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### MINIMUM DETECTION LIMIT FOR METHOD 5 EPA Contract No. 68-02-0163 Work Assignment 3-06

September 30, 1996

Prepared For: Mr. Mike Ciolek Emission Characterization Group B EMAO, OAQPS, EPA MO-19 Research Triangle Pk, NC 27711

Prepared By Mr. Roger T. Shigehara

Entropy, Incorporated P.O. Box 12291 Research Triangle Park, NC 27709

### CONTENTS
1.0 Introduction

................................................. 1 2.0 Discussion of Sources of Errors and Associated Studies

.................. 2 2.1 Accuracy of Analytical Balance

.............................. 2 2.2 Precision of Weighing

......................... : ........... 2 2.3 Precision/accuracy of Sample Recovery

......................... 3 3.0 Experimental Design and Results

.................................. 3 3.1 Phase I

............................................... 4 3.2 Phase II

............................................... 8 4.0 QA Report

................................................. 10 5.0 Conclusions.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 

### TABLES Table 1 - Particulate Matter Analysis

................................. 5, 6, 7 Table 2 - Sample Train Blank

.......................................... 9 APPENDIX Raw Data1.0 INTRODUCTION The U.S. Environmental Protection Agency (EPA), Source Characterization Group B (SCGBL Emissions Monitoring and Analysis Division (EMAD), OAQPS requested Entropy, Inc. to determine the minimum particulate catch of EPA Method 5 (40 CFR Part 60, Appendix A, Revised as of July 1, 1995). The Method 5 sampling train consists typically of a stainless steel nozzle, heated glass lined probe and filter holder with a glass mat filter, impingers and a metering system. The particulate matter (PM) is withdrawn"isokinetically from the source and collected on the filter maintained at 120 ± 14°C or other specified temperature. The PM is recovered from the sampling train (from the nozzle tip to the front half of the filter holder) and determined gravimetrically. The basic sample recovery procedure (Section 4.2 of Method 5) is as follows: 

### Filter. Using a pair of tweezers and/or clean disposable surgical gloves, the filter is removed from the filter holder and placed in a sample container. A dry Nylon bristle brush and/or a sharp-edged blade is used to transfer into the jar any PM and/or filter fibers that adhere to the filter holder gasket. 

### Front-Half. PM in the front-half portion of the train, i.e., from nozzle tip to the front half of the filter holder, is recovered using acetone and a Nylon brush. The components in the front-half includes the probe nozzle, Swagelok fitting, probe liner, and front half of the filter holder. These components are first rinsed with acetone and brushed at least three times or until there are no visible particles, followed by a final acetone rinse. 

### Blank. 200 mL of acetone is saved from the wash bottle. Samples are transported to a laboratory for gravimetric analysis. In the laboratory, the basic analytical procedure (Section 4.3 of Method 5) is as follows: Dry 

### Filter. The filter and any loose PM from the sample container are transferred to a tared container, desiccated for 24 hours in a Drierite desiccator. It is then weighed to constant weight as described below. 

### Acetone Rinse andBlank. The contents of the acetone rinse and the acetone blank containers are transferred to tared containers. The sample containers (acetone rinse and filter) are rinsed with a minimal amount of acetone into this tared container. The amount of acetone is weighed to ± O. 1 gram to determine the blank correction. The acetone samples are then evaporated to dryness at ambient temperature and pressure and weighed to constant weight. 

### Constant Weight Procedure. Samples are desiccated for at least 24 hours, removed from the desiccator, and weighed to ±0.1 mg. Samples are then placed back into desiccator for at least 6 hours and weighed again. This procedure is repeated until two successive weighings agree to within ± 0.5 mg. All weighings are done in a laboratory at a temperature of 68 ± 1OOF, relative humidity of s;; 50 percent, and atmospheric pressure. With lower emission standards or limits, sampling times must be increased considerably to obtain the minimum particulate catch of 50 mg, a value commonly used by EPA as a guideline and based on an EPA study. According to Gary McAlister in a memorandum to the file dated September 4, 1974: 1"Data from the Environmental Protection Agency report, "Additional Studies on Obtaining Replicate Particulate Samples from Stationary Sources," by William J. Mitchell, indicate that particulate catches of about 50 mg are adequate to insure an error of no more than 10%. The report contains the results of six separate sampling periods where four simultaneous samples were taken from a single source. The mean of each run was about 50- 60 mg and none of the individual samples varied from the mean by more than 10%. This is clear experimental evidence that particulate catches in the range of 50 mg are large enough to limit inherent errors to less than 10% of total catch weight, but this is the only experimental data available for estimating minimum particulate catch." Because sampling time must be increased beyond the typical 1-3 hours (in some cases, as much as 1 8 hours) to collect about 50 mg at the normal sampling rate of about 0.75 cfm, EPA has requested Entropy to develop and conduct a laboratory experiment to determine the minimum particulate catch that would be accurate to within ± 10% so that sampling times can be shortened.


