Officer. The Site Manager's responsibility specific to QA/QC is to approve all QA/QC procedurei to be uied in the conduct of the project, to provide additional authority when required to aupport the ESE Project QA Superviior, and to approve of any revisions to the project QC Plan. AR30IOI9 o
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2.2.4 CHEMICAL ANALYSIS SUPERVISOR The Project Chemical Analysis Supervisor is responsible for effective day-to-day coordination of all USATHAMA analytical activity. The Chemical Analysis Supervisor's QA/QC responsibility ii to provide guidance and technical support in resolution of QC problems; to support QA/QC preparation of control simples; ind to provide guidance in preparation of analytical lots to ensure efficient, comprehensive analyiis of all required parameters. Thii supervisor alao provides additional authority, when needed, to support the QA Superviior in analytical natters and must approve all revisions of the (ft Plan regarding analytical activities.
2.2.5 ESE ANALYTICAL OR FIELD TEAM LEADER ESE Team Leaders are responsible for provision of accurate field or laboratory data produced by analysts and sampling personnel under their supervision. They are responsible to the ESE Project Q/t Supervisor to ,-Sj) ens»re that all QC procedures are followed and documentation provided, ' \ The QA role of the Team Leader is, therefore, to assist the QA Supervisor in enforcing QA/QC procedures,
2.2.6 ESE ANALYSTS AND SAMPLING PERSONNEL It is the responsibility of the analysts and field team members to perform the required QA/QC procedures and to document all observations in logbooks in permanent ink. It is the responsibility of the analyst to perform preliminary QC checks to ensure that each batch of data being generated meets all analytical criteria. The field team member or analyst muse also bring any unusual observation or analytical problem to the immediate attention of his/her Team Leader or the ESE Project QA Supervisor.
Each analyst is responsible for ensuring that sufficient quantities of reagents of adequate quality are available for the performance of the required analyses. AR30102©
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QA.l/QAPUN/3.1 O 11/07/84 3.0 ANALYTICAL SYSTEMS CONTROLS
3.1 SAMPLE MANAGEMENT A critical step in the processing of samples involves the initial '" check-in and preparation for analysis. Proper chain-of-custody, efficient processing to meet holding tines, and avoidance of cross-contamination are vital to the integrity of the final data,
Samples are received by the Chemical Analysis Superviior. They are unpacked and the logaheets compared with the contents, Samples are acheduled for processing, and the log sheets are given to the Data Management Coordinator, who activates the sample numbers for analysis, Printouti are generated with updated site identifications (IDs) and sample dates. If any sample processing is required, it will take place immediately,
••—' Sample log-in at the laboratory will be monitored by the QA Supervisor, The QA Supervisor ligns the computer logsheet after verification of complete conformance of the log to the sample set and verification of the information contained on the sample labels, Any inconsistencies or unusual circumstances, such as broken or leaking containers, improper preiervation, or noncompliance with holding or shipping requirements will be identified in writing to the ESE .Site Manager and the Field Team Leader, Corrective action will be recommended and approved by the ESE Site Manager and the USATHAMA Project Officer. When such corrective action involves resampling, this activity may occur based on ESE Project Manager approval, only to expedite the field effort.
Establishment of Army lots will be performed by the Project QA Supervisor after the samples have been logged into the ESE computerized data management system. The QA Supervisor will place samples ta'Pnn i analytical lota based on analysis and sample matrix type,"Ril?T/umbTBroi o tamples per lot will depend on the number of samples which can be
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conveniently and efficiently analyzed as a group. The factora which will be taken into consideration in establishing lot size include: (1) the type of analysis; (2) the analysis complexity; (3) the holding tine for the simple; and (4) the time conitrainti imposed by well development, sampling, and shipping coniiderationi. The batch lot will be optimized to provide efficient analyiis while meeting the holding time criteria for the samples.
The anticipated minimum lot size for sample analysis will be 10 samples. Smaller lot sizes nay be necessary due to the limited number of simples being collected at any particular installation, especially complex sample analysis or extraction procedurei, or holding time constraints. Every attempt will be made to maximize the number of samples per lot,
The following QA procedures will be implemented to monitor sample management. The management of samples , up through the point of '^i':']' deiignating the aliquot to the analyzed, is under the supervision of the I QA Supervisor. o The QA Supervisor will make a trip to each site to inspect the sampling. The QA Supervisor will document the sampling procedures and ensure that procedures described in the scope of work are followed, o The QA Superviaor will ensure that samples are being labeled, preaerved, stored, and transported according to the prescribed methods. o If the QA Supervisor determines that significant deviations from the sampling protocol have occurred, resulting in a compromise of the sample integrity, all samples taken prior to the inspection, subsequent to any previous inspection, will be discarded and fresh famplea taken. o The QA Superviior will control the introduction of control samples (spikes and blanks) into the sample flow, AR30I022 ©
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3.2 SAMPLING .This section describes the QC procedures to be followed during environmental matrix sampling, To ensure samples representative of the system under study, samples must be collected in properly cleaned container!, promptly and properly preserved, and traniported to the laboratory in a manner which minimizes the chance for significant change in constituents. The type of sample (grab, composite, etc,) and the location rationale of the sample point are deicribed in the task Technical Plan. Proven sampling, preservation, and shipping method! which comply with USATHAMA and U.S. Environmental Protection Agency (EP/0 ipecifications will be used to the extent possible. USATHAMA specifications will take precedence over any other specifications, The Field Team Leader is responsible for proper sample collection, documentation, preservation, and shipment. The QA Superviaor monitors the receipt of samples, audits the field sampling procedures, and monitors compliance with preservation and holding time specifications. 0 At least one site visit will be performed by the QA Supervisor during each sampling effort to audit sampling performance. The QA Supervisor may require new samples to be collected if the sample collection procedures are unsatisfactory. Fig. 3.2-1 shows an example of the Field Sampling Audit Checklist, which should be filled out by the QA Supervisor during the site visit,
Pre-printed field notebooks will be made available to sampling personnel. > Notebook pages will describe all the information that is required and the format that is consistent with entry into Installation Restoration Data Management System (IR-DMS), Many qualitative observations (e.g., sketches) that cannot be entered into IR-DMS and that must be used for preparation of later project reports should be retained in permanent record.
Field notebooks will be reviewed and signed by the appropriate Field o Team Leader on a daily basis and reviewed by the QA Supe|Vj^§rQa| Qljjj3 A-ll USATHAMA.2/SAMPCHK.l Section Nuaber 6 Ravlsion Nunbar 1 Data of Revision 11/6/80
Projict ______Project Number _ Data ______Auditor ____ Project Location ______Tltla of Auditor
Item _____ Yes/No Comment 1. Does aach nambir of thi field team clearly understand his/her role and position In both the project and field team itructura?
2. Has a Field Sampling Plan bean filed In the proper manner?
3. Does aach team have In Its possession a copy of the Sampling and Analysis Plan of the QA Plan?
4. Is a permanent field notebook being kept?
5. Does the notebook contain all required information?
6. Has the Field Team Leader signed all pagea In the notebook at the end of aach day?
7. Has all field instrument calibra- tion Information been placed In the notebook?
8. Are iimplas taken from representative locations?
FIGURE 3.2-1 USATHAMA FIELD SAMPLING AUDIT CHECKLIST AND ENGINEERING, INC. I A-12 USATHAMA.2/SAMFCHK.2 Section Number 6 Revision Number 1 Data of Ravlaion 11/6/80
Itaa ______Yes/No Comment 9. Does tht field tiaa have a copy of detailed calibration and operation Instructions for avary Instrument?
10. Are InstruBints properly calibrated at lasst dally?
11. Are replicate samples taken at 10 percent of the sample sites?
12. Are naples preserved in the proper Banner?
13. Are cample containers appropriate for the parameters to be studied?
14. Are preservative acids and reagents of known, high purity and appropri- ate for the analysis?
15. Are samples shipped so that they arrive at the laboratory within holding tines?
16. Are labels with all required inforaatlon affixed to each umplt container?
17. Has back-up identification of aach sample container been aide?
18. Ara proper preservation codes used on the sample labels?
FIGURE 3.2-1 USATHAMA FIELD SAMPLING AUDIT CHECKLIST ENVIRONMENTAL SCIENCE (Continued, Page 2 of 3) AND ENGINEERING, INC.
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USATHAMA. 2/SAMPCHK. 3 Section Number 6 Revision Number 1 Data of Revision 11/6/80
Ita'n" Yes/No Comment 19. Has a standard shipping fora been Included In each package?
20. Are samples properly logged in on arrival at the lab?
21. Are the sanplas collected in a aafa and legal manner? ——— ————— ————— ———— !§> 22. Ware fltld instrumentation and supplies properly requested?
23. Have a Receiving Clerk and alternates bean appointed?
Source: Environmental Science and Engineering, Inc., 1980.
—————— AIUU'Uft!J — !^ FIGURE 3.2-1 ENVIRONMENTAL SCIENCE '"ip USATHAMA FIELD SAMPLING AUDIT CHECKLIST (Continued, Page 3 of 3) AND ENGINEERING, INC. \
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end of the sampling effort to ensure that each page is accurate, understandable, and complete. A copy of the computerized sample logsheet will accompany the samples as a part of the chain-of-custody record.
•• The following QC practices (consistent with the USATHAMA QA Program) will be used during field sampling
3.2.1 VOLATILES Air sampling for volatile compounds is highly dependent on ismpling time, flow rate, and collection device. The collection procedure ii coniidered an integral part of the analytical method for air simples and will be included in the method documentation.
Loss of volatile compounds from water samples can occur through evaporation. Care should be tsken to preclude aeration of the sample i 'j with any gaa, to fill bottles completely with the samples allowing no air spsce, and to analyze within the specified holding times.
Volatile compounds may be analyzed in soil samples only if s solvent extraction step such as tetraglyme extraction is used in the analysis.
3.2.2 GROUND HATER Ground water sampling should not be performed until after newly installed monitor wells have been allowed to reach equilibrium (no less than 14 days sfter well development). All observations and pertinent data developed during ground water sampling will be recorded in a field notebook similar to the field notebook used for lurface water sampling (lee Sec. 3,2.3). The following procedurei will be followed on «"ch sampling day. 1, The depth to water will be meaaured and recorded in the field notebook. O AR301027
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2, Samples will be taken after the fluid in the icreen, well casing, and annului has been exchanged five tines, The amount of fluid exchanged will be measured and recorded in the field notebook. All sampling will be accomplished by a dedicated bailer constructed of polyvinyl chloride (PVC). No glue will be used in the construction of theie baileri. 3, To protect the welli from contamination during ssmpling procedures, the following guidelines will be followed. a, A aeparate bailer will be supplied for, and attached to, each well. This bailer will remain in place in the well during the monitoring phases. b. When a pump is used to purge the standing water from the well, the pump and associated hotel will be thoroughly ... cleaned between the samples uaing water from an approved •ource, c, All sampling equipment will be placed on disposable polyethylene plastic sheeting spread on the ground at the KJ well to prevent toil contamination from tainting the ground water samples, Each polyethylene sheet ia to be used at only one well and then discarded to avoid cross-contamination.
4. The sample will be collected in a manner which will minimize its aeration and prevent oxidation of reduced compounds in the sample, The container will be filled to overflowing without air bubbles and tightly capped. 5, Samples for metal analyses will be vacuum filtered in the field through a 0,45-micron (u) filter, chilled to 4 degrees Celsius ('C), appropriately preserved, and immediately transported to the laboratory, 6, Each simple bottle and cap will be rinaed with water from the well at the time of sampling, 7, Onsite measurements of water quality will include conductivity, pH, and temperature. Calibration standards will to each set of measurements. Calibration standarda for
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conductivity shall consist of lolutioni of potassium chloride . : having conductivities of approximately 1400, 700, and 150 unlios/cm. pH buffer solutions at pH 7.0, 10.0, and 4.0 are used to calibrate pH Deters,
3.2.3 SURFACE HATER Prior to surface water sampling, the following data will be noted and recorded in the field notebook: 1, Site number or location; 2. Date; 3. Tine (24-hour system); 4. Antecedent weather conditions, if Known; 5, In situ parameter measurements; 6, Fractions and preservatives; 7. Any other pertinent observations (odor, fish, etc.); and 8. Signature of sampler and date.
At the conclusion of each day in the field, the Field Team Leader will review each page of the notebook for errors and omissions, He/she will then date and ilgn each reviewed page,
All field instrument calibrationi will be recorded in a designated portion of the notebook at the time of the calibration. Advene trends in instrument calibration behavior will be corrected,
A aingle mid-current sampling point will be used for most streams where lateral nixing is complete. Sampling will take place at approximately 1/2 to 2/3 of the water depth at its deepest point.
Sampling the edge of a stream from the bank will be avoided if poasible, If unavoidable, sampling will be on the outside of a bend where the current flows along the bank, This will svoid collection of quiet or even stagnant water of a quality that does not represent that O of the main flow. Care will be taken to ssmple at a
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with complete vertical and lateral mixing. Simples will not be caken immediately below a waite lource or tributary, unless there is a specific reason to do so,
Sanpling in shallow lakes with good vertical nixing (ai indicated by In situ neasurements) will be accomplished with surface grab samples. Care will be taken that oil or gasoline leakage from the boat motor, if uied, doei not affect the witer being sampled.
In rivera, atraami, and very shallow lakes, frsctions will be taken as a grab sample. The sample container will be held just beneath the surface of the water and allowed to fill,
Prior to the sample collection, each sample bottle will be rinsed with the stream water immediately downstream from the sampling point, Surface water samples will not be filtered prior to analysis,
3.2.4 AIR To avoid contamination when air sampling, air will be passed through the collection device before it is pasted through the pump. All observations during the air sampling effort will be recorded in the field notebook, including the tine of umpling initiation and completion. Sampling ratei will be measured in the complete umpling train, with the measurement process not altering the flow through the umpling train. Neither sampling time nor rate will exceed the time or rate determined during method certification,
3,2.5 SOIL Prior to sampling, turface vegetation, rocks, leaves, snd debris will be removed, Appropriate point sampling or compositing techniques, aa defined in the task Technical Plan, will be used to ensure that the simple ia representative of the area ssmpled and the type of information (e.g., depth of contamination) desired. Soil samples wilAHejlOitvaaJ an amber or foil-wrapped glass wide-mouth jsr with Teflon*-lined lid.
A-1B QA.l/QAPLAN/3.8 11/07/84 O "" Sample containers will be labeled with a preprinted label, chilled to 4'C, and shipped to the laboratory for analysis. Sampling equipment will be thoroughly cleaned between ismpling locations with water from an approved lource. Sampling equipment will be rimed and scrubbed with acetone and hexane after the water rinse and allowed to air dry. If a '" composite sample is required, a suitable compositing technique, such as that shown in Fig, 3,2-2, will be used, Each composite soil sample will consist of a homogenized composite of five subsanples taken within a 3- to 10-meter (m) radius at the aelected sampling point, Each point sample taken from the surface to a specified depth should be quartered to approximately 0,5 kilogram (kg) and placed in the sample container,
Mixing of lubiamplea in the field to form a compoiite sample should be performed by placing the lubiamplei in a steel or aluminum tray lined with aluminum foil (dull side up). No plastic should be allowed to contact soil samples requiring organic analysis.
0 3.2.6 SEDIMENTS All sediment samples will be collected with a hand piston sampler or other appropriate device, After sampling, depth of water at each sampling point will be measured and recorded. Sampling equipment will be thoroughly cleaned with water from an approved source snd solvent rinsed with acetone and hexane and allowed to air dry.
Sediment samples will be placed in amber glass or foil-wrapped containera with Teflon*-lined lids, shipped under ice, and itored at 4'C.
Observations recorded in the field notebook at time of soil sampling will consist of: 1. Site identification; 2. Description of location, including diitance from surveyor'i stake to sample point; AR30 I 03 I o 3. Date; ......
A-19 Figure 3.2-2 SURFACE SOIL COMPOSITE ENVIRONMENTAL SCIENCE SAMPLING METHOD AND ENGINEERING, INC.
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0 4. Time (24-hour lyitem); 5. Deicription of vegetation; 6, Characteristics of soil; 7. Sample number; 8, Fractions and preservations; 9. Other obiervationi; and 10, Signature of sampler.
3,3 SAMPLE PRESERVATION The Field Team Leader is responsible for proper sampling, labeling of samples, preservation, and shipment of samples to the laboratory in a proper manner to neet required holding tines. Table 3,3-1 identifies the proper container, preservation, and holding times that will be used for USATHAMA projects. Anber-glais bottles or bottlei wrapped to prevent light expoiure will be uied for all samples to be analyzed for organic species, Plsstic containers will be constructed fron linear polyethylene, The holding times in Table 3,3-1 will apply to both water o •nd soil/sediment samples,
Table 3.3-2 identifies the proper preparation of sampling containers to ensure that all ssmples properly represent constituents within the environmental matrix sampled. Responsibility for properly prepared sampling containera and preservation reagenti rests with the Chemical Analysis Supervisor, based on the notification of the sampling schedule by the Field Team Leader and/or ESE Site Manager.
