9130194: SS12-1 SUMMARY SHEET 12 Inorganic Lead

Run #1 Run #2 Run #3 Avg ClientlPlant Name FDS 5 Job No. FDS 5 Sampling Location FDS 5 Run ID # FDS 5

Test Date FDS 5 Run Start Time FDS 5 Run Finish Time FDS 5 Net Traverse Points FDS 1 Traverse Matrix (Rectangular) FDS 1 Net Run Time, min 8 FDS 5

Nozzle Diameter, in. D" FDS 5 Dry Gas Meter Calibration Factor Y CDS 5 Average AH (orifice meter), in. H,O AH FDS 5

Barometric Pressure, in. Hg 'b FDS 5 Stack Static Pressure, in. H,O PQ FDS 5 Absolute Stack Pressure, in. Hg PS ss 5 Average Stack Temperature, OF ts FDS 5 Average Absolute Stack Temperature, R TS FDS 5

Carbon Dioxide, % dry %CO, FDS 3 Oxygen, % dry %O, FDS3 . Carbon Monoxide + Nitrogen, % dry %KO+ N,) FDS 3 Dry Molecular Weight, Ib/lb-mole Md FDS 3

Average DGM Temperature, OF t m FDS 5 Volume of Metered Gas Sample, dcf Vm FDS 5 Volume of Metered Gas Sample, dscf 'm(std) ss 5

Volume Water Condensed, mL "lc FDS 5 Volume of Water Vapor, scf 'w(std) ss 5 Moisture Content, fraction Bws ss 5 Pitot Tube Coefficient CP CDS 2a Average Velocity Pressure, in. H,O AP FDS 5 Average [(tSi +460) AP]'/~ [TSi API"~ FDS 5 Velocity, ftlsec VS ss 5

Stack Area, ft2 A FDS 1 Volumetric Flow Rate, dscfh Qsd ss 5 Volumetric Flow Rate, wscfh QSW ss 5 lsokinetic Sampling Rate, % %I ss 5

Pb Concentration from Cal Curve, pg CC LDS 12 Sample Volume, mL VS LDS 12 Aliquot Volume, mL va LDS 12 Dilution Factor, if applicable F Total Pb in Sample, pg "Pb ss 12 Pb Concentration, Ib/dscf cPb ss 12 Post-test Calibration Checks Temperature and Barometer CDS 2d Metering System CDS 5

CiPb Cpb= 2.205 x - Vrn(std) 9130194: F12-1 FIELD PROCEDURE 12 Inorganic Lead Note: The sampling procedure is the same as that in FP 5, except for the following (use FDS 5 for the sampling data). A. Sampling Drain the 0.1 N HNO, through the outlet arm of each impinger into Container 1. Use a filter with a lot assay for lead; the No. 4. Repeat this operation a second filter need not be weighed. time; inspect the impingers for any 2. Assemble the train as shown in Figure F12- abnormal conditions. 1. Use impingers rather than an alternative Wipe the socket joints of the glassware condenser system. connecting the impingers free of silicone 3. In each of the first two impingers, place grease and rinse each piece of 100 mL 0.1 N HNO, (rather than water). glassware twice with 0.1 N HNO,; transfer this rinse into Container No. 4. 4. Use as sample storage containers 1 L JDo not rinse or brush the alass- fritted borosilicate glass bottles with screw-cap filter suooort.) liners that are either rubber-backed Teflon or leak-free and resistant to chemical attack by Mark the height of the fluid level and 0.1 N HNO,. label and identify the container.

