## EVALUATION OF METHOD 0050

## FOR HmROGEN CHLORIDE TASK C STUDIES OF SAMPLING ATMOSPHERES CONTAlNINGMMONIUM CHLORlDE

Draft Internal Report

Prepared for: Robert 

### G.Fuerst Atmospheric Research and Exposure

, . 

### Assessment Laboratory Methods Research and Development Division I 

### . Source Methods Research Branch . % 

### U.S. Environmental Protection Agency Research Triangle Park, North Carolina 27711

September 30, 1993


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# q1 /DCN NO.: 93-275-065-52-15 Radian No.: 275-065-52 EPA NO.: 68-Dl-0010

EVALUATION OF METHOD 0050 FOR HYDROGEN CHLORIDE TASK C STUDIES OF SAMPLING ATMOSPHERES CONTAINING AMMONIUM CHLORIDE

Draft Internal Report Prepared for: Robert G. Fuerst Atmospheric Research and Exposure Assessment Laboratory Methods Research and Development Division Source Methods Research Branch U.S. Environmental Protection Agency Research Triangle Park, North Carolina 27711
Prepared by: Joette Steger

P.O. Box 13000 Research Triangle Park, North Carolina 27709
September 30, 1993DISCLAIMER
This document is intendedfor internal Agency use only. Mention of trade names or commercialproducts does not consititute endorsement or recommendationfor use.EXECUTIVE SUMMARY
A key issue with methods used to measure hydrogen chloride (HC1) is a positive bias on sources containing ammonium chloride (NH,Cl). The objective of the study was to experimentally test Methods 0050 and 26A by spiking an NH,C1 aerosol into the sampling train to identify the source of the bias. This objective was accomplished by dynamically spiking 15 trains at two temperatures in the laboratory with NH4C1,two levels of HC1, and two levels of moisture. Twelve of the 15 trains were spiked with NH4C1at 250°F (121°C). Five of these trains were spiked at low levels of moisture. One of these five trains used a Teflon@ instead of quartz filter and one train was spiked with an NH,C1 solution prepared in methanol. The other seven trains were spiked at high levels of moisture. Three of these seven trains were also spiked with HCl. Finally, three of the 15 trains were spiked with NH4C1at 400°F (205°C).
Under all conditions tested, the presence of NH4C1in the sampled gas introduced a positive bias into the HC1 measurement. This positive bias resulted from the NH4C1 penetrating the filter and dissociating in the 0.1N H,S04 solution. A significant positive bias in the HCl measurement was observed even when the amount of NH4C1spiked was 

### as low as 2.44 ppmv. The positive bias in the HC1 measurement increased when the temperatures of the probe and filter increased. The positive bias in the HCl measurement may also be affected by the quantity of moisture in the sampled stream, increasing as the amount of moisture in the sampled stream decreases. The positive bias in the HCl measurement appears to be independent of the type of filter used in the sample train. When both HC1 and NH,CI are present in the sampled gas, a synergistic affect occurs, increasing the positive bias in the HC1 measurement. It may be possible to correct for the positive bias in the HC1 measurement by analyzing for ammonium ion and assuming the sole source of the ammonium ion is disassociated NH4C1. Finally, NH4Clshould be listed as an interferant in the method and the method should include adiscussion of the trade off between filter and probe temperature and the negative and positive biases that will be introduced under various scenarios.TABLE OF CONTENTS Page



## ... Disclaimer 

## ......................................................in ExecutiveSumrnary 

## ................................................. iv Tables 

## ..........................................................vii



# . .. Figures 

## .......................................................... vlii 1.0 INTRODUCTION.. 

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## . . . . . . 1-4 2.0 EXPERIMENTAL PROCEDURE 

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## . . 2-1 2.2 Method 0050 Sampling Train


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# . .. . . . .. .. . . . .. . 2-6 2.4 Preparation of Reference Samples 

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## . . 2-11 3.0 RESULTS AND DISCUSSION 

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# .. . . . . 3-1 3.1 Baseline Experiments 

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# . . . . .. . 3-6 3.4 Hydrogen Chloride Experiments 

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# . . 3-7 3.5 Filter Experiment 

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# .. . 3-8 3.6 Aerosol Spiking Solvent Experiment


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## . .3-11 4.0 CONCLUSIONS


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# .. . . . 4-1 5.0 REFERENCES 

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## . . . . . . APPENDICES A TRAIN DATA OPERATING DATA SHEETS B TRAIN RECOVERY DATA SHEETS C ANALYSIS DATA SHEETSLIST OF TABLES Page Summary of Train Parameters and the Amount of Ammonium Chloride and HCl Spiked


### .............................................. 2-2 Flow Rate. Purge Time. and Amount of HCl Spiked into each Reference Sample 

## .................................................... 2-5 Sample Train Reagent Type and Quantity by Impinger 

## ................. 2-8 Summary of Spiked Train Experiments Sampling at 0.76 CFM for Two Hours 

## ..................................................... 3-2 Distribution of Ammonium Chloride in Each Train Fraction 

## ............ 3-3 Summary of Measured HCl Bias for Each Test Condition


### .............. 3-4 Summary of Analysis of Variance Results


### ........................... 3-5 Spiked HCl Recoveries Corrected Based on Ammonium Ion Analysis 

## ...... 3-9 Summary of Reference Samples Prepared Using 262 ppmv HCl Gas


### ......3-10

viiLIST OF FIGURES 

### Page 2-1 Mass Flow Controller and Impinger Set-up Used for Reference Samples H-1t0H-3 

## ................................................. 2-4



## .............. 2-2 Method 0050 Train Used for Ammonium Chloride Studies 

### 2-7 2-3 High Pressure Aerosol Spiking System Used to Dynamically Spike Ammonium Chloride into a Method 0050 Train 

## ...................... 2-9

viii

### 1.0 

### INTRODUCTION
The U.S. EPA and Radian designed experiments to evaluate the positive bias of Method 0050 and Method 26A when sampling stack atmospheres containing ammonium chloride. The experimental design was successful in isolating the problem and identifying the cause of the bias when sampling atmospheres containing ammonium chloride.