3.4 SAMPLE PREPARATION The following paragraphs describe the preparation of water, soil, sediment, and standard samples for analysis, The Project QA Supervisor will monitor the sample preparation procedure to assure compliance with USATHAMA requirements. AR30I033 o
A-21 Or,;.,.,\'AL (Red)
Table 3.3-1. Cantainsrs, Prisarvaclon, snd Holding Tiau
Mlxlisum Measurement_____Container____Preservative___Holding Time Acidity P Cool, 4'C 14 diys Alkalinity p Cool, 4'C 14 diyi Amnnli P Cool, 4'C 28 diyi to ?H<2
Biochemical oxygen demand P Cool, 4'C 48 hours B1ochei»1c«l oxygen demand P Cool, 4'C 48 hours Cirbonietous Bronldt P None required 28 days CtiMleil oxygin demand P Cool, 4'C 28 diyt H2S04 to pH<2 Chloride P None required 28 days Chlorine, tatil riitduil P Determine on site 2 hours Color P Cool, 4'C 48 hours Cyanide, tatil and mumble P Cool, 4'C 14 diys to chlorliutlon " NiOH to pH>12 . 0.008S Ni2S2fl3f Olssolvtd oxygtn Probt S bottlt i top Oitimlni on site 1 hour Hlnkler fi bottle 1 top Fix on site 8 hours Fluorlde P None required 29 days Hirdneii P HN03 to pH<2 6 mntns Hydrogen ton (pH) P Determine on site 2 hours KJeldinl ind orgenle P Cool, 4'C 28 days • nitrogen h^SQ* to pH<2
Chromium VI P Cool, 4'C 43 hours Mercury P HNOj to pH<2 29 d«ys Keuli except ibove P HNOj ta pH<2 6 months
Ml trite P Cool, 4'C 48 hours Nitrate-nitrite P Cool, 4'C . 28 days H2S04 to pH<2 Nitrite ' P Cool, 4'C 48 hours 011 and Sreise S Cool, 4'C 29 days HjSOj ta pH<2 Orjinlc Carton "G Cool- , 4'>PH A-22 Table 3,3-1, Containers, Prasarvscion, and Holding Tiaai (Continued, ?t(i 2 of 3 Maximum Htnurement Container Preservitlve Holding Time Organic Compounds* *G, teflon- Cool, 4'C 7 dtyi wtractaoiaj i including lined eip .(until extraction) phtttilites, nltroiamlnei 0.008? Na2S203r 30 days orgenochlorlne pesticides, (after extraction) PCa'i, nltroaroiMtlei, liophorone, polynueleer iromtlc hydrocirboni, Italoethers, chlorinated hydrocirbons ind TC30) Extractives (phenols) *G, teflon- Cool, 4'C 7 diys lined cap .(until extraction) 0.008S Na2S203r 30 days (after extraction) Purgeables (halocarbonj, *B, teflon- Cool, 4'C , 14 days aromatlci, Acroleln, Jined septum 0.008* Na2S203~ and Acrylonltrill) ••—N ———————————————————————————————————— '._) OrtJiopnoiphate P Filter on site 48 hours -^ Cool, 4'C Pesticides *G, teflon- Cool, 4'C 7 days lined cap .(until extraction) 0,0081 Na2S203r 30 days (after extraction) Phenols *G Cool, 4'C 29 days H2S04 ta pH<2 Phosphorus (elemental) G Cool, 4'C 4Q hours Phosphorus, total P,G Cool, 4'C 29 days H2S04 to pH<2 Residue, total Cool, 4'C 14 days Residue, filterable Cool, 4'C 14 days Residue, nonflluraole Cool, 4'C 7 days Residue, settleaale Cool, 4'C 7 days Residue, volatile Cool, 4'C 7 nays Sills* Cool, 4'C 29 days Specific cunductance Cool, 4'C 29 days Sulfate Cool, 4'C 29 days Sulflde Cool, 4'C 29 days Zinc Acetate AR30I035 O A-23 Table 3,3-1, Cantainin, Prisirvation, and Holding lisas (Continued, Page 3 of 3) Maximum Measurement Container Preservative Holding Time Sulflte P Cool, 4'C 48 hours Surfactants P Cool, 4'C 48 hours Temperature P Determine on site Immediately Turbidity P Cool, 4'C 48 hours i - Polyethylene (P) or Gliss (G). b - Simple preservation should be performed Immediately upon sample collection. For composite simples each aliquot should be preserved it the time of collection. When use of in automatic simpler mikes It Impassible ta preserve each aliquot, then simples miy be preserved by maintaining it 4'C until compositing ind sample splitting Is completed, c • Samples should be analyzed is soon is possible ifter collection, The times listed ire the maximum tints that .imples may be held before analysis and still considered valid,! Simples rv/be held for longer periods only If the laboratory his data on file ta sin- • that the specific types of samples under study ire stable for the longer ti,ie. Some simples may not be stable far the maximum time period given In the table. A laboratory Is obligated to hold the simple for i shorter time If knowledge exists ta shew this Is necessary ta maintain simple Integrity. d • Simples should be filtered Immediately on site btfore adding preservative for dissolved metals. e • Guidance applies ta samples to bf analyzed, by GC, 1C, or GC/MS for specific organic compounds. f - This should only be used In the presance of residual chlorine. (Conpounds not, found on Table 3,3-1 should ba preserved a: 4'C: icaraia; 1 weak). *Aabar-glass bottle. ' < H.SO, • Sulfurie acid. NaOH Sodiua hydroxide, Sodiua thlosulfata. Nitric acid. in To lyehlorlnat ad bishenyls . TC3D Tatrachloradibanzo-p-diaxln . GC Gas chranatography. 1C Liquid chxonatography. GC/MS Cas ehranatography/aass speewonacry Sourcs; HA, 1979. AR30I036 A-24 QA.1/VIB332-1.1 O 09/20/84 Table 3,3-2. Simple Container Cleaning Procedures Analysis/ Cleaning Paraneter Container Type Matrix Procedure* CC/MS Analyses Amber-Glasi Bottle Hater 1 Organic Compound! with Teflon'-Lined Cap Class Msson Jar— Soil/Sedinent 1 Foil-Wrapped with Teflon*-Lined Cap Volatile Organics Amber Septum Vial Water 2 with Teflon*-Lined Septum GC/HPLC Analyses Amber Glsss Bottle Water 1 Organic Compounds with Teflon'-Lined Cap Glass Mason Jar-- Soil/Sediment 1 o Foil-Wrapped with Teflon*-Lined Cap Total Phenoli Amber-Glass Msson Water 1 Jar with Teflon*- Lined Cap Oil and Grease Amber-Glsss Mason Water 3 Jar with Teflon*- Soil/Sediment Lined Cap Organic Carbon Amber-Class Mason Soil/Sediment 1 Jar with Teflon*- Lined Cap Metals Linear Polyethylene Hater 3 Cubitainer Glass Mason Jar with Soil/Sedinent 1 Teflon*-Lined Cap JR30I037 O A-25 QA.1/VTB332-1.2 11/06/84 Table 3,3-2. Sample Container Cleaning Procedurei (Continued, Page 2 of 2) Analysis/ Cleaning Parameter Container Type Matrix Procedure* Anionii Cyanide, Nitrates, Linear Polyethylene Water 4 Sulfate, Phosphate, Cubitainer Fluoride, Chloride, Other Inorganics Glass Mason Jar with Soil/Sediment 1 Teflon*-Lined Cap * 1—Thoroughly wash contsiner with hot detergent and water; triple rinse with tap water; triple rinse with D.I, water; rinse with (nanograde) acetone; rinae with (nanograde) hexane; bake at 200'C for 2 houra, except 1-gal amber jugs, always use new jugs and air dry. 2—Thoroughly wash container with hot detergent and water; triple rinse with tap water; triple rinse with D.I. water; air-dry; bake at 200'C for 2 hours; soak septa for leversl hours in nethinol; bake at 150'C for at least 1 hour, (Note: Always use new bottles, do not reuse bottles), 3—Rinse with 2 to 3 ml of ultrex nitric acid and drain thoroughly, 4—No cleaning procedure required; use new cubitainer. 5—Thoroughly wash container with hot detergent and water; triple rinse with tap water; triple rinse with D,I. water; rinse with nanograde freon; air dry. Abbreviations GC/HPLC • Gas chromatography/high-pressure liquid chromatography. D.I, • Deionized, Source; ESE, 1983. AR301038 A-26 QA.l/QAPLAN/3.10 11/07/84 3.4.1 WATER SAMPLES With the exception of ground water samples for netals analyses (which are filtered in the field) and tanplei for volatilei analyiii, nil ground water samples will be filtered through 0.45-u membrane filtera, Surface water aimplei will not be filtered. Filtration will be perforned on a Millipore extraction procedure (EP) toxicity positive- pressure filtering device, A supply of clesn amber jugs will receive the ssmple filtrate, The filtration device, which is stainless steel coated with Teflon*, will be washed carefully with soap and water and rinsed with D.I. water, acetone, and hexane before each sample is filtered. The following series of filters nay be required for each filtration; glass fiber prefilter and 0.8-u, 0.6-u, and 0.45-u membranes. This layering of filters prevents clogging of the 0,45-u filter during filtration of heavily sedimented ground water. The device is sealed, and the sample is introduced to the filtration chamber, Nitrogen pressure is applied to the water sample slowly and should not O exceed 40 pounds per square inch (psi). If samples containing high levels of contamination are expected, the suspected high-level samples will be filtered last and the suspected low-level samples filtered first to minimize the possibility of cross contamination. Samples for volatiles determination will not be filtered to avoid analyte loss by volatilization. 3,4.2 SOIL SAMPLES Percent moisture for soils and sediments will be determined prior to analysis using a procedure comparable to American Society for Testing and Materials (ASTM) Method D2216-71 (ASTM, 1981) on sieved and air-dried soils and wet sedinents. Unless specified differently in the Project Technical Plan, toils will be dried and sieved before analysis. Samples will be placed in 13-inch (in) by 15-in aluminum trays, which are lined o (dull side up) and labeled with the sample number and air dried at room A-27 QA.l/QAPLArt/3.11 11/07/84 tenperature. While drying, soil samples will be crushed gently with a nortar or the bottom of a small beaker, After soils are dried and thoroughly crushed, aliquots undergoing netals analyses will be sifted through a US Series 600 polyethylene sieve, and thoie undergoing organic analyiei will be lifted through a US Seriei 600 bran aieve to remove rocki and vegetative material. Before every umple is sifted, the aieve will be thoroughly scrubbed with soap and water and rinsed with D.I. water, acetone, and hexane, Braaa sieves are used for organica analysis to avoid phthalate contamination which occura with polyethylene sieves, and, converaely, the plastic sieves are used for metals analysis to avoid trace metal contamination, Becauie the soils may be heavily contaminated with haxaUous chemicali, appropriate aafety precautioni (as established in the Project Safety Plan), which may include the use of gloyes, respirators, or a dust mask, will be taken during sieving, The unused and unsifted portion of the soil sample will be returned to its original container, The sifted sample will be placed in a clean, labeled glass jar with a Teflon'-lined lid, 3,4.3 SEDIMENT SAMPLES Because of the long drying times involved in processing and sieving very wet sediments, sediments will be analyzed in their "wet" condition. The sediment sample will be made as homogeneous as possible by vigorous mixing with a spatula before a subsample is tsken, 3.4.4 STANDARD SAMPLES Preparation of standard toil and water for methodi development and analytical systems control is described in Sec. 3.8.2. Standard soil consists of uncontarainated toil from USATHAMA-approved source. 3.5 SUBSAMPLIMG Subsampling the field soil sample to size will be performed by the snalyst upon arrival of the sample at the ESE laboratory, All subsampling should be accomplished using proper quarteringAR30IOl» techniques. 0 A-28 QA.l/QAPLAN/3.12 o 11/07/84 3,6 CONTROL SAMPLES Control samples will be introduced into the train of actual samples as a nonitor on che performance of the analytical systen. Control samples will consist of spiked standard tanplea and blinks. In GC/MS analyies, natural samples are ipiked ai control samples, Results from spiked control samples will be used to construct control charts to monitor variations in the precision and accuracy of routine analyses. The specific type and number of control samples and the construction of control charts are described in Sec. 4,2, 3.7 REFERENCE MATERIALS When available, SARMs supplied by USATHAMA must be used to prepare calibration stsndards and spiking standards. SARMs or interim SARMs are naterials that have undergone extensive purity and stability checks. When SARMs are not available or their quantities limited, "as is" chemicals nay be uied as interim reference materials, However, the "as is" material should be stored at O'C and a portion retained for a compariion with the approved SARMs when available. All reference compounds used in the USATHAMA projects will be stored at O'C and protected from light. The QA Supervisor will request SAKMs as required. The QA Supervisor maintains a record of receipt of SARMs and monitors their use. 3.8 ANALYTICAL METHODS AND CERTIFICATION 3.8.1 RATIONALE Two different types of snalyses recognized by the USATHArtA QA program (semiquantitative and quantitative analyais) may be conducted during tasks assigned under theie contracti. Each type of analysis requirei a different level of documentation, including precision and accuracy data and a different set of daily or batch-related QC criteria, The following sections outline the testing procedures which will be used to define the detection limit, precision, snd sccuracy of each analytical o method. AR30IO••••••M " • A-29 QA.l/QAPLAN/3.13 11/07/84 Method certification in standard nedia will certify the laboratory to run isniquantitative or quantitative analyses for a given analyte, Documentation of the analytical teiting certification will be submitted to USATHAMA for approval before uie of the analytical method for • analyiii, 3.8.2 METHOD CERTIFICATION The following paragraphs describe the procedurei to be used to certify analytical methods. All methods certification and documentation data will be developed in atandard natrices. The standard matrix for documentation of inorganic analyses (e.g., sulfate, nitrate, or metals) in water will be deionized water conforming to ASTM Type II grade water. The atandard matrix for documentation of organic analyaia will be deionized, organic-free (ASTM Type IV) water containing 100 milligrams per liter (mg/1) each of sulfate and chloride prepared as follows: 1, Add 1,48 grama (g) of dried reagent grade anhydrous sodium sulfate to a 1-liter (1) volumetric flask and dilute to volume, 2, Add 1.65 g of dried reagent grade sodium chloride to a 1-1 volumetric flask and dilute to volume, 3. Transfer 100 ml of each (1 and 2) to a 1-1 flask and dilute to volume, The resulting solution is 100 mg/1 esch of chloride and sulfate ions. These two types of water will be used as blanks or will be spiked with the compound!s) of interest prior to processing through the complete analytical protocol. The data for documentation of both inorganic and organic analyses in soils snd aquatic sediments will be developed using sn uncontaminated "standard" soil matrix. An aliquot of sieved dee Sec. 3,4.2) "itindard" toil will be carried through each set of docuraeitBttofl I Ql|2 ' ' ' A-30 QA.l/QAPLAN/3.14 11/07/84 ssnples to act as a blank. Added concentrations of the subject analyte(s) will be dissolved in a volume of solvent just sufficient to wet the soil. This solution is poured over the subsample of soil and allowed to itand for 1 hour prior to beginning analysis, and the solvent ii allowed to evaporate. The "itandard" toil will consist of a homogeneous simple of sufficient size to provide a single continuous source for all nethod documentation and subsequent analytical system control. The "itandard" aoil will be •elected to conform with the type of toil to be encountered, However, any natural toil which contains no, or a very low level of, analytes to be detected may be used with the approval of the ESE Site Manager, QA Supervisor, USATHAMA Project Officer, and the USATHAMA Analytical Branch, If, and only if, a column is to be used Cor the extraction, the analyte' may be dissolved in the minimum quantity of the solvent consistent with 0 volumetric transfer. The solution is placed on the column and allowed , to soak in before additional extracting solvent is introduced. Certain compounds or elements (e.g., nitrate or iron) will be present as a natural component of the soil, This bsckground will be accounted for where it exists, and the detection limit for the particular method will be considered as the statistically resolvable quantity above the background concentration. Semiquantitative Analyses Semiquantitstive snalytical methods are used in USATHAMA programs to screen samples for the presence of unknown, as well as known, contaminants. The detection limit of the totsl method will be estimated by spiking stsndard matrices of interest (water, toil, etc.) with the ipecific O analytes or surrogate analytes at 0 (blank), 0.5X, X, 2X> •'•••a^iOW1! Wk '3 "• A-31 ORIGINAL (Red) QA.l/QAPLAN/3.15 11/07/84 where X is the desired or required detection limit. The analyte should ^ be dissolved in a water-miscible solvent to prepare the ipiking solution, The ipiked level i should be at dote as possible to those listed, but a reasonable attempt at producing these levels will be considered acceptable, The spiked simples will be analyzed through the entire analytical method. After analysis, the detection Unit will be calculated using the USATHAMA detection limit program. The detection Unit determined by this process will be reported as the detection limit of the semiquantitative method. In summary, certification of a semiquantitative method requires the following: 1, One spiked stsndard matrix sample at each of five concentration levels, plus a blank analyzed in a single day, 2, The detection limit calculated using the USATHAMA detection limit program, 3, The precision of semiquanticative analyses will be reported as "999," on data management entries, /^p 4, The accuracy will be the slope of the best-fit linear regression line of found versus target concentration. 5. The best-fit linear regression line must hsve a minimum correlation coefficient of 0,996 for the calculation of the detection limit and accuracy, Exceptions to this criterion must be approved by the USATHAMA Analytical Branch. 6. Documentation of the procedures .in USATHAMA format. Semiquantitative certification for the GC/MS analysis will be performed using a mixture of actual analytes and surrogate standards, Quantitative Analyses Requirements for certification of a quantitative method are as follows; 1. One spiked standard sample it each of five concentration levels, plus a blank analyzed each day for 4 separate days, 2. Tne detection limit will be calculated using the detection limit program, A-32 (Red) QA.l/QAPLAN/3.16 o 11/28/84 3. The precision of the quantitative analyses will be the standard error of the best-fit linear regression line of found-versus- target concentration values for the dsta generated during the certification testing, 4. The accuracy of the quantitative analyses will be the slope of '" the best-fit linear regression line of found-versui-target concentration, 5. Documentation of the procedures in USATHAMA format. 