EPA 600/R-
October 1997
Acetonitrile Field Test
Report
Work Assignment 45
By
Joette L. Steger
Joan T. Bursey
David Epperson
Eastern Research Group
P.O. Box 2010
1600 Perimeter Park
Morrisville, North Carolina 27560-2010
68-D4-0022
Merrill D. Jackson
Prepared for:
Robert G. Fuerst
National Exposure Research Laboratory
Human Exposure and Atmospheric Sciences Division
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
National Exposure Research Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
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Disclaimer
The information in this document has been funded wholly by the United States
Environmental Protection Agency under EPA Contract Number 68-D4-0022 to Eastern
Research Group. It has been subjected to Agency review and approved for publication.
Mention of trade names or commercial products does not constitute endorsement or
recommendation for use.
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Acknowledgments
Under EPA Contract No. 68-D4-0022 Eastern Research Group prepared this report
with the supervision and guidance of Mr. Robert Fuerst, EPA Work Assignment Manager, in
the National Exposure Research Laboratory, Air Measurements Research Division, Methods
Branch, Research Triangle Park, North Carolina. The Eastern Research Group Project
Manager was Joan T. Bursey, and the Principal Investigator was Joette L. Steger. We wish to
acknowledge the contributions of the following individuals to the success of this program:
Amy Bederka, Jenia Doerle, Danny Harrison, Jim Howes, Linn Nguyen, and Mark Owens.
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Abstract
Field experiments were conducted at a hazardous waste incinerator. The ability of a
specially-designed sampling train to quantitatively collect acetonitrile was evaluated. Ten
quadruple runs were conducted. Each run consisted of four acetonitrile sampling trains
sampling simultaneously. The sampling and analytical methods were evaluated using Method
301 (" Protocol for the Field Validation of Emission Concentrations from Stationary Sources")
statistical procedures.
The acetonitrile sampling train was based on the Method 0010 train which collects
semivolatile compounds on Amberlite XAD-2* sorbent. The Method 0010 train was modified
by replacing the Amberlite XAD-2* with Carboxen™-1000. Forty-eight grams of 45/60 mesh
Carboxen™-1000 was used. Carboxen™-1000 is a spherical carbon molecular sieve with an
average pore diameter of 70 angstroms and a surface area greater than 1200 square meters per
gram.
Earlier laboratory studies (Work Assignment 4 of Contract 68-D4-0022 and Work
Assignment 58 of Contract 68-D1-0010) indicated: Carboxen™-1000 was able to retain 100%
of acetonitrile in aqueous solutions eluted through the sorbent; was able to release greater than
90% of the acetonitrile when extracted with methylene chloride; and successfully collected
acetonitrile from moist air when used as a sorbent in the acetonitrile sampling train.
The acetonitrile sampling train was evaluated in the field to demonstrate its ability to
determine acetonitrile in the gaseous waste stream from a hazardous waste incinerator. Two
of the quadruple trains were dynamically spiked with an aqueous solution of acetonitrile.
Method 301 statistical analysis was performed. The mean recovery for the 20 spiked trains
was 100%. The relative standard deviation in the measured acetonitrile for the 20 spiked
trains was 13%. The relative standard deviation for the 20 unspiked trains was 17%. Both
relative standard deviations were therefore within the Method 301 criteria of <50%. The
calculated bias was insignificant; therefore, a bias correction factor was not needed.
This report was submitted in fulfillment of EPA Contract No. 68-D4-0022 by Eastern
Research Group under the sponsorship of the United States Environmental Protection Agency.
This report covers a period from February 21, 1996 to September 30, 1996, and work was
completed as of September 30, 1996.
IV
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Table of Contents
Disclaimer ii
Acknowledgments iii
Abstract iv
Tables ix
Figures x
Section 1 Introduction 1
Background 2
Work Assignment 58, EPA Contract 68-D1-0010 2
Work Assignment 4, EPA Contract 68-D4-0022 5
Work Assignment 45, EPA Contract 68-D4-0022 6
Section 2 Conclusions and Recommendations 8
Section 3 Experimental Design, Materials, Equipment, and Procedures 10
Experimental Design 10
Spiking 11
Precision and Accuracy Assessment 12
Materials 13
Acetonitrile Field Spiking Solution 13
Carboxen™-1000 Sorbent Modules 13
Silica Gel 13
Analytical Calibration Standards 14
Calibration Check Standards 14
Acetonitrile Method Spike Solution 15
Surrogate Standards 15
Equipment 15
Dynamic Spiking System 15
Sampling Trains 17
Quad Probe 20
Quad Train Assembly 21
Analytical Instrumentation 21
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Table of Contents, Continued
Procedures 21
Train Sampling Procedures 21
Sample Recovery Procedures 23
Field and Laboratory Blanks 26
Sampling Storage and Shipping Procedures 27
Procedures Used to Prepare Samples for Analysis 27
Analytical Procedures 30
Data Reduction Procedures 31
Statistical Analysis Procedures 33
Section 4 Results and Discussion 40
Field Sampling 40
Analysis 41
Probe Rinse Results 42
Filter Extract Results 42
Front and Back Half Rinse Results 43
Sorbent Results 43
Condensate Analysis 44
Acetonitrile Recovery 44
Acetonitrile Breakthrough 45
Statistical Analysis 46
Discussion 47
Section 5 Quality Assurance/Quality Control 50
Sampling QA/QC Procedures 50
Method Performance Criteria 50
Field Equipment Calibrations 50
Sampling Operation/Recovery Procedures 52
Representative Sampling 53
Documentation 53
Sample Custody 53
VI
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Table of Contents, Continued
Laboratory QA/QC Procedures 54
Sample Custody/Tracking 54
Calibration Curve 56
Daily QC Checks 56
System Blanks 56
Replicate Analysis 56
Replicate Samples 57
Method Spikes 57
Matrix Spikes/Matrix Spike Duplicates 58
Surrogate Recoveries 58
Field Train, Field Trip, and Field Reagent Blanks 60
Section 6 References 61
vn
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Table of Contents, Continued
Appendices
A Acetonitrile Sampling Method
B Results from Preliminary Laboratory Studies, Work Assignment 4 Contract 68-
D4-0022
C Preparation Data
C. 1 Field Spiking Solution Preparation and Analysis
C.2 Sorbent Preparation and Analysis
D Field Data Forms
D.I Sampling Equipment Calibration
D.2 Sampling Train Data
E Result Summary Tables
E.I Method 301 Calculations
E.2 Sampling Parameters
E.3 Acetonitrile Spike Amounts
E.4 Probe Rinse Analysis Results
E.5 Filter Analysis Results
E.6 WA 45 Sample Train Results
E.7 WA 45 Spike Recoveries
E.8 Breakthrough Analysis for the Double Sorbent Trains
E.9 Breakthrough Analysis for the Single Sorbent Trains
F. Quality Control Results
F.I Leak Rates
F.2 GC/FID Calibration Data
F.3 Calibration Check Standard Recoveries
F.4 Replicate Injection Results
F.5 Replicate Sample Results
F.6 Matrix Spike and Matrix Spike Duplicate Results
Vlll
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Tables
3-1 Gas Chromatography/Flame lonization Detection Operating Conditions 31
4-1 Summary of Method 301 Statistical Analysis 47
5-1 Summary of Acceptance Criteria, Control Limits, and Corrective Action 51
5-2 Laboratory Quality Control Procedures 55
IX
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Figures
3-1 Dynamic Spiking System 16
3-2 Sampling Train, with Single Sorbent Module 18
3-3 Sampling Train, with Double Sorbent Module 19
3-4 Sample Recovery Scheme for Acetonitrile Emissions Testing 24
3-5 Diagram of the Reverse Gravity Elution Setup for Extracting Acetonitrile from the
Carboxen™-1000 Using Methylene Chloride 29
x
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Section 1
Introduction
There is a wide interest in developing and evaluating a method for measurement of
acetonitrile emissions from stationary sources of air pollution. Acetonitrile is a component of
many industrial hazardous waste streams, especially from fiberglass and synthetic fiber
manufacturing. Acetonitrile is listed as one of the most difficult compounds to incinerate
according to the University of Dayton Research Institute incinerability ranking.1 Acetonitrile
has been suggested as an excellent non-halogenated compound to use as a hazardous constituent
spike during Resource Conservation and Recovery Act (RCRA) Subpart-B trial burn tests.
Lack of an effective sampling and analysis method has prevented its utilization. Eastern
Research Group, under contract to the U.S. Environmental Protection Agency (EPA), has
developed and evaluated a method for sampling and analyzing acetonitrile from stationary
sources. The results of a field test of that method are provided in this report.
In previous laboratory studies (Work Assignments [WAs] 5 and 22 on Contract 68-D1-
0010), several approaches for sampling and analysis were evaluated.2 A Method 53 train with
six to eight impingers containing water was used to trap the acetonitrile, but the acetonitrile
migrated throughout the impingers resulting in poor recovery. Addition of a chilled-water
condenser did not completely prevent the acetonitrile migration. A mineral oil vapor barrier in
the condensate trap did prevent the migration, but collection of the acetonitrile was not
satisfactorily improved. The Method 53 train was removed from consideration in favor of
using the sorbent-based SW-846 Method 00104 train with an alternate sorbent.
Additional laboratory studies (WA 58 of Contract 68-D1-0010)5 evaluated eight
sorbents for their suitability as an alternate sorbent to use in the Method 00104 sampling train
for collecting and measuring acetonitrile. Five potential alternate sorbents were identified:
Ambersorb* XEN-563, Anasorb* 747, Carboxen™-569, Carboxen™-1000, and Porapak* T.
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Laboratory evaluation of a sorbent-based sampling method using the modified
Method 00104 train was completed (WA 4 of Contract 68-D4-0022). Final laboratory method
evaluation indicated that 48 grams (g) of Carboxen™-1000 (the amount that fits in a
Method 00104 sorbent module) is sufficient to collect and recover 90 to 100% of the
acetonitrile under the conditions tested. Greater than 90% of the acetonitrile can be recovered
by eluting the sample from the sorbent. The estimated detection limit for the method is
60 ppbv (100
A field test of the acetonitrile sampling train developed in the laboratory was conducted
under this work assignment (WA 45 of Contract 68-D4-0022). The field test experimental
design followed guidance outlined in EPA Method 301, 6 "Protocol for the Field Validation of
Emission Concentrations from Stationary Sources," 40 Code of Federal Regulations (CFR)
Part 63. The field test data were used to determine the method's precision and accuracy.
The field test used a "quad train" approach in which four acetonitrile sampling trains
were operated simultaneously to collect flue gas samples. A Method 00104 sampling train,
modified by placing Carboxen™-1000 in the sorbent module, was used to collect gaseous
acetonitrile from a hazardous waste incinerator. The acetonitrile was then desorbed from the
Carboxen™-1000 with methylene chloride. The resulting organic extract was analyzed by gas
chromatography with flame ionization detection (GC/FID). A copy of the method as it was
evaluated is presented in Appendix A.
Background
The method development work leading to the field evaluation is summarized in this
subsection.
Work Assignment 58, EPA Contract 68-D1-00105
On WA 58, eight sorbents were evaluated for their:
• Ability to remove acetonitrile from aqueous solution,
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Desorption efficiency using three desorption solvents and two desorption
techniques, and
Performance in a Method 00104 train using the experimental sorbent in place of
Amberlite' XAD-2.
Experimental procedures and results are summarized here and discussed in detail in
Reference 5.
The objective of WA 58 was accomplished in three steps:
Eight sorbents were evaluated for their ability to remove acetonitrile from
aqueous solution. The five sorbents with the best performance were further
evaluated in quadruplicate to determine reproducibility and precision.
Desorption efficiency for these five sorbents was determined using three
desorption solvents and a static desorption technique. For the static desorption
technique, the sorbent was placed in a vial, a solvent was added, and the vial
was mixed by shaking and allowed to stand for 30 minutes. Three of these
sorbents were further evaluated using two desorption solvents and a dynamic
desorption technique. A fourth sorbent was further evaluated with only one
solvent by the dynamic desorption technique. For the dynamic desorption
technique, the sorbent was packed into a column and solvent was poured
through the column, collected, and analyzed. Recovery, aliquot-to-aliquot
reproducibility, and analytical precision were determined for two of the sorbents
using one solvent and a dynamic desorption technique.
The two sorbents with the best acetonitrile recoveries in the benchtop studies
were evaluated using a laboratory-based synthetic gas generator and a
Method 00104 train, with the sorbent replacing Amberlite* XAD-2. Acetonitrile
was spiked into the train as an aqueous solution. One of the sorbents was
evaluated in quadruplicate to determine recovery and aliquot-to-aliquot
reproducibility.
The results and conclusions from WA 58 provided the means for selecting the sorbent
to be used for the field studies. Laboratory tests performed in WA 58 established three criteria
for sorbent collection: 1) removal of acetonitrile from aqueous solutions, 2) ease of
preparation of clean sorbent, and 3) recovery of acetonitrile from the sorbent.
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Removal of acetonitrile from aqueous solutions is an important selection criterion for a
sorbent in this method because water vapor and water aerosol are common to most combustion
sources. Two of the eight sorbents, Amberlite* 200C(H) and Porapak* N, were eliminated
from further study due to poor recovery of acetonitrile from aqueous solutions. Five of the
six sorbents remaining from the original group, Ambersorb* XEN-563, Anasorb* 747,
Carboxen™-569, Carboxen™-1000, and Porapak* T removed more than 85% of the
acetonitrile from an aqueous solution. Ambersorb* XEN-563, Carboxen™-1000, and
Porapak* T removed the most acetonitrile from aqueous solution with the best reproducibility.
Ease of preparation of clean sorbent provide another criterion to eliminate sorbents.
Ambersorb' XEN-563, Anasorb* 747, Carboxen™-569, Carboxen™-1000, and Porapak" T
could be used from the manufacturer without extensive cleanup. Amberlite* XAD-7 was the
third sorbent to be eliminated because it required chemical cleanup to remove interferences
before use.
Recovery of acetonitrile from the sorbent after sampling is the third criterion a sorbent
must satisfy to be selected for this method. Desorption and recovery results from the
laboratory studies showed:
When static desorption was used, only Carboxen™-1000 demonstrated
acetonitrile desorption recoveries above 90%.
Carboxen™-1000 retained four times as much water as Ambersorb* XEN-563.
Regardless of the sorbent, addition of a 1 % butanol modifier to methylene
chloride always showed better recovery of acetonitrile than neat methylene
chloride.
When 1:1 carbon disulfide:dimethylformamide was used as the solvent, higher
recoveries were observed with dynamic desorption than with static desorption.
When methylene chloride was used as the desorption solvent, the effect of
dynamic desorption varied, sometimes increasing recoveries, sometimes
decreasing recoveries, and sometimes not affecting recoveries at all.
Acetonitrile recoveries from Porapak* T were poor using static desorption with
4
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1:1 carbon disulfide:dimethylformamide, methylene chloride, and 99:1
methylene chloride:butanol.
Dynamic desorption from Ambersorb" XEN-563 with methylene chloride
provided higher desorption recoveries with more precision than dynamic
desorption from Carboxen™-1000 with methylene chloride.
Carboxen™-1000 and Ambersorb® XEN-563 were selected for laboratory controlled
sampling train spiking experiments. These two sorbents yielded the following results:
The acetonitrile recoveries from the spiked train experiments using
Ambersorb" XEN-563 had poor precision, with recoveries ranging from 47 to
70 percent.
The acetonitrile recovery from Ambersorb* XEN-563 in a spiked train may be
related to the volume of gas sampled and the flow rate, increasing as the sample
volume and flow rate decrease.
More acetonitrile was recovered in the train using Carboxen™-1000 than with
Ambersorb* XEN 563.
The advantage of using Carboxen™-1000 is that it retains >99% of the acetonitrile
spiked. The disadvantages are that Carboxen™-1000 is not available in bulk quantities and it
is expensive and difficult to obtain. The advantages of Ambersorb* XEN-563 are that it is
available in bulk quantities, it is affordable, and it retains more than 90% of the acetonitrile
spiked. The disadvantage is that as much as 10% of the spiked acetonitrile breaks through the
sorbent and is lost during sampling.
Work Assignment 4 EPA Contract 68-D4-0022
On WA 4 progress was made toward the objectives of developing a sampling and
analysis method for acetonitrile and to evaluate the method in the field. The ability of the
remaining sorbents to remove acetonitrile from hot, moist, gaseous stationary source emissions
was studied. The five sorbents determined to be best at recovering acetonitrile from an
aqueous solution were evaluated (Porapak* T, Amber sorb* 5 63, Carboxen™-1000, Anasorb*
747, and Carboxen™-569). Porapak*T swelled in the sorbent module when water was added.
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The sorbent module broke and Porapak* T was removed from consideration. These various
sorbents were able to collect greater than 95% of the spiked acetonitrile using a Method 0010"
train with multiple sorbent traps under the most rigorous test conditions. A desorption
procedure to recover greater than 90% of the acetonitrile from the sorbent was developed. A
potential field test site was identified and a draft field test plan was prepared.
Several conclusions were reached based on the WA 4 experiments:
Carboxen™-1000 was the only sorbent tested that was able to quantitatively
remove acetonitrile from moist air using one 48-g sorbent module. For the
other three sorbents, approximately 80% of the available acetonitrile was
captured on each of the two or three sorbent modules used (i.e., 80% on the
first sorbent module, 16% on the second sorbent module, 3% on the third
sorbent module).
Reverse gravity elution of approximately 1 to 1.5 column volumes (50 to
90 mL) of solvent through the sorbent module quantitatively removes the
acetonitrile from the sorbent, resulting in recoveries >80% in all cases and
>90% in most cases. Acetonitrile was quantitatively extracted (recoveries
>90%) from Ambersorb*563, Carboxen™-1000, and Anasorb* 747 using
methylene chloride. In some cases, a water layer was removed from the sorbent
with the organic extract. Thus, a modifier may be needed to help solvate the
entrapped water that is extracted from the sorbent with the methylene chloride
so that a single-phase extract is produced.
The acetonitrile was not efficiently extracted (recoveries <40%) from the
Carboxen™-569 using methylene chloride. Adequate acetonitrile recoveries
from the Carboxen™-569 were obtained using a 1:1 carbon disulfide:dimethyl
formamide solution.
Additional details of these experiments and results are provided in Appendix B.
Work Assignment 45 EPA Contract 68-D4-0022
An acetonitrile sampling train was configured based on the results of the laboratory
methods development work. The Method 00104 train used to collect semi volatile compounds
was modified by replacing the Amberlite XAD-2* normally used in Method 00104 with 48
grams of 45/60 mesh Carboxen™-1000.
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Field experiments at a hazardous waste incinerator were used to evaluate the ability of
the acetonitrile sampling train to quantitatively collect acetonitrile. EPA Method 3016 was
used as the basis for the experimental design to evaluate the method accuracy and precision.
The sampling train was evaluated in the field by dynamically spiking two of the quadruple
trains with an aqueous solution of acetonitrile. A total of ten quadruple source runs were
conducted to generate enough data to use EPA Method 3016 for statistical evaluation of the
sampling train. A complete copy of the sampling and analytical method as used in this work
assignment is presented in Appendix A.
This report is divided into six sections. Section 2 describes the conclusions and
recommendations. Section 3 explains the experimental design and describes the materials,
equipment, and procedures used. The results are presented and discussed in Section 4.
Quality assurance/quality control (QA/QC) activities and results are described in Section 5.
References are provided in Section 6. The sampling and analytical method that was evaluated
is included as Appendix A.
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Section 2
Conclusions and Recommendations
The work completed on WA 45 used a modified Method 00104 train at a hazardous
waste incinerator to collect and measure acetonitrile. The Method 00104 train was modified by
using 48 g of Carboxen™-1000 in place of the Amberlite* XAD-2 sorbent. The following
conclusions are based on the results of this work:
The acetonitrile train, consisting of a Method 00104 train with 48 g of
Carboxen™-1000 in the sorbent module, successfully samples and collects
acetonitrile from stationary gaseous emission sources.
The bias calculated for acetonitrile using Method 3016 statistical procedures was
insignificant. Thus, no bias correction factor is needed.
The relative standard deviations were 13% for spiked trains and 17% for
unspiked trains. These standard deviations are within the Method 3016 criteria
of < 50%.
The mean recovery of 100% and relative standard deviation of 13% for the
spiked trains is within the EPA's Quality Assurance Handbook 7 requirements
of 50 to 150% recovery and 50% relative standard deviation.
Greater than 90% of the recovered acetonitrile was collected on the
Carboxen™-1000. Essentially no acetonitrile was collected in the probe rinses,
in the rinse of the front half of the filter holder, or on the filters.
For the four spiked trains containing dual sorbent modules, less than 2% of the
acetonitrile broke through to the second module for three of the trains and less
than 8% broke through in the fourth train.
For the 16 spiked trains containing single sorbent modules, less than 5% of the
acetonitrile broke through to the condensate for eight of the trains and less than
9% broke through for 15 trains.
Based on the results of this study, recommendations include:
• Evaluate the acetonitrile sampling train for other polar, water-soluble
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compounds such as methyl ethyl ketone, methyl isobutyl ketone, acetone, and
quinone.
• Use two sorbent modules in series when sampling sources containing > 15%
moisture.
• Investigate improved or alternate procedures for desorbing the Carboxen™-1000
to recover the acetonitrile. Possible alternate procedures include using high
pressure, low temperature extraction techniques.
• Develop and test procedures for recovering and reactivating used
Carboxen™-1000.
• Evaluate the acetonitrile sampling train at a second field site at a source other
than a hazardous waste incinerator. The evaluation should include, in addition
to acetonitrile, other polar, water-soluble compounds such as methyl ethyl
ketone and methyl isobutyl ketone.
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Section 3
Experimental Design, Materials, Equipment, and Procedures
The experimental design, materials, equipment, and procedures used to accomplish the
Method 3016 field evaluation of the laboratory evaluated acetonitrile sampling train are
described in detail in this section.
Experimental Design
The purpose of the sampling program was:
• To evaluate the laboratory developed acetonitrile sampling and analytical
methods, and
• To determine the performance (precision and accuracy) of the laboratory
developed methods under field conditions.
The field test included ten quadruple runs. For each quadruple run, four independent
flue gas samples were collected simultaneously from an incinerator emission source. Two of
the flue gas streams were dynamically spiked with known concentrations of acetonitrile. The
precision of the test method was estimated from the variation in results obtained for pairs of
spiked and unspiked samples. Accuracy (bias) was determined from the differences between
the spiked and measured quantities of acetonitrile.
The collected samples were processed and analyzed at the laboratory following
procedures discussed in detail later in this section. Both the sorbent extract and condensate
samples collected from each of the trains were analyzed for all of the quad runs to determine
whether acetonitrile breaks through the sorbent. The impinger components of the trains were
not analyzed and were archived.
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For Run 4 (day 2) and Run 5 (day 3), five of the seven recovered components were
analyzed separately. These five components are:
• The rinse of the front half of the filter housing;
• The 1:1 methylene chloride:methanol extract of the filter;
• The methylene chloride extract of the sorbent;
• The rinses of the back half of the filter housing and condenser; and
• The condensate and condensate rinses.
Probe rinses were collected at the end of each day. The probe rinses from the second
and third day were also analyzed, in order to coincide with the detailed analyses performed on
Runs 4 and 5 taken on the same days. The analytical results from these six components were
examined. Because no acetonitrile was detected in these fractions, the Work Assignment
Manager (WAM) decided not to analyze the rinse of the front half of the filter housing, the 1:1
methylene chloride:methanol extract of the filter, the rinses of the back half of the filter
housing and condenser for the remaining eight quad trains. For the same reason, the WAM
also decided not to analyze the probe rinses from the remaining test days. The analytical
results from the sorbent extract and condensate samples were combined for statistical analysis.
Spiking
Two of the four trains making up the quad assembly were spiked during each quad run.
Ten complete quad runs resulted in a total of 20 spiked and 20 unspiked trains. Acetonitrile in
water was used to spike the trains. Acetonitrile was spiked at a level equivalent to
45 ± 5 ppmv (73 ±8 milligrams [mg] total) in the flue gas stream. (No acetonitrile was
detected in the pre-test site survey samples.)
The spiking procedure for the field validation was identical to that used in the
laboratory study for acetonitrile (Appendix B) and field tests for aldehydes and ketones8 and
phenol and the cresols9. During each quad run, standard acetonitrile solution was introduced
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to two of the four trains. The flow rate of the liquid spike into each train was nominally
0.25 to 0.33 mL/min. This spike rate resulted in the introduction of 55 to 91 mg of
acetonitrile in each spiked acetonitrile train over a 1-hour sampling period. Approximately
960 L (34 ft3) of sample were collected.
Precision and Accuracy Assessment
This test program was designed to assess precision and accuracy. Precision is defined
as the estimate of variability in the data obtained from the entire measurement system
(sampling and analysis). At least two (paired) sampling trains are needed to establish
precision. Accuracy (bias) is defined as any systematic positive or negative difference between
the measured value and the true value. Percent recovery is defined as any gain or loss of a
given compound compared to a known spiked value.
Ten quad runs (40 sample trains) were scheduled during the testing program.
Acceptability criteria for the runs are detailed in Section 5 of this report. All 40 independent
trains were completed and accepted during the test period. This completion rate exceeded the
minimum requirement of at least six quad runs (24 independent trains) for statistical analysis
by Method 301.6 This number of runs provided a sample population large enough to produce
credible data quality assessments as described later in this section.
The latest version of the "Protocol for the Field Validation of Emission Concentrations
from Stationary Sources" (EPA Method 301)6 describes the data analysis method necessary to
evaluate both the bias and the precision of emission concentration data from stationary sources.
Method 3016 was used for the statistical evaluation of the test data for this field evaluation.
The Method 3016 calculations are described later in this section.
Additional assessment of the precision and accuracy using criteria from the Quality
Assurance/Quality Control (QA/QC) Procedures for Hazardous Waste Incineration Handbook
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(EPA/625/6-89/023, January 1990)7 was also performed using the criteria for SW 846
Method 00104 (±50% accuracy and 50% precision).
Materials
The methanol and methylene chloride used throughout the experiments was pesticide
grade or better. The water used throughout the experiments was high performance liquid
chromatography (HPLC) grade or better.
Acetonitrile Field Spiking Solution
An acetonitrile field spiking solution was prepared by weighing 8.0615 g of acetonitrile
into a 2-L volumetric flask and diluting to volume with water. After mixing, the field spiking
solution was placed in 20 100-mL wide-mouth jars and refrigerated at 4°C. A 0.25 mL aliquot
of field spiking solution was diluted to 10 mL with water and analyzed in duplicate by
GC/FID. Analyzed recoveries were 89.7 and 89.4 percent. The average analyzed
concentration of 3.6095 mg/mL was used to calculate the amount of acetonitrile spiked into
each train. An aliquot of the field spiking solution was retained at the laboratory. Field
spiking solution preparation and analysis data are presented in Appendix C-l.
Carboxen™-1000 Sorbent Modules
Carboxen™-1000 (45/60 mesh) was purchased in bulk from Supelco, Incorporated
(Bellefonte, Pennsylvania). Seventy sorbent modules were packed with 48.00 ± 0.04 g of
Carboxen™-1000. The Carboxen™-1000 was used as received. Each sorbent module was
labeled with a unique number. Three traps were spiked with 1 mL of surrogate and extracted
with 70 ± 2 mL of methylene chloride. The extracts were analyzed by GC/FID. No
acetonitrile was detected in the sorbent. Sorbent preparation and analysis data are presented in
Appendix C-2.
S/7/ca Gel
The 6-16 mesh indicating silica gel was dried at 180°C (350°F) for 2 hours (hr) before
use. Dried silica gel was stored in air-tight containers at room temperature.
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Analytical Calibration Standards
Calibration standards at six levels were prepared in methanol and in methylene chloride
from stock standards. An acetonitrile and propionitrile stock standard in methanol was
prepared at a concentration of 1.11 mg/mL acetonitrile and 1.036 mg/mL propionitrile by
weighing 111.1 ±0.1 mg of acetonitrile and 103.6 mg/mL of propionitrile into a 100 mL
volumetric flask and diluting to the line with methanol. Calibration standards in methanol
were prepared by diluting 0.045, 0.18, 0.45, 2.5, 4.5, and 22.5 mL of stock standard to 50
mL with methanol to provide a standard curve with calibration points at nominally 1, 4, 10,
50,100, and 500 micrograms per milliliter (/xg/mL).
An acetonitrile and propionitrile stock standard in methylene chloride was prepared at a
concentration of 1.500 mg/mL acetonitrile and 1.165 mg/mL propionitrile by weighing
150.0±0.1 mg of acetonitrile and 116.5 mg/mL of propionitrile into a 100 mL volumetric
flask and diluting to the line with methylene chloride. Calibration standards in methylene
chloride were prepared by diluting 0.035, 0.13, 0.33, 1.5, 3.5, and 17.0 mL of stock standard
to 50 mL with methanol to provide a standard curve with calibration points at nominally 1, 4,
10, 50,100, and 500 micrograms per milliliter (/xg/mL).
Calibration Check Standards
Calibration check standards at nominally 80 /zg/mL were prepared from independently
prepared stock standards. An acetonitrile and propionitrile calibration check stock standard in
methanol was prepared at a concentration of 2.132 mg/mL acetonitrile and 2.172 mg/mL
propionitrile by weighing 106.6±0.1 mg of acetonitrile and 108.6 mg/mL of propionitrile into
a 50 mL volumetric flask and diluting to the line with methanol. The calibration check
standard in methanol was prepared by diluting 2.0 mL of stock standard to 50 mL with
methanol to provide a calibration check standard of 85 /zg/mL of acetonitrile and 87 /zg/mL of
propionitrile.
An acetonitrile and propionitrile calibration check stock standard in methylene chloride
was prepared at a concentration of 2.248 mg/mL acetonitrile and 1.970 mg/mL propionitrile
14
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by weighing 112.4±0.1 mg of acetonitrile and 98.5 mg/mL of propionitrile into a 50 mL
volumetric flask and diluting to the line with methylene chloride. The calibration check
standard in methylene chloride was prepared by diluting 2.0 mL of stock standard to 50 mL
with methylene chloride to provide a calibration check standard of 90 /ig/mL of acetonitrile
and 79 /*g/mL of propionitrile. The calibration check standards were transferred to bottles
with Teflon®-lined screw caps and stored at 4±2°C.
Acetonitrile Method Spike Solution
An acetonitrile method spike solution was prepared by weighing 2.501 g of acetonitrile
into a 2-L volumetric flask and diluting to volume with water.
Surrogate Standards
Surrogate standards at nominally 10 /*g/mL were prepared from stock standards. A
propionitrile surrogate stock standard in water was prepared at a concentration of 100 mg/mL
propionitrile by weighing 10.0±0.1 g of propionitrile into a 100 mL volumetric flask and
diluting to the line with water. The surrogate standard in water was prepared by diluting
5.0 mL of stock standard to 50 mL with water to provide a surrogate standard of 10.0 /ig/mL
of propionitrile. The surrogate stock and surrogate standards were transferred to bottles with
Teflon*-lined screw caps and stored at 4 ± 2°C.
Equipment
Commercially available equipment was used whenever possible. Custom designed
equipment and different applications of commercially available equipment are described in
detail in this section.
Dynamic Spiking System
The dynamic spiking system is shown in Figure 3-1. A single-channel, variable-speed
motor-driven syringe pump equipped with a 50-mL gas-tight syringe was used to continuously
infuse an aqueous 3.6 mg/mL solution of acetonitrile into the spiked sampling trains. The
syringe pump was set at a rate so that approximately 20±2 mL of solution was infused into the
15
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From Probe
a
99
V
o"
90
ryj
re
3/8" 1.0. Glass Elbow
(Temperature Controlled)
Finer
1/16" O.O. Stainless Steel
(Glass Lined)
Beveled End
7\
Motor Driven
Syringe Pump
Heated Filter Enclosure
To
"Acetonilrile Train
Train
-------
sampling train over a 1-hr period. The infusion rate was adjusted so that a bead of solution
was continually present on the needle tip without ever becoming large enough to drip off the
needle into the sample train. Thus, the liquid spike volatilizes as it enters the heated gas
stream and becomes a gaseous spike at this point.
A heated spiking elbow made of glass wrapped in heat tape was used between the
heated filter and the sampling train probe. The Teflon* line from the syringe pump was
connected to a piece of glass-lined stainless steel tubing with a beveled tip that formed the
syringe needle. This needle entered the spiking elbow so that the solution would infuse
parallel to the gas sample flow. A small area of the elbow was left unwrapped to allow a
window for the operator to observe the syringe needle tip to ensure the liquid spike was
maintained as a droplet. The actual volume of liquid spiked was measured gravimetrically by
recording pre- and post-test syringe weights. The operation of the liquid dynamic spiking
system has been evaluated for acetonitrile in the laboratory, under Work Assignment 4 of
Contract No. 68-D4-0022 (Appendix B).
Sampling Trains
Two acetonitrile sampling train configurations, shown in Figures 3-2 and 3-3, were
used in the field evaluation. Both of the train configurations used standard SW-846
Method 0010" equipment with some modifications and required four impingers connected in
series. The train in Figure 3-2 uses the standard Method 0010 configuration with a single
sorbent module after the condenser. This configuration was used for eight of the runs. The
train in Figure 3-3 uses two sorbent modules in series. This double sorbent module train was
used for two of the runs. The double sorbent modules allowed the efficiency of the sorbent for
collecting acetonitrile to be better evaluated. The condensate does not quantitatively retain
acetonitrile. Therefore, breakthrough calculations for the single sorbent trains may be biased
low.
Gas was extracted isokinetically from the source duct through a glass nozzle/probe
system and filter heated to 120 ± 14°C (248 ± 25°F). This temperature is above the boiling
17
-------
S-Type Pitot
Tube
Thermocouple
Thermocouples
Thermocouple
Carboxen 1000
Recirculation Pump
Thermocouples condensate water Gel
Dry Gas \
Meter J
O ) RumP
Vacuum
Line
Figure 3-2. Sampling Train, with Single Sorbent Module
18
-------
Stack
Wall
S-Type Pitot Tube
Figure 3-3. Sampling Train, with Double Sorbent Module
19
-------
point of water to prevent the formation of any water droplets and reduce the possibility of
acetonitrile being lost in the probe.
The sample gas stream passed through a condenser, the sorbent modules containing
Carboxen™-1000, and a four-bottle impinger train immersed in ice water. The first impinger
was a short-stemmed impinger used as a knockout to catch condensate. The second and third
impingers were Greenburg-Smith impingers each containing 100 mL of water. For both train
configurations, the fourth impinger was a 500-mL Greenburg-Smith impinger modified by
replacing the tip with a 1.3-cm ('/6-inch) inside diameter glass tube extending to 1.3 cm (¥2
inch) from the bottom of the outer cylinder. The fourth impinger was filled about % full with
anhydrous silica gel as a desiccant. The last impinger was connected to a sampling pump
followed by a dry gas meter (DGM) for measuring sample volume.
Eight of the 10 quad runs used the single sorbent module train shown in Figure 3-2.
For the last test on the second day of sampling (Run 4) and the first test on the third day of
sampling (Run 5), the train contained two sequential sorbent modules, as shown in
Figure 3-3, to evaluate collection efficiency and breakthrough.
Quad Probe
A special probe assembly was required to allow simultaneous sampling at essentially
the same point with four independent sampling trains. The probe assembly minimized the
variations in the velocity of the stack gas within the area occupied by the four sampling nozzles
and met the criteria detailed in EPA Method 301.6>1° The tips of the four probe nozzles were
collocated in the same plane perpendicular to the gas flow and within a 6 cm by 6 cm square
area. EPA Method 3016 specifies that the flow at the probe tips can be considered similar if
the area encompassed by the probe tip arrangement is less than 5 % of the stack cross-sectional
area. For this location the area encompassed by the probe tip arrangement was approximately
1 % of the stack cross-sectional area.
20
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Quad Train Assembly
Four independent sampling trains comprised the quad train assembly. Although four
meter boxes were required to operate each train, the velocity head (AP) was determined using
only one of the four control boxes. The sampling trains were identified as Trains A, B, C, and
D. Trains A and B were designated as "spiked" trains. Spiking compounds were dynamically
added to these trains in the field to determine bias.
The quad probe assembly, heated filters, condensers, sorbents, and impinger trains
were mounted on a trolley so that the four similar trains could be moved into and out of the
stack as one unit. The four probes were approximately 76 cm (30 inches) long to allow them
to extend midway into the stack gas flow. During each quad test the sample flow rate through
each train was approximately 16 L/min (0.6 cubic feet per minute [cfm]) for a nominal sample
size of 0.96 cubic meters (34 cubic feet) over a 1-hour sampling period.
Analytical Instrumentation
The samples were analyzed on a Varian* 3400 gas chromatograph (GC). The GC had a
heated injection port and was connected to a flame ionization detector. Data were collected
and reported using a Nelson Turbochrome* data system. A Varian* 8100 autosampler was used
to inject 1 to 3 \iL of sample in methanol or methylene chloride. The DB-WAX analytical
column was 30 m long with an inside diameter of 0.53 mm and a 1.5 micron (n) film thickness.
Procedures
Standard train operating, recovery, and laboratory procedures were used.
Train Sampling Procedures
Glassware Preparation: All glassware used for sampling was thoroughly cleaned prior
to use, including the probe, condenser, sorbent module, impingers, all sample bottles, and all
utensils used during sample recovery. All glassware was washed with hot soapy water, rinsed
with hot tap water, rinsed with distilled water, and dried. The glassware was triple-rinsed with
methanol and then triple-rinsed with methylene chloride.
21
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Method 0010" Equipment Preparation: All the train equipment, including meter boxes,
nozzles, pitot tubes, and umbilicals, was calibrated and leak-checked. Reference calibration
procedures were followed when available, and the results were properly documented and
retained. The calibration data forms are included in Appendix D-l. A discussion of the
techniques used to calibrate this equipment is presented in Section 5.
Sampling Operations: Flue gas samples were collected isokinetically over a 1-hour
period from a single sampling point identified from a preliminary velocity traverse. A total of
approximately 960 L (34 ft3) of sample was collected. Before testing, a leak-check of pitot
lines was performed according to EPA Method 2.u
Preparation of Sample Train: The four acetonitrile sample trains were filled and
partially assembled in the recovery trailer. The impinger buckets were clearly marked as
Train A, B, C, or D. Tared impingers were used. Approximately 100 mL of water was
transferred to the second and third impingers. The first impinger remained empty and 200 to
300 g of silica gel was placed in the fourth impinger. The filter was loaded in the filter
housing. Openings were covered with Teflon* film or aluminum foil. The assembled filter
housing, condenser, and sorbent module were placed in the impinger bucket with the impingers
and sent to the sampling location.
Final assembly of the sample trains as shown in Figures 3-2 and 3-3 occurred at the
sampling location. One-piece glass liners and nozzles were used. Thermocouples were
attached to measure the stack temperature and probe outlet, condenser outlet, and impinger
outlet gas stream temperatures. Crushed ice was added to each impinger bucket, and the probe
and filter heaters were turned on and allowed to stabilize at 120 ± 14°C (248 ± 25°F).
The acetonitrile trains were leak-checked before and after sampling. The leak rates and
sampling start and stop times were recorded on the sampling task log. Also, any other events
that occurred during sampling were recorded on the task log (such as pitot cleaning,
thermocouple malfunctions, heater malfunctions, and any other unusual occurrences).
22
-------
Sampling train data was recorded every 10 minutes on standard data forms. The data forms
are provided in Appendix D-2. With the single-sampling point arrangement used in the quad
test, the pitot tube was connected to only one of the four DGM boxes.
Leak Check Procedures: To leak-check the assembled train, the nozzle end was capped
and a vacuum was pulled in the system. With the system evacuated, the volume of gas flowing
through the system was timed for 60 seconds. All of the trains met the final leak rate criteria
of s0.566 L/min (0.02 acfm) or $4% of the average sampling rate; therefore, no runs were
invalidated and no corrections were made. After the leak rate was determined, the cap was
slowly removed from the nozzle end until the vacuum dropped off, and then the pump was
turned off. The pitot tube lines were leak-checked at least once per day before the start of the
day's first run.
Sample Recovery Procedures
Recovery of the sample trains is summarized in Figure 3-4. The probes and nozzles
were recovered on the sampling platform at the end of each test day. The sample bottles
containing the probe and nozzle washings (at the end of the day only) and each of the sampling
trains (at the end of each test) were moved to the recovery trailer. Each impinger was
carefully removed from the impinger bucket, the outside was wiped dry, and the final
impinger weight was determined and recorded.
The acetonitrile sample was then collected and distributed into containers as follows:
Container 1 - Nozzle and Probe Rinse: At the end of each test day, the contents of the
probe/nozzle were collected by rinsing with 1:1 methylene chloride :methanol into a 500 mL
pre-weighed amber glass bottle. Glassware surfaces exposed to the gas sample stream were
brushed with a Teflon* brush to ensure recovery of fine paniculate matter into the sample.
The Teflon* brush was rinsed with recovery solvent into the sample bottle.
23
-------
Fitter Holder First Second and
Nozzle, and Filter Back Half Sorbent knptnger Third Silica
Fi
ter PR
Exte
pbe Mower «
ision Front Half Cone
td Moo
enser
ute(s) (Cone
Kno
ensate (Wi
Kout) Impii
ter) wi
igers Impnger
Remove from Rinse with Pint* «/ith
Fitter 1:1 Methylene riMettwtene Rme Cap Weigh for Weigh for Weigh for
Holder and Place Chloride/Methanol r^je/Metf-ano! with Ends Moi.
in 1:1 Methylene at End of Day Methanol G
Chloride,
Fi
Methanol
Collect Collect
Contents Contents
into Sample into Sample
Conj
ter Prt
ainer Con
3be Fron
ainer
tHalf Cond
enser Sor
sture Moi<
lin G
iture Moisture
lin Gain
Empty Empty tnsoect am
Contents Contents Q Jrf
into Sample into Sample Spent
Container Container
I I
Rinse with Rinse with
Methanol and Methanol and
Ad
Con
bent Cond
Ito Ad
ainer Com
ensaie Impi
3 to
ainer
nger
Fraction Rinse Rinse Rinse Fraction Fraction Fraction
Fraction Fraction Fraction
Figure 3-4. Sample Recovery Scheme for Acetonitrile Emissions Testing
24
-------
Container 2 - Rinse of Front Half of Filter Housing: The contents of the front half of
the filter housing were collected by rinsing with 1:1 methylene chloride.-methanol into a
500 mL pre-weighed amber glass bottle. Exposed glassware surfaces were brushed with a
Teflon* brush to ensure recovery of fine paniculate matter into the sample bottle. The Teflon*
brush was rinsed with recovery solvent into the sample bottle.
Container 3 - Filter: The filters were transferred to a pre-weighed amber glass bottle
and fully submersed in 150 mL of 1:1 methylene chloride :methanol. The bottle was sealed
with Teflon* tape and then sealed in a plastic bag.
Container 4 - Sorbent Module: The sorbent modules were sealed with ground glass
plugs held in place with clamps. The sealed sorbent modules were then sealed in a plastic bag.
Container 5 - Back Half of Filter Housing and Condenser Rinse: The back half of filter
housing and condenser washing solution were combined as one sample. Methanol was used to
rinse these components and any connectors three times.
Container 6 - Condensate Knockout and Knockout Rinse: The contents of the
condensate knockout (first impinger) was collected separately. Methanol was used to rinse this
impinger and associated connectors three times. The methanol rinse was combined with the
water collected from the gas stream during the sample run.
Container 7 - Second and Third Impinger Contents, and Methanol Rinses from the
Impingers: The contents of each of the two impingers containing water and the impinger
connectors were collected as one sample. Methanol was used to rinse the impingers and
connectors three times. The methanol rinse was combined with the water.
25
-------
Field and Laboratory Blanks
The following blanks were collected and retained during the sampling and analytical
program:
Field Train Blanks: Two field train blanks were collected. A quad sampling train was
assembled in the staging area, taken to the sampling location, and leak-checked before and
after the test period. The probe and filter of the field train blank was heated as during a
sample test. No gaseous sample passed through the sampling train. The sampling train was
recovered in the same manner as the flue gas samples. The field train blank samples were
returned to the laboratory, processed, and analyzed with the flue gas samples. The probe rinse,
front half rinse, filter, sorbent module, back half rinse/condenser rinse, and condensate and
rinse were analyzed. The impinger contents were archived.
Field Trip Blanks: Two sorbent modules containing Carboxen™-1000 and two filters
(in petri dishes) were collected and submitted to the laboratory with the samples as trip blanks.
The field trip blanks were returned to the laboratory, processed, and analyzed with the flue gas
samples. The filters were extracted with 150 mL of 1:1 methanol:methylene chloride in the
laboratory before being processed with the other filter samples.
Field Reagent Blanks: One 100- to 200-mL aliquot of each lot of methylene chloride ,
methanol, and water was collected for analysis as reagent blanks on the second and fourth day
of sampling. The field reagent blank samples were returned to the laboratory, processed, and
analyzed with the flue gas samples.
Laboratory Method Blanks: After the sorbent modules were packed, several sorbent
modules were retained at the laboratory for use as laboratory method blanks. Several filters
were also retained. The laboratory method blank samples were generated in the laboratory,
processed, and analyzed with the flue gas samples.
26
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Sample Storage and Shipping Procedures
Sample containers were checked to ensure that complete labels were affixed. The
labels identified Trains A, B, C, or D, as appropriate. Teflon'-lined lids were tightened and
secured with Teflon* tape. The sample bottles, filters, and sorbent modules were stored in a
cooler on ice, and were returned to the laboratory in these coolers after completion of the field
sampling. As the samples were packed for travel, chain-of-custody forms were completed.
The chain-of-custody forms are provided in Appendix D-3.
Procedures Used to Prepare Samples for Analysis
Sorbent Extraction: The sorbent samples were spiked with propionitrile (10 mg) in
aqueous solution and extracted into methylene chloride using the procedures developed on
WA 4 of Contract 68-D4-0022 (Appendix B). The extraction method used reverse gravity
elution through the sorbent module as shown in Figure 3-5. The reverse gravity elution
apparatus consists of a solvent reservoir maintained at a height greater than the sorbent
module. The solvent reservoir is connected to the sorbent module via a three-way valve. The
three-way valve is used to fill the solvent transfer line with solvent before the extraction and to
drain the sorbent module after extraction. The extract is collected in a graduated centrifuge
tube or graduated cylinder.
To extract the sorbent, the solvent transfer line is filled with solvent by opening the
valve on the solvent reservoir and turning the three-way valve to the waste stream. The
sorbent module is then filled with methylene chloride by turning the three-way valve to the
sorbent module. The dichloromethane is eluted through the sorbent module and collected in
the graduated container. After 70 mL of extract is collected, the valves on the sample
reservoir are closed and the methylene chloride extract volume is measured. The extract is
transferred to a glass vial with a Teflon'-lined screw cap and stored at 4 ± 2°C. The
three-way valve is then turned to the waste stream so that the solvent in the sorbent module can
drain. The sorbent module is then replaced with the next sample to be extracted.
27
-------
The sorbent extract was transferred to an autosampler vial and analyzed by GC/FID
using the methylene chloride calibration curve. Except for Trains 4A, 4B, 5A and 5B, the
sorbent extracts were analyzed on the most sensitive detector setting (Range 12) using a 1
injection volume. Trains 4A, 4B, 5A, and 5B were analyzed on a less sensitive detector
setting (Renge 11).
Condensate and Knockout Impinger Rinse: For the condensate samples, the sample
volumes were measured and a 1-mL aliquot was transferred to an autosampler vial, spiked with
50 //g propionitrile, and analyzed by GC/FID using a 3 ^L injection volume. A 3 /iL injection
volume was used to lower the detection limit. Larger injection volumes could not be used
because the methanol used to recover the samples could not be adequately resolved from the
acetonitrile. The condensate samples from Runs 4 and 5 were analyzed using a 1 ^L injection
volume. The sample results were quantitated using the acetonitrile calibration curve prepared
in methanol.