The EPA reference method used for collecting hydrogen chloride (HC1) and chlorine (Cl,) in stack gas emissions from hazardous waste incinerators, municipal waste combustors, and boilers and industrial furnaces is SW-846 Method 0050. EPA SW-846 Method 0050 was developed to determine emission rates of hydrogen halides 

### (HX) and halogens 

### (X,) from stationary sources. The New Source Performance Standards (NSPS) sampling procedure for HX is 40 

### CFR Part 60, Method 26A. Method 26A is essentially the same as the sampling procedures in Method 0050.
In Method 0050, gaseous and particulate pollutants are withdrawn isokinetically from the stationary source and are collected in a cyclone (optional), on a filter, and in absorbing solutions. The cyclone is used to collect liquid droplets and particulate matter. The cyclone is usually included in the sampling train to protect the filter when high levels of moisture and high levels of particulate matter are present. However, the cyclone may be removed from the train when the source emissions do not contain liquid droplets. It is important to protect the filter from high moisture because a wet filter will create a larger pressure drop in the train. The filter prevents halide salts from entering the impingers and biasing the results. The absorbing solutions consist of two impingers containing 0.1 N sulfuric acid (H,S04) and two impingers containing 0.1 

### N sodium hydroxide (NaOH).During HC1/C12 sampling, it is critical to maintain all surfaces between the stationary source wall and the filter at or above stack temperatures. Unheated sampling lines or cold spots in the sampling system can result in the deposition of water as condensate and possibly other materials on these cooled surfaces which may result in anomalous results.

In a previous study,' the overall recommendations for collecting and analyzing HCl under either dry or humid conditions were: Operate the collection system at high (170°C [33g°F]) temperatures; and Use care to avoid the presence of moisture droplets in delivering HC1 gases to impingers.
No clear preference for glass or Teflon@ probe composition could be discerned from experimental data, so no recommendation can be made for choosing one over the other. Glass probes were used in this study.
SW-846 Method 0050 is particularly well-suited for sampling at stationary sources that emit acid particulate matter and acidic vapor and that are controlled by wet scrubbers because the method collects acid aerosols, particulate matter, and gas phase 

### HX. The acid particulate matter usually consists of HX dissolved in water droplets present as an aerosol. Other particulate matter, including halide salts, is collected on the filter. Acidic (0.1 N H,SO,) and alkaline (0.1 N NaOH) absorbing solutions are used to collect HX and X2,respectively. In the acidic absorbing solution, HX is solubilized to form halide ions (X-). Halogen gases, which have very low solubility in the acidic absorbing solution, pass through the acidic solution to the alkaline solution, where they are hydrolyzed to form a proton (H'), a X-, and a hypohalous acid (HXO). Ion chromatography (IC) is used to perform the analysis for X' in the absorbing solutions. The acidic and alkaline solutions are analyzed separately. The method is applicable tothe determination of HC1, hydrogen bromide (HBr), hydrogen fluoride (HF), chlorine (Cl,), and bromine (Br2). Questions have been raised about potential problems with the measurement of HC1 during compliance testing at cement kilns firing municipal solid waste due to interference by NH4C1. Ammonium chloride and other ammonium salts can be formed by the combination of acid gases, such as HC1, present in emissions with available ammonia. Ammonia is contained in raw materials which are used in the production of cement, and ammonia is also a frequent combustion by-product. Ammonia may be present in emissions as a result of the injection of ammonia into a combustor for the control of nitrogen oxide. Visible plumes of NH,C1 have been observed from cement kilns, raising the possibility that the chloride ions detected in the impinger solution for either Method 0050 or Method 26A are the result of the dissociation of NH4C1,rather than formation of HC1.
Ammonium chloride can exist in saturated pure mixtures as a molecular gas in equilibrium with its components (ammonia and chloride). However, NH4C1has a strong tendency to dissociate at temperatures from 554°F to 626"~.' Because of this strong tendency to dissociate, NH4Cl is not thought to exist as a molecule in the gas phase, especially in unsaturated mixt~res.~ Though stack temperatures in many cement kilns and municipal waste combustors are lower (approximately 300°F), the concentration of ammonium and chloride in the stack is much lower (<10ppm HC1 and < 10 ppm ammonia), so the conditions favor dissociation2. The implication is that NH,C1 is not found in the stack gas in the gas phase. At ambient atmospheric conditions (6g°F), gaseous NH,C1 and particulate matter associated with NH,C1 have been detected at concentrations up to 5 micrograms per cubic meter.4Gaseous NH4Cl has not been found to be an interferant with continuous emission monitoring systems (CEMS). Solid NH4Cl collected on filters during Method 0050 or Method 26A sampling procedures should not skew chloride measurements since solid NH4C1sublimes at 664°F while the filter holder temperature in Method 0050 and Method 26A is maintained at stack conditions (300°F [149"C] or higher). EPA Laboratory studies have shown that NH4Cl condensed onto particulate matter which is caught by the filter will have a high vapor pressure at stack temperatures. Pulling stack gas through the filter can allow NH4C1to evaporate and pass through the filter to collect in the impinger solutions. However, an attempt to correlate ammonium ion concentrations in impinger solutions with chloride ions has not demonstrated a consistent relationship between the two ions. Ammonium chloride is therefore not the only source of chloride ions. Considering the physical data for NH,Cl which indicate complete disassociation into ammonia and HC1, it is not likely that a significant percentage of the chloride which is detected at cement kilns with Method 0050 or Method 26A originates from gaseous NH4Clin the stack.
A key issue with methods used to measure HC1 is a positive bias on sources containing ammonium chloride. Both Method 0050 and Method 26A show the positive bias and therefore may provide accurate results on sources emitting ammonium chloride.
1.2 Obiectives
This report of HCl and chloride sampling and analysis methods presents experimental results that address questions raised about the effect of ammonium chloride. The questions include:
Does ammonium chloride penetrate the filter? How can interference from ammonium chloride be mitigated?The objective of the study was to experimentally test Method 

### 0050 by spiking ammonium chloride into the sample train under various conditions to confirm the observed bias when ammonium chloride is present and to determine the cause of any bias observed.2.0 EXPERIMENTAL PROCEDURE


### This section describes the experimental test design and procedures used in this study, including a description of the Method 0050 

### train and analytical procedures.
2.1 Ex~erimental Test Desi~n
A 

### total of 15 

### trains were dynamically spiked in the laboratory with ammonium chloride aerosol, two levels 

### of HC1 ranging from 0 

### to 21 

### ppmv, and two levels of moisture 

# - nominally 4 and 20 

### percent. Quartz filters were used for 14 

### of the trains and for the remaining train a Teflon@-coated filter was used. Fourteen of the trains were spiked with an aqueous ammonium chloride solution and one of the trains (M-17) was 

### spiked with an ammonium chloride solution prepared in methanol. The probe and filter temperature, filter type, moisture added, and flow rate, generated concentration, and total amount of ammonium chloride and HC1 spiked for each run are provided in Table 2-1.