3.9 ANALYST CERTIFICATION A lisi: of qualified personnel for each sampling and analytical task will be provided by the appropriate Department Managers to the Project QA Supervisor, The QA Supervisor will keep a logbook arranged by type of analysis (e.g., Autoanalyzer, atonic absorption, GC, GC/MS, etc.), Analysts' nanes will be entered under the qualified headings with the Departnent Manager's initials and date certified (Fig, 3.9-1). At O regular intervals, each Department Manager will review the capabilities of each analyst and recommend whether certification should be continued. A sinilsr log will be maintained for the field sampling team members. During the conduct of this project, the QA Supervisor will inspect the laboratory periodically to determine if analyses are being perforned only by certified analysts. Data reports require the name of the analyst on the report sheet, All sample lots will be checked to verify that certified analysts performed the analyses. Analysts will demonstrate their proficiency in conducting a particular chemical analysis by showing evidence of acceptable performance on past routine QC sanples analyzed with each batch of samples. In additiont for any analytical method, analyiti or an analytical team consisting of specific individuals will be considered to be certified to run a particular analysis, if they hsve been involved inAlCvMbJplng4M o precision snd accuracy data needed for method documentation, The precision and accuracy data generated during nethod documentation muit A-33 \(Red)/ UULBISTzn torLtiW A-l,* AMalTsia TT "Ss Data Ca^a • t. , SOURCI: I3E, 1H9. TYPICAlwRTIFICATION ENVIRONMENTAL SCIENCE { AUDrf PAGE AND ENGINEERING, INC. A-34 QA.l/QAPLAN/3,17 o 11/07/84 be acceptable to the Analytical Team Leader and the QA Superviior. Mew analysts performing an eatabliihed analytical procedure will be conaidered to be conditionally certified until tre tint let of QA/^C dati are generated. These QC data are required Icr every lot of simples analyzed. If these QC data are in control based on precision and accuracy control charts, the snalyst or analytical team will be considered to be certified to run that particular analysis, QC data which do not neet established, QC requirements will be rejected, and corrective action which may include reanalyiii of the lot of sample* and further training of the analytical team, will be taken, AR30IO•'M A-35 .,., \(Red), QA.l/QAPLAil/4.1 11/07/81 4,0 ANALYSIS OF SAMPLES The following describea the QC procedures snd retirements for sample analyses conducted during this project, These QC requirements are in addition to any specific calibration requirement! presented in Sec. 5.0. All iimples will be analyzed within the certified range of the analytical method. Dilution of a simple extract with extracting solvent or of the original ssmple nitrix with distilled/deionized water ihould be performed if the concentration of analyte is greater than the certified range of the method. 4.1 LABORATORY INSTRUMENT QC CONTROLS Daily QC of the analytical systems ensures that accurate and reproduc- ible results are produced. The analyst must check instrumental calibration data for compliance with QC requirements, Out-of-control data will be automatically flagged and brought to the analyst's attention. Table 4.1-1 describes the instrumental checks to be implemented by ESE for USATHAMA projects. Initial calibration should be performed under the following conditions: (1) when an analysis is first set-up or prior to the first set of samples, (2) when the instrument has been idle for long periods of time, (3) when the instrument detector has been subject to major maintenance, or (4) when the instrument fails the daily calibration QC checks. Deviations from the USATHAMA instrumental QC requirements will occur for certain analyses, The requirement for recalibration of the instrumental system at the end of each day's run is not practical lor necessary for certain analyses using standard EPA procedures because of the excessive time required for calibration. For most analyses (cyanide, phenols, GC, HPLC, nutrients, etc.), only one calibration standard will be repeated AR30IIU8 A-36 QA.1/VTB411-1.1 09/20/84 ' J Table 4.1-1. Summary of Instrumental Systems Control Requirements Requirement Analytical Control Limits o Initial Calibration o Calibration curve—concentration (using actual analytes series 0 (blank), 0.5X, X, 2X, 5X, or surrogates) and 10X, where X is the concentration of analyte in the instrumental (GC/MS uses surrogates standard corresponding to an analyte and actual analytes) concentration in the sample at the • desired detection limit o Dsily Calibration o Calibration curve—concentration (except GC/MS) series 0 (blank), X, 5X, and 10X minimum o All samples analyzed must be bracketed by standards above and below and be within the established certified range of the method o Calibration standard is repeated at end of day or analytical run, and response of the standard must agree ' with previous response within +15X o Correlation coefficient of standard curve XJ.995 o Daily GC/MS Calibration o One calibration standard is run and calculated response factor for . surrogate analytes must agree with initial calibration response factors within +252 or new calibration curve run ~ o All samples analyzed must be within • the linear range of the instrument and the certified range of the method o Instrument calibration with DFTPP or BFB ICAP • Inductively coupled argon plasma, » . . DFTPP • Decafluorotriphenylphosphine, BFB • Bromofluorobenzene. Source: ESE, 1983. AR30IIU9 O A-37 , QA.1/QAPLA.V4.2 11/07/84 at the end of the day. [All samples will be bracketed by calibration standards.] 4.2 CONTROL SAMPLES Control simples are spiked samples of itandard water or "itandard" soil which are run with each lot of samples, As part of the automated QC checks, the ESE data management system checks the results of control spikes run with each Army lot and flags all data that are out of control. Table 4,2-1 summarizes the control samples and control charts required for the USATHAMA projects, In applying the QC requirements presented in Table 4,2-1 to quantitative analyses and parameters, at least three control samples will be run on each day of instrumental analysis. In applying the QC requirements presented in Table 4.2-1 to some analyses and parameters, modifications to these requirements may be necessary. For certain GC, high-pressure liquid chromatography (HPLC), and GC/MS analyses, the daily through put of samples is severely limited by the instrument analysis runtime. In these cases, ESE will define a group of samples which are extracted in 1 day as a lot and apply the control spike requirements to this extraction lot. At least one control spike extract will be analyzed on each day of instrument analysis, USATHAMA approval of this deviation will be required prior to sample analysis. Since certification for semiquantitative analyses only requires that one target-versus-found curve be established, the designation' of control limits for accuracy baaed upon the standard deviation of the slopes of a number of target-versus-found curves is not possible. In this case, ESE will use historical data from previous analyses (if any) or will set up temporary control limits on the slope of the control sample curves of +20 percent. As the number of control samples analyzed increases, criteria based on +3 (standard deviation of slope) will be established, A-38 QA.1/VTB421-1.1 11/06/84 n Table 4.2-1. QC Requirements by Sample Lot Requirement Analytical Control Limits o Control Samples o At least one standard matrix method (Quantitative/Serai- blank for each daily lot or extrac- ,„ quantitative Analyses) tion batch (Except GC/MS) o Three standard matrix control spikes at approximately 2X, 5X, and 10X, where X is the documented detection limit per daily lot o Control Samples o At least one standard matrix method (GC/MS Semiquantitative blank for each daily lot or extrac- Analyses) tion batch spiked with deuterated surrogate standards. o Deuterated surrogate standards spiked at approximately 2X, 5X, and 10X, where X is the concentration in the matrix corresponding to the documented detection limit, The original matrix of each sample and x method blank is spiked with one of 1 the above levels, Lot must contain _..•' at least one spiked o Accuracy Control Chart o Plot slope of regression line of (Quantitative and found-versus-target concentrations of Semiquantitative) < spikes o Control limits (+3S) and warning limits (+2S) will be initially based on the sTandard deviation of the slope of regression lines obtained during method certification, Control limits-are updated based on results of spiked samples analyses performed with each lot of samples, o Precision Control Charts o Plot mean found concentration for the (Quantitative Analysis 5X spike level during the method Only) certification o Control limits (+33) and warning • limits (+2S) wilT be initially based on the sTandard deviation of 5X level during method certification, Limits are updated based on results of 5X spikes performed with each lot of samples. * If more than one lot is analyzed or processed in 1 day, only one > ] control spike sample required per lot, but three control wifcQsft I 051 >^ required for day. HI*1*"! .. ' Source; ESE, 1983. QA.l/QAPLAN/4,3 11/07/84 The Laboratory QA Coordinator is responsible for introducing the control samples into each analytical lot before analysis. Subsequent to analysis, the Project QA Superviior reviews and approves all control sample data by Army lots before the results are I'lniraitted to USATHAMA as Level 1 data, Precision, accuracy, and the detection limit for each analytical lot which passes QC criteris are automatically entered into . the appropriate chemical analysis file for transmission to USATHAMA, The QC results for the QC control simples also are included in the format required by the Installation Restoration (1R) Data Management User's Guide (USATHAMA, 1984). Failure to pass the instrumental calibration or control sample QC criteria represents an out-of-control situation and calls for corrective action as required by the USATHAMA QA Plan, which may require rerunning and/or resampling and rerunning the entire lot samples. Written 'W-'V notification of QC failure is provided to the ESE Site Manager and the Chemistry Supervisor. AR30I052 A-40 QA.l/QAPLAN/5.1 O Il/06/d4 5.0 INSTRUMENT CALIBRATION AND W.-.'IENANCE "• A calibration procedure establishes the relationship between an accurately known calibration standard and the measurement of that standard by an instrument. Calibration is not to be confused with standardization. Standards are run each time an instrument is used, while instrument calibration is performed only at specified intervslt. Operiting procedures must be available for all equipment and analytical instrumentation. Such procedures are generally provided by the ( manufacturer. An up-to-date report for each calibration standard used in the calibra- '~NN tion system should be provided. If calibration services are performed by a commercial laboratory on a contract basis, copies of reports issued by them should be maintained on file. All contractor calibration reports are kept in a suitable file by the QA Supervisor and contain the following information: 1. Report number; 2. Identification or serial number of the calibration standard to which the report pertains; 3. Conditions under which the calibration was performed (temperature, relative humidity, etc.); 4. Accuracy of calibration standards (expressed in percentage or other suitable terms); < , , 5. Deviation or corrections; and 6. Corrections that must be applied if standard conditions of temperature, etc., are not met or differ from those at place of calibration. AR30I053 A-41 QA.l/QAPLAN/5.2 11/06/84 Contracts for calibration services should require the contractor to supply records on traceability of their calibration standards, All equipment which can be calibrated should hav < affixed to it, in plain sight, a tag bearing the following information: Description: _____ Identification No,: Lilt Calibrated; _ Calibrated By: __ Calibration Expires: NOTE: Uie of this instrument beyond the calibration expiration date is prohibited. When the equipment size or its intended use limits the application of labels, sn identifying code should be applied. ft' Equipment past due for calibration should be removed from service either physically or, if this is impractical, impounded by tagging or other means, 5.1 FIELD INSTRUMENT CALIBRATION Instruments used to perform field measurements (e.g., pH, temperature, conductivity, water level) will be calibrated in accordance with procedures outlined in the appropriate operating manual.' 'All equipment will be calibrated daily or after every 20 observations. Calibration checks will be performed after measurements are made at each sampling site, All calibration data and calibration checks will be entered,i^nto the field notebook. Failure of an instrument to maintain accurate calibration will be reported to the Field Team Leader, who must take immediate corrective action to ensure that accurate field data accompany any samples. The faulty instrument is tagged and cannot be used until A-42 •. '•-.' QA.l/QAPUri/5.3 O repaired and until recalibration is verified by the Project QA Supervisor. In the event that field measurements must be made using instruments having questionable accuracy or calibration, the Field Team Leader must « immediately identify the problem to the QA Superviior, If recommended corrective action involves including suspected measurements in the sampling record, this must be approved in writing by the ESE Site Manager, USATHAMA Project Officer, and the USATHAMA Analytical Branch. Generally, if proper field measurements cannot be performed, alternative means will be employed to verify the field data, which will be discarded, or the system will be resarapled when accurate field measurements can be performed. These corrective actions will be agreed upon by the QA Supervisor, ESE Site Manager, USATHAMA Project Officer, and USATHAMA Analytical Branch. •~N 5.2 ANALYTICAL NOTEBOOKS AMP INSTRUMENT LOGBOOKS '~j// The ultimate repository for information concerning analyses performed in the laboratory is the analyst's personal laboratory notebook and the instrument logbooks, Each analyst is required to have a personal notebook designated by a unique number. Responsibility for maintaining complete laboratory notes lies with each analyst. The ESE QA Supervisor may audit Isboratory notebooks without notice. The list of assigned .notebooks is maintained by the ESE Chemistry Division Secretary and contains the' following information; 1. Notebook number, 2. Assignee, • ... 3, Responsible Group Leader, and 4, Disposition or location and date, Laboratory notebooks will not be taken from ESE without wri^iQQ | 055 ,_^ permission of the Chemical Analysis Supervisor and the ESE Sue A-43 .,, \(Red) QA.l/QAPLAN/5.4 11/06/84 Manager, Every entry into the notebook should be dated and signed, Entries in the personal notebook will vary depending on the role of the individual in the laboratory and the type of wort being performed. At a minimum, the personal notebook should contain: 1, A reference to or a description of the procedures used for sample work-up or analysis, 2, A summary of the samples extracted or analyzed, 3, Weighings and calculations of standard concentrations, snd 4, Infornation on spiking procedures and observations and comments on the procedures or simples. An instrument logbook will be maintained for certain analyses. Each time an instrument is used for sample analysis, the following information is entered; 1. Date of analysis; 2, Project name and number; 3. Number of samples analyzed, type of sample; 4, Time spent on analysis (start to finish); 5, Preventive maintenance performed, if any; 6, Time spent on preventive maintenance; 7, Instrument calibration performed, if any; and 8, Name of analyst, Additional notes are made in the instrument logs when required. These notes are particularly important when abnormal instrument or analytical performance is observed, It is the analyst's responsibility to ensure that instrument logs are'properly filled out and kept up to date, The QA Supervisor monitors and audits the status of instrument logbooks. No samples are to be run on any instrument which fails calibration and not until it is clearly demonstrated that the instrument is back in control. AR30I056 A-44 ORI3INAI (Keen QA.l/QAPLAH/5.5 n 5.3 SPECIFIC ANALYTICAL SYSTEMS CONTROL 5.3.1 METALS SYSTEM CONTROL The following are the routine QC procedurei required for flame and graphite furnace atonic absorption analysis (AAS,, 1, Instrument calibration ii checked using stindard solutions. •H Instrument response ii plotted (uiing a hand calculator) againit concentration. The slope is compared to historical slope data to verify that the performance of the instrument is latisfactory. The control charts are kept in'the instrument logbook, which also contains a record of routine maintenance and documentation relating to any downtime due to instrument malfunctions, If readings are excessively low, the analyst will check gas flows, burner or cell alignment, wave length, slit width, photomultiplier voltate, and lamp intensity for problems, 2, Blanks and spiked samples are analyzed with each batch of .._y samples, ._,-' 3, Strip chart recorder tracings for standard solutions, samples, spikes, and duplicates are all stamped for identification and filed in the instrument roon, Analyses run on the ICAP system will require specific instrument calibration and maintenance controls. Routine maintenance on the Jerrill-Ash ICAP system by the manufacturer's representatives is performed on an annual basis. In addition, a quarterly service contract is maintained on the minicomputer. Periodically, the analyst will dismantle, clean, and reassemble the torch and nebulizer to prevent serious sensitivity problems., , , Calibration with selected standards will be performed daily to ensure that the instrument performance has not deteriorated. The failure to achieve standardization could require cleaning, including changing the tubing of the sample delivery system. Spare parts are avainwlvvor Ot57 system components most likely to experience failure. A-45 c...-,., ttec,') (JA.l/QAPLAN/j.6 11/06/84 - © 5.3.2 NITRITE PLUS NITRATE, SULFATE, AND PHOSPHATE ANALYSES The following are the routine QC procedures required for nitrate and sulfate analysis using Technicon Autoanalyzer ami Hach Turbidimeter: 1. Standard calibration aetting must be wi..in specified limits for each standard range and each parameter; /« 2, Color and turbidity blanks must be run on all samples with visible color; and 3, A notebook containing strip charts, sample logs, instrument maintenance and stsndard conditions will be kept by psraueter, All deviations from the standard conditions must be recorded and corrected, with all corrective action explained, Additional maintenance of the Technicon Autoanalyzers will include daily inspection of pump tubes for deterioration and replacement. The temperature of the instrument room and reagent will be controlled to maintain equipment stability. ' J.J.J uu GC septa will be replaced on a weekly basis or more frequently as needed when symptoms of septum deterioration are noted. Frequent injections will require replacement on a daily basis. When the supply of gas in the cylinders falls below 100 psi, carrier and detector gases will be changed to prevent contaminants from reaching the detector or columns. Molecular sieves and oxygen traps used in the gas lines will be replaced on a regular basis. GC detectors will be removed and cleaned at least periodically to remove accumulations, which can affect instrument performance. Instrument calibration curves will be monitored and compared-to . . historical performance criteria. Excessive noise, low response, and poor precision are indicators of a dirty detector and may cause more frequent detector cleaning. Spare columns, packing materials, instrument cables, and PC boards will be available in c*>a/|lj?'WMkf]!