Back Half of Filter Housing and Condenser Rinse: For the Runs 4 and 5, the sample
volumes were measured. A 1-mL aliquot was transferred to an autosampler vial, spiked with
50 //g of propionitrile, and analyzed by GC/FID using a 1 fjL injection volume. The sample
results were quantitated using the acetonitrile calibration curve prepared in methanol. The data
were presented to the WAM who decided to archive samples from the remaining runs because
no acetonitrile was detected in this fraction.
Probe Rinse: For the second and third test days, the sample volumes were measured.
A 1-mL aliquot was transferred to an autosampler vial, spiked with 50 /^g propionitrile, and
analyzed by GC/FID. A 1 ^L sample was injected. The sample results were quantitated using
the acetonitrile calibration curve prepared in methanol. The data were presented to the WAM.
No acetonitrile was detected in this fraction. Thus, the WAM decided to archive samples from
the remaining days.
28
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Separately Funnel
Union
3/8" Teflor£>
Tubing
1/8" Teflon®
Tubing
Union
larizedGassWbol
Sorbent Module
QassFnt
Figure 3-5. Diagram of the Reverse Gravity Elution Setup for Extracting Acetonitrile
from Carboxen™-1000 Using Methylene Chloride
29
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Rinse of Front Half of Filter Housing: For Runs 4 and 5, the sample volumes were
measured. A 1-mL aliquot was transferred to an autosampler vial, spiked with 50 ^g of
propionitrile, and analyzed by GC/FID. A 1 //L sample was injected. The sample results
were quantitated using the acetonitrile calibration curve prepared in methanol. The data were
presented to the WAM. No acetonitrile was detected in this fraction. Thus, the WAM decided
to archive samples from the remaining runs.
Filter: For Runs 4 and 5, a 2-mL aliquot of 1:1 methylene chloride:methanol extract
was removed from the sample bottle containing the filter. The aliquot was spiked with 100 ^g
of propionitrile, filtered through an 0.45 //m filter, and transferred to an autosampler vial.
The extract was analyzed by GC/FID using a 7 ^L injection volume. The sample results were
quantitated using an average response factor for five standards prepared in methylene chloride
that were injected in duplicate with the filter samples. An average response factor was used
rather than a linear regression because the weighted (1/x) linear regression curve had a
correlation coefficient less than 0.995, was biased at the low end, and all of the filter extract
responses were less than the lowest calibration standard. The data were presented to the
WAM. No acetonitrile was detected in this fraction. Thus, the WAM decided not to analyze
any of the remaining samples. The samples from the remaining runs were archived.
Analytical Procedures
All of the samples were analyzed by gas chromatography with flame ionization
detection (GC/FID) using the conditions in Table 4-1.
Before analyzing any samples, the GC/FID was calibrated with a five or six-point
calibration curve according to the criteria specified in Section 5. Calibration curves were
established for the two types of samples being analyzed. Two curves were established for the
methylene chloride extracts (sorbent samples) and one curve was established for methanol
(condensate and rinse samples). Most of the sorbent extracts were analyzed with a six-point
curve on the most sensitive range of the detector. Extracts from Trains 4A, 4B, 5A, and 5B
were analyzed with a 5-point curve on a less sensitive detector range. For a daily calibration
30
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Table 3-1. Gas Chromatography/Flame lonization Detection Operating Conditions
Parameter Value
Injection Temperature 280°C
Carrier Gas Helium
Makeup Gas Nitrogen
Flow Rate 5 mL/min carrier
30 mL/min makeup
Injection Volume 1 //L or 3 /uL (condensate samples only)
Detector - Flame lonization at 300°C
Column Oven Program 44°C for 3 minutes, then 10°C per minute to
124°C and hold 2 minutes
Retention Times 4.8 minutes Acetonitrile
5.2 minutes Propionitrile
check, the GC/FID system had to meet the Calibration Check Standard criteria in Section 5.
After making any changes to the GC/FID system, a calibration check was performed to verify
the validity of the calibration curve. When the calibration check did not meet method
acceptance criteria, the GC/FID was recalibrated.
Data Reduction Procedures
Calculations for Calibration Curve: A least squares linear regression analysis of the
calibration standards data was used to calculate a correlation coefficient, slope, and intercept.
Concentration was used as the X-term, and response was used as the Y-term.
Calculation of Acetonitrile Concentration in Samples: The concentration of acetonitrile
in the samples was calculated as follows:
_ . ....,,. Sample Response - Intercept
Concentration Acetomtnle in Sample = — (3-1)
Slope
31
-------
Calculation of Total Acetonitrile Weight in Samples: The total weight of acetonitrile in
the sorbent samples was calculated from the concentration and the volume of methylene
chloride that was used to fill the sorbent module to extract the acetonitrile from the sorbent.
Total ACN in Sample (ng) = Concentration ACN in Sample (ng/mL) x Total Volume ofMeCI2 Used (mL) (3.2)
The total weight of acetonitrile in the other samples was calculated from the
concentration and the volume of sample plus rinses used to recover the sample.
Total ACN in Sample (ng) = Concentration ACN in Sample(ng/mL) x Total Sample Volume(mL) (3-3)
Calculation of Total Acetonitrile Weight in Train: The total weight of acetonitrile in
the sample train was calculated by adding the total acetonitrile weight in each of the analyzed
components. This weight was compared to the total acetonitrile weight spiked into the train
and the total acetonitrile weight measured in the unspiked trains.
Calculation of Acetonitrile Recovery. The recovery was calculated as shown in
Equation 3-4:
R = 100% x __ (3_4)
where:
R = percent recovery,
S = measured quantity in the spiked sample,
M = mean value of the unspiked samples in the run, and
CS = calculated spike quantity.
Normalization of Acetonitrile Quantities: All acetonitrile quantities were normalized to
one standard cubic meter using Equation 3-5:
32
-------
/ ni
m' = - (3-5)
where:
m' = normalized quantity;
m = measured quantity;
V = sample volume.
The values were normalized to account for the differences in the sample volumes collected by
each individual train.
Statistical Analysis Procedures
Precision and Accuracy Assessment; The test program was designed to determine the
precision and bias of the method for acetonitrile. Precision is defined as the estimate of
variability in the data obtained from the entire system (i.e., sampling and analysis). At least
two (paired) sampling trains are needed to establish precision. Bias is defined as any
systematic positive or negative difference between the measured value and the true value.
Percent recovery is defined as any gain or loss of a given compound compared to a known
spiked value. Ten quad runs (i.e., 40 sampling trains) were used to assess the acetonitrile
method.
Method 3016 describes the data analysis method necessary to evaluate both the bias and
precision of emission concentration data from stationary sources. Method 3016 was used for
the statistical evaluation of the test data for this work assignment.
Method 3016 procedures involve introducing a known concentration of an analyte
(dynamic spiking in the field) to determine the bias of the method. Method 3016 also involves
collecting multiple simultaneous samples to determine the precision of the method. When
there is not a validated method available, the qualification of a method involves collecting a
minimum of 24 samples using the quadruplet (quad) sampling system. In this work
assignment, 40 samples were collected using the quad sampling system. In each quad set, half
33
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of the samples (two of the four trains) are spiked with the reference material. The remaining
trains are not spiked.
Method 3016 assumes that the amount spiked into designated trains in the field is
constant. However, with dynamic spiking in the field, maintaining a constant spiking amount
is not possible. An amount of 45 mg of acetonitrile was targeted as the spiking level, but the
spiked level was not constant for every train or for every run. Therefore, the procedures of
Method 30 16 were modified slightly to allow for different spiked amounts.
Assessment of Precision According to Method 3016: In Method 3016 procedures, the precision
of the spiked compound is calculated using the difference, dj, between the measured
concentration of acetonitrile spiked for each spiked train. The calculation assumes that there is
no difference between a pair of spiked trains. However, if different amounts of the compound
of interest are spiked into the two paired trains, an inherent difference in the two trains is
created. Thus, a difference between the pair of trains is likely to exist: This difference could
be the result of either the difference in the spiked amounts or the difference of the performance
of each train (imprecision of the method). To account for the differences in the spiked
amounts within a pair of trains, a modification to the formula is necessary. Accounting for the
differences in the spiked amounts will give a more accurate measure of the true difference
(precision) of the paired trains. The difference, d,, was calculated by the following equation:
di = (Sn - CSn) - (Sa - CSa) (3-6)
where
i = run number (i.e., 1, 2, 3, ...);
1 = first spiked train of the run;
2 = second spiked train of the run;
S = mg/m3 reported in the spiked train; and
CS = theoretically calculated amount, mg/m3, spiked into the train.
For run 2, dj is calculated as follows:
34
-------
= (70.64-79.05) - (68.22-68.03) = -8.61 jig
Precision is reported as the standard deviation (SD) between the paired measurements
of each spiked compound, SDS, given by the following equation:
L (3-7)
2n
where
n = the number of runs (the number of paired samples) and
dj = the difference between the paired sampling train measurements (from
equation 2).
The relative standard deviation (RSD) of the evaluated spiked method is calculated as:
SD
o/oRSD = —^*100 (3.8)
Sm
where
Sm = mean of the measured spiked samples.
According to Method 301,6 the evaluated method is acceptable if the %RSD is not
greater than 50 percent.
The %RSD for acetonitrile in the 10 complete runs is 13.45% and was calculated as
follows:
%RSD .k . = 10-0954*100 = 13.45%
splked 75.0788
According to Method 301,6 precision of the unspiked samples is calculated using the
difference between the measured concentration, dj, of acetonitrile in each unspiked train.
Differences in spiked amounts do not affect the unspiked trains; therefore, the difference was
35
-------
calculated by the following equation:
d, = M,, - M.a (3-9)
where
i = run number (1, 2, 3, ...);
1 = first unspiked train of the run;
2 = second unspiked train of the run; and
M = reported amount of the compound per cubic meter in the unspiked train.
For run 2, the dj is calculated as follows:
d2 =0.0339-0.0411 = -0.0072 mg/m3
indicating a difference of approximately 0.0072 mg/m3 between the reported amounts of
acetonitrile in the two unspiked trains in Run 2.
Precision is reported as the standard deviation between the paired measurements of
acetonitrile in the unspiked trains, SDU, given by the following equation:
(3-10)
where
n = the number of runs (the number of paired samples) and
dj = the difference of paired unspiked sampling train amounts.
The percent relative standard deviation of the unspiked trains is calculated as:
SD
O/ORSD =
M
m
where
Mm = means of the measured values for the unspiked samples.
According to Method 30 1,6 the evaluated method is acceptable if the %RSD is not
greater than 50 percent. An RSD value of 17.09% was calculated for acetonitrile for unspiked
36
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trains as follows:
%RSDU ... = °-00672*100 = 17.09%
unspiked
Assessment of Bias According to Method 3016: The experimental approach was designed for
the determination of bias for acetonitrile. Bias for acetonitrile was calculated using the spiked
samples, and the calculated (or theoretical) value of acetonitrile spiked. Because of differing
spiked amounts, the equation as given in Method 30 16 was modified to calculate bias for each
spiked train.
Bias, b, of the method for acetonitrile for each spiked train of each run is defined as:
. _ ~
bu - Su *
where
i = run number (i.e., 1, 2, 3, ...);
j = 1 or 2 (to indicate the first sample or the second sample);
by = bias for the j"1 spiked sample of the i"1 run;
Sjj = reported amount of acetonitrile in the j"1 spiked sample of the 1th run;
Mi, = reported amount of acetonitrile in the first unspiked sample for the i*
run;
Ma = reported amount of acetonitrile in the second unspiked sample for the i*
run; and
CSjj = calculated (or theoretical) value of the spiked acetonitrile in the 'f* spiked
sample of the i* run.
The bias for acetonitrile in the first train (train A) of Run 2 is calculated as follows:
. . (0.0339*0.041!)
The overall bias is then defined as:
B = * (3-13)
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where
bjj = bias for the j* spiked sample of the i* run and
n = the number of samples used in the calculation (i.e., 2 times the number
of runs).
The standard deviation of the bias is then calculated as follows:
SD =
(3-14)
n-1
The bias, B, calculated from equation (3-13) must be tested to determine if it is
statistically different from 0.0. A /-test is used to make this determination. The /-test
compares the calculated /-statistic of the test data with the critical /-value for the degrees of
freedom in the test data and the desired level of significance. The bias was tested using a two-
tailed /-distribution at the 95% level of confidence with n-1 degrees of freedom. The r-statistic
is calculated as shown below in equation (3-15):
SD
(3-15)
where
| B | = the absolute value of the bias;
SD = the standard deviation as calculated in (equation 3-14); and
n = the number of spiked trains used in the calculation.
This /-test evaluates the null hypothesis that the bias is equal to zero versus the alternate
hypothesis that the bias is not equal to zero. If the calculated value of the r-statistic is greater
than the absolute value of the two-tailed critical value for the specified degrees of freedom and
level of significance, then the bias is significant. If the calculated value of the /-statistic is less
than the absolute value of the critical value for the specified degrees of freedom and level of
significance, then the bias is assumed to be zero. The critical /-statistic for the samples with
38
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ten runs (20 spiked trains) is 2.093. The /-statistic is calculated as follows:
t = -MIL = 0.035
2.1167
y/20
If the /-test shows that the bias is statistically significant, a correction factor is
calculated as follows:
CF=
+JL (3-16)
cs
where
B = the bias (calculated in equation 3-13) and
CS = the average calculated (or theoretical) spiked amount.
If the CF is within the range of 0.70 to 1.30, the method is considered acceptable for
that compound.
Because the /-test indicated that the bias was not significant (i.e., 0.035 <2.093), the
correction factor need not be calculated. Calculations are shown in Appendix Table E-l.
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Section 4Results and Discussion
Results of the acetonitrile field sampling and analysis evaluation are reported and
discussed in this section.
Field Sampling
Ten quad train runs were completed at the field test site as described in Section 3.
Trains A and B were spiked. Trains C and D were unspiked. A summary of the sampling
parameters recorded for each run is provided in Appendix Table E-2. The inside diameter of
all of the sampling nozzles was 5.97 mm (0.235 inches). The static pressure in the stack was
positive, and remained constant at approximately 6.35 mm (0.25 inches) of water during all
test runs. The average sample volume collected was 0.959 ± 0.041 dry standard cubic meters
(33.9 ± 1.5 dry standard cubic feet). The sampling time was 60 minutes.
Additional liquid from the spiking solution was infused into Trains A and B. Thus, the
percentage of moisture in the stack gas calculated using Trains A and B was always higher than
that calculated for Trains C and D. Moisture values for Trains C and D ranged from 15 to
28% by volume. Moisture values were low (15 %) for Run 6 because the process was
interrupted during the run. The process interruption did not affect the test data. The source
did not contain acetonitrile so acetonitrile levels in the unspiked trains were not reduced.
The stack temperature and velocity for each run were measured using a single
thermocouple and S-Type pilot tube on the sampling probe assembly. Individual stack gas
temperature and pilot tube differential pressure measurements were taken every 10 minutes for
each of the four trains at the time the other stack sampling dala (gas meter reading, probe
temperature, etc.) were recorded. This measuremeni scheme resulted in some slighlly different
temperature and velocity data for individual trains for the same run, even though measurements
were made with a common probe. These temperature and differential pressure measurement
40
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differences did not affect the test data because the sample for all four trains was collected from
the same point, the volumes collected were recorded, and the data were corrected for the slight
differences in sample volume.
The percent isokinetic determination was slightly outside of the 90 to 110% criteria for
Trains 1A (112%), IB (116%), 6C (89.4%) and 9B (112%). These excursions outside the
isokinetic criteria did not affect the test data because no acetonitrile was present in the source.
The spiking system was operated to inject approximately equal quantities of spiking
solution into Trains A and B during each sampling run. The actual amounts spiked varied
from train to train because the syringe pumps did not always deliver exactly the same amount
of spiking solution. Appendix Table E-3 shows the quantity of acetonitrile spiked into Trains
A and B during each run. Spiked quantities were determined by weighing the spiking syringes
before and after each test run. The density of the spike solution was assumed to be 1 g/mL.
An average of 12.1 ± 1.1 mg of acetonitrile was spiked into the trains.
Analysis
The samples were collected in seven fractions:
• The probe rinse,
• The rinse of the front half of the filter housing,
The filter,
• The rinse of the back half of the filter and the condenser rinse,
• The sorbent,
• The condensate, and
• The impinger contents.
The probe rinse was collected at the end of each day. The other fractions were
collected for each train. Runs 4 and 5 had two sorbent fractions. All of the fractions for Runs
41
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4 and 5, except for the impinger fraction, were analyzed. Runs 1 through 3 and Runs 6
through 10, had one sorbent fraction. Only the sorbent and condensate fractions were analyzed
for these runs.
Probe Rinse Results
The eight probe rinses from the second and third sampling days were analyzed. Runs 4
and 5 were collected on these two days. The results for the probe rinse analyses are reported
in Appendix Table E-4. No acetonitrile was detected in the analyzed probe rinses. No
acetonitrile was expected to be found in the probe rinse because acetonitrile is volatile. The
probe was maintained at a temperature higher than the boiling point of acetonitrile. Therefore,
the acetonitrile was quantitatively transferred through the heated probe.
The instrument detection limit was estimated based on one-fifth of the lowest standard
concentration. The probe rinse sample volume was multiplied by the estimated instrument
detection limit. Based on these calculations the probe rinse samples contained less than 10 to
30 total micrograms of acetonitrile. Because no acetonitrile was detected in the probe rinses,
the WAM directed that the remaining probe rinses be archived.
Filter Extract Results
The 18 filter extracts from Runs 4 and 5, the field train blanks, and the trip blanks were
analyzed. The results for the filter extract analyses are reported in Appendix Table E-5.
Acetonitrile was detected at levels near the detection limit in all of the filter extracts. More
acetonitrile was detected in the field train blanks than in the filters from Runs 4 and 5. The
data for Runs 4 and 5 were corrected for the field train blanks.
No acetonitrile was expected to be found in the filter extracts because acetonitrile is
volatile. The source did not contain paniculate that could collect on the filter and sorb
acetonitrile. The filter was maintained at a temperature higher than the boiling point of
acetonitrile. Therefore, the acetonitrile was quantitatively transferred through the heated filter.
42
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The instrument detection limit was estimated based on one-fifth of the lowest standard
concentration. The filter extract volume was multiplied by the estimated instrument detection
limit. Based on these calculations the filters contained less than 30 total micrograms of
acetonitrile. Because no acetonitrile was detected in the filters, the WAM directed that the
remaining filter extracts be archived.
Front and Back Half Rinse Results
The 16 front and back half rinses from Runs 4 and 5 and the field train blanks were
analyzed. No acetonitrile was detected in any of these rinses.
No acetonitrile was expected to be found in the front half rinse because acetonitrile is
volatile. The filter holder was maintained at a temperature higher than the boiling point of
acetonitrile. Therefore, the acetonitrile was quantitatively transferred through the heated filter
holder.
The instrument detection limit was estimated based on one-fifth of the lowest standard
concentration. The rinse volume was multiplied by the estimated instrument detection limit.
Based on these calculations the front half rinses contained less than 10 to 20 total micrograms
of acetonitrile. The back half rinses contained less than 20 to 30 micrograms of acetonitrile.
Because no acetonitrile was detected in these rinses, the WAM directed that the remaining
front and back half rinses be archived.
Sorbent Results
All 40 first sorbents from all 10 runs and eight second sorbents from Runs 4 and 5 were
analyzed. All of the acetonitrile values reported for the sorbents from the unspiked trains were
extrapolated beyond the lowest point of the calibration curve and are estimated values only.
For the spiked trains, the first sorbent in the train collected from 68 to 114% of the
spiked acetonitrile. These percentages equate to 47 to 104 mg. Thus, the capacity of the
sorbent appears to be at least 104 mg of acetonitrile, 1.04 m3, and 303.3 g of water. Method
43
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performance may decrease when greater than 104 mg of acetonitrile is collected, or when more
than 1.04 m3 of air is sampled, or more than 303.3 g of water is condensed from the source.
Appendix Table E-6 shows the results of the analysis for the sorbents for each run.
Condensate Analysis
All 40 condensates from all 10 runs were analyzed. Acetonitrile was detected only in
the condensates of the spiked single sorbent trains. No acetonitrile was detected in the
condensate from Run 6. Run 6 contained less moisture because the process was interrupted
during the run.
For the other 14 spiked single sorbent trains, the condensate in the train collected from
< 1 to almost 11 mg of acetonitrile. An average of 4 mg of acetonitrile was detected in these
condensates. The relative standard deviation was 64%. The high relative standard deviation
indicates that there is much variability in the amount of acetonitrile collected in the
condensate.
The instrument detection limit was estimated based on one fifth of the lowest standard
concentration. The condensate volume was multiplied by the estimated instrument detection
limit. Based on these calculations the condensate from the unspiked trains for Runs 1 through
3 and 6 through 10 contained less than 10 to 30 total micrograms of acetonitrile. All of the
condensates from Runs 4 and 5 contained less than 40 to 60 micrograms.
Acetonitrile Recovery
Appendix Table E-7 shows the percentage of acetonitrile recovered in all of the
analyzed components of each spiked sampling train. Recoveries for the 20 trains ranged from
74 to 119%. The average recovery was 100%. The relative standard deviation was 13%.
44
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Acetonitrile Breakthrough
The second sorbent module in Runs 4 and 5 were analyzed. Therefore, breakthrough
of acetonitrile into the second sorbent could be examined. Any amount of compound detected
in the second sorbent was classified as having broken through the first sorbent module.
Acetonitrile breakthrough for the double sorbent trains is shown in Appendix Table E-8.
From 20 to 34 /zg of acetonitrile was detected in the sorbent modules from the four
unspiked double sorbent module trains. These quantities of acetonitrile are close to the
estimated detection limit. The levels were approximately equal in the first and second sorbent
module, indicating that the measured values may be due to background variation rather than
actual acetonitrile present in the sampled source. Although breakthroughs were calculated, the
calculated values are probably not meaningful.
For the four spiked double sorbent module trains, breakthrough ranged from 2 to
8 percent. The average breakthrough was 4 percent. The relative standard deviation was
90 percent. Three of the trains exhibited 2% breakthrough. One train exhibited 8 %
breakthrough. Thus, breakthrough of acetonitrile can be inconsistent. No reason was
identified to explain why breakthrough was higher in the one train.
The condensate fraction was analyzed for Runs 1 through 3 and Runs 6 through 10.
Therefore, breakthrough of acetonitrile into the condensate could be estimated. Acetonitrile is
not quantitatively collected in water. Thus, some of the acetonitrile that broke through the
sorbent may not have been collected. Therefore, breakthrough calculations for the single
sorbent modules may be biased low. Any amount of acetonitrile detected in the condensate
was classified as having broken through the sorbent module. Acetonitrile breakthrough for the
single sorbent trains is shown in Appendix Table E-9.
No acetonitrile was detected in the condensate for the unspiked single sorbent module
trains. Thus, no breakthrough analysis was possible using these samples. For the 16 spiked
double sorbent module trains, breakthrough ranged from 0 to 11 percent. The average
45
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breakthrough was 5 percent. The relative standard deviation was 73 percent.
Two of the trains exhibited 0% breakthrough. These were the two spiked trains from
Run 6. During Run 6, the process went down. Thus, less moisture was collected during
Run 6 than during the other runs. The amount of moisture in the source may contribute to the
amount of acetonitrile that breaks through the sorbent.
One train exhibited 11% breakthrough. Calculated breakthrough for all of the other
trains was less than 10 percent. Again, breakthrough of acetonitrile was inconsistent. No
explanation of why breakthrough was higher hi some trains was identified. Breakthrough was
< 10% for 95% of the spiked trains. For 50% of the spiked trains, breakthrough was <5%.
Use of two sorbent modules in series may be necessary when sampling sources containing
>15% moisture.
Statistical Analysis
Method validation statistics were generated according to EPA Method 3016 guidelines.
Data for all analyzed fractions from all ten runs were used. Before statistical analysis, all
compound quantities from the analytical reports were normalized using the gas volume
sampled by each train. Normalization of the data was required because each train collected
slightly different sample volumes.
Results for the statistical analysis for acetonitrile are shown hi Table 4-1. The RSD and
bias correction factor were calculated using the EPA Method 3016 with the typographical
errors corrected as posted on the EPA bulletin board. Using the criteria of 50% maximum for
the RSD and 1.000 ± 0.300 for the bias correction factor, the method validation test was
successful for acetonitrile.
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Table 4-1. Summary of Method 301 Statistical Analysis
Parameter Acetonitrile
Relative Standard Deviation Spiked (%) 13.4
Relative Standard Deviation Unspiked (%) 17.1
Bias (mg) 0.07
Bias Significant? No
Bias Correction Factor Not Needed
Disposition . Acceptable
The acetonitrile train also meets the criteria from the Quality Assurance/Quality Control
(QA/QC) Procedures for Hazardous Waste Incineration Handbook (EPA/625/6-89/023,
January 1990)7 for SW 846 Method 0010.4 The average recovery of 100% is within the QA
Handbook7 criteria of ±50% accuracy. The relative standard deviation for the spiked trains of
13% is within the QA Handbook7 criteria of 50% precision.
Discussion
Three comparisons of the data were made. Total acetonitrile recovered in the train was
compared to acetonitrile recovered in the first sorbent module. Total acetonitrile recovered
was also compared to acetonitrile breakthrough. Finally, acetonitrile recovered in the first
sorbent module was compared to acetonitrile breakthrough.
Plots of the data were made. These plots are shown in Appendix Figures E-l to E-3.
Linear least squares calculations were also performed. A >90% correlation existed between
the total recovery and the amount recovered from the first sorbent module. This correlation
indicates that any action that will increase the retention on and recovery from the first sorbent
module will improve the performance of the train.
No correlation was found between the total acetonitrile recovered and the amount of
acetonitrile that broke through the first sorbent module. Also, no correlation was found
47
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between the acetonitrile recovered on the first sorbent module and the amount that broke
through. As expected, in general, the recovery on the first sorbent module increased as the
breakthough decreased.
The effect of gas volume sampled and moisture collected on the total acetonitrile
recovery, the recovery of acetonitrile in the first sorbent, and the acetonitrile breakthrough was
also investigated. Plots of the data were made. These plots are provided as Appendix Figures
E-4 to E-7. Linear least squares calculations were also performed.
No correlation was found between the volume of gas sampled and the total acetonitrile
recovery, the recovery of acetonitrile in the first sorbent or the acetonitrile breakthrough. No
correlation was found between the moisture collected and the total acetonitrile recovery or the
recovery of acetonitrile in the first sorbent.
A slight correlation (33%) was found between the moisture collected and the percent
acetonitrile that broke through the first sorbent module. As the moisture collected increased,
the breakthrough increased. This slight correlation may indicate that the performance of the
train may be dependent on the amount of moisture present in the source. Additional
performance studies of the sampling train should be conducted to determine if a limit on the
amount of moisture which can be collected needs to be added to the method.
The in-situ extraction of the sorbent modules as described in Section 3 is highly
dependent on the technique of the operator. Alternate extraction procedures that will allow the
sorbent to be extracted automatically would increase the rigor of the method. New extraction
techniques, such as high pressure, low temperature extraction, may be applicable. Additional
method development should be performed to improve the extraction procedure.
Also, Carboxen™-1000 should be a suitable sorbent for collecting other polar, water
soluble compounds such as alcohols, ketones, and ethers. Additional performance studies
48
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should be conducted to expand the acetonitrile method to other compounds listed in the Clean
Air Act, such as methyl ethyl ketone and methyl isobutyl ketone.
49
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Section 5
Quality Assurance/Quality Control
The quality assurance/quality control (QA/QC) activities for the sampling and analytical
procedures associated with the acetonitrile test method development program are presented in
this section. In addition to employing the sampling and analytical QA/QC procedures, the
project staff was organized to allow review of project activities and provide QC coordination
throughout the term of the evaluation program.
Sampling QA/QC Procedures
The sampling QA/QC program for this project included data quality objectives;
sampling performance criteria; field equipment calibrations; field spiking consistency,
sampling and recovery procedures; representative sampling; complete documentation of field
data and abnormalities; and adequate field sample custody procedures.
Method Performance Criteria
Acceptance criteria, control limits, and corrective actions for sample collection using
the acetonitrile sampling train are provided in Table 5-1.
Field Equipment Calibrations
Field equipment was calibrated following standard procedures. Documentation of pre-
and post-test calibrations was maintained and are provided in Appendix D-l.
S-Type Pitot Tube Calibration: Prior to field sampling, pitot tubes were inspected and
documented as meeting EPA specifications in Section 3.1.1 of the Quality Assurance
Handbook for Air Pollution Measurement Systems, Volume III, Stationary Source Specific
Methods (EPA 600/4-77-027b).12 A pitot tube coefficient of 0.84 was used for velocity
calculations.
50
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Table 5-1
Summary of Acceptance Criteria, Control Limits, and Corrective Action
Criteria
Control Limits'
Corrective Action
Final Leak Rate
<0.00057 acmm or 4% of
sampling rate, whichever
is less
None: Results are
questionable and should be
reviewed and compared
with other (3) train results
Dry Gas Meter Calibration
Average post-test Adjust sample volumes
correction factor (A) agree using the factor that gives
within ±5% of average largest volume
pre-test correction factor
Individual Correction Factor (X)
Average Correction Factor
Intermediate Dry Gas Meter
Analytical Balance (top loader)
Barometric Pressure
Agree within 2 % of
average factor
1.00 ±1%
Calibrated every six
months against EPA
standard
0.1 g of ASTM Class 1
(NBS Class S) Weights
Within 2.5 mm Hg of
mercury-in-glass
barometer
Redo correction factor
Adjust the dry gas meter
and recalibrate
Not applicable
Repair balance and
recalibrate
Recalibrate
"Control limits are established based on previous test programs conducted by the EPA.
Sampling Nozzle Calibration: Glass nozzles were used for isokinetic sampling. All
nozzles were thoroughly cleaned, visually inspected, and calibrated according to the procedure
outlined in Section 3.4.2 of EPA's Quality Assurance Handbook (EPA 600/4-77-027b).4
Dry Gas Meter Calibration: DGMs were used in the acetonitrile sample trains to
measure the sample volume. All DGMs were calibrated to document the volume correction
factor prior to the departure of the equipment to the field. Post-test calibration checks were
51
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performed after the equipment had been returned to the laboratory. All DGMs met the
acceptance criteria listed in Table 5-1.
Dry gas meter calibrations were performed at the laboratory using an American* wet
test meter as an intermediate standard. The intermediate standard is calibrated every six
months against the EPA spirometer at EPA's Emission Measurement Laboratory in Research
Triangle Park (RTP), North Carolina.
Prior to calibration, a positive pressure leak-check of the system was performed using
the procedure outlined in Section 3.3.2 of EPA's Quality Assurance Handbook* The system
was placed under approximately 250 mm (10 inches) H2O pressure and a gauge oil manometer
demonstrated that no decrease in pressure occurred over a 1-minute period.
After the sampling console was assembled and leak-checked, the pump was allowed to
run for 15 minutes to allow the pump and DGM to warm up. The valve was then adjusted to
obtain the desired flow rate. For the pre-test calibrations, data were collected at the orifice
manometer settings (AH) of 13,25,38,51,76, and 102 mm (0.5, 1.0, 1.5, 2.0, 3.0, and
4.0 inches) H2O. Gas volumes of 0.14 m3 (5 ft3) were used for the two lower orifice settings,
and volumes of 0.28 m3 (10 ft3) were used for the higher settings. The individual gas meter
correction factors (YJ) were calculated for each orifice setting and averaged. The method
requires that each of the individual correction factors fall within ±2% of the average
correction factor or the meter will be cleaned, adjusted, and recalibrated. An additional
requirement for the average correction factor to be between 0.9900 and 1.0100 (1.00 ± 0.01)
was also used. For the post-test calibration, the meter was calibrated three times at the average
orifice setting and vacuum which were used during the actual test.
Sampling Operation/Recovery Procedures
To ensure consistency between trains/runs, two individuals conducted the sampling,
and two individuals cleaned up, recovered, and reassembled the glassware. This protocol
served to eliminate propagation of multiple operator variance. All team members were
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familiar with the procedures detailed in the site specific field test plan. Sampling trains were
leak-checked before and after each run. The leak rate of each train was within the specified
limits. The recorded leak rates for each train are presented in Appendix Table F-l. All
samples except four (Trains 1A, IB, 6C, and 9B) were withdrawn at a rate within 10% of
isokinetic with the stack gas velocity. Isokinetic rate data are presented with the sampling
parameters in Appendix Table E-2.
Representative Sampling
The uniformity of sampling between trains was verified by comparing gas volumes and
moisture content values. Velocity head and flue gas temperature were compared between runs
to assess the variability in stack gas conditions.
Documentation
Field data sheets were completed and checked after each test run. Test progress and
any notable events affecting the sampling or process were recorded in field log notebook.
Documentation of pre- and post-test calibrations and inspections were maintained. Field data
sheets are provided in Appendix D-2.
Sample Custody
The custody procedures emphasized careful documentation of sample collection and
field analytical data and the use of chain-of-custody records for samples being transferred. The
sample recovery leader ensured that all samples taken were accounted for and that proper
custody and documentation procedures were followed for the field sampling efforts. A master
sample logbook was maintained by the recovery task leader to provide a hard copy of all
sample collection activities. Flue gas sampling data were also maintained by the recovery task
leader.
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Following sample collection, all samples were given a unique alphanumeric sample
identification code. Sample labels were completed and affixed to the sample container. The
sample volumes were determined and recorded and the liquid levels were marked on each
bottle. The sample identification code was recorded on the sample label and in the sample
logbook. The samples were stored on ice hi a secure area until they were packed.
As the samples were packed for travel, chain-of-custody forms were completed for each
shipment container. The chain-of-custody forms and written instructions specifying the
treatment of each sample were also enclosed in the sample shipment container. Shipping
containers were labeled with up arrows to clearly indicate the upright position of sample
bottles. The samples were returned to the laboratory on ice in a vehicle at the end of the test
period.
Laboratory QA/QC Procedures
The laboratory QA program for this project included proper handling, logging, and
tracking of incoming samples; procedure validations including calibration curves, daily QC
checks, and replicate analyses; and collection and analysis of field train, field trip, and field
reagent blanks, method spikes, and field and laboratory spikes. A summary of the laboratory
QC procedures is provided in Table 5-2.
Sample Custody/Tracking
The field samples were received at the laboratory in coolers and on ice. The chain-of-
custody forms and sample bottle labels were compared to verify receipt of samples. While the
samples were being logged in they were kept in coolers on ice. A copy of the sample log
notebook was also provided to the laboratory representative. Any discrepancies or
abnormalities (leakage, etc.) were noted. The samples were logged into the tracking system.
Samples were stored at 4°C to prevent loss of acetonitrile. The chain-of-custody forms are
provided in Appendix D-3.
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Table 5-2
Laboratory Quality Control Procedures
Parameter
Linearity
Check
Retention Time
Calibration
Check
System Blank
Replicate1
Analyses
Replicate6
Samples
Method1
Spikes/
Method Spike
Duplicates
Matrix"
Spikes/
Matrix Spike
Duplicates
Surrogate
Recoveries
Quality
Control
Check
Run 5-point curve
Analyze check
standard
Analyze check
standard
Analyze solvent
Re-inject sample
Prepare duplicate
aliquot
Analyze extract of
spiked sorbent
Spike an aliquot of
sample
Spike samples with
surrogate
Frequency
At setup or when
check std. is out-
of-range
1/10 samples
1/10 samples; min.
2/set
1/10 samples
min. 2/set
1/10 sorbent
extracts or I/set
1/10 non-sorbent
samples or I/set
1/20 samples or
I/set
1/20 Samples or
I/set
Every sample
Acceptance
Criteria
Correl. coeff.
iO.995
±3 standard
deviations of
average calibration
relative retention
time
±15% of
calibration curve
One-fifth of lowest
standard
±10% of first
injection
±20% of first
sample
±20% of spiked
amount
±50% of spiked
amount
±50% of spiked
amount*
±25% of spiked
amount"
Corrective
Action
Check integration,
reintegrate. If necessary,
recalibrate
Check instrument
function for plug, etc.
Lower initial column
temperature; Adjust
column temperature
program.
Check integration,
remake standard or
recalibrate.
Locate source of
contamination; reanalyze
Check integration, check
instrument function,
reanalyze
Check integration, check
instrument function,
reanalyze
Check integration, check
instrument function,
reanalyze, reprepare if
possible
Check integration, check
instrument function,
reanalyze, reprepare if
possible
Check integration, check
instrument function,
reanalyze
"Applicable to sorbent extract samples only.
""Applicable to non-sorbent samples only.
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Calibration Curve
After initially setting up the instrument, calibration curves as described in Section 3
were prepared and analyzed. The calibration data are presented in Appendix Table F-2. All of
the calibration curves used had correlation coefficients greater than 0.998.
Daily QC Checks
A check standard as described in Section 3 was prepared. The check standard was used
to check instrument response and the calibration curve. The check standard was analyzed
before and after all sample analysis sessions and after every 10 to 20 samples. Two of the
calibration check standard recoveries for the filter analyses were outside the quality control
limits. The WAM directed that the samples not be reanalyzed because the levels of acetonitrile
detected in the filter extracts for the train samples were less than the levels of acetonitrile
detected in the field train blanks. The calibration check standard recoveries are presented in
Appendix Table F-3.
System Blanks
Neat methylene chloride, methanol, or water (system blank) was analyzed at least once
per day to ensure that the system was not contaminated. If a response was obtained that was
^0.2 of the lowest calibration standard concentration, the source of contamination was located
and eliminated before analyzing samples.
Replicate Analyses
Every tenth sample was injected in duplicate. The replicate injection results are
reported in Appendix Table F-4. A total of 21 replicate injections was made. Acetonitrile was
not detected in 11 samples. Of the 10 samples where acetonitrile was detected, four were
nonsorbent samples (two filters and two condensates) and six were sorbent extracts.
The percent difference for the four nonsorbent replicate injections ranged from -4.70 to
-2.56 percent. These results were within the quality control criteria. Surrogate recoveries for
the 13 nonsorbent duplicate injections ranged from 78 to 98%. The average nonsorbent
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surrogate recovery was 88% with a standard deviation of 8. Surrogate recoveries for the
nonsorbent samples also met the quality control criteria.
The percent difference for the six sorbent replicate injections ranged from -14.9 to
19.6 percent. These two results were outside the quality control criteria. The other four
results ranged from -5.47 to 4.23. These results were within the quality control criteria.
Surrogate recoveries for the eight sorbent duplicate injections ranged from 51 to 100%. Four
of the sorbents appeared to be spiked with the surrogate stock standard rather than the
surrogate standard. The reported surrogate recoveries for these four samples were corrected
making that assumption. The average sorbent surrogate recovery was 74% with a standard
deviation of 19. Surrogate recoveries for the sorbent samples also met the quality control
criteria.
Replicate Samples
Every tenth non-sorbent sample was analyzed in duplicate by taking a second aliquot of
sample out of the sample container and preparing it for analysis using the same procedures as
for the initial sample. The replicate sample results are reported in Appendix Table F-5. A
total of 12 replicate samples was prepared. Acetonitrile was not detected in 8 samples. The
percent difference for the remaining four replicate samples ranged from -5.36 to
+ 3.34 percent. These results were within the quality control criteria. Surrogate recoveries
for the duplicate samples ranged from 77 to 97%. The average surrogate recovery was 89%
with a standard deviation of 7. Surrogate recoveries also met the quality control criteria.
Method Spikes
One method spike/method spike duplicate for every 20 sorbent samples was prepared.
The recoveries for method spikes were within ±20% of the spike value. If the method spike
recoveries were outside of this range, the cause was identified and corrected. Depending on
the reason for the unsatisfactory recoveries, the samples were reanalyzed or flagged.
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Matrix Spikes/Matrix Spike Duplicates
One matrix spike/matrix spike duplicate for every 20 non-sorbent samples was
prepared. An aliquot of sample was removed, spiked with acetonitrile, and prepared for
analysis using the same procedure as for the unspiked sample.
The matrix spike and matrix spike duplicate sample results are reported in Appendix
Table F-6. A total of eight matrix spike and eight matrix spike duplicate samples were
prepared.
The percent recovery for the 16 spiked samples ranged from 53 to 111 percent. The
average matrix spike recovery was 80% with a standard deviation of 18. These results were
within the quality control criteria of 50 to 150 percent.
Surrogate recoveries for the spiked samples ranged from 75 to 102%. The average
surrogate recovery was 88% with a standard deviation of 8. Surrogate recoveries also met the
quality control criteria of 75 to 125 percent.
Surrogate Recoveries
All samples were spiked with a surrogate as described in Section 5.1. The surrogate
recoveries were within ±50% of the spiked value for all sorbent samples and with ±25% of
the spiked value for all non-sorbent samples. If the surrogate spike recoveries were outside of
this range, the cause was identified and corrected. Depending on the reasons for the
unsatisfactory recoveries, the samples were reanalyzed or flagged.
Probe rinse: Surrogate recoveries for the probe rinses ranged from 77 to 89 percent. The
average surrogate recovery was 84 percent. The relative standard deviation was 4%. Thus,
the surrogate recoveries for the probe rinse samples were within the quality control criteria of
75 to 125% recovery.
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Filter extracts: Surrogate recoveries for the filter extracts were calculated using an average
response factor calculated from five standards injected in duplicate. The surrogate recoveries
ranged from 75 to 83 percent. The average surrogate recovery was 80 percent. The relative
standard deviation was 3%. Thus, the surrogate recoveries for the filter extract samples were
within the quality control criteria of 75 to 125% recovery.
Front and Back Half Rinses: Surrogate recoveries for the front and back half rinses ranged
from 75 to 92 percent. The average surrogate recovery was 85 percent. The relative standard
deviation was 6%. Thus, the surrogate recoveries for the front and back half rinse samples
were within the quality control criteria of 75 to 125% recovery.
Sorbent Extracts: Twenty-eight of the sorbent extracts had surrogate recoveries between 400
and 1100 percent. Review of the notebook indicated that these samples were prepared on the
same days as each other and on different days from the samples with surrogate recoveries
between 60 and 160 percent. The surrogate spiking solution was prepared from a stock
solution by making a one-to-ten dilution. Because the surrogate recoveries were 10 times
higher than expected, it appeared that the samples were spiked with the stock solution rather
than the diluted surrogate standard. Therefore, the surrogate recoveries for these 28 sorbent
extracts were corrected.
Surrogate recoveries for the sorbent extracts after correction ranged from 43 to
158 percent. These two surrogate recoveries were outside the quality control criteria. The
remaining 46 sorbent extracts had surrogate recoveries between 55 and 135 percent. These
surrogate recoveries were within the quality control criteria of 50 to 150% recovery. The
average surrogate recovery for all 48 sorbent extracts was 89 percent. The relative standard
deviation was 25 %.
Condensates: Surrogate recoveries for the condensates ranged from 73 to 108 percent. Only
one of the 40 condensate samples was outside of the quality control criteria of 75 to 125%
recovery. This sample was analyzed several times; however, the surrogate recovery was
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always slightly low. This sample was prepared in duplicate and the duplicate surrogate
recovery was within the quality control criteria. The average surrogate recovery for the 40
condensate samples was 91 percent. The relative standard deviation was 7%.
Field Train, Field Trip, and Field Reagent Blanks
Two field train blanks of the quad trains were collected as described in Section 3. One
field train blank was collected on the second day of sampling and the second was collected on
the fourth day of sampling. Both were processed in the same manner as collected samples.
The field train blank results are reported in Appendix Table F-7. From 72 to 88.7 /zg of
acetonitrile was detected in the filter extracts (after blank correction for the acetonitrile
detected in the trip blanks). An average of 78.6 /ig of acetonitrile was detected in the field
blanks. These values were only slightly above the estimated detection limit of 30 /zg. The
relative standard deviation was 7 percent. No acetonitrile was detected in any of the other
blank train components.
Field reagent blanks of recovery solvents and unused filters and sorbent modules
packed with Carboxen™-1000 (field trip blanks) were also collected in the field and shipped to
the laboratory. The field reagent blank and trip blank results are reported in Appendix
Table F-8.
Field train and field reagent blank analytical results serve as indicators of preparation
and recovery contamination. Field trip blank analytical results serve as indicators of
contamination occurring from transportation of samples to and from the field test site. A total
of 33.3 and 33.9 /zg of acetonitrile (after correction for the laboratory method blanks) was
detected in the filter trip blanks. This is only slightly greater than the estimated detection limit
of 30 /zg. No acetonitrile was detected in the sorbent trip blanks or field reagent blanks.
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Section 6
References
1. Environmental Science and Technology, 24, pp 316-328, 1990.
2. Joette Steger and Steve Hoskinson, Development of a Method for Determination of
Acetonitrile. Draft Interim Summary Report for Work Assignment 22,
Contract No. 68-D1-0010, U.S. Environmental Protection Agency, Atmospheric and
Exposure Assessment Laboratory, Methods Research and Development Division, Source
Methods Research Branch, Research Triangle Park, North Carolina 27711.
September 29, 1992.
3. U.S. Environmental Protection Agency. Method 5-Determination of Paniculate
Emissions from Stationary Sources. Code of Federal Regulations, Title 40, Part 60,
Appendix A. Washington, D.C. Office of the Federal Register,.
4. EPA Method 0010, Test Methods for Evaluating Solid Waste: Physical/Chemical
Methods. SW-846, Third Edition. September 1986 Office of Solid Waste and
Emergency Response, U.S. Environmental Protection Agency, Washington, D.C. 20460.
5. Joette Steger and Cheryl Klassa, Evaluation of Sorbents for the Collection and Analysis
of Acetonitrile from Stationary Sources. Draft Internal Report for Work Assignment 58,
Contract No. 68-D1-0010, Environmental Protection Agency, Atmospheric and Exposure
Asessment Laboratory, Methods Research Development Division, Source Methods
Research Branch, Research Triangle Park, North Carolina 27711. October 29, 1993.
6. U.S. Environmental Protection Agency. Method 301-Protocol for the Field Evaluation of
Emission Concentrations from Stationary Sources. Code of Federal Regulations, Title
40, Part 63. Washington, D.C. Office of the Federal Register, July 1, 1987.
7. U.S. Environmental Protection Agency. Quality Assurance/Quality Control (OA/QQ
Procedures for Hazardous Waste Incineration Handbook. EPA/625/6-89/023, Center for
Environmental Research Information, Office of Research and Development, U.S.
Environmental Protection Agency, Cincinnati, Ohio 45268. January 1990.
8. Gerald S. Workman, Jr. and Joette L. Steger, Field Evaluation of the DNPH Method for
Aldehydes and Ketones. Final Report for Work Assignment 12, Contract No. 68-D4-
0022, Environmental Protection Agency, National Exposure Research Laboratory, Air
Measurements Research Division, Methods Branch, Research Triangle Park, NC.
January 1996.
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9. Joan T. Bursey, Jeffrey LaCosse, James F. McGaughey, Joette L. Steger, and Thomas
Selegue, Development and Field Evaluation of Sampling and Analytical Methodology for
High Levels of Phenol and the Cresols. Final Report for Work Assignment 3, Contract
No. 68-D4-0022, Environmental Protection Agency, National Exposure Research
Laboratory, Air Measurements Research Division, Methods Branch, Research Triangle
Park,NC. June 1996.
10. Mitchell, William J.; Midgett, M. Rodney. "Means to Evaluate Performance Stationary
Source Test Methods." Environmental Science and Technology. January 1976. 10:85.
11. U.S. Environmental Protection Agency. Method 2. 40 CFR Part 60, Appendix A.
12. U.S. Environmental Protection Agency. Quality Assurance Handbook for Air Pollution
Measurement Systems, Volume III, Stationary Source Specific Methods
(EPA 600/4-77-027b)
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APPENDIX A
METHOD XXXX
Sampling and Analysis
for
Acetonitrile Emissions from Stationary Sources
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METHOD XXXX
METHOD XXXX - SAMPLING AND ANALYSIS FOR
ACETOMTRILE EMISSIONS FROM STATIONARY SOURCES
1.0 SCOPE AND APPLICATION.
1.1 Method XXXX is applicable to the collection and analysis of acetonitrile.
Pertinent information regarding acetonitrile is listed in Table XXXX-1. This method has been
validated for acetonitrile at a hazardous waste incinerator and is believed to be applicable to
other processes where acetonitrile may be emitted. This method is not inclusive with respect
to specifications (e.g., equipment and supplies) and sampling procedures essential to its
performance. Some material is incorporated by reference from other methods in the sampling
procedure. Therefore, to obtain reliable results, testers using this method should have a
thorough knowledge of at least the following test methods: EPA Method 1, EPA Method 2,
EPA Method 3, EPA Method 4, and EPA Method 5.