### Four of the 14 

### trains with quartz filters were spiked with aqueous ammonium chloride and added moisture while being operated at 121°C (250°F). 

### These experiments were designed to determine the effect of ammonium chloride on the chloride levels measured in the sulfuric acid collection solutions when the train was operated using the conditions recommended in the method. Triplicate trains with quartz filters were spiked with aqueous ammonium chloride and moisture while being operated at 200°C (400°F). 

### These experiments were designed to determine the effect of train operating temperature on the amount of ammonium chloride that breaks through the filter.Table 2-1 Summary of Train Parameters and the Amount of Ammonium Chloride and HCI Spiked



## " Capillary spiking nozzle plugged during run. Run ID and Date (1993) C-1 917 C-2 917 C-3 918 C-4 9/10 C-5 9/10 C-6 9/10 C-6W 9/13 D-7 9/13 D-8 9/14 C-9 9/16 C-10 9/16 C-11 9/17 D-15 9/23 D-16 9/23 M-17 9/23 Probe Temp.

("C)

124 126 128 121 194 207 210 125 123 123 124 121 123 121 122 Filter Quartz Quartz Quartz Quartz Quartz Quartz Quartz Quartz Teflon@ Quartz Quartz Quartz Quartz Quartz Quartz Moisture (O/O

15.5 16.2 18.9 22.0 21.4 22.4 21.8

4.18 4.48 17.9 18.7 19.2 4.04 4.03 4.63 Ammonium mL

60

70 65 60 60 60 60 60 60 62 60 50 60 85 mL/min 0 0 0 0 0 0 0 0 0 1780 1768 1753 0 0 0 Chloride
ppmv

29.5

2.44 34.2 31.8 29.1 29.1 29.4 29.1 29.1 29.1 30.1 29.1 24.4 29.1 41.2 Spiked Total mg 180

15.0 210 195 180 180 180 180 180 180 186 180 150 180 255 HCI Spiked
ppmv

0 0 0 0 0 0 0 0 0
I 21.6 2 1.5 21.3

0 0 0 Total mg 0 0 0 0 0 0 0 0 0 91.0 90.4 89.6

0 0 0Triplicate trains with quartz filters were spiked with aqueous ammonium chloride and no added moisture while being operated at 121°C (250°F). These experiments were designed to determine the effect of moisture on the amount of ammonium chloride that breaks through the filter.
One train with a Teflon@-coated filter was spiked with aqueous ammonium chloride and no added moisture while being operated at 121°C (250°F). This experiment was designed to determine the effect of the filter material on the amount of ammonium chloride that breaks through the filter. Triplicate trains with quartz filters were spiked with aqueous ammonium chloride and HC1 while operating the train.at 121°C(250°F) where less ammonium chloride broke through. These experiments were designed to determine the bias in the HC1 measurement introduced by the presence of ammonium chloride.
One train with a quartz filter was spiked with ammonium chloride in methanol solution and no added moisture while being operated at 121°C (250°F). This experiment was designed to determine the effect of the aerosol spiking solution solvent on the amount of ammonium chloride that broke through the filter.
Before the start of each run where HCl was spiked, a reference sample was generated, as shown in Figure 2-1, by purging the spike gas directly into a series of two impingers containing 100mL of 0.1 

### N H,SO,. Flow rates and collection times for the reference samples are provided in Table 2-2. The reference samples were designed to confirm the concentration of HC1 in the supply cylinder and the amount of HCl dynamically spiked into the sample train.Uqukl NHdCI Splko In Teflon Glear GI-r Probo Too Tea Unor To

I 1 1 S~~DIO 

## II \ Hoatod Probo

Flow Controller
I 

## Ir I Sway Vahm

sway Valvo Purgeto Vent

HCI Cyllndw Sbarn Ha Gsr & NH4CI In Injocbdat Sam. Point

Mlnl Buck flow Calibrator

To Vent

f

Figure 2-1. Mass Flow Controller and Impinger Set-up Used for Reference Samples H1 to H-3.Table 2-2 Flow Rate, Purge Time, and Amount HCl Spiked into each Reference Sample2.2 Method 0050 Samolin~ Train
The Method 0050 sampling train was assembled as shown in Figure 2-2 from all glass components and charged with reagents as described in Table 2-3. All of the trains were spiked with ammonium chloride aerosol as described in Section 2.3. For Runs C-9 through C-11, a tee connector was used between the nozzle and probe to introduce the gaseous 262 ppmv hydrogen chloride (HC1) in nitrogen. The flow rate of the HC1 gas was controlled with a Tylan@ mass flow controller for Runs C-9 through C-11. Gas flow rate was confirmed using a mini-Buck calibrator.
A beaker of water on a hot plate was used to generate steam for Runs C-1 through C-6W and Runs C-9 through C-11. The nozzle was placed directly over the beaker. Room air conditioned, by adding steam, was pulled through the train at approximately 0.75 ft3/minute for two hours. For all of the runs, the probe and filter hot box were heated to 121°C (250°F) or 200°C (400°F) before starting the purge gas through the train.
2.3 Aerosol Soiking System
The ammonium chloride was spiked into the train as an aerosol using a high pressure aerosol injection system developed under Work Assignment 32 of EPA Contract No. 68-Dl-0010for dynamically spiking aryl amines into a Modified Method 5 sample train. The high pressure aerosol injection system was further evaluated and refined for spiking an aqueous ammonium chloride solution. The final design is shown in Figure 2-3.
The aerosol spiking system consisted of a nitrogen cylinder equipped with a high pressure regulator. The regulator was connected to a 114-inch stainless steel tee with a 3-foot long piece of 114-inch outer diameter (O.D.) stainless steel tubing. One end ofFigure 2-2. Method 0050 Train Used for Ammonium Chloride StudiesTable 2-3 Sample Train Reagent Type and Quantity by Impinger