(CQ |i or malfunction to minimize instrument downtime. " ' • • • - „,,. A-46 ORIGINAL /7>: .1) QA.l/QAPLAH/5.7 11/06/84 - O """" 5.3.4 GC/MS ANALYSIS Qaily instrument control will be practiced to ensure that the instrument is calibrated and in proper working condition, '.lie GC/MS will be tuned periodically with perfluorotributylamine to calii.iite the miss axia and to ensure proper relative abundances. The instrument performance will '« be nonitored with a reference compound such as decilfluorotriphenylphosphine, bronofluorobenzene, and/or with a composite mixture of compounds representative of the samples being analyzed. An instrument tuning log will be maintained to identify any deterioration of initruoient performance, The composite reference mixture will be particularly useful for monitoring the relative sensitivity of the mass ipectronetry (MS) and the integrity of the chroroatographic column. Failure to achieve calibration will require implementation of aource cleaning procedures. In addition, all routine analytical systems controls performed for GC will slso be performed for the GC/MS equipment. The ionizing source O will be periodically dismantled, thoroughly cleaned, and reassembled to prevent serious sensitivity problems, AR30I059 A-4 7 (Red), QA.l/QAPLAN/6.1 09/20/84 6.0 AUDITING AND REPORTING OF DATA The Project QA Superviior ia reiponiible for reviving and approving all field and sampling analytical data before transmittal of data to USATHAMA. Further, all data transmitted to USATHAMA must be validated by the Project QA Supervisor or his representative according to procedures specified in "Sampling and Procedures and Tables for Inspection by Attributes, Military Standard" (MIL-STD-1'05D, April 19, 1963), For the efficient flow of laboratory data to USATHAMA, it is critical that the QA and supervisory reviews of data be orgsnized in s planned methodology which includes successful interface with the data management program, ESE has developed a USATHAMA project data review and transmittal procedure which requires that a formal review and sign-off sheet accompany chemical analysis results of each completed lot of samples, The data are routed to several individuals for approval. This form is presented in Fig, 6,1-1, ESE will use this review procedure for the proposed project, 6.1 SEMIQUANTITATIVE ANALYSES Results will be reported in terms of concentrations in the original matrix and will be corrected for recoveries, moisture, systematic errors, etc,, if these are known. Lack of indications of the presence of specific compounds to be reported should be reported .as "less than" the detection limit. Estimates of concentrations of species which have not been subjected to the detection limit procedure, as in the CC/MS screening procedure, nay be reported based on the response compared .to the response of a reference compound or internal standard provided that; (1) the instrumental response of the species is not less than one-tenth of the response at the documented detection limit of the reference compound; (2) the detection limit of the reference coiopound.hu.been estimated; (3) the estimated concentration contains only oWa3g1irircmr A-48 ARMY DATA RtVIHV AND TRANSMITTAL KH,. ARMY LOTi SROJICT NAMIi Ul lATCHUi IROJICT NUMIIRi Oftti Inlttilf Camm^mf 1, Omit) Usdtr (Amy litcft exploit-All Ul ' litttMi Crauptd In Amy lucn 1, Data SyitM Cwrdlnsur (MAMOC, Ul fttport) 1, Cms kaMsr Rtvltw ind Appravsl *, ClMflM SuatrvlKr Rsvliw snd Appnvil • • 1, Dm Syilm CMrdlnsior (Camciid Ul Rtport/ MMSQC USATHAMA Riportl 1, C,h*Mlol S'upn-vlsar Apprtvil j ?, O.A Suptrvlsar (Ul Riport, USATHAMA Rtport, MARSQC) 1, Oi» Syitm Caordlnnor Rrrlm Md f\l» t. TnnMrillil (0 Army (WTC) Noiti fiiu My M rnuita 10 mt us fn\Ki Minifir is orniminifv om IUBIK; ta ftvlilon trt^f th« ftvttm at th* OA Suotrvlioi* Irt SttST^^^ COMMINTS. |M|| ' ' ' SOURCE: Ut, 1113. Figure 6.1-1 AR30IU&I ARMY DATA REVIEW FORM ENVIRONMENTAL SCIENCE (Reduced) AND ENGINEERING, INC. | A-4 9 ORIGIN \ (Rf «•!, QA.l/QAPLAN/6.2 09/20/84 figure; (4) the estimated concentration is annotated as based on the reference compound; and (5) the estimated concentration is reported as the concentration in the original matrix assuming 10U percent recovery. Results of the semiquantitative analyses will be entered into the Data Management System of USATHAMA, as outlined in the lit Data Management User's Guide (USATHAMA, 1981) with the following conditions: 1. Four characters (3 digits plus a decimal) to represent the slope of the least squares regression line of 'found-versus- target concentration values for QC standard additions data in spiked standard or natural samples obtained on the date of analysis will be entered in the "Accuracy" columns. 2, For semiquantitative analyses in which estimates are based on a reference compound, the 3 digits for accuracy will be "000." 3, The precision of semiquantitative analysis will be reported as "999." on data management entries. 6.2 QUANTITATIVE ANALYSES Estimates of concentration levels in quality control and actual samples will be reported to USATHAMA accprding to the guidance as outlined in the program tasking and the Data Management Users Guide. Reported values will be corrected for recoveries and moisture over the total analytical method to offer the best estimate of the actual concentration in the original matrix. Values less than the average detection limit will be reported as "less than" the detection limit. Conversely, detection limits higher than the average detection limit (as in the case of a sample with high background levels) will be reported as "less than" the higher detection limit. The slope of the best-fit linear regression line of found-versus-target concentration values from control spike data in standard samples obtained from the method certification will be reported as the accuracy. AR30I062 A-50 QA.l/QAPLAN/b.3 09/20/84 '*s*^ The standard error of the best-fit linear regression line of found-versui-target concentration valuei from control spike data in itandard simples obtsined during method certification will be reported as the precision of the measurements for that day. '" , The documented detection limit will be used to report data for the quantitative method. 0 o AR3QI063 A-51 f. Qh.l/QAPLAN/alB.l U9/20/U4 BIBLIOGRAPHY American Society for Testing snd Materials (ASTM). 1981. Laboratory Determination of Water (Moisture) Content for Soil/Rock/Soil- Aggregate Mixtures (D2216-71). In: Annual Book of ASTM Standards; Part 19, Natural Bedding Stones; Soil and Rock; Peats, Mosses, and Humus. Philadelphia, Pa. U.S. Army Toxic and Hazardous Materials Agency (USATHAMA). 1981. • Installation Restoration (IR) Data Management User's Guide, Volume 1, General Procedures, Edgewood, Md, U.S. Environmental Protection Agency (EPA), 1979, Guidelines Establishing Test Procedures for the Analysis of Pollutants; Proposed Regulations; Correction. Federal Regiiter 44(244):75050-75052, AR30I061* A-52 APPENDIX B DATA MANAGEMENT PLAN o o AR30I06" '"5 : D-ECSWVOW.l/APPB-TOC.l TABLE OF CONTENTS Section Page 3.0 DATA MANAGEMENT PLAN B-l 3.1 PLAN SUMMARY B-l 3.2 SYSTEM DESCRIPTION B-4 3.2.1 REQUIREMENTS PRIOR TO SAMPLE COLLECTION B-4 3.2.2 FIELD ACTIVITIES AND REQUIREMENTS B-8 3.2,3 FIELD NOTEBOOKS ' B-9 3.2.4 SAMPLE LOCATION COORDINATES B-10 3.2.5 REQUIREMENTS PRIOR TO SAMPLE ANALYSIS B-10 3.2.6 SAMPLE IDENTIFICATION NUMBERS B-U 3.2.7 REQUIREMENTS FOR SAMPLE ANALYSIS AND DATA INTERPRETATION B-l2 3.3 INTERLOCKING ESE AND USATHAHA DATA BASE MANAGEMENT SYSTEMS B-l3 3.3.1 DATA FORMATTING B-13 3.3.2 DATA TRANSMISSION B-16 3.3.3 DATA FILE STATUS TRACKING B-16 3.4 USATHAMA DATA BASE MANAGEMENT SYSTEM OPERATION B-16 3.4.1 DATA-FILE-LEVEL STATUS CONTROL B-18 3.4.2 DATA FILES B-19 3.4.3 LOGGING OF TRANSMISSIONS B-20 AR30I066 .m B-i _ ECSVHFS. 2/HANPLAN/DAM, 1 C\ 12/13/83 3. 0 DATA MANAGEMENT P! AN 3.1 PLAN SUMMARY Thia docuaant deicribis the Data Hanaganent Plan that will be used for Contract DAAK11-83-D-0007 per formed for USATHAMA by ESE. As specified in the contract, all data, will be presented to USATHAMA in final form for entry into the IR-DMS Univac 1100/61. USATHAMA has provided' a Tektronix 4051 System and IR Data Management Uier'i Guide (USATHAMA, 1981) to ESE {or this purpose. Thia plan describes the integration of the ESE and IR-DMS syitaas, an overview of which ii praiented in Fig, 3, 1-1, snd the data acquisition and control activities associated with, sample collection, laboratory , analysis, QC, and data reduction, The way in which quantitative and leniquantitative data will be handled in thii turvey ii ihown in more detail in Fig, 3, 1-2. Automated data handling at ESE facilitatea the coordination of the laboratory and field portiona of a lurvey and monitoring for QC, Holding tinei are readily nonitored, the atatui of analyses ii conitantly updated, and analytical results ire automatically checked againit preprogrammed QC criteria, All of thii information ii available aa computer printouts and remaini permanently itored for reference. Data will be validated by checking the accuracy of analytical raiulti and transcription, The plan deicribei each of the atepi required to control the flow of data from field trip preparation, eanple collection, and field note recording through data reduction, validation, and aiienbly in the required format for itonge in IR-DMS, Thii plan includei: 1, Data logging and chain-of-cuitody recording procedurei luch ai: a, Field notebook requirement!, b. Sanpl. labeling procedure,, AR 30 I 067 3-1 ESE Pra-Fiald Setup . 1 Field Data and Saopls Collection ESE Data HanagsMnt And Quality Control ___iyitii___ Laboratory Data Bate DSATHAKA Methods Irenefer to IR-DMS Dociaantition And Validate Data Ban SOURCE; ESE, 1119. ENVIRONMENTAL CONTAMINATION SURVEY Figure 3.1-1 Vlnt Hill Farms Station OVERVIEW OF THE DATA MANAGEMENT Warrantor!, Virginia PUN U.S. Army Toxic and HKM Abtrdun Proving QrourtdT B-2 \lfted) rnruu mvr i/li/u n uii•M UflMlln util mi fcilir In* UKIII ntMnu BUT IfltMIlM Ml M IM • MllfluilM il tfrlril » Snm IMMII • Umltr nmt *uiM Itoii • MiiliMUi a «r un IAUWUM n , QA IB?IXVIHI uqnn mma.a "mrtuuin* rut SOURCE! ESE, 1963. ENVIRONMENTAL CONTAMINATION SURVEY Figure 3.1-2 Vlnt Hill Farms Station OVERVIEW OF THE DATA MANAGEMENT Werrenton, Virginia PROCEDURES FOR USATHAMA ANALYSES y s Toxic and Hazardous O Abtrdein Proving Ground; Maryland B-3 ECSVHFS.2/MAHPLAN/DAM.2 10/28/83 c, Sample tranimittal formi, and d, Analysis report forni. 2. Detaili of the procedurei for interfacing ESE computerised QC data handling methodi with IR-DMS, 3. Data coding and tape generation procedurei. Thii format will conform to requireaenti ipscifiid in the IR Data Management Uiar'i Guide (USATHAMA, 1981). 4. Procedurei for tranifir of data from ESE to USATHAMA. Before being lent to USATHAMA, data muit paei the QC checka in the ESE data ayitea and be reviewed by the appropriate diecipline manager. Once thii review it complete, the data will be traneferred to the USATHAMA data lyittm using the Tektronix ai an intermediary between ESE'e Prine computer and USATHAMA'a Univac computer. The data will firit be traniferred from the Prime to the Tektronix and itored on tape. The data will then be tranemitted from the Tektronix to the Univac via a long-diitance telephone connection. In the event of equipment failure, a 9-track magnetic tape will be tent to USATHAMA. A procedure will be developed for reporting data weekly without duplicating previous data traniminioni. The data will originally be loaded in ai Level 1 data. The data will be checked by the' Data Management Sub project Manager uiing USATHAMA' s data checking program. If the data pan thii check, they will be upgraded to invalidated Level 2 files. The ESE QA Superviior will perform e dita validation check at appropriate interval!, ind if the data pan, they will be upgraded to validated Level 2 files. 3.2 SYSTEM DESCRIPTION 3.2.1 REQUIREMENTS PRIOR TO SAMPLE COLLECTION The Site Geologist ii responsible for organising field efforti. At the outlet of the project, a New Project Setup (NFS) form ii completed by the Subproject Minager or deiignatad itaff member and entered into the ESE computer by the Data Management Supervisor. AR30I070 "•Q B-4 ECSVHFS.2/MANPLAN/DAM.3 n 10/28/83 '••"' Prior to eech field trip, a Pre-Field Setup (PFS) form ie completed by the Site Geologiet. Information requirenente for the PFS form are: 1. A liat of eample i tit ion ducripton, 2. A lilt of fractioni to be collected at tech itat ion, 3. A lilt of parametere [by Storage and Retrieval (8TORET) number! ,, required, and 4. A field eampling plan, The information from the PFS form ii entered in the computer by the Data Management Supervisor. Entry of the PFS form results in the following events; 1. Sample numbers ere sssigned to stations. 2. Sample labels (Fig. 3.2-0 are printed for each fraction to be collected, 3. A logsheet (Fig. 3.2-2) which detiili the fractioni and preeervation requirements is printed. Use of the computer eliminates transcription errors between sample numbers on i labels and on the logsheet, The Data Management Supervisor sends the logsheet and sample libels to the Site Geologist. A field sampling plan ia included as part of the PFS and is distributed to the Fiild Team, Analytical Croup Leaders, and Laboratory Data Aaiiitant. The following information ia'required in the field sampling plan: 1. Project organisation; 2, Deperture and return detei; 3. Lodging accommodationi and telephone numbers; 4. Sample collection plan and sample return echedule; and 5. Liet of parameters with short holding times. BR30I07I B-5 l«r»f1,TMI41) VINT HIM, r»f!nr STATION 3 Vl-tFKW s«Nn.t« DATC rr.it HI C(INn a'/IH T ittu FARM STATIOVMITDN W IANPUH Dare TIM PN CPNH '/INT IIKI, r«l!NS (ITHT70N rXfl,0(l Mnri.c9 n pan V»Mr-Dn«tW PN COND VINT NIII. r«nnn ITATION i»nri,f3 R par, e VHPOnuUt PN COM VINT HIM, r*mif! DTATinN f.xruon e«Npi,3 H HATWHFD: rj«Wr PH CONO '/INT H;I.|, MMir 1T»TtCN PDTC TINC COND VINT Mill. r»Mn ST«n(lH ItXPl.O* •JHFDU IDNPLCP. OUT! rtflC PN COND "C VINT HIM FORBf BTATIOH (TXfl.OK n»Tt rtnc PH COND , VINT HILL rnKiia DTATION i -M IANPI.M n«rcUHFD rtnUc PN COND VINT NII.L FARM KTATION UHPTIU 3HNPI.IP. . PATC TTNt KH COND VINT MILL ruitnn ! 3-6 o [1 *• •• *-0 0 «»! *•* 8' SI ei» i I I»O | •SI6SISS o 'i o i fr n t tr o ECSVHFS. 2/MANPLAN/DAM.4 12/14/83 Each field group which ii lit up on the eystem includei the following data entriae to facilitate converting data into the IR-DMS format; ESE and EPA* 8TORET Niabiri ______.'aranetarit_____ 99759 Site Type 99738 Saapla Depth (cm) 72005 Sampling Technique 99598 Extraction Date, Julian (GC/MS, GC) . • * EPA • U,S, Environaental Protection Agency, t ca • cantiaetan, CC • gee chromatography, Amy lot aaeignaenti by iimplei end anelyies determined by the QA Superviior ere entered into the computer at thii time, 3. 2. 2 FIELD ACTIVITIES AND REQUIREMENTS During sample collection, field notee will be taken in a waterproof notebook, ai described in Sec, 3,3, The field notes will include ell of the information neceesary for later input into computer records, ss specified in the USATHAMA IR-DMS. All sauplea collected will be immediately preserved, ind the varioui frictioni of a temple will be identified by an alphabetic luffix ippended to the sample mnber, A few example! include: UP~Chilled Peiticide N—Acidified with Nitric Acid V—Volatile Organic! Before shipping to the ESE laboratory, the Site Geologist will fill out a logsheet to include information on date and time of lample^collection end a liat of eamplei being ihipped, Sample fractions which do not require immediate analyiii are normally returned with the Field Team. The Site Geologist is responsible for AR30I07I* 3-8 ECSVHFS.2/MANPLAH/DAM.5 O\ 10/28/83 eniuring chat correct collection, preiervation, and shipping procedures are followed. The labels shown in Fig. 3.2-1 will be und at all times to reduce the ponibility of erroneoue inilyiii of improper eaaple fractioni. *, The required method of ihipaent ii a function of the holding times of the conetituenta being analysed. For inetance, if e particular fraction ie to be analysed for a parameter with a holding time of 12 houri, the eeaple must be ehipped 10 thet it will arrive at the laboratory and be analysed within 12 houri of the time of aemple collection. Other frectiona of that aama tanpli may be ehipped either later or by slower transportation, if permitted by holding tiaia, 3.2.3 FIELD NOTEBOOKS The field notebook, as the permenent record of all field activities, J must be both accurate and complete. The notebook! for thii project will be permanently bound with waterproof iheete, All field notei will be delivered to USATHAMA at the end of the contract. To increaie the poeiibility of recovery if a field notebook ii loit, the following itattoenti will appear on the firit pegs following the title pegs: If found, pi me return to: ENVIRONMENTAL SCIENCE AND ENGINEERING, INC. P.O. Box ESE Gaineiville, Florida 32602 (904) 372-3318 • A Reward Will Be Offered At the concluaion of each day in the field, the Field Teen Leader will review each page of the notebook for errori end omissions snd will date and eign each reviewed page. After reviewing the field notebooke, the Site Geologist or an assistant will transfer the field notes into the ...», appropriate data input notebook, Alternatively, the Site.C»f>k>p|istnOi} c B-9 EC8VHFS.2/HANPLAN/DAM.6 10/28/83 en aeeietant could fill out the data input notebooks while in the field, if hi/she is familiar with the codes for dsta entriee. This formet ellowe direct input of the data into the Tektrorix for conetructing a data tape, The field notebook! will alio contein ell field initrunint cclibretioni for later verification of field data. Recording of the field inetrument calibrations will permit detection of adverse trende 10 that corrective actions can be taken. 3.2.4 SAMPLE LOCATION COORDINATES Sempling sites will be located and recorded on the appropriate input form, A local grid coordinate eystem will be eet up et eech eite. If e euiteble benchmsrk ii available, thin coordinetee will be converted, and each templing location will be identified ueing the Univerial Traniveree Mercator or State Planar coordinate eyetem. 