### 2.0 DISCUSSION OF SOURCES OF ERRORS AND ASSOCIATED STUDIES The sources of errors are: (1) calibration of the analytical balance; (2) sample recovery from the sampling train and sample containers; (3) taring of beakers and filters; (4) desiccation and weighing to constant weight, and (5) contamination of samples. Item (5) and errors associated with isokinetic sampling and source variations are not being considered in this study. 2.1 Accuracy of Analytical Balance Method 5 specifies an analytical balance capable of measuring to within ± 0.1 mg, which presumably is the accuracy specification. With low PM catches, PM is determined from the difference of initial and final weighings. Any inaccuracy (bias) will cancel itself provided that all weighings are done on the same balance and standardized to the same standard (contro!), e.g., the 5-g Class-S standard. The control is necessary to indicate that a gross miscalibration has not occurred between the initial (tare) and final weighings. 2.2 Precision of Weighing The total PM catch is the sum of three masses: (1) filter catch; (2) front-half catch; and (3) acetone blank. Each of these masses is determined from two weighings
-- tare and tare plus sample catch/acetone residue
-- and, thus, a total of six weighings; however, since the filter catch determination requires two initial tares -- filter and beaker, there is a total of seven weighings. The only reference that included repetitive measurements that allowed the calculation of precision was an EPA study by J.W. Brown, "Laboratory Tests for Investigation of Glass Beaker Weight Changes Following Desiccation." The report was undated, but was estimated to be conducted during 1979 by the author. Although this study was designed to investigate beaker weight changes upon exposure to room humidity, results from this study provided precision information of tare weights and 

### 2

### acetone blank weights. In this study, the results of repetitive weighings of six cleaned and desiccated beakers with at least 8 hours of desiccation between weighings were presented. Although the relative humidity exceeded 50% on a number of occasions, the variations from the previous reading were no more than ±0.5 mg. The SO's for the ten weighings ranged from 0.16 to 0.20 mg. EPA Method 5 requires all measurements be made to constant weight, i.e., to ± 0.5 mg for two successive weighings. It is, however, not explicit on which of the two successive weights to use, i.e., the first, the second, or the average. When the average of two successive weights that differed by no more than ±0.5 mg was used, each average had a deviation of no more than ± 0.2 mg. When the second value of two successive weights was used, the maximum deviation was ± 0.4 mg. In this same study, acetone residue from two sources or suppliers were measured. Six 250-mL glass beakers were cleaned and tared, then 250 mL of acetone was added to the beakers, dried, and desiccated to constant weight. In determining the acetone blank residue, the average of the two weights was used. For the six determinations. the Fisher acetone gave an average of 1.4 mg/250 

### mL with a SO of 0.2 mg/250 

### mL; the Burdick and Jackson acetone gave an average of 5.9 mg/250 

### mL with a SO of 0.7 mg/250 

### ml. According to the Method 5 specification, the acetone residue should not exceed**~** 2.0 mg/250 

### ml. 

# v."
..+.l

.... 

### Based on the SO of 0.20 mg, the SO of determining acetone residue (tare and tare/beaker weights) would be estimated at 0.28 mg (square root of the sums of the squares of the SO's for the tare and tare plus sample). The 50's for the residue blanks for the Fisher acetone was 0.20 mg; however, the Burdick and Jackson acetone was 0.68 