### 5 

## I 200 

## I Silica Gel 

## I Straight Stem Impinger Type Greenburg-Smith Tip w/plate Straight Stem Greenburg-Smith 

### Tip w/plate Straight Stem 4 Reagent Type 0.1N H2S0, 0.1N H,SO, 0.1N NaOH Impinger Number 1
2 3 Reagent Quantity 

## (s) 100 100 100 100 0.1N NaOH

### High pressure ~~rosol spiking system 

### 2-3. - - --* 

### into a Method 0050 

### Train* 

# - -.

"--.-"- 

### Used to spikethe tee was connected to a pressure release valve so that the spiking system could be vented after use and before disassembling. The other end of the tee was connected to a 107-mL stainless steel high pressure vessel with 1116-inch O.D. stainless steel tubing.
The high pressure vessel made from an empty high performance liquid chromatography columnwas modified by drilling a port in the side so that the vessel could be refilled without disassembling the spiking system. An on/off valve was connected to the port using an 118-inchNPT to 114-inch Swageloke stainless steel fitting. The other end of the onloff valve was connected using 114-inch O.D. Teflon@ tubing to a 1-Liter polyethylene bottle with a 25-mL bottle top dispenser.
The outlet end of the high pressure vessel was connected to an on/off valve. The onloff valve was connected through 1116-inch stainless steel tubing to a piece of capillary fused silica tubing (1pm inner diameter). The fused silica tubing was placed inside a sheath of 114-inchTeflon@ tubing and inserted into a 518-inch glass tee with screw cap ends. The middle leg of the glass tee terminated in a female socket that was placed 114 inches above an erlenmeyer flask of boiling water.
The performance of the dynamic aerosol high pressure spiking system was evaluated at several operating pressures between 850 and 1500psig to determine the operating limits of the system. The injection system operated best at higher pressures with 1000psig as a minimum operating pressure. At 1250psig the system operated satisfactorily; however, an operating pressure of 1500 psig provided the most reliable and constant delivery rate of approximately 0.5 mL/min.
For one train the aqueous ammonium chloride solution was substituted with a solution of ammonium chloride in methanol. The methanol solution made a finer aerosol than the aqueous solution and sprayed into the train at a faster rate using the same capillary restrictor and cylinder pressure.2.4 Pre~aration of Reference Sam~les
Before the start of each run where HC1 was spiked (Runs C-9 through C-11), a reference sample was generated by purging the spike gas directly into a series of two impingers, as shown in Figure 2-1, containing 100 mL of 0.1N sulfuric acid. The reference samples were generated by purging the gas at the flow rate used to spike the train for 10minutes.
2.5 Sam~le Train Recoverv Procedures
The trains were recovered in four fractions: the front half, consisting of the probe and front half filter holder rinses; the filter; the acidic portion, consisting of the back half filter holder rinse and both 0.1N 

### H,SO, impingers; and the basic portion, consisting of the 0.1N NaOH impingers. All of the impingers were weighed before being recovered into the appropriate tared bottles. The impingers and other train components were rinsed three times with deionized water and the rinses were added to the appropriate recovery bottles.
2.6 Ion Chromatomaahic Analysis
The samples were analyzed on a completely inert, metal-free Dionex DX-300 gradient chromatography system for ion chromatography. For chloride determination, an AG4A guard column and an AS4A-SC anion separator column were used. Chloride was eluted using a buffer solution consisting of 17-mmoiar sodium carbonate and 18-mmolar sodium bicarbonate. For ammonium determination, a CGlO guard column and a CSlO cation separator column were used. Ammonium was eluted using a buffer solution consisting of 40-mmolar HC1 and 4-mmolar 

### D,L-2,3-diaminopropionic acidmonohydrochloride. Data from the Dionex-300 were processed through a Perkin-Elmer Nelson 2600 chromatography data system. Before sample analysis, the instrument was calibrated using four standards over the range of 5.0 to 20.0 ppm for chloride and 5.0 to 20.0 ppm for ammonium. A least squares fit applied to the data points resulted in curves with correlations of 0.9950 or better. Quality control samples made from separate sources of chloride and ammonium were analyzed using the established curve before and after every 20 samples. For the sample analysis to be acceptable, the quality control sample analysis had to be within k 10% of the target concentration. A blank and duplicate sample were run for every sample set or for every 20 samples. A matrix spike and matrix spike duplicate were run for every sample set or for every 20 samples. For the data analysis to be acceptable, the matrix spike and matrix spike duplicate analysis recoveries had to be within +.20%aof target. Any samples with responses above the calibration curve were diluted and reanalyzed.3.0 RESULTS AND DISCUSSION
This section reports and discusses the results of the experiments described in Section 2. Table 3-1 tabulates the measured bias for HC1 determination for all of the runs. Table 3-2 shows the distribution of the ammonium chloride in the train. Table 3-3 summarizes the measured bias for HC1 determination for each condition tested. Table 3-4 provides the results of an analysis of variance procedure conducted onthe four groups of data containing triplicate determinations.
3.1 

### Baseline Emeriments
Runs C-1 through C-4 were designed to determine whether a positive bias occurs when ammonium chloride is present in the sampled gas and to demonstrate that the spiking, sampling, and analytical systems were functioning properly. The initial experiment started with spiking a 2.7 g/L ammonium chloride solution into the train at approximately 

### 0.5 mL/minute. The probe and quartz filter were heated to 125°C and moisture was added at 18 k 4 percent.
For Run C-2 the capillary spiking nozzle plugged, reducing the amount of ammonium chloride spiked into the train. This data indicate that even small amounts of ammonium chloride in the sampled gas can cause measureable bias in the determined HCl concentration. Bias for all four runs at 125°C ranged from 

## + 1.38 to +24.3 mg HC1. Between 34 and 87% of the ammonium chloride spiked was accounted for in the four train components analyzed. Approximately 10to 80% of the ammonium chloride remained in the probe and an additional 0.06 to 8.7% was collected on the filter. An additional 

### 5 to 20% was collected in the H,SO, impingers. Less than 1% was collected in the NaOH impingers.Run Date Filter/Probe Amount/Concentration Number (1993) Temp. ("C) NH4CI Spiked 

### I C-1 

### 1 9-7 

### 1 124 ( 29.5 ppmv (180 mg) Table 3-1 Summary of Spiked Train Experiments Sampling at 0.76 CFM for Two Hours



### c-2" 9-7 126 2.44 ppmv (15.0 mg) C-3 

# 1 9-8 

# 1 128 

# 1

. 34.2 ppmv (210 mg) C-4 9-10 121 31.8 ppmv ( 195 mg) C-5 9- 10 194 29.1 ppmv (180 mg) C-6 9-10 207 29.1 ppmv (180 mg) 

## I C-6W 

## 1 9-13 

## 1 2 10 

## 1 29.4 ppmv (180 mg)

D-7 9-13 125 29.1 ppmv (180 mg) ID-8' 19-14 

# 1 123 

# 1 29.1 ppmv (180 mg)

- - C-9 9-16 123 29.1 ppmv ( 180 mg) C-10 9-16 124 30.1 ppmv (186 mg) 1 C-11 9-17 121 29.1ppmv(180mg) 