3.2.5 REQUIREMENTS PRIOR TO SAMPLE ANALYSIS Samplee will be received by the Laboratory Coordinator deiignated by the Chemical Analyses Superviior. TJie Laboritory Coordinator checks in the eamplae and verifiee the couplet anesi of the logeheet. If eny problems exiit, the Field Teea ie immediately notified. The Laboratory Coordinator muet than: 1. Obtain control eamplei from the QA Superviior, 2. Notify the Analytical Coordinators thai; eemplei have arrived, 3. Eneure thet the lamplee are properly etored, and' 4, Send the completed logiheet to the Data Manegement Superviior, The information from the logiheet ie then entered into the computer to ectivau the parameter lilt for the lamplei collected and received -by the laboratory. Thii operation ii called a Poet-Field Entry (PFE). Upon input of the PFE, the computer identifiei the par mat en that have leea than 3-day holding timee. A notice of eemple arrival and ehort holding times ii then immediitely tent to the Analytical GrouAR30I07p Leadera,6 -• '• Q B-10 (~\ • ECSVHFS.2/MAHPLAN/DAM.7 •••„;•' 10/28/83 Army lot eeeignaent notices are eleo lent et thii time. Each notice containi: 1. Army lot deeignetion; 2. Anelyais(ee) in this lot; 3. QC simples, typei, and amounts required; " 4. Sample maber, eite identificetion (ID), installation, sample type, end dete of collection for each eample; and 5. Extraction time limit (if sppliceble). In addition to eliminating tranicription errors, thii Any lot notice form provide! the correct mnber of ipike and replicete eemplee to be analysed, 3.2.6 SAMPLE IDENTIFICATION NUMBERS ESE ueci a batch method for analysing, checking QC, and calculating j ~^ final reeulte of eaaplee. Prior to analysing a batch of lamplei, the enalyat will be aieigned a specified group of lamplee by the computer, end the esmplt-pareaeter ititui will be updated to "IL" (in laboratory). The beaii for thii grouping technique ii that date are analyzed in group! of samples for the came parameter(i) with the seme stsndard curved) and QC checki. The analytical batch ie eiiigned a unique batch control nixnber, which ii itorid with all final data, eo data can be checked by referring to the originel reeulti, The bitch control number will be ueed in the USATHAMA projecti to assign the three-cherecter alphabetical prefix to the USATHAMA lample number 10 that there will be a one-to-one corralit ion between batch number and alphabetical prefix. Each eample in the batch will then be migned a numerical euffix, itarting with 001, to the three-character alphabetical prefix, The leboratory betchei will be aide project-specific 10 chat only USATHAMA lamplee will be included in eny betchei thet contein USATHAMA saoplis, Uiing thii icheme, there will be en indirect relationahip between ESE'i unique lample number and the USATHAMA sample number (i.e., data for ESE O Sample No. 71200 could be reported ei AAA001, AAR004, and {f#>$(>) M)77 3-11 ,. ECSVHFS.2/MANPLAN/DAM.8 10/28/83 x*. AAA002 lample could not be reported for ESE Sample No, 71200, if the >above conditions exist), 3.2.7 REQUIREMENTS FOR SAMPLE ANALYSIS AND DATA INTERPRETATION The analyiie of each laboratory batch ueually coniists of a nlti-itige proceee, In the firet etage, inetrument calibration, the ESE data management eyetem includei eeveral QC checka. The linear regreeeion equation and correlation coefficient are calculated from the cilibrition curve data, and the correlation coefficient ie teeted to determine whether it ie within en acceptable range epecific to the pirniter, In addition, the conatancy of the calibration response ie checked by compering preanalysis and poetenelyeie itandard riipoi.se and/or response tec tori. Eech Army lot will include et leeet three control eamplee ipiked into e etandard or natural matrix. When the Army lot analyeii ii complete, a lineer regreeeion line of found-vereue-terget concentretion ie calculated. The elope of thia line ie the accuracy of the lot, The ESE Dete Management Program comparea thii accuracy with the accuracy obtained during certification to determine if it ie within the control limite. For quantitative analyeee, the etandard error of the regreeiion line on the date of analyeie it uied to calculate the precieion for that lot. The preciiion will be compared to certification to eee if it ii within 3 itandard devietion uniti. If the deta fail the QC chacke, appropriate actione (such ee reanalyzing the eamplei or correcting transcription or data reduction errore) are taken. When the data pass, the finel deta are etored in a computer data file, along with a lot control ninber end e etetue of the final concentration (i.e., >, <, etc,), Analyiti uie the computer to reeerve lamplee for anelyiii end to interactively check celibretion curvee and QC reeulte. By illowing thi analyit to enter directly and check QC and sample data. MOMikiit|k -i a notificetion to the analyst of QC problem! reiulti, so that any -'- • ("T B-12 ECSVHFS. 2/MANPLAN/DAM. 9 12/14/83 /-> ,,,,' necaisary corrective action can be taken before more analyiei are completed. Laboratory anelyete are not permitted to update senple ricorde, Whan the enalyet has entered the QC end eample data, the Army lot, including workiheeti end any other pertinei I documentetion, ii turned in to tha Data Management Superviior. The computer ie uied to re tone t the data in both USATHAMA format and itandard ESE report format " for preliminary review. These printout!, along with the deta package from the laboratory analyet, are attached to the Army data transmittal fora (Fig, 3,2-3) for approval by appropriate coordinatore and the QA Suparvieor. Than the file ie tranimittid to a Level 1'file in IR-DMS, either by telephone using the Tetronix 4051 or by mailing a 9-track magnetic tape to USATHAMA. The program for generating the final report hat the capability of organizing the STORET nunberi and tempie number! in any icquance speci- fied. An example of the report format ie preeented in Fig, 3,2-4, 3.3 INTERLOCKING ESE AND USATHAMA DATA BASE MANAGEMENT SYSTEMS • 3. 3.1 DATA FORMATTING \ ^j All of the QC check! and data minipulitione deicribed in the preceding lection ere performed on ESE'i Prime 750 computer eyetem, The data bate for thii lyitem uiei a keyed-index icceii technique, with a highly organized let of internel file pointers, The lyvtem hai been modified to contain information apecific to converting data from ESE'a data bate to USATHAMA format. Filee have been organized on the ayitem to contain information luch ai converiioni between STORET numbers ind USATHAMA abbreviationi, ai well ei method! documentation data, When all of the data have been entered into the eyatem for a particular let of data, a program ia run to acceii all of the pertinent data baiei for reformatting into USATHAMA format and to itore the reformatted data in the chemical aampling and analysis data file, The Prime 750/IR-DMS interface will be adapted to future chinges in USATHAMA formatting, ,ae applicable, Theie changee are periodically announced via mailings or updatii to the IR Data Management User's Guide ind modified eoftware tepee, The remaining date entries, luch 11 the field drilling fil file, will be entered from forms filled out by the Field Team" O B-13 s>A«^^.«NCH**3.^.P^*c *• ARMY DATA RIVIEW AND TRANSMITTAL FORM ® ARMY LOTi PROJICT NAMI: III BATCHES i PROJECT NUMBER: Out Inlllili ComiMflts I.. Croup laidir (Army ailcft Cmpltli-AII ISI •atthei Creupod In Aney Inch 2, Oita SyitM Coordlnitor (MARSgc, ISI Riport) 1, Croup Uidir Rivliw ind Approvil . «, Chmfcal Suptrvfior Rovltw ind Approvil 1. Dm lyiltm Coordinator (Corrielod ISI Riport/ MARSQC USATHAMA Riport) 1, ChMteil Supervisor Approvil 7, OA Supirvlwr (HE Riport, /. USATHAMA Report, MARSQC) \ , 1, Dm Syittm Coordlniior R«vl«» ind Fill 1, TrtfliMltUI to Army (WTC) Mom Bill My bt rilMitfl to (hi ESE ProlKi Minigir is priiiminiry Oils luOjKt to rtvlilofl tfttr th« ftvttm of tha OA Supvrvtiop tn Sup 7. COMMENTS i • . SOURCE: ESE, 1113. ENVIRONMENTAL CONTAMINATION SURVEY Flgurt 3.2-3 Vlnt Hill Farms Station ARMY DATA REVIEW FORM Warrenton, Vlijiglaj n 1 n R 0 (Raduced) U.S. Army Toxic and Hazardous Matarlals Agancy Abardaan Proving Ground, Maryland B-14 o |i ( S • I ' • * • 2 i 3 • 2 2 ; 2 n H i ' :s 3 i s s « . B .. r, g . . , j 5 7 , • s * * - • • s s»5555 53! • s s • ' f!§i l-f Hi!i o :: s : S 3 !f2!;3g u. N »*»§"^O 1 1 ; aI :! 5 si *1 i1^' u2 •«« «.ij..ii ; : s : : 5 s : M S S ! * S S • I s IS I J 5S s s S s O ,______ B-15 ECSVHFS.2/MANPLAN/DAM,10 10/28/83 3.3.2 DATA TRANSMISSION ESE haa developed a direct interfece between ttvi Tektronix 4051 and ESE'e Prime 710, tiling thii interface, data fi ie on the Prime 790 cen be treneferred to the Tektronix 4051 and eent by telephone to USATHAMA, 3.3.3 DATA FILE STATUS TRACKING A program hae been developed at ESE to track data filei at varioui itifti of development end to keep all project participant! epprieed of data file itatue (Fig. 3,3-1). The program indicatee when files sre eent to USATHAMA, when they ere loeded to Level 1 and Level 2, when the appropriate data-checking routine ie peeeed (if applicable), end when filee are validated. A copy of the file etetue for an entire project will ba included with the Monthly Technicel Stitui Riport. 3.4 USATHAMA DATA BASE MANAGEMENT SYSTEM OF OPERATION The IR Data Management Uier'i Guide (USATHAMA, 1981) furniehed by the Data Kenagement Staff of the Central Proem ing Site, Aberdeen, Md,, providee the formatting requirement! and field codei, ee well ae e lieting of the. loftware and hardware available to eccen the USATHAMA IR-DMS, In thii ayateo, field liboritoriii uee Tektronix 4051 System to liet end prepare validated data reaulting from environmentel lurveye, Ae shown in Fig, 3,1-1, IR-DMS receives data from the ESE dete handling system. The data have passed the required QC criteria, The IR Data Management User'e Guide (USATHAMA, 1981) epecifiei formatting for the poeeible data antriei. A combination of program! developed by USATHAMA for the Tektronix 4051 and ESE for the Prime 790 will be ueed.for entering, checking, and formatting data into IR-DMS/ According to the contract apicificationa, data will be trenimitted to USATHAMA weekly, Deta entering IR-DMS are input to the tint level of a three-level eyitem. AR 30 I 082 B-16 8 *»l£ lillfiilifhis- ssslfilifllSSss d; Si iiiiiiliihiiii Ii S ? I Ills aaaaaaaaasssaSa • z' =as355S55||5SBs ^ "Sis* [IB f 5: |S« i o!£ Ig; B-17 0 ECSVHFS, 2/MANPUN/DAM. 11 10/28/83 3.4,1 DATA-FILE-LEVEL STATUS CONTROL 1 The levele epproech hei been adopted by USATHAMA to clarify the etatue of deta filei. A Level 1 file ie considered to he eny data file that: (1) containi unvalidated date, (2) ii not atructured according to thi foraate outlinid in thii document, or (3) ie a ecratch file thet a user might have. Level 1 filee are the eole rieponsibility of the originating ueer end will be processed iamediately after verification of accurate tranraiiiion of the data to the UNIVAC. The Level 1 files will be deleted ae aoon ai the data ere elevated to Level 2, A meximum of 30 calendar day! ii allowed before the Level 1 deta file ie automatically deleted from etorage by USATHAMA, in accordance with the new IR-DMS policy of Sept. 9, 1983. All chemical data filei ere proceeied through USATHAMA '• chemical data checking program, Thii program checke for file format and content end rejecti eny data not meeting all requirements. Rejected dete are corrected and, if necenary, riviiwed by the QA Supervieor end the Data Managenent Coordinator and then rechecked by the date-checking routine, When the filei pen the data check, they will be upgraded to Level 2 by the ESE Dete Management Coordinator. All filee produced ai a result of the USATHAMA data-checking routine! will be deleted ee loon ei the deta they contain have been tranif erred to Level 2. Level 2 filei are itructured according to the format i outlined in the T_ Data Management Uaer'e Guide (USATHAMA, 1981). .Recorda containid in Level 2 filei may be acceeaed in e read-only mode by any user. After validation by the QA Superviior, the ESE Deta Management Coordinator notifiei USATHAMA that the unvelidatad flag may be renovid from the Level 2 filei, A Level 3 file will be i Data Bate Management System loided from Level 2 filei thit have been validated. ARSOIOSu. B-1B ICSVHFS.2/MANPLAN/DAM.12 ^ 10/28/83 3.4.2 DATA FILES Three typei of deta filei are generated by FieM Team activitiae; (1) the map file, (2) the field drilling file, ,i".d (3) the ground water stabilised file, In eddition, certain field sampling; information must be collected and entered into the chemical data filea, »* » Map File The map file ie a listing of sample eitee and corresponding north -and eeet coordinatee. There may be more than one nap file for each initillition. The well eitee ere itirveyed, and the coordinatei are lubnitted by the Site Geologiet to the Deta Management Coordinator, who createe the well map file, Before lampling ii initiated, the lurface water, aediment, end eoil eemple lite coordinitee are ueuelly eetabliihid end entered into another nip file, A computer printout of the file ii checked and corrected by the Site Geoloiiit, The data are • submitted to USATHAMA in Level 1 end lubiequently validated by ESE'e QA "~~> Superviior, according to Military Standard (MIL-STD) 105D. Once validated, thii map file ii elevated to Level 2. This mutt take place before any other data ii processed. Field Drilling File The week after well drilling ii completed, the Site Geologist enteri field drilling data on USATKAMA'a IR-DMS forms and subniti then to the Data Management Coordinator, The information ii entered into the data management lyitem, ind e computer printout ii generated and returned to the ESE Site Geologist for proofing. Corrections are noted on the eheet, end the sheet is returned to the Data Management Coordinator. After correction! have been made, the deta are lubnitted to USATHAMA and loaded onto the USATHAMA deta ayatem in Level 1, Once the field ' ' drilling file is submitted to USATHAMA in Level 1, the data are checked with USATHAMA1s CEOTEST program, which checks for correspondence between sitee in the map and field drilling files, accurate entry of deta, and completeneis in the field drilling file, Errore ere printed out for o correction in the Level 1 file. Vi lid a tion takee pi ice B-19 ECSVHFS.2/MANPLAN/DAM.13 10/28/83 run error-free. After the ESE QA Supervisor his validated the field drilling and wall map file, the deta am elevatod to Level 2. Stabilised Ground Hater File The ground weter atabilised file ie a compilation of etatic water levele in the welle at the timi of lanpling. It ie submitted by the ESE Site Geologiet eftar the lanpling trip, along with the map file information. The ground water itibilind file ie eubmitted on IR-DMS forme end 'under- gon the eeme entry, checking, and validation procedurei ei the field drilling file, including checking with the GEOTEST program. Chemical Analyeie File Field data which will be incorporated into chemical filee ere eubmitted within 10 dayi of sampling, This information includee sampling date, technique end depth, eite end initillation abbreviatione, and aample type. It ie eubmitted to the Date Management Coordinator and ii |,<|jf|:; verified in the deta management eyetem, 3.4.3 LOGGING OF TRANSMISSIONS All attenpti by the ESE Data Management Coordinator to tranimit or manipulate data in the IR-DMS will be documented in a logbook at ESE, This log will contain; 1. Date of attempt, 2. Name of perion making the call, • 3. Initillation name, 4. Work performed, and S. Problem! encountered. AR30I086 B-20 o APPENDIX C ESE ANALYTICAL LABORATORY SAFETY PLAN AR30I067 O CHEMISTRY DEPARTMENT IAS SAFETY MANUAL Fripared By; ENVIRONMENTAL SCIENCE AND ENGINEERING, INC, Gaineiville, Florida April 1984 AR30I088 C-l o 04/09/14 APPROVALS Thii latity plan hai been reid ind undiritood and ii approvad for un in thi Chetiitrjr laboratoriii, 4/09/84 Chimiitry Diviiion Minigir ' Dati /~*\ i £L+L..urnri^r 4.>, /flt«(At~______^_____4/09/8A- EH Sifity Minagir Dati AR30I089 O C-2 D-CH84.1/8M-TOC.1 08/13/84 ENVIRONMENTAL SCIENCE AND ENGINEERING, INC. LABORATORY SAFETY MANUAL TABLE OF CONTENTS FOREWORD 1.0 RESPONSIBILITY FOR LABORATORY SAFETY 2.0 ACCIDENT REPORTING AND INVESTIGATION 3.0 GENERAL LABORATORY SAFETY 3,1 PERSONAL PRACTICES 3,2 lOUiEUEPING 3.3 1ATERIAL HANDLING AND STORAGE 3.3.1 HANDLING 3.3.2 STORAGE 3.3,2,1 Solventi 3.3.2.2 Acids and Bam 3.3.2,3 Compreiied Cans 3,3,2,4 Corrosive Matimli 3.3.2.5 Miaeellaneoui Storage Procedures 3.4 SPILLS AHD LEAKS' 3.4.1 BASIC SPILL PROCEDURES 3.4.2 HANDLING OF SPILLED LIQUIDS 3.4.3 HANDLING OF SPILLED SOLIDS 3.4.4 MERCURY SPILLS 3.4.9 LEAKING GAS CYLINDERS 3.9 HASTE DISPOSAL 3.9,1 SOLID HASTES 3.9.2 LIQUID HASTES 3.9,3 HASTE SOLVENTS 3.9.4 MISCELLANEOUS DISPOSAL PROCEDURES AR30I09• 0 C-3 D-CH84.1/SM-TOC.2 08/13/84 TABLE OF CONTENTS (Continued, Pege 2 of 3) Section '- 3,6 LABORATORY EQUIPMENT 3,6,1 GENERAL EQUIPMENT 3.6.2 GLASSRARE 3.7 SAFE LABORATORY PROCEDURES 3,7.1 PROCEDURES WITH GLASSWARE 3,7.2 DSE OF EVACUATED GLASSWARE 3,7.3 SAFE PROCEDURES WITH CHEMICALS 3.7.3.1 General Chamicali 3.7.3,2 Aclda 3.7.3,3 Bain 3.7.3.4 Volatili ind Flamable Matariali 3.7.3,3 Cain '~\ 3.7.4 MISCELLANEOUS SAFE PROCEDURES ^ 3.8 SAFETY EQUIPMENT 3.8.1 EMERGENCY EQUIPMENT 3.8.1,1 Fire Control Equipment 3,8.1,2 Other Emergency Equipment 3,8,2 PROTECTIVE EQUIPMENT 3,8,2,1 Parionil Protective Equipment 3.8.2,2 Other Protective Equipment 3,9 EMERGENCY PROCEDURES 3.9.1 FIRE OR EXPLOSION 3.9.2 CHEMICAL SPILLS 3,9.3 CHEMICAL INGESTION 3.9.4 FIRST AID 3.10 EMERGENCY PHONE NUMBERS 4.0 SPECIFIC CHEMICAL HAZARDS O AR30I09I C-4 D-CH84.1/SM-TOC.3 08/13/84 TABLE OF CONTENTS (Continued, Pige 3 of 3) Section 3.0 HAZARDOUS MATERIALS 9.1 GENERAL PROCEDURES 9.1.1 DETERMINATION OF HAZARDOUS MATERIALS 3.1.2 PERSONNEL 9.1.3 LABORATORY SAFETY PLANS 3.1.4 PERSONAL PROTECTION 3.1.3 SUSPECT SAMPLING HANDLING AND STORAGE 9.1.6 KNOWN CARCINOGEN SAMPLE HANDLING AND STORAGE 9.1.7 SPILLS AND LEAKS 9.1.8 HASTE DISPOSAL 9.2 SPECIFIC TYPES OF HAZARDOUS MATERIALS 9.2.1 CHEMICAL CARCINOGENS 9.2.2 RADIOACTIVE SUBSTANCES 9.2,2,1 Leboratory Procedurei 9,2,2,2 Storm and Hind ling" 9,2.2.3 Spilli 9.2,'2.4 Haite Diipoial 6,0 REFERENCES AR30I092 C-5 ; ! D-CH84.1/SM-LOT.1.1 04/09/84 LIST OF TABLES tibli 3-1 HCB Riagent • 9-1 Chiaicetl Carcioo|ini o o AR30I09" -•3 . C-6 D-CHB4.1/SM-F.1 4/02/84 FOREWORD The Chemistry Department laboratory Safety Menual ia intended ai a reference for both new end current employee!. The minual ihould be read and itudied by new employeei prior to eny laboratory work. Employeee ihould becoae familiar with iti .format 10 that neceeiary information can be quickly and eesily located. New employee! alio ihould become familiar with laboratory areai, They ehould know where eafety equipment ie loceted, where activitiei ihould bi completed, and where queetione can be anawered, Current employeei ihould riview regularly the procedurei in thii menuil. They ahould make eure that they ere working Mfely in the leboritory ind that the laboratory ii a eafe work place. Current employeei omit alio know lafe procedurei 10 that thiy are able to help teach new employees proper and lafe working methodi, Ho lafaty manual will eniure hiving i lafe leboratory. A liboritory ii only ai lafe n the people working therein make it. Thii minual will help lab perionnel take poiitive itepi in building i safe and accident- free liboritory, AR30I091| C-7 D-CU84.1/SM-1.1 O 4/09/84 1.0 RESPONSIBILITY FOR LABORATORY SAFETY Laboratory lafety ie everyone1! reeponiibility, It ii the job of all laboretory pereoanel to eifely complete lab ectivitiei not only to protect theuelvei but elio their co-workeri end laboratory equipment, Suparviiore and employee! muit work ee a team to develop a tafi laboratory. The tupirviior must!, 1. Eniure thet all employeei ire working in a lafe manner; 2. Periodically review laboratory aafety rulee with employeei; 3. Eneuri that each employee knowi the hitardi and pricautioni to be taken with e particular activity; 4. Eniure thet new employeei are properly oriented ai to general eafety, fire control, emergency equipment location, etc.; end 3. Enforce all safety rules ei eitabliihid by Environmental Science and Engineering, Inc. (ESE), Lab employees must; 1, Adhere to all tafity rules n iitablished by ESE; 2. Cooperate with lab lupetvisors and thiir initructioni; 3, Find out proper procedurei from the auperviior or provided riference miterial; 4. Be familiar with the hatirdi and pricautioni to be tiken with in nsigned ictivity; 9, Be alert to co-workeri and their activitiei. If co-workeri are working unnfely, inform them of the proper procedures ind report the incident to their supervisor; 6, Be familiar with emergency procedurei ind ivicuition routei; and 7. Report any hazirdi that ire observed. AR30I095 C-8 D-CH84.1/SM-2.1 4/09/84 2.0 ACCIDENT REPORTING AND INVESTIGATION Deepite teking preceutionary meaiuree, leboratory eccidenti may occur. The actione taken efter an accident are ei important ae the procedurei teken to privent en accident. The pott-accident procedurei will help prevent limilar iccidints in the future, Poet-eccident procedurei are ei followii • 1. Employeee ihould iawdietely report all accidente to'thiir euperrieor, no matter bow minor; 2. The eupervieor ihould immediately begin inveitigationi into the accident and take aeceiiary, immediete action; 3. The euperviior ihould fill out en accident report within 24 houri of the incident end submit it to the Chemistry Diviiion Meneger for review; 4. Once the ceun of the eccident ii determined, corrective meiiurei ihould be completed n loon 11 poiiible; and 9. Thi accident ehould be dieeuiiid with all amployeee n to why it happened end the way to prevent it from occurring egein, It is alio importint that inployiee report any hasardi that they obaerve while in the laboratory. A reported hatard ihould be corrected 11 toon ei poiiible to prevent injury to an employee or damage to laboratory equipment. AR30I096 C-9 _ D-CH84.1/SM-3.1 i ) 04/09/84 3.0 GENERAL LABORATORY SAFETY Thii lection coven lafa procedurei to which impli;eei ihould adhere during all laboratory activitin. Sifi procedure! for specific hasardi and activitin ari diicuned liter in thii lamial. All pereonnel working ia thi laboratory lust be knowledgeible of thin proeidurn ind precticei, 3.1 PERSONAL PRACTICES Personnel conduct ii a kiy to laboritory lafaty. All laboratory perionnel ihould conduct thimnlvn according to the bnic rules liitid below, 1, New work or new procedurei ire to be attempted only upon perminion ind init rue tion of a luparviior. 