### mg. Apparently, the residue 

### from the latter acetone had an effect on the precision; a

# f**j~4** 

### similar effect is seen when weighing samples with sulfuric acid. ,/

# f**~** .tA/I,,(JV 1.:.). 

### Using the SO of 0.20 mg for each weighing, four

# Weighin~OUld give an

# S~f 0.4 mg. The 2u 

### level would then be estimated at 0.8 mg. Thus, the minimum detection limit for a 

### ± 10% accuracy would be 8.0 mg. 2.3 Precision/Accuracy of Sample Recovery 

### EPA conducted various studies or investigations concerning sampling train blanks. the residual amount. The precision and accuracy of sample recovery are highly variable, depending on cleaning techniques before and after sampling. With extensive cleaning, sampling train blanks can be reduced to less than 1.0 to 2.0 mg. However, the EPA studies did not show whether this amount is due to inefficient cleaning before and after testing or due to particulate matter being generated from the probe or brush.
3.0 EXPERIMENTAL DESIGN AND RESULTS The laboratory work was conducted in two phases. The objective of Phase I is to determine the precision of weighing conducted according to EPA Method 5 (40 CFR Part 60, Appendix A, Revised as of July 1, 1995).



### 33.1 Phase I In Phase I, zero, 5 and 1O-mg samples of fly ash were added to tared Teflon bags (a total of 

### 10 bags each), dried and brought to constant weight. The purpose of this step was to give an estimate of the precision of taring and weighing of samples. Then a drop of distilled water (to simulate moisture) and 

### 200 mL of acetone were added to the beakers, evaporated, and brought to constant weight. In addition to giving an estimate of the precision of the weighing of acetone blanks and treated samples, the purpose of this part was to give an estimate of the accuracy of the procedure (i.e., the effect of any reaction between moisture, acetone, and the sample). The results are summarized in Table 1. Negative weights were obtained for those samples with fly ash. There are three possible reasons for these negative weights
-- (1) sample was lost during the addition of the drop of water and acetone; (2) sample was lost during the evaporation of the acetone in the hood; or (3) the water and acetone caused the release of some adsorbed gases on the fly ash. The WAM decided not to investigate the causes for these losses at this time. Using the analysis of the acetone blanks without the addition of fly ash, the SO was determined to be 

### 0.36 mg. Using the 

### 20- level or 

### 0.72, the minimum PM catch for a 

### ± 10% accuracy would be 

### 7.2 mg. In addition to determining acetone blank residues, the analytical balance was checked against a 5-g Class S standard weight to ± 

### 0.1 mg after every five samples or a total of 39 times. The average was 4.9998 and the SO was 

### 0.066 mg. No value deviated by more than 

### 0.1 mg, except once, when the deviation was 

## +0.2 mg. Although a bias of 

### 0.2 mg existed, it did not affect the sample weights because the same balance was used for all weighings and the sample weights depended on differences. A Teflon bag/filter was also weighed as a "control" at the same intervals as the 5-g Class S standard weight. Since the filter was not included in two of the weighings, the control was weighed 

### 37 times. The average was 

### 4.1477 g and the SD was 

### 0.26 mg.

4TABLE 1. PARTICULATE MATTER ANALYSIS O-mg Particulate Matter Teflon BaglFilte Teflon Bag Teflon/Fly TBIFAlFWgt TBIFAIF/A Wgt Acetone Fly 10# Tare Wgt, Ash Wgt, Initial 2 3 Initial 2 3 BlankWgt Ash 9 9 9 9 9 9 9 9 9 mg mg Control 31131 3.6784 4.1475 4.1475 4.1479 4.1478 5-g Class S Std 4.9999 4.9997 4.9998 4.9998 4.9998 111 3.6759 3.6759 4.1361 4.1365 4.1370 4.1368 0.0006 0.6 0.0 212 3.6122 3.6122 4.0755 4.0756 4.0759 4.0757 0.0003 0.3 0.0 313 3.4058 3.4058 3.8700 3.8701 3.8705 3.8705 0.0004 0.4 0.0 (J1 3.4028 3.8677 3.8677 4/4 3.4028 3.8684 3.8688 0.0009 0.9 0.0 5/5 3.7667 3.7667 4.2386 4.2390 4.2395 4.2396 0.0008 0.8 0.0 Control 31131 3.6782 4.1475 4.1475 4.1478 4.1479 4.1470 5-g Class S Std 4.9999 5.0000 4.9998 4.9998 4.9998 4.9998 6/6 3.5287 3.5287 3.9982 3.9983 3.9991 3.9991 0.0008 0.8 0.0 717 3.5457 3.5457 4.0115 4.0116 4.0123 4.0120 0.0006 0.6 0.0 8/8 3.5843 3.5843 4.0535 4.0533 4.0539 4.0535 0.0003 0.3 0.0 9/9 3.1344 3.1344 3.6358 3.6357 3.6386 3.6365 3.6365 0.0008 0.8 0.0 10110 3.6939 3.6939 4.1613 4.1625 4.1628 4.1623 4.1624 -0.0003 -0.3 0.0 SO 0.36TABLE 1. PARTICULATE MATTER ANALYSIS 5-mg Particulate Matter Teflon BaglFilte Teflon Bag TeflonIFly TBIFAIF Wgt TBIFAIF/A Wgt Acetone Fly 10# Tare Wgt, Ash Wgt, Initial 2 3 Initial 2 3 BlankWgt Ash 9 9 9 9 9 9 9 9 9 mg mg Control 31/31 4.1476 4.1477 4.1478 4.1471 4.1473 4.1477 5-g Class S Std 4.9998 4.9998 4.9998 4.9997 4.9998 4.9997 11/11 3.5772 3.5825 4.0554 4.0551 4.0551 4.0552 -0.0001 -0.1 5.3 12112 3.7136 3.7188 4.1936 4.1936 4.1932 4.1931 -0.0004 -0.4 5.2 