TABLE XXXX-1. ACETONITRILE PERTINENT INFORMATION
Method Sensitivity
Compound Name CAS No.' Matrix Total mgb Total ppmvc
Acetonitrile
75-05-8
Incinerator, 0 ppmv ACN
Incinerator, 45 ppmv ACN
0.003
5
0.002
3
a Chemical Abstract Services Registry Number.
b Based on the standard deviation calculated by Method 301.
c For a Icubic meter (35 cubic foot) sample, based on the standard deviation by
Method 301.
1.2 When this method is used to analyze unfamiliar sample matrices, support
compound identification by at least one additional qualitative technique. A gas
chromatograph/mass spectrometer (GC/MS) may be used for the qualitative confirmation of
results from the target analyte, using the extract produced by this method.
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1.3 The method sensitivity is listed in Table XXXX-1. The method sensitivity for a
specific sample may differ from Table XXXX-1 depending on the nature of interferences in the
sample matrix.
1.4 Sample collection under this method must be performed by testers trained and
experienced with isokinetic sampling techniques. The analytical procedures in this method are
restricted to use by, or under the supervision of, analysts experienced in the use of
chromatography and in the interpretation of chromatograms. Each analyst must demonstrate
the ability to generate acceptable results with this method.
2.0 SUMMARY OF METHOD.
2.1 Gaseous and paniculate pollutants are withdrawn from an emission source at an
isokinetic sampling rate and are collected in a multicomponent sampling train. The volume of
sample collected is dependent on the type of source sampled, the estimated level of analyte in
the source, and the detection limit required for the application. The maximum sample volume
collected during method evaluation was 1.04 cubic meters (36.75 cubic feet). Method
performance may decrease when larger sample volumes are collected.
2.2 The primary components of the sampling train include a heated probe, a heated
filter, a condenser, a sorbent module contain 48 g of Carboxen™-1000, a knockout impinger,
two impingers containing water, and an impinger containing silica gel. Acetonitrile present in
the source gas stream sorbs on the Carboxen™-1000.
2.3 The CarboxenTW-1000 is extracted with 70 mL of methylene chloride in the
laboratory. The methylene chloride extract volume is accurately measured.
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METHOD XXXX
2.4 An aliquot of extracted sample is then analyzed by gas chromatography with
flame ionization detector (GC/FID). Gas chromatographic conditions are described in
Section 11.4. The conditions permit the separation and measurement of acetonitrile in the
extract.
2.5 Filters are extracted with 1:1 methylene chloride:methanol; extracts are
analyzed by GC/FID. Retention of acetonitrile on the filter depends upon the amount and
nature of the paniculate material present in the source; the amount of analyte may range from
"not detected" to significant. If a representative number (10%) of filter extracts are analyzed
and no analytes are observed, remaining extracts may be archived.
3.0 DEFINITIONS.
Calibration Check Standard - Calibration standard made from a second source of
acetonitrile used to verify the calibration curve before analyzing samples.
Field Reagent Blank - Aliquots of the sorbent, filters and water used in the sampling
train and the solvents used to recover the train that are collected in the field and returned to the
laboratory for analysis.
Field Spike - An aliquot of sorbent, filter, or reagent that is spiked with a known
amount of analyte in the field.
Field Train Blank - A sampling train that is assembled, taken to the sampling area,
leak checked, and recovered as though it were a normal train sample although no gaseous
sample is collected.
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METHOD XXXX
Isokinetic Variation - Measure of how proportional the sampling rate is to the source
gas velocity.
Laboratory Method Blank - Blank sorbent, filter media or reagent that is carried
through the sample preparation procedures with the samples and that is used to evaluate
whether any contamination occurred in the laboratory.
Method Spike - An aliquot of sorbent that is spiked with a known amount of analyte in
the laboratory and then carried through the sample preparation procedures with the samples.
Matrix Spike - An aliquot of sample that is spiked with a known amount of analyte in
the laboratory and then carried through the sample preparation procedures with the samples.
Replicate Analysis - A second injection of a prepared sample into the analytical
system.
Replicate Sample - A second aliquot of sample that is carried through the sample
preparation procedures with the samples.
4.0 INTERFERENCES.
4.1 High concentrations of highly-polar solvents, such as acetone, that have the
same retention time or nearly the same retention time as acetonitrile, and that also respond to
the FID, will interfere with the analysis. Prior knowledge of the qualitative composition of the
gas stream will aid in minimizing this type of interference. It is recommended that the sorbent
traps be packed within one month of use. The sorbent traps must be stored in an
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METHOD XXXX
uncontaminated environment both before and after sampling in order to minimize blank
problems.
4.2 Method interferences may be caused by contaminants in solvents, reagents,
glassware, and other sample processing hardware. These method interferences lead to discrete
artifacts and/or elevated baselines in the chromatograms. All reagents and glassware must be
routinely demonstrated to be free from interferences under the conditions of the analysis by
analyzing laboratory reagent blanks.
4.2.1 Glassware must be scrupulously cleaned. Clean all glassware as soon as
possible after use by rinsing with the last solvent used. This rinse should be followed
by washing with hot water and laboratory detergent, and rinsing with tap water and
distilled water. Glassware should then be drained and heated in a laboratory oven at
130°C (266°F) for several hours before use. Solvent rinses using methanol and
methylene chloride may be substituted for the oven heating. After drying and cooling,
glassware should be stored in a clean environment to prevent any accumulation of dust
or other contaminants.
4.2.2 The use of high purity reagents and solvents helps to minimize
interference problems. Purification of solvents by distillation in all-glass systems may
be required.
4.3 Matrix interferences may be caused by contaminants that are desorbed from the
sample. The extent of matrix interferences will vary considerably from source to source,
depending upon the nature and diversity of the matrix being sampled. If interferences occur in
subsequent samples, some additional cleanup may be necessary.
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METHOD XXXX
4.4 The extent of interferences that may be encountered using gas chromatographic
techniques has not been fully assessed. Although the GC/FID conditions described allow for
resolution of acetonitrile, other matrix components may interfere.
5.0 SAFETY.
5.1 The toxicity or carcinogenicity of each reagent used in this method has not been
precisely defined. However, each chemical compound should be treated as a potential health
hazard. From this viewpoint, exposure to these chemicals must be reduced to the lowest
possible level by whatever means are available. The laboratory is responsible for maintaining
a current awareness file of Occupational Safety & Health Administration (OSHA) regulations
regarding the safe handling of the chemicals specified in this method. A reference file of
material safety data sheets (MSDSs) should also be made available to all personnel involved in
the chemical analysis. Additional references to laboratory safety are available.
5.2 Acetonitrile is relatively volatile and has a vapor pressure of 1.42. Acetonitrile
is an irritant with an odor threshold near the OSHA Time-Weighted Average (TWA). Acute
inhalation exposure can cause irritation of the nose and throat. Over-exposure may cause
chemical asphyxiation similar to hydrogen cyanide poisoning. The OSHA 8-hour TWA
exposure limit is 40 ppmV. The 15-minute Short-Term Exposure Limit (STEL) is 60 ppmV.
6.0 EQUIPMENT AND SUPPLIES.
6.1 A schematic diagram of the sampling train is shown in Figure XXXX-1. This
sampling train configuration is adapted from SW 846 Method 0010 procedures. The sampling
train consists of the following components: Probe Nozzle, Pitot Tube, Differential Pressure
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METHOD XXXX
Gauge, Metering System, Temperature Sensor, Barometer, and Gas Density Determination
Equipment.
6.1.1 Probe Nozzle. Quartz or glass with sharp leading edge at a tapered
30° angle. The taper shall be on the outside to preserve a constant inner diameter. The
nozzle shall be of a buttonhook or elbow design. A range of nozzle sizes suitable for
isokinetic sampling should be available in increments of 0.16 cm (1/16 in), e.g.,0.32
to 1.27 cm (1/8 to 1/2 in), or larger if higher volume sampling trains are used. Each
nozzle shall be calibrated according to the procedures outlined in Section 10.1.
6.1.2 Probe Liner. Borosilicate or quartz-glass tubing with a heating system
capable of maintaining a probe gas temperature of 120 ± 14°C (248 ± 25 °F) at the
exit end during sampling. (The tester may opt to operate the equipment at a
temperature lower than that specified.) Because the actual temperature at the outlet of
the probe is not usually monitored during sampling, probes constructed according to
APTD-0581 and utilizing the calibration curves of APTD-0576 (or calibrated according
to the procedure outlined in APTD-0576) are considered acceptable. Either borosilicate
or quartz glass probe liners may be used for stack temperature up to about 480 °C
(900°F). Quartz glass liners shall be used for temperatures between 480 and 900°C
(900 and 1600°F). The softening temperature for borosilicate is 820°C (1508°F), and
for quartz glass 1500°C (2732°F). Water-cooling of the stainless steel sheath will be
necessary at temperatures approaching and exceeding 500°C.
6.1.3 Heated Filter. A glass or quartz filter, similar to that used with
Method 5, is used to collect paniculate material for subsequent extraction and analysis.
The filter is supported by a Teflon* filter support which is housed in an all-glass filter
holder. The filter is maintained at 120 ± 14°C (248 ± 25°F) during sampling.
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METHOD XXXX
6.1.4 Pitot Tube. Type S, as described in Section 2.1 of promulgated EPA
Method 2 (Section 6.1 of Reformatted Draft EPA Method 2), or other appropriate
devices (see Vollaro, 1976 in Section 16.0, References). The pitot tube shall be
attached to the probe to allow constant monitoring of the stack gas velocity. The
impact (high-pressure) opening plane of the pitot tube shall be even with or above the
nozzle entry plane (see EPA Method 2, Figure 6-2b) during sampling. The Type S
pitot tube assembly shall have a known coefficient, determined as outlined in
Section 4.0 of promulgated EPA Method 2 (Section 10.0 of Reformatted Draft EPA
Method 2).
6.1.5 Differential Pressure Gauge. Two inclined manometers or equivalent
devices as described in Section 2.2 of Promulgated EPA Method 2 (Section 6.2 of
Reformatted EPA Method 2). One manometer shall be used for velocity-head readings
and the other for orifice differential pressure (AH) readings.
6.1.6 Temperature Sensor. A temperature sensor capable of measuring
temperature to within ± 3°C (± 5.4°F) shall be installed so that the temperature at the
impinger outlet can be regulated and monitored during sampling.
6.1.7 Condenser. A coil type Graham condenser fabricated of borosilicate
glass, teflon®, or other inert material shall be used to cool the gas exiting the filter to a
temperature of 20°C (68°F) or less and condense any moisture before the sample
passes through the sorbent.
6.1.8 Sorbent Module. The sorbent module shall be fabricated of borosilicate
glass, Teflon® or other inert material sized to contain approximately 48 g of
Carboxen™-1000 (Supelco) and shall be jacketed to maintain the internal gas
temperature at 17±3°C(62.5±5.4°F). The most commonly used coolant is ice water
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METHOD XXXX
from the impinger ice-water bath, constantly circulated through the outer jacket, using
rubber or plastic tubing and a peristaltic pump. The sorbent module should be outfitted
with a glass well or depression, appropiately sized to accommodate a small
thermocouple in the trap for monitoring the gas entry temperature. The condenser and
sorbent module shall be oriented to direct the flow of condensate formed vertically
downward from the conditioning section, through the sorbent, and into the first
impinger of the impinger train.
6.1.9 Impinger Train. The sampling train requires a minimum of four 500 mL
impingers, connected in series immediately following the sorbent module, as shown in
Figure XXXX-1, with ground glass (or equivalent) vacuum-tight fittings. For the
second, third, and fourth impingers, use the Greenburg-Smith design, modified by
replacing the tip with a 1.27 cm (1/2 in.) inside diameter glass tube extending to
1.27 cm (1/2 in.) from the bottom of the flask. For the first impinger, use a
Greenburg-Smith impinger with a short stem. The second and third impingers contain
100 mL of DI water. The first impinger remains empty and the fourth impinger is
filled with a known amount (2/3 full) of desicant.
6.1.10 Metering System. The necessary components are a vacuum gauge, leak-
free pump, temperature sensors capable of measuring temperature within ±3°C
(±5.4°F), dry gas meter (DGM) capable of measuring volume to within 1%, and
related equipment as shown in Figure XXXX-1. At a minimum, the pump should be
capable of 113 liters per minute (L/min) (4 cubic feet per minute (cfm)) free flow, and
the DGM should have a recording capacity of 0-28.36 cubic meters (0-999.9 cubic feet)
with a resolution of 0.14 liters (0.005 cubic feet). Other metering systems may be used
which are capable of maintaining sample rates within 10% of isokinetic and of
determining sample volumes to within 2% of the actual value. The metering system
must be used in conjunction with a pilot tube to enable checks of isokinetic sampling
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METHOD XXXX
rates. Sampling trains using metering systems designed for flow rates higher than those
described in APTD-0581 and APTD-0576 may be used, provided that the specifications
of this method are met.
6.1.11 Barometer. Mercury, aneroid, or other barometer capable of measuring
atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
NOTE: The barometric pressure reading may be obtained from a nearby
National Weather Service Station. In this case, the station value (which is the absolute
barometric pressure) shall be requested and an adjustment for elevation differences
between the weather station and sampling point be made at a rate of minus 2.5 mm
(0.1 in.) Hg per 30 meters (100 ft.) elevation increase or plus 2.5 mm (0.1 in.) Hg per
30 meters (100 ft.) elevation decrease.
6.1.12 Gas Density Determination Equipment. Temperature sensor and
pressure gauge (as described in Sections 2.3 and 2.4 of Promulgated EPA Method 2 as
well as Sections 6.3 and 6.4 of Reformatted Method 2), and gas analyzer, if necessary,
as described in EPA Method 3. The temperature sensor shall, preferably, be
permanently attached to the pitot tube or sampling probe in a fixed configuration so that
the tip of the sensor extends beyond the leading edge of the probe sheath and does not
touch any metal. Alternatively, the sensor may be attached just prior to use in the field.
Note, however, that if the temperature sensor is attached in the field, the sensor must
be placed in an interference-free arrangement with respect to the Type S pitot openings
(as illustrated in Promulgated EPA Method 2, Figure 2-7, as well as Reformatted
Method 2, Figure 2-4). As a second alternative, if a difference of no more than 1 % in
the average velocity measurement is to be introduced, the temperature sensor need not
be attached to the probe or pitot tube. (This alternative is subject to the approval of the
Administrator.)
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METHOD XXXX
6.1.13 Viton® AO-ring.
6.1.14 Heat Resistant Tape.
6.1.15 Teflon® tape.
6.1.16 Silanized glass wool.
6.2 Sample Recovery. The following items are required for sample recovery.
6.2.1 Probe Liner and Probe Nozzle Brushes. Teflon® bristle brushes with
stainless steel wire or Teflon® handles are required. The probe brush must have
extensions of stainless steel, Teflon®, or inert material at least as long as the probe.
The brushes must be properly sized and shaped to brush out the probe liner and the
probe nozzle.
6.2.2 Wash Bottles. Three wash bottles are required. Teflon® or glass wash
bottles are recommended; polyethylene wash bottles should not be used because organic
contaminants may be extracted by exposure to organic solvents used for sample
recovery.
6.2.3 Graduated Cylinder and/or Balance. These will be used to measure
condensed water to the nearest 1 mL or 0.5 g. Graduated cylinders must have divisions
not >2 mL. Laboratory balances capable of weighing to ±0.5 g or better are
required.
6.2.4 Glass Sample Storage Containers. Chemically resistant borosilicate
amber glass bottles, 500 mL or 1000 mL. Bottles should be tinted to prevent
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METHOD XXXX
photochemical reactions. Screw-cap liners shall be either Teflon® or constructed to be
leak-free and resistant to chemical attack by organic solvents. Narrow-mouth glass
bottles have been found to exhibit less tendency toward leakage.
6.2.5 Plastic Storage Containers. Screw-cap polypropylene or polyethlene
containers to store silica gel.
6.2.6 Rubber Policeman and Funnel. To aid in the transfer of material into
and out of containers in the field.
6.2.7 Cooler. To store and ship sample containers.
6.2.8 Crushed Ice. Quantities ranging from 10-50 Ib may be necessary during
a sampling run, depending upon the temperature of ambient air and the moisture
content of the gas stream. Samples must be stored and shipped cold; sufficient ice for
this purpose must be allowed.
6.2.9 Stopcock Grease. The use of silicone grease is not permitted. Silicone
grease usage is not necessary if screw-on connectors and Teflon® sleeves or
ground-glass joints are used.
6.2.10 Impinger Solution. The impinger solution is organic-free reagent water.
This solution can be prepared in the laboratory or commercially-prepared organic-free
reagent water may be used.
6.3 Analysis.
6.3.1 Separatory Funnel. 1 L, with Teflon® stopcock.
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6.3.2 Concentrator Tube or Graduated Cylinder. 100 mL graduated or
equivalent. A ground glass stopper may be used to prevent evaporation of extracts.
6.3.3 Vials. 10, 100 mL, glass with Teflon® lined screw caps or crimp tops.
6.3.4 Analytical Balance. Capable of accurately weighing to the nearest
0.1 mg.
6.3.5 Glass Ampules. 1 mL in size. Used for storing stock acetonitrile
standard.
6.3.6 Gas Chromatograph.
6.3.6.1 Oven system. Capable of maintaining temperatures between
44 and 94 °C (111 and 201 °F) to within ±0.5 °C (±0.9 °F) and ramping at a
rate of 10°C/minute (18 °F/min).
6.3.6.2 Autosampler with 10 /xL syringe capable of injecting
1 to 7/xL.
6.3.6.3 Column. 0.5 mm ID x 30 m, 1.5 /xm film thickness,
DB-WAX (or equivalent).
6.3.6.4 Flame lonization Detector.
6.3.6.5 Strip Chart Recorder Compatible With Detector. Use of a
data system for measuring peak areas and retention times is recommended.
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METHOD XXXX
6.3.7 Volumetric Flasks.
6.3.8 Extraction Apparatus as shown in Figure XXXX-2. The extraction
apparatus consists of a solvent reservoir maintained at a height greater than the sorbent
module and connected to the sorbent module via a three-way valve.
7.0 REAGENTS AND STANDARDS.
7.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated,
all reagents shall conform to the specifications of the Committee on Analytical Reagents of the
American Chemical Society, where such specifications are available. Other grades may be
used, provided that the reagent is of sufficiently high purity to use without jeopardizing
accuracy.
7.2 Organic-free reagent water. All references to water in this method refer to
organic-free reagent water, as defined in Chapter One of SW-846 (see Reference 2 in
Section 16.0).
7.3 Silica Gel. Indicating type, 6-16 mesh. If the silica gel has been used
previously, dry at 180°C (350°F) for 2 hours before using. New silica gel may be used as
received. Alternatively, other types of desiccants (equivalent or better) may be used.
7.4 Carboxen^-lOOO. 45-60 mesh. Use as received from supplier.
7.4.1 Within 30 days of proposed use, pack three sorbent modules with 48 g of
CarboxenTW-1000. Hold the sorbent in place with silanized glass wool.
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METHOD XXXX
7.4.2 Extract the Carboxen™-1000 with methylene chloride and analyze the
extract as described in Section 11.1 and 11.5.
7.4.3 If the Carboxen™-1000 has passed the Quality Control criteria in
Section 9.2.4, the sorbent may be packed into sorbent modules, the sorbent modules
sealed, and then packaged to meet necessary shipping requirements and sent to the
sampling area. If the Quality Control criteria are not met the sorbent may be cleaned;
or, new sorbent may be purchased and the extraction sequence repeated.
7.4.4 If the sorbent is not used in the field within 30 days of being packed,
three sorbent modules may be taken and analyzed as described in Section 11.3. If the
sorbent meets the Quality Control requirements in Section 9.2.4, the sorbent may be
used. If the sorbent does not meet the Quality Control requirements in Section 9.2.4,
the sorbent must be cleaned or replaced with new sorbent that has been tested and
passed the Quality Control requirements in Section 9.2.4.
7.5 Field Spike Standard Preparation. To prepare an acetonitrile field spiking
standard at 3.94 mg/mL, use a 250 /xL gas-tight syringe to transfer 0.25 mL of acetonitrile
(0.787 g/mL) to a 50 mL volumetric flask containing approximately 50 mL of water. Dilute to
50 mL with water.
7.6 Methylene Chloride, CH2C12. Methylene chloride (suitable for residue and
pesticide analysis, GC/MS, HPLC, GC Spectrophotometry or equivalent) is required for
rinsing glassware, recovery of sample trains, and extracting sorbent samples.
7.7 Methanol, CH3OH. Methanol (HPLC grade or equivalent) is required for
recovery of sample trains.
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METHOD XXXX
7.8 Acetonitrile, CH3CN. Acetonitrile (HPLC grade or equivalent) is required for
preparing calibration standards and spiking standards.
7.9 Stock standard solutions.
7.9.1 Preparation of Calibration Standards for Chromatographic Analyses.
7.9.1.1 Stock Acetonitrile and Propionitrile Standards. Prepare stock
acetonitrile and propionitrile standards at a concentration of 2 mg/mL by
weighing 100 mg (± 0.1 mg) of acetonitrile and 100 mg (±0.1 mg) of
propionitrile into 100 mL volumetric flasks and diluting to the line with
methylene chloride (flask 1) and methanol (flask 2). From these stock solutions,
prepare the calibration standards. Transfer the solutions to vials with Teflon®-
lined caps and store at 4°C (39°F).
7.9.1.2 Calibration Standards. Prepare calibration standards by
diluting 45, 180, 450, 2500, 4500, and 22,500 /xL of the acetonitrile and
propionitrile stock solutions to 50 mL with methylene chloride or methanol to
provide standard curves with calibration points at 1,4, 10, 50, 100, and
500 /xg/mL of acetonitrile.
7.9.1.3 Check Standards. Prepare check standards of 80 /xg/mL of
acetonitrile by taking 2 mL of a separately prepared 2 mg/mL acetonitrile stock
standard and diluting to 50 mL with methylene chloride or methanol.
7.9.2 Standard solutions must be replaced after six months, or sooner if
comparison with check standards indicates a problem.
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METHOD XXXX
7.10 Surrogate standard preparation.
Prepare a surrogate standard at a concentration of 10 mg/mL by weighing
500 mg (±0.1 mg) of propionitrile into a 50 mL volumetric flask and diluting to the
line with water. Transfer the surrogate standard to bottles with Teflon®-lined screw
caps and store at 4 ± 2°C.
8.0 SAMPLE COLLECTION, PRESERVATION, STORAGE AND TRANSPORT.
8.1 Because of the complexity of this method, field personnel should be trained in
and experienced with the stationary source test procedures in order to obtain reliable results.
8.2 Laboratory Preparation.
8.2.1 All the components must be maintained and calibrated according to the
procedure described in APTD-0576 (Reference 3 in Section 16.0), unless otherwise
specified.
8.2.2 Weigh several 200 to 300 g portions of silica gel to the nearest 0.5 g and
place the silica gel in airtight containers. Record on each container the total weight of
the silica gel plus containers. As an alternative to preweighing the silica gel, it may be
weighed directly in the impinger just prior to train assembly.
8.3 Preliminary Field Determinations.
8.3.1 Select the sampling site and the minimum number of sampling points
according to EPA Method 1 or other relevant criteria. Determine the stack pressure,
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METHOD XXXX
temperature, and range of velocity heads using EPA Method 2. Check the pitot lines
for leaks according to Promulgated EPA Method 2, Section 3.1 (Reformatted EPA
Method 2, Section 8.1). Determine the stack gas moisture content using EPA
Approximation Method 4 or its alternatives to establish estimates of isokinetic
sampling-rate settings. Determine the stack gas dry molecular weight, as described in
Promulgated EPA Method 2, Section 3.6 (Reformatted EPA Method 2, Section 8.6). If
integrated EPA Method 3 sampling is used for molecular weight determination, the
integrated bag sample shall be taken simultaneously with, and for the same total length
of time as, the sample run.
8.3.2 Select a nozzle size based on the range of velocity heads so that it is not
necessary to change the nozzle size in order to maintain isokinetic sampling rates.
During the sampling run, do not change the nozzle. Ensure that the proper differential
pressure gauge is chosen for the range of velocity heads encountered (as described in
Section 2.2 of Promulgated EPA Method 2, as well as Section 8.2 of Reformatted EPA
Method 2).
8.3.3 Select a suitable probe liner and probe length so that all traverse points
can be sampled. For large stacks, to reduce the length of the probe, consider sampling
from opposite sides of the stack.
8.3.4 Select a total sampling time greater than or equal to the minimum total
sampling time specified in the test procedures for the specific industry. A total
sampling time must be selected so that (1) the sampling time per point is not less than 2
minutes (or some greater time interval as specified by the Administrator), and (2) the
sample volume taken (corrected to standard conditions) will exceed the required
minimum total gas sample volume. The latter is based on an approximate average
sampling rate.
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METHOD XXXX
8.3.5 The sampling time at each point shall be the same. It is recommended
that the number of minutes sampled at each point be an integer or an integer plus one-
half minute, in order to avoid timekeeping errors.
8.3.6 In some circumstances (e.g., batch cycles) it may be necessary to sample
for shorter times at the traverse points and to obtain smaller gas-volume samples. In
these cases, careful documentation must be maintained in order to allow accurate
concentration calculation.
8.4 Preparation of Collection Train.
8.4.1 During preparation and assembly of the sampling train, keep all openings
where contamination can occur covered with Teflon® film or aluminum foil until just
prior to assembly or until sampling is about to begin.
8.4.2 Place 100 mL of organic free water in the second and third impingers.
Leave the first impinger empty. Transfer approximately 200 to 300 g of pre-weighed
silica gel from its container to the fourth impinger. Be careful to ensure that the silica
gel is not entrained and carried out from the impinger during sampling. Place the silica
gel container in a clean place for later use in the sample recovery. Alternatively, the
weight of the silica gel plus impinger may be determined to the nearest 0.5 g and
recorded. For moisture determination, weigh all of the impingers after filling them
with reagent.
8.4.3 When glass probe liners are used, install the selected nozzle using a
Viton*-A O-ring when stack temperatures are <260°C (SOOT) and a woven
glass-fiber gasket when temperatures are higher. See APTD-0576 (Rom, 1972) for
details. Other connection systems utilizing either 316 stainless steel or Teflon® ferrules
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METHOD XXXX
may be used. Mark the probe with heat-resistant tape or by some other method to
denote the proper distance into the stack or duct for each sampling point.
8.4.4 Assemble the train as shown in Figure XXXX-1. During assembly, do
not use any silicone grease on ground-glass joints upstream of the impingers. Use
Teflon® tape, if required. A very light coating of silicone grease may be used on
ground-glass joints downstream of the impingers, but the silicone grease should be
limited to the outer portion of the ground-glass joints to minimize silicone grease
contamination. See APTD-0576 (Rom, 1972) for details. If necessary, Teflon® tape
may be used to seal leaks. Connect all temperature sensors to an appropriate
potentiometer/display unit. Check all temperature sensors at ambient temperatures.
8.4.5 Place crushed ice around the impingers.
8.4.6 Turn on and set the probe heating system at the desired operating
temperature. Allow time for the temperature to stabilize.
8.5 Leak-Check Procedures.
8.5.1 Pre-test Leak Check.
8.5.1.1 A pre-test leak check is not required but is highly
recommended.
8.5.1.2 After the sampling train has been assembled, turn on and set
the probe heating system to the desired operating temperature. Allow time for
the temperature to stabilize. If a Viton® A O-ring or other leak-free connection
is used in assembling the probe nozzle to the probe liner, leak-check the train at
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METHOD XXXX
the sampling site by plugging the nozzle and pulling a 381 mm Hg (15 in. Hg)
vacuum. Leakage rates in excess of 4% of the average sampling rate or
>0.00057 mVmin (0.020 cfm), whichever is less, are unacceptable.
NOTE: A lower vacuum pressure may be used, provided that the
lower vacuum pressure is not exceeded during the test.
8.5.1.3 If a heat resistant string is used, do not connect the probe to
the train during the leak check. Instead, leak-check the train by first attaching a
carbon-filled leak check impinger to the inlet and then plugging the inlet and
pulling a 381 mm Hg (15 in. Hg) vacuum. (A lower vacuum pressure may be
used if this lower vacuum pressure is not exceeded during the test.) Next,
connect the probe to the train and leak-check at approximately 25 mm Hg
(1 in. Hg) vacuum. Alternatively, leak-check the probe with the rest of the
sampling train in one step at 381 mm Hg (15 in. Hg) vacuum. Leakage rates in
excess of (a) 4% of the average sampling rate or (b) > 0.00057 m3/min
(0.020 cfm), are unacceptable.
8.5.1.4 The following leak check instructions for the sampling train
described in APTD-0576 and APTD-0581 (References 3 and 4 of Section 16.0,
respectively) may be helpful. Start the pump with the fine-adjust valve fully
open and coarse-adjust valve completely closed. Partially open the coarse-adjust
valve and slowly close the fine-adjust valve until the desired vacuum is reached.
Do not reverse direction of the fine-adjust valve, as liquid will back up into the
train. If the desired vacuum is exceeded, either perform the leak check at this
higher vacuum or end the leak check, as shown below, and start over.
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METHOD XXXX
8.5.1.5 When the leak check is completed, first slowly remove the
plug from the inlet to the probe. When the vacuum drops to 127 mm (5 in. Hg)
or less, immediately close the coarse-adjust valve. Switch off the pumping
system and reopen the fine-adjust valve. Do not reopen the fine-adjust valve
until the coarse-adjust valve has been closed to prevent the liquid in the
impingers from being forced backward in the sampling line and silica gel from
being entrained backward into the third impinger.
8.5.2 Leak Checks During Sampling Run.
8.5.2.1 If, during the sampling run, a component change
(i.e., impinger) becomes necessary, conduct a leak check immediately after the
interruption of sampling and before the change is made. Conduct the leak check
according to the procedure described in Section 8.5.1, but conduct it at a
vacuum greater than or equal to the maximum value recorded up to that point in
the test. If the leakage rate is found to be no greater than 0.00057 nvVmin
(0.020 cfm) or 4% of the average sampling rate (whichever is less), the results
are acceptable and no correction will need to be applied to the total volume of
dry gas metered. If a higher leakage rate is obtained, void the sampling run.
NOTE: Any correction of the sample volume by calculation reduces
the integrity of the pollutant concentration data generated and must be avoided.
8.5.2.2 Immediately after a component change and before sampling is
reinitiated, conduct a leak check similar to a pre-test leak check.
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METHOD XXXX
8.5.3 Post-test Leak Check.
8.5.3.1 A leak check of the sampling train is mandatory at the
conclusion of each sampling run. Conduct the leak check in accordance with the
same procedures as the pre-test leak check, except conduct the post-test leak
check at a vacuum greater than or equal to the maximum value reached during
the sampling run. If the leakage rate is found to be no greater than
0.00057 m3/min (0.020 cfm) or 4% of the average sampling rate (whichever is
less), the results are acceptable. If, however, a higher leakage rate is obtained,
record the leakage rate, correct the sample volume (as shown in Section 12.0 of
this method) , formally note that this correction has been made to the data, and
consider the data obtained of questionable reliability, or void the sampling run.
8.6 Sampling Train Operation.
8.6.1 During the sampling run, maintain an isokinetic sampling rate to within
10% of true isokinetic, below 28 L/min (1.0 cfm). Maintain a temperature around the
probe of 120° ± 14°C (248° ± 25°F).
8.6.2 For each run, record the data on a data sheet such as the one shown in
Figure XXXX-3. Be sure to record the initial DGM reading. Record the DGM
readings at the beginning and end of each sampling time increment, when changes in
flow rates are made, before and after each leak check, and when sampling is halted.
Take other readings indicated by Figure XXXX-3 at least once at each sample point
during each time increment and additional readings when significant adjustments (20%
variation in velocity head readings) necessitate additional adjustments in flow rate.
Level and zero the manometer. Because the manometer level and zero may drift due to
vibrations and temperature changes, make periodic checks during the traverse.
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METHOD XXXX
8.6.3 Clean the stack access portholes prior to the test run to eliminate the
chance of collecting deposited material. To begin sampling, remove the nozzle cap,
verify that the probe heating systems are at the specified temperature, and verify that
the pilot tube and probe are properly positioned. Position the nozzle at the first
traverse point with the tip pointing directly into the gas stream. Immediately start the
pump and adjust the flow to isokinetic conditions. Nomographs, which aid in the rapid
adjustment of the isokinetic sampling rate without excessive computations, are
available. These nomographs are designed for use when the Type S pitot tube
coefficient is 0.84 ± 0.02 and the stack gas equivalent density (dry molecular weight)
is equal to 29 ± 4. APTD-0576 (Reference 3 in Section 16.0) details the procedure for
using the nomographs. If the stack gas molecular weight and the pitot tube coefficient
are outside the above ranges, do not use the nomographs unless appropriate steps are
taken to compensate for the deviations.
8.6.4 When the stack is under significant negative pressure (equivalent to the
height of the impinger stem), take care to close the coarse adjust valve before inserting
the probe into the stack in order to prevent liquid from backing up into the probe. If
necessary, the pump may be turned on with the coarse adjust valve closed.
8.6.5 When the probe is in position, block off the openings around the probe
and stack access porthole to prevent unrepresentative dilution of the gas stream.
8.6.6 Traverse the stack cross-section, as required by EPA Method 1. To
minimize the chance of extracting deposited material be careful not to bump the probe
nozzle into the stack walls when sampling near the walls when removing or inserting
the probe through the access porthole.
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METHOD XXXX
8.6.7 During the test run, make periodic adjustments to keep the temperature
of the probe and the heated filter at the proper levels. Add more ice and, if necessary,
salt, to maintain a temperature of <20°C (68°F) at the silica gel outlet. Also,
periodically check the level and zero of the manometer.
8.6.8 A single train shall be used for the entire sampling run, except in cases
where simultaneous sampling is required in two or more separate ducts; at two or more
different locations within the same duct; or, in cases where equipment failure
necessitates a change of trains. Additional train(s) may also be used for sampling when
the capacity of a single train is exceeded.
8.6.9 When two or more trains are used, components from each train shall be
analyzed. If multiple trains have been used because the capacity of a single train would
be exceeded, first impingers from each train may be combined, and second impingers
from each train may be combined.
8.6.10 At the end of the sampling run, turn off the coarse adjust valve, remove
the probe and nozzle from the stack, turn off the pump, record the final dry gas meter
reading, and conduct a post-test leak check as outlined in Section 8.5.3. Also, leak
check the pitot lines as described in EPA Method 2 (Section 8.1 of Reformatted Method
2). The lines must pass this leak check in order to validate the velocity-head data.
8.6.11 Calculate percent isokinetic variation (as described in Section 6.11 of
Method 5, as well as see Section 12.11 of Reformatted Method 5) to determine whether
the run was valid or another test should be performed.
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METHOD XXXX
8.7 Sample Recovery.
8.7.1 Preparation.
8.7.1.1 Proper cleanup procedure begins as soon as the probe is
removed from the stack at the end of the sampling period. Allow the probe to
cool. When the probe can be handled safely, wipe off all external particulate
matter near the tip of the probe nozzle and place a cap over the tip to prevent
losing or gaining particulate matter. Do not cap the probe tip tightly while the
sampling train is cooling because a vacuum will be created drawing liquid from
the impingers back through the sampling train.
8.7.1.2 Before moving the sampling train to the cleanup site, remove
the probe from the sampling train and cap the open outlet, being careful not to
lose any condensate that might be present. Remove the umbilical cord from the
last impinger and cap the impinger. If a flexible line is used, let any condensed
water or liquid drain into the impingers. Cap off any open impinger inlets and
outlets. Ground glass stoppers, Teflon® caps, or caps of other inert materials
may be used to seal all openings.
8.7.1.3 Transfer the probe and impinger assembly to an area that is
clean and protected from wind so that the chances of contaminating or losing the
sample are minimized.
8.7.1.4 Inspect the train before and during disassembly, and note any
abnormal conditions.
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METHOD XXXX
8.7.1.5 Save a portion of all washing solutions (methylene chloride,
methanol, water) used for cleanup as a reagent blank. Transfer 200 mL of each
solution directly from the wash bottle and place each in a separate prelabeled
sample "reagent blank" container (see Section 8.7.3).
8.7.2 Sample Containers.
8.7.2.1 Container 1. Using two people, rinse the probe/nozzle with
1:1 methylene chloride:methanol by tilting and rotating the probe while
squirting solvent into the upper end so that all of the surfaces are wetted with
the rinse solution. Let the solvent drain into the container. If paniculate is
visible, use a Teflon® brush to loosen and remove the paniculate material and
follow with a second rinse. After the rinses have been collected, seal the
container and add the proper label.
8.7.2.1.1 Carefully remove the probe nozzle and rinse the inside
surface with 1:1 methylene chloride:methanol from a wash bottle. Brush
with a Teflon® bristle brush, and rinse until the rinse shows no visible
particles. Make a final rinse of the inside surface. Brush and rinse the
inside parts of the Swagelok® fitting with 1:1 methylene
chloride:methanol the same way.
8.7.2.1.2 Rinse the probe liner with 1:1 methylene
chloride:methanol. While squirting the 1:1 methylene chloride:methanol
into the upper end of the probe, tilt and rotate the probe so that all inside
surfaces will be wetted with rinse solvent. Let the rinse solvent drain
from the lower end into the sample container. The tester may use a
funnel (glass) to aid in transferring the liquid washes to the container.
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METHOD XXXX
Follow the rinse with a Teflon® brush. Hold the probe in an inclined
position, and squirt rinse solvent into the upper end as the probe brush is
being pushed with a twisting action through the probe. Hold the sample
container underneath the lower end of the probe, and catch any rinse
solvent, water, and paniculate matter that is brushed from the probe.
Run the brush through the probe three times or more. Rinse the brush
with rinse solvent, and quantitatively collect these washings in the
sample container. After the brushing, make a final rinse of the probe as
described above.
NOTE: Two people should clean the probe in order to
minimize sample losses. Between sampling runs, brushes must be kept
clean and free from contamination.
8.7.2.1.3 After all rinse solvent washings and paniculate matter
have been collected in the sample container, tighten the lid so the solvent
will not leak out when the container is shipped to the laboratory. Mark
the height of the fluid level to determine whether leakage occurs during
transport. Seal the container with Teflon® tape. Label the container
clearly to identify its contents.
8.7.2.2 Container 2. Disassemble the filter holder and carefully
remove the filter with Teflon® tweezers and place in a precleaned glass bottle.
Cover the filter with 150 rnL of 1:1 methylene chloride rmethanol, add the
proper label, and seal with Teflon® tape. Rinse the front half of the filter
holder, the filter support, and any other connecting glass pieces with 1:1
methylene chloride:methanol and add the rinses to Container No. 1. Mark the
liquid level in Container No. 1 and seal for shipment.
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METHOD XXXX
8.7.2.3 Container 3. Rinse the back half of the filter holder with
methanol and add to Container No. 3. Mark the liquid level, seal the container,
and add the proper sample label.
8.7.2.4 Container No. 4. Seal the sorbent module with ground glass
plugs held in place with clamps. Add the proper label and seal the sorbent
module in a plastic bag.
8.7.2.5 Container No. 5. Pour the contents of Impinger No. 1 (the
condensate knockout) into Container No. 5 along with the methanol rinses of the
impinger. Mark the liquid level, seal the container, and add the proper sample
label.
8.7.2.6 Container No. 6. Pour the contents of Impingers No. 2 and 3
along with the respective rinses into Container No. 6. Mark the liquid level,
seal the container, and add the proper label.
8.7.3 Reagent Blanks. Prepare reagent blanks by transferring 200 mL
of organic free water and 200 mL of each wash solvent to separate amber glass
jars. Process the reagent blanks in the same manner as the samples.
8.7.4 Moisture determination. If a moisture determination is to be
made, measure the volume (or weight) gain of each impinger as well as the
impinger containing the silica gel before transferring the contents to the sample
containers.
8.7.5 Sample preparation for shipment. Prior to shipment, recheck all
sample containers to ensure that the caps are well secured. Seal the lids with
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METHOD XXXX
Teflon® tape. Ship all samples upright, packed in ice, using the proper shipping
materials as prescribed for hazardous materials.
9.0 QUALITY CONTROL.
9.1 Sampling. Sampling quality control procedures are listed in Table XXXX-2.
See APTD-0576 (Reference 3 in Section 16.0) for additional Method 5 quality control.
9.2 Analysis. The quality assurance program required for this method includes the
analysis of the field, reagent and method blanks, procedure validations, and analysis of field
spikes.
The assessment of combustion data and positive identification and quantitation of
acetonitrile depend on the integrity of the samples received and the precision and accuracy of
the analytical methodology. Quality assurance procedures for this method are designed to
monitor the performance of the analytical methodology and to provide the required information
to take corrective action if problems are observed in laboratory operations or in field sampling
activities. Table XXXX-3 lists laboratory quality control procedures.
9.2.1 Field Train Blanks. Field train blanks must be submitted with the
samples collected at each sampling site. The field train blanks include the sample
bottles containing aliquots of sample recovery solvents, methylene chloride, methanol,
and water, and unused filter and sorbent. At a minimum, assemble one complete
sampling train in the field staging area, take it to the sampling area, and leak-check it at
the beginning and end of the testing (or for the same total number of times as the actual
sampling train). Heat the probe of the blank train during the sample test. Recover the
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METHOD XXXX
TABLE XXXX-2. SAMPLING QUALITY CONTROL PROCEDURES
Criteria
Control Limits"
Corrective Action
Final Leak Rate
Dry Gas Meter Calibration
Individual Correction
Factor (y)
Average Correction Factor
Intermediate Dry Gas Meter
Analytical Balance (top
loader)
Barometer
<0.00057 m3/min or 4% of
sampling rate, whichever is
less.
Post average factor agrees
±5% of pre-factor.
Agree within 2% of average
factor.
1.00 ± 1%.
Calibrated every six months
against EPA standard.
0. Ig of ASTM Class 1
(NIST Class S) Weights.
Within 2.55 mm Hg of
mercury-in-glass barometer.
None: Results are
questionable and should be
compared with other train
results.
Adjust sample volumes using
the factor that gives the
smallest volume.
Redo correction factor.
Adjust the dry gas meter and
recalibrate.
Repair balance and
recalibrate.
Recalibrate.
aControl limits are established based on previous test programs conducted by the EPA.
XXXX-31
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METHOD XXXX
TABLE XXXX-3. LABORATORY QUALITY CONTROL PROCEDURES
FOR GC/FID ANALYSES
Parameter
Linearity Check
Retention Time
Quality
Control Check
Run 5-point
curve.
Analyze check
standard.
Frequency
At setup or when
check standard is
out-of-range.
1/10 samples.
Acceptance Criteria
Correlation coefficient
*0.995.
Within three standard
deviations of average
calibration relative
retention time.
Corrective Action
Check integration, reintegrate
If necessary recalibrate.
Check instrument function for
plug, leak, etc. Change
septum.
Calibration Check Analyze check 1/10 samples
standard. minimum 2/set.
System Blank
Method Spike/
Method Spike
Duplicate"
Analyze
solvent.
1/10 samples
minimum 2/set.
Analyze extract I/set or
of spiked 1/20 samples.
sorbent
Matrix Analyze spiked I/set or 1/20
Spike/Matrix samples. samples
Spike Duplicate6
Replicate
Samples6
Replicate
Analyses
Method Blank
Surrogate
Recoveries
Analyze I/set or 1/10
duplicate nonsorbent
sample aliquot samples
Re-inject
sample.
1/10 samples or
I/set
Extract blank I/set or 1/20
sorbent, filter, samples
Spike samples
with surrogate
Every sample
±15% of calibration
curve.
20% of lowest
standard.
±20% of spiked
amount.
±50% of spiked
amount
±20% of first aliquot
±15% of first
injection
20% of lowest
standard
±50% of spiked
amount1
±25% of spiked
amount6
Check integration, remake
standard. Or recalibrate.
Locate source of
contamination; reanalyze.
Check integration, check
instrument function,
reanalyze, reprepare if
possible.
Check integration, check
instrument function,
reanalyze, reprepare if
possible.
Check integration, check
instrument function,
reanalyze, reprepare if
possible.
Check integration, check
instrument function,
reanalyze.
Locate source of
contamination, reanalyze,
reprepare if possible.
Check integration, check
instrument function,
reanalyze.
'Applicable to sorbent extract samples only.
""Applicable to nonsorbent samples only.
XXXX - 32
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METHOD XXXX
train as if it were an actual test sample. Do not pass any gaseous sample through the
blank sampling train.
9.2.2 Field Trip and Field Reagent Blanks. Collect field reagent blanks of
recovery solvents and unused filters and sorbent modules packed with Carboxen™-1000
(field trip blanks) in the field as separate samples and return them to the laboratory for
analysis to evaluate artifacts that may be observed in the actual samples.
9.2.3 Laboratory Method Blanks. Prepare a method blank for each set of
analytical operations to evaluate contamination and artifacts that can be derived from
glassware, reagents, and sample handling in the laboratory.
9.2.4 Field Spike. Introduce 1 mL of the Field Spike Standard into a sorbent
module containing 48 g of Carboxen™-1000 using a syringe with a needle that is long
enough to pentrate the sorbent bed. Follow standard sorbent recovery procedures and
use the spike as a check on field handling and recovery procedures. Retain an aliquot
of the field spike standard in the laboratory for comparative analysis.
9.2.5 Preparation of Carboxen™-1000 Sorbent. Pack the sorbent modules
with 48 g of Carboxen™-1000. Use the sorbent as it is received from the
manufacturer. Randomly select a minimum of six of the packed sorbent modules. To
ensure that the background in the sorbent is acceptable for field use, extract and analyze
at least three of the sorbent modules according to the procedure in Section 11 before
collecting samples. Save the other three (or more) sorbent modules for use as
laboratory method blanks when the analysis is performed.
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METHOD XXXX
10.0 CALIBRATION AND STANDARDIZATION.
NOTE: Maintain a laboratory log of all calibrations.
10.1 Probe Nozzle. Calibrate probe nozzles before their initial use in the field.
Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025 mm
(0.001 in.). Make measurements at three separate places across the diameter and obtain the
average of the measurements. The difference between the high and low numbers shall not
exceed 0.1 mm (0.004 in.). When the nozzles become nicked, dented, or corroded, replace
them. Permanently and uniquely identify each nozzle.
10.2 Pilot Tube Assembly. Calibrate the Type S pilot tube assembly according to the
procedure outlined in Seclion 4 of Promulgated EPA Melhod 2 (Seclion 10.1 of Reformatted
Meihod 2), or assign a nominal coefficieni of 0.84 if il is nol visibly nicked or corroded, and,
if il meels design and inlercomponeni spacing specificaiions.
10.3 Melering Sysiem.
10.3.1 Calibralion Prior lo Use. Before ils inilial use in Ihe field, calibrate
the metering system according lo the procedure outlined in APTD-0576 (Reference 3 of
Seclion 16.0). Instead of physically adjusling the DGM dial readings to correspond lo
Ihe wel-lesl meter readings, calibralion faclors may be used lo correcl Ihe gas meter dial
readings malhemalically lo the proper values. Before calibrating the metering system,
il is suggested that a leak check be conducted. For metering systems having diaphragm
pumps, a leak check procedure may nol delecl leaks wilhin Ihe pump. For these cases,
use the following leak check procedure. Make a ten-minute calibralion run ai 0.00057
nrVmin (0.020 cftn). Al Ihe end of Ihe run, take the difference of the measured wet-lesl
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METHOD XXXX
and dry-gas meter volumes and divide the difference by 10 to get the leak rate. The
leak rate should not exceed 0.00057 nrVmin (0.020 cfm).
10.3.2 Calibration After Use. After each field use, check the calibration of
the metering system by performing three calibration runs at a single intermediate orifice
setting (based on the previous field test). Set the vacuum at the maximum value
reached during the test series. To adjust the vacuum, insert a valve between the wet-
test meter and the inlet of the metering system. Calculate the average value of the
calibration factor. If the value has changed by more the 5%, recalibrate the meter over
the full range of orifice settings, as outlined in APTD-0576 (Reference 3 of
Section 16.0).