2. Mithodi ihould bi followed n outlined. Bifori undertaking an unfamiliar opiration, lairn the method of operation and the ,__ hnardi Involved, Location of any eafety equipment ihould bi ':) known, Pricautioni indicatid in analytical proeidurn ihould bi fully undiritood and appliid, 3, Stunt experiments are forbiddin. 4, Running ii not pirmitti'd, 9. Horsepliy ii not pirmittid, 6, Work while under the influinci of ilcohol, narcotics, or controlled tubitincei ii icrictly prohibited, 7, Eating, looking, or drinking in thi liboritory is prohibited, 8, Laboratory equipnint oay not be uaid 11 .contiiniri for eating or drinking, 9. Labontory mg'inti tuch is sodium chloride thill not bi uiid for food, AR30I097 C-10 D-CH84.1/SM-3.2 04/09/84 10, Suction by mouth (whin using pipits, etc,) ii prohibited, Rubber luction bulbi are to be uiad, 3.2 HOUSEKEEPING A clean and orderly laboratory helpi reduci the frequency of laboratory accidentii Eiployin ihould follow the guidilinii listed bilow to develop and maintain a clean, orderly, and iifi laboratory, 1, Aielee and wilkwayi shall be kept clean, dry, and free of obetructioni or tripping haiardi; 2, Fire extingulihen, lye wiihn, ihowiri, and other safety. equipment will be kept deer and accessible it all tlmn; 3, All itimi will be kept in their proper itongi plici whin not in uii; 4, All bench topi will be kept free of broken glinwiri, spilled chemicili, piper, iquipaint not .in uie, etc.; 3. All equipment end working lurficei ihill bi cleined frequently to privint iccumulition of duit ind dirt; 6. All drivers ind cibiniti will be kipt doted whin not in UHJ T. All rngenti will bi itored in ippropriite ind properly nirkid contiinsri in deiignitid storage irns (in "Mitiriil Kindling and Storige"); and 8, Electrical cordi ouit bi kipt from dangling in thi laboratory aiilii, 3.3 MATERIAL HANDLING AND STORAGE Thi propir hindling ind itorigi of laboratory oitiriils ii crucial in protecting liboritory pirionnil. Improper hindling ind itoriga cm liid to fin, explosion, burnt, toxic vapor ixpoiure, and other dangeroui lituationi, Thii nction coviri gineril handling and itorigi of materiali. Further detaili for ipecific mitiriili can be found latir in thii manual. AR30I098 C-ll o-,: ' D-CHB4.1/SM-3.3 04/09/84 3,3.1 HANDLING 1. All material! lhall bi properly labeled) labeling ihould include meterial, concentration, date of preparation, preparir and recipe uied; 2. All eolventi, acidi, and baiei shall be carried in protective bucket! when in quintitin of 1 gallon or mori; 3. Heavy loada lhall not be lifted without adequate aeiistanci;. 4. Food or biverege containiri lhall not bi und to itore samples or other toxic matiriali; and 3. Whin flammable liquidi ira being trmifirnd from oni ntal container to another, both containiri lhall bi electrically grounded, J.3.2 STORAGE 3.3.2,1 Solvent! 1, Solvinti ihill not be itored in thi liboritory ixcept in thi i l amounts for iamidiite use; •i"*****' 2, Aftir uie, solvent jug eipi ihould bi riplicid tightly, and the jug returned to thi fireproof cibineti outiidi thi building; 3, Large quantitiai of lolvinti iri itond in a iiparati building whili imall quintitin iri kipt in thi fireproof cibinits for immediati use; ind 4. Fliomabli matiriils ihould be stored In fireproof, properly marked container! in well-vintilitid irias, 3.3.2.2 Aeidi and Bun 1. Acidi ind bun ihill bi itorid iiparatily. 2. Acidi ind bun ibove 2N ihill bi itored in npiriti leid or plntic triyi idiquiti to contain thi liquid \t bmkage or ipillige occur. Diluti icidi in quantitin leu thin 1 liter may be kept on the reagint ihelf, but ccncintntid icidi ihould be kept in the leid tny under thi link. AR30I099 G C-12 D-CH84.1/SM-3.4 04/09/84 3.3,2,3 Comnraiiad Cam 1. Compreeied gaeei ihould be itorid end uied only in well- vent iletad areai. 2. Cylindere of gun muet be eupported and tecured to prevent rolling or toppling over and ehould be pieced away from heat and open flaw. 3. Cylindere ehould be lebeled and grouped by type. 4. Empty end full cylindere ehould be etored eeperately, " 3. When not in uee, the cylinder muet be capped if a reguletor ii , not initallid. 6. Oxygen ihould be stored eeparately from flimmable or combuitible niteriali. 3,3.2,4 Corroiiva Miteriali >' v 1. Strongly corroiive liquidi lhall be handled only in areai where emple weter ie available, 2. Corroiiva liquidi ihould be itored and handled below eyi-level. 3. Dropleti of corroiive liquidi on the lidee of bottlei after pouring lhall be removed before the. bottle ii riturned to itorage, 3,3,2,3 Miieallineoui Storaga Procedures 1. Itemi on shelves shall be placed so that they will not be eaiily ipillid; 2. Reegenti ehould be grouped judiciously to circumvent dangiri of hanrdoui comb'inationi dee Table 3-1); a. Acids and bain itored teparately, b. Hater-eenaitive chemicall itored away from watir, and c. Oxidisers stored away from reducers; ' 3. Chemicels should not be stored on bench topi or in ventilition hoodi; 4. All ippiratui and reegenti, ifter un, ihould be returned promptly to thair piece of itorige; and AR30IIOO C-13 Table 3-1. MCB Hiagenta Laboratory Safety Incompatible Chemicals fluorine ixaiiiromwirytning Sepatin Hortge VIM mould bi provided lor Hydnxirtone Fluorine, eworine, Dromltie, "bcompiiiWe etienHeni," chemical* which n»y rue: (ouune, propane, chromic icid, radium pirailoe Hgeuw and cruli i huirdoui condlllon Deciun btfirene, guollni, 04 Me ruction, Some Mimplee ol lAesi Incompallnle lurpenUne, etc.) cnamfcHi are MM In mi Irtlowlng UCle. Hydracyanld KM Nllrtc KM, allull lunplnilliMOflipiagleCtieinlcili Hydrofluoric Kid Ammonli, iqueaue or Chemical____ KHB Cut el dnU.1 WIUi; • irinyaraui inhydroui Acetic Kid Chromic Kid, nllrie Kid, Hydrogen peroiildi Coppir, chromium, tan, moil Hyarwyl compound!, imyteni meuie or weir win, election, Qfrcel, perchloric icM. acetone, orginlc mnerlili, piraiMM, perminginitee miyne. nllromeinani, ' Advene CWorini, BromKii, eoppir, "ammibli flquldi, ccmOustlbli ftjoflne, Hlvir, mereury milirlili /uuinimitili, Wiier.carBcniiirKhlortdiflr HySrogensulMe Fuming nltrtc aeld, ouMKIng suUi it powdered oiher chloriniied hydrocareons, ••"* llumlnum or mag- caroon dtonioi, tni nalogeni Mini Aenyleni, emmonli (iqueoui ntHurn, sodium, or •nnydroiu), hydrogen pct*llll"n Mercury Acityleni, lulmlnlc eels, Ammonia, inhydrout Mercury (In minometen, lor ' immonli Initanci), cliMrlne, cilclum nypdcniorlli, Iodine, Bromine, Nltflc icid Acetic icid, inlllne, chromic hydrofluoric icid (inhydroui) (concenmed) MM, hydrocyinlc scld, Ammonium nlirili Acidi, minis powden, flimmibli llquldt, chleretee, nltrtlee, sulfur, finely divided Onillc icid Silver, mercury SuSSi"MmBUIIid" Perchloric icid Acetic inhydridi, bUmum ind ' Id illoyi, llconol, piper, wood Aniline Nllrlc Kid, hydrdgm peroxide _ pWM|um Cerbon lelrichlorldi, cirbon Bromine Ssmi ee for cniorlne dloilde, wiier Cirbon, iciiveied Cilclum nypocniome, ill Poimlum cniorili Sulfurlc ind oihir icidi dialling eginls Poiiulum per- Sullunc ind oiner icidi Chloriiee Ammonium Mill, icids, menu cniorili (HI ilio powdiri, lullur finny divided Chlorine) Suilnui0' """"""'*• •oieisium Qlycirin, ilhylene glycol, '" perminginiie oeniiiqihyde, lullunc icid Chromic icid ^^{^^p';^, Sliver ' .Acelylen., o».llc ec.d. lirtshc SS ilimS Kdi in «*• """"I"1"1"""""""" genenl Sodium Carton lilricntorldi, cirbon Chlortni Ammonii, icityline, buiidleni, dld«lde, wiier butane, meinene, propini (or Jodlum peromdi tlhyl or methyl ilconol, giecul omw petroleum gieee), eciUo icid, icitlo ennycnde, hydrogen, sodium eiroide, bmuldenyde, cirbo'n dliuiflde, turpentine, benieni, finely glycefM, ethyleni gtycol, einyl. divided melils KIUII, miihyl iciuie, furfuril Chlonni dlo«ldi Ammonii, methene, phosphlni, iullurlo icid Pouulum cniorili, potiulum hydrogm lullldi perchlorin, poiiiilum Coppefnnn.r, AcetyleneUM^M., hydrogen«a,n«.ini peromoninii.ae* mpermMginn „„>,„ ||g|Js (ot mi)1|1r compound| |uens Cumene Hydro- Acidi, orgsmc or inorginic u Mdlum; llmtum) peronci Remmiole nguidi Ammonium nilreie, cnromic Adipted Irom mi Oinjroui CflimicABsB'fl'}1'! fl I ecu. nydrogen oeromoe, mine Dureiu ol Plre Prevention, Cily ol LoiTliyiiliTirl ' U I, icid, looium peromoe, ine Depinmeni, Thn lul is not eomoiete, nor ere in • • • O nilogini incomoitioie luoiuncn mown C-14 D-CH84.1/SM-3.! 04/09/84 9. Packing matiritis, large boxei, etc, ihill not be allowed to accumulate on the floor of the stonrooa or the laboratory, They ihould be returned to receiving. 3.4 SPILLS AMD LEAK Spilled corroeive liquidi, enumid to be water, have been the ceun of aumeroui chemical burne. Spilli and leaki are dangeroui and mult bi deelt with quickly and properly. All laboratory perioontl ihould bi • femiliar with ipill and leak clean-up procedurei. 3.4.1 BASIC SPILL PROCEDURES 1. Determine the nature of the spill and providi immediate weter rineing to any affected body parti; 2. Notify parioni In the immediate area about the ipill; 3. Evacuati all noneiiantiil pereonn'el from thi ipill tree; 4. If the ipillid utiriil ii flammable, turn off ignition and heat lourcei; 9. Avoid bnathing vapori of thi spilled miter ill; if neceniry, uie e reipiritor; 6, Leave on or eitibliih ixhauit vintilitiun if it is nfe to do 10; 7, Secure luppliei to effect clianup; S, During cliinup, wear appropriate apparal, glovii, nfity glanei, etc,; and 9. Notify thi nfity officir if i carcinoginic lubitinci is involved, 3.4.2 HANDLING OF SPILLED LIQUIDS 1. Confine or contain the epill to a email am; do not lit It ipriid; •> , , C-15 I ) D-CH84.1/SM-3.6 04/09/84 2. For imall quantitiai of inorganic acide or bins, uia a neutralising agent or an abiorbent mixtu-M luch ai todi aih or diatomaceoue earth; 3. For email quantitiis of othir materiale, abiorb thi ipill with a non-reictivi meterial euch ai vermiculita, or dry tend; 4. For large amounts of inorganic acide or baeee, flush the area with large imounti of water; 3. Hop up the ipill, wringing out the mop in a link or a pail equipped with rollere; 6. Carefully pick up and cleen any cartone or bottlea that have been epleihed or immoreed; 7. If the ipillid material ii extremely volatile, let it evaporate end be exhaueted by the mechanical ventilation lyitem provided it ie eperk proof; ind 8. Diipoii of reiiduei eccording to the eafa disposal procedure. •—/ 3.4.3 HANDLING OF SPILLED SOLIDS 1. Low-toxicity solids' should be swept up with a broom and duit pin ind pliced in a solid wnti contiinir for dliposil, Hiita chamicali should not be put in liboritory waate baiketi. 2. For highly toxic tolidi, vacuum with a vacuum clianer in REPA filter. 3.4.4 MERCURY SPILLS 1. Collect by uiing a hoia connected to a heavy walled flaik under vacuum, end 2. Wain area with lodiuta or calcium tulfidi to rindar my nmiining mercury inert, 3.4.3 LEAKING GAS CYLINDERS 1. Uae soapy wster to detect leak. Never uae a flama. o AR30II03 C-16 D-CHB4.1/SH-3.7 04/09/84 2. If leak cannot be itopped by tightining velve, then for smsll leaks; a. Place e plsstic bsg, rubber shroud, :i similar device over the top and tape it to the cylinder to confine the leak; b, For flammable, inert, or oxidising gain, move to en isolsted erea and post signs stating hasards and warningi; c. For corroiive gem, move the cylinder to an iiolated, well- ventilated eree end uee tuitable meani to direct the gn to a chemical neutraliser. Poet warning eigni; end d. For toxic uaiei, tame as corrosive geees. 3. If leak is large or is e serioui heeard, pereonel protection (8CBA) may be neceeeery, Evacuate area and call for emergency help, 3.3 HASTE DISPOSAL Haete material can creete lefety problems both in the leboratory and in the environment, It ii important that all waite meteriali ginerated in the laboratory be diipoied of promptly and properly. 3.9.1 SOLID HASTES 1. Adequate facilitiei are luppliad for the diipoial of waite paper. Paper ihould not accumulate on the tablet or bench tops, 2, Packing materiali lhall be returned to the ihipping and receiving clerka for disposal immediately after unpacking, 3. Broken, chipped, or cracked glaiiware beyond repair ahall be diipoied of in containiri marked "Broken Clan," 4, Chemical waitei ihould not be mixed to ensure thit no dangerous reactioni occur, See Table 3-1 for incompatible lubitancei, 3.3.2 LIQUID HASTES 1. Only certain water-ioluble lubetancei ihould be diipoied of in the laboratory link. When in doubt aik your luperviior. AR30IIOI, C-17 D-CH84.1/SM-3.8 04/09/84 2, Strong acidi and baiae ihill be diluted to Ins than 1H prior to being diicarded in the sinks. 3. Highly toxic, flammable, malodoroui, or lachrymetory chemicali ehould not be diipoied of in the link. 3.3.3 HASTE SOLVENTS 1. waita eolvente will be dispossd of in deeigneted red waste cini in the laboratory. Cane are labeled for: a. Aliphatics solvente, b. Aroma tics solvents, and c. Chlorinated eolvente, 2. IB the HFLC laboratories, red cans are provided for particular lolvent eombinitioni. Whin the red ceni ere full,' a deeignetid perion will empty them in eegregited 39-gellon drum in e central area outaide the building. 3. Proper penonal protection will be worn when emptying the red cam. 4, A grounding cable will be connected between the can and the barrel to avoid electricel ipark, 3. The contrecting weite diip'oial firm will pick up the barrels every 60 deyi, For hatardoui and radioactive wnte diipoial, tee the appropriate lection, 3.3.4 MISCELLANEOUS DISPOSAL PROCEDURES 1. All waetee contained in glaiiwiri muit bi disposed of ind the glaiaware mult be thoroughly rinsed by the enslyit prior 'to delivery to the weihroom, lince the glaaiware wether ii not eware of the poeiible hasardoui niture of the vista, 2. If there ii doubt as to what should be done with waite material, tee the tupirviior, AR30II05 O C-18 D-CH84.1/SM-3.9 04/09/84 3, Deed umpling containiri mult be properly diipoied of, biting very eware of what kind of eample wee contained in it, 3.6 LABORATORY EQUIPMENT 3.6.1 GENERAL EQUIPMENT 1, Equipment ihell not be pieced near the edgei of bench tope where it could be knocked to the floor; 2. Employen ibell report ell malfunctioning equipment to their euperviiori who will arrange for proper repeir; 3. All equipment will be vied only for iti intended uee; 4. All hot pletei, motori, pumpi, weter outleti, ovene, etc, will bit tuned off when not in uie; 3. Hake certein that all electrical equipment ii properly grounded end iniuleted, Never remove the third wire ground from a plug. If needed, contect maintenence if there ii a potential electrical hasard; 6. Exteniion cordi muit be of lufficient electrical rating to handle the anticipated electrical load; and 7. Frayed or broken exteniion cordi or power cordi muit not bi uied. Replece them promptly. 3.6.2 GLASSWARE Clinwan ii uied extensively io liboratoriei, Hhile it cm be tafaly und for handling of hasardoui matiriili, if miiuied, glinwire can become viry dangeroui in the liboritory, Employiei ihould follow the preceutione lilted below and alio thon Uitid in the next eection, "Safe Procidurei," when hindling glaiiware, 1. Cracked or chipped glaiiwara shsll be disposed of in the proper uannir. If the item ie very expeniive or cinnot be eaeily . . replaced, it ihould be repaired and all iharp edgei firi polished, AR30II06 '""• O C-19 D-CH84.1/SM-3.10 04/09/84 2, All glaiiwari ihould be checked for cracka or chipi prior to uie. 3, Broken gists in the eink shall be removed and diepoead of promptly. Broken glees in the prninci of water mey not be viaible. 4, All broken glieiware ihould be iwept up end diipond of promptly with a broom and duttpan, 3.7 SATE LABORATORY PROCEDURES Safe procedurei ihould become hebiti with laboratory penonnrl. While there may be a fatter way to do lomithirrg, the employee smit ilwiyi nmenber that the lafe way ii the batter of the two. During indoctrination, it ii alio importint that niw imploym learn the life procidurei during indoctrination, 3.7.1 PROCEDURES WITH GLASSWARE 1. To iniert glut tubing into itoppen or r'ubbir tubings, employeei ihould follow the procedure detiilad below: a. Fire polish the end of all glass tubings, b. Chooie rubbir tubing and bore holea in atoppers so that proper fit ii obtained. Cork itoppen ihould be rolled to toften before boring. AR30II07 C-20 D-CH84.1/SM-3.11 04/09/84 c. Lubricate the glaii with water and glycerin, d. Hear leather glovee. Insert the tubing through the itopper uiing a ilight twitting thruet. e. Pull tin tubing whenever poeiible. Push tubing only when etarting through hole, In tone ciiei, it may be convenient to perform Stepi a and b alone; then, leaving the cork borer ineerted in the stopper, proceed ss followi: f. Iniert the gleet in the berrel of the cork borer to 'the depth deeired. g. While wiiring liather glovee, remove the cork borer with a twieting motion. 2. Gleee or metal tubing ehall be ineerted entirely through stoppere to aesure that the end mey not be closed over by heat or solvent action, 3. To remove glaee tubing or thermometers from rubber, it is deeirsble to cut swsy the rubber, Thie is particularly true if the tubing or atopper hai been in place over an extended period of time, or if it hae bein subjictid to heet, 4. When heating materiali in glen by miani of a gai fline, the glaai lhall be protected from direct contact with the flame through the uee of e wire gage, 3, When placing liquidi in bottlii which have a poiitiva cloiure, more than 3 percent of the volume shall bi reierved ei air tpaci to allow for expaniion, 6, Frotin stopcocks or ground glni itoppen lhall not bi forced, Either; i, Uie a itopcock puller, or b, If the niture of the eontenti of the vetiil permitt, cool , the ihell until the plug ii cold, then heat the ehell of ' the joint momentarily. Hithdriw the plug quickly before it expande from the heat. AR30II08 C-21 D-CH84.1/SM-3.12 04/09/84 3,7.2 GLASSWARE UNDER VACUUM PROCEDURES 1. All glanwari undir vacuum ihill be proti'.tid from phyiical ahock which might cauaa crackt, mult ing in collapn with imploiive violinci. 