### en 13113 3.7080 3.7138 4.1842 4.1846 4.1849 4.1844 0.0002 0.2 5.8 14114 3.5777 3.5830 4.0536 4.0539 4.0537 4.0535 -0.0002 -0.2 5.3 15/15 3.5123 3.5168 3.9882 3.9878 3.9877 3.9877 -0.0003 -0.3 4.5 Control 31/31 4.1478 4.1478 4.1479 4.1479 4.1480 4.1480 4.1478 5-g Class S Std 4.9998 4.9998 4.9998 4.9998 4.9999 4.9998 4.9998 16/16 3.6263 3.6315 4.1020 4.1024 4.1020 4.1018 -0.0003 -0.3 5.2 17/17 3.5375 3.5434 4.0186 4.0186 4.0188 4.0185 0.0000 0.0 5.9 18/18 3.7014 3.7071 4.1786 4.1786 4.1784 4.1782 -0.0003 -0.3 5.7 19119 3.6443 3.6490 4.1198 4.1200 4.1202 4.1197 0.0000 0.0 4.7 20/20 3.6983 3.7037 4.1771 4.1776 4.1778 4.1764 4.1768 -0.0008 -0.8 5.4 SO 0.29TABLE 1. PARTICULATE MAnER ANALYSIS 10-mg Particulate Matter Teflon BaglFilte Teflon Bag TefionIFly TBIFAIF Wgt TBIFAIF/A Wgt Acetone Fly 10# Tare Wgt, Ash Wgt, Initial 

### 2 3 Initial 2 3 BlankWgt Ash 9 9 9 9 9 9 9 9 9 mg mg Control 31131 4.1478 4.1477 4.1472 4.1474 4.1478 4.1479 4.1480 5-g Class S Std 4.9998 4.9997 4.9997 4.9998 4.9997 4.9998 4.9997 

# " 21/21 3.4918 3.5052 3.9678 3.9674 3.9645 3.9646 -0.0031 -3.1 13.4 22122 3.4684 3.4799 3.9481 3.9481 3.9476 3.9473 -0.0007 -0.7 11.5 23123 3.4914 3.5027 3.9739 3.9733 3.9734 3.9722 3.9720 -0.0015 -1.5 11.3 24/24 3.4933 3.5038 3.9745 3.9744 3.9730 3.9731 -0.0014 -1.4 10.5 25/25 3.7587 3.7712 4.2329 4.2318 4.2320 4.2318 4.2315 -0.0002 -0.2 12.5 Control 31131 4.1473 4.1474 4.1478 4.1480 4.1477 4.1480 4.1478 4.1478 5-g Class S Std 4.9997 4.9998 4.9998 4.9998 4.9997 4.9998 4.9998 4.9997 26/26 3.5098 3.5214 3.9905 3.9900 3.9890 3.9889 -0.0013 -1.3 11.6 27/27 3.3998 3.4112 3.8792 3.8788 3.8771 3.8771 -0.0019 -1.9 11.4 28/28 3.2646 3.2753 3.7474 3.7464 3.7467 3.7462 3.7462 -0.0004 -0.4 10.7 29/29 3.5090 3.5193 3.9910 3.9908 3.9905 3.9898 3.9901 -0.0008 -0.8 10.3 30130 3.2644 3.2752 3.7498 3.7498 3.7481 3.7481 -0.0017 -1.7 10.83.2 Phase" The objective of Phase II was to determine the sampling train blank. Phase II was conducted in two parts as follows: 