# ~ D-15 9-23 123 24.4 ppmv (150 mg) 

# I
D-16 9-23 121 29.1 ppmv (180 mg) M-17d 9-23 122 41.2 ppmv (255 mg) Si a Bias = Measured 

### - Spiked Capillary spiking nozzle plugged during run Teflon. filter used instead of quartz Percent Moisture Spiked Measured (mg)

NH4Cl in methanol solution used instead of aqueous NH4CI solutionTable3-2DistributionofAmmonium ChlorideinEachTrain Fraction11IRunNumberPercentIAmmonium Chloride Recovered(%)Probe/Front'4NaOHHalfRinseFilterImpingers ImpingersTotal28.40.0619.4~0.0747.9310.58.714.8~0.7734.7777.90.35.86~0.0684.123.2 High Temperature Experiments
Runs C-5, C-6, and C-6W were designed to determine the effectof train operating temperature on the positive bias that has been reported when ammonium chloride is present in the sampled gas. The high temperature experiments started with spiking a 2.7272 g/L ammonium chloride solution into the train at approximately 0.5 mL/minute. The probe and quartz filter were heated to 204°C and moisture was added at 21.9 r 0.5 percent.
Bias for all three runs at 204°C ranged from 

## + 112 to 

## + 115 mg HCl. Between 91 and 94% of the ammonium chloride spiked was accounted for in the four train components analyzed. Less than 1% of the ammonium chloride remained in the probe or was collected on the filter. Over 90% was collected in the H2S0, impingers. Less than 1%was collected in the NaOH impingers. Thus, the bias in the HCl measurement from the presence of ammonium chloride was significantly increased by raising the temperature of the probe and filter to 204°C. Thus, when ammonium chloride is present in the sampled gas, the operating temperature of the train should be kept as low as possible, preferably 121°C or below.
3.3 Moisture Experiments
Runs D-7, D-15, and D-16 were designed to determine the effect of moisture on the positive bias that has been reported when ammonium chloride is present in the sampled gas. The moisture experiments started with spiking a 2.7272 g/L ammonium chloride solution into the train at approximately 0.5 mL/minute. The probe and quartz filter were heated to 123°C and moisture was added at 4.08 2 0.1 percent.
Bias for all three runs at 4.08% moisture ranged from 

## + 19.4 to +39.3 mg HCl. Between 86 and 100% of the ammonium chloride spiked was accounted for in the fourtrain components analyzed. Between 55 and 71% of the ammonium chloride remained in the probe or was collected on the filter. Between 20 and 32% was collected in the H2S04 impingers. Less than 9% was collected in the NaOH impingers. Thus, the bias in the HCl measurement from the presence of ammonium chloride was approximately doubled by decreasing the moisture in the sampled gas. Thus, when ammonium chloride is present in the sampled gas, the amount of moisture in the sampled gas may affect the bias in the HC1 measurement.
3.4 Hvdroeen Chloride Ex~eriments
Runs C-9 through C-11 were designed to determine the synergistic effect on the bias in the HC1 measurement introduced by the presence of ammonium chloride. The HCl experiments started with spiking a 2.7272 g/L ammonium chloride solution into the train at approximately 0.5 mL/minute while simultaneously spiking a 262 ppmv HCl gas standard into the train at 1.767 

## + 0.014 L/min. The probe and quartz filter were heated to 123°C and moisture was added at 18.6 

### a 0.7 percent.
Bias for all three runs where the sampled stream contained 21.5 k 0.2 ppmv HCl and 29.4 

### a 0.7 ppmv ammonium chloride ranged from +52.0 to +69.4 mg HC1. Based on the ammonium ion analysis, between 107 and 112% of the ammonium chloride spiked was accounted for in the four train components analyzed. Between 19 and 52% of the ammonium chloride remained in the probe. Between 4 and 19% was collected on the filter. Between 31 and 48% was collected in the H,SO, impingers. Less than 25% was collected in the NaOH impingers. Thus, the bias in the HC1 measurement when both ammonium chloride and HC1 were present in the sampled gas approximately quadrupled. When ammonium chloride and HC1 are present in the sampled gas, the bias in the 

### HCl measurement may be greater than when only ammonium chloride is present.The HC1 measurements were corrected for the ammonium ion measured in the 0.1N H2S04 assuming that all of the ammonium ion collected was from ammonium chloride. The corrected HCl measurements are reported in Table 3-5 and ranged from 110 to 132 percent. Thus, it may be possible to correct the HC1 results by also analyzing the samples for ammonium ion.
Before the start of each run, a reference sample was generated by purging the spike gas directly into a series of three impingers. The first two impingers contained 0.1N H2S04 and the last impinger contained 0.1N NaOH. Table 3-6 summarizes the reference results for Runs H-1 through H-3. The reference samples were generated by purging the gas at the flow rate used to spike the train for 10 minutes. The reference sample recoveries varied from 96.1 to 164 percent.
3.5 Filter Experiment
Run D-8 was designed to determine the affect of the filter material on the breakthrough of ammonium chloride into the impinger train. The filter experiment started with spiking a 2.7272 g/L ammonium chloride solution into the train at approximately 0.5 mL/rninute. The probe and Teflon@ filter were heated to 123°C and moisture was added at 4.48 percent.
Bias for the run where the sample train used a Teflon@ filter was +27.3 mg HCl. Based on the ammonium ion analysis, 81% of the ammonium chloride spiked was accounted for in the four train components analyzed. Approximately 47% of the ammonium chloride remained in the probe. Another 5.94% was collected on the filter. The H2S04 impingers collected 22 percent. Less than 7% was collected in the NaOH impingers. Thus, the bias in the HCl measurement when a Teflon@ filter was used was similar to the bias obtained when quartz filters were used under the same samplingTable 3-6 Summary of Reference Samples Prepared Using 261 ppmv HCl Gas Recovery 

### 132 96.1 164 Reference Number 

### H-1 

### H-2 H-3 Date 

### 9-16-93 9-16-93 9-17-93 Flow Rate (L/minute) 

### 1.780 1.770 1.751 Collect ion Time (minutes) 

### 10 10 10 Amount HCl Spiked (mg) 

### 7.58 7.54 7.46Table 

### 3-6 Summary of Reference Samples Prepared Using 261 ppmv HCI Gas
Reference Number Date Flow Rate (L/minute) 1.780 Collection Time (minutes) 10 Amount HCl Spiked (mg) 7.58 7.54 Recovery 132 96.1Table 3-6 Summary of Reference Samples Prepared Using 261 ppmv HCl Gas Recovery (%) 132 96.1 