10.3.3 Leak check of metering system. Leak check the portion of the
sampling train from the pump to the orifice meter (see Figure XXXX-1) prior to initial
use and after each shipment. Leakage after the pump will result in less volume being
recorded than is actually sampled. Use the following procedure. Close the main valve
on the meter box. Insert a one-hole rubber stopper with rubber tubing attached into the
orifice exhaust pipe. Disconnect and vent the low side of the orifice manometer. Close
off the low side orifice tap. Pressurize the system to 13 - 18 cm
(5 - 7 in.) water column by blowing into the rubber tubing. Pinch off the tubing and
observe the manometer for 1 minute. A loss of pressure on the manometer indicates a
leak in the meter box. Leaks must be corrected.
NOTE: If the DGM coefficient values obtained before and after a test series
differ by > 5 %, either the test series must be voided or calculations for the test series
must be performed using whichever meter coefficient value (i.e., before or after) gives
the lower value of total sample volume.
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METHOD XXXX
10.4 Probe Heater. Calibrate the probe heating system before its initial use in the
field according to the procedure outlined in APTD-0576 (Reference 3 of Section 16.0). Probes
constructed according to APTD-0581 (Reference 4 of Section 16.0) need not be calibrated if
the calibration curves in APTD-0576 (Reference 3 of Section 16.0) are used.
10.5 Temperature Sensors. Each temperature sensor must be permanently and
uniquely marked on the casing. All mercury-in-glass reference thermometers must conform to
ASTM E-l 63C or 63F specifications. Temperature sensors should be calibrated in the
laboratory with and without the use of extension leads. If extension leads are used in the field,
the temperature sensor readings at the ambient air temperatures, with and without the extension
lead, must be noted and recorded. Correction is necessary if using an extension lead produces
a change > 1.5%.
10.5.1 Impinger and DGM Temperature Sensors. For the temperature sensors
used to measure the temperature of the gas leaving the impinger train, a three-point
calibration at ice water, room air, and boiling water temperatures is necessary. Accept
the temperature sensors only if the readings at all three temperatures agree to ± 2°C
(± 3.6°F) with those of the absolute value of the reference thermometer.
10.5.2 Probe and Stack Temperature Sensor. For the temperature sensors
used to indicate the probe and stack temperatures, conduct a three-point calibration at
ice water, boiling water, and hot oil bath temperatures. Use of a point at room air
temperature is recommended. The thermometer and thermocouple must agree to within
1.5% at each of the calibration points. A calibration curve (equation) may be
constructed (calculated) and the data extrapolated to cover the entire temperature range
suggested by the manufacturer.
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METHOD XXXX
10.6 Barometer. Adjust the barometer initially and before each test series to agree to
within ±2.5 mm Hg (0.1 in. Hg) of the mercury barometer or the correct barometric pressure
value reported by a nearby National Weather Service Station (same altitude above sea level).
10.7 Top-Loading Electronic Balance. Calibrate the balance before each test series,
using ASTM Class 1 (NIST Class S) standard weights. The weights must be within ±0.5% of
the standards, or the balance must be adjusted to meet these limits.
10.8 Analytical Calibration.
10.8.1 Establish GC/FID operating parameters to produce a retention time
equivalent to that indicated in Table XXXX-1. Suggested chromatographic conditions
are provided in Section 11.4. Prepare calibration standards according to the procedure
in Section 7.9.1. Calibrate the chromatographic system using the external standard
technique.
10.8.2 External Standard Calibration Procedure.
10.8.2.1 Analyze each calibration standard using the
chromatographic conditions listed in Section 11.2, and tabulate peak area against
concentration injected. The results may be used to prepare a calibration curve
for acetonitrile.
10.8.2.2 The working calibration curve must be verified on
each working day by the measurement of the calibration check standard. If the
response for any analyte varies from the previously established responses by
more than 15% (see Table XXXX-3), the test must be repeated using a fresh
calibration standard, but only after it is verified that the analytical system is in
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METHOD XXXX
control. Alternatively, a new calibration curve may be prepared for that
compound. If an autosampler is available, it is convenient to prepare a
calibration curve daily by analyzing standards along with test samples.
10.8.2.3 Periodically use the check standard prepared in
Section 7.9.1.3 to check the instrument response and calibration curve.
11.0 PROCEDURES.
11.1 Extraction of Sorbent Samples.
11.1.1 With the glass wool in place, spike the sorbent trap with 1 mL of the
surrogate spiking solution prepared according to the procedure in Section 7.10. Use a
syringe with a needle long enough to pentrate the glass wool and enter the sorbent bed.
Do not spike the solution on the glass wool.
11.1.2 Connect the bottom of the sorbent module (the end with the glass frit)
to the solvent module and connect the top of the sorbent module to the graduated
container used to collect the extract.
11.1.3 Fill the solvent reservoir with methylene chloride.
11.1.4 Fill the solvent transfer line with solvent by opening the valve on the
solvent reservoir and turning the three-way valve to the waste stream.
11.1.5 Fill the sorbent module with methylene chloride by turning the
three-way valve to the sorbent module.
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METHOD XXXX
11.1.6 Elute the methylene chloride through the sorbent module and collect it
in the graduated container. After 70 mL of extract is collected, close the valve on the
solvent reservoir.
11.1.7 Remove the extract transfer line from the graduated extract container
and measure and record the volume of the extract.
11.1.8 Transfer the extract to a glass vial with a Teflon®-lined screw cap and
store at 4 ±2°C.
11.1.9 Turn the three-way valve to the waste stream so that the solvent in the
sorbent module can drain. Remove the extracted sorbent module from the extraction
apparatus.
11.2 Preparation of Filter Samples.
11.2.1 Transfer to a vial a 2 mL aliquot of the methylene chloride solution
used to immerse the filter during sample recovery.
11.2.2 Spike the aliquot with 100 jig of propionitrile (10 jiL of 10 mg/mL
surrogate standard).
11.2.3 Filter the aliquot through a 0.45 /xm filter.
11.2.4 Transfer the aliquot to an autosampler vial and store at 4°C (39°F)
until analysis.
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METHOD XXXX
11.3 Preparation of Condensate and Rinse Samples.
11.3.1 Determine the sample volume by measuring the sample volume or by
using the sample weight and density.
11.3.2 Transfer a 1 mL aliquot to an autosampler vial.
11.3.3 Spike the aliquot with 100 fig of propionitrile (10 /zL of 10 mg/mL
surrogate standard).
11.3.4 Transfer the aliquot to an autosampler vial and store at 4°C (39°F)
until analysis.
11.4 Chromatographic Conditions.
Column: DB-WAX (0.53 mm ID x 30 m, 1.5 /zm film), or
equivalent
Makeup Gas: Helium
Column Temperature Initial 44 °C
Program: Hold for 3 minutes
Ramp at 10°C/minute
Final 124 °C
Hold for 2 minutes
Detector: Flame lonization at 300°C
Flow Rate: 5 mL/min carrier
30 mL/min makeup
Injection Volume: 1 (iL standards and extracts
3 fiL condensates and rinses
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METHOD XXXX
Retention Time: 4.8 minutes Acetonitrile
5.2 minutes Propionitrile
11.5 Analysis.
11.5.1 Analyze samples by GC/FID using conditions established in
Section 11.4. Table XXXX-1 lists the retention times and MDLs that were obtained
under these conditions. Other GC columns, chromatographic conditions, or detectors
may be used if the requirements for Section 9.2. are met, or if the data are within the
limits described in Table XXXX-1.
11.5.2 The width of the retention time window used to make identifications
should be based upon measurements of actual retention time variations of standards
over the course of a day. Three times the standard deviation of a retention time for a
compound can be used to calculate a suggested window size. However, the experience
of the analyst should weigh heavily in the interpretation of the chromatograms.
11.5.3 If the peak area exceeds the linear range of the calibration curve, a
smaller sample volume should be used. Alternatively, the final solution may be diluted
with methylene chloride or methanol and reanalyzed.
11.5.4 If the peak area measurement is prevented by the presence of observed
interferences, further cleanup is required. However, no method has been evaluated for
this procedure.
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METHOD XXXX
12.0 DATA ANALYSIS AND CALCULATIONS.
Carry out calculations, retaining at least one extra decimal figure beyond that of the
acquired data. Round off figures after final calculations.
12.1 Nomenclature:
An
ACNC
ACNT
Cf
DF
MVOL
Pbar
PS
PSU,
m(sid)
Cross-sectional area of nozzle, m2 (ft2)
Concentration of acetonitrile in sample (/zg/mL)
Total acetonitrile in sample (/xg)
Water va[pr om tje gas stream, proportion by volume
Concentration of acetonitrile in stack gas (mg/dscm)
Dilution factor
Total volume of sample or MeCl2 extract (mL)
Barometric pressure at the sampling site, mm Hg (in. Hg)
Absolute stack-gas pressure, mm Hg (in. Hg)
Standard absolute pressure, 760 mm Hg (29.92 in. Hg)
Absolute average dry-gas meter temperature, K (°R)
Absolute average stack-gas temperature, K (°R)
Total volume of liquid collected in the impingers and
silica gel, mL
Volume of gas sample as measured by dry-gas meter,
dscm (dscf)
volume of gas sample as measured by dry gas meter,
corrected to standard conditions, dscm (dscf)
Dry-gas-meter calibration factor, dimensionless
XXXX-42
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September 1996
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METHOD XXXX
AH = Average pressure differential across the orifice meter,
mm H2O (in. H2O)
e = Total sampling time, min
12.2 Concentration of Acetonitrile in Sample. Use least squares linear regression
analysis of the calibration standards to calculate a correlation coefficient, slope, and intercept.
Concentrations are the X-variable, and response is the Y-variable.
12.3 Calculation of Total Weight of Acetonitrile in the Sample. Determine the total
acetonitrile in ^g using the following equation:
ACNT = ACNC x MVOL x DF Eq. XXXX-1
If acetonitrile is detected in more than one component, sum the total acetonitrile
weights for each component to obtain the total weight of acetonitrile in the train.
12.4 Acetonitrile concentration in stack gas. Determine the acetonitrile concentration
in the stack gas using the following equation:
„ K (total acetonitrile, mg)
cf = r; Eq. XXXX-2
m(std)
where:
K =35.31 frVm3 if Vm(std) is expressed in English units
= 1.00 m3/m3 if Vro(std) is expressed in metric units
12.5 Average Dry Gas Meter Temperature and Average Orifice Pressure Drop are
obtained from the data sheet.
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METHOD XXXX
12.6 Dry Gas Volume: Calculate Vm(std) and adjust for leakage, if necessary, using
the equation in Section 6.3 of EPA Method 5.
12.7 Volume of Water Vapor and Moisture Content: Calculate the volume of water
vapor and moisture content from equations 5-2 and 5-3 of EPA Method 5.
12.8 Conversion Factors.
From
scf
g/ft3
g/ft3
g/ft3
Ifi
m3
gr/ft3
lb/ft3
g/m3
Multiply by
0.02832
15.43
2.205 x 10'3
35.31
12.9 Isokinetic Variation.
12.7.1 Calculation from Raw Data.
I =
100 Ts
K3V1C +
V,J
Tm
Pbar *
AH
13.6
Eq. XXXX-3
where:
K3
0.003454 mm Hg-m3/mL-K for metric units, or
0.002669 in. Hg-ftVmL-'R for English units.
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METHOD XXXX
12.7.2 Calculation for Intermediate Values.
TV ....PJOO
I =
ls*m(stdrstdj
T V
v l s * m(std)
= K4
PsVsAnG(l-Bws)
Where:
K4 = 4.320 for metric units, or
K4 = 0.09450 for English units.
13.0 METHOD PERFORMANCE.
13.1 Method performance evaluation: The expected method performance parameters
for precision, accuracy, and detection limits are provided in Table XXXX-6.
13.2 The MDL concentrations listed in Table XXXX-1 were obtained using field
train blank sample results or instrument detection limits.
14.0 POLLUTION PREVENTION. Reserved
15.0 WASTE MANAGEMENT. Reserved
16.0 REFERENCES.
1. U.S. Environmental Protection Agency, 40 CFR, Part 60, Appendix A,
Methods 1-5.
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METHOD XXXX
2. EPA Methods 0010, Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods. SW 846, Third Edition. September 1988, Office
of Solid Waste and Emergency Response, U.S. Environmental Protection
Agency, Washington, D.C. 20460.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source
Sampling Equipment. Environmental Protection Agency. Research Triangle
Park, NC., 27711. APTD-0576. March 1972.
4. Martin, Robert M. Construction Details of Isokinetic Source-Sampling
Equipment. Environmental Protection Agency. Research Triangle Park, NC.,
27711. APTD-0581. April 1971.
5. Quality Assurance Handbook for Air Pollution Measurement Systems. Volume
HI: Stationary Sources of Specific Methods (Interim Edition). U.S.
Environmental Protection Agency. Office of Research & Development,
Washington D.C., 20460. EPA/600/R-94-038c. April 1994.
6. U.S. Environmental Protection Agency. Method 301-Protocol for the Field
Validation of Emission Concentrations from Stationary Sources. Code of
Federal Regulations, Title 40, Part 63. Washington, D.D. Office of the
Federal Register, July 1, 1987.
7. Steger, J.L., Bursey, J.T., and Epperson, D., Acetonitrile Field Test, Draft
Report, Eastern Research Group under Work Assignment 45, Contract 68-D4-
0022 to U.S. Environmental Protection Agency, Research Triangle Park, NC,
September 1995.
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METHOD XXXX
8. Vollaro, R.F., A survey of Commercially Available Instrumentation for the
Measurement of Low-Range Gas Velocities, Research Triangle Park, North
Carolina, U.S. Environmental Protection Agency, Emissions Measurement
Branch, November 1976 (unpublished paper).
9. SchJickenrieder, L. M., Adams, J. W., and Thrun, K. B., Modified Method 5
Train and Source Assessment Sampling System: Operator's Manual, U.S.
Environmental Protection Agency, EPA/600/8-85-003 (1985).
10. Shigehara, R. T., Adjustments in the EPA Nomograph for Differential Pitot
Type Coefficients and Dry Molecular Weight, Stack Sampling News, 2:4-11
(October 1974).
11. Johnson, L.D., Fuerst, R.G., Steger, J.L. and Bursey, J.T., "Evaluation of a
Sampling Method for Acetonitrile Emissions from Stationary Sources,"
presented at EPA/A&WMA International Symposium: Measurement of Toxic
and Related Air Pollutants, Research Triangle Park, NC, April 1997.
12. Steger, J.L. and Hoskinson, S., Development of a Method for Determination of
Acetonitrile, Draft Interim Report, Radian Corp. under Work Assignments 5 &
22, Contract 68-D1-0010 to U.S. Environmental Protection Agency, Research
Triangle Park, NC, September 1992.
13. Steger, J.L. and Klassa, C., Evaluation of Sorbents for Collecting Acetonitrile
from Stationary Sources, Draft Internal Report, Radian Corp. under Work
Assignment 58, Contract 68-D1-0010 to U.S. Environmental Protection
Agency, Research Triangle Park, NC, October 1993.
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METHOD XXXX
14. Steger, J.L., Acetonitrile Method Development and Field Test, Letter Report,
Radian Corp. under Work Assignment 4, Contract 68-D4-0022 to U.S.
Environmental Protection Agency, Research Triangle Park, NC, September
1995.
17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA.
17.1 Table XXXX-6 summarizes validation data results from Method 301 field testing.
Further details are included in References 11 through 14.
TABLE XXXX-6. EXPECTED METHOD PERFORMANCE BASED ON EPA
METHOD 301 VALIDATION TESTS
Detection Concentration
Precision Limit Level Test
Compound (% RSD)" Biasb (ppbv)c (ppmv) Matrix
Acetonitrile ±13 -0.15 60 45 Incinerator
a Relative Standard Deviation (%) for dual spiked trains as calculated by EPA Method 301.
b Bias for dual spiked trains as calculated by EPA Method 301. The bias was not significant so
no bias correction factor is needed.
c Based on ten times the calculated detection limits for the field train blank samples for a 1 m3
(35.3 cubic foot) sample.
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METHOD XXXX
Thermocouple
Thermocouple
Carboxen 1000
Thermocouples Condensate
Vacuum
Line
Figure XXXX-1. Acetonitrile Sampling Train
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METHOD XXXX
Separatory Funnel
Union
1/8" Teflon©
Tubing
Union
.Silanized Glass VMbol
Sorbent Module
Glass Frit
Figure XXXX-2. Reverse Gravity Extraction Apparatus
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QATA SHEET
Run
Pag* lot
Plant
Oat*
Operator
Sampling Location
Sample Type
Run Number
Slellc Pretture (±) (In. H2O)
Beromelric Pretture (In. H2O)
XAO Trap Number
Filter Healer Setting (T)
Probe Length ft Type
Probe Healer Setting (*F)
Minimum Semple Volume (13)
Initial Leak Check
Final Leak Check
Meter Box Number
Meter delta H @
DOM Factor (Y)
Noule Type ft ID (In.)
Ambler* Tempereture (*F)
Ateumed Molriure (% H2O)
K-Factor
OhVBHt of Duct
Schematic of Traverse Point Layout
and I •oe>4 ••
Tieve'ie
Point
Number
Sampling
Time
(mln)
dock
Time
(24hr)
Qae
Reading
Velocity
Head
((deHa P.).
ln.H2O)
Stack
T*
CF)
Orince P
Oiler
(delta H.
Detlred
reieure
entfal
InHZO)
Actual
Probe
Temp.
m
FBter
Temp.
rn
Adeorbent
Trap
Temp.
cn
Dry Oai
Inlet
(Tmln)
9n9l9t
Ou>*t
(Tmout)
Ert
Temp.
rn
Pump
Vacuum
fJn.Hg)
X
X
X
X
•S
ff
cr »
0 <
-"
o
3 Comment*
C
-------
APPENDIX B
Results from Preliminary
Laboratory Studies on
Work Assignment 4,
Contract 68-D4-0022
-------
APPENDIX B
This appendix provides a description of the technical activities and results obtained for
the laboratory studies conducted on Work Assignment No. 04, entitled "Acetonitrile Method
Development and Field Test," for EPA Contract No. 68-D4-0022, during the period of
performance between October 1, 1994 and September 30, 1995. This appendix provides a
summary of the work completed, an explanation of how it was done, and an analysis of the
results. The purpose of this appendix is to provide additional background information on how
and why the sorbent used in the field evaluation was chosen.
EXECUTIVE SUMMARY
A key issue with using acetonitrile as a test chemical for evaluating the destruction
efficiency performance of incinerators is the lack of an effective sampling method. The
objectives of this study were to develop a sampling and analysis method for acetonitrile and to
evaluate the method in the field according to the procedures outlined in EPA Method 301,
"Protocol for the Field Validation of Emission Concentrations from Stationary Sources,"
40 CFR Part 63'. Progress toward these objectives were begun by studying the ability of
various sorbents (Ambersorb* XEN-563, Carboxen™-1000, Anasorb*747, and
Carboxen™-569) to remove acetonitrile from hot, moist, gaseous stationary source emissions.
These various sorbents were able to collect greater than 95% of the spiked acetonitrile using an
SW-846 Method 00102 train under the most rigorous test conditions. A desorption procedure
to recover greater than 90% of the acetonitrile from the sorbent was developed. A potential
field test site was identified and a draft field test plan was prepared.
B-l
-------
Several conclusions were reached based on the desorption experiments:
• Carboxen™-1000 was the only sorbent tested that was able to quantitatively
remove acetonitrile from moist air using one sorbent module. For the other
three sorbents, approximately 80% of the available acetonitrile was captured on
each sorbent module.
• Reverse gravity elution of approximately 1 to 1.5 column volumes (50 to
90 mL) of solvent through the sorbent module quantitatively removes the
acetonitrile from the sorbent, resulting in recoveries >80% in all cases and
>90% in most cases. Acetonitrile was quantitatively extracted (recoveries
>90%) from Ambersorb* XEN-563, Carboxen^-lOOO, and Anasorb" 747 using
methylene chloride. In some cases, a water layer was removed from the sorbent
with the organic extract. Thus, a modifier may be needed to help solvate the
entrapped water that is extracted from the sorbent with the methylene chloride
so that a single-phase extract is produced.
• The acetonitrile was not efficiently extracted (recoveries <40%) from the
Carboxen™-569 using methylene chloride. Adequate acetonitrile recoveries
from the Carboxen™-569 were obtained using a 1:1 carbon disulfide:dimethyl
formamide solution.
INTRODUCTION
The U.S. EPA and Radian designed experiments to develop and evaluate a sampling
and analysis method for acetonitrile from stationary sources. The experimental designs were
successful in making progress toward the development of a rigorous method for acetonitrile.
Background
There is a wide interest in developing and evaluating a method for measuring
acetonitrile emissions from stationary sources of air pollution. Acetonitrile is a component of
many industrial hazardous waste streams, especially from fiberglass and synthetic fiber
manufacturing. Acetonitrile is listed as one of the most difficult to incinerate compounds
under the University of Dayton Research Institute incinerability ranking.3 Acetonitrile has
been suggested as an excellent non-halogenated compound to use as a hazardous constituent
spike during Resource Conservation and Recovery Act (RCRA) Subpart B trial burn tests.
Lack of an effective sampling method has prevented its utilization. Therefore, the EPA must
B-2
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develop a method for sampling and analyzing acetonitrile from stationary sources. Since
moisture is likely to be present in acetonitrile emissions, the sampling method must be
isokinetic.
Radian Corporation assisted the Methods Branch of the Air Measurements Division of
the National Exposure Research Laboratory (NERL) in developing and evaluating sampling
and analytical methods for acetonitrile from stationary sources, particularly incinerators. In
previous studies done under Work Assignments 5, 22, and 58 on Contract 68-D1-0010 with
Radian Corporation, several approaches for sampling analysis were evaluated.415 An EPA
Method 56 train with six to eight impingers containing water was used to collect the
acetonitrile. However, the acetonitrile migrated throughout the impingers during sampling
resulting in low recoveries. Addition of a chilled-water condenser did not completely prevent
the acetonitrile migration. A mineral oil vapor barrier in the condensate trap did prevent the
migration but collection of the acetonitrile was not satisfactorily improved. Additional
laboratory evaluation of a sorbent-based sampling method using a modified Method 00107 was
completed on this work assignment (Work Assignment 4).
Objectives
To develop and evaluate an acetonitrile sampling train, the following questions served
as a guideline:
How efficient is the sorbent at collecting acetonitrile from hot, wet stationary source
emissions?
How can > 90% of the acetonitrile be desorbed from the sorbent?
The objective of the study was to develop a sampling and analysis method for acetonitrile
and evaluate the proposed method at an incinerator using the procedures in Method 301.'
Because the method required more laboratory method development than originally planned, the
field evaluation was not completed.
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CONCLUSIONS AND RECOMMENDATIONS
Based on the results of the work completed, the following preliminary conclusions can be
made.
• Of the four sorbents studied, Carboxen™-1000 was the easiest sorbent to extract and
the best sorbent at collecting acetonitrile from hot, moist air.
• Reversed gravity elution of 50 to 90 mL of solvent through the sorbent module
successfully desorbs the acetonitrile from the sorbent recovering >80% of the spiked
acetonitrile in all cases and >90% in most cases.
The feasibility of using Carboxen™-1000 in the acetonitrile train needs to be determined.
First, long-term availability of bulk quantities of the sorbent must be assessed. Second,
procedures for cleaning, reactivating, and reusing the sorbent should be developed and
evaluated. Third, procedures for improving the desorption procedure and for handling water
extracted from the sorbent modules should be identified, developed and evaluated. The ideal
extract will be a single phase to simplify the analysis. Finally, when sufficient quantities of
bulk Carboxen™-1000 are commercially available, a Method 301' field validation using
Carboxen™-1000 in the sampling train should be conducted. The sorbent module should
contain 48 g of Carboxen™-1000 and should be extracted with 70 mL of methylene chloride
using the reverse gravity elution procedure.
EVALUATION OF THE REVERSED GRAVITY EXTRACTION PROCEDURE
Studies were conducted to develop procedures for extracting the acetonitrile from the
sorbent. Because the initial extraction approaches failed to provide reproducible results and
the irreproducibility was believed to be caused by channelling of the solvent through the
sorbent, the extraction method was modified to use reverse gravity elution through the sorbent
module as shown in Figure B-l.
To evaluate the reverse gravity elution procedure, eight sorbent modules were statically
spiked with 250 mg of acetonitrile by pouring 200 mL of water containing the acetonitrile
B-4
-------
through the sorbent module. The eluent was analyzed and the amount of acetonitrile retained
was calculated by difference. The results are presented in Table B-l. One sorbent module
(WA4-7-001) was extracted using the new apparatus. First, the sorbent module was filled
with methylene chloride from the bottom (frit end) to the top. Then, seven successive 10-mL
aliquots of methylene chloride extract were collected. Before collecting the final, seventh
10-mL aliquot, the methylene chloride was allowed to remain in contact with the sorbent for
approximately one half hour. All seven aliquots were analyzed individually by gas
chromatography with flame ionization detection (GC/FID).
The amount of acetonitrile recovered in each fraction is shown in Table B-2. A total of
97% of the spiked acetonitrile was recovered with > 90% of the spiked acetonitrile recovered
in the first 50 mL. Based on these results the reverse gravity elution procedure was further
evaluated using statically and dynamically spiked sorbents.
Four more of the statically spiked sorbent modules containing 48 g of
Ambersorb* XEN-563 were extracted with seven 10-mL aliquots of methylene chloride to
• determine the reproducibility of the procedure. The results, including Module WA4-7-001,
are reported in Table B-3. Recoveries ranged from 93 to 99% with 89 to 96% of the
acetonitrile being recovered in the first 50 mL of methylene chloride eluted through the
sorbent. For one of the sorbent modules (WA4-7-003) the methylene chloride was allowed to
sit in the sorbent module for approximately 30 minutes before being eluted. The 30 minute
static time did not improve the overall recovery of acetonitrile from the sorbent or affect the
distribution of the acetonitrile in the extracts.
For the next experiment, three statically spiked sorbent modules containing 48 g of
Ambersorb* XEN-563 were extracted with a 50-mL aliquot of methylene chloride followed by
a 20-mL aliquot. These results are reported in Table B-4. Recoveries ranged from 98 to 99%
with an average of 94% of the acetonitrile recovered in the first 50-mL extract. Based on
these results, the recommended sorbent extraction procedure is to use reverse gravity elution,
B-5
-------
collecting the extract in two aliquots consisting of a 50-mL first aliquot and a 20-mL second
aliquot.
Because the data showed that the extraction procedure was precise and provided high
recoveries using statically spiked sorbents, four sorbent modules were dynamically spiked
using the most rigorous test conditions (high acetonitrile concentrations in the presence of high
moisture sampled at a high flow rate). Dynamic evaluation of the extraction procedure was
performed to ensure that the extraction procedure was sufficiently rigorous so that it was
unaffected by any differences in acetonitrile interaction with the sorbent caused by the spiking
procedure. Acetonitrile recoveries for the dynamically spiked train samples are reported in
Table B-5. From 72 to 78% of the acetonitrile was recovered in the sorbent extracts,
indicating that the extraction procedure was precise. An additional 12 to 18% of the spiked
acetonitrile was recovered in the condensate knockout indicating that a significant quantity of
acetonitrile broke through the 48 g of Ambersorb* XEN-563 packed in the sorbent module.
LABORATORY TRAIN EVALUATION OF THE AMBERSORB® XEN-563
Because only approximately 80% of the spiked acetonitrile was recovered on the sorbent
and approximately 15% of the acetonitrile was in the condensate knockout, additional
laboratory train spiking experiments were conducted using three sorbent modules in series as
shown in Figure B-2. These experiments were designed to evaluate whether two sorbent
modules of Ambersorb* XEN-563 would be adequate to retain all of the sampled acetonitrile.
Conditions for the train spiking experiments are reported in Table B-6.
The Ambersorb* XEN-563 sorbent modules from the two three-sorbent module trains were
extracted using the gravity elution procedure and the extracts were analyzed by GC/FID. The
results are reported in Table B-7. Approximately 80% of the acetonitrile was captured on the
first sorbent module, 16% on the second sorbent module, 3% on the third sorbent module and
1 % in the knockout. Thus, each sorbent module appeared to capture only 80% of the
acetonitrile to which it was exposed. Although the Ambersorb* XEN-563 sorbent effectively
B-6
-------
removes acetonitrile from water, the efficiency of the sorbent for removing acetonitrile from
hot, moist air is inadequate for use in the acetonitrile train.
OTHER SORBENT STUDIES
Because the Ambersorb* XEN-563 is not efficient at removing acetonitrile from air,
additional sorbents were purchased and evaluated. The sorbents chosen were the four
sorbents, besides Ambersorb* XEN-569 that appeared most promising after initial screening
studies performed on Work Assignment 58 of EPA Contract 68-D1-00105: Porpapak* T,
Anasorb*747, Carboxen™-1000, and Carbpxen™-569. The amount of sorbent used was the
amount of sorbent that would fit into a standard Method 00102 sorbent module: 24 g for
Porapak*T, 60 g for Carboxen™-569, 50 g for Anasorb* 747, and 48 g for
Caroboxen™-1000. First, the ability of the reverse gravity elution procedure using methylene
chloride as the solvent to extract acetonitrile from the sorbent was evaluated. Then, the ability
of the sorbent to remove acetonitrile from moist air was determined by dynamically spiking
sampling trains containing multiple sorbent modules in series.
Sorbent Extraction Studies
Aliquots of sorbent were packed into standard Method 00102 modules and statically spiked
with an aqueous solution containing acetonitrile. The volume of the spiking solution was
measured before and after elution through the sorbent. The concentration of acetonitrile in the
eluant was also measured by GC/FID. The amount of acetonitrile and water retained on the
sorbent were calculated based on the difference between the measured values before and after
exposure to the sorbent.
Information on the static spiking of the sorbents is presented in Table B-8. The Porapak* T
swelled when it became wet and its expansion caused the sorbent module to break. Because
the Porapak* T could not be statically spiked using the current spiking procedures, studies with
Porapak* T were discontinued. The remaining three sorbents were successfully spiked using
B-7
-------
the static spiking procedures. Greater than 96% of the acetonitrile was retained on the
sorbents and less than 15% of the water used as the spiking medium was retained. The
Carboxen™-1000 retained the most acetonitrile and the most water and the Carboxen™-569
retained the least acetonitrile and the least amount of water.
The statically spiked sorbent modules were extracted with methylene chloride using the
reverse gravity elution system. For the first extract, 50 mL of solution was collected and for
the second extract 20 mL of solution was collected. In some cases, the extract consisted of
two layers because the water retained by the sorbent was displaced by the organic solvent and
sufficient water was present so that it could not be solubilized by the organic solvent. When
10 mL or more of water was present, the sorbent was extracted with a third aliquot of organic
solvent.
The results are reported in Table B-9. Less than a third of the acetonitrile was recovered
from the Carboxen™-569 when methylene chloride was used as the extraction solvent. Based
on the extraction study completed on WA 585, the evaluated solvent system that recovered the
•most acetonitrile from Carboxen™-569 was a solution of 50% carbon disulfide and 50%
dimethyl formamide. Two additional traps were packed with Carboxen™-569, statically
spiked with the aqueous acetonitrile solution, and extracted with 1:1 carbon
disulfiderdimethylformamide. Extraction recoveries were still low (approximately 80%) but
adequate for evaluating the sorbent's ability for removing acetonitrile from a gas stream.
Methylene chloride recovered greater than 90% of the acetonitrile from the other two sorbents.
Multiple Sorbent Module Train Studies
Next the ability of the sorbents to remove acetonitrile from air containing high levels of
moisture was evaluated using trains containing multiple sorbents in series. Because a limited
supply of Carboxen™-1000 was available, only two Carboxen™-1000 traps were used in series
as shown in Figure B-3. For the other two sorbents, three traps were used in series as shown
in Figure B-2. The trains were dynamically spiked with an aqueous solution of acetonitrile,
B-8
-------
and recovered using 50:50 methanohmethylene chloride to rinse the front half of the train and
methane! to recover the condenser and condensate.
The results are reported in Table B-10. The Carboxen™-1000 performed the best of the
three sorbents evaluated. It was the most efficient sorbent at capturing the acetonitrile and it
was the easiest sorbent to extract. Only 1 % of the spiked acetonitrile was recovered from the
second sorbent module and < 1 % of the spiked acetonitrile made it into the knockout. Less
than 10% of the acetonitrile was recovered in the second methylene chloride extract. The two
disadvantages to using Carboxen™-1000 are that the supplier may not be willing to make the
sorbent available and the expense (approximately $400 per sorbent module).
Anasorb* 747 and Carboxen™-569 performed similarly to Ambersorb* XEN-563 with
regards to capturing the acetonitrile from air. Both sorbents captured approximately 80% of
the available acetonitrile in each sorbent module (i.e. approximately 80% in the first module,
approximately 16% in the second module, approximately 4% in the third module, and
approximately 1 % in the knockout). However, the acetonitrile could be removed from the
Anasorb* 747 with methylene chloride making it easier to extract than the Carboxen™-569
which had to be extracted with a 1:1 carbon disulfide:dimethylformamide solution.
REFERENCES
1. U.S. Environmental Protection Agency. Method 301-Protocol for the Field Validation of
Emission Concentrations from Stationary Sources. Code of Federal Regulations, Title 40,
Part 63. Washington, D.C. Office of the Federal Register, July 1, 1987.
2. EPA Method 0010. Test Methods for Evaluating Solid Waste: Physical/Chemical
Methods SW-846, Third Edition. September 1986, Office of Solid Waste and
Emergency Response, U.S. Environmental Protection Agency, Washington, D.C. 20460.
3. Environmental Science and Technology, 24, pp 316-328, 1990.
4. Joette Steger and Steve Hoskinson, Development of a Method for Determination of
Acetonitrile. Draft Interim Summary Report for Work Assignment 22,
Contract No. 68-D1-0010, U.S. Environmental Protection Agency, Atmospheric and
Exposure Assessment Laboratory, Methods Research and Development Division, Source
B-9
-------
Methods Research Branch, Research Triangle Park, North Carolina 27711.
September 29, 1992.
5. Joette Steger and Cheryl Klassa, Evaluation of Sorbents for the Collection and Analysis of
Acetonitrile from Stationary Sources. Draft Internal Report for Work Assignment 58,
Contract No. 68-D1-0010, Environmental Protection Agency, Atmospheric and Exposure
Asessment Laboratory, Methods Research Development Division, Source Methods
Research Branch, Research Triangle Park, North Carolina 27711. October 29, 1993.
6. Method 5 - Determination of Paniculate Emissions from Stationary Sources. Part 60,
Appendix A of 40 CFR Chapter 1 (July 1, 1989 Edition).
B-10
-------
TABLE B-l. RETAINED ACETONITRILE CALCULATED BY DIFFERENCE
Sample Run
WA4-7-OOI
WA4-7-002
WA4-7-003
WA4-7-004
WA4-7-005
WA4-7-006
WA4-7-007
WA4-7-008
Amount of
Ambersorb
(R)
48.02
48.00
48.00
48.02
48.03
48.02
48.04
48.03
Amount of
ACN' Spike
(mR)
250.26
250.26
250.26
250.26
250.26
250.26
250.26
250.26
Volume of
Eluant
Collected
(mL)
190
188
184
185
182
190
184
188
ACN*
Concentration
in 11,0
Collected
(mR/mL)
0.0049
0.0191
0.0012*
0.0175
0.0196
0.0104
0.0019
0.00 121*
Total ACN trt
H,0
(IHR)
0.9310
3.5908
0.2208
3.2375
3.5672
1.9760
0.3496
0.2256
Amount of
ACN Retained
tn Trap
(mg)
249.33
246.67
250.04
247.02
246.69
248.28
249.91
250.03
% of Spiked
ACN Retained
by Trap
99.63
98.57
99.91
98.71
98.57
99.21
99.86
99.91
"ACN = Acetonitrile; 250 mg of ACN contained in 200 mL of water.
kArea below lowest standard area.
'Analyzed by GC/FID using Direct Aqueous Injection.
-------
TABLE B-2. ACETONITRILE RECOVERY FOR GRAVITY ELUTION
(PRELIMINARY RESULTS FOR WA4-7-001 CONTAINING 48.02 G OF
AMBERSORB SPIKED WITH 249 MG OF ACETONITRILE)
Fraction Number
1
2
3
4
5
6
7
Total
Elapsed Time
(min)
9
4
2
3
2
4
30"
54
Volume of
Extract
(mL
12.6'
8.4'
8.781
9.0*
9.0
10.2
10.5
68.5
Acetonitrile Recovered
<£>
104.0
50.1
37.9
23.0
13.6
9.3
4.3
242
(%)
41.8
20.1
15.2
9.24
5.45
3.7
1.7
97.2
"Measured volumes corrected for tube volume (0.67 mL average for three measurements).
""Extract allowed to sit in sorbent for approximately one-half hour.
B-12
-------
TABLE B-3. ACETONITRILE RECOVERY FOR GRAVITY ELUTION (RESULTS FOR 48 G OF
AMBERSORB SPIKED WITH 250 MG OF ACETONITRILE)
Fraction
Number
1
2
3
4
5
6
7
Total
Acetonitrile Recovered
(R)
VVA4-7-
001
104'
50.1 '
37.9*
23.0'
13.6
9.3
4.3 fc
242
WA4-7-
002
131
53.4
26.3
15.3
8.12
3.90
2.00
240.
WA4-7-
003
129 k
55.4
29.8
18.3
7.85
4.60
2.25
247
WA4-7-
004
98.4
57.9
34.8
18.2
11.7
5.80
2.67
229
WA4-7-
005
98.5
60.8
38.7
19.2
10.1
4.95
2.70
235
(%)
WA4-7-
001
41.8
20.1
15.2
9.24
5.45
3.7
1.7
97.2
WA4-7-
002
53.1
21.7
10.6
6.20
3.29
1.58
0.81
97.3
WA4-7-
003
51.6
22.2
11.9
7.32
3.14
1.84
0.90
98.9
WA4-7-
004
39.8
23.4
14.1
7.34
4.75
2.35
1.08
92.8
WA4-7-
005
39.9
24.6
15.7
7.79
4.09
2.01
1.09
95.2
Od
'Measured volumes corrected for tube volume (0.67 mL average for three measurements).
""Extract allowed to sit in sorbent for approximately one half hour.
-------
TABLE B-4. ACETONITRILE RECOVERY FOR GRAVITY ELUTION
(RESULTS USING A 50 ML ALIQUOT OF SOLVENT FOLLOWED BY A
20 ML ALIQUOT)
Sample ID
WA4-7-006
WA4-7-007
WA4-7-008
Average
Standard Deviation
Relative Standard Deviation (%)
Acefonitrile Recovered
Weight (g)
Extfl
230
241
230
234
6.35
2.72
Ext 12
13.5
3.88
18.3
11.9
7.34
61.7
Total
243
244
248
245
2.65
92.6
Fraction (%)
Extfl
92.5
96.2
91.8
93.5
2.36
2.53
Ext*2
5.42
1.56
7.32
4.77
2.94
61.6
Total
97.9
97.8
99.2
98.3
0.781
0.794
B-14
-------
TABLE B-5. LABORATORY TRAIN SPIKING RESULTS FOR TRAINS SPIKED AT HIGH
ACETONITRILE CONCENTRATIONS AND EXTRACTED USING REVERSE GRAVITY FEED
Run
WA4-8-002
WA4-8-003
WA4-8-004
WA4-8-005
Average
Standard Deviation
Relative Standard Deviation
Concentration
of ACN in
Simulated Stack
Gas
(ppmv)
54
62
43
50
52
8
15%
Moisture
(%)
33
31
27
29
30
3
9%
Sampling
Rate
(CFM)
0.69
0.69
0.69
0.71
0.70
0.01
1%
Percent Acetonitrlle Recovered
Extract
r
74
68
71
73
72
3
4%
2fc
4
4
5
3
4
1
20%
Knockout
14
12
17
18
15
3
18%
Total
92
84
93
94
91
5
5%
w
•—•
LA
'Approximately 50 mL extraction volume.
fc Approximately 20 mL extraction volume.
-------
TABLE B-6. LABORATORY TRAIN SPIKING CONDITIONS FOR
TRAINS SPIKED AT HIGH ACETONITRILE CONCENTRATIONS
CONTAINING THREE SORBENT MODULES IN SERIES
Run
WA4-9-Run 1
WA4-9-Run 2
Averaee
Percent Difference*
Acetonitrile
Concentration
(ppmv)
50
65
58
26
Total
Acetonitrile
Spiked (mg)
104
106
105
2
Moisture (%)
29
28
28
4
Sample Rate
(CFM)
0.71
0.55
0.63
25
"Percent Difference = Difference between Run 1 and Run 2 divided by the average of Runs 1 and 2.
B-16
-------
TABLE B-7. LABORATORY TRAIN SPIKING RESULTS FOR TRAINS SPIKED AT HIGH ACETONITRILE
CONCENTRATIONS CONTAINING THREE AMBERSORB SORBENT MODULES IN SERIES
Run
WA4-9-Run 1
WA4-9-Run 2
Average
Percent
Difference*
Acetonitrile
Concentration
(ppmv)
50
65
58
, 26
Moisture
(%)
29
28
28
4
Sampling
Rate
(CFM)
0.71
0.55
0.63
25
Percent Acetonitrile Recovered
Sorbent Module #
1
Extract
r
82
71
76
14
2"
3
5
4
50
2
Extract
r
13
10
12
25
2"
2
1
2
50
3
Extract
1*
4
5
4
25
2"
0
0
0
0
Knock-
out
1
1
1
0
Total
105
93
99
12
w
"Approximately 50 mL extraction volume.
""Approximately 20 mL extraction volume.
'Percent Difference = (Difference/Average) x 100
-------
TABLE B-8. PERCENT ACETONITRILE RETAINED DURING STATIC SPIKING
(250 MG SPIKE)
Sample ID
WA4- 10-001
WA4- 10-002
WA4- 10-005
WA4-10-010
WA4-10-011
WA4-10-012
WA4-10-013
Sorbent
Carboxen 569
Carboxen 569
Carboxen 1000
Carboxen 569
Carboxen 569
Anasorb 747
Anasorb 747
Sorbent
Weight (g)
60
60
48
60
60
50
50
Water Volume (mL)
Spiked
200
200
198
198
200
201
200
Recovered
184
185
161
184
184
174
176
Acetonitrile Retained
Grams
252
252
250
247
243
253
251
%
100
100
100
99
96
100
100
w
1
oo
-------
TABLE B-9. EXTRACTION RECOVERY FOR 250 MG STATIC SPIKE
Sample ID
WA4- 10-001
WA4- 10-002
WA4- 10-005
WA4-10-010
WA4- 10-011
WA4-10-012
WA4-10-013
Sorbent
Carboxen 569
Carboxen 569
Carboxen 1000
Carboxen 569
Carboxen 569
Anasorb 747
Anasorb 747
Solvent
MC
MC
MC
CS7/DMF
CS,/DMF
MC
MC
Volume of
Organic Extract
(mL)
Ext 1/Ext 2/Ext 3
52.5/23.5/NT
50.0/20.5/NT
30/20.7/20.8
37/18/20
40/20/21.5
37/21.2/21.4
44/20.9/21.2
Volume of
Water
Extract
(mL)
Ext I/
Ext2
0/0
0/0
20/0
13/2
10/0
13/0
6/0
Percent Acetonttrlle Recovered'
Organic Extract
#1
24
17
74
61
63
63
69
#2
9
4
2
15
6
15
13
*3
NT
NT
<1
4
6
6
6
Water
Extract11
ffl
0
0
27
2
2
12
3
12
0
0
0
1
0
0
0
Total
33
21
103
83
77
96
91
w
MC = Methylene Chloride
CS2/DMF =1:1 Carbon disulflde and dimethyl formamide
1 Calculated based on the volume of extract recovered.
b Sometimes the extract contained two layers.
-------
TABLE B-10. LABORATORY TRAIN SPIKING RESULTS FOR TRAINS SPIKED AT HIGH ACETONITRILE
CONCENTRATIONS CONTAINING MULTIPLE SORBENT MODULES IN SERIES
Run
WA4-10-
Run 1
WA4-IO-
Run2
WA4-10-
Run3
WA4-IO-
Run4
WA4-IO-
RunS
WA4-10-
Run6
Sorhenl
Carboxen
1000
Carboxen
1000
Carboxen
569*
Carboxen
569°
Ana sorb
747
Anasorb
747
Cone. Of
ACNIn
Simulated
Stack Gas
(ppmv)
33
32
34
44
38
35
Moisture
(%)
24
19
27
27
26
27
Sampling
Rate
(CFM)
0.72
0.72
0.70
0.69
0.59
0.64
Percent Acefonltrile Recovered
Sot-bent
I
Extract
I"
82
91
74'
72'
53
65
2"
7
8
1
13
11
10
3"
NT
NT
-------
Separator/ Funnel
H!
e
W
n
3
KJ 2,
o
-a
*+
5'
o
to
2
3rtT Teflon*
Tubing
Union
Sllanlzed Glass Wool
Sorbent Module
-------
Stack
Wai!
S-Type Prtot Tube
thermocouple
Figure B-2. Acetonitrile Sampling Train with Three Sorbent Modules
in Series
B-22
-------
Stack
Wall
hcrrnoooupte
S-Type Pilot Tube
Orifice
I I .' '
i
i T
Dry Gas \
n
B
\
7?
Meter I
Figure 3-B. Acetonitrile Sampling Train with Double Sorbent Modules
B-23
-------
APPENDIX C-l
Field Spiking Solution
Preparation and Analysis
-------
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ojoo
o?cc
osoo
Vol Adj Amt
.*•/•! oes*rv»e
.ant X-Vilue
0.006000
O.Oi:iOO
0.060600
; 0.1:1:00
0.60COCC
C*i-vilueC
0.006131
0.014543
0.058102
0.118360
0.606144
Mlta
-0.002131
-0.002443
0.002498
0.002820
-0.000144
Wilt.
-26.209
-16.799
4.2*9
2.382
-0.123
oest rves
T-V*lu*
>«€l36.000000
/J9063. 500000 1
/ 322145. 750000/
I 632294. OOOOOQT
\ 3i40i::. ooqopC
T-valut
3519:. 699219
•651". 320312
335573. 718750
€V4 €!£.'. 812500
3i3?:c:. 7ioooo
Delta
10?43. 300161
12546.119688
-12821.968150
-14481.812500
3820.250000
%L1«.
I9.?;i
14.501
o.;;:
-------
re Version: 4.0
09:52 AM
: 4/15/96
le Narr.= :
File :
ence File:
C:\TC4V C-C 5 \ C -: "-•" 0 01. RAW
C:\TC4\GC5\KA45SPK-.SE1'
GC_5 Rack/Vial: 0/0
: 1.0000
Date: 4/15'?? 09:19 AM
Cycle: 1 Channel : A
Operator: TIN
Ciluti:- Fa-tor : 1.
— T< r- ten >c
o IP cp IP 8= f»
' 3 O O — -
-------
aof t>.-sre V-srsior.: -3. C < IC2 f->
1E/P6
Date: 4/
?2r;ple Name
i'=ta file
'•s-u-r'-re file
09:52 AM
0.121 MG./ML 5TD ^5lDE=>
C:\TC-5vGC5\CfE":
C: \ TC4 \ GC5\WA-J 5S PK. SEQ
GC 5 Rark/Vial: 0/0
Date: 4/15/96 C?:3? AM
Cycle: 2 Channel : A
Operator: TLM
Diiutirn Farter :
'•^•Tt-TTri n i i
M I i I i Mi [ I M I i I i I ' iTi| I It I I M i I | 1 Till Ml I M 1 I I j I II I j I ; i 1 | I 1 I I j I I M j I i I I I
0 2 ' 4 6 B 10 12 14
Time [min]
WA 45 REPORT
•j» Componeni
• Nam*
1
3
•9
c
:
1
9
9
10
11
i:
i;
!•) Propiorutnle
i?
i ,-
-
7
?