### 1 . Obtain two sampling trains with a stainless steel nozzle, 8-ft glass-lined probe, filter holder, and rest of sampling train. 2 Before the first runs, clean the components from the probe nozzle to the fronthalf of the filter holder according to LP 5-EPA-7. Discard this rinse. 3. Part 

### 1: Keeping the components from each of the trains together, clean the components from the probe nozzle to the front-half of the filter holder according to LP 5-EPA-7. Use the same components (including Nylon brushes for probe and filter holder recoveries) for six runs each, twelve runs altogether. The purpose of this experiment is to determine the sampling train blank. Note: Use 200 mL acetone for cleanup. If 200 mL is insufficient, establish an adequate volume and use this same volume for all runs. 4. Part 2: Assemble the two sampling trains. Attach a filter at the inlet to the probe nozzle, sample room air at about 0.75 cfm (or at aH@), disassemble, and recover the sample. In this part of the experiment, the impingers will be left out, no leak-check will be performed, and the probe and filter holder will not be heated as they are not pertinent to this project. Use the same procedure as that in Part 1. The purpose of this experiment is to determine whether the sampling train blank increases after sampling room air as past EPA experiments have shown. Conduct the following run times:

• 30 minutes, one run for each train • 60 minutes, one run for each train • 90 minutes, one run for each train • 120 minutes, one run for each train Table 2 summarizes the results. The blank for probe #1 ranged from 2.6 to 5.3 mg for the first six washes, then dropped to 1.2 mg on the seventh wash. Probe #2 gave

, 9.3 mg on the first wash (particulate matter was observed in this wash), 1.0 to 1.3 mg on the next five washes, and 0.5 mg on the seventh. (Note: Although the experimental design called for six washes, a seventh run was made when particulate matter was observed on the first wash for probe #2.) It appears that several washes are necessary in order to decrease the blank values to below 1.0 mg. When room air was sampled, the sampling train blanks ranged from 0.5 to 0.9 mg for probes #1 and #2 for all runs (i.e, 30- to 120-minute runs), with one run (probe #2, 60- minute run) giving 0.1 mg. Thus, it appears that the blank values do not increase after sampling room air.



### 8TABLE 2. SAMPLE TRAIN BLANK Tetlan BaglFilter TB Tare Wgt, 9 Acetone TBIBInk Wgt, 9 BlnkWgt 10# Initial 2 mL Initial 2 mg Control 31/31 3.6804 3.6804 3.6800 3.6803 5-g Class S Std 4.9998 4.9998 4.9998 4.9998 1-1/1 3.6759 3.6760 200 3.6799 3.6803 3.6 1-2/2 3.6122 3.6123 200 3.6181 3.6181 5.3 1-3/3 3.4054 3.4054 200 3.4085 3.4086 2.6 1-414 3.4021 3.4020 200 3.4057 3.4056 3.1 1-5/5 3.7668 3.7670 200 3.7703 3.7703 2.9 Control 31/31 3.6802 3.6804 3.6802 3.6804 5-g Class S Std 4.9998 4.9998 4.9998 4.9997 1-6/6 3.5285 3.5284 200 3.5322 3.5320 3.1 1-7/13 3.7080 3.7080 200 3.7095 3.7099 1.2 Control 31/31 3.6802 3.6803 3.6803 3.6802 5-g Class S Std 4.9998 4.9997 4.9998 4.9997 2-1n 3.5459 3.5458 200 3.583 3.5484 19.3 2-2/8 3.5845 3.5846 200 3.5862 3.5865 1.3 2-3/9 3.1634 3.1634 200 3.1651 3.1652 1.2 2-4/10 3.6937 3.6938 200 3.6952 3.6953 1.0 2-5111 3.5775 3.5773 200 3.5792 3.5792 1.3 Control 31/31 3.6802 3.6801 3.6806 3.6804 5-g Class S Std 4.9998 4.9998 4.9998 4.9998 2-6/12 3.7115 3.7116 200 3.7129 3.7132 1.0 2-7114 3.5777 3.5776 200 3.5787 3.5786 0.5 Control 31/31 3.6803 3.6802 3.6803 3.6805 5-g Class S Std 4.9997 4.9997 4.9993 4.9997 1-30115 3.5117 3.5117 200 3.5127 3.5131 0.7 2-30/16 3.6261 3.6260 200 3.6269 3.6272 0.5 Control 31/31 3.6803 3.6802 3.6802 3.6799 5-g Class S Std 4.9997 4.9997 4.9998 4.9997 1-60/17 3.5369 3.5372 200 3.5379 3.5382 0.5 2-60118 3.7016 3.7018 200 3.7023 3.7023 0.1 1-90/19 3.6448 3.6448 200 3.6458 3.6462 0.7 2-90/20 3.6950 3.6951 200 3.6964 3.6966 0.9 Control 31/31 3.6805 3.6803 3.6802 3.6801 5-g Class S Std 4.9998 4.9998 4.9998 4.9998 1-120/21 3.4868 3.4869 200 3.4879 3.4880 0.6 2-120/22 3.4683 3.4683 200 3.4695 3.4696 0.7 Acetone Blank