## I H-3 

## 1 9-17-93 

## 1 1.751 

## 1 10 

## 1 7.46 

## 1 164 

## I

Reference Number H-1 H-2 Date 9-16-93 9-16-93 Amount HCl Spiked (mg) 7.58 7.54 Flow Rate (L/minute) 1.780 1.770 Collect ion Time (minutes) 10 10conditions. Thus, the type of filter used in the sample train does not appear to affect the bias in the HC1 measurement.
3.6 Aerosol S~iking Solvent Ex~eriment
Run M-17 was designed to determine the affect of the aerosol spiking solvent on the breakthrough of ammonium chloride into the impinger train. The solvent experiment started with spiking a 2.7272 g/L ammonium chloride in methanol solution into the train at approximately 0.7 mL/minute. The probe and quartz filter were heated to 122°C and moisture was added at 4.63 percent.
Bias for the run where the ammonium chloride was spiked 

### as an aerosol in methanol solution was +37.7 mg HC1. Based on the ammonium ion analysis, 86.82% of the ammonium chloride spiked was accounted for in the four train components analyzed. Approximately 54% of the ammonium chloride remained in the probe. Another 

### 3.7% was collected on the filter. The 

### H,SO, impingers collected 24.4 percent. Less than 5% was collected in the NaOH impingers. Thus, the bias in the HC1 measurement when the ammonium chloride was spiked as a methanol solution appeared to be slightly higher than the bias obtained when an aqueous ammonium chloride spiking solution was used. Thus, the way the ammonium chloride is spiked into the train may affect the magnitude but not the direction of the bias in the HC1 measurement.4.0 

### CONCLUSIONS
The following conclusions were based on the results of the experimental work:

. The presence of ammonium chloride in the sampled gas positively biases

the HCl measurements; A significant positive bias in the HC1 measurement was observed even when the amount of ammonium chloride spiked was as low as 2.44 ppmv; The positive bias in the HC1 measurement increases when the temperatures of the probe and filter are increased; The positive bias in the HCI measurement may also be affected by the quantity of moisture in the sampled stream, increasing as the amount of of moisture in the sampled stream decreases; The type of filter used in the sample train does not appear to affect the positive bias in the HC1 measurement; When both HC1 and ammonium chloride are present in the sampled gas, a synergistic affect occurs, increasing the positive bias in the HCl measurement; It may be possible to correct for the positive bias in the HC1 measurement by analyzing for ammonium ion and assuming the ammonium ion is disassociated ammonium chloride; Ammonium chloride should be listed as an interferent in the method; and The method should include a discussion of the trade off between filter and probe temperature and the negative and positive biases that will be introduced under various scenarios.

Based on the results from Task A of this work assignment, operating the train at higher temperatures increases the precision of the HCl measurement and reduces the loss of HC1 in the cyclone.' Additional data is also available to show that operating the train at 200°C (400°F) also eliminates the negative bias reported when sampling sources containing less than 20 ppmv HCL6 However, based on the results of the experimentsreported here, operating at higher temperatures significantly increases the positive bias in the HCl measurement when ammonium chloride is present in the source sample. People using the method on sources where ammonium chloride is present may want to use continuous emission monitoring when possible. When ammonium chloride is present and the levels of HCl are above 20 ppmv and the source sample is not saturated with water, maintaining the probe and filter temperature at 120°C or lower and measuring the ammonium ion to allow the HCl measurement to be corrected may provide HCl measurements with minimal bias. For sources where no information is available on the presence of ammonium chloride, maintaining the probe and filter at 200°C (400°F) and analyzing for ammonium ion in the 0.1N H,SO, impingers may provide the best results.
There are three recommendations for additional work. First, the sample train, operated at 121 -c 14" (250 2 25"F), should be spiked with 25 ppmv HCl and ammonia with approximately 20% moisture to determine whether the presence of ammonia biases the HCl measurement. It is possible that HCl and ammonia could react to form ammonium chloride and precipitate in the probe. Second, the sample train, operated at 121 5 14" (250 5 25"F), should be spiked with 25 ppmv HCl and ammonium salts other than ammonium chloride with approximately 20% moisture to determine whether the presence of other ammonium salts biases the HC1 measurement. Again it is possible that HCI and ammonium salts could react to form ammonium chloride and precipitate in the probe. Third, sampling should be conducted at an actual source where both HCI and ammonium chloride, ammonia, or other ammonium salts are present.REFERENCES Tests of Diminishment of Gaseous HCl by Method 5 Train Components Under Dry and Humid Conditions, W. C. Eaton and 

### L. Jaffe, EPA Contract No.68-Dl-0009, Work Assignments 008 and 1-116, November, 1992. A Comprehensive Treatise in Inorganic and Theoretical Chemistry. J.W. Mellor. Vol. 11. Longmans, Green and Co., New York. 1922 and 1946. Stability of the Gaseous Ammonium Chloride Molecule. P. Goldfinger and G. Verhaegen. The Journal of Chemical Physics, Vol 50(3). February 1, 1969. Quantitative Estimation of Sodium and Ammonium Nitrate, Ammonium Chloride, and Ammonium Sulfate in Ambient Particulate Matter. 

### K. Yoshizumi and 

### T. Okita. Journal of the Air Pollution Control Association, Vol. 33(3). March, 1983. Evaluation of Method 0050 for Hydrogen Chloride. Task A: Cyclone Purge Studies, EPA Contract 68-Dl-0010, Work Assignment 

### 52, August, 1993. Letter to Mr. Robert Fuerst, US. EPA, Research Triangle Park, North Carolina, fromJoette Steger, Radian Corporation, Morrisville, North Carolina, EPA Contract No. 68-Dl-0010, Work Assignment 52, September, 30, 1993.APPENDIX A TRAIN DATA OPERATING DATA SHEETSI//iiiFIELDDATAOperatorKFactuN/fi~02~0.7.AmbientTern~erahrerRRobeHeaterSettinarR0OX02Method'AbbW\IIDharamofDuctReadandRecordAllDataEverMinutesI---Pbnt.AREALDateSamplingLocslian-SampleTypeon~~mber.-IDryCiasMeterbperatuemiPumpIIoutlet~xitVacuum--Length and~ypNodeID(in.)MeterEoxNumberMeterAH@.~d.WA*a7-16-736tfCJILI~-01TraverseITimeITime1ReadingIHead(RessueICiasIRobe1FilterITerraFtGL5-j/N-30)-b5\.QUO<---H~I~M0'~outjon(m~uct~hnemions(in)FiltwNumberAssumedMdstue(%),02(%)tJ/ALm$/$v9&"luaoI.sW)