C
^
-
4
c
^
-
•i
i
1
^
•
£.
f
Time
(mini
0
1
1
1
1
2
2
2
2
3
3
4
.844
. b4i
.6"?
.64i
.99"
.201
.531
.866
.947
.150
.566
.142
5. 091
S
6
<
e
«
^
•j
i
i
t
e
9
9
0
9
10
10
10
10
11
11
.ce:
.023
.466
.701
.»54
.142
.236
.564
.77?
.63?
.769
.454
.56?
.74;
.6"
.09-)
.266
.367
.584
.13:
.2?E
Area
IPV-S]
303.
6177.
:£26.
773£.
20010.
26729.
1074.
10092.
16306.
370327.
1646.
48714430.
47527.
255:.
£93:26.
607442.
31098.
1079.
1607.
1J19.
2833.
7115.
130?15.
50064.
336.
40C.
600.
1355.
47-1.
7105.
921.
317.
169876.
71«8.
00
77
OC
JO
:3
50
50
73
00
27
00
00
00
CO
00
s:
97
50
69
61
€?
61
-1
39
2£
?i
00
95
o:
50
00
14
30
00
Height
lllV]
26.
2457.
415.
30?1.
5667.
£426.
219.
2175.
3507.
61877.
435.
25
42
01
27
33
09
87
33
94
38
03
1.0S««06
26368.
602.
iS2325.
162642.
7933.
253.
316.
409.
540.
225.
ni«7.
• 546.
70.
151.
n:.
173.
146.
2507.
224.
97.
48126.
1260.
55
63
33
64
75
84
15
26
56
16
31
29
27
o:
84
4*
:s
49
13
90
32
93
*r«j
It)
«e-04
0.01
0.01
o.o:
0.04
0.05
0.00
0.02
0.04
0.73
0.00
JS.57
0.13
0.01
1.36
1.19
O.Of
0.00
0.00
0.00
0.01
0.01
0.26
0.10
7«-04
8*- 04
0.00
0.00
»*-04
0.01
0.00
6*-04
0.33
0.01
EL Xrt»/Beight
Is]
BE
BE
IV
w
VE
BV
VI
BV
W
VB
BE
•BT
•TT
*TT
*TT •
BV
VB
BB
BV
VB
BV
VB
BV
VB
BV
VB
BV
W
VB
BI
KB
BV
BE
tv
11.54
2.51
6.33
2.50
3.41
4.16
4.69
4.64
5.22
4.52
3.76
46.61
2.56
3.18
. 4.55
3.73
3.92
4.25
5.09
4.69
5.24
31. 60
7.63
5.86
4.ei
2.61
4.63
7.e:
2.91
2.83
4.11
3.24
3.53
5.71
X«v .
taount
0
0
0
0
0
0
0
0
0
0
0
48
0
0
0
0
0
0
.0003
.0062
.0026
.0077
.0200
.0267
.0011
.0101
.0163
.3703
.0016
.7144
.0065
.0026
.6932
.6074
.0311
.0011
0.0016
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0019
.0026
.0071
.1309
.0501
.0003
.0004
.0008
.0014
.0004
.0071
.0009
.0003
.1699
.0072
-------
//
Sequence File: C
4.0<1C29>
10:11 AM
0.10 MG/ML SPIKE SOLM
C:\TC4\GC5\C6D0003.RAW
C:\TC4\GC5\WA45SPK.SEQ
GC 5 Rack/Viai: 0/0
£2-e: 4/i5/?f 09:58 AM
Cycle: 3 Channel : A
Operator: TLM
Eliuticr. Fs"cr : 1.0:
30
*nco •»
f»r- CD co
II III
I I i I I I I N I II I I II I i I II il I i : . i ! I 1 I : i MM I II I I I I I I M I I
IT
14
WA 45 REPORT
**t Component
• Nam*
I
^
3
i
c
C
1
•
*
'.')
:i
., t" :n.:^ft^
* v/
-•» /f££J*77)f1*T-r /g
•_~
;*
••
20
H
"*
_I
_t
•e
jS
-~
.*
..-
•r;
~
:-
Time
(nan)
0.442
0.537
0.7^8
1.568
1.468
2.031
2.191
2.762
3.131
4.244
4.404
4 inn
^^ . /uu
'&. 5.003
5fr(» 5.500
5.9?3
€.325
6.630
7.031
7.556
7.883
.470
.595
.956
.535
.966
10.160
10.95;
11.068
11.277
11.728
12.70?
Area
(uv-s)
187.00
369.00
300.00
6354.00
4697.47
9523.03
4540.50
287.00
313954.50
39349.50
34920.50
^fiQfii nn
*D?O i . UU
174.00
356.00
488573.00
£43.00
1025.50
326.77
4275.43
1976.29
2306.84
213.00
«?568.1«5
840.00
738.03
5280.11
12192.66
£523.?:
1339. 6£
94042.31
57325.51
luv;
81.43
67.64
li.?9
3327.26
2736.44
2086.48
624.45
57.40
57990.62
2810.56
3683.62
30.12
J3.CO
142940.3d
si.ee
244.01
€2.47
112.16
104.18
753.36
53.85
9684.21
S9.4?
148. »9
367.34
6*4.40
1126.1?
190.64
7319.09
499J.73
\\\
0.02
0.03
0.02
0.56
0.39
0.78
0.37
0.02
25.78
3.23
2.8?
251
» a
0.01
0.03
40.12
0.05
0.08
0.03
0.35
0.16
0.1«
0.02
8.01
0.07
0.06
0.43
1.00
0.54
0.11
7.72
4.71
IL Arva/Height
(s)
BB
BV
VB
EB
BV
VB
BB
11
IB
•BT
*TT
•TT
It
gg
BV
BI
EB
BB
BV
W
VI
It
rv
VB
BB
BV
W
W
w
w
w
VI
2.30
5.46
15.97
2.06
1.72
4.56
7.27
5.00
5.41
14.00
9.48
}K^
. Si
5.78
6.72
3.42
12.39
4.20
5.23
38.12
18.57
3.06
3.96
10.07
9.39
4.95
14.37
17.55
5.79
7.03
12.85
11.47
RJV
taount
0.0002
0.0004
0.0003
0.0069
0.0047
0.0095
0.0045
0.0003
0.3140
0.0333
0.0349
-0.0002
0.4886 T (/>(jl L^T ^^*X ' LS~
0.0006 J? ft
0.0010 C\ /} \\lCj ^J^'
0.0003 / *^' '
0.0043
0.0020
0.0023
0.0002 -ir
0.09?6 1 , tf\*
°'°OC? / If t*'ll""J^ ^ ft*
0.0052 '^^\n, \~
0.0122 • — , •, 1 i~V '
0.00£5 «/•'*
0.0013
0.0940
0.0573
1217(65.50 250199.71 100.00
1.1908
-------
rtft>/=re Version: 4.0
: = te: 4/15/96
'=Tiple Name :
eq'jence File:
r.strument :
10:31 AM
0.10 KG/hC, SPIKE SOLN
C: \TC4 \ GC5\C€D0004 . RAN
C: \TC4 \GC5\VF.45SPK.SECj
GC_5 Rack/Vial: 0/0
: 1.0:00
Date: 4/15/96 10:18 AM
Cycle: 4 Channel : A
Operator: TLM
Diluticr. Fa-rt-rr : 1.00
enKCIOCM
c- w r- e; •"> to
tc ie ic
CM V— «•". COO
00
«C
1 1 1 1 1 II
i i 1 1 i I I I I I I i I M I I
1 II I1 An— rm Mill 1 1 II III 1 II I n i n i i
CE «-
11
Ml! I I M I I I I
2
I i 1 | I ! I I j I I II | i I II | I I I I | 1 I I i | I II I | I I II | I 1 I I | II I I j II II | I I I I j I I I J
4 6 6 10 12 14
Time [min]
WA 45 REPORT
T*k Component
• M«mt
1
2
4
c
€
"*
e
a
:o
. i
i:
13
.J
.5 Acrrsrr-ni*.
*"
• ? $££fof)fib~i '/£
:o
:i
* ~
. i
.;
_•£
--
It
.•»
t>
i
::
* j
.4
;
'r
Tune
Imin]
0.442
0.530
o.7i:
1.023
1.56-
1.867
2.029
2.140
2.209
2.756
3.116
3.806
4.247
4.417
4Ln «-«?3
*m> 4.996
y/isf3l 0
0.0038 ''
0.0036
0.0104
0.0772
-------
-T i i ;
i-nle Name
1C:45 AM
0.121 MG/ML 5
C: *7C4\GC5\
C:\ TC4\GC5\fcl55 ?K. SEQ
GC 5 Ra-rk/Vial: 0/0
Date: 4/15/96 10:37 AM
Cycle: 5 Channel : A
Operator: TLN
Dilution Far~:r : 1.'
^ w w.
D ^r ID iT>
. ; C O — -
II I 1 1 I
u"> Of* C
tT, O>— ^
II
O
r*
tc>
I
J-w-v^. ,
I ' 111 11i i| I
0 2
TT
TT
NN
8
Time [min]
10
12
14
WA 45 REPORT
E3
Tsmponent Tim*
Name (min)
0.442
0.533
0.84*
1.551
1.694
1.850
2.005
2.217
2.348
2.547
2.962
3.168
3.603
4.175
fropitrutril* 5.12,2
5.687
6.047
6.494
6.720
8.283
Arc*
luv-s]
197.00
6J5.00
626.00
5?f S.'O
2196.00
6381.63
14904.41
14060.61
1298.00
1106.51
23014.65
272925.50
1432.00
47638997.50
67407.00
2776.00
71?550.50
618049.35
20727.04
23386.39
Height
79.46
79.28
31.64
287:. 17
332.07
3138.51
4438.71
3816.11
229.75
176.61
2989.94
60369.17
368.04
1.06**06
25876.10
828.28
155920.33
162699.19
7194.69
7.14t~13
Art*
4t-04
0.00
0.00
0.01
0.00
0.01
0.03
0.03
0.00
0.00
0.05
O.S5
0.00
J6.J?
0.14
0.01
1.46
1.25
0.04
0.05
BL Arta/Rtignt
19)
BB
BV
VB
BI
IV
W
w
VI
tv
w
w
w
BB
«BT
•TT
•TT
•TT
BV
W
VB
2.48
7.88
15.78
2.09
6.58
2.03
3.36
3.68
5.65
6.27
7.70
4.52
3.89
44.95
2.60
3.35
4.62
3.80
2.88
3««16
Mount
o.ooo:
0.0006
0.0006
0.0060
0.00:2
0.0064
0.0149
0.0141
0.0013 -
0.0011 'If
0.0230 . I?
0.2729 1 | 1 '
0.0014 -7 '
47.6390 ( ',1
0.0085 >«,\
0.0028 b
-------
28 •
Book No. aM'/J^ 0 TITLE L*- irn/jAfLrrmon
-------
APPENDIX C-2
Sorbent Preparation
and Analysis
-------
TITLE "T^f? flu^p
Project
29
-------
Project No
BookM« an228TITLE T^p
=rom Page No
K), i
... ;
..-I.--
.3H.
HP !
. . . 1 42, ; ; ; .....
. Ml ; ., i .
. eo., .: ...:
; -ti: . .
._i_jy_.._t
. .:3M i
, ..; T3
... r31
-40 ;
-Hi
Mt.'oOft
.- 00}'
^.OU
To Page No
& Understood by me,
Date
Invented by
Date
-------
ige No— ,
I . ...j_j-.
t ... ..,——
I . I ' A I
-7 P^H-^-
-------
'. i JLAc/l ;
'
To Page No
nderstood
lnv*nt*d by
Da
-------
T'jrr'C-rr.rcr, Sequence File :
Crested ty : JLSTEGER
£ditec by" : JLSTE-3ER
T: \TC4\GC5\S6DH.SE-r
on : 4/23/96 OJ-.03 PM
on : 4/23/96 C?:32 FM
Nurr.h-er cf Times Edited : 1
Sequence File Header Information:
Number of Rows : 24
Instrument Type : 7£C / 900 Series Intelligent Interface
Injection Type : DUAL
•tM
*
2
3
4
5
£
1
e
9
10
11
1 .
;•)
14
IS
1?
17
IB
i*
:o
n
i;
12
24
Type
Sample
Staple
Sample
Simple
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sampl*
Simple
Sampi*
Sample
sample
Sample
Sampii
Sample
Sample
Sample
Sample
Sample
Cample
Cample
Mane
100 ug/ml QC st
100 U9/BL QC St
H»C12 Ilanic
MeCI2 llant
Extract 68
Extract £8
Extract 69
Extract 89
Extract 70
Extract 70
100 ufl.'ml OC
100 ug/ml £C
MeC12 Ilar.K
MeCi: Elan*
Extract 66
Extract 66
Extract €?
Extract £5
Extract 70
Extract 7C
100 uqrrr.i y:
100 ug/m:. ?C
MeCi: £:*,-,<
MeC12 Elan*
C«quence sample Descriptions - Channel X
Caap.lt Stuay Naae Sample ISTD Cample
Kumt*r Amount Mount Volume
1
1
2
2
3
3
4
4
5
5
6
6
7
7
3
3
4
4
5
5
6
6
7
7
VMS SORB!
W4S SOME
W4S SOUI
«45 SOUE
W4S SOUE
«45 SOUE •
W45 SOMI
WX45 SOUt
Vk45 SORBI
VX4S SOK£E
Vk4S SOR3E
W11S SOUE
W4S SOR2E
Vk4S SOUE
W4!> SOR£E
¥X4i SOUt
HA4S SOREE
W14i SOKEE
WX45 SORir
¥X4b SOR£E
W*4i SOUE
W.4S SOR3E
W4S SOUE
W*4i SOUE
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
:.ooo
1.000
1.000
1.000
1.000
l.OOC
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
l.OOC
1.000
1.00'J
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
1.000
1.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
7.000
Oil.
factcr
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
l.OCC
1.000
1.000
1.000
1.000
1.000
1.000
1.000
l.OOC
1.000
1.000
1.000
l.OOC
1.000
Mult Dr/isor
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
l.OOC
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
1.000
Addend
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
norm.
factor
100.01
100. Ot
100. 01
100. OC
100. OC
100. OC
100.01
100. OC
100.M
100.00
100. or
lOu.OC
100. OC
lOO.Ot
100. Ot
100. OC
100. OC
100.00
100. OC
100.00
100. OC
100. OC
100.00
100. 00
av Site Kiel
3 -
4 -
i.
€ -
7 -
8 -
Q
•.;
;;
j;
13 -
14 -
15 -
lj
r -
1" -
• j
j._i -
;;
;j
.; ;
;j -
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
(•
Vial Inst
Method
1
1
•4
2
3
3
4
4
5
5
e
6
7
7
3
3
4
4
5
5
6
6
7
7
W45-KC
WA45-MC
W4i-MC
W4&-MC
WX45-MC
HX4S-MC
VX4S-MC
W4J-MC
W4S-MC
TO4S--MC
W4S-MC
HX45-MC
MA4S-MC
m4S-Mc
W45-MC
HX4&-MC
VA45-MC
lfX4&-MC
W4S-MC
W45-MC
W4S-MC
WA4S-MC
VA4S-MC
Process
Methcxl
W145-MC
10,4 i-MC
W4&-MC
W14S-MC
W4S-MC
W4J-MC
VX4&-MC
WX4S-MC
WX45-MC
W45-MC
W45-MC
VS^S-MC
¥X4S-MC
V&4S-MC
WX4S-MC
M4&-MC
W4S-MC
W45-MC
HX4&-MC
W45-MC
VA4&-MC
WA4S-MC
W145-MC
W45--MC
Sequence Process Information - Channel X
Calit Report Raw Result Baseline
Kttr.cc romat rile rile me
siEi
W45-MC
VX4S-MC
¥X4i-X
WX4&-MC
¥X45-MC
MA4S-M7
HX4&-MC
Hk4^-W
WX41-V7
IA4&-MC
WX4S-MC
Wk4&-MC
m4^-MC
VX4S-MC
VX4i-«*T
HX4&-MC
VA4S-MC
W4J-MC
W4J-MC
W!»4 5-MC
W4i-MC
SB
Vk4^-MC
WX4S-MC
IA4&-MC
H*4S-MC
WX4S-MC
WX4S-MC
VX4&-MC
W4&-MC
¥X4S-MC
IOk4^-MC
NR4&-MC
WX4&-MC
HX4&-MC
WX4S-MC
KX45-MC
IA4&-MC
WX4&-MC
»4i-MC
TO4S-M7
¥A4i-Mt
WX4 i-MC
sfidv^Ol
S6dw002
>6dw003
•60W004
•towoos
•60W006
•60W007
•CdWOOS
S60W009
• •OV010
•Mwci:
I60W012
• 60W013
•COW014
•60W015
S60w01£
•60VC17
•60W011)
•60W019
<(OV020
S60W021
seowo::
s6ovcr:
I6dw?24
S6dw001
S6dw002
*6dw003
• 60W004
»6OvOOi
•60W006
• 60W007
•COV008
•60W009
• 6dw010
seowoii
• 6OW012
•60W013
•6dw014
•60W01S
•fidvoie
•60W017
•60W018
*6dw019
>6dw020
•60W021
•Sdvc::
•6dvOJ?
S6dv0;j
Modified Cal Uvel update Out
JUv File Rpt Maim RT Dtv
DETR'Jl
- - DETAU1
DEFRUI
DETAU1
DETAU1
DETRUl
DEFRU1
DETAU1
DETAU1
- - DEFA'Jl
oiraui
DIFAUI
- - - DIFAUl
- - DETAU1
- - - DIFAUl
DETAU1
- - DEDIU1
- - DETAL'l
DE7AUI
- - DETRU1
— — • D£f XU1
— — * OEFAUL
— — ~ Dir^ui,
OE7AU1
-------
.:ftware Version:
2a-e: 4/23/9£
id.T.cle Name :
l=rk File :
Sequence File:
Instrument :
ci.-pie Amount
05:
FiX
100 cg/rr.L vC standard
D:\TC4\GC5\Sc DKO 01. R.V.-
C:\TC4\GC5\5£DK.SEQ
GC_5 Rack/Vial: 0/0
: I.OGOG
4'23/?c- 02:2? PM
, . Channel : A
Operator: JLSteger
Diluticn Factor : 1.00
*N »*"» *A UT-Q »*"»
^ r^ ^i tf ** r-" ^ o w
i i 11 ii i
T^ArvJ-i
10 o i/i oq
to
CO ^ (O^ OUUCO
o m 01—
o Q Q_-
I I I j I I I I j I T I I i M I ITI i i TT IT TT I I i Tl I I TlIT MI I I I I I I I I 1 I I I I I I I I | M I I I I I I
0 2 4 6 a 10 12 14
Tim* [mm]
WA 45 REPORT
*t Component
Name
^
^
I
I
5
€
•
!
»
•
I
z
>
*
: *c«tonitrile
= Propionitra.1*
•
A
i
*
Tim*
(nun)
0.420
0.525
1.233
1.553
1.849
2.016
2.197
2.316
2.532
3.035
3.136
3.439
3.559
4.175
5.982
6.40!
6.645
7.545
8.661
9.069
9.172
9. 821
10.081
1C. 567
10.67?
10.959
11.166
11.704
11.949
i:.085
i:.2ei
12.404
12.729
luv-s]
162.
353.
185.
9051.
7596.
32034.
255.
9815.
372.
484025.
245869.
2080.
43449.
38629428.
428528.
559863.
755.
2333.
3405.
239.
103.
262.
183.
426.
5'0.
5892.
5263.
4309.
1401.
1056.
554.
2610.
748.
CO
00
00
66
32
00
50
00
00
47
09
06
38
iO
00
00
00
00
00
50
50
33
50
13
cc
79
36
•J t
59
53
27
8?
55
Height
luv]
46.30
62.43
13.39
3849.59
3777.62
6242.44
111.01
3319.53
81.91
79972.38
71429.63
307.53
12850.68
1.12«-06
121359. (8
161783.48
120.88
442.14
421.65
59.17
29.43
19.81
47.08
47.58
84.09
828.30
1204.57
316.46
236.86
141.96
102.76
177.32
103.74
Art*
IV
4C-04
9*-04
Sf-04
0.02
0.02
0.08
6*-04
0.02
fe-04
1.20
0.61
0.01
0.11
95.42
1.06
1.38
0.00
0.01
0.01
6*-04
3«-04
7t-04
Sc-04
0.00
O.OC
0.01
0.01
0.01
0.00
0.00
0.00
0.01
0.00
Bi Arct/Stignt
Is!
11
BE
IB
IV
w
VI
IV
VI
11
IV
w
w
VI
•IT
TT
It
KB
IB
IB
IB
11
VI
IB
IV
w
w
w
w
w
w
w
w
VB
3.50
5.75
13.81
2.35
2.01
3.89
2.30
2.96
3
1
.54
.05
.44
.76
.38
.56
.53
.10
.25
.28
.06
.05
.52
.25
.90
.96
6.7?
7.11
4.39
13.62
5.92
7.44
5.39
14.72
7.22
Raw Ad]. Ant.
Amount lug/aLj
0
0
0
0
0
0
0
0
0
0
0
0
0
38
100
101
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0002
.0004
.0002
.0091
.0076
.0320
.0003
.0098
.0004
.4840
.2459
.0021
.0434
.6294
.4996
.0572
.0008
.0023
.0034
.0002
.0001
.0003
.0002
.0004
.0006
.0059
.0053
.0043
.0014
.0011
.0006
.0026
.0007
o.ooo:
0.0004
0.0002
0.0091
0.0076
0.0320
0.0003
0.0098
0.0004
0.4840
0.2459
0.0021
0.0434
38.6294
100.4996
101.0572
0.0008
0.0023
0.0034
0.0002
0.0001
0.0003
0.0002
0.0004
0.0006
0.0059
0.0053
0.004:
0.0014
0.0011
0.0006
0.0026
0.0007
-------
cftwcre Version: •5.0
=:e: 4/23/96 06:06 FM
£2-pie Nar.e
S=t"= File
Sequence File;
Instrument :
-zr.ple Ar.our.t
100 ug/ml •!"- star.c2rci
D: \TC4\G~5 \5£DWOC1. =JkW Date: 4'23/Sc 02:45 PK.
C:\TC4\GC5\S6DW.SE~ Cycle: 2 Channel : A
GC_5 Rack'Vial: C'C Operator: JLSteger
1 0 ^ ^ ~- r>' ~ <• - • r^ E"* <---»• • 1 0n
• J. • W w ~ '» !,'_ .1 — - .*. O * . - a _ . 0. • -/ -
ci —'•-' r>j
I III
—
-------
Version: -J.C<1C19>
3=-e: 4/23/56
52-pie Name :
3=ts File :
Sequence File:
Instrument :
=2~pie Amount
05:58 FM
MeC12 Blank
C:\TC4\GC5^.£6D«C03.RJW Date: 4/23/96 03:09 ?M
C:\TC4\GC5\5cDK.SE9 Cycle: 3 Channel : A
GC_5 Rack/Vial: 0/0 Operator: JLSteger
: l.OOOC Dilution Faotor : l.C-0
o CN
r* m
co P* 9^> in 0*
to - - — - - - - - -- -
O — — -<>i«*-i CN >">>"> >— in
o_ _
1 1 1 1
3T
S.
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31
Tim
0.
0.
1.
1.
1.
2.
2 .
2.
2.
2.
2 .
3.
3.
3.
3.
6.
• 1.
J.
9.
9.
10.
10.
1 C •
11.
11.
12.
*
r.l
634
toe
191
524
860
025
14?
229
371
476
777
069
332
649
JJ2
650
500
131
367
634
126
€44
?75
179
57-
925
Art a
tpV-Si
164.
266.
274.
6717.
206.
12503.
22890.
20860.
598.
26318.
696.
71809.
1134530.
110411.
59341828.
2706.
28?.
1703.
2798.
494.
582.
240.
716.
1677.
11387.
10883.
50
00
00
50
50
67
64
02
CO
66
00
71
29
00
00
75
25
69
22
41
00
00
54
46
00
00
Height
IpV)
58.24
63.46
23.63
3054.99
70.67
4088.47
4310.26
4316.94
223.05
6568.04
• 2.68
12118.86
203064.53
37009.94
1.12»-06
77.72
0.00
396.68
209.28
64.03
179.81
26.97
95.64
545.93
979.10
1220.72
Art*
3«-04
4t-04
5*-04
0.01
}«-04
0.02
0.04
0.03
le-03
0.04
0.00
0.12
1.87
0.18
97.63
0.00
5«-04
0.00
0.00
••-04
1C-03
4t-04
0.00
0.00
o.o:
0.02
BL 1
BB
ll
BB
BE
BV
W
W
VI
rv
VI
BB
BV
VB
BB
•BB
BV
VB
W
W
VB
BB
B£
BV
VB
IB
BB
irta/Bcignt
2.82
4.19
11.59
:.20
2.92
3.06
5.31
4.83
2.68
4.01
1.42
5.93
5.59
2.98
53.16
34.82
..__
4.29
13.37
7.72
3.24
8.90
9.58
3.07
12.24
8.92
K*
Amo
0
0
0
0
0
0
0
0
0
0
0
0
0
0
•
0
0
0
0
0
0
0
0
0
0
0
tf Ac
unt l
.0000
.0000
.0000
.0010
.0000
.0018
.0033
.0030
.0001
.0038
.0001
.0103
.1621
.0158
.4774
.0698
.0000
.0002
.0004
.0001
.0001
.0000
.0001
.0002
.0017
.0016
!]. Amt.
ug/ml)
0.0000
0.0000
0.0000
0.0010
0.0000
0.0018
0.0033
0.0030
0.0001
0.0038
0.0001
0.0103
0.1621
0.0158
1.4774
0.0698
0.0000
0.0002
0.0004
0.0001
0.0001
0.0000
0.0001
0.0002
0.0017
0.0016
6078435:.91 1.40e-06 100.00
8.7529
8.7529
-------
Version: 4.0
late: 4/23/56 05:56 FM
iB.T.pie Name :
I/a-a File :
Sequence File:
Instrument :
ssrncle Amount
MeCil clank
D:\TC4\GC5\StDW004.RAW Date: 4/13/56 03:16 PM
C:\TC4\GC5\56DK.SEC1 Cycle: 4 Channel : A
GC_5 Rack/Vial: 0/0 Operator: JLSteger
: I.COCO Dilution Farter : l.C;
c. —
I II I I I I I I I i I I I I I I I I I ! I
f. -".BO— uioo "> in ^
in •- •- r* O* f*
b bo- —'—r>i (N «N
I II I I II
11 11 I II I 11 III I I III I 11 III I i 1 I I j I I I I I I I I 11 i II 11 I
6 8 10 12 14
Time [min]
WA 45 REPORT
fett Component
( Nlme
1
t
3
4
5
6
7
6
0
10
11
i:
i:
;;
15
16
* '
16
1?
2Z
21 Acctonitnlt
;;
27
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; j
;t
^~
:?
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3?
31
j;
34
1C
Tlfl*
lisir.l
0.100
C.J3P
0.613
1.535
1.904
2.037
2.256
2.519
2.746
2.925
3.053
3.112
3.263
3.576
3.714
3.851
4.092
5.076
5.161
5.762
€.162
7.235
7.316
9.151
?.414
9.515
10.166
10.734
10.983
11.205
11.551
11.762
12.354
12.738
Art*
lwv-s)
375
ie:
555
77?6
2750
11863
100553
17230
1211
15108
72934
C2956
€70414
1377
72104
544
51962420
80072
31699
2229
30465
S3540
87513
1205
1891
729
6891
437
493
1456
J?ll
1512
246
1£3
.03
.00
.00
.50
.32
.95
.66
.36
.59
.38
.69
.77
.23
.31
.03
.00
.39
.00
.00
.00
.00
.4-
.15
.00
.81
.19
.00
.ee
.15
.48
.20
.to
.00
.50
•tight
IpV]
33.72
59.23
36.33
3786.30
551.46
3580.12
16770.90
4187.40
183.07
3153.28
13473.12
13419.17
115291.44
361.44
21946.77
103.65
l.lle*06
24923.02
12119.75
£63.77
7416.66
2599.74
2595.95
269.67
259.67
255.01
2323.19
63.02
53.49
401.66
862.80
255.03
71.47
41.22
Art*
It]
7t-04
3*-04
0.00
0.01
0.01
0.02
0.19
0.03
0.00
0.03
0.14
0.12
1.26
0.00
0.14
0.00
»7.47
0.15
0.06
0.00
0.06
0.10
0.16
0.00
0.00
0.00
0.01
t*-04
**-04
0.00
0.02
0.00
S*-04
3*-04
BL Arti/Beignt
Is]
BB
BB
BB
BB
BV
W
W
VB
BV
w
W
W
w
w
VI
EB
•BT
TT
•TT
TT
TT
•W
• VB
BV
W
VB
U
BV
W
VB
BV
VB
BB
BB
11.12
2.74
14.48
.06
.99
.32
.00
.11
.62
.79
.41
.€9
.81
.75
.29
.25
46.88
3.21
2. €2
3.36
4.11
20.59
33.71
4.47
7.2?
2.86
2.97
6.95
9.22
3. €3
11.23
5.93
3.44
3.97
RJV Ad]. Ant.
Aoount !u5/sL>
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
7
0
0
0
1
0
0
0
0
0
0
0
0
0
0
0
0
0
.0001
.0000
.0001
.0011
.0004
.0017
.0144
.0025
.0002
.0022
.0104
.0090
.0958
.0002
.0103
.0001
.4232
.0114
.0045
.0003
.0207
.0076
.0125
.0002
.0003
.0001
.0010
.0001
.0001
.0002
.0014
.0002
.0000
.0000
0.0001
0.0000
0.0001
0.0011
0.0004
0.0017
0.0144
0.0025
0.0002
0.0022
0.0104
0.0090
0.0956
0.0002
0.0103
0.0001
7.4232
0.0114
0.0045
0.0003 _ 1
1.0207 -f ^f ~ O.nt **&'*•*'-
0.0076
0.0125
0.0002
0.0003
0.0001
3.0010
0.0001
0.0001
0.0002
0.0014
0.0002
o.oooc
0.0000
-------
Software Versic-r.: 4.0<1C2?>
I-2ie: 4/23/96 G6:2'"7 PM
Sa.-r.ple Name : Extract 66
1-2-a File : D:\TC4\C-C5\S6DWOC5.RArt Dace: 4/23.'.-£ 03:4*
.Sequence File: C:\TC4\GC5\56DW.SEv Cycle: 5 Channel : A
Ir.ctrumer.- : GC_5 Rack/Vial: 0/0 Operator: JLf-eger
** ?• •*• *• * o zij^ <", * • *^ *• • ** o^^'^ ~) •
i.o-:
4O OTMOO rfl
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I I I I III 111 I
l II I I Mil
II I I I I I II I III I II Ii
in i i nil i1 nn
1 1 ii 1 1 1 1 1 1 n 1 1 1 1 1 1 1 1 M 1 1 1 1 1 1 i 1 1 1 1 1 1 M i i i 1 1 1 1 1 1 1
n 1 1 1 1 1 1 1 i MI TI i
'
i rn
WA 45 REPORT
=*-*k Component
• Name
1
2
3
<
5
C
*?
4
a
I-
ii
I.
IS
14
15
le
17 Acttonitnle
18
l> Propionitrilf
ii
Ii
^2
;;
^4
••e
^iT
J~
;j
Ti
10
J*
XI
2.'
Ti
Tune
(mini
0
1
1
1
2
2
2
2
5
5
5
6
6
6
6
6
7
7
7
g
e
1C
10
.735
.519
.704
.836
.017
.270
.482
.701
.984
.087
.336
.651
.942
.065
.501
.717
.163
.369
.560
.792
.971
.293
.385
.718
.257
.364
.512
.112
.427
.525
.775
.875
.172
.641
ltlV'3]
444
6796
1335
93686
20756
134877
24J57
1061
34628
39023
1253216
82837
57468678
182855
12668
133J
30324
1249
791503
12746
1226
9941
613
1012
680
711
1114
2776
2060
1760
242
1499
9257
417
.00
.00
.82
.83
.61
.50
.73
.57
.29
.44
.20
.50
.00
.00
.00
.00
.00
.00
.00
.50
.79
.63
.56
.00
.25
.75
.00
.00
.36
.64
.38
.62
.00
.63
Height
luv)
59.32
3617.1?
638.45
19547.81
5308.31
19182.75
5514.70
148.06
4147.18
8137.89
208557.17
28093.07
1.02*»0€
45932.47
1549.64
-1039.00
7020.03
300.52
202816.75
3387.48
204.76
802.34
269.33
326.75
154.62
140.41
203.63
531.43
517.63
426.21
76.29
294.66
2976.70
124.03
Are*
7«-04
0.01
0.00
0.16
0.03
0.22
0.04
0.00
0.06
0.06
2.08
0.14
95.39
0.30
0.02
0.00
0.05
0.00
1.31
0.02
0.00
0.02
0.00
0.00
0.00
0.00
0.00
0.00
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0.0134
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0.0193
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0.0049
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0.0000
0.0002
0.0013
0.0001
-------
re version:
=te: 4/23/56
I-: pie Name :
its file :
•r—jence file:
06:35 FK
Extrsc- 68
D:\TC4\GC5\5cjW006.R-W Date: 4/23/?c 04:06 PM
C:\TC4\GC5\SiDVJ.SEQ Cycle: 6 Channel : A
GC_5 Rack'Vial: 0/0 Operator: JLSteger
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2.110
2.287
2.474
2.700
2.986
l.n75
3.359
3.634
3.892
5.051
5.750
6.165
6.371
6.561
6.793
7.223
7.400
7.721
8.36?
8.397
8.524
8.778
9.129
9.437
J.530
9.782
9.864
10.177
Area
IwV-s)
156.50
924.00
6124.50
2349.54
105896.70
20481.34
5106.17
90226.39
28054.86
370.00
46794.56
41062.60
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1605.52
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1228.00
1175.21
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1416.79
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3644.30
2023.22
1935.98
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1440.00
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Height
luV)
58.50
57.22
3233.79
953.61
20108.64
5096.54
1387.13
14663.21
5748.10
73.91
8171.20
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241068.42
32917.23
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95744.60
429.92
6467.79
327.52
227507.85
3874.66
46.75
326.75
156.80
217.93
155.20
251.62
36.18
647.81
553.86
396.30
75.04
295.82
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2e-04
0.00
0.01
0.00
0.17
0.03
0.01
0.14
0.04
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0.07
0.06
2.22
0.15
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0.04
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3.68
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4.62
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4.16
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3.94
3.78
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3.42
5.39
4.39
5.63
2.82
5.63
3.65
4.16
3.54
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Amount
0.0000
0.0001
0.0009
0.0003
0.0151
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0.0007
0.0129
0.0040
0.0001
0.0067
0.0059
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0.0136
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0.0857
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0.9024
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23.1266
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0.0002
0.0002
0.0001
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0.0000
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0.0000
0.0001
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0.0151
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0.0007
0.0129
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0.0136
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0.0857
0.0001
0.9024
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23.1266
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0.0001
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0.0002
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0.0001
0.0002
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0.0005
0.0003
O.OOC3
0.0000
0.0002
0.0014
-------
ire Version: 4.0<1C29>
4/23/56 06:34 PM
:?. File : D: \TC4 \GC5\S6DW007. RAW Date: 4/23/96 04:27 PM
Tuence File: C:\7C4\GC5\56DW.SEO. Cycle: 7 Channel : A
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1.817
2.012
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3.344
3.605
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4.444
5.469
5.729
5.827
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6.154
6.157
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6.763
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48569
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0.00
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0.01
0.00
0.20
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0.07
0.04
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0.10
2.42
0.15
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1.47
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0.00
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2.11
4.52
5.33
2.77
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6.00
2.84
65.06
6.76
2.87
2.99
2.14
4.30
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4.87
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3.43
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3.91
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6.13
4.24
4.63
3.85
3.96
5.85
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5.55
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Amount
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
0
0
n
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0
0
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0
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0
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0
0
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.0001
.0069
.0043
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.0099
.2491
.0157
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.2024
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.9057
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.0001
.0003
.0010
.noo3
.0001
.0003
.0000
.0000
.0004
.0004
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nj. Ant.
(ug/nL)
0.0001
0.0000
o.ooin
0.0002
0.020J
0.0023
0.0001
0.0069
0.0043
0.0000
0.0099
0.2491
0.0157
9.2901
0.2024
0.0008
0.0001
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0.7121 ^'*°- Oi|0*H>P* " •• 1'
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-------
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0 246 B 10 12 14
Time [min]
WA 45 REPORT
P?i* Component
;
•
J
c
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1
9
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11
1.
1 1
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15
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0.635
0.755
1.S01
1.614
1.663
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1.995
2.086
2.26f
2.440
2.667
2.DR9
3.036
j.Jt3
3.M?
3.806
4.971
5.413
5. £96
5.79i
6.119
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6.747
7.071
7.161
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8.233
8.355
6.513
6.726
6.864
9.103
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1906
2467
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19311
4675
57779
32669
263
21152
33830
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1232214
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1152
21
-------
^fcware Version: 4.
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fari
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pie Name :
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n
1 M |TTTTjn I I j M I I j Mil j I I II | M I I | I M i J I I I I | M I I | I M I
6 8 10 12 14
[min]
WA 45 REPORT
Component Time
Name (nun]
0.
0.
1.
:.
i.
i.
i.
i.
2.
2.
2.
2,
2.
3.
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617
359
468
596
659
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966
448
697
796
8?5
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322
520
747
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382
663
936
244
370
510
735
107
Area
[pV-s]
147
625
111
6216
1432
2401
166657
28924
48445
37163
190
18759
36355
2061117
121560
69254913
1353860
6353
1000
1694
1421
20783
2560
3631342
21740
768
2466
7581
615
1361
1316
2571
556
2552
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.00
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.26
.67
.33
.26
.50
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.57
.62
.11
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.00
.00
Height
Inv)
56.45
47.16
12.00
3666.98
556.64
620.98
21984.73
4471.41
9132.44
6119.86
77.00
3641.23
6997.97
325152.83
44766.30
1.01*«06
194933.77
2463.26
330.09
€16.59
330.28
5195.96
504.15
399269.23
6336.51
-291.61
626.63
2158.19
73.46
300.68
265.36
531.31
142.66
407.35
Art a
(»]
2C-04
6C-04
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0.01
0.00
0.00
0.22
0.04
0.06
0.05
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0.02
0.05
2.66
0.16
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1.76
0.01
0.00
0.00
0.00
0.03
0.00
4.72
0.03
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0.00
0.01
0.00
0.00
0.00
0.00
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0.00
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[5]
BB
BB
BB
n
rv
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w
w
w
VI
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BV
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2.61
13.25
9.29
2.24
2.57
2.93
7.59
6.47
5.30
6.07
2.47
4.68
5.20
6.34
2.72
€6.71
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2.56
3.03
3.06
4.30
4.00
5.12
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3.43
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3.92
3.51
11.10
4.60
4.61
4.64
3.J1
6.26
Aav Ad]. Ant.
Amount (ug/mL)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
0
0
0
93
0
0
0
0
0
0
0
0
0
0
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0.
0.
0.
0.
0.
0.
0.
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0.
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0.
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0.
0.
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0000
0001
0000
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0002
0003
0238
0041
0069
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0000
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0052
2944
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8936
1934
0009
0001
0003
0002
6963
0004
6385
00:i
0001
0004
0011
0001
0002
0002
0004
0001
0004
-------
re Version: 4.0<1C29>
•are: 4/23/96
ar.cle Name :
sta File ;
'eq'jence File:
r.strument :
05:59 PM
100 ug/mL QC
C:\TC4\GC5\S6DWG11.RAW Date: 4/23/96 05:46 PM
C:\TC4\GC5\S6DW.SEv Cycle: 11 Channel : A
GC_5 Rack/Vial: 0/0 Operator: JLSteger
: 1.0000 Dilution Fartr-r : l.C-
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Time [min}
I I | I I I I | I I I I] I
12 14
111
WA 45 REPORT
«*t Component
1
^
I
4
I
6
7
9
9
i:
11
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; j
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24
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Time
(nun)
0.438
0.631
1.092
1 .546
1 .719
1.638
2.062
2.320
2.556
3.051
3.569
4.056
5.011
5.099
5.690
6.042
6.464
6.732
7.291
7.664
8.537
9.147
9.427
9.496
9.933
10.155
10.636
11.063
11.198
11.602
11.777
12.151
12.340
i:.sn
Xr*a
Ipv-sj
160
624
255
7513
3683
6744
S6859
11262
1406
531122
49113
51286500
Height
lUV)
.00
.00
.50
.94
.94
.49
.63
.00
.00
.00
.00
.50
14561.50
44164
2122
509856
616494
229
14939
1373
569
761
£42
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202
2257
9339
916
1477
2192
2258
520
619
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.50
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63.
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06
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92
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63
10
55
79
54
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It]
Je-04
0.00
5*-04
0.01
0.01
0.01
0.11
0.02
0.00
1.00
0.09
96.43
0.03
0.06
0.00
0.96
1.16
4*-04
0.03
0.00
0.00
0.00
o.on
0.00
4*-04
0.00
0.02
0.00
0.00
0.00
0.00
le-03
0.00
0.00
BL Area/Height
U)
BB
BB
BB
BV
W
W
VB
BB
BB
BB
BB
•BT
•TT
•TT
•TT
TT
BB
BB
BB
BB
BB
BV
W
W
VB
BB
BB
BV
VB
BV
W
W
W
W
3.04
16.02
8.31
2.61
4.79
2.61
4.19
3.05
6.32
5.83
3.77
47.27
2.25
2.50
3.64
3.69
3.32
2.73
14.62
3.17
5.17
5. CO
4.79
11.41
-2.68
2.95
17.32
7.22
4.96
10.20
9.29
6.23
4.70
9.14
Ksv 1
taount
0
0
0
0
0
0
0
0
0
0
0
51
0
0
0
119
111
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0002
.0006
.0003
.007E
.0037
.0067
.0569
.0113
.0014
.5311
.0491
.2665
.0146
.0442
.0021
.5729
.6403
.0002
.0149
.0014
.0006
.0008
.0006
.0019
.0002
.002';
.ooe:-
.COG-
.0011
.0022
.0023
.0005
.0006
.0024
Wj. Amt.
-------
.•=re version:
4/23/95 0£:1S PM
.e flame : 100 ug/rr.L QC
File : C:\TC-l\GCf-\S£:-?J012.RA'/; Date: 4/23/96 06:
rr.re File: C:\TC-i\GC5\S6DW.SEQ Cycle: 12 Channel :
••-iment : GC_5 Rack/Vial: 0/0 Operator: JLSteger
e .-jr.v'jr.t : l.OCC'C Diluti:n Factor
•T 13
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CO
II
I I II I I I
to
I
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1 II
Ml I i I I I I I I I II I i I I i I I II
I I I I
0 2 4
1 j i i II | I M I ] I I M | I I I I | M I i | II I I | I I Tljl
6 10 12 14
Time [min]
WA 45 REPORT
Component Tune
Name tmin]
0
0
1
1
1
1
2
2
2
3
3
4
4
5
5
iretonitrile 6
Tcpionieril* 6
6
7
7
6
9
9
•}
10
10
11
11
11
11
11
i:
12
12
.44:
.679
.364
.537
.717
.834
.056
.313
.548
.043
.558
.058
.99:
.oe:
.674
.030
.470
.727
.277
.650
.526
.130
.41?
.490
.141
.e:s
.os:
.183
.604
.760
.896
.133
.309
.45:
Area
luv-s)
153
980
731
652?
3912
7549
54589
12017
1544
541150
50365
50991149
19401
41936
2114
517891
630283
£74
14921
1424
125
2678
766
1412
3226
6213
801
3024
869
(43
177
SIS
411
10:
.50
.00
.00
. 0?
.00
.36
.00
.82
.73
.00
.00
.50
.00
.00
.00
.50
.CO
.50
.00
.00
.00
.85
.55
.60
.00
.00
.50
.50
.00
.00
.00
.00
.00
.00
H»l?h
IllVI
56
54
4:
3523
738
2904
11913
3796
236
91(41
14701
995339
7638
16953
571
134260
188483
203
10(9
451
(0
C30
161
249
1031
557
108
976
102
168
65
78
123
22
t
.03
.90
.33
.3:
.17
.74
.42
.76
.51
.56
.39
.97
.97
.78
.88
.67
.82
.88
.35
.13
.41
.67
.59
.61
.26
.88
.31
.76
.82
.01
.94
.82
.15
.(9
Area
It)
3e-04
0.00
0.00
o.o:
0.01
0.01
0.10
0.02
0.00
1.02
0.10
96.35
0.04
0.08
0.00
0.98
1.13
0.00
0.03
0.00
2t-04
0.01
O.OC
0.00
0.01
0.02
0.00
0.01
0.00
0.00
3«-04
le-03
8e-04
2«-04
SL Arta/Beight
1*1
BB
SB
BV
W
W
w
w
w
VB
BB
BB
•BT
•TT
•TT
•TT
•TT
BB
• BS
IS
IS
BB
BV
W
VB
BB
BB
BV
VB
BV
W
W
VB
SB
BB
2.74
17.85
17.27
2.4:
5.30
2.60
4.S8
3.17
6.53
S.91
3.43
SI. 23
2.S4
2.47
3.70
3.86
3.34
3.31
13.95
3.16
2.07
4.25
4.74
5.66
3.13
14.72
7.40
3.10
a. 45
3.83
2.68
6.53
3.34
4.49
Rav Adj. Amt.
Aaount (uq/mD
0
0
0
0
0
0
0
0
0
0
0
so
0
0
0
121
113
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0002
.0010
.0007
.0085
.0039
.0075
.0546
.0120
.0015
.541:
.0504
.9911
.0194
.0419
.0021
.4574
.7682
.0007
.0149
.0014
.0001
.0027
.0008
.0014
.0032
.0082
.0008
.0030
.0009
.0006
.0002
.0005
.0004
.0001
0.0002
0.0010
0.0007
0.00?5
0.0079
0.0075
0.0546
0.0i:0
0.0015
0.5412
0.0504
50.9911
0.0194
0.0419
0.0021
121.4574
113.768:
0.0007
0.0149
0.0014
0.0001
0.00:7
o.ocoe
0.0014
0.00:2
o.ooe:
0.0009
0.0030
0.0009
0.0006
o.ooo:
0.0005
0.0004
0.0001
-------
5iftv;=re Version: 4.G<1C29>
2i:e: 4/23/9'
=-:r.;erice File:
•.strumenc :
06:46 ?M
M& r 17' fi i a n k
D: '* T ?4 \ GC5 \ 5 •?ZSv" 1 3 .
C:\TC4\GC5\S6DW.SECj
GC 5 Rack/Vial: 0/0
" T'nte: 4/23/f": 06:25 PM
Cycle: 13 Channel : A
Operator: -JLStsger
1C
o
I
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02
T:rrc [min]
f rrrr] M M | [TriTTrnrpr
rTfTf 1 1 1 M 1 1 1
10 12
14
WA 45 REPORT
~*^ K Cowpon^n* Tin*?
• N*n* Imir. ]
: 0.642
: 1.512
1 ) .770
4 1.8€?
: 2.006
" 2.105
' 2.265
0 2.4)99
1 7.69.S
10 2.908
ii 3.070
I"1 3.339
i: 3.631
* ^ J • BJi
:•• S.oift
it *r«tonitril« 6.137
i" e.Tjj
1« 7.225
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-i y.422
10.144
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:; H.604
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156.00
7238.50
141. 67
2257.25
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4324.56
36163.36
2ye06.12
434.00
15825.48
77677.00
1271765.52
126530.00
57j j32 ji . 50
720742.00
24391.50
iJO.OO
6850.00
522.00
556.00
14000.17
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41A.50
6414.20
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391.39
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311. 41
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64.17
2813.09
97.09
464.39
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€798.58
C3J2.24
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3635.20
105JJ.39
22121B.40
43064.00
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C380.64
oi.SJ
«7.30
141.78
114.07
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53:. so
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?45.47
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99. SO
51.55
B*.4u
81.96
^**
3e-04
0.01
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0.00
0.01
0.01
0.06
0.05
7*-04
0.03
0.13
2.11
0.21
)e*uo
1.19
0.04
5*-04
0.01
»*-04
J*-0«
0.0?