# =0.51 mg Example Notation: 1-60/17 means probe #1, 60-minute run, Teflon bag #17.

9

### The results in Table 2 shows that with sufficient cleaning, the sampling train blank values can be reduced to less than 1.0 mg.


### 4.0 QA REPORT 

### The objectives of a QA 

### program were to produce data that are complete, representative, and of known precision and accuracy. The completeness objective was 100%. This objective was met. The representativeness objective did not apply to this study since it deals with the "when," "how," and "how many" measurements that are taken to satisfy the state or federal regulations, which were not addressed in this 

### WA. The goal of this study was to quantify the precision and accuracy for measurement data obtained by following the performance specifications in Method 5. The study met this goal. The performance specifications were as follows:
• Constant weight to ±0.5 mg. • Acetone residue**~** 

### 0.001 wt%. • Relative humidity of laboratory**~** 

### 50%. • Laboratory temperature at 68 ± 10o

### F. • Ambient pressure.


### 5.0 CONCLUSIONS 

### Based on the analysis of the acetone blanks without the addition of fly ash, the SO was determined to be 0.36 mg. Using the 

### 2a level or 0.72, the minimum 

### PM catch for a ± 10% accuracy would be 7.2 mg. This value is based on reducing the number of weighings to two, i.e., weighing the filter and Teflon bag together to obtain the initial tare weight and weighing the acetone rinse/filter catch/Teflon bag for the final weight; the beaker used in the initial tare is also used to evaporate the front-half acetone rinse. The sampling train blank can be reduced to less than 1.0 mg with sufficient cleaning. Sampling room air does not increase the blank value.

10

### APPENDIXFli

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### Entropy, Incorporated Rev. 0: 8/27/96 LDS 5-EPA-1 PARTICULATE MATTER
- PHASE I Page 

# -L of ).. Client Source Characterization Group B/EMAD Analyst

# _.=L=!Ifvu L !

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### Entropy, Incorporated Rev. 0: 8/27/96 LDS 5-EPA-7 PARTICULATE MATTER
- PHASE I .., ")**Page~** of-- Client Source Characterization Group B/EMAD Analyst ( L!h-u 01IA- (<- ) A---

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### Entropy, Incorporated Rev. 0: 8/27/96 LDS 5-EPA-1

Client Source Characterization Group B/EMAD PARTICULATE MATTER
- PHASE I Page 

### I of.J Analyst 

# [Cfu-J r {' "1 (=t;, »A

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### Entropy, Incorporated Rev. 0: 8/27/96 LDS 5-EPA-7 PARTICULATE MATTER
- PHASE I 1 

### 1 Page .:>C of -4. Client Source Characterization Group B/EMAD Analyst 

# Ltvu 'i'f.:

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### MEMORANDUM TO: FROM: RE:

DATE: Roger Shigehara, Entropy, Inc. Cary Eaton, RTI 

## t»**~** 

### Review ofProcedures and Observations During Preparation and Weighing of Phase I Study ofParticulate Matter to Determine Minimum Detection Limit for EPA Method 5 September 20, 1996 RTI procedures for preparing and weighing the Teflon bags for Phase I ofthe study were reviewed. You had noted that the 5 mg and especially the 10 mg loadings had shown loss of weight when the final and initial weight values were compared. Listed below are items that might bear on loss processes. All bags were handled using either stainless steel forceps and/or dust-free plastic gloves. Describe the pouring ofacetone into the Teflon bag. Fisher A949-4 HPLC grade acetone, lot 