# 4: PC:APPENDIX 

### B TRAIN 

### RECOVERY DATA SHEETS

## MOISTURERECOVERY FORM FOR 

## METHOD 4.

Impinger Weight Irnpingcr Impinger 

### Amount of Impinger Tip 

# 1 Weight 

# I Number Solution Solution Configuration 

### Final Initial Gain (g) (g) 

### 1 (g) 

## 0-IM 1 

# Haso, I 00W\ 

# 8qu.3 

# oabx an.1

' I J



### Total Weight 

### Gain (g) 

# 37Y.0

# !

I

## RADIAN COICOIITlOl 

## MOISTURE RECOVERY FORM FOR METHOD L



### Impinger 

### Number 

### Impinger Solution Amount of Solution 

## I Impinger 

### W Impingcr 

### Tip Configuration

# I Final

Total Weight Gain

## MOISTURE RECOVERY FORM FOR METHOD 4



# . Plant Date Sampling Location Sample Typc 

### Run Number Irn~inner Box

### Number

Total Weight Gain (g)

# / q%a - 

### 0

# 1 tAl 

## wVSX Q- 3-73 

# c?'~ S- 

## HWE~
I



### Impinger Number
1
2


### 3 

### Impinger Solution



# o4N 

# hY+ 0

## IN (LSOu 

## 04 

# N.l ot, Amount 

### of Solution (g) 

## \

# e 0

100 

### \ 00 Impingcr Tip Configuration Impinger Weight I 

### Final 

### 1 1 

### Weight Initial 

### Gain 

### i 

# 4YISC 

# sL;#+

4s .I p\& w.7 

# 7.333

Gll,s 

# 61a-5 

# an.% I 577.6 

## /5+-3 

# 5%-o 23-4 I

### MOISTURE RECOVERY FORM FOR METHOD 4
Plant Date SamplingLocation Sample ~ype 

### Run Number Impinger. 

### BoxNumber Recovery 

### Person. Recovery Rinses Sample Identification Filter

### Number Xk&D Number



### Total Weight Gain ( ~y 

### b 

## 64\L\I 

## - 2


## LM 2.5.1.-0.~53) 

## /A
Impinger Number 

### Impinger Solution Amount of Solution 

### ( Configuration1 Final i 

### Initial Impinger Tip Impinger 

### W

## RADIAN COICOIITIOU 

## MOISTURE RECOVERY FORM FOR METHOD 4

Recovery Person Recovery Rinses -SampleIdentification FilterNumber 

### XADNumber

Total Weight Gain (g) 

## $$ 

## I

## MOISTURE

## RECOVERY FORMFOR METHOD
Plant Date Sampling Location Sample Type 

### Run Number Impinger Box

### Number RecoveryPerson Recovery Rinses Sample Identification FilterNumber 

### XADNumber

Total Weight Gain 

## Sd 

## 7-10-73

hb

3,


## LMW *-So92

Impinger Number


### 1
2


### 3 

### Impinger Solution 

## 0-iN 

# o, 0-1 

# N k5sf. O.IN 

# n, GH Impinger 1 

### Amount of

Solution 

## 1 

## 1

## o3
1 OQ
\Or3 

### Final (g) 

# glb-S 625-7 Impingcr Tip Configuration

G/IS 

### w/

## pl rf-c 

# 5Ls~\ 

# &/ I

# s \-I pI+e Initia 

### (R) 

# s66- 

# 796. 

# 564.

## MOISTURERECOVERY FORM FORMETHOD 4

Impingcr Number

Total Weight Gain (g) (g) 

## G.lN 1 

### \OQ 

## 63.3 I I 1 I I 

### Impinger Solution



## 75-1

# 1 j Amount of

Solution Impinger Tip Configuration Impinger Weight Final Initial Weight Gain

## MOISTURE RECOVERY FORM FOR METHOD 4
Plant Date Sampling

### Location SampleType

,

### Run Number Impinger

### BoxNumber

Total Weight Gain ( 

### ARhprC 

### PA X3. 

### 743-73



### LC&

1

Impinger Number



### 1 Recovery Person I 

### KLPj

Impinger Solution 

## c-IN Recovery

### Rinses Sample Identification Filter Number 

### ,XADNumber

1 I 

# t-uo~t I I 

# 4 ++e I 

### X 

## "1 '91 %O

I \ 

### (0 .SSW



## 597.7 Amount of



### Solution 

## S6L.b Impinger 

### Tip Configuration

I Impinger 

### W



## loo Final 

## &

# [S Initial (g)

## MOISTURE

## RECOVERY FORM 

## FOR METHOD 4

Impinger Weight 

### Impinger Impinger Amount of 

### Impinger Tip Weight 

### Number Solution Solution Configuration Final Initial Gain 

### (R) (g) 

### 1 (g) 

### c.iN 

## \GQ 

# G $ 1 

# kaSolt 6S%a 

# 612 

# w.~

## MOISTURE RECOVERY FORM FOR METHOD 4
Plant Date. SamplingLocation Sample Type Run Number Impinger

### BoxNumber Recovery Person Recovery Rinses Sample Identification FilterNumber 

### XAD Numbcr

Total Weight Gain 

### 1VA 

### 53, 

### 4- ((0 

## -73 LC\ 

### k 

## t+cl 

## / CIa 

# c -Ic! I 

# RLM 7X y/ 

## D1 b3C I 

## kl\ w 

### K\

# < 3p?by

## ,W/RU~
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### Lrq-ajb (~.'~667)' 

## N!A
Impinger Number Impinger Solution Amount 

### of Solution Impinger Tip Impinger

### W ~onfi~urationl Final Initial

## RADBm COW~OO~WIO~ 

## MOISTURE RECOVERY FORM FOR METHOD 4

Impinger Impinger Number Solution Plant Date

Impinger Weight Impinger 

### Tip Weight Configuration Final 

# I ~nitial

# 1 Gain 

# I I"(-RE,& WM L 7 

## C5a 7- 1 

### L 

## -19

7


### Total Weight Gain (g) 

### Sampling Location 

## 1 LC$ 

## L. Sample Type 

### Run Number 

### Impingcr Box

### Number RecoveryPerson Recovery Rinses Sample Identification Filter Number 

### XADNumber 

### /LIl L 

### -fQ 3\ 

### 13,LM TXy/

# nI B-0 

# , (S(E. &la 

# c-Y) CW, 

### LF'! a7 

## (fi-SsW) N 

## /h . /

### MOISTURE RECOVERY FORM FOR METHOD 4

Impinger 

### W Impinger Impinger Amount of Impinger Tip Number Solution Solution Configurationi Final t 

### Initial Plant Date

Total Weight Gain 

## &RE LvHq? 

### S 1 

## 9

# - 17-'I3 

### Sampling Location Sample Type 

### Run Number Impinger 

### BoxNumber 

### RecoveryPerson Recovery Rinses Sample Identification Filter

### Number

. 