0.01
0.00
0.00
0.01
O.uO
n.on
«*-04
0.00
S»-04
11 *
IB
BB
BV
W
VV
W
W
vt
BB
IV
VV
VB
Bl
*fcT
•TT
•BB
•us
BB
BB
At
BV
VE
»v
VB
BV
VV
v;
W
VV
VB
ui
2.43
2.57
3.S4
4.86
2.74
4.93
5.32
4.66
4.96
4.35
7.33
5.75
2.94
51. «
7.05
3.82
3.54
10.92
3.68
4.6*
3.m
15.90
7. ie
3.74
10.03
4.*6
11.69
4.n
12.61
3. BO
R4W AC
Jkjncur.t i
0.3000
0.3010
0.9000
0.0303
0.0010
0.0006
0.0052
0.6042
0.000}
0.0023
O.Olil
0.1817
o.om
i.2647
0.1010
0.9172
C.uOOO
0.0010
0.0001
C.OOOi
0.0070
0.0012
O.uOOi
0.0101
0.3009
O.OOOj
o.ooo?
0.0001
u • 0 u 0 i
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IJ. Amt.
lug/mi)
0.0000
0.0010
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0.0003
0.0010
0.0006
0.0052
0.0042
0.0001
0.002:
O.Olli
0.1817
0.0181
•.2647
0.1030
0.8172
0.0000
0.0010
0.0001
C.OOOI
0.0020
0.0012
0.0001
0.0001
0.0009
O.OOOJ
0.000?
0.0001
0.0002
0.0000
«n.16J733.00 1.5V»Ofi 100.00
1.43K8
-------
Version: <5.0<1C.I?>
:e: 4/23/96
•pie Name :
: ?. Fi 1 e :
T-ence File:
•trument :
06:59 FM
MeC12 512-k
D:'*TC4\G'?5 \S7-DWO 14. RAW Date: 4/23/96 06:45 PM
C:\TC4\GC5\S6DW.SECj Cycle: 14 Channel : A
GC_5 Racfc'Viai: C/D Operator: JLSteger
'. r,r\.~*r. r\;li.»>~.-r*->-. •••**- .tp."i
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i 11 \ \ 1 TrrprrTrjTTrTp"n~r["n'rT]"i 11 \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ 111 \ 11111111111
a
Tim* [min]
10
14
WA 45 REPORT
«
5
5
T
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in
LI
12
L«
15
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M
Component Tia»
Name [mini
0.643
1.169
1.503
1.750
l.*57
2.000
2.095
2. 254
2.452
2.675
2.164
3.052
3.331
1.607
3.158
5.010
5.711
AcetoiutrU* 6.124
6.731
7.225
7.S13
1.S65
3.123
9.404
9. 47*
10. 131
10.568
10.975
11.165
11.571
11.747
i:.i2o
i:.302
11.454
Ar«<
IMV-S]
173.50
222.00
822«.SO
177.00
659.00
5153.84
3698.75
32398.00
30411.41
609.00
47863.38
47167.71
1338324.41
132448.00
59148871.50
630847.00
853.00
26065.00
599.64
535D.1J
3891.77
130.00
911.69
1217.98
73:.33
14316.47
10348.67
3956.83
1154.53
5128.62
2241.79
454.69
209. «0
335.25
Btl^nt
UV]
62.87
26.58
3591.72
64.13
234.48
2484.59
675.98
6079.39
6533.38
112.58
6700.15
9492.69
229746.03
44561.35
1.10e*06
92:44.10
437.86
6598.14
98.86
530.30
4.«4*-14
59.75
179.53
214.81
245.38
4*u*.0e
502.42
261.16
282.04
532.33
351.84
79. 4»
79.05
36.75
Arta
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3»- 04
4C-04
0.01
5«-04
0.00
0.01
0.01
0.05
0.05
lt-03
0.0*
0.08
2.18
C.22
96.17
1.03
0.00
0.04
l»-03
0.01
0.01
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O.OC
o.on
0.00
0.02
0.02
0.01
0.00
0.01
0.00
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5*-04
1L Arta/Height
(s)
IB
BE
BE
IB
BB
IV
w
w
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11
BV
W
VI
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TT
Bl
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BV
W
VB
U
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2.76
8.35
2.29
4.32
2.61
2.07
5.47
5.33
4.65
5.41
7.14
4.97
5.83'
2.97
53.86
6.64
1.95
3.95
6.07
10.10
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2.18
5.08
5.67
2.99
2.98
20.60
15.15
4.09
9.63
6.37
5.72
2.66
9.12
Rjv Ad]. Amt.
Amount (ug/mu
0.0000
0.0000
0.0012
0.0000
0.0001
0.0007
0.0005
0.0046
0.0043
0.0001
0.0068
0.0067
0.1912
0.0189
•.4498
0.0901
0.0001
0.6733
0.0001
0.0008
0.0006
0.0000
0.0001
0.0002
0.0001
0.0020
0.0015
0.0006
0.0002
0.0007
0.0003
0.0001
0.0000
0.0000
0.0000
0.0000
0.0012
0.0000
0.0001
0.0007
0.0005
0.0046
0.0043
0.0001
0.0066
0.0067
0.1912
0.0169
6.4496
0.0901
0.0001
0.8733
0.0001
0.0008
0.0006
0.0000
0.0001
0.0002
0.0001
O.C020
0.001S
0.0006
0.0002
0.0007
0.0003
0.0001
0.0000
0.0000
-------
Software Version: 4.0<1C2?>
^£-e: 4/23/56 08:59 PM
r-ar.nle Name :
:••*-'& File :
frequence File:
Instrument :
Ext.rsrr. f-rs
I>: \T74\GC5\56DW015.RrtW Date: 47
C:\TC4\GC5\S6DW.SEQ Cycle: 15
GC_5 Rack/'Vial: 0/0 Operator:
3/96 0~
Channel
JLSteger
05
A
FM
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V7A 45 REPORT
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875.
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1266.
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50
50
00
00
50
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16
07
51
to
50
on
50
00
on
93
57
50
00
Height
iuv]
43.75
54.68
35.70
35.19
3/60.03
192.37
20423.76
3299.91
S790.10
5956.94
11.76
S77B.1?
9414.92
260962.23
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1.03**06
111961.42
1965.20
325.44
530.46
5514.01
412.54
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4831.01
448.14
410.35
431. «1
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169.64
216.10
51.11
55.24
761.11
€17.28
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2e-04
0.00
4*-04
2«-04
0.01
0-04
0.19
0.02
0.04
0.05
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0.06
0.07
2.48
o.n
93.36
1.61
O.ffl
0.00
0.00
0.03
0.00
l.S*
0.03
0.01
0.00
0.00
0.00
0.00
0.00
4*-04
3*-04
0.01
0.00
BL *
BB
BV
W
VB
BE
n
BX
EB
BV
VB
Bb
KV
VB
Bb
BB
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•rr
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BV
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3.36
16.12
1.46
4.39
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6.26
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5.21
3.15
6.15
5.30
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2.69
2.86
3.15
3.19
4.98
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3.80
8.48
3.91
3.37
4.00
3.60
4.65
5.04
3.25
4.99
3.26
H«v A
Amount
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
0
0
20
0
0
0
0
0
0
0
0
0
0
0
.0000
.0001
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.0000
.0010
.0001
.0163
.0016
.0043
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.0071
.2436
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.1567
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(ug/mL)
0.0000
0.0001
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0.0000
0.0010
0.0001
0.0183
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0.0043
0.0045
0.0000
0.0055
0.0011
0.2436"
0.0161
9.1561
0.1119
0.0006
0.0001
0.0002
0.10«5
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28.1U13
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0.0005
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0.0001
0.0001
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0.0000
0.0000
0.0005
0.0003
-------
; = -e: 4/23/96 05:01 ?N
rar.pie Name :
I = t = File :
Sequence File:
Instrument :
;sr.ci.e Amount
extract 09
D:\TC4\GC5\SeDW016.RAW Date: 4/23/96 07
C:vTC4\GC5\S6DW.SEQ Cycle: 16 Channel
GC_5 Rack/Vial: 0/0 Operator: JLSteger
: l.COCO Dilution Factor
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PM
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6
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Component Time
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0
0
0
1
1
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.79
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6C-04
2*-04
0.00
0.01
0.01
0.20
0.04
0.06
0.05
0.00
0.06
0.06
2.64
0.18
93.54
1.35
0.00
0.03
0.00
1.67
0.03
0.01
0.00
0.00
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15.52
2.58
20.84
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6.85
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5.09
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6.44
6.54
4.91
6.12
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6.69
4.09
4.60
5.12
3.98
2.61
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3.29
3.74
4.59
lUv Ad]. Ant.
Amount (ug/mL)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
29
0
0
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0
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0
0
0
0
0
0
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.0007
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0.0001
0.0000
0.0001
0.0012
0.0006
0.0200
0.0040
0.0060
0.0053
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0.0056
0.0058
0.2604
0.0173
9.2335
0.1328
0.0002
0.7622
0.0003
29.6998
0.0029
0.0005
0.0003
0.0002
0.0001
0.0001
0.0001
0.0002
0.0000
0.0000
0.0007
0.0003
0.0000
O.OOC2
-------
Date: 4/23/96 0"7:44 PM
C:\TC4\GC5\5tDW.5EQ Cycle: 17 Channel : A
G~_5 Rack/Vial: 0/0 Operator: JLSteger
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Time [min]
WA 45 REPORT
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1
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7
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11
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3.434
3.638
3.142
5.064
5.572
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5.879
5.980
6.209
6.410
6.607
6.835
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7.258
7.464
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8.011
8.333
8.453
8.601
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6.973
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3025
143«6i
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28534
324
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110630
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1.55
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4.60
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Amount lug/ml)
0
C
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
0
0
0
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0
0
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0
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0
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.0041
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.2499
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.7627
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.2605
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.000:
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.0000
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.0000
.0000
0.0001
0.9000
0.0000
0.0010
0.0004
0.0206
0.0007
0.0010
0.0045
0.0041
0.0000
0.0115
0.2499
0.0158
9.1S93
0.1569
0.0009
0.0002
0.0002
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0.7627
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O.OOC3
0.0003
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0.0000
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0.0003
0.0000
0.0000
-------
--"--ftware Version: 4.3
:-a-e: 4/23/96
farr.ple Na.T.e :
i 2~a File :
"equs.nce File:
Ir.strumerit :
•i.-T^ie Amount
09:3? PM
Ex-race c9
D:'*TC4\GC5\5£Iv7018.RAW Date: 4/13/96 06:04 PM
C:vTC4\GC5\S£DW.SEQ Cycle: IS Channel : A
GC_5 Rack'Vial: 0/0 Operator: JLSteger
T l.OCOC Dilution Factor : l.GC
to «fif»»O-^
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0
0
1
1
1
2
2
2
2
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3
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5
5
5
5
6
(
6
6
7
7
7
7
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8
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9
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164067
22491
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230
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1904649
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66410240
1069478
1200
1389
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22960
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3550791
24266
1696
2122
2339
7889
197
1274
1355
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13333
2994
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2.59
0.16
90.36
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0.0000
0.0001
0.0010
0.0005
0.0234
0.0032
0.0054
0.0051
0.0000
0.0017
0.2721
0.0171
9.4872
0.1528
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0.7692
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91.5614
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0.0002
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0.0003
0.0011
0.0000
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0.0002
0.0004
0.0001
0.0019
0.0004
0.0015
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0.0010
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0.0234
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0.0054
0.0051
0.0000
0.0017
0.2721
0.0171
9.4872
0.1528
0.0002
0.0002
0.0002
0.7692
0.0003
91.5614
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0.0003
0.0011
0.0000
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0.0001
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Time [min]
I M I M M
14
WA 45 REPORT
tit Component
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1
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Aaount lug/ml)
0
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0
0
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0.0043
0.0056
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0.0064
0.3129
0.0124
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0.1598
0.0001
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0.7224
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97.6620
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0.0004
0.0011
0.0000
0.0003
0.0003
0.0004
0.0002
0.0001
0.0001
0.0003
0.0007
-------
:-?.ie: 4'23/96
Fs.T.pie Name
"^a t a Fi 1 e
? e ~* u e n c e File:
09:26 FM
Extract ~o
D:\TC4y3r5\SfDK02C'.RAW Date: 4/23/96 08:43 PM
r
-------
5c.fr~=re Version: 4.0<1C2S>
I-ste; 4/23/96
Ssr^le Name :
2/51i File :
Sequence File:
Instrument :
fs:?rle Amount
09:16 PM
C:\TC4\GC5\S6DW021.RAW Date: 4/23/96 09:03 PM
C:\TC4\GC5\S6DW.SEQ Cycle: 21 Channel : A
GC 5 Rack/Vial:. 0/0 Operator: JLSteger
Dilution Factor : 1.00
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0 2 4 6 8 10 12 14
Time (min]
WA 45 REPORT
ttr component
1
^
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4
5
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7
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9
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3
4
5
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1
;
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;
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0.642
0.769
1.191
1.285
1.500
1.735
1.851
1.996
2.294
2.436
2.673
3.026
3.402
3.567
3.758
S.007
5.727
6.085
C.S36
7.175
7.600
7.700
.315
.538
.672
.1)9''
.135
.436
9.509
9.855
10.154
10.658
11.184
11.779
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(19.
985.
363.
8722.
225.
644.
3707.
33340.
39529.
382.
73547.
1*37094.
17691'..
65048248.
999076.
764.
1112029.
2332794.
1953.
977.
S437.
981.
727.
774.
1011.
•69.
364.
16S6.
389.
11716.
5115.
2S19.
4952.
50
61
35
04
00
00
00
00
70
60
00
00
26
24
00
00
00
00
00
00
00
00
19
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95
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75
71
29
00
00
10
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49.
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65.
219.
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6146.
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92.
7509.
298372.
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1.05**
146409.
396.
274624.
579(67.
268.
17
70
34
90
21
51
33
73
40
79
59
85
86
70
06
98
86
93
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482.
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87
59
33
43
13
91
23
68
73
44
40
• 6
63
Arc*
2C-04
0.00
0.00
S*-04
0.01
3*-04
9*-04
0.01
0.05
0.05
S*-04
0.10
2.S4
0.24
• 9.83
1.38
0.00
2. SO
3.22
0.00
0.00
0.01
0.00
0.00
0.00
0.00
0.00
S*-04
0.00
S*-04
0.02
0.01
0.00
0.01
BL A
BB
BV
W
VB
Bt
D
BB
BB
BV
vz
BB
BB
BV
VB
•BT
•TT
BB
BB
BB
BV
VB
BB
BV
W
W
w
VB
BV
VB
BB
BB
BB
BB
BB
rtt/Beight
Is)
2.42
9.91
19.57
7.26
2.45
3.43
2.94
1.90
4.94
S.72
4.63
9.79
C.16
2.74
C2.06
6.82
1.92
6.60
4.02
7.28
1*»1S
3.48
11.33
3.61
10.65
7.17
3.40
4.04
6.38
1.51
3.18
10.60
7.12
11.47
Mw Ad). Amt.
Aanunt (u9/mL)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
M
M
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0000
.0001
.0001
.0001
.0012
.0000
.0001
.0005
.0046
.0056
.0001
.0105
.2624
.0253
.2926
.1427
.0001
.7089
.1539
.0003
.0001
.0006
.0001
.0001
.0001
.0001
.0001
.0001
.0002
.0001
.0017
.0007
.0004
.0007
0.0000
0.0001
0.0001
0.0001
0.0012
0.0000
0.0001
0.0005
0.0046
0.0056
o.ooni
0.0105
0.2624
0.0253
9.2926
0.1427
0.0001
CO. 7089
60.1539
0.0003
0.0001
0.0006
0.0001
0.0001
O.OOC1
0.0001
0.0001
0.0001
0.0002
0.0001
0.0017
0.0007
0.0004
0.0007
-------
£-,ftware Version: -!.0
2te: 4/23/95
=rr.ple Name :
sta File :
rquence File:
•.3trument :
i-ide Amount
09:35 PM
/«» fpt* Oc
C:\TC4\GC5\55DW022.FAW Date: 4/23/?c 09:22 FM
C:\TC4\GC5\S6DW.SEQ Cycle: 22 Chanr.sl : A
GC_5 Rack/Vial: O'O Operator: JLSte-ger
: 1.0000 liiution F=:tor : 1.00
«o-=
40—=
20-=
(O r» in p*. . o >~>* »» cr>
O — — — r»i CNfM (N rsi
II I I II II I I I II
A^JVUH
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2
2
2
2
3
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3
3
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5
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Propiorutrilt i
7
7
7
8
8
9
9
9
10
10
11
11
11
12
12
.64:
.730
.513
.760
.974
.014
.096
.296
.465
.697
.988
.063
.400
.6i:
.825
.010
.530
.113
.560
.212
.633
.724
.560
.919
.155
.44?
.5:3
.177
.668
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.71:
.so:
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.369
Art*
lllV-S)
135
(05
7887
102
558
5361
3746
29527
36128
342
42176
34583
1627937
157594
S3912721
1273432
5485
1622203
2086E55
1483
670
4589
456
188
603
107«
• 29
10444
10110
552
1496
1080
429
114
.00
.00
.50
.50
.00
.95
.21
.63
.21
.00
.77
.23
.50
.00
.00
.00
.00
.00
.00
.25
.25
.50
.50
.50
^f
.«5
.80
.52
.48
.00
.69
.31
.25
.75
Blight
(pV)
56.
74.
3111.
49.
212.
2480.
«2.
6227.
«50.
79.
5860.
7902.
2M239.
55765.
l.OCt*
184021.
2192.
258913.
528(46.
219.
0.
1398.
167.
73.
229.
186.
223.
3138.
669.
213.
183.
254.
76.
42.
07
49
17
74
44
36
29
28
19
• 8
95
66
19
52
06
94
30
95
78
14
00
09
30
6S
11
7;
62
51
47
30
63
83
29
27
Arta
m
2*-04
9«-04
0.01
1«-04
84-04
0.01
0.01
0.04
0.05
5*-04
0.06
0.05
2.30
0.22
90.17
1.80
0.01
2.29
2.94
0.00
9«-04
0.01
«*-04
3<-04
0.00
0.00
0.00
0.01
0.01
8»-04
0.00
0.00
6*-04
2t-04
1L Xrti/Bci^nt
[31
BB
SB
SB
Bl
BB
BV
w
w
VI
BI
BV
VB
BB
11
•BT
TT
TT
BB
BI
BV
VB
BI
BB
BB
BV
W
VB
BV
VB
as
BV
VB
BV
VB
2.41
8.12
2.54
:.oe
2.63
2.16
S.<6
4.74
5.43
4.28
7.20
4.38
(.07
2.83
(0.34
6.92
2.50
6.27
3.95
5.12
-----
3.28
2.72
2.5e
:.si
S.7»
3.71
3.13
15.10
2.59
8.15
4.24
5.63
2.71
HJV *S]. Ant.
Amount (ug/BL)
0
0
0
0
0
0
.0000
.0001
.0011
.0000
.0001
.0008
0.0005
0
0
0
0
0
0
0
9
0
0
54
S3
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0042
.0052
.0000
.0060
.0049
.2326
.0225
.1304
.1813
.0008
.3491
.8069
.0002
.0001
.0007
.0001
.0000
.0001
.000:
.0001
.0015
.0014
.0001
.0002
.0002
.0001
.0000
0.0000
0.0001
0.0011
0.0000
0.0001
0.0008
0.0005
0.0042
0.0052
0.0000
0.0060
0.0049
0.2326
0.0225
9.1304
0.1819
0.0008
54.3491
53.8069
0.0002
0.0001
0.0007
0.0001
0.0000
0.0001
o.ooo:
0.0001
0.0015
0.0014
0.0001
0.0002
0.0002
0.0001
0.0000
-------
Software Version: 4.0<1C29>
I=te: 4/23/96 09:55,PM
S=r.p-le Name
I-ata File :
Sequence File;
Instrument :
Ssrr.cie Amount
C:\TC4\GC5\S6DW023.RAW Date: 4/23/96 09:42 PM
C:\TC4\GC5\S6DW.SEn Cycle: 23 Channel : A
GC_5 Rack/Vial: 0/0 "Operator: JLSteger
: l.OODO Dilution Factor : 1.00
n ^
- 100 •»•»/•»
CO • ' '• —' «N «NP>icN to
II I II II II II I I _L I
20-E
*^ ^ ^Tf^ ^3 *f* 4^5*O^
rvO'»>r'- O ^ICCC
in IM \ I i
flVXV
10 o u*i ^ r* GOO
p inr». — *. —^
ih iriui to' ic fv.'r>."
Ill III
co f^r^o1 ^' o co *o
(O Is- «•• OOOO W ••- ^ r^
°\~. T •? O OO— ~"-
BE
BE
•BT
•TT
•TT
•TT
•TT
•TT
•TT
•TT
BS
BE
BV
VB
BE
BV
W
w
w
VB
9.14
2.67
16.61
11.64
6.33
3.15
7.42
4.17
3.33
5.99
5.36
5.52
5.31
9.34
6.13
2.60
59.20
7.07
2.12
3.42
1
1
.78
.50
.51
.65
.15
.72
.00
.32
.30
.16
.00
.43
.69
.42
KJV Ad]. Amt.
Amount (uj/nL)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0001
.0000
.0002
.0001
.0001
.0014
.0002
.0003
.0012
.0006
.0050
.0054
.0001
.0100
.2404
.0231
9.2466
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.1426
.0009
.0002
.7663
.0001
.0001
.0001
.0000
.0001
.0001
.0002
.0001
.0019
.0015
.0005
.0005
.0002
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
9.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0001
0000
0002
0001
0001
0014
0002
0003
0012
0006
0050
0054
0001
0100
2404
0231
2468
1426
0009
0002
7683
0001
0001
0001
0000
0001
0001
0002
0001
0019
0015
0005
0005
0002
-------
cftware Version: 4.0<1C2?>
:=te: 4/23/96 10:15 PM
5=T.pl e Name
i 1
Sequence File:
Ir.5trurr.erit :
Sannie Amount
C:\TC4\GC5\ScDWQ24.RAW Date: 4/23/96 10:02 PM
C:\TC4\GC5\S5DW.SEQ Cycle: 24 Channel : A
GC_5 Rack/Vial: 0/0 Operator: JLSteger
JL . '-/ • J « •„•
Dilution Factor
1.00
OO WCN-^C— Q C»*">T
r<» f» p "o» i*.. p •» icc
irii/S (0 to
III I
ineo oo O tN
°? d
II
I I II i I
do— — •
— — •- —
III II
I I I
I I I I I I"
n rnn IT
i i M ; | M M | i i i i i M i i i i i i i T i i i i i i i i i i T i i ri M pirni
2 4 6 8 10 12
Time [min]
14
WA 45 REPORT
at
Component Tune
Name (nun]
0
0
1
1
1
1
1
2
2
2
2
2
2
3
3
3
3
5
5
5
A;*toru'cil* 6
6
7
7
8
9
4
•3
q
10
10
10
11
11
.64:
.731
.19?
.336
.519
.763
.882
.021
.109
.307
.476
.712
.997
.081
.415
.627
.142
.050
.513
.76£
.Hi
.730
.225
.418
.94?
.192
.491
.5£~
.904
.206
.700
.985
.117
.742
Area
(pv-sj
154
204
260
208
8733
962
1997
7738
5726
34042
36412
402
44423
31482
1615994
156343
63884058
1027723
5432
1423
22629
622
4924
596
240
655
755
1189
405
11951
6256
1297
536
• 86
.50
.00
.00
.40
.00
.00
.08
.93
.20
.80
.60
.00
.50
.50
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.00
.50
.91
.09
.00
.00
.82
.18
.00
.20
Height
IWV]
59.27
40.46
29.02
23.35
3452.76
156.59
465.71
2559.86
964.35
6384.57
6770.76
75.05
6315.68
7052.68
251570.11
54372.20
1.07«»06
145528.11
2095.46
394.18
5902.74
126.49
421.99
122.81
78.60
169.08
152.62
274.56
47.41
3853.09
527.51
216.45
83.36
131.37
Area
(»]
2«-04
3«-04
4e-04
3*-04
0.01
0.00
0.00
0.01
0.01
0.05
0.05
C*-04
0.07
0.05
2.41
0.23
»5.47
1.54
0.01
0.00
0.03
»*-04
0.01
9»-04
4e-04
le-03
0.00
0.00
6e-04
0.02
0.01
0.00
8e-04
0.00
BL Area/Height
Is]
BB 2.61
BB 5.04
BB 8.96
BV 8.92
VI 2.53
BV . 6.14
W 4.29
W 3.02
W 5.94
W 5.33
VB 5.38
BB 5.36
BV 7.03
VB 4.46
BB 6.13
BB 2.88
•BT 59.63
TT 7.06
•TT
TT
•TT
•TT
•TT 1
•TT
BB
BB
BV
VB
BB
BB
BV 1
W
VB
BV
.59
.61
.83
.93
.67
.85
.05
.88
.95
.33
.54
.10
.86
.99
.43
.75
Rav Adj. Amt.
Amount (ug/mL)
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
9.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0000
0000
0000
0000
0012
0001
0003
0011
0008
0049
0052
0001
0063
0045
2309
0222
1263
1468
0008
0002
7581
0001
0007
0001
0000
0001
0001
0002
0001
0017
0009
0002
0001
0001
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
9
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.0000
.0000
.0000
.0000
.0012
.0001
.0003
.0011
.0008
.0049
.0052
.0001
.0063
.0045
.2309
.0223
.1263
.1468
.0008
.0002
.7581
.0001
.0007
.0001
.0000
.0001
.0001
.0002
.0001
.0017
.0009
0.0002
0
0
.0001
.0001
-------
APPENDIX D-l
Sampling Equipment
Calibration
-------
S-Type Pitot Tube
Inspection Data Sheet
Company Name.
J 1
**r~ M
8BT 0BM>>>TV>inQ tt|
.
Pre-sample
-f6
Post-sample
Date
lies
i
M
IJO'
•Z*
-L°
1°
1°
1°
1°
.1*
,Z65
,v&
ftfl
.ofr
.oft.
^
Lsvet?
Obstructions?
Damaged?
•10* < o, < 10*
•10'O>
~, c>
£-
1*
1"
("
O
1
0
.1^
>U3
.~z-£$
'1ft
.£>'*•
.0 It,
^
Comments:
Pitot tub«/prob« number mtsts or txesedt »K specifications crhsris and/or applicabl* design
features and is hereby assigned a phot tube calibration factor of 0.84.
Signature
-------
NOZZLE CALIBRATION SHEET
Plant
-------
mnunrrs
CFA MTrOOft 5
Mater tax Pre-Teet Calibration
Cm 11 eh Meter Ooc end Cnallah Calibration Mater
riu
••rial
S11
S111I7
tote: -
Calibration Mttor Pactor Tc:
-> tf.TO (In. N)
•> 1.00Z3 (nuefeer)
TaBporatire
Inlet Outlet
(da* n
NT MS Hrm tUOIK
•laacwd «*lw Veluee Voluet .
..eft Ttae Initial Plnel . Tetel
(In BO) (Bin) (eu ft) (CM ft) (cu ft)
S.OO S.SO M0.7M W7.M9 «.H3 >lnltlal-> 12.0 «0
; \Plml — > 111.0 fl
s.oo a. oo fcr.Mv tooo.tn U.TU. i'initi«t-> tot.o «
CALIHAT101 «m KAOIKI CALIHUTIOI
t.OO §.00 1000.411 1006.O1
4» ' lnltl«t>» 102.0 f
'• Vi«i— > lof.o 100.
1.00 12.00 10M.C1 1013.MO 7.M»* .lnltt«l-» 101.0 WC
.Plml — > 101.0 102.
0.50 21.00 1013.090 1022.774 l.tK iln1tl»t-> 101.0 102.
.riiwl — > tOi.O IOC.
Initial Plml fM*l Inlet Outlet
(cu ft) (CM ft) CCM ft) (eke P>
7A7JM m.OiV A.S29 . 73.5 73.5
773.M* 7B.H9 ll.fTO 74.0 74.0
•
7*5 .Olf 791.107 S.9OO r-7*.0 74.0
7ti.oo7 TMJB «.S4i n.o n.o
7N.SS5 006.5*1 0.224 74.0 74.0
otr CAS
•CTO CALIOUTIOlrACTQK
T~
V»U» Varlatl
Oil Fid CU.IHATI01
•
V»lw VwUttcn
(In CO) (In B20)
.900 -0.001
.904 0.003
,900 -0.001
.982 0.001
•0.001
1.
1.9B
i.iu
1.750
0.072
0.053
0.059
•-O.OM
•0.123
•
Mete: Per Cellbratlen Pactor Y, the retle ef the ro«dln| ef the calibration avtor to tiM aVy fee «eter,
acceptable telerence ef IndMduel valuas fra» the avereee la *-0.02.
Per Orifice Calibration foeter dm, th« erlflew dlfferentlel ereeeure In tnchet ef 020 thet eqjetet te 0.75 ef» ef al>
at M r and 29.92 lnch« ef Ml. eeeeptable trterante ef Indlvlduel valuee frea the awerete la »-0.2.
I certify thet the efceve Dry Oee Meter MS e»tibr»t«d In accordance «rfth I.Pa. Methed 5 . eerHrai* 7.1 ;Cf« 40 Part 40,
the Preelaten Met Teet Meter • ttAI*. Mhlck I* tim MM calibrated Mini the Aeerlcan fell Prever I J7B5.
la treceeMe te the letleml »reeu ef Standards (l.l.f.T.).
*M
certificate
Signature
9 MOT, i*Id)
MturejL
Oate
-------
37
EWl MR03D S
Meter tat Jre-Teet Calibration
Engl*.si Miter to*, and English Calibration Meter units
Fill
F:\PATAHLr\CALIBRAT\CALJ
511
Serial
107V
Date:
BarcMtrle treasure:
Calibration Meter Factor Te:
•>7/1/96
•> 29.42 (in. Mg)
•> 1.0023 (rufeorl
err CAS METEI MAC KG
Heaped Voluw VolUBt VeluBt
a* Tis» Initial final Total
(In 825) UifO (cu ft) (eu ft) (eu ft)
•AS CAUfcUTlOt MFTH RIADIIBS CALIBRATION NETEI
Teeperature VolUB* Voluae VolUBt . Teeperetur*
Inltt Out lot • Initial Html Total lalot Outlot
r) (dot F) (cu ft) (cu ft) (cu ft) ' (dos P) (d* P)
5 JO
3.00
2.00
1.00
0.50
4.00
4.00
7 JO
11.00
19 JO
192.880
200.428
206.44*
212.577
233.723
200.428
>
206.44*
212.577
218.90*
2*1.883
7.548
4.036
4.113
4.327
0.140
Inltlal->
Fiml— >
Initials
Fiml — >
lnltlal->
Fiml— >
Initial-*
Fiml — >
Initial-*
Fiml— >
92.
102.
100.
105.
103.
10*.
100.
96.
95.
99. (
90.
90.
90.
91.
fl.
92.
92.
91.
91.
) 91.
1M.47S 20.792 7.317
203.792 209.611 5.819
209.611 215.470 5.859
215.470 221.481 4.011
235.5*1 2(3.2*1 7.723
79.0 79.0
79.0 79.0
79.0 79.0
79.0 79.0
79.0 80.0
MT 6AS METE*
METER CA11UAT10H FACTOR
T
Volut Variation
(ruter) (ruter)
0.966 0.003
0.990 0.007
0.989 0.006
0.978 -0.005
0.973 -0.010
Avorafl* 0.983
MT CAS METER
ORIFICE CALIBRATION FACTC
d»
Valuo Variation
(In 120) (in 120)
1.192 0.052
1.793 : -0.0*6
1.139 0.000
1.179 0.040
1.79* -0.0*6
Awrae* 1.O9
•etc: For Calibration Factor T. tfco ratio of ttw roadini of tho catlbratlon Mtor to tte dry fas aotor/
(t toloraneo of Inrflvidal valuo* fro> tfco av«ra>t la »-0.02.
For Orifico Calibration Factor dK3, the or If let differential pretsuro In ineho* «f 120 that oquotn to 0.75 cfa of ai
•t M t ** W-W Incho* of N. acetptablo toloranct of Individual valutc froo th* ovorao* Is »-0.2.
I certify ttut tM abovt Dry «as Meter HOS calibrated in accordance with C.».A. Method S , parejraph 7.1 ;CFt *0 Part 60.
using the Frecision Wet Test Meter # 11AE6, t^lch in turn MM calibrated using the American 8ell F-rover ff 3785,
certificate • '107, irfilch Is traceable to the Motional ftureau of Standards (N.I.S.T.).
ftate
-------
AW llfrftUKNTI
|»A tCTNOO S
Meter 8ex Fro-TMt Calibration
fnflllah Meter 8ox and English Calibration Item Units
nil
ferial
r:
ri
Pt \9ATAF t LIVCAL !UAnCALJCNU.ftSr\P9l.nCL .5f \A-U.W1
S11
itt:
A-38
itrle FrMsure:
Calibration Meter Factor Te:
-»4/27/9«
•> 29.80 (In. 8f>
•> 1.0023 (mater)
MY MS MCTEI ttADIM
llaaoad Voluae Voluae Veluae
aft TIM Initial Final Taut
Cin aft; tain; lew to ecu to ecu ft)
MS CALIUATIOH MITtI 8EADIMCS CALIUUTIOSJ NTTO.
Teaperature Voluae Value* Value* Teaporaturo
Inlat Outlet Initial Final Tatal Inlat Outlet
(OB* '
1.00 4.00 JC.in J90.747 7j|M Initial-* *.
Final—> 101.
1.00 t.OO 190.767 39S.4S2 7.M5 Initial-* fS.
Final—* 102.
2.00 t.OO 398.452 405.424 7.174 Initial-* 99.
final—* 103.
1.00 ».00 405.tot 422.092 U.4M Initial-* 101.
final—* 103.
0.50 14.00 422.092 432.006 f.914 Initial-* 101.
final—* 101.
•7.0*
Ccu ft) (cw ft) (cu ft) (del F) (de« F)
44.492 73.950 7.258 81.0 81.0
73.950 »1.457 7.507
•1.457 88.439 4.982
•.439 104.389 15.950
•9.8
90.0
90.0
91.0
91.0 104.389 113.948 9.559
93.0
•1.0. 81.0
•1.0 81.0
81.0 81.0
•1.0 81.0
»'*--
Avaraa*
MT 8AS IKTO
METU CAtlBUTIOB FACTO*
t
Value Vwlatlen
(rua>r} (mater)
0.990 ••.003
•.993 8.000
0.994 8.002
0.994 •.002
0.993 -8.001
0.994
OtT MS MTT0
Oil FlCt CAUttATION FACTOi
Value
(In 820)
.941
.929
.874
.735
,770
Avara>i 1.850
Variation
(In 820)
•.092
•.079
•.025
-0.115
-0.080
•atat Far Call brat I an Faetar T, tfce ratle af the reading af tl»a eallkratlan aeter ta tha aVy faa aeter, ^
'" accaptable telarance af individual wlua* fra* the avvrate la +-0.02.
Hr Or I flee Calibration Faetar aM, tka arlflee differential praaaure In IneKaa »f 820 that aquataa ta 0.75 eta af
at 48 F anl 29.92 Incnee af N. •eeaptable tolerance af Individual values froa the avarata Is *-0.2.
f certify that the above Dry CM Meter MM calibrated in accordance tilth |.».A. Method 5 . aaraaraeh 7.1 ;CFI 40 »art 4
Uilnf tha Fraclaton Wat Taat Meter $ ItAfe, ah I eh in turn MM calibrated ualnf the Aaarican tell Frovar f 3785.
Ctrtlflcate f F107, Mhlch la traceable ta the tatlanal 8uraau af Standards (I.I.S.T.).
8lanature
•ate
-------
APEX INSTRUMENTS
t>A METHOD 5
Meter Box Pre-Test Calibration
Engliah Meter Box and English Calibration Meter Itolts
Pliant**: P:\DATAnLE\CALimT\CALjeNU.W\DW_PttL.5P\A-39.UK1
Serial
r:
r:
511
A-39
•ate:
BaroMtric Proooure:
Calibration Htttr Factor Te:
•>7/1/96
•> 29.62 (in.
•> 1.0023 (
MT 6AS METER BEADING
Elasped Voluo* Veluat Volute
•ft Tl0»
Initial final Total
CAS CALIWATIOH NETEt lEADtHKS CALIMATIOM NETEI
Tovpcraturt VolUH Volu» VoluH Ta^traturt
Inltt Outlet Initial Final Total Inlot Out lit
(in CO) (Bin) 103.
3.00 7.00 110.702 187.758 7.056 Initials 101.
Piml—> 110.
2.00 12.50 187.758 196.23* 10.476 lnltial» 105.
Final—> 107.
1.00 19.00 196.234 209.524 11.290 tafttal-> 102.
Hml—> 105.
0.50 U.OO 227.695 235.253 7.558 lfrit1al-> 76.
> fl.
P) (dog P) (cu ft) (cu ft) (cu ft) (do*. P) (dtg f>
246.169 252.410 6.241 ' S1.0 (1.0
264.419 271.246 6.827 81.0 81 .0
271.246 281.317 10.071 81.0 81.0
281.317 292.130 10.813 81.0 81.0
303.100 310.S59 7.459 82.0 82.0
83
85
89
fl.
fl.
f2.
f2.
fS.
76.
79.
OtT CM NETEX
METE* CALIWATIO* PACTOR
T
Valut Variation
(rutfwr) (rubcr)
0.966 -0.002
0.992 0.004
0.990 0.002
0.968 -0.001
0.983 -0.003
OtT CM METER
01IFICC CALIHUTIOM PACTOR
elta
Valut Variation
(in CO) (in 120)
Average 0.968
.839
.788
.742
.742
.695
1.761
0.078
0.027
-0.019
-0.019
-0.066
•ott: Por Calibration factor T. tfca ratio of dM reading of tfc* calibration avttr to tti* dry fas aetar.
•ccoptabla toltranct of Individual wiluM froa tka av»ra|i la *-0.02.
Por Ortftet Calibration factor dM, tfca •riftct dlfferantial prmsurt In inch** of 820 that equates to 0.75 cfo of •
•t 68 P ond 29.92 inches of N. occoptable tolerance of individual values fro» the overaoe ia «-0.2.
I certify that the above Dry 6as Meter MM calibrated in accordance with E.P.A. Method 5 . paragraph 7.1 ;CPR 40 »art 60.
using the Precision Wet Test Meter f 11AE6, Mhicti In turn MBS calibrated using the American Bell Proven t 3785,
certificate 9 P107, whifl^ls traceable to the Motional Bureau of Standards (N.I.S.T.). .
Signature
Oate
-------
APEX INSTRUMENTS
ErA METHOD 5
Mtter lex Pre-Test Calibration
English Meter lex and English Calibration Meter Untt*
•octal MuBber:
••rial NuBber:
r I \DAT AFILEXCA1.1UATXCALJC MU .DSTNKM.MCL .»\20120. WC1
522
20120
Data:
•irneatrlc Proasure:
Calibration Mater factor Tc:
•>7/1/96
•> 29.62 (in. Ml)
•> 1.0023 (nuober)
ORT GAS METER 8EAOIHC
Clasped Voluat Volue* Voluae
oft
(in K20)
5.00
3.00
2.00
1.00
0.50
Tioc
(•in)
7.00
10.00
11.00
13.00
15.00
Initial
(cu ft)
765.875
774.712
784.661
793.810
811.074
Final
(cu ft)
774.712
784.661
793.810
801.411
817.339
Total
(cu ft)
•.837_
>
9.949
9.149
7.601
6.265
ln!tlal->
Final— >
lnltial«>
Final— >
Initials
Final— >
ln!ttal*>
Final— >
Initial^
Final— >
CAS
Taoperature
Inlet Outlet
(deg F) (deg F)
84.0 79.0
95.0 82.0
95.
94.
88.
103.
91.
93.
82.0
84.0
84.0
•6.0
87.0
•8.0
91.0 89.0
101.0 89.0
CALIBRATION NETU
VolUB* VoluB*
Initial Final
(eu ft) (cu ft)
121.419 150.101
150.101 159.805
159.805 148.660
148.660 156.001
165.504 171.541
REAP INGS
Voluoe
Total
(eu ft)
•.682
9.704
8.855
7.541
6.037
CALIBRATION METER
Teaperature
Inlet Outlet
(deg F) (deg F)
t
78.0 78.0
78.0 78.0
78.0 78.0
78.0 78.0
78.0 78.0
Awraat
MT 6AS NETU
METU CALIBRATION FACTOR
T
Value Variation
0.985 -0.003
0.990 0.002
0.987 -0.001
0.987 -0.001
0.991 0.003
0.98*
OtT 6AS METER
WIFICE CALIKRATION FACTOR
Value Variation
(in H20) (in H20)
.854
.809
.746
.766
.754
1.782
0.072
0.027
-0.036
-0.016
-0.048
•etc: For Calibration Factor T. CM ratio of tiw raodinj of the calibration oxter to the dry •** Meter.
acceptable tolerance of individual value* frea ttw overeat ia +-C.02.
For Orifice Calibration Factor oM, the orifice differential pressure in inches of 820 that equates to 0.75 efo of ,
•t 68 F and 29.92 inches of a*, acceptable tolerance of individual values fro* the overage ia +-0.2.
1 certify that the above Dry Cas Meter Mas calibrated in accordance with E.'.A. Method 5 , paragraph 7.1 ;CFR 40 Part 60
using the Precision Wet Test Meter ff 11AE6, Mhich in turn Mt calibrated using th« Aoerican 8ell Prover 0 3785,
certificate f F107, Mhich/is traceable to tht Rational Bureau of Standards (N.I.S.T.).
Signature
Oate
~ /'
-------
APPENDIX D-2
Sampling Train Data
-------
FIELD DATA
P*g*tof
i_^
Pbnt
Oat*
temping locator*
SimpteTyp*
Run Number
Operator
Ambtent Temperature (T)
Baromeklc Prettu- • (In)
Strife PreMure (In H2O)
tf**tr
£ / f T
Prob« Ungtft end Typ«
Mate AH®
Yd
KFtetar
Box 3«Mno (T)
InMLMikChwk
**
IS
HrigMofloeafonpl)
DuclOlmvmlona (In)
AvtumMl Motolur* (%)
02 W
C02(%)
OZ^COZ M*t»d
Final LMk Ch«:k
«n4 Record MDMa Every
T
* *
Diagram of Duct
**«
0 Samplng
Tim*
(m»n)
Clock
Tim*
Vrti
VclocRy
AP
(lr»H20)
OrMc*
DlfterwiW
AH(biH20)
Oat
IpCf S
rn
T«np«ra
-------
FIELD DATA
Pagatof
WT
Pknt
Date
Samplng Locaton
8ampteTyp«
Hun NuMiuar
Operator
Ambient lamparatura (T)
Daromatb Piaaawa (In)
State PraMur* (In H2O)
.L5
ProbaLangtiandTypa
Nouto ID (In.)
MatarAH®
Yd
. //
Prob«HMrtv S^tng (T)
\\tfHm Box S^tng (T)
nraM |.Mm CrMCK
r5*
fr*r?
0
IW||lil of Locafco (fl)
DuctDlm«nrioni (In)
FVtac NumiMr
AMunwd Motahv* (%)
02 (%)
C02(%)
MoMur«Cofl«ctod(g)
FVwUjMkCtwck
ft>
0 00 £>
tt>"
RMMlmd record All 0»ta
($"
MlnulM
Diagram of Duct
(mtn)
dock
Tfciw
Vm (IF)
Velocity
AP
0nH2O)
OrHIc*
f^Mwr*
DMwcnM
Flu*
T«np«ralur*
rn
Twnpcralura
rn
Twnpcwlur*
(T)
Dn/QMHMw
T«np«r«(ura
OuM
ExM
Pump
Vacuum
(h.Ho)
to
m
M
5*
27?
-7?
/5
£7/1
<£>
-5
-------
FIELD DATA
\ Pap* lot
Ptent
SampbTypa
Run Number
Operator
Ambient Temperature (T)
Bwomevlc Pressure (In)
Static Preeture (In H2O)
Probe langti and Type
Yd
K Factor
HMt« BOM S^lno (T)
InM LMk Ctwck
Height of Locatton (fl)
DuctDlmeneli
i (In)
FNtarNumbw
Aciumwl Moltlur* (%)
02(%)
CO2(%)
Mohh** Cofl*ctod (g)
Final LMk Chwrk
Z07*
657
/-c
Raad and RaocrdAH Date Ev«rv /C>
Dtagram el Duel
-------
«••»••• Vi«l
HbLU UAIA
t-
Plant
Onto
QampbTyp*
Hun rfUffnMT
Operator
Bvonwfrfc Pr«Mirc (In)
State Prattur* (In H2O)
Nan* 10 0".)
K Actor
Pfot»H««t«r 8*MhQ (T)
H«it«r
fF)
InMlMkCrwck
'*'*/,< 4
Height of Loc««on(fl)
OuctDlmwwtorwl
AMUm«d MoMur* (%)
02 (%)
02/C02 HMhod
MoMur*Coltactod(o)
5:5" a
Tim*
(mini
0
Cteck
Tim*
(24-rtl
OMMtotar
-
KimQ
on
dAHDrtiEv^rY /O Mfcuitx
Veloclly | OrHte*
AP
0hH20)
AH(krtH2O)
nu*
rn
T«mp«r«tur«
rn
fR
DryGMMtotar
Twnpcralur*
rn
OuM
rn
ExM
Pump
Vacuum
to
'
%r
/.otf
'>
ft
5-O
t //
5T&
-------
| Pag* t of
Date
aampfcig Ux*ten
Nonl.lO(ln.)
M«tarBmNumtMr
Run NuniDCf
Opmtor
Ambtont T«mp«alur« (T)
H^gMofLoc««on(»l)
FINwNomb*
02(%)
C02(%)
-------
FIELD DATA
f •
c_l
Phrt
Date
Run Number
Operator
Ambient Temperature fF)
DaromeHc PraMure (In)
StafcPreeeure(lnH2O)
PfolwLMigViandTyp*
Monte K> (In.)
Yd
KF«ctor
lerBoKSefltng (*F)
7£/T
0 •(>£)&+f
Duct Dlmentten* (In)
02 (%)
C02(%)
Final LMkCtwck
f}f,
Read and Record All Data Every ^-) Mlnutee
Sf>
DtagmnofDuet
Number
Tim*
(mlo)
dock
Tim*
IM-W
Vkn
VctocMy
AP
(^H201
OrHIc*
AH(lnH20)
T«mp«r«tur*
Pfob*
TMnpwalur*
Fltar
DryOMlUMw
T«mp«ra(ur«
CMM
ExN
Pump
Vacuum
gnHn)
art
Ifr
6/5
f?g
7-7 V
r
?7^
^z:
Comment*:
.57
-------
I
o
LD
I
1
I
1
<$<*&
I
I"
NV
V5*
^
fc^Js
1
s
E
1
I
I
9
1
1
le
me
fcvK"^^v>t
^•^^^s
N
I
Vr^
s.
xjO
^*
X-
-------
FIELD DATA
Pug* 1 of
M3L
Phrt
Date
Sampla Type
nunNumbar
Operator
Ambtent Tamparalurc fT)
Baromafrfc Praam* • (In)
State Praatur* (In H2O)
<-C
M«tar AH®
Yd
K Factor
(T)
l"*«l twh Clwch
DurtDlmamlona(ln)
FWwMumbw
Aatumad MoMur* (%)
»0
/7"
RaadandRacordAIIDataEvafy/6> Mlnutaa
/*
Diagram of Duct
Tim*
(mln)
JMggy.