2, Flit bottom fliiki ihill not be lubjectid to vacuum unlaii conitructid with haavy wills ipecificilly for luch iirvice, 3, Stmdard wall (iphiricil) flaiki, lirgir than 1 liter, when und in vacuum lervice ihill be guirdid by i ihield that it idequiti to stop all flying glan ihould collapn occur, • 4. Cork or rubber itoppiri uied in glaiawiri undir vacuum shall be carefully choien to be of tuch tin thit they will not be drawn into the opening which they are intended to clou, 9, Vicuum in any lyitem lhall be relieved before any attimpt it mede to diiainmbli the equipment, 6, Rot fliiki contiining uncondenied vipori or itiim ihill not ba itoppered; to do 10 will subject them to vicuua on cooling/ 3,7,3 SAFE PROCEDURES WITH CHEMICALS Many chemicali und in thi laboratory are viry dingiroui, Unknown ructions could occur it my time evin with the moit itible compounds if aubjected to the wrong conditioni, Employiet ihould bi fimiliir with ill hisirdi aiiociitid with chiaicili they ire uiing, Thi following art pricautioni which ihould bi uied whin hindling chimieili. For ipicific chimicili, in the "Specific Chimicil Rnardi" iiccion of this ninuil, 3.7,3,1 Caneril Chemieeli 1, All unknown chimicili, reigincs, iimplai, itc, an to bi considered hnardoui until niurinca to thi contriry ii obtiined. '* • . . 2, Little known reictions miy bi encountered in ixpirimintil work, Propoiid programi ihould be diicuned with thi tupirviior before attimpting divilopnint work. O AR30U09 C-22 D-CHB4.1/SM-3.13 04/09/84 3, When opening bottlet contiining diitolvid gam (NH^OR, HC1, etc,) or impoulei of liquidi of high vapor pritiure (Brj, icityl chloride, etc,), care shall be tiken that j.ta ayei iri protected from any poiiible ipriy. a, In no ceie lhall the container be opened when the contenti are above room temperature; b. If opened cautioutly, teriw-capi on itindird 9-pint bottlei will tend to give io» protection by directing any ipriy• downward; c. Glan ttoppiri, onci removed, will generilly, but not elweyt, relieve prenuri by permitting gii leakage, Therefore, when using such bottles (including ihilf reagenti), the bottle ihould be held eway from the face while removing the stopper, 4. Tilting for odor of unknown meterikli ihould bi doni cautiously and alwayi with the lungi full to that unplmint gnn/vipori miy be expelled promptly; preliminary taiti ihould bi midi by wafting the gam/vipori by hind motion from the open contiinir toward the noil, 9. Gam/vapori of my variity may bi toxic or may produce unpleaiant rnulti if inhaled in sufficient concentratione or over extended amount! of timi, Tharifon, any riaction which involves the evolution of gnn/vipori will bi cirried out where ventilation ii adequate. All opintioni which produce hitirdous giiai, fumii, or vapori ihill be carried out in thi hood, 6, Corroiiva, toxic, hot, or flioubli liquidi und in lirgi volume ihill bi guarded to Chit equipment filluri will not lead to danger to perionnel, 7. Oxidising igenti (e.g., perchloric acid and bromine) in conticc with orginie ind othir reducing iginti miy produce i violent . , reiction, fire, or axploiion. Thiy may bi uied only in ipicific initincii undir direct tupirviiion. AR301UO C-23 D-CH84.1/SM-3.14 04/09/84 8. Organic meterialu in contact with the ikin may havi unpredictable effecti, In none initancei'. levere catei of diraatitii have been traced to chemicele by which othert were unaffected. 3.7.3.2 Acidi 1. Acidi in contict with the ekin will cauie burnt. Should an acid be epilled on the body, the effected area ihould bi promptly waehed with large amounti of water. 2. When handling concentrated acidi; a, Rubber glovei ihould be worn; b, Spleth proof gogglee ind aproni ihould be worn; c. Hydrofluoric, perchloric, end tulfurout icidi ihould never be obtained in quantitiei gfeater than 1 liter; d, Alweyi pour acids into water; e, Whin emptying acidi ind cllining tolutioni into the dnin, firit fill the link with witer, pour the acid into the link, then lit,the witer drain out, Allow the tap to remain on full for e few additional minutei, , t 3.7.3,3 Bim 1, Bans will cause burnt if they contict the ikin, If thii occurs, the irea ihould be wished with copiout mounti of witer, 2. Concentrated bnei ihould not bi scored in glass itoppered boctlei or thi glut ttoppiri will frieti in plica, 3. Concentritid ammonium hydroxide and solutions of potasiium and todium hydroxide which are 10 N or above shill be treited is concentritid icidi. 3.7.3.4 Volitile and Flimmible Materials 1. No opin flimei art permitted in the ireai where volitili lolventt are uied or itored, AR30IIU I! C-24 D-CH84.1/SM-3.13 04/09/84 2. Volatile eolventi that ari immiicibla with water lhall bi retained in approved tafety cam labeled "watte lolvenc." If the lolvint containe tracei of a corroiive acid, the eolvent will be waihed with dilute (1 N) NaOH solution to neutralise the ecid. 3. A eeparate building shall be used for bulk quantitiai of lolventi, . 4. A 1-gillon eolvent bottle ihould be placed in a protective cerrier when ueed, 3. Flemsuble liquidi ihould be utid only in a properly functioning fume hood. 6. Voletile eolventi, when ehaken in aeparatory futmeli, may develop considereble preesure. Rupture with expletive violence may be evoided by frequent removal of the ttoppir or by opening the etopcock when the funnel ii inverted. 7. Volatile, flammable materieli thill not be plecid in oveni or furnacet. 3.7,3.3 Caiee ESE leboratories use a variety of giien for analytical initrumentition, Improper uie and maintenance of gai cylinderi end the gam themtelvii could cauii tarioui injury and damage, Ccmpreiied gnei ihould be handled with the following precautioni in mind, 1, Comprened gu cylinderi ihould be .iicurid with a chain or cylinder itand, 2. The nature of the geiaa ihould be notid by liboritory perionnel, 3, Trapa ehould be used to prevent back contamination of the cylinder, 4. Proper regulator! ihould bi uied with each cylinder. Regulator adaptin ihould never be uied. AB30III2 C-25 D-CH84.1/SM-3.16 04/09/84 3, Thi miin valve ehould be cloaed whin the cylinder ii not being ueed. The preiiure in the reguletor ihould be reduced to etmotpheric prmura, 6, Steel cylinderi ihould never be immeriad in liquid nitrogin, 7, Cylindere ehould not be stored nesr sourest of hest. 8. Liq'uified geees shall not be placed in any container which can ba accidently aealed. • 9, Never connect a gas cylinder regulator that has been used for eny gn other than 02 to an 0] cylinder, 3.7,4 Miieallineoui Safe Procedures 1, The cover of the centrifuge ahall not be lifted until rotetion has etopped. The cover ehall be cloeed when not in uee, 2, When uiing a cork borer, the stopper thill not be held in the palm of thi hind. Rather, it ihould be placed large end down on a toft, flat lurface end held betwein the thumb ind forefinger. The cork borer shall be kept tharp and ihould bi lubricated with watir or glycirin to privent binding. It is not to be forced through the etopper, but rather twitted to cut the miteriil, The uii of leather glovat gives iddid protiction in caie of ilippige. 3, Rigidity of equipment aliemblin ihill be inured by the uie of c Imp ing devices, 4, Furnace and oven doors lhall be provided with vents or nfety latchn which will releaie readily in caie'of internal prinure, 3, Stopperi ihould not be tat down while liquidi are being poured. 6, Hot platii ihould nivir be assumed to be cold, 7, When traniporting hot items, tongi or heit protective glovn lhall be uied, ' ' ' 8, Keep timporiry wiring to a minimum, Remove it or have a permanent let up tubitituted, 9, Do not overloid linei with too miny ittachmenti, o AR30III3 C-26 D-CH84.1/SM-3.17 04/09/84 10, Equipment end glanwiri ihould not be etored, even temporarily, on a hot plate. 3.8 SAFETY EQUIPMENT Sefety equipment may be divided into two general claaaee: firet, that ueed for the protection of life or property in ceie of emergency or unueual happening; and eecond, that und diily at protiction againit known and anticipated hasarda. All employees should become familiar with the location and uee of thii equipment. 3.8.1 EMERGENCY EQUIPMENT 3.8.1.1 Fire Control Equipment 1. No obitruction, even temporary, ehell prevent acceit to fire equipment. 2. All ESE laboratoriei ere equipped with ABC type fire extinguiiheri. Then extinguiihert are effective egeinit burning paper, liquidi, ind electrical lyitimi. Belt reiulti ere obtained when the COj ii blown directly on the burning material from a distinct of 3 or 4 feet, 3, Fire blanketi art placed ttritegically in laboratory areai for uie in the event that penonal clothing catchn firi., 4. An extinguiiher which hai been uied lhall not be returned to its bracket but shall be turned ovir for recharging, 3, All extinguiiheri ind alarmi will be impacted monthly, 3,8,1,2 Other Emergency Equipment 1, Eye waah fountaina are available for irrigation of the eyei ihould corroiive liquidi be ipliihed in thin. 2, Sifety ihowiri ihould be und without heiitation in the event thet ecid, etc,, it ipillid on the clothing or ikin, 3, A telf-conteined briathing apparatui ii provided for protection from hasardoui vaport or gam re lined in a laboratory accident. AR30IIU C-27 /'~~\ D-CH84.1/3M-3.18 04/09/84 3.8.2 PROTECTIVE EQUIPMENT 3.8.2.1 Parsonal Protective Equipment 1, Laboratory coati or aproni iball be worn by all pertont hindling chemicili in thi laboratory and by tuch other perioni whoii '" eetivitiei tubjict them to hisardi due to ipilli or splashes. 2. Closed-toe ihoei mutt be worn it sll times in the leboratory, 3. Eyi protection ii riquind it all timet while in thi liboncory. Safety glaiiit ire provided and muit be worn by all parionnil who do not norailly weir glaiiei. 4. Full face thieldi ihould be worn if there ii a potential for iplaihing of highly corroiive or toxic chenicali. 3, Glovet cm protect the wearer from many Ujuriii: a, fine protictive glovei ire provided ind ihould bi uied when handling hot or cold objects. b, Liather glovei lhall be uaed whan handling broken glanwiri, whin iniirting glut tubei into rubber itoppirt, ind for •'~\ like operitioni when i firm griip of a mill object is •-' required but protection from corrosive chemicili ii not noceiiary, c, Riavy rubber gauntlet glovei ihill bi used in hindling lirgi volumei of corroeive liquide, Ciri lhall bi ixirciiid when glcvai bicomi wit biciuie rubber it prom to become ilippiry, d, Surgicil glovii or other light-weight gloves ire provided ind ihould be used for protection igiinit toxic, irrititing, 'or ridioietivi maCiriili in thoce. operitioni requiring dixtiroui uii of thi fingeri, 6, Riipiricori with proper cirtridgee muec ba worn when inilysii cinnot bi completed in a hood and toxic matariali iri involved. AR30III5 O C-2B D-CH84.1/SM-3.19 04/09/84 3>8,2>2 Other Froteccive Equipment 1. Mital carti are provided for traniporting liboritory equipment, chemicili, end glanwsri. 2. Ventilation a. Ventilation hoodi ihould be uied when heiardoui funi, gssn, or liquidi art being uied. b. Hood windows inould bi lowered for control of fumei and to provide phytical protection in operetloni involving thi hiating (and where poiiible, othir handling) of flammable, corroiive, or potintially exploiivi matiriili. A lowired window ihall not be raited until it ii eitibliihed chic no basardoui operetion ii being carried on behind it, c, All hoodi ere larked for a mh lavsl that will allow the hood to ventilate at 100 fpm, Saihas ihould be miintainid at thii livil or below whenever poiiibli, d. Hood air velocltiei will be checked on a quirtirly bnii, 3. Safety ehieldi are to be und in opiritioni involving ponibli exploiioni or flying pirticlee, Somi type of ihield ihould bi uied for diitillationi in glut which involvi appriciibli quanticiis of corroiivi matiriali or flimmabli tolvinti, ind/or uie of vicuum technique, Shieldi ihould alio bi uied for reactioni of unknown charaetariitici or thoti which may conceivably become exploeive or otherwiie uncontrollable. The ventilation hood window ii oadi of iificy glut and ii in adequate ihield in many ciiei, 4, Soap and watir, if und friquintly on the Hindi and.armt, will move uniuipecced biti of irrititing materiali. 9, Stip liddiri or foot itooli shill be used for niching high objecti. Hindrails, chairs, pilid boxii, or other makiihift devices ihould not be tubititutid, Whin not in use, lidderi end- •cools ihill bi itored in such i way that thiy riprmnt no tripping hatard. AR30IM6 C-29 D-CH84.1/SN-3.20 0 04/09/84 3.9 EHERSENCY PROCEDURES While eccident prevention it the primary goal of laboratory tafity proeidurn, emergenciee may ttill occur, Whit action employeei tike cm influence eke extent of injury and damage, Thi procidurei below are intended to be uied in the cm of in emergency and to minimise injury and diuge. 3.9.1 FIRE OR EXPLOSION .. • • 1, Hinor fire i. Alert all laboratory perionnil ind send for aniitinci, b. Immediately attack the fire with the portable fire extinguithiri availibli. c. Alweyi fight thi fin from a petition iccetilbli to an exit. d. If electrical firi, do not uie water until electricity ii off. 2, If fire geti out of control or ii a mijor firi: o i. Pull firi alarm and immediately contict firi dipirtmint, b. Confine the fire by doting doors, hood snhii, etc,, to prevint furthir ipriading, c. Aititt any injured pereonnil, d. Evacuate the irn, 3, Perionnil on firn i. Hrip in firi blinkit to imothir flimee or douee under iifeey ihowir. b. Cill for midical help immediitily, 3,9,2 CHEMICAL SPILLS 1, Area ipill—lie Section 3,4, "Spilli ind Liaki." 2, Chemicili ipillid over lirgi am of body; i. Quickly remove ill conciminatid clothing, > ... b. Get pereon to nfity ihouer ind flood irii for it lint 13 minutei. O C-30 D-CH84.1/SH-3.21 Vajl,' 04/09/84 c, With area with mild detirgent or toit. and watir. d, Call for midical help. 3. Chemlcali iplllid in confined am on ikin; a. Fluih'irn with cold water and wath with mild toip, b, If oo viiible burn, wish with wan watir and toap. c. If there Ie a delayed action, obtain medical attention immediately. ' 3.9.3 CHEMICAL INGESTION 1. Encourage victim to drink lirgi amounts of water, 2. Obtain immidiate medical aatiitince. 3. Contact local poison control cintir. 3.9.4 FIRST AID All liboratory perionnel ihould obtiin training in tint aid and cardiopulmonary muicitition (CPR). Only thoie triinid in tint lid or CPR ihould admioittar lift living techniques, ai improper iction using (aj|J;: CPR could ciuie an injury more iiveri thin thi victim hn ilrndy suffired, CPR techniquei will not bi detailed here. Firtt aid tichniquei for certain problem will bi lucid. 1, Heavy bleeding: a. Lay the patient down. b. Apply firm prniuri to wound with clian cloth or hand, c. Do not apply a tourniquet unleis thi injury it in imputition or the binding cinnot bi stopped, , d. If toumiquit ii und, record the timi it was ippliid, i, Call immidiitily for medicil miitinci, 2, Shock; Shock uiuilly icccmpaniii eevere injury. The lymptoni of ihock art: ., . , , a, Paleneii, b. Cold, climmy ikin, AR30IM8 C-31 ,~ ' D-CH84.1/SM-3.22 i j 04/09/84 c, Perepiretion beade on forehead, palmi, d, Weakness, a. Hausee, f, Shallow breathing, end ,- g. Week pulse, ' Treatment ihould bi ei followt; e, Correct the cauee (uiuslly bleeding); b. Keep the patient lying down; c, Keep patient's airway open; turn the heed to the eide in ceee he'/she vomiti; d, Keep petient wsrm; and e. Call immedietely for medical help. 3. Electric Shock: e, Turn off the power immediately either at the tource or at the circuit breaker, b. Do not touch the victim until he or ihe ii iiparatid from ' •, the current tource, and "~^ c. Call immediately for medical help, 4. Other injuries; a, Keep patient quiet, ' b. Keep petient warm and itill, and c. Call for immediate medical attention, 3.10 EMERGENCY PHONE NUMBERS Emergency , 911 Ambulance (non-emergency) 374-3222 Fire ' 911 Poiion Control Center 372-4321 or 392-3389 , Sheriff, Alachua County 378-1641 * • North Florida Regional Hoipitil 377-8911 Shindi Teiching Hoipital; Emergency Room 392-3991 Othir Officei 392-9000 AR301 I 19 Alichui General Hoipital 372-4321 -- • . . „•? G C-32 D-CH84.1/SM-4.1 04/09/84 4.0 SPECIFIC CHEMICAL HAZARDS ISE laboratoriee, ai iteted earlier, uie and analyse a wide renge of chimicili, It ii important that all laboratory perionnel are familiar with the materials that are ueed or encountered in deily ectivitiee. The following ie e lieting of ipecific compounde, their hesardi, and pracautioni to be taken when handling theie compoundi. Not all compoundi can be lieted here. For thoee thet are not, refer to your tupirviior, the "Hirck Index," or the Material Safety Data eheett which cen be obtained from Joe Plunket, the Chemical Purchasing Coordinstor, Acetic ecid can cauee bunts if ipillid or eplaihed on the ikin. It penetratei the ekin mily and can caute dirmititii and ulceri. Affected areei ihould bi wnhid with witer immediately, Acetic acid ii particularly dingirous in contact with chromic acid, toiurn piroxide, or nitric ecid, Amino eompoundt may cauti nrioue illneit if the vapori are inhalid or if the liquid ii illowed to have contact with the ikin, Some eminoi are highly toxic, otheri ire only slightly toxic. Ammonium hydroxide is corrosive and will cause burnt if ipillid or iplaihed on the ikin, Affected areai ihould bi fluthed immediately with large imounti of watir, Vipori are irritating to the eyei ind mucous membnnei. The chemical ihould be uied only in a, well-ventilated area, Ammonium hydroxide when combined with iiveril lubttancai luch at mircury, tilver, and iodine forma exploeive compoundi, Amoniacal silver nitrite lhall never be hept on hand, even in email quantitiii, for more thin i few houri, Haiti materials ihould be neutriliced with.icid prior to, , diiponl, Arianic. antimony, and their coapoundi ere toxic, Ingeition of imill quantitiei may mult in deith, fln30l12ann/-> 0 C-33 ,'"> D-CH84.1/SM-4.2 .._,' 04/09/84 Barium compoundi ind the compoundi of thi heavy mitili ire extremity poiionoui, Among then are the talti of cidmiua, copper, leid, molybdenum, end bsryllium. ,„ liniene ii flimmible end toxic if the vapor ii inhaled or if the liquid ia ipillid on the ikin. Thi riagent ii to bi diipaniid only in a will- vantilatid area. . Bromine ii extremely poiionoui and corroiive. Even the vepori will produce ikin bum, All handling of liquid bromine ihall be carried out in a well-ventilated aree, Bruetna ii an ixtrimily toxic lubitince, Ingiitlon of imill quint it in may mult in diith. Carbon dliulfide, while toxic, ii most hnirdoui dui Co iti high f"\ flemmibility. Iti vapori an expletive in air in the rangi of 1.23 to '•—' 90 percent by volume, ind it ignitii tpontiniouily at about 423'C, Thus, the hiat of i hot pliti or even i light bulb may enily ignite the vapori. Carbon diiulfidi ihill be used in a flimi-fm hood, Chlorine and nirehloritis (perchloric acid) may product violint , ixploiioni when in contact with organic or other reducing materiali, They are to be ueed in thii laboratory only upon ipicific tuthoritition ind diriction. Chloroform ii toxic if inhalad, ind contict with the ikin ihould bi avoided linci ebiorpcion through thi porit oiy product thi iimi physiological iffecti 11 inhilicion. Exciiiive drynen with subsequent cricking of thi ikin may alio result from contict. Rubbir glovii ihould be worn, ind chloroform ihould be uied only in i well-ventilitid int. Chloroform is neither flimmabli nor exploeivi, AR30II2I O C-34 D-CH84.1/SM-4.3 04/09/84 Chlorine, tee "Uilogini." Chromic acid and ehromatai are etrong oxidising agenta, and many organic mstsriali will be ignited upon contact with them, Cvinidai. cyanogen, and hydrocyanic acid (pruetic scid) are extremely toxic. Death ii almoit immediate if theea are taken internally or if inhaled. Then ihould not be etored or mixed with ecid solution. Dry lee, like liquid eir end other liquified gsses, ihill never be pieced in a container which cen be eccidentilly leilid. It ilio cauiei tevere froitbite on the ikin and lhall, therefore, be hendled vith heavy glovei or tongt, Etheri in itorige hive e tendency to form peroxides, which are expletive if heeted, No ethere ihould be distilled or otherwite iviporitid to drynen unlm snslysis shows the peroxide content, ei hydrogen peroxide, to be not grester than 0,10 percent. Ethyl aeetata is a fire hatard and ihould be uied only in a flimi-free hood. It ii irritating to mucous surfsces, psrticularly the eyei, gumt, end reepiratory paaaagei. Repeeted or prolonged expoium may cause eerioue irrirstions, Surgical glovii ire required when hindling, Fluorine, fluoridei, and hydrofluoric acid are'extremely poiionum. The halogen and the acid are quite corroiive and in contact with the ikin yield ilow-hnling tores. Hydrofluoric acid ihould not be ttored in glut bottlae, ^ • .i Halogena (chlorine, fluorine, bromine) and halogen icidi ere corrosivi. Vepori are irritating to the reapiratory tyitim membrines ai will ia the fleeh. AR30II22 C-35 ~ D-CH84.1/SM-4.4 :•' } 04/09/84 -.