### XAD Number I b 

# w\ 1 C\> 2 

## 'K.Lr\ 7~ 

# ~/m

## RAIblAN ComComaTIOw 

## MOISTURE RECOVERY FORM FOR METHOD 4
Plant Date

Impinger Weight Amount of Impinger 

### Tip 

## 1 Weight 

### &EAL 

## bA F5? 

## 3-23 

### -73

Recovery Person Recovery Rinses 

### 3U b/ %F

- - 

### Solution configuration Final Initial ~ain (g) I (g) 

### (g)

I I/- 

### Sample Identification Filter Number

, 

### XADNumber

Total Weight Gain (g)

# ( S7 

# .3 

# 1
I I \ 

### LM 

## 2\g [0-5%%\ L /

## MOISTURERECOVERYFORM FOR METHOD 4
Plant Dat SamplingLocation SampleType 

### Run Number Impinger Box

### Number .RecoveryPerson Recovery' 

### Rinses Sample Identification FilterNumber 

### XAD 

### Number 

### ~~RFAL LvAG55 

## 7- X-3 

### -73 b 

### w\\C\7 

### 0'-\b

\ 

### R

## L.M 3Y 

## -,/ DX 

### p?G 

### , 

### N~L)[ \ 

## ZG\Ch\c- W/C 

# sbtr Cl?.i"k.%\-' M V1iSi-7 (cr5

, 

### Impinger Number

Total Weight Gain 2


### 3
4 

### Impinger Solution 

### 0-/)I 1

r 

### 0.1 

## N 

# HxS 0, 

## O-IN 

# NQ OH. G-I tJ 

## NaGh Amount of Solution (g) 

### lo@
l (Ic


### 1 Qo 

### \ QQ 

### Impinger Tip Configuration 

# (37,Lf 

# s&-c; $1~ 

# E/ $ ~r/ 

# y\

# hte S\unls~~ 

# 6(S.( Impinger W 

### Final

(g)


## k,

## c7-

%bLt 

## $71.3 Initial



### 553-3.,; 

## $'/I. 

## 6 565.'

# RADIAN CORPORATION
MOISTURE RECOVERY FORM FOR METHODS 4, 5, 6

Date 

## 93.3 -93 Sarnpl ing 1ocati on 

# J-A Sample type 

# Hc\ /LIX Sample Idcnti ficationCode: 

# N~I 

# ~h'~~q~e$
XAD trap # 

### --

Run number 

# -'I 7 Sample box number 3 ~1 ean-up person 

# R{M solvent rinses 

## 3X

# W/ Dl

Total Weight Gain (grams) 

## 4748- Amount of Imoinaer Weiaht (~ramsl Impinger Imp inger Solution Impinger Tip Weight

Number So1uti on (a) Confiaurati on Final Initial Gain

, 

### I 

## lo-IN I 

### i 1 

### I 

# / S8.Mi IS.8. 

# I Wo, I I 2 

### I 

## 0.N 

# I 1 00 

# / 5G,3\t 

# 1 6-33

# 2'

# 1 c;~~.~ 

# l 76.7 %$Cq I I I 

## 0.N I I 

# I N4 I 100 

### I 

# ..I !\(kt 

# 1 -SW.I~ $70.~; 

# \a.y 61

# s C-\H I I 

### I J 

### 1 

### Ns 

## OV I \GO 

### I 

## +J

# : SXY-I 

# 77q.3 73' I 

# SIC I 5 

### I 

### I I 

## &EL I 100 

### I () 

### I I 

## ~~7.51 

## b7Y.9I 2A-6j I I 

### I I I

### MOISTURERECOVERY FORM FOR METHOD L

i 

# I 

# I I Impinger 

## u Impinger Amount 

### of 

### Impinger Tip Solution 

# I Solution Configuration 

# I Final 

# 1 initial 

## RFAL W

## A #53, 7- 

## & -73 L& 

### M\

d 

### 3 

## Wl"r 3~ 

## yHn-h0 HC\ L% xh+qc3 \ 

# - N/A 

# '

Total Weight Gain Plant Datc Sampling Location Sample Type 

### Run 

### Number Impinger 

### BoxNumber Recovery 

### Person Recovery Rinses Sample 

### Identlflcation Filter 

### ~umber

### XADNumber

## RADIW COICOIITION 

## MOISTURE

## RECOVERY FORM FOR 

## METHOD 4

Impinger Number Impinger Solution

Total Weight Gain (g) (g) 

### (g) 

## 1 1 

## I Amount of

Solution



## 3, 

# 1

I 

### Impingcr Tip Configuration Impinger Weight Final Initial Weight Gain

## RADIAN COICommTlOl 

## MOISTURE RECOVERYFORM FOR METHOD

Irnpinger 

## ' Impingcr Impinger Amount 

### of Impingcr Tip Number Solution Solution Configuration Final Initii (g) 

### 1 (2.

## IN 1 

# WC, l@C 

# s?-fyU Piant Date Sampling Location Sample Type 

### Run Number Impinger Box

### Number Recovery Person 

### Recovery Rinses Sample Identification ,Filter

### Number 

### XADNumber

Total Weight Gai: 

## AKEAL LwA#Sa 

### 9-\7-'r?

, 

### LC& 

# w\ \ 

# c\ - 7. 

### 3 3X w/ 

### DT 

### #,.O



# w\

. ~C%YIWC, 

## 7 .SM



## . Tw~
1 

# !I'/AAPPENDIX C ANALYSIS DATA SHEETSWA#52HydrogenChloride/ChlorideStudiesTaskCLessthanfivetimesthedetectionlimit.WA#52HydrogenChloride/ChlorideStudiesTaskCWA#52HydrogenChloride/ChlorideStudiesTaskCLessthanfive times thedetection limit.WA#52HydrogenChloride/ChlorideStudiesTaskCIRunC-1717-8I73.0.10.5033136.7117.122.11Lessthanfivetimesthedetectionlimit.WA#52HydrogenChloride/ChlorideStudiesTaskC*Lessthanfietimesthe detectionlimit.