6. Sample Recovery C. Alternatives 1. The sample recovery procedure for 1. Simultaneous Determination of Particulate Containers 1, 2, and 3 is the same as that and Lead Emissions. Method 5 (FF? 5) may in FP 5, except for the following: be used to simultaneously determine Pb provided that: a. Use 0.1 N HNO, as the rinse rather than water; save a blank of the acid. a. Acetone is used to remove particulate from the probe and inside of the filter b. Use glass rather than a polyethylene holder as specified by Method 5. funnel. b. 0.1 N HNO, is used in the impingers. 2. Container No. 4 (Impingers). Several sample containers may be used. Clean each C. A glass fiber filter with a low Pb of the first three impingers and connecting background is used. glassware in the following manner: d. The entire train contents, including the a. Wipe the impinger ball joints free of impingers, are treated and analyzed for silicone grease, and cap the joints. Pb. b. Rotate and agitate each impinger, so that 2. Filter Location. A filter may be used the impinger contents might serve as a between the third and fourth impingers rinse solution. provided that the filter is included for analysis for Pb. C. Remove the outlet ball joint cap, and drain the contents through this opening 3. In-Stack Filter. An in-stack filter may be into a 500-mL graduated cylinder; do not used provided that: separate the impinger parts (inner and a. A glass-lined probe and at least two outer tubes) during this operation. impingers, each containing 100 mL Measure the liquid volume to within 0.1 N HNO,, are used after the in-stack 2 mL. Alternatively, weigh the liquid to filter. within 0.5 g. Note any color or film observed in the impinger catch. b. The probe and impinger contents are recovered and analyzed for Pb. d. Transfer the contents to Container No. 4. (Recover sample from the nozzle with e. Measure and record the total amount of acetone if a particulate analysis is to be 0.1 N HNO, used for rinsing in this step made.) and in step f below. Pour about 30 mL 0.1 N HNO, into each of the first three impingers and agitate the impingers. Figure Fl2-1. Inorganic Lead Sampling Train. 9/30/94:L12-1 LABORATORY PROCEDURE 12 Inorganic Lead

A. Reagent heparation b. Then transfer the residue from Containers No. 2 and No. 4 to the 1. Nitric Acid, 0.1 N. Dilute 6.5 mL conc. HNO, 125-mL Erlenmeyer flask that contains to 1 L with water. the filter using rubber policeman and 2. HNO,, 6 N. Dilute 390 mL conc. HNO, to 1 L 10 mL 50% HNO, for every 100 mg of with water. sample collected in the train or a minimum of 30 mL 50% HNO,, 3. HNO,, 50% (vlv). Dilute 500 mL conc. HNO, whichever is larger. to 1 L with water. C. Place the Erlenmeyer flask on a hot 4. Stock Lead Standard Solution, 1000 pg plate, and heat with periodic stirring for Pb/mL. Dissolve 0.1 598 g Pb(NO,), in about 30 min at just below the boiling point. 60 rnL water, add 2 mL conc. HNO,, and If the sample volume falls below 15 mL, dilute to 100 mL with water. add more 50% HNO,. Add 10 mL 3% 5. Working Lead Standards. Pipet 0.0, 1.0, H,02, and continue heating for 10 min. 2.0, 3.0, 4.0, and 5.0 mL stock lead Add 50 mL hot (8OOC) water, and heat standard solution into 250-mL volumetric for 20 min. Remove the flask from the flasks. Add 5 mL conc. HNO, to each flask, hot plate, and allow to cool. and dilute to volume with water. These d. Filter the sample through a Millipore working standards contain 0.0,4.0, 8.0, membrane filter, or equivalent, and 12.0, 16.0, and 20.0 pg Pb/mL, respectively. transfer the filtrate to a 250-mL Prepare, as needed, additional standards at volumetric flask. Dilute to volume with other concentrations in a similar manner. water. 6. Hydrogen Peroxide, 3%. Dilute 10 mL 30% 4. Filter Blank H202to 100 mL with water. a. Take two filters from each lot of filters / 6. Sample Reparation used in the sampling train. 1. Container No. 1 (Filter) b. Cut each filter into strips, and place each filter in a separate 125-mL a. Cut the filter into strips and transfer the Erlenmeyer flask. strips and all loose particulate matter into a 125-mL Erlenmeyer flask. If the c. Add 15 mL 50% HNO,, and treat as estimated particulate catch is greater described in step B using 10 mL than 800 mg, use a 250-mL flask (see 3% H202and 50 mL hot water. Filter step B3). and dilute to a total volume of 100 mL with water. b. Rinse the petri dish with 10 mL 50% HNO, to insure a quantitative 5. HNO, Blank transfer, and add to the flask. a. Take the entire 200 mL O.l.N HNO, to 2. Containers No. 2 and No. 4 (Probe and dryness on a steam bath. Impingers) b. Add 15 mL 50% HNO,, and treat as a. Check the liquid level in Containers No. 2 described in section B3 using 10 mL and No. 4, and determine and record 3% H,O, and 50 mL hot water. Dilute loss (if any) on LDS 12. to a total volume of 100 mL with water. b. Combine the contents of Containers C. Analysis No. 2 and No. 4, and take to dryness on a hot plate. 1. Calibrate the spectrophotometer as follows: 3. Sample Extraction for Lead a. Measure the absorbance of the standard solutions using the instrument settings a. Based on the approximate stack gas recommended by the spectrophotometer particulate concentration and the total manufacturer. Repeat until good volume of stack gas sampled, estimate agreement ( 5 3%) is obtained the total weight of particulate sample * between two consecutive readings. collected. 9/30/94:L12-2 b. Plot the absorbance (y-axis) versus D. Check for Matrix Effects concentration in pg PblmL (x-axis). Check at least one sample from each source Draw or compute a straight line through using the Method of Additions as follows: the linear portion of the curve. Do not force the calibration curve through zero, 1. Add or spike an equal volume of standard but if the curve does not pass through solution to an aliquot of the sample solution, the origin or s k0.003 absorbance then measure the absorbance of the resulting units, check for incorrectly prepared solution and the absorbance of an aliquot of standards and for curvature in the unspiked sample. calibration curve. 2. Calculate the Pb concentration C, in pg/mL c. To determine stability of the calibration of the sample solution. Volume corrections curve, run a blank and a standard after are not required if the solutions as analyzed every five samples, and recalibrate, as are made to the same final volume. necessary. Therefore, C, and C, represent Pb concentrations before dilutions. 2. Lead Determination 3. Method of Additions procedures described a. Determine the absorbance for each on pages 9-4 and 9-5 of the section entitled source sample, the filter blank, and "General Information" of the Perkin Elmer 0.1 N HNO, blank. Analyze each sample Corporation Atomic Absorption three times in this manner. Make Spectrophotometry Manual, No. 303-01 52 appropriate dilutions, as required, to may also be used. bring all sample Pb concentrations into the linear absorbance range of the 4. If the results of the Method of Additions spectrophotometer. procedure used on the single source sample is > *5% of the value obtained by'the b. If the Pb concentration of a sample is at routine atomic absorption analysis, then the low end of the calibration curve and reanalyze all samples from thesource using high accuracy is required, take the the Method of Additions procedure. sample to dryness on a hot plate and dissolve the residue in the appropriate volume of water to bring it into the optimum range of the calibration curve. c. If high concentrations of copper are present, analyze the samples at 283.3 nm. 3. Container No. 3 (Silica Gel). If not done in the field, weigh the spent silica gel (or silica gel plus impinger) to the nearest 0.5 g. 9130194: LD12-1 LABORATORY DATA SHEET 12 Inorganic Lead