### # 963519, with a stated residue of0.3 ppm was used in all phases ofthe experiments. To add the acetone to the Teflon bags, it was first poured from the bottle directly into a 250 

### mL capacity polyethylene graduated cylinder having graduations in 2 mL 

### intervals. 200 mL 

### was carefully poured from the cylinder into the Teflon bag which contained either 0, app. 5 mg, or app. 10 mg offlyash. No splashing ofacetone or flyash up the walls or out ofthe bag was observed. Describe the appearance ofthe flyash in the acetone. After the 200 

### mL ofacetone was in the Teflon bag, the flyash became dispersed throughout the solution and was barely visible. There was no "skim" offlyash visible on the surface ofthe acetone. Larger flyash particles could be seen "floating" around in the liquid. Describe the drying process. The Teflon bags were placed in clean polyethylene beakers to hold them steady while they were in the laboratory hood(s) which operated at a face velocity of approximately 100 feet per minute. Dueto power failures during and following the hurricane, at least one set ofthe bags had to be moved from one hood to another to complete the acetone/water evaporation process. Bags were placed in a large, covered, polyethylene box during transport to keep them clean and prevent entry ofambient dusts. The flyash tended to follow the acetone down as evaporation occurred. Little flyash was observed on the sides ofthe Teflon bag; most ofit deposited on the bottom surface ofthe bag. It 

### was found that the bags could be removed from the supporting beakers without falling over in the flowing air. This removed the insulating effect ofthe beaker and sped up the evaporation process.

### MEMORANDUM TO: FROM: RE:

DATE: Roger Shigehara, Entropy, Inc. Cary Eaton, RTI 

# td Le Results ofPhase II ofStudy to Determine Minimum Detection Limit for EPA Method 

### 5 October 7, 1996 Results from our laboratory experiments to determine the minimum detection limit for EPA Method 5 are attached as completed tables ofinformation. The quality assurance plan, as revised for Group B, was followed. The enclosed data sheets are arranged as follows: 1. LDS 5-EPA-8 data sheets. There are four (4) sheets. Pages 1 of4, 2 of4, and the first two entries on page 3 of4, record the weighings for dried rinsate from inlets and probes # 1 and #2 which were rinsed with acetone and brushed out. As specified, a separate brush was used for each probe was used throughout Phase II. The total acetone rinse volume was approximately 200 mL. 

### Seven rinses were made ofeach probe in succession. They are labeled I-lstl1 corresponding to probe #1, 1st rinse, Teflon beaker #1. You asked that 7 runs be made so that the first rinse (i.e., 1-1 stl1 and 2-1 st/7) ofeach probe could be considered an initial cleaning and the data discarded. Thus the statistics would be based on runs 2 through 7. 2. LDS 5-EPA-8 data sheets. Pages 3 of4 and 4 of4 record the weighings for dried rinsate from inlets and probes and the first halfofthe filter holder for probes # 1 and #2 which were used in an actual operating sampling system. They are labeled as 

### 1-30/15, etc., corresponding to system (probe) # 1,30 minutes run time @ 0.75 cfin, and Teflon beaker # 15. The total acetone rinse was approximately 180 mL. 

### 3. FDS 5-EPA-6 data sheets. There are eight (8) sheets. These sheets record the clock time and the readings ofthe dry gas meter and gauges for the Method 5 systems. The # 1 filter, inlet, probe, and filter holder were used with sampling box #N20; the #2 filter, inlet, probe, and filter holder were used with sampling box #N36. Readings were taken at 5- minute intervals, as specified. The weighing laboratory temperature and humidity were always within the specified range. A graph ofthe conditions in Room 509H ofthe RTI Animal Care Facility is enclosed for your information. The top line corresponds to temperature (degrees F); it is always very close to 74. The bottom line corresponds to percent relative humidity. None ofthe spikes above 50% RH occurred during the time weighings were actually being conducted. They correspond to system upsets due to the hurricane, etc. and are usually very brief The barometric pressure was not always recorded. 

### It was generally around 756 to 758 mm mercury. Ifthese data are needed they can be retrieved from the weather bureau records at the airport at a later time.

### Entropy, Incorporated Rev. 0: 8/27/96 LDS 5-EPA-8 SAMPLE TRAIN BLANK
- PHASE II Page / of 

# !:L.
Client Source Characterization Group B/EMAD J • / Analyst 

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