—'' Hydrochloric acid, lie "Halogeni and halogen acide," Hydrofluoric acid, tee "Fluorine." ,„ Hvdroien peroxide, on itinding, tendi to decompoie with ivolutlon of gai, Hfdroean ml fide ii extremely poiionoui even in trice imounti. All riactioni involving thii gn lhall be carried out in a well-ventilated arai, Mercury ii haxardoui chiefly through thi ponibllity of inhaling thi vipors. Iti vipor priisuri ii ippriciabli even at room timperaturi (iquivalint to 0,04 mg/l at 30'C) and toxic quantitiei art probable under unfavorable conditloni. Sifety iay be murid by edequata ventilation, by cleaning up ipillid aercury promptly, and by maintaining a minimum of uneCopped contiinirs, Compoundi of mercury iri ixtrimily toxic; hindi 0 ehould bi wnhad thoroughly aftir hindling them (ne Ammonium Hydroxide). Methyl alcohol ii extremely, toxic ind miy lied to blindnm or diith if tikin into the digiitivi or rnpiritory tyitini or if ibiorbid through the ikin. Ici effect virin lomcwhit imong individuils. Methyl eehyl kecone it i flimmabli liquid and a dangeroul firi hmrd (set Section 3,4, Liboritory Proeidurn), Nitric acid, on contict with uny organic matirlali, may lead to fire or exploiion. It may only be used to remove orginic mitiriali 11 diricced by thi inalytical procedures or by your tupirvisor. Nitric icid ii extrimily corroeive to thi fleih, ind iti fuaii iri highly irrititing to the BUCOUI nembrinii of the eyii ind rnpiritory tnct>. . , , o AR30II23 C-36 D-CH84.1/SM-4.3 04/09/W Oxilte ie id and iti iilti have a cauitic iction on the ikin and on the internal organi if iwillowid, When ingested in livrgi quantf.ttii, death may follow quickly. Oione ii produced by the diichergi of a high potintiil voltigi in air, It may be encountered when operating certain initruminti, Thi MAC for oeone in air (8-hour work diy) ii 0,1 ppm, Expoiura to 1 ppm for ihort periodi will product drynin of thi lyii ind rnpiratory' trict ind headache. Expoiuri to 1 ppm for axtinded pariodt of time or higher. coneentrationi for a thorter period miy mult in tevere or even fitil injury to thi lungi, Oione hat a characteriitic odor thit can' bi detected by mil whin thi concentration exceed! 0,013 ppm. When thi odor of osom ii noticeeble, lieve thi aria or diicontlnui thi operation of the equipment that it producing thi ospns until the concincrition cm be determined ind/ or idiquici vintilicion'iitibUthid. Perchloric icld hit a trimendoui, potintiil dntruccive power md ihould ^ —"" " be handled with extreme caution. Whin hindling pirchloric icid, protective rubber glovei, apront, and a face shield or anti-ipliih goggles ihould bi worn. Oni drop of pirchloric icid iplishid on the eye will ilmqic eirtainly cauie thi Ion of that lye, Perchloric icid is e itrong oxidant, and extreme cirn should bi ixirciiid when uilng ic to deitroy tncii of orginic meter ill. Orginlc matiriil (e.g., piper toweli) contiining even one drop of perchloric icid ihill not bi diipoied of in waiti containiri until the aeterial hae bun thoroughly fluihid with nicer to dilute ind remove the perchloric icid, Diiooiored icid, which miani chic it ii contiminatad with orginic or inorginic miciriil, ihould be diipoied of lunedlitily. Bottlli of pirchloric acid ihould be kept on a glaii or porciliin (unchippid) tny, e '\ t i , Perehloroethyline ii toxic whin inhaled, ingested, or following prolonged or repeiced contict with thi ikin, AR30ll2lt C-37 •) D-CH84.1/SM-4.6 '-••'' 04/09/84 Peroxidai ire strong oxidising egenti, Thiy may r/e und only in cirtain apecified initincii, Orginic piroxidee an highlj axploiive (in "Ithare"), Phosphoric icid ii highly corroiive and will cauii painful burnt upon contict with the ikin, Affectid iriai ihould bi immidiitaly waihed with water. The acid generatei coniideribli heat upon addition to water, end mixing ihill, therefore, be carried out in a Pyrex vettel. Alwayi pour thi concentrated ecid into the water, never the rivern, Potaiiium hydroxide and iti solution iri extremely corroiivi, Solution of the solid in watir liberatei coniidiribli heat, and mixing ihill, thirefore, be carried out with cire in Pyrex or metil contiinin, Silver nitreee ii toxic if taken internally, On contact with the ikin, the lilt or iti lolution ciun ikin diicoloritioni. Flush ifficted pirts O immediately with large amounts of watir, Sodium hydroxide. Ill "Potmium hydroxide." »• Sulfuroue icid fuaii (or lulfur dioxidi) iri highly toxic, Concintntioni as low as 0,3 to 1 ppm can bi ditected by the ivirigi individual by taeti, rather than thi iinsi of smell. Work with sulfurous icid ihould bi doni in i hood, SuUurte acid la highly corroiive and will cauii pilnful b'urni upon contict with the ikin, Afficcid iriii ihould be immidiicily wiihed with water, Thi acid giniritii coniidiribli hiit upon iddition Co wicir, ind mixing ihill bi performed slowly in i Pyrix venel. The concint'ricid icid ihould ilwayi bi pound into wicir, never the reverie. Toluene ii flinoibli, and the vapore are noderecely toxic (in Section 3.4). o AR30II25 C-38 D-CH84,l/SH-4,7 04/09/84 Trtehloroathylini ii modiritely toxic whin the vipori are inhaled or when the liquid ie ipillid on the ikin. Avoid breathing and akin contact with organic eolventi. Many aolventi are more toxic than generelly thought. Heated mixtum of concentrated perchloric ecid end orginic matter aay explode violently. Avoid thii hisird by taking thi following precautioni; (1) do oot add perchloric acid to a hot lolution that'nay contain orginic matter, (2) alwayi pritriat iimpln containing organic metter with HHOj prior to eddltion of HCIO^, (3) uea a mixture of nitric and perchloric acidi in itarting thi digiition itap, (4) evoid repeited fuming! with pirchloric icid in ordinary hoodi, For work with perchloric ac'id, connect e water pump to a glm fume eridicitor, 49301126 C-39 D-CH84.1/SM-9.1 04/09/84 3.0 HAZARDOUS MATERIALS ESE hee become highly involved with hacardoui waite lite inveetigetion and with sample analyiii from thna litei. Theie material!, in addition to haserdoui materiali already being uied and analyied in ESE liboritoriei, muet be handled with care due to their increaied potintiil for heelth problem! in pereonnel expoeed. While ell nfety procedurei addreeeed in thii minual, to thii point, apply to activitiai involving besardoue miteriale, thii lection detail! additionel procedurei deeling specifically with haxardoui matiriali and waitn. 5.1 GENERAL PROCEDURES 3.1.1 DETERMINATION OF HAZARDOUS MATERIALS Sample! or material! from haierdoue waete projecti will be labeled "hesardoua" prior to irriving at the laboratory by the Field Teim Leidir. If e leboratory employee or tupirviior hai a queition about othir materials with which they will be working, he csn refer to: 1. Identificstion and Listing of Hstardoui Waits, Fidaral Regiiter, 43(98), May 19, 1980, Part 261. 2. Dantiroui Propertiee of Industrie! Materials. Sax. 3. ACGIH TLVi, 1983-84. Hitardoui wntei an generilly chiricterind at thoie mitiriali which ere: 1. Highly toxic; 2, Carcinogenic; 3. Radioactive; 4. Flammable; 9. Exploiive; or 6, Reactive, tuch ai; —Oxidizers, —Reductinti, C-40 D-CH84.1/SH-9.2 04/09/84 —Corroiivei, or —Watar-reective lubitancei. There ere numeroue cleiiificition lyitimi for citigorising hmrdoui chemical!, None ere entirely latlifictory 10 it ii important for the. employee or aupervlior to find out' all he cen about the materiil or materials in quiitlon. If questions itill remain about a potentially hmrdoui matirill, contict the Corporati Safety Officer or,other eifity profmional. 9.1.2 PERSONNEL All pinonnil involvid in the handling in* analyiii of hmrdoui materiali, will be citigoriiid according to thiir potinclil livil of expoiuri to thi mittriil, The Project Manager in coopiricion with the Laboratory Safity Minagar will citigcrizi the liboritory pirionnil. All liboritory perionnil involvid in thi handling of hatirdoui miciriili muit undergo triining relitid to'thiir activiciei in the liboritory, ESE11 "Hiilth ind Sifity Proeidurn for Hmrdoui Projicci" lilts thi triining which is offered to perionnil involved in hmrdoui projecti, Thi imount of triining a parion riciivis will depend on the imount of involvement. All liboritory pirionnil involved in hmrdoui projicti wt'll undergo baeeline medical axaminationi prior to iny work involving thi hmrdoui •itirials. Then iximinicioni will include i 1, Hiicory, ., , , . 2. Lung cipicicy, 3, Hurt—EKG, 4. Eyei, 9, Audiomitry, AR30H28 C-41 D-CH84.1/SM-9.3 04/09/84 i, Cheit X-ray, end *». 7. Blood profile. Eximiutioni will be given on in annuil baili u long ai pirionnil iri involvid with hnardoui projects, 9.1.3 LABORATORY SAFETY PlANS All liboritory perionnel ehould thoroughly reviiw thi Liboratory Sifity Plan for iich hmrdoui projict with which thiy art involvid. Thii plan will include: „, 1. Deicriptioni of the chemicil ind physical charactiriitici of thi anticipated iimpln, 2. Procedurei for life handling, . _ s 3. Appropriate itorigi proeidurn, ' ._J 4. Spill cleunup procedurei, 3. Proper procedum for analysis, and 6. Propir wnti diiponl mithodi, t It ii thi laboratory imployii'i responsibility to know thi hmrdi of ind pricautioni to be tiken with the hmrdoui oatariali. It ii thi Projict Liboritory Minigar'i rnponiibility to naki lure liboritory pirionnil hivi mn and read thi Liboritory Sifity Plan. 9.1.4 PERSONAL PROTECTION It ii s cinder d policy whin hindling nmplii in thi liboratory chit extreme ceucion bi tikin. Simples (all into thru bnic eatigoriii. Then citigoriii iri at followi; ., , , , I, Cliin umplii—choii tamplii chit do not contiin carcinogenic or haiardoui micariili; 2, Suipect iimplei—thoie nmplii thit iri tuipictid of contiining carcinogenic or haiardoui matirials; and flR30H29 C-42 u,,. D-CH84.1/SM-9.4 04/09/84 3. Know carcinogenic eamplei-thoie aiaplei thit ere known to contain carcinogenic matiriali, When handling all water nmplii thi following iifaty procedurei ihould bi employed by all laboratory piriotmil: 1. Heir glovei, 2. Wear eye protection, 3. Weer laboratory coati, 4. Wear protective footwear. 9, Wear rnpiritory protection if working outiidi of i hood (euepect or known carcinogen handling). Each protective meaiuri ii ixtrimily importint for thi health and tafity of all laboratory pirionnil, Sifity glmii iri provided for all . laboritory perionnil by thi Chemiitry Division, These protective eye glmii ari impact miitint. Safety glami iri availabli for viiitori to thi laboratory. Then glints iri locitid at eech entrance to the laboratory, and ere to bi worn by everyone intiring thi liboritory, Thi vititor glmei, howivir, are not approvid for ngulir or continuid uia in thi laboritory, biciuse thiy iri not ipprovid nfity glum, Thi uii of liboritory coiti it for thi prediction of the analyits1 clochn ind ikin, in thi evint of in iccidant, Protictivi footviir mini cloud coe ehoei that do not riidily abiorb lolvenci or witir nmplii, 9.1.9 SUSPECT SAMPLE HANDLING AND STORAGE Suipict tamplii will bi markid with yillow tigi whin thi nmplii era chicked into the liboritory or 11 toon n it ii known thit thirl ii i potiibli hisard by thi liboritory coordinator. At thi time of check in, tuipict eamplii will be indicated on thi log ihiec. Uiing chis michod of digging iniurn thit thi tampli will automatically receive tpaciil hindling procidum in the liboricory ind in diiponl, In iddicion to eifecy proeidurn outlined ibove, the simple container ehould be opined AR30II30. © C-43 D-CH84.1/SM-9.9 04/09/84 in the hood and, when appropriate, the temple ihould be handled and analysed in the hood with lufficient ventilation. The clean and tutpict lamplee ere itored in the main cold room at 4'C, with impact tamplei cliirly labeled. • 9.1.6 KNOWN CARCINOGENIC SAMPLE HANDLING AND STORAGE Atteched ii i lilt of known carcinogini. Whin nmplii an known to contain then uteriilt, extra ciucions will be takan. Then procedurei include; 1. Marking clearly the temple containiri with RED tigi. 2. Storing the erapln in thi toxic liboricory.* 3. Determining prior to milyiii lift temple handling levels for the general laboratory and thin diluting to that acceptable level. Dilution and handling of tamplii ihould be conducted in Ii -^\ the toxic liboratory 4. When neeimry, inilyiing the nmplii in thi toxic liboritory. * Accill to thi toxic liboratory it limited to qualified perionnel, 9.1.7 SPILL AND LEAKS 1. All ipilli ind Inki will bi cliinid up according to procedurei deicribed in Section 3.4 of thii manual. 2. If necemry, appropriate perionil protiction will bi worn by employees. Thi iilf-contiinid breaching ippirat,ui miy bi nicmary. 3, All ipilli will bi reported immediitily to the Laboracory Manager, 3.1.8 WASTE DISPOSAL 1. All waate matiriils will be plicid into iapirmiiblt and mlid containiri. C-44 D-CH84.1/SM-9.6 04/09/84 2, Thin containin will be labeled, DANGER—HAZARDOUS MATERIAL, with the name of the matsrial on the label. 6 3. The containers will bi tumid over to the Chtmlttry Departmnt Purchaaing Coordinator. 4. Kmployeee will notify the Projict Laboratory Manager. 9. Appropriate diipoiil methods will be followed according to EPA rigulitioni. 6. The compiny Safety Officir will bi coniulcid if necemry, 9,2 SPECIFIC TYPES OF HAZARDOUS MATERIALS 9.2.1 CHEMICAL CAMIHOGENS The 1983-84 ACGIH Threihold limit Vilui manuil litti potintiil chimicil carcinogini in Appendix A (tie Tabli 9-1). The following procedurei ihould bi followid when hindling these lubitincii, 1, All perionnil ihould be properly equipped to eniurt no contict with thi materials. 2. An unbreakable outer container thill bi uiid to triniport chimicil carcinogini, • 3, Scorige veiieli containing chemical carcinogeni thtll be libilid DANCER-CHEMICAL CARCINOGEN. 4, Ditpoial eontalnari will be libeled 11 abovi with thi nini of thi chimicil, 9.2.2 RADIOACTIVE SUBSTANCES 9.2.2.1 Liboritory Procedure! 1. No perion ihould work in the liboritory without wiiring i pirional dosimeter. 2. Impervious glovii will be worn it ill timii, 3, If, in the courti of work, pirional contamination It tuipiccid, a survey with a tuitibli inicrumint ehould be mede iomediicily, Thii ihould bi followid by wiihing ind i further eurvey. Routine preciutioniry lurveyi ihould bi rude periodically, AR30II32 C-45 D-CH64.1/SM-VTB9-1.1 04/09/84 Table 3-1. Chemical Carcinogeni Aerylonitrile 4-Amlnodlphinyl (p-Kenylamlne) Aebeetot Benuidine bit(chloromethyl)ether Chromite ore . Then lubttancit iri known to Chromium VI ceuta cancir in man. All contact Coal tar pitch volatilii ihould be ivoldid. -Nepbthylimini Nickel eulfide roeiting 4-nltrodiphanyl Vinyl chloride Sumeceed of Careinoeenie Potential Amltrol 3,3-Dichlorobentidine Antimony trioxide production Dimethylcarbamyl chloride Arnnic trioxidi production 1,1-Dimithyl hydruine (UDKH) Beneene Dimethyl tulfate Benso(i)pyrine Ethylene dibromide Beryllium Ethylini oxide 1,3-Butadiane Formaldehyde Cadmium oxidi production Rixichlorobucadiine Carbon tetraehloridi Haxamethyl phoiphorimidi Chloroform Hydrasine ChloroMthyl methyl ithir 4,4-Mithylini bis(2-chloroinilini) Chromitii of liid or sine Mithyl hydruine Chryiene Methyl iodide 2-Nltropropine N-Nitroiodimichylimine N-Phenyl-beti-niphthylimini Phenylhydrizini Propane lulfone beti-Propiolictoni Propylenilmini o-Tolidint o-Tolidini Vinyl bromide Vinyl cyclohexine dioxide Source: ACGIR, 1984. AR30II33 O C-46 D-CH84.1/SM-3.7 04/09/84 4. Before a worker leavei the laboratory, handt ihould bi wiihed, and checked with e beta-gamma eurvey miter. Contamination remaining after thorough waehing ehould be reported to the euperviior. 9. to apparatua ihould be wished in the public water-eewage lyitem if it contiini any activity above background when measured with a counter-type lurviy meter. 9.2.2.2 Storata and Handling 1. All radioactive materiale ihould bi etored in specially deeignated areai, 2. All work with thill materials ihould be cerried out in authorised ereae only. ff], ^ 9.2.2.3 Soille 1. Blot up liquid while wearing rubber glovei, 2, All disposable materials contaminated by the ipill and cleaning procees should be pieced in e "contsninsted" traih can, 3, The aree of the epill ind the type of activity (e.g., Iodine- 131) ehould be marked clearly. 3.2.2.4 Haiti Diipoial ' 1. Active liquid waitii ihould be pound into the libeled container! providid. Thiy ihould niver be poured down i itandard drain. '\ » i , 2. Active eolid waitei ind contiminitid matiriili ihould bi placed in traih and libeled "contaminated." 3. Active materiali ind wiitei are to be retained within the radioiiotope laboratory and at spacifiid pointi withi.chin tht i laboratory until proper diaponl, Aft30U3!» 047 D-CH84.1/SM-6.1 04/03/84 6.0 REFERENCES The following references deel with liboritory lafaty and chimicil hesarde. If at any time an employee hai doubts as to what the eafe proceduree are for a laboratory activity, he ehould consult this manual, hie supervieor, or one of these references, 1, Merck Index—provided in ell leboratories. . 2. Material Safety Data Sheeti—available through Joe Plunket, Chemiitry Purchaiing Coordinator. 3. Prudent Preettcee for Handline Haiardoui Chemicili in Liboratoriei by National Academy Pren—available through Charlei Haury, ESE Certified Industrial Hygieniit. 4. Threihold Limit Viluee for Chemical Subitancei ind Physical Aginti in the Work Environment with Intended Changei tor 1963-64 by ACGIH- .•"~\ -available through C. Haury. 3, OSHA reguletione—29 CFR 1910—available in ESE library, 6. EPA regulatloni—RCRA, TSCA. AR30II35 O •"""•" C-48