Client/Plant Name Job # Datenime

Spectrophotometer ID# Wavelength nm Analyst

Working Standards (pg Pb/mL) 0.0 4 .O 8 .O 12.0 16.0 20.0

Absorbance 1, A, Absorbance 2, A,

Q/C Chk (A1 - A,)/A, (S*3%) (J)

Plot of calibration curve attached? Curve s k0.003 absorbance units of the origin?.

Note: If copper is present in high concentrations, use 283.3 nm to analyze the samples.

Volume (mL) Absorbance,'A (OD)

Run these calibration checks (blank and standard) every 5 samples. *+Subtract filter and 0.1 N HNO, blanks from average absorbance. Dilutions?

Matrix Check Spike: C, = Pb concentration c, = c, ___4 C, = Pb standard concentration, pg/mL =

4 - As A, i= Absorbance, unspiked sample A = Ahcnrhanrn cniknrl camnln ,.t I I"_". I"..""I WF.'."" W".. y." -C, s f 0.05 unspiked concentration?

Note: If the 5% specification is not met, run all samples using Method of Addition.

QA/QC Check Completeness - Legibility - Accuracy - Specifications- Reasonableness -

Checked by: Personnel (SignaturelDate) Team Leader (Signature/Date) 9/30/94: LD12a-1 LABORATORY DATA SHEET 12a Matrix Analysis

Client/Plant Name Job #

Daterrime Analyst

Note: This is a generic form for the Methods of Addition. Add the proper units. Make any adjustments as appropriate.

Q.A/QC Check Completeness - Legibility - Accuracy - Specifications Reasonableness -

Checked by: Personnel (SignaturelDate) Team Leader (Signature/Date)