Clock
Tim*
-hr)
Vrti
AP
gfiH2O)
OrHte*
DlftaranM
AH(bH20)
Twnpmriur*
DryOMM«tar
OuM
B*
Pump
Vacuum
JH.HB)
/LSI
t'6-CS
x
to
an
-------
FIELD DATA
Pag* tof
Ptont
Date
ottfitpwiQ Loo won
Operator
Ambtont Twnpwalur* (T)
Oaronirtle Pra*tu* (In)
Stofc Pr«Mura (In H2O)
kA-*«f
IT5L
•t,ts'
Yd
K Factor
PVotM HMtar S^flhg (T)
H«rt« BON S^tng (T)
00(1
Duct Dfrnamfam (In)
ntm Numbw
teminwd Motafur* (%)
02(%)
C02(%)
02/COZM^hod
Motofur* Coflwtod (g)
Final L-KCtwck
R»cord Aft Date Evary
Minute*
/-i/,
Dtngniin of Duct
Clock
71m*
w-w
/O/
so
OMMctar
fl-- ,^| i,
rwnn^
Vm (IP)
VclocMy
• • --- •
rfvMl
AP
OrHte*
Pr •*•(*•
AH(lnH20)
Fhw
Gftt
m
Prob*
T«np«ra1ur*
rn
DryOMftfotar
T«mp«ratur*
End
Pump
Vacuum
On.Hfl)
3L£L
o
22
fo'/>.
-------
FIELD DATA
/
OHto
9amptng locaton
Sampfe Typ*
RunNumbw
Operator
Ambtont T«mp«rafc*« (T)
BvonMfrfe ftMtur* (In)
State PtMtur* (In H2O)
Prob* L»nqtfi and Typ»
Noote ID (In.)
MrtwAH®
Yd
KFKtor
(T)
H«rt«r Box StMng (T)
MM L«ik ChKk
*/£>:?
HwgHt of Location (A)
DuclOlnwnslonB(ln)
FKtarNumbv
At.unwd Mohtur* (%)
CO2(%)
02/C02Mt«wd
fTnrt LMk Chwjk
t
7
•r'™^—^ • ~JIMJ_
6001
-------
FIELD DATA
M44S.
Date
Imping I
SamptoTyp*
Run Number
Operator
Ambient Temperature (T)
Baromefrfe Pteenre (In)
Slate Pretture (In H2O)
Probe Unoftar
M«tar Box Numbw
Yd
K Factor
Probe Heat
NM LMk ChKk
^
.1 1
75*
DuclD>men»tone(ln)
Actumwi Motolur* (%)
02(%)
C02(%)
02/C02KtotM>d
Mohtur* Coltoctod (g)
Final tMk Crwck
.&
"
\a 0/£ &f\
Diagram of Duet
Comments:
-------
FIELD DATA
| Pag*«of / i
Phnt
Date
SamptoTyp*
^Z"
RunNunb«r
Operator
Ambtont Twnpmlw* (T)
Baronwfrlc Pt »MU • (In)
8McPtMtura(lnH2O)
Noal«IO(ln.)
MtotarBoxNumbw
Mrtw AH®
Yd
P»ob»H«rtwS^«ng(T)
H«rt«r Box S^flng (T)
(nMLMkCtwck
-T-7
DuclDlm««lorw(ln)
FRtarNumb*
C02(%)
/5" ^
HMd«ndR»eordAI>PrtiEy«ry //; Mfcmm
Dbor.metDuct
damping
Tfen*
(mln)
dock
Tfen*
124-hr)
GMM*tar
RMKflng
Vm
2s
AP
OrHte*
FhM
Qi*
T«np«r«1ur*
Tcmparalur*
_ r° _
Tcmpwalur*
OuM
EMM
Pump
VlKuum
So
5V
/-//I
^r
l/tJ
7 70
•77
?:
-------
FIELD DATA
Pugalot
Phnl
Data
Samplnq locaten
SamptoTypa
RunNumbar
Operator
Ambtent Tamparatura (*F)
Baromafrlc Ftantra (In)
State Ptaitura (In H2O) /,
•v<
Nonl»IO(ln.)
MatarBoxNumbw
Yd
K Factor
Ftob* HMtar
(T)
HMtcr Box S*«n0 (T)
//? /y
DuctDknamlorM(ln)
Ai«um«d Moltlur* (%)
C02(%)
Mo*t»i,.Cofl*ctod(g)
76
"
/ ?/»
tfcad and Raccrd All Data Evary
Thn*
dock
Thrw
04-hr)
Vm 01*)
AP
flhHXn
OrMc*
Ftattu*
AHftnH20)
FhM
OM
TMnparatur*
Twnpcralur*
Twnparakt*
DryGMMatar
Twnparakva
Exft
Pump
Vacuum
P"."fl)
tf/ti? .
&r
'
&Q
-%T
f.o:
.
74
&l
rift,
/ft,
7,0
Commante:
-------
FIELD DATA
Phnt
Oil*
Samptnp Locator)
tamptoTyp*
RunNumbw
Operator
Ambient Temperature (T)
Barometfe Preeetr* (hi)
Strife Pteeeur*(lnH2O)
PVob«LMig«i«ndTyp«
Nonl. ID (In.)
MM» Bon NumtMT
AH®
Yd
K Factor
fF)
HMttr Box S«Mn0 (T)
X
DuctObnenelonel
C02(%)
Final LMkChwk
.S£±
230.0
< All Pafc Every (O MViute>
MaoramolDwcl
Tlnw
(Mn)
Chick
Tlnw
04-hr)
OMMctar
fl, , •„ ,
MMOwlQ
Vm (IP)
Velocity
AP
(lhH2O)
OrHte*
DMcrenaat
tHtoWOi
FhM
Qa*
>&L
Twnpvnrtura
OryOMlUMw
"^T1
OuM
Pump
Vacuum
0".Hol
tt>
ft '10
m
7*10
7-r
'740
T
74
-------
HhLU IMIA
Pagatol /
Data
9amplng Locatfon
Sflinpto Typa
flufi Nufnoar
Oparatar
AmMant Tamparatura (*F)
BaromaMc Prattua (In)
State Pranura (In H2O)
Non«alD(ln.)
M^arBwcNumbar
Yd
KFaclor
nobaHaatarSaMngrn
MMtMlcChacIc
HrfgMo* located fll)
DuctDlmao«lona(ln)
F«»«Numb«
02(%)
C02(%)
Mohlur* Cofl^tod (9)
r-^T -
-2JL
2/0.
"
Raad.ndRacwd/MIDateEvarv /fc? Mlnulaa
Dl.or.mof Duct
Uma
(mtn)
Clock
TTma
VfW
VatocMy
AP
(lhH2O)
Orlfte*
DNtarwKM
AH(lnM20)
Flua
Twvipw ftluf •
rn
nob*
T«np«ralur«
rn
rn
DryQMMatar
Tamparatura
Hat
rn
Ootat
rn
ExN
m
Pump
Vacuum
_ftLHfll_
*€
TO
.60
S*/
7
t r /
*£
C,
-------
FIELD DATA
page i of
Out*
Sampinqi
C.
Operator
Ambbnt Ttmpmrtira (T)
romefrfe PreMure (hi)
State PreMure (hi H2O)
Monte IP (In.)
M«tar Box Numbw
Yd
KF^ter
Probe Heater 8eMhg (T)
InMLMkCfwck
DuctDhnenttene(ln)
Rl«Numb«
Aetumed MoMure (%)
02(%)
coz(%)
MoWur. Counted (g)
Final L«ili Ch«:lc
34
"
'203,^
d M Data
Every fr>
Minutes
/*t.
"
Digram of Duct
oBfVlfDwlQ
Tkn*
(mln)
Clock
ThiM
(24-hr)
CJ
QMM«tor
AP
OrMc*
f^Mttf*
AH(lnH20)
Fhw
out
TwnfMratur*
rn
Temperature
rn
Fltor
I1pWtt
rn
m
OuM
rn
End
rn
Pump
Vacuum
(In.Hfl)
/5V-7
/CV
76
/5 5" 7
We.
.9-
zr*/
Go
Comments;
-------
UttIM
/ ^ -
tot
Ptant
fete
Samplng locator
Sampte Typa
ftunNumbar
Operator
Ambtent Tamparatura (T)
Baromafrfc Praaaua (In)
State Praatura (In H2O)
/f//V
^7
igftandTypa
Monte ID (In.)
WteterBoKNumbw
Yd
KFacter
Hwilw Box SMtng fF)
NteJ LMh Clwch
*»*tt/'
Baad and Bacord All Date Evary
/.7/..
rtelghto(Loca«on(n)
DuctDtmamlona(h)
FKterNumlMr
Motolur»Coltecte
-------
• •••••••Ttem
HtLU UAIA
| Page I of
Phnt
Onto
Snnipls Type*
tan Number
Operator
Ambient Temperalur* (T)
Parometle Pressure (In)
Stefc Preesure (In H2O)
^ff/
Probe Lsngti and Type
Monte 10 (ki.)
Mvtaf Box Numbw
MctarAH®
Yd
7Z
ftotw H«rt» 9«fllng (T)
HMrtw Box S«Mng (T)
InMLMkClwcIc
Duct Dimensions (In)
Ff tor Number
Assumed Moltture (%)
02 (*)
CO2(%)
Mo»ttureConee»ed(o)
7'vAr
Trawwm
mmi »n^o Hmyo ^B_PMsi cvJcy ^f^^_ minfls0
/»
//•
Diagram of Duel
Tim*
Clock
Tkn*
124-W
OM Meter
H_ • Ihi !•
rmoifiy
Vm (tl*)
Veloclly
> • --- a
Meen
AP
Orhtee
Pteestr*
AHflnHZP)
Gtas
iipem
(T)
rn
TemperaKve
m
DryQMMctor
OuM
rn
EMU
rn
Pump
Vacuum
SO
A/i
7
I
/'
* <
S:
/Vtf
.5-7
5r.
Comments:
-------
HELD UAIA
| Pug* tot
fctf-lvf
2
Phnt
Onto
Simplno Locrtc
cttnifHt Typo
Run Number
Operator
Ambtont Twnpmrtur* (T)
Otrom«>lc f>«Mtr* (In)
Stale r>«Mur» (In H2O)
4-.IS
Prob* l«ngtfi «r
Nozzto ID (In.)
Yd
K Factor
f>ob« HM«W 8«Mno (T)
Mwrtw
(T)
NM LMk C»wck
^^
r^
.*?
MkmtM
Dfaor«m of Duel
Tim*
(mh)
Clock
Tim*
(24-
S)
r*-^m^M—^
HBBuw^
Vm fir)
AP
OnH20)
OrMc*
AH(lnH2O)
rn
rn
Fltar
f1pVfl
rn
OuM
rn
B«H
m
Pump
Vacuum
(HH)
/tft
/•/£>
/ST-
i±
77 /
Jiti.
~$t
J-i.
f-L.
'
->
f5/
To
£7
','CJ
Con
itto:
-------
FIELD DATA
•>—^ I _J ••»
IVQ9 1 Of / ^,
Phnt
Onto
damping locator)
SampteTyp*
Operator
AmWtnt Tcmporafur* (T)
OaioiiMtlc r\Maur« (In)
State f**nur« (In H2O)
2f-f /
NontoPQn.)
M*torBoxNum(Mr
Yd
HMtw Box S^tng f F)
C -5
DuctDbiwrwioml
Aitunwd Mohlur* (%)
02(%)
C02(»)
02/C02 KMhod
Mol«lur«Coltoctod(Q)
rteeordAIOrtiEy>n/
Vxv
/KX
MknrtM
DtagramofDuet
NOfODW
Tlnw
(•»*»)
CkKk
Tim*
(24-
OsvlUMw
Velocity
AP
»H20)
OrMc*
AH(lnH20)
Fhw
DryGMMtotor
OuM
ExH
Pump
Vacuum
t'O
//^ C> /
^/^
uo
,7^
•7ft
t-
/. f. J-
1C*
7t
'/£)-?
Commcnto:
-------
FIELD DATA
P»Q«tol
Data
Samplng locato
(nntplt Type
Hun NuvntMT
Operator
MfllDMVn TWnfMftmff 9 \*j
Baronwtlc Praatwa (In)
State Praatura (In H2O)
/5
M«tarBoNHumlMr
Yd
KRwtar
Prob« H«ri« Siting (T)
H«rt«r Box 3«Wng ff)
MMLMkCtwcIc
Duc«Dlmanalona(ln)
02(%)
C02(%)
MohluwColteclKlfa)
Mlnutot
DtogwMncfDuel
Tlm«
Clock
Tim*
7-
Vhi (W)
AP
flhH20)
OrNIc*
AH(lnH20)
Qua
vtfMTtt
rn
TwnfMratur*
rn
T«np«nrtur«
rn
DryQMMtatar
T«mp«r«tur*
Exft
m
Pump
Vacuum
(In. Ho)
srr
07 5. /S.
S.tt?
at ,
-Go
C-CJ
f/Ab
H
6,, fJ
-------
FIELD DATA
_££.
Onto
temping Locato
SimptoTyp*
Run Number
Operator
Ambient Temperature fF)
Baromavfe Preetue (In)
Slate Praeaura (In H2O)
PtatMUnQfiandTyp*
NontelD(ln.)
Mctar BOR NumtMr
S«Mng (T)
(T)
DuctDkiMralont (In)
FttarNumtMr
02(%)
C02(»)
OZ/C02M^»od
Mohtur* CoKKlwJ (g)
/c» <,
Read and Record AH Data gvery /fc<> Mtnutee
,/
Diagram of Duct
Ratal
11m*
(iran)
Clock
11m*
GM-M
Vh*
V«toclly
AP
OriH20)
Orlfc*
AH(|nH20)
Gti«
T«np«nrtur«
rn
T*mp«ralur«
rn
m
DryQnM**
rn
OuM
rn
EMU
rn
Pump
Vacuum
dh.Ha)
{£>
I.O&
/-rV
<7 If
'
7/
T.-73
7-2,
O/
GO
/. /v
n-
Comment*:
-------
FIELD DATA
T72
Ptant
ttato
temping Loc«<
tempteTyp*
Run Number
Operator
Ambbnt Tampmriur* (T)
Bwonwfrlc Pr«Mua (In)
State PrMtura (In H2O)
ig* and Type
Monte 10 (fci.)
MctarBcmNumtMr
Yd
KF*e»or
H«rt« Box teMng fF)
(nMLMkCtwck
^
ltel|j|M of Locaton (fl)
DuctDlmanilona(ln)
FKtarNumNr
Actumwl Motolura (%)
02(%)
OZ/C02M^hod
Flrad LMh Chuck
?S
O,£>o1ei
Raad and RacordM Data Evwv t£> Minute*
Diagram of Duel
temping
Tim*
(mln)
V
QuM«tar
Velocity
AP
0hH20)
Orlflc*
PfMMT*
AH(lnH20)
Fhw
PfdM
Twnpmriura
rn
Twnpmtur*
rn
OryQnIUtotar
Tcmpmriur*
OutM
rn
Pump
Vacuum
(In. Ho)
^
SO
SSS
Ssx
Commvnte:
-------
HhLU UAIA
Plant
Onto
9tmpin0 Locaion
Sample Type
Run Number
Operator
Ambtant Temperalura (T)
DaromaHc Praaaur* (In)
State Praaaur* (In H2OJ
Probe Lanqti and Type
Malar Bon Numbw
Yd
KF«c»or
InMlMltChack
?vxv/
tf
rWghl of Location («)
Aaaum«lMohlur.(%)
C02(%)
OZ/C02Ma«wd
Mohlur.Coltoc»«l(o)
MlnulM
DtagwmofDoel
Number
Time
(mhi)
Clock
Tlnw
Vm
Valoclly
HMd
6P
Or Me*
Preeau*
DWaranM
AHflnHgO)
GMa
Twnpwalura
PfOtM
OryOaaMatar
Tamparalur*
/O
^
, O
•)'
-------
UMIM
Ptart
fete
Simptng Lneato
RunNumMr
Operator
mwfrlc Pr*t«w« (In)
State Pt*uu?« (In H2O)
r'
M«tarBtf«T'
Mohtur* Coltetod (g)
FVwILMkChMk
. 0
tot and Award MtetaEvwy /6 Mlnuta*
OtagMim of Dud
Tim*
(fnln)
Clock
Tim*
(24-hr
OmM*tar
VWOCnJf
AP
Ordlc*
OHtarcnM
AH(lnH20)
Flu*
en
rn
m
Twnpwtrtur*
m
OuM
ExM
rn
Pomp
Vacuum
/v
7V
7.7-s
ft
/
7 f
#/
-------
FIELD DATA
Pap* t of (
MA4 frr
Phnt
out*
oumplng LocAVon
StmptoTyp*
Hun NIHMUM
Operator
Ambtont Twnpmlur* (T)
Bwonwfrfe (torn* (In)
StaVe Pr«MUr» (In H2O)
7-C
»«ndTn»
Yd
KFKtor
H«H« Box S«Mng (T)
I wl(|iit of Location (fl)
OuclDlmw«ten«(ln)
FltarNumbv
A«.um«l Mofetur* (%)
C02(%)
02/C02M*hod
/ <
Mlnuta*
/ /i
ij
Diagram of Duct
Hunbw
Tim*
(mtn)
V
Clock
Tim*
04-hr)
OMM*tar
Velocity
AP
0nH20)
Or Me*
DNtarcnM
AHOnH2O)
FHi*
OM
Twnparalur*
rn
Prob*
Twnp«ralur«
r
(D
DryOMMtotar
fn
OuM
rn
Ex*
rn
Pump
Vacuum
On. HO)
/
O/
art
-^^%
3#
^Z-
-------
FIELO DATA
Pftg* t ot
Phnt
Oat*
Simplnq Loeaton
Run NimitiM
Operator
Ambient Temperature (T)
Beromefrfc Preeeure (hi)
State Preeture (In H2O)
ZL&.
Frob^ LftnQwi 0nd Typ^
NonlelD(ln.)
Yd
KFwrtor
FVob«H«nir ScMng (T)
MWLMkChKk
Mwgfil of Locflvon (ft)
Duct Dlmenelone (In)
FWfV NUfTnMT
02(%)
C02(%)
O2/CO2M«t»d
Mofe(ur«Coll«e«Mf(g)
FinM L9AVC OiWCfC
Reed end Record All Defci Every fa
/O
Dtagram of Duel
Poinl
Tim*
(mln)
/J
dock
Tim*
04-hr)
3A
Vm (IP)
AP
(jhHSO)
Orlflc*
AH(»nH20)
Fhw
rn
rn
m
OryGknKMw
Twnpwalur*
rn
OuM
rn
ExH
rn
Pomp
*
/O
?s&(
7-70
0
-*
7-1V
• /
Comment*;
-------
FIELD DATA
Pap* tot
phnt
Data
Operator
Ambtent T*mp*r*1ur* fF)
Bvonwfrlc P/*Mur* (In)
StafcP/*MW*(lnH20)
^
s.ts
ftob* LwigVi and Typ*
NoKzl* ID (In.)
M*tarAH@
Yd
K Factor
P>ob*H
H«it*r Box S^Hnp fF)
fowl Little Cn9CK
H^gMef LocaSon (fl)
n*lont(ln)
AMum*d Moltlur* (%)
02(%)
Mottlur*CollMtod(o)
o, 0 Q1&A ****L** ct*ch
/>, ^^
RMM! and Raoord AM Data &*gJC2__ Minute*
J54
-rr
/-//'/
* £'
Diagram o» Duel
Ttamn*
Tim*
Mr*
dock
Tim*
R4-hr)
Vhi (fl*)
V*k»cNy
AP
(lnH2O)
OHIe*
AH(lnH20)
Flu*
Ga*
7W
Ftob*
T*mp*r*lur*
raw
T*mp«nrtur*
OuM
Pump
Vacuum
JkHflLJ
10
f
•^1
75
&
Z.C/
r
r
•
-------
FIELD DATA
Pug*! of
*££le Preeeu-a (b)
Stofc Preeeure (In H2O)
bo
£
Probe Lengtfi and Type
Monte ID (In.)
DOM rfUfDDW
Yd
Pro(wHaa«ar S^ng (T)
HMlar BOM S«Mng (T)
rrivM LMIVC Cntclc
Height of toca«on(n)
DuetDlmerwlone(ln)
Aatumad Mohtur* (%)
02(%)
£Z£
C02(%)
Moto(uraCoflactod(g)
^-/- Final Leak Check
C.v
L^72"
Read and Record AH Pate Every /£?M1nu>ee
//
Diagram of Duel
TNNWM
Tim*
(mln)
(J
Clock
Ttma
(24-hr)
^
GMMatar
t* --- *• ---
nOTKIWly
Vm (fin
Velocity
AP
0hH20)
OrMca
AHflnHZO)
Fhw
Qit
Ttntpwslure
rn
Tamparalura
rn
DryGMMMar
Tamparalura
Outat
Exll
rn
Pump
Vacuum
At Ho)
D
AT/
•
o
ftj
Com mania;
-------
>• A T!•«
kX^Vf
HhLU UAIA
/
Phnt
Oat*
Qaiiipliilj Locflvon
SftmptoTyp*
Run Number
Ambtent TwnfMrartur* (T)
Bar ornate PTMSU* (In)
State PtMtur* (In H2O)
Pfob.Ungti«ndTyp«
Yd
(T)
DuclDlm«»fan.(ln)
FVtarNimb*
Aitunwd MoMur* (%)
02 (%)
C02(%)
02/C02 Mrthod
flnrt LMh Ctuclc
O,0 /I-
Balm
NumtMf
Time
(mln)
fWd.ndR.ewdAJIOrt.Evwv
"7 /£/,
Mfcwte.
Dt.gr.rn of Duel
Clock
Tim*
(M-lw)
VWocMy
AP
0hH20)
Orlfc*
DNtarcnW
AH0nH20)
FHM
rn
rn
TwnfMnrim
m
Ou
-------
•CMIMMM
FIELD DATA
| P»
Onto
Samplng tocate
Run Number
Operator
Ambtont Temperature (T)
Paromatte Ftattua (In)
SMcf*aMura(frtH2O)
2£.
to
+.ZL
f^oba Laogfi and Typa
Natato 10 (In.)
MCMT DOX rfUrtnMT
MMwAH®
Yd
K Factor
Hwrtvr Box 3«Mng f F)
NMLMkCfwck
DuctOlpMralont (In)
FWwNumbw
02(%)
C02(%)
02/C02M.fwd
MoMur«CoDwlwl(o)
Final LMkChwk
"
avJtp
7*
-------
«••*•••*••!
HbLU UAIA
Papa I of
Phnt
Date
SamptoType
Run Number
Operator
Ambient Temperature (T)
Proba Langtfi and Typa
Nonla ID (In.)
MOTV BOX rvUfTnMT
Y-
K Factor
,/7P7
n« loot (In)
Filar Mumbar
Aaaumad MoWure (%)
02(»)
C02(%)
- 19 3
'Jfo
&&
-------
FIELD DATA
/ /
| P»q«1of
Data
Stamping Location
SampfeTypa
Operator
Amblant Tamparatur* (T)
Baromafrte Praaaura (In)
State Pi aaaura (In H2O)
Pf ob« Ltngfi and Typ*
Moot* ID (hi.)
Mctar BOK Nunibw
Yd
K Factor
H«rt«r Bm S^ttng (T)
InlMLMkChKk
DuctDtnanafana (h)
02(%)
C02(%)
02yC02M^od
H»ad and BacordM Date Evary
MmutM
Diagram of D«cl
PjDM
Numbar
T1m«
(mtn)
Ctert
AP
(ViH2O)
AH(lnH2O)
HIM
On*
rn
rn
Fltar
npwtt
rn
OryGMMMv
Twnpwalur*
OuM
rn
ExN
rn
Pump
Vacuum
(In. Hg)
t'fi
2.0
10
SVf
-------
ft//7#f5
HhLU UA1A
/_v
Phnl
Date
9ampln0 Locavoo
9flmpto Type
Run Number
Operator
Ambient Temperature (T)
OaromeUe
State PreMure (In H2O)
ProlwUngtfiandTyp*
**** Bo" Numb*
M^r AH®
Yd
Probe Heater Sating (T)
Box S«Mno (T)
MM L«ik Cheek
DuctDlmerwloni(ln)
FKferNumb*
A««um«dMoWur»(%)
02 (%)
C02(%)
- 20^
^
ead
d All Date Every
.»
(O
Minute*
Diagram of Duet
Tkne
-&*-
Clock
Tim*
VWocHy
AP
0nH20)
Or Me*
f*Miira
DlftorwiM
FhM
rn
P>ob*
Twnpcrarturv
rn
FMir
Twnpcralur*
rn
Dry ON Meter
Temperature
OuM
rn
End
-£L
Pump
Vacuum
Ho)
fO
SJ67-
to
&-
7-7
Ooninwntet
-------
I It-l-L/ L/MIM
^ /
l4/£*
Phnl
Onto
(tempi* Typ«
Run Numb*
Operator
Ambtont Temperature (7)
Barometric PreMtre (ki)
State Pretture (in H2O)
indType
Nanf«IO(ln.)
KtatarAH®
Yd
KFcdor
Probe Heeler 8eKng(T)
Heater Box
MM IM* Cheek
•7T
DuctDlm«mte»«(>n)
A>«unMdMaltlur«(%)
C02(%)
MoMur«Co«K«wl(o)
> 2.
Ri«d and Record All Orti&wryyC' Mkwtee
Comments:
-------
HbLU UAIA
-*-y=—.*—
Phnt
Onto
Stamping Locafcn
Run Number
Operator
Ambient Temperature (T)
Oarometlc Preeeure (In)
State Preeeure (In H2O)
«£
umdType
Mart, ID (h.)
Mttar Box Number
fF)
I i«M0tif of Locfltfon (fl)
DuctDlmenelone(ln)
FUtarNumbv
Aiiumwi Mohtur* (%)
02(%)
MoMur*Coltocl«l(g)
, % <*ffV MfcuHee
(o-A
Mwiif Re
•£
OrW
DtagramofDiiet
Tim*
Clock
71m*
•• *^B Ir __n_
/?//g
Vhi
AP
Mc«
PTMMF*
DNtorcnM
AH
^p
OryOMWtotar
Twnptralur*
5V
Comnwnte:
-------
FIELD DATA
/ /
JK_
(tato
Stamping locator)
Sfcmpk* Typ»
Run Number
Operator
Ambient Temperature (T)
Barometric Preewe (In)
State Pressure (In H2O)
Monte ID (In.)
BOX riUflWW
Yd
KFtetor
Probe Heater 8eHnq(T)
InM LMk Check
V MQI it of Locttoon (W)
DuctCHmen«lona(ln)
02(%)
C02(%)
FVwILMkChKk
"
7"£r
Tr«ig«e
Used and Record All Ortatverv //I Mtnutea
DtagrcmofDuct
Numb*
Tim*
(mln)
o
Clock
Time
IN-hr)
Vm (fl*)
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FIELD DATA
P«g«tof
Phnt
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Run Number
Operator
Ambient Temperature (T)
Baromefrfc PreMure (In)
State PreMure (hi H2O)
Nonto ID (In.)
MMwBoxNumlMr
Yd
KFMar
HMlw Box S^Ung fF)
HelflMo!ljDC«ton(n)
Ouc1DlnMrMlonfl(lh)
A««im«l MoMm (%)
02(%)
co2(%)
Moh1ur«Coltoc««l(g)
nn«iL«*ct-ci,
MlnutM
Dhor«mofOuel
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(mln)
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FIELD DATA
*//!#<(?..
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Samplng tocafen
SamptoTyp*
RunNumbw
Operator
Ambtent TwnfMratur* (T)
r>ob» langti and Typ»
Nort.lO(ln.)
Yd
S.&7
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Aaninwd Mottlur* (%)
02(%)
C02(%)
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Ambbnt Temperature (T)
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KtatarBoKNumtMr
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KFBrtor
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Duc«Dlm»n»lone(ln)
A>«um«l Moltlur* (%)
02(%)
C02(%)
r^>^
-------
MOISTURE RECOVERY FORM FOR METHOD 4
72AP
'Plant
Date
Sampling Location
Sample Type
Rnn'Number .
Impinger'Box Number
RecoveryTersoin
Recovery Rinses
Sample Identification
'Filter/Number
XAD Number
723
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ft
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S" 03
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Number
lmpinger
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Amount of
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Configuration
Impinger Weight
Final
Initial
Weight
Gain
(E)
A/A
(Ts
563.3
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625.3
Cd
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
.Date
Sampling Location •**
Sample'Type
Run Number
Impinger"Box Number -
RecoveryTerson ? ; -^f^:
Recovery Rinses
Sample Identification :
Filter'Number :•
XAD Number
1LB
ft.
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UAfc- 12
SpLkJLJ/
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant •
SamplnrK Location
Rim'Number -
Imj>ingef "Box Number
Re coveryTerson -
Recovery Rinses
Sample Identification -
XAB Number
Pun / tiunrL C
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Total Weight Gain (g)
25*2.1-
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Sampling Location
SampleType
Run-Number-
ImpingerBox Number
'Recovery Rinses :
Sample Identification
XAB Number
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Number
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Solution
Amount of
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Configuration
Impinger Weight
iTinal
(g)
Initial
Weight
Gain
(g)
A/A
I
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551.3
Gt)
I
10.3
Total Weight Gain (g
2523
-------
MOISTURE RECOVERY FORM FOR METHOD 4
..f
Plant
Date ..- • • • •>-•••
Sampling Location * -^
SampleType ': f >v
Run Number '"# : -•; --^
Impinger" Box Number ~
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Filter Number ; ^ - ^
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lmpin&er
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Amount of
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Configuration
Impinger Weight
OFinal
Initial
Weight
Gain
(g)
MA
633.1
i
55?,
2.t>
Gtl
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
SampleType
RBn'Nuihber
ImpingefBox Number •
RecoveryTerson
Recovery Rinses :
Sample Identification
Filter-Number ^
Number
V
IkiS: /// HtnUMrfL
5 - 35
Total Weight Gain (g)
2K-M
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample'Tjrpe
Run Number
Impinger'Box Number
Recovery~Person '•
'Recovery Rinses
Sample Identification
XAB Number
3?
5 - 3 9
'Imjpinger
Number
Solution
Amount of
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Configuration
Iznpinger Weight
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Initial
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Gain
(R)
A/fl
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Gtl
bff.?
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample'Type
Run Number
Impijjger Box Number
RecoveryTerson '
Recovery "Rinses
Sample Identification :-
XAS Number
-------
MOISTURE RECOVERY FORM FOR METHOD 4
r
'Plant
Date
Sampling Location
Sample Type
Run Number '
ImpiDger Box Number
RecoveryTersoh
Recovery Rinses
Sample Identification
Filter Number
XAB Number
A.
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45- 51 t nyigq-
-------
RADIAN
T2AP
LCarb
TImpinger
Number
1
2
3
4
5
6
7
MOISTURE RECOVERY FORM FOR METHOD 4
*
Plant
Date • .- ' • .- • -•-.
Sampling Lo cation ;' --
Sample'Type ?.v?'
Run Number •«•'-•••• • •* ~: /-.
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?79.f
555. 6
553.1
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(g)
(i^3,2
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72?. 2
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Total Weight Gain (g)
Weight
Gain
23S.1
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I.D
RD
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-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
.Date
Sampling Lo cation
Sample Type
Run 'Number
Impingef Box Number
RecoveryTersoh '
Recovery Rinses
Sample Identification
Filter Number
XAS Number
/jn
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Number
Solution
Amount of
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Configuration
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Initial
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Gain
(R)
A/A
tk.0
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6.9
Total Weight Gain (g)
-------
RADIAN
7J&P
L&irb
"'Impinger
Number
1
2
3
4
5
6
7
MOISTURE RECOVERY FORM FOR METHOD 4
•
Plant -:-: •'•-^0 •-:;,::.: ^
.Date ::v;:-:-:-:* >: : ' • :.:^-:r-:-- *•••?.
Sampling" Location * fS
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Recovery~Person •':-'•'•• --'
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553.0
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Weight
Gain
(E)
2SD.1
M
W
^
^^^
2ID3
-------
MOISTURE RECOVERY FORM FOR METHOD 4
7&P
Plant
Date
Sampling Location
SampleType
Run Number;
Impinger'Box Number
RecoveryTersoh
Recovery Rinses
Sample Identification •
Filter Number
Number
- 75
Impinger
Number
Impinger
'Solution
Amount of
Solution
Configuration
Impinger Weight
(K)
Initial
Weight
Gain
(E)
A/fl
642.
O.D
i
2.1
Total Weight Gain (g)
23^-0
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
17&P
Plant
Bate
Sampling Location
Sample Type
Run Number
Impinger'Box Number
RecoveryTerson
Recovery Rinses
Sample Identification
Filter Number •'•
XAD Number
A.
tieif:/;i
n
Impinger
Number
Impinger
Solution
Amount of
^Solution :
Configuration
Impinger Weight
Final
ft!)
Initial
(g)
Weight
Gain
(B)
A/fl
5*3.1
i
i
51*1.1*
l.o
Total Weight Gain (g)
253.$
-------
MOISTURE RECOVERY FORM FOR METHOD 4
71&P
Plant
.Bate
Samplfng'Location
Sample Type
Hun Number ;
Impiager'Box Number
RecoveryTersoh
•Recovery 'Rinses '•
Sample Identification •
Filter Number
Number
/Lfi
ft.
tf*tS: ///
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
.Date
Sampling Location
Sample Type
RTin'Number
Impinger Box Number
RecoveryPersoii
Recovery Rinses
Sample Identification
Filter Number
Number
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Number
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Solution
Amount of
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ImpingefTip
Configuration
Impinger Weight
;>Final
(K)
Initial
Weight
Gain
A/A
619.9
Cs
I
SSS.o
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Sampling Location
Sample Type
Run Number .
Impingef'Box Number '
RecoveryTeTSOh i
Recovery Rinses -
Sample Identification
XAD Number
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Total Weight Gain (g)
220.^
-------
RADIAN
7&P
Lfarb
"Impinger
Number
1
2
3
4
5
6
7
MOISTURE RECOVERY FORM FOR METHOD 4
•
Plant -
Date .•••*. ..-.-• -•-
Sampling Location * '-
Sample'Type =••• ?'••• --•;'
Run Number />< <••••• ••••*.':«<.•"•
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51*1.3
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Total Weight Gain (g)
Weight
Gain
(E)
2335
M
2.3
IH
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OjJQ Q i
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample^Type
Run "Number .
ImpingerBox Number-
RecoveryTersoh
Recovery Rinses
Sample Identification
Filter Number •
XAB Number
SO.
A.
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U/ffo- /N
III 4
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Sampling Location
Sample Type
Run Number
Impinger Box Number
RecoveryTerson "
Recovery Rinses
Sample Identification
Filter Number •
XAS Number
/?.
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Number
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Amount of
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Configuration
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Gain
(E)
A/fl
51S.1-
i
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Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
r
Plant
Date
Sampling Location
Sample Type
Run Number
Impineef Box Number
RecoveryTersoii
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Sample Identification
Filter Number
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Number
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Amount of
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Configuration
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Final
Initial
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Gain
(K)
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555.3
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Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
SampleType
Run Number
Impinger Box Number
RecoveryTerson
RecoveryRinses
Sample Identification •
Filter Number ;
XAD Number
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I BarAfa&.'fyttM
32
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample Type
RTTO Number :
Impingef "Box Number
RecoveiyTerson. '
Sample Identification
Filter/Number
Number
233
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Number
n&er
Solution
Amount of
Solution ..-
Configuration
Impinger Weight
Initial
(B)
Weight
Gain
(g)
A/fl
115,3
I
553.1
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Sampting Location
SampleType
Run Number
JmpinRer"Box Number
RecoveryTerson
Recovery :Rinses
Sample Identification
XAB Number
8>R iLP
-------
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Bate :
Sampling Location
SampleType '
Run Number
Impinger Box Number
RecovenTRinses :
Sample Identification :
Number
&J£'Htt)H
.
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Number
er
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Amount of
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Impinger Weight
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Weight
Gain
(B)
A/fl
223. 1
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5^,3
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Total Weight Gain (g)
237,5 ;
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
.Date
Sampling' Location -•-
Sample Type
Run Number '•'••'•
ImpinRer" Box Number
RecoveryTerion •
Recovery Rinses >r :•.
Sample Identification •
XAD Number •
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Gain
(R)
A/A
mt&Gai.
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241.8
57?.?
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55?.
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11.3
Total Weight Gain (g
-------
MOISTURE RECOVERY FORM FOR METHOD 4
r
72AP
Plant
Date :
Sampling Location •-•**
Sample Type
Run'Numbe
Impinge* Box Number -
RecoveryTerson
Recovery Rinses
Sample Identification
Filter Number •
XAB Number
fPft
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- i $•
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Sampling Location
Sample'Type
Run-Number :
Impinger Box Number
RecoveryTerson
Recovery Rinses
Sample Identification
XAB Number
D
BarktbJP? H,t>H
Total Weight Gain (g)
212.?
-------
MOISTURE RECOVERY FORM FOR METHOD 4
..£
Plant
SampKnrR Location
Sample*Type
Rnn'Number .
I m pin e er Box Number -
RecoveryTersoh
Recovery 'Rinses
Sample Identification
Filter Number
XAD Number •
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A,
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45- f
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Date
Sampling" Location
SainpleType :
Rira'Number
Imp inger'Box Number ^
RecoverfPersoh
Recovery Rinses :
Sample Identification •
Number
JLfi
A.
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HttH
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Date :
SampHnfrLo cation -r
SampleType
Ruri'Number
Impin^er'Box Number 3
RecoveryTcTsoJi
Recovery Rinses '
Sample Identification •
XAS Number -
A.
fa If: /!/
Bark
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ft 45- 1? '$
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Solution
Amount of
Solntion""
Configuration
ImpingeT Weight
Final
Initial
CO
Weight
Gain
(e)
A/fl
i
2, 1
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Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
•plant
Date
Sampling Location %>
Satnple'Type
Run Number :'
JmpinRer" Box Number -
Recovery~PeTson ':£'-
Recovery Rioses
Sample Identification ^
Filter Number
Number
/Lfi
£h>/>i-
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I??
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Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Sampling Location
SampleType
Run-Number -
Impinger Box Number
RecoveryTcTson
Recovery Rinses -•
Sample Identification
Number
/Lfi
A.
tf*lf:f;i
L RarktUJf HsfiH
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lmpinger
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Amount of
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Configuration
Impinger Weight
Final
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Initial
Weight
Gain
A/fl
GS
If 5? 3
if PL a
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I
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Gtl
i
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
.Date
Sampling Location N -?
SampleType
Impinger' Box Number -i
Recovery~Persoh ^
Recovery Rinses
Sample Identification -'•
XAD Number
7fe/7/V^-/X
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Number
Impin&er
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Configuraton
Impioeer Weight
f el
Initial
;Weight
Gain
A/A
8033
551 • "7-
0.3
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517.0
GcJ
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Rnn'NumbeT
ImpinRcr Box Number -
RecoveryTerson v:.
Recovery Rinse* ^:£,.:../.?;£i
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XAD Number
727
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Inpinger Weight
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-------
RADIAN
L&rb
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1
2
3
4
5
6
7
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MOISTURE RECOVERY FORM FOR METHOD 4
•
Plant • •: •'•".:: '---r :•••>-•:
Date
Sampling Location " ••"•'
Sample'Type : ?>
Run ''Number - : • • ;-:": -, •-••• ^-.v.
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W1.0
57i5.0
53f.O
t,^.r
Total Weight Gain (g)
^Weight
Gain
CB)
2(/l,H
-0,1
I.I
•?.4
^\
m>
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
.Date
Sampling" Location
SampleType
Impingef "Box Number ^
Recovery-Rinses
XAD Number •
S(L
3s)/* j'n? HZ&> r
(b
f\
A.
BedL&JL'HitH
Total Weight Gain (g)
29I..1
r
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Run Number
Impingef "Box Number
Recovery Rinses :
Sample Identification
Number
*un IL
/Lfi
A.
- 223
uufi-45-
;impinger
: Number
Solution
Amount of
olution •
/I//?
Configuration
ImpinRcr Weight
4 SI.
Initial
:Weight
Gain
i
I
549,
0.
Gti
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
TZA?
Plant
.Date
Sampling Location
SampleTjpe
Ruri"NumbeT ,
Impinger'Box Nuinber
Recovery Rinses :
Sample Identification
•
Filter-Number-
XA© Number
10
iJ*
U* IS
•//I'/// //.
-211
dM-MrfL
2?/
'Inajpingef
^Number
n&e
Solution
Amount of
^Solution '
ImpingerTip
Configuration
ImpinRcr Weight
iFinal
fsrt
Initial
CR')
^Weight
Gain
A/fl
^31,2.
263.?
595- D
54?.
1.?
GcJ
10. 1
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
•plant
Date
Sampling Location
SampleType
Imp ingerBox Number ^
RecoversTPersoh T"
Recovery llinses -::
.Sample Identification ;-':;
XAD Number
/ -/
D
/Lfi
A.
BarkfoJf-'HtfiH
- 2W
'Impinger
Number
•Solution
Amotmt of
Solution ^
ImpingefTip
Configuration
Impinger Weight
IFinal
Initial
(R)
;Weight
Gain
(R)
A/ft
1.0
i
i
I.D
5//&L
Gtl
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
SampHuE Location
Sample'Type
Ruif Number ' •<&
ImpingerBox Number
RecoveryTerson
Recovery Rinses
Sample Identification
Filter'Number
Number
- -04-
U*&Htt>H
ilmpinger
Number
Ixnpinger.
-Solution
Amount of
olution ;
Configuration
Impinger Weight
IFinal
Initial
^Weight
Gain
6s
65?. (
i
i
-o.z
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Date
Samplnrg Location
"Run Number .
Impingef "Box Number
RecoveryTersoh
Recovery Rinses
Sample Identification
Filter Number
Number
/UP
Kfa
Impinger
Number
lmpinger
Solution
Amount of
"Solution ;
ImpingefTip
A -•••^ . . *
Configuration
Impinger Weight
iTinal
CK)
Initial
Weight
Gain
A/fl
-0-3
554. (
554.0
i
555.1
o.o
I
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Samplfnjj Location
SampleType
Rnri'Number :
ImpiD Rer Box Number
Recovery Rinses '
Sample Identification '
FilterNumber
XAD Number
/y/i
/UP
/fc£i//2£/?<.
:impinger
Number
olution
Amount of
"Solution ~
ImpingefTip
Configuration
Impinger Weight
(g)
Initial
(g)
-Weight
Gain
(E)
A/A
650-1-
(TS
j
i
Total Weight Gain (g)
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Bate
Sampling Location
Sample Type
Run' Number
Impin f?ef Box Number
RecoveryTcTson
Recovery Rinses
Sample Identification
Filter Number
XADNumber
01ft
ite£V/ZS7't
Z)
/Lfi
tit&H&H
Wf<.
Total Weight Gain (g)
-1.0
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
SampleType •
HmrNumber ;
Im pin ger'Box Number ~
RecoveryTersoh
RecoveryHinses
Sample Identification '
XAB Number '
fPA
A.
/Lfi
A.
&7>/v- tklf: ///
Rarkttdt* fafiH
Z~ "5/6
. • .. •-• ••
.:lmpinger
'Number
Solution
Amount of
.Solution •
ImpingefTip
Configuration
Impinger Weight
Final
Initial
(Bl
'Weight
Gain
(El
cs
-aa
I
-0.1-
y
0.2
Total Weight Gain (g)
-2.1
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Sampling Location
Rnn-'Number ;
Impiuger~Box Number -
RecovcryTerson
RecoveryRinses
Sample Identification :
XAD Number
ULfi^
SC.
Pun A2. AunrL ft
/Lfi
RarklW fot)H
- 3/6,
'Impinger
Number
nger
• Solution"
Amotmt of
^Solution :
Confiruration
"* ' '**
Impinger Weight
Initial
'Weight
Gain
(Jrt
A/A
Uft-l
-13
i
i
55D-T
$/'//'&.
Total Weight Gain (g)
-------
MOISTURE RECOVERY FORM FOR METHOD 4
'Plant
Bate
Sampling Location
Sample'Type
Impmger Box Number
RecoveryTerson.
Recovery iRinsesr:
Sample Identification
XAB Number
~ 322.
3(7-
-------
RADIAN
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Samplme Location
Sample'Type '-
'Number
Irppingef "Box Number
Recovery~Person •
Recovery/Rinses
Sample Identification
FilterNumber
XAD Number
un
/Lfi
A,
•I*. 1,1 nnun- nri*-. oui nr
- 323 -» UAfo- 32?
BecM&IL'HttH
UA4S- 323
Total Weight Gain (g)
-------
APPENDIX D-3
Chain-of-Custody Forms
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanbmg. SC
RECOVERY PERSON
DATE: t/-23-9t,
/Of cU
RECEIVED BY-
DATE:
t<
(/
I/
u
V
V
V
t
I/
\X
t
V
Vx
V
W
I/
V
\/
I/
»/
\
i/
Vx
U
Sample #
WA4S4JI
WA4S-OJ
4&A4S-OJ
10A4J.04
CONDENSER- MKHI
KNOCKOUT 1ST IMP - MtOH
7*3 IMPS - McOlt
FILTER
niR-l.l MtOH/MtCLJ
TRAP - C ARDOXEN 1 000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - McOM
7*3 IMPS -McOH
FILTER
FHR-l:IMcOH/McCU
TRAP-CARBOXEN 1000
BUR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - MtOH
1*3 IMPS- MfOII
FILTER
FHR-MMcOH/McCU
TRAP-CARBOXEN 1000
BHR W/ CONDENSER • MtOII
KNOCKOUT 1 ST IMP - MeOlt
7*3 IMPS • McOH
Comments
.
Pagel
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanbiirg. SC
RECOVERY PERSON:
DATE:
RECEIVED BY:^
DATE:
u
\,
V
**
\s
V-
V
Is
\,
tx
u
u
u
I,
V
L
1,
V
V-
L
t
\x
V
u
Sample *
ftA4J-23
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg. SC
RECOVERY PERSON
DATE:
RECEIVED BY:
DATE:
V
V,
k
\
1
v
V
V
V
U
V
V
V
V
V
>
\.
I
Sample *
J0A43-49
• Cjt
rW rt^ j- JO
'WA43-37
WA43-3*
0M43-39
WA43-«0
WA434I
WA43-6]
WA4343
WA45-44
WA4343
WA43-6«
WA4347
WA434*
WA43-«9
WA43-70
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanbiirg, SC
RECOVERY PERSON:
DATE:
RECEIVED B
DATE:
V,
V
w
ij
I/
t
J
*•
V
I
I/
L
\^
u
t
V
t
u
V
u
V
I.
t
I.
Sample!
• 04
- ACN- FHR- D- 04
- ACN- TRAP. D- 04
• ACN. BHR. D- 04
- ACN- COND. D. 04
• ACN- 2A3IMP- D- 04
Sample Type
M 301 ACETONmULE
M 301 ACETONrTHILE
M30I ACETONtTRILE
M30I ACETONtTRIU
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M30I ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONITRILE
Preservative
FILTER
FUR- I.I MfOH/MKXl
TRAP-CARDOXEN 1000
DHR W/ CONDENSER • McOII
KNOCKOUT 1ST IMP - MtOH
7*3 IMPS - M«OH
FILTER
niR-MMcOH/McCU
TRAP • CARDOXEN 1000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - MtOII
7*3 IMPS - MtOII
FILTER
FHR.|:IMcOH/McCL2
TRAP-CARBOXEN 1000
nilR W/ CONDENSER . MtOII
KNOCKOUT 1ST IMP - MtOII
7*3 IMPS . MtOH
FILTER
FHR.|:IMcOII/MtCU
TRAP • CARBOXEN 1000
BUR W/ CONDENSER • McOII
KNOCKOUT 1ST IMP - MtOII
7*3 IMPS - MtOII
Comments
flui AVLuJ)
)*LhAOuJLQ
&U) AJLMtA
^ <~f\ A*J\uA
Page 4
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg, SC
RECOVERY PERSON:
DATE:
RECEIVED BY
DATE:
t
u
V
L
c
I
V
V
V
I
iJ
u
i/
I
V
*/
i'
I
I
L
V
i,
I
l>
Sample *
•WA4J-97
1YA45-9I
WA«S-99
&A45-IOO
WA4S-IOI
fcA45-102
^A43-I03
- ACN- 7*3IMf- A- 03
- ACN- F- B- OS
- ACN- FHR- B- 03
. ACN- TRAP- B- 03
- ACN- BUR- B- 03
. ACN- COND- B- 03
. ACN- 7A3IMP- B- 03
. ACN- F- C- 03
• ACN- FHR- C- 03
. ACN- TRAP- C- 03
- ACN- BHR- C- 03
. ACN- COND- C- OS
- ACN- 7WIMP- C- 03
_- ACN- F- D- 03
• ACN- FHR. D- 03
_. ACN- TRAP- D- 03
- ACN- BHR- tV 03
. ACN- COND- D- 03
f • ACN- 7AJIMP- D- OS
Sample Type
M30I ACETONITRILE
M 301 ACCTONITRILE
M JOI ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M30I ACETONITRILE
M 301 ACETONTTRILE
MJOI ACETONITRILE
M JOI ACETONITRILE
MJOI ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONmULE
M 301 ACETONTTRItE
M JOI ACETONfTRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONmULE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONITRILE
Preservative
FILTER
FHR-l:IMcOII/MtCL2
TRAP-CARHOXEN 1000
nilt W/ CONDENSER - McOII
KNOCKOUT 1ST IMP - McOII
7*3 IMPS - McOH
FILTER
FHR-l:IMcOH/MfCL2
TRAP-CAROOXEN 1000
nilR W/ CONDENSER • McOII
KNOCKOUT 1ST IMP - McOII
7*3 IMPS -McOH
FILTER
FHR-l:IMfOH/McCL2
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - McOII
KNOCKOUT 1ST IMP - McOH
7*3 IMPS - McOH
FILTER
FHR-l:IMcOH/McCL2
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - McOII
KNOCKOUT 1ST IMP - McOII
7A3 IMPS - McOH
Comments
WwJLLrui
& ifl JLU\9
iStlSlJtiAJ
l^i/iJ^Jie
Page 5
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITR1LE
Spartanburg, SC
RECOVERY PERSON:
DATE:
RECEIVED BY
DATE:
1
\
t,
u
t
1
t
t-
V
ix
V
I/
V
V
V
V
u
t
V
t
I
\,
Sample i)
KrA45-m
tfA43-lll
f
WA43-113
4A43-I24
1WA43.I23
T-' ACN- F- A- 06
i • ACN- FUR- A- 06
• ACN- TRAP- A- 0<
• ACN- BUR- A- M
. ACN- COND- A- 06
• ACN- 1A3IMP. A* M
- ACN- F- B- M
. ACN- TOR- B- M
• ACN* TRAP. B- M
• ACN. BHR. D- M
• ACN* COND- B- M
• ACN- 2*3IMP- B- M
i - ACN- F- C- «
. ACN- TOR- C. M
• ACN- TRAP- C- M
. ACN- BHR- C- M
- ACN- COND- C- 06
• ACN- 2A3IMP- C- M
- ACN- F- D- M
- ACN- FHR- D- 06
• ACN- TRAP- D- 06
• ACN- BHR- D- M
• ACN. COND- D- M
' - ACN- 2*3IMP- D- 06
Sample Type
M 301 ACETONtTRILE
M 301 ACETONITRILE
M JOI AuETuNIIRILt
M 301 ACETONITRILE
M 301 ACETONrTRILE
M 301 ACETONrTRILE
M 301 ACETONrTRILE
M 301 ACETONrTRILE
M 301 ACETONrTRILE
M 301 ACETONrTRILE
M 301 ACETONtTRILE
M 301 ACETONrTRILE
M 301 ACETONtTRILE
M 301 ACETONrTRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONTTRtLE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONTTRrLE
M 301 ACETONTTRILE
M 301 ACETONrTRILE
M 301 ACETONTTRILE
M 301 ACETONITRII£
Preservative
FILTER
FUR -1:1 McOH/McCL2
a<\
TRAP • CARtlOXEN 1000 «//7'
BHR W/ CONDENSER • McOH
KNOCKOUT 1ST IMP - McOH
)A3 IMPS • McOH
FILTER
FHR-l:IMcOH/McCL2
TRAP • CARDOXEN 1000
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg, SC
RECOVERY PERSON
DATE:
RECEIVED BY
DATE:
I
ix
V
V
l>
is
I
u
I/
I
t
I/
t,
I
lx
L
U
t
«/
lx
V
lx
t
t
Sample *
WA43-I43
WA43-14«
WA45-H7
WA43.I4S
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg. SC
RECOVERY PERSON:
DATE:
RECEIVED BY: X/iU/flf
DATE:
t
I
V
L
L
V
X,
L
V
t
I
V
u
\x
u
S
L-
i/
V
L
V
».
u
V
Sample 0
WA43-K9
WA4S-I70
WA43-I7I
VVA4S-I72
WA4S-I7J
WA43-I74
WA43-I73
WA45-I76
W/WJ-IT7
WA43-I78
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanbtirg. SC
RECOVERY PERSON:
PATE:
RECEIVED BY
DATE:
I
V
V/
V
I/
u
u
t
V
V
I
c
t
I/
I
V
t
V
V
V
Sample *
nv
'I: ACN- F- A- 09
. ACN. FHR- A- 09
,- ACN- TRAP- A- 09
- ACN- BHR. A- 09
• ACN- COND- A- 09
- ACN- 1A3IMP- A- 09
• ACN- F- B- 09
- ACN- FHR- B- 09
- ACN- TRAP. B- 09
• ACN- BHR- B- 09
- ACN- COND- B- 09
• ACN- 1A3IMP- B- 09
- ACN- F- C- 09
- ACN- FHR. C- 09
• ACN- TRAP- C- 09
. ACN- BHR- C- 09
• ACN- COND- C- 09
• ACN- 1*3IMP- C- 09
- ACN- F- D- 09
• ACN- FHR- D- 09
• ACN- TRAP- O- 09
• ACN- BHR- D- 09
• ACN- COND- D- 09
. ACN- }*3IMP- D- 09
Sample Type
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONTTRJLE
M 301 ACETONTTRILE
M 301 ACETONTT1ULE
M 301 ACETONTTRILE
M 301 ACETONTTRJLE
M 301 ACETONTTRILE
M 301 ACETONTT1ULE
M 301 ACETONTTRJLE
M 301 ACETONmULE
M 301 ACETONTT1ULE
M 301 ACETONTTRJLE
M 301 ACETONTTRILE
M 301 ACETONTTRJLE
M 301 ACETONTTRILE
M 301 ACETONTTRJLE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
Preservative
FILTER
FHR.|:IMcOH/McCL3
TRAP CAROOXEN 1000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - McOH
7*3 IMPS - McOH
FILTER
FIIR-ltlMcOH/McCLl
TRAP-CARBOXEN 1000
BHR W/ CONDENSER * McOH
KNOCKOUT 1ST IMP - McOH
2*3 IMPS -McOH
FILTER
FHR-l:IM«OH/McCU
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - McOH
7*3 IMPS • McOH
FILTER
FHR-l:IMcOH/McCU
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - McOH
7*3 IMPS . McOH
Comments
Page 9
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg. SC
RECOVERY PERSON:
DATE:
RECEIVED BY:Mj-LLdi
DATE:
\
I
V
t,
V
t
(J
V
V
Is
V
u
\
V
V
V,
V
V
\
V
V
V
u
v/
Sample #
»tf/W3-7l7
WA43-7II
WA4S-7I?
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRJLE
Spartanbtirg, SC
RECOVERY PERSON:
DATE:
,1 I,
iM*.
RECEIVED BY
DATE:
•
t
u
U
Vx
t
I
V
u
I/
V
V.
X.
V
\
iwr
Sample*
WA43-24I
WA43-142
WA4S-243
WA43-144
bWA43-)43
WA43-14«
WA43-147
WA43-74I
WA43-149
WA43-2JO
WA43-23I
WA43-231
WA43-133
&A43-234
WA43-J35
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg,:
RECOVERY PERS
DATE:
RECEIVED BY:
DATE:
P«gt12
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spannnburg. SC
RECOVERY
DATE:
RECEIVED BY:
DATE:
V.
I
Ix
I
I
V
I
I
v,
I
t
i
u
u
\
t
I
V
t
V
V
L.
V
V
Sample *
4rA43-2ft
/
WA43-2I2
f
WA43-2I3
WA43-2S4
rfA43-2t3
-------
CHAIN OF CUSTODY - EPA WA4J ACETONITRJLE
Sparttnburg, SC
RECOVERY PERSON
DATE:
RECEIVED BY:
DATE:
u
C
I
V.
I
I
u
V
I
t
t
t-
u
\X
t
I
t
I
V
V
V
I
Sample f
WA43-303
&A43-3M
WA43-307
WA43-3M
^A43-30?
WA43-3IO
FB2
Sample Type
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRTLE
M 301 ACETONnRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONtTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRTLE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M 301 ACETONTTRTLE
M 301 ACETONTTRILE
M 301 ACETONTTRILE
M30IACETONTTRILE
M 301 ACETONTTRILE
Preservative
FILTER FIELD BK2
FHR • 1:1 McOH/McCU HELD BK2
TRAP - CARIKIXEN 1000 FIELD BK2
BHR W/COND. • McOH HELD DK2
KNKOUT 1ST IMP - MtOH FIELD BK2
2*3 IMPS • McOH FIELD BK2
FILTER FIELD BK2
FHR - 1 :l McOH/MfCU FIELD BK2
TRAP - CARBOXEN 1000 HELD BK2
BHR W/COND. - McOH HELD BK2
KNKOUT 1ST IMP • McOII HELD BK2
2*3 IMPS . MtOH HELD BK2
FILTER FIELD BK2
FHR - 1:1 McOWMcCU FIELD BK2
TRAP • CARBOXEN 1000 HELD BK2
BHR W/ COND. • McOH FIELD BK2
KNKOUT 1ST IMP - McOH FIELD BK2
2*3 IMPS - McOH HELD BKJ
FILTER FIELD BK1
FHR . I.I McOH/McCL3 HELD BK2
TRAP . CARBOXEN 1000 HELD BKJ
BHR W/COND. • McOH FIELD BK2
KNKOUT 1ST IMP - McOH FIELD BK2
2*3 IMPS - McOH HELD BK2
Comments
-
Page 14
-------
CHAIN OF CUSTODY - EPA WA45 ACETON1TRILE
Sparianburg, SC
RECOVERY PERSON:
DATE:
RECEIVED BY:
DATE:
TRAT-CARBOXENIOOOTRIfBICI
TRAT-CARBOXEN lOOOTRIfnW
Page 15
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg. SC
COVERY PERSON.
RECEIVED ftY.
DATE:
Simple 1
WA45-346
WA4 3-347
WA4 3-341
WA43-349
WA4S-3JO
WA43-33I
WA4J-3J7
WA43-333
WA43-334
WA4S-3S3
WA43-337
WA43-33S
WA43-339
WA43-360
WA4J-36I
WA4 3-362
WA4 3-363
WA43-364
WA43-363
WA4 3-366
WA45-367
WA43-36I
WA4 3-369
"X. Field I.D.
WA45- _^WACN- F- A-
WA45- _ | - A^WJHR. A-
WA43- - ACN- TR^^ A-
WA43- - ACN- BUR- ^W
WA43- - ACN- COND- A- ^S
WA43- - ACN- 7»3IMP. A-
WA43- - ACN. F- B-
WA43- • ACN. FHR. B-
WA43- • ACN- THAT- B-
WA43- - ACN- DHR. 5-
u/Ajt ArtJ murv n.
WA43- - ACN- 1A3IMP- B-
WA4J- - ACN- F- C-
WA4J- - ACN- FHR- C-
WA43- - ACN- TRAP- C-
WA43- • ACN. BHR. C-
WA43- - ACN- COND- C-
WA43- • ACN- 7A3IMP- C-
WA43- - ACN- F- D-
WA43- - ACN- FHR- D-
WA45- - ACN- TRAP- D-
WA43- - ACN- BHR. D-
WA43- - ACN- CONtV D-
WA43- - ACN- 7A3IMP- D-
Sample Type
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONtTRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
fcuKflCFrONmilLE
M 301 AUtoNITRILE
M 301 ACETONHuLE
M 301 ACETONITRII^V
M 301 ACETONnHILB <
u ini ArrroutTVli t m
M 301 ACETONITRILE *
M 301 ACETONTTRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONrTRILE
M 301 ACETONrrRILE
M 301 ACETONITRtLE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONITRILE
M 301 ACETONtTRILE
M 301 ACETONtTRlLE
Preservative
FILTER
FHR - 1:1 M«OH/McCLl
TRAP - CAR BOXEN 1000
BHR W/CONDENSF.R • M«OH
KNOCKOUT 1ST IMP - M«OH
2*3 IMPS . McOH
FILTER
FHR-l:tM
-------
CHAIN OF CUSTODY - EPA WA45 ACETONFTRILE
Spartanburg, SC
(VERY PERSON:
DA
RECEIVED B
DATE:
Sample *
WA4S-370
WA43-37I
WA4S-37J
WA4S-373
WA4S-374
WA43-375
WA4S-37*
WA43-377
WA4S-37I
WA4S-37*
WA43-3N
WA43-3SI
WA43-JW
WA43-3S3
WA43-3I4
WA43-3i3
WA4S-3M
WA43-3S7
WA43-3M
WA43-3S9
WA43-390
WA43-39I
WA43-397
WA43-393
^X, Field I.D.
WA43-^V_. ACN- F- A-
WA43- ^VACN- FHR- A-
WA43- - ASfcTRAP- A-
WA43- • ACN- WHt A-
WA43- - ACN- COND^^A.
WA43- - ACN- J*3IMP- A^.
WA43- . ACN- F- B-
WA43- - ACN- FHR- B-
WA43. • ACN- TRAP- B-
WA43- • ACN- BHR. B-
WA43- - ACN-CONIV B-
WA43- • ACN. 7A3IMP. B-
WA43- . ACN- F- C-
WA43- • ACN- FHR. C-
WA43- . ACN- TRAP- C-
WA43- • ACN. BHR- C-
WA43- • ACN- COND- C-
WA43- • ACN- 1A3IMP- C-
WA43. • ACN- F. D-
WA43- • ACN- FHR- O-
WA43- • ACN- TRAP- D-
WA43- . ACN- BHR- D-
WA43- - ACN- COND- D-
WA43- • ACN- 2A3IMP- D-
Sample Type
M 301 ACETONfTRILE
M 301 ACETONrnULE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONTTRILE
M 301 ACETONITRILE
UJOI ACETONITRILE
M Kh^CETONrnULE
M 301 AcSnnTRILE
M 301 ACETONSuLE
M 301 ACETONtTRIL^Ml
JH
M 301 ACETONtTRILE/7
M30I ACETONtTRIt//
M 301 ACETONrrRIlf /C
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M30IACETONITRILE
M 301 ACETONITRILE
M 301 ACETONITRILE
M30I ACETONfTRILE
M 301 ACETONrrRII,E
Preservative
FILTER
FHR. 1:1 MK>H/M«CL1
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - McOH
KNOCKOUT 1ST IMP - McOH
IA3 IMPS • McOH
FILTER
FHR.1:IMfOH/M«CL2
TRAP-CARBOXEN 1000
BHR W/ CONDENSER - M«OH
KMpCKOUT 1ST IMP - MtOII
Hb IMPS -McOH
^iW^V.
iff^ftv/McCU
** ^V
TRAP - CARBOXmjOOO
BHR W/ CONt>ENSER%%CHI
KNOCKOUT 1ST IMP • MtOM^.
1*3 IMPS- McOH ^V^
nLTER ^
FHR.|:IMcOWMV
^V^
Page 17
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRJLE
Spartsnbtirg, SC
RECOVERY PERSON:
DATE: _
RECEIVED BY:.
DATE: "
Sample *
Field I.D.
Sample Type
npl<
Wt
Preservative
Comments
1VA4S-394
WA«.
ft .fifc
M 301
WA4S-39S
WA4S-
ACN-
M 301 ACETONtnULE
WA43-J96
WA43-
ACN-
M JOI ACETONrTRILE
WA4J-
ACN-
M 301 ACETONITRILE
WA43-39I
WA43.
•^ACN-
M 301 ACETONITKILE
WA43-
• ACN-
6
M 301 ACETONtTIULE
WA4 3-400
WA45-
• ACN-
MJOI ACFrONtTHILE
WA45-40I
WA43- I " • ACN-
AcrnwrrniLE
VA43-401
WA45-
. PA
M 301 ACETomTRILE
WA43-
ACN-
M 301 ACETONtTIULE
WA45-
ACN-
MJOI ACETONrrtlLE
WA43-
I . ACN-J
. 0.
M 301 ACETONITKILE
ITA45-406
WA45-MM>ACN-
M30I ACETONITRtLE
WA45-
- ACN-
M 301 ACETONITRtLE
WA43-
ACN-
M 301 ACETONtTRILE
WA43.
ACN-
M 301 ACETONITRtLE
-------
CHAIN OF CUSTODY - EPA WA45 ACETONITRILE
Spartanburg. SC
RY PERSON:
RECEIVED BY:
DATE
Sample #
WA45-4I9
WA4 5-470
WA45-42I
WA45-4JJ
WA4S-4J3
WA45-4J4
WA4S-4I5
WA4 3-476
WA4 5-477
WA4 5-471
WA4 5-479
WA45-4JO
WA4 5-431
WA45-4J7
WA45-433
WA4S-434
WA43-435
WA4S-43*
WA4S-437
WA4 5-431
WA4S-439
WA4 5-440
WA4 5-441
WA45-447
WA45-443
WA4 5-444
^V Field I.D.
WA45- ^ICN-
WA45- - ACN^. - - -
WA45- • ACN- ^V^ • -
WA43- - ACN- -^V^ -
WA45- • ACN- - - >
WA45- - ACN- - - -
WA45- • ACN-
WA4J- • ACN-
WA45- - ACN- - - -
WA45- - ACN. - - -
WA45- • ACN- . • - -
WA45- • ACN- - • -
WA45- • ACN- • • -
WA45- • ACN. • - -
WA45- • ACN- • - -
WA45- • ACN. • • •
WA45- • ACN- • • -
WA45- - ACN- - - -
WA45- . ACN- - - -
WA45- - ACN- - - -
WA45- - ACN- - - -
WA45- - ACN- . - -
WA43- - ACN- - - -
WA45- - ACN- - - -
WA45- - ACN- - - -
WA43- - ACN- - - -
Sample Type
M 301 ACETONmULE
M 301 ACETONmtlLE
M 301 ACETONITRILE
M 301 ACETONrrRILE
M 301 ACETONmULE
M%^ACETONtTRILE
M 301 M^pNrTWLE
M 301 ACETONKaiLE
M 301 ACETONITRI^.
M 301 ACETONmULE
M 301 ACETONmULE
M30I ACETONrrRILE
M 301 ACETONTTRILE
M 301 ACETONmULE
M 301 ACETONTTRILE
M 301 ACETONrrRILE
M 301 ACETONrrRILE
M 301 ACETONmULE
M 301 ACETONmULE
M 301 ACETONmULE
M 301 ACETONmULE
M 301 ACETONITRILE
M 301 ACETONmULE
M 301 ACETONmULE
M 301 ACETONmULE
M 301 ACETONITRILE
Preservative
V
^SJjf^
''JJJ
WJ^X.
Tr ^)9w/\>
7C \
x
>
Page 19
Continents
^
X
N.
X.
V
\
X
x
X
X
-------
APPENDIX E
Result Summary
Table and Figures
-------
Table E-l.
Method 301 Calculations
Compound: Acetonitrile for Manual Method
Calculation of Precision, Bias, and Correction Factor
Run
1
2
3
4
5
6
7
8
9
10
Spiked Trains
Train A
73.77
70.64
78.30
76.60
82.45
52.21
68.84
80.28
82.62
102.85
Train B
74.07
68.22
80.45
69.48
79.91
58.46
79.78
62.02
51.67
108.97
Amount Spiked
Train A
70.08
79.05
81.83
77.18
81.69
70.71
82.02
73.45
80.17
94.09
Train B
66.52
68.03
70.81
71.44
77.10
54.14
69.66
70.79
68.94
91.60
Unspiked Trains
Train C
0.0425
0.0339
0.0546
0.0586
0.0573
0.0515
0.0312
0.0205
0.0255
0.0376
Train
D
0.0362
0.0411
0.0350
0.0534
0.0554
0.0476
0.0275
0.0324
0.0216
0.0230
Amount (mg)
A-SpA
+3.69
-8.41
-3.53
-0.59
+0.75
-18.50
-13.18
+6.83
+2.45
+8.76
B-SpB
+7.56
+0.20
+9.64
-1.96
+2.82
+4.32
+ 10.12
-8.77
-17.27
+ 17.38
Spiked Train
Precision
di
-3.87
-8.61
-13.17
+ 1.37
-2.06
-22.82
-23.30
+ 15.60
+ 19.72
-8.62
di2
14.96
74.09
173.33
1.88
4.24
520.72
542.76
243.30
388.72
74.31
Bias
Train A
3.65
-8.45
-3.58
-0.64
0.70
-18.55
-13.1
6.80
2.42
8.73
Train B
7.52
0.16
9.59
-2.01
2.76
4.27
10.09
-8.80
-17.29
17.35
SDs = 10.0954 B= 0.07
RSDs = 1 3 .45% SD = 9.4660
(Acceptable)
SDm= 2.1167
t= 0.035
tcrit= 2.093
Precision of Unspiked
Trains
di
0.00633
-0.00712
0.01957
0.00519
0.00192
0.00386
0.00363
-0.01190
0.00390
0.01462
di2
0.0000400
0.0000507
0.0003828
0.0000270
0.0000037
0.0000149
0.0000132
0.0001416
0.0000152
0.0002137
SDu= 0.00672
RSDu= 17.09%
(Acceptable)
Bias is insignificant
-------
Table E-2. Sampling Parameters
Run/
Train
1A
IB
1C
ID
2A
2B
2C
2D
3A
3B
3C
3D
4A
4B
4C
4D
5A
5B
5C
5D
6Ah
6Bb
6Cb
6Db
7A
7B
7C
7D
Sampling
Duration
(min)
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
60
Moisture (%)
28.0
27.8
26.9
27.1
27.3
27.1
24.9
24.8
25.8
24.8
22.6
22.9
24.6
24.5
22.4
22.4
25.4
26.0
23.1
22.6
17.4
17.0
15.2
15.0
25.3
25.3
24.01
23.4
Standard
Meter
Volume
(dscm)
0.958
0.993
0.917
0.906
1.00
1.04
0.993
1.04
0.944
0.994
0.933
0.946
0.940
0.960
0.932
0.959
0.866
0.941
0.869
0.881
0.975
1.02
0.961
0.978
0.933
1.00
0.934
0.930
Stack
Temperature
(°C)
66.0
66.3
66.3
66.2
66.3
66.2
66.2
66.2
65.3
65.5
65.5
65.3
66.4
66.6
66.4
66.4
65.6
65.6
65.2
66.2
55.5
54.9
55.5
55.6
65.8
65.9
65.6
66.1
Stack Gas
Velocity
(mpm)
817
817
815
816
892
891
887
887
883
881
880
878
874
874
870
887
810
818
811
811
856
851
843
844
841
841
838
838
Percent
Isokinetic
112.'
116.'
106
110
107
110
103
108
99.1
103
94.2
96.2
98.4
100
95.2
96.2
98.4
107
95.6
96.5
91.9
96.0
89.4'
90.8
101
109
100
98.9
-------
Table £-2. (Continued)
Run/
Train
8A
SB
8C
8D
9A
9B
9C
9D
10A
10B
IOC
10D
Sampling
Duration
(min)
60
60
60
60
60
60
60
60
60
60
60
60
Moisture (%)
24.9
24.9
22.9
23.3
29.2
29.5
27.8
27.5
29.8
28.9
27.9
27.1
Standard
Meter
Volume
(dscm)
0.973
1.03
0.979
0.959
0.950
1.00
0.954
0.955
0.936
0.997
0.954
0.943
Stack
Temperature
(°C)
65.8
65.7
65.6
65.6
65.9
65.7
65.8
65.9
66.2
65.8
66.0
66.0
Stack Gas
Velocity
(mpm)
871
871
867
868
876
876
873
872
877
875
873
872
Percent
Isokinetic
101
107
99.8
98.1
106
112.'
104
104
105
110
105
102
"Outside limits of 90 to 110 percent
Incinerator process interrupted during run
-------
Table E-3. VVA 45 Spike Quantities
Quantity
Run Train A
1 67.1
2 79.0
3 77.2
4 72.6
5 70.7
6 68.9
7 76.5
8 71.5
9 76.2
10 88.1
Acetonitrile Spiked" (mg)
Train B
66.1
70.7
70.4
68.6
72.6
55.2
69.7
72.9
68.9
91.3
'Spike Quantity = (Anal. Conc.)[(Initial Wt. - Final Wt.)/(Density)]
Density = 1 g/mL
Anal. Cone. = 3.6095 g/mL
-------
Table E-4. Probe Rinse Results
WA45-245
WA45-246
WA45-247
WA45-248
WA45-249
WA45-250
WA45-251
WA45-252
Sample ID
Probe Rinse A (4/24/96)
Probe Rinse B (4/24/96)
Probe Rinse C (4/24/96)
Probe Rinse D (4/24/96)
Probe Rinse A (4/25/96)
Probe Rinse B (4/25/96)
Probe Rinse C (4/25/96)
Probe Rinse D (4/25/96)
Amount Surrogate Recovery
(Total mg) (%)
<0.02
<0.02
<0.02
<0.01
<0.02
<0.03
<0.02
<0.02
82
84
89
77
86
83
85
83
Detection Limit = (l/5)(Low Standard Concentration)(Sample Volume)
-------
Table £-5. Filter Analysis Results
Amount Measured (Total mg) Surrogate Recovery
Sample ID
WA45-73 4A-F
WA45-79 4B-F
WA45-85 4C-F
WA45-91 4D-F
WA45-97 5A-F
WA45-1035B-F
WA45-1095C-F
WA45-1155D-Fa
WA45-281 FB1A-F
WA45-287FB1B-F
WA45-293FB1C-F
WA45-299FB1 D-F
WA45-305 FB2 A-F
WA45-311 FB2B-F
WA45-317FB2C-F
WA45-323 FB2 D-Fa
WA45-331 TB1-F
WA45-332 TB2-F
Unconnected
0.0370
0.0344
0.0572
0.0796
0.0507
0.0370
0.0572
0.062
0.132
0.144
0.140
0.129
0.133
0.135
0.131
0.127
0.0550
0.0556
Blank Corrected'
O.030
<0.030
< 0.030
< 0.030
< 0.030
< 0.030
< 0.030
< 0.030
0.0766
0.0887
0.0845
0.0738
0.0777
0.0797
0.0756
0.0720
0.0333
0.0339
( '°)
81
82
82
81
83
78
80
82
75
79
79
75
77
81
78
82
81
80
* Average of two injections
b Runs 4 and 5 were blank corrected by subtracting the field train blank results. The field train
blank results were blank corrected by substracting the field trip blank results. The field trip
blank results were blank corrected by substracting the laboratory method blank results.
-------
Table E-6. WA 45 Sample Train Results
Total Amount Acetonitrile (nig)
Run/Train
1A
IB
1C
ID
2A
2B
2C
2D
3A
3B
3C
3D
4A
4B
4C
4D
5A
Front Half
Rinse
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0.02a
<0.02a
<0.02"
<0.01
<0.02
Filter
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0.03c-g
<0.03c-g
<0.03C-B
<0.03c-g
<0.03c-g
Back Half
Rinse
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<0.03"
<0.03a
<0.03a
<0.03"
<0.03
First
Sorbent
65. 4a
69.2a
0.0390ef
0.0328e-f
67. 6f
69.8a-f
0.0337a-e-f
0.0427e-f
70.4f
77.6f
0.0509e-f
0.033 le-f
66.0b
65.6"
0.0342
0.0307a
70.0b
Second
Sorbent
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
5.96b
1.02b
0.0204
0.0217a
1.39"
Condensate
5.38d
4.23
<0.02
<0.02
3.02
1.12
<0.02
<0.02
3.47
2.41
<0.02
<0.02
<0.06a
<0.06a
<0.05a
<0.05
<0.06
Total
70.7
73.6
0.0390
0.0328
70.6
71.0
0.0337
0.0427
73.9
80.0
0.0509
0.0331
72.0
66.7
0.0546
0.0524
71.4
-------
Table E-6. WA 45 Sample Train Results (Continued)
Total Amount Acetonitrile (mg)
Run/Train
5C
5D
6A
6B
6C
6D
7A
7B
1C
ID
8A
8B
8C
8D
9A
9B
9C
9D
Front Half
Rinse
<0.02
<0.01
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Filter
<0.03c-g
<0.03c-g
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Back Half
Rinse
<0.03
<0.03
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
First
Sorbent
0.0243"
0.0253"
50.9af
59.6af
0.0495e-f
0.0466e-f
63.6a-f
74. 5f
0.0291ef
0.0256e-f
76. lf
58.1f
0.0201ef
0.03 lT-f
76.6f
47.0f-h
0.0243e-j
0.0206e
Second
Sorbent
0.0255"
0.0235"
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
Condensate
<0.05
<0.04
<0.01
<0.01
<0.01
<0.01
0.666
5.30
<0.02
<0.02
2.02
5.69
<0.02
<0.02
1.91
4.63
<0.03
<0.02
Total
0.0572
0.0488
50.9
59.6
0.0495
0.0466
64.2
79.8
0.0291
0.0256
78.1
63.9
0.0201
0.0311
78.5
51.7
0.0243
0.0206
-------
Table E-6. WA 45 Sample Train Results (Continued)
Total Amount Acetonitrile (mg)
Run/Train
10A
10B
IOC
10D
Front Half
Rinse
NA
NA
NA
NA
Filter
NA
NA
NA
NA
Back Half
Rinse
NA
NA
NA
NA
First
Sorbent
ss. r
104f
0.0359e-f
0.0217e-f
Second
Sorbent
NU
NU
NU
NU
Condensate
10.6
5.01
<0.02
<0.02
Total
96.3
109
0.0359
0.0217
NA = Not Analyzed
NU = Not Used
'Initial system blank outside quality control limit of < 1/5 lowest standard
bReplicate injection outside quality control limit of ± 10 percent
c Initial system blank and final calibration check standard outside QC limits
d Surrogate recovery low (73%)
e Estimated values based on extrapolation of data past lowest standard.
f Surrogate recoveries were high. Stock surrogate was probably spiked. Surrogate recoveries were corrected.
g Filter extracts were corrected by subracting the acetonitrile detected in the field train blank filter extracts.
h Surrogate recovery was low after correction (43%)
' Surrogate recovery was high (158%)
-------
Table E-7. WA 45 Spike Recoveries
Run
1
2
3
4
5
6
7
8
9
10
Acetonitrile Recovery* I
Train A
105
89.3
95.6
99.2
101
73.8
83.9
109
103
109
(%)
Train B
111
100
114
97.2
104
108
114
87.6
74.9
119
"Spike Recovery = (100)(Amount Recovered in Train)/(Amount Spiked)
-------
Table E-8. Breakthrough Analysis for the Double Sorbent Trains
Run/Train
4A
4B
4C
4D
5A
5B
5C
5D
Spiked Train
Spiked Train
Spiked Train
Spiked Train
Spiked Train
Amount
First Sorbent Trap
66. Ob
65. 6b
0.0342
0.0307C
70. Ob
73. 4b
0.0243C
0.0253C
Average
Standard Deviation
Relative Standard Deviation
Maximum
Minimum
(Total mg)
Second Sorbent Trap
5.96"
1.02b
0.0204
0.0217C
1.39"
1.74b
0.0255C
0.0235C
(%)
Unspiked Train Average
"Breakthrough
Breakthrough" (%)
8.28
1.53
37.4
41.4
1.95
2.32
51.2
48.2
3.52
3.19
90.6
8.28
1.53
44.5
= 100( Amount in Second Sorbent Trap1)
(Total in Both Sorbent Traps)
bReplicate injection outside quality control limit of ±10 percent
Initial system blank outside quality control limit of
-------
Table E-9.
Breakthrough Analysis for the Single Sorbent Trains
Run/Train
1A
IB
1C
ID
2A
2B
2C
2D
3A
3B
3C
3D
6A
6B
6C
6D
7A
7B
7C
7D
8A
8B
8C
8D
9A
9B
Amount
Sorbent
65. 4a
69.2a
0.0390c-d
0.0328c'd
67. 6d
69.8a-d
0.0337a-c'd
0.0427c'd
70.4
77.6
0.0509c'd
0.0331c-d
50.9a-d
59.6a'd
0.0495c-d
0.0466c'd
63.6a'd
74.5d
0.0291c-d
0.0256c-d
76.1d
58.1"
0.0201c-d
0.031 lc-d
76.6d
47.0d'c
(Total mg)
Condensate
5.38"
4.23
<0.02
<0.02
3.02
1.12
<0.02
<0.02
3.47
2.41
<0.02
<0.02
<0.01
<0.01
<0.01
<0.01
0.666
5.30
<0.02
<0.02
2.02
5.69
<0.02
<0.02
1.91
4.63
Breakthrough
(%)
7.60%
5.76%
0.00%
0.00%
4.28%
1.58%
0.00%
0.00%
4.70%
3.01%
0.00%
0.00%
0.00%
0.00%
0.00%
0.00%
1.04%
6.64%
0.00%
0.00%
2.59%
8.92%
0.00%
0.00%
2.43%
8.97%
-------
Table E-9. (Continued)
Breakthrough Analysis for the Single Sorbent Trains
Amount (Total mg)
Run/Train Sorbent
9C 0.0243c-f
9D 0.0206C
10A 85.7"
10B 104d
IOC 0.0359c'd
10D 0.0217c-d
Spiked Train Average
Spiked Train Standard Deviation
Condensate
<0.03
<0.02
10.6
5.01
<0.02
<0.02
Spiked Train Relative Standard Deviation (%)
Spiked Train Maximum
Spiked Train Minimum
Unspiked Train Average
Breakthrough
(%)
0.00%
0.00%
11.01%
4.60%
0.00%
0.00%
4.57%
3.36%
73.40%
11.01%
0.00%
0.00%
NA = Not Analyzed
NU = Not Used
"Initial system blank outside quality control limit of < 1/5 lowest standard.
Surrogate recovery low (73%).
'Estimated values based on extrapolation of data past lowest standard.
""Surrogate recoveries were high. Stock surrogate was probably spiked. Surrogate recoveries
were corrected.
'surrogate recovery was low after correction.
Surrogate recovery was high.
-------
TOTAL VERSUS SORBENT RECOVERY
120%
LLJ
CO
o:
§100%
CO
on
O
O
LLJ
o:
90%
80%
70%
60%
70%
80% 90% 100% 110%
TOTAL ACETONITRILE RECOVERED
120%
Figure E-1. Total Acetonitrile Recovery Versus Recovery in the First Sorbent Module
-------
Total Recovery Versus Breakthrough
12%
10%
O)
o 8%
OJ
2
CO
0)
6%
I 4%
0)
2%
0%
70%
80%
90% 100%
Total Acetonitrile Recovered
110%
120%
Figure E-2. Total Acetonitrile Recovery Versus Percent Breakthrough the First Sorbent Module
-------
SORBENT RECOVERY VERSUS BREAKTHROUG
12%
o
a:
8%
§56%
LLJ
_J
o:
1=4%
O
LJU
< °
0%
60% 70%
80% 90% 100%
SORBENT RECOVERY
110% 120%
Figure E-3. Acetonitrile Recovery in the First Sorbent Versus Percent Breakthrough
-------
Effect of Gas Sample Volume
120%
110%
100%
4-1
c
o 90%
-------
Effect of Gas Sample Volume
0)
Q_
12%
10%
8%
*
>6%
4%
2%
0%
0.85
0.90 0.95 1.00
VOLUME SAMPLED (cubic meters)
1.05
BREAKTHROUGH
Figure E-5. Effect of Volume Sampled on Acetonitrile Breakthrough
-------
Effect of Condensed Moisture
120%
110%
100%
o 90%
-------
Effect of Condensed Moisture
12%
160 180
200 220 240 260 280
Condensed Moisture (grams)
300 320
BREAKTHROUGH
Figure E--7. Effect of Moisture Collected on Acetonitrile Breakthrough
-------
APPENDIX F
Quality Control
Results
-------
Table F-l.
Leak Rates
Run
1A
IB
1C
ID
2A
2B
2C
2D
3A
3B
3C
3D
4A
4B
4C
4D
5A
5B
5C
5D
6A
6B
6C
6D
Pretest
Leak Rate
(mVmin)
0.00020
0.00020
0.00040
0.00014
0.00008
0.00025
0.00042
0.00028
0.00040
0.00014
0.00042
0.00031
0.00028
0.00028
0.00037
0.00040
0.00023
0.00034
0.00037
0.00040
0.00017
0.00034
0.00037
0.00031
Vacuum
(mm Hg)
381
381
381
381
254
254
305
254
254
305
381
330
279
381
381
381
381
381
432
381
330
381
356
356
Post-Test
Leak Rate
(mVmin)
0.00023
0.00017
0.00031
0.00020
0.00014
0.00020
0.00034
0.00025
0.00042
0.00017
0.00025
0.00017
0.00025
0.00034
0.00042
0.00045
0.00020
0.00042
0.00028
0.00025
0.0001 1
0.00014
0.00025
0.00040
Vacuum
(mm Hg)
305
254
254
229
305
229
229
254
254
203
305
254
254
457
381
305
381
432
381
356
254
254
254
381
-------
Table F-l. (Continued)
Leak Rates
Run
7A
7B
7C
7D
8A
8B
8C
8D
9A
9B
9C
9D
10A
10B
IOC
10D
Pretest
Leak Rate
(m3/min)
0.00020
0.00031
0.00037
0.00025
0.00020
0.00020
0.00040
0.00020
0.00031
0.00020
0.00045
0.00020
0.00011
0.00028
0.00020
0.00017
Vacuum
(mm Hg)
305
254
381
305
254-
254
305
305
381
254
381
305
254
330
305
254
Post-Test
Leak Rate
(m'/min)
0.0001 1
0.00025
0.00031
0.00020
0.00048
0.00031
0.00034
0.00023
0.00020
0.00025
0.00031
0.00017
0.00014
0.00017
0.00037
0.00014
Vacuum
(mm Hg)
305
254
254
305
305
254
305
203
305
381
381
356
254
229
305
229
-------
Table F-2. Gas Chromatography/Flame lonization Detection Calibration
Data
Compound
Acetonitrile
Propionitrile
Solvent
Methanol'
Methylene
chlorideb
Methylene
chloride0
Methanol"
Methylene
chlorideb
Methylene
chloride0
Slope
1.91E-07
2.19E-07
2.08E-06
1.42E-07
1.61E-07
1.56E-06
Intercept
-1.42E-03
1.56E-04
-3.61 E-04
-3.38E-05
-3.22E-05
-5.23E-04
Correlation
Coefficient
0.99833
0.99967
0.99946
0.99893
0.99952
0.99967
Meets
Acceptance
Criteria
Yes
Yes
Yes
Yes
Yes
Yes
Concentration (mg/mL) = Area x Slope + Intercept
"Curve used for all condensate samples and rinses
bCurve used for all sorbent extract samples except for Trains 4A, 4B, 5A and 5B.
°Curve used for sorbent extracts from Trains 4A, 4B, 5A, and 5B.
-------
Table F-3. Calibration Check Standard Recoveries
Standard
Concentration
(mg/mL) File
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.090
0.04264
0.04264
0.04264
0.04264
0.04264
c6fd002.
c6fd016.
c6fd030.
c6fd044.
c6fe002.
c6fe016b.
c6fe030.
c6fe044.
c6ff002.
c6ff016.
c6ff031.
c6ff046.
c6fg014.
c6fg015.
c6fg016.
c6fg033.
c6fg049.
c6fj002a
c6fj002b
c6fj016
c6fj031
c6fk002.
c6fk016.
s6fw001.
s6fw014.
s6fw027.
s6fw028a.
s6gf081.
s6gh010.
s6gh023.
s6gh036.
s6gh049.
Date
6/4/96
6/4/96
6/4/96
6/4/96
6/5/96
6/5/96
6/5/96
6/6/96
6/6/96
6/6/96
6/6/96
6/7/96
6/9/96
6/9/96
6/9/96
6/10/96
6/10/96
6/10/96
6/10/96
6/10/96
6/10/96
6/11/96
6/11/96
6/23/96
6/23/96
6/23/96
6/23/96
7/8/96
7/8/96
7/9/96
7/9/96
7/9/96
Time
09:19:00
13:56:00
18:35:00
23:12:00
10:25:00
15:36:00
20:14:00
00:50:00
09:29:00
14:06:00
19:06:00
00:03:00
18:38:00
18:58:00
19:17:00
00:49:00
06:14:00
09:43:00
11:20:00
15:53:00
20:45:00
09:40:00
14:12:00
07:56:00
12:41:00
16:53:00
18:32:00
18:32:00
22:46:00
03:14:00
07:29:00
11:44:00
Percent of
Sample Type Target
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Filter Data
Filter Data
Filter Data
Filter Data
Filter Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Trap Data
Condensate Data
Condensate Data
Condensate Data
Condensate Data
Condensate Data
106
93
91
88
96
98
105
103
95
107
109
104
98
102
94
84a
83a
97
99
100
112
89
85
90
96
83b
89
105
89
103
102
104
-------
Table F-3. Calibration Check Standard Recoveries (Continued)
Standard
Concentration
(mg/mL)
0.04264
0.04264
File
s6gh049.
s6eh074a
Date
7/9/96
7/10/96
Time
16:00:00
20:14:00
Sample Type
Condensate Data
Condensate Data
Percent of
Target
104
101
' Calibration check standard was outside quality control limit. Data was not analyzed because
the acetonitrile detected in the filters was below the lowest calibration standard and was less
than what was detected in the field train blanks. The affected data were flagged.
b Calibration check standard was immediately reanalyzed (after the system blank) and the
reanalyzed recovery fell within the quality control limits. The samples were not reanalyzed.
The affected data were not flagged.
-------
Table F-4. Replicate Injection Results
WA45-03
WA45-05
WA45-05
WA45-81
WA45-94
WA45-110
WA45-115
WA45-123
WA45-131
WA45-147
WA45-161
WA45-189
WA45-195
WA45-239
WA45-250
WA45-283
WA45-290
WA45-318
WA45-323
WA45-325
WA45.-403
Sample ID
Run 1 A Trap
Run 1 A Cond
Run 1 A Cond Reanal
Run 4 B Trap 1
Run 4 D BHR
Run 5 C FHR
Run 5 D F
Run 6 A Trap
Run 6 B Cond
Run 7A Trap
Run 7 C Cond
Run 8 D Trap
Run 9 A Trap
Run 10 D Cond
Probe Rinse B (4/25/96)
FBK1 A Trap
FBK1 B BHR
FBK2CFHR
FBK 2 D F
FBK2 D Trap
FBK1 B PR
Difference*
(%)
4.23
-4.13
-4.70
19.6C
ND
ND
-3.64"
-4.31f
ND
-14.9c-f
ND
-5.47
1.34
ND
ND
ND
ND
ND
-2.56C
ND
ND
Surrogate
Recovery1" (%)
85
96
97
100
78
80
81
53g
91
64g
91
51g
91g
96
78
86
94
98
83
64
85
ND = No acetonitrile detected in either injection.
" % Difference = Injection 2 - Injection 1
Injection 1
b Surrogate Recovery for Duplicate Injection
c Outside Quality Control Limits of ±10%
d Initial system blank and final calibration check standard outside QC limits
e Initial and final calibration check standards outside of QC limits
f Initial system blank was outside the QC limits
B Traps appeared to be spiked with stock surrogate, reported surrogate recoveries are corrected
-------
Table F-5. Replicate Sample Results
WA45-05
WA45-05
WA45-94
WA45-110
WA45-115
WA45-131
WA45-161
WA45-239
WA45-250
WA45-290
WA45-318
WA45-323
WA45-403
Sample ID
Run 1 A Cond
Run 1 A Cond Reanal
Run 4 D BHR
Run 5 C FHR
Run 5 D F
Run 6B Cond
Run 7 C Cond
Run 10 D Cond
Probe Rinse B (4/25/96)
FBK1 B BHR
FBK2 C FHR
FBK2DF
FBK1 R PR
Difference1
(%)
-5.36
-4.70
ND
ND
-3.14e
ND
ND
ND
ND
ND
ND
+3.34"
ND
Surrogate
Recovery1" (%)
95
97
92
77
83
89
94
97
81
92
89
81
8S
ND = No acetonitrile detected in either aliquot.
a % Difference
= Duplicate - [(Injection 1 + Injection
2)/2]
(Injection 1 + Injection 2)/2
b Surrogate Recovery for Duplicate Sample
c Initial system blank and final calibration check standard outside QC limits
d Initial and final calibration check standards outside of QC limits
-------
Table F-6. Matrix Spike and Matrix Spike Duplicate Results
Recovery"
Sample ID (%)
WA45-05 MS
WA45-05 MSD
WA45-73 MS
WA45-73 MSD
WA45-94 MS
WA45-94 MSD
WA45-110MS
WA45-110MSD
WA45-161 MS
WA45-161 MSD
WA45-239 MS
WA45-239 MSD
WA45-250 MS
WA45-250 MSD
WA45-318MS
WA45-318 MSD
WA45-403 MS
WA45-403 MSD
Run 1 A Cond
Run 1 A Cond
Run 4 A F
Run 4 A F
Run 4 D BHR
Run 4 D BHR
Run 5 C FHR
Run 5 C FHR
Run 7 C Cond
Run 7 C Cond
Run 10D Cond
Run 10D Cond
Probe Rinse B (4/25/96)
Probe Rinse B (4/25/96)
FBK2CFHR
FBK2 C FHR
FBK1 B PR
FRK1 B PR
111
109
82C
82C
53
74
70
70
109
105
106
108
69
72
71
69
72
70
Surrogate
Recovery1" (%)
89
98
83
82
92
91
88
82
92
102
96
95
90
85
90
75
81
85
' % Recovery = 100(MS/MSD Amount - Sample Amount)
Spike Amount
b Surrogate Recovery for MS/MSD Sample
c Initial and final calibration check standards outside of QC limits
Quality Control Limits of ±50%
-------
Table F-7.
W A 45 Field Train Blank Results
Sample
Field Train Blank 1 A
WA45-402
(FBK1 PR A)
WA45-282
(FBK1 A FHR)
WA45-281 (F)
WA45-284
(FBK1 A BHR)
WA45-283
(FBK1 A TRAP)
WA45-285
(FBK1 A COND)
Field Train Blank 1 B
WA45-403
(FBK1PRB)
WA45-288
(FBK1 B FHR)
WA45-287 (F)
WA45-290
(FBK1 B BHR)
WA45-289
(FBK1 B TRAP)
WA45-291
(FBK1 B COND)
Field Train Blank 1 C
WA45-404
(FBK1PRC)
WA45-294
Amount
Acetonitrile
(Total mg)
-------
Table F-7. (Continued)
\VA 45 Field Train Blank Results
Sample
WA45-293 (F)
WA45-296
(FBK1 CBHR)
WA45-295
(FBK1 C TRAP)
WA45-297
(FBK1 C COND)
Field Train Blank 1 D
WA45-405
(FBK1 PR D)
WA45-300
(FBK1DFHR)
WA45-299 (F)
WA45-302
(FBK1 DBHR)
WA45-301
(FBK1 DTRAP)
WA45-303
(FBK1 D COND)
Field Train Blank 2 A
WA45-406
(FBK2 PR A)
WA45-306
(FBK2 A FHR)
WA45-305 (F)
WA45-308
Amount
Acetonitrile
(Total me)
0.0845b
<0.03a
<0.01
<0.02a
0.02'
<0.02a
0.073 8b
O.04"
<0.01
<0.02a
<0.02
<0.02B
0.0777b
<0.03a
Surrogate
Recovery
(%)
79
92
87
89
82
83
75
87
57
88
83
85
77
90
(FBK2 A BHR)
-------
Table F-7. (Continued)
WA 45 Field Train Blank Results
Sample
WA45-307
(FBK2 A TRAP)
WA45-309
(FBK2 A COND)
Field Train Blank 2 B
WA45-407
(FBK2 PR B)
WA45-312
(FBK2 B FHR)
WA45-311 (F)
WA45-314
(FBK2 B BHR)
WA45-313
(FBK2 B TRAP)
WA45-315
(FBK2 BCOND)
Field Train Blank 2 C
WA45-408
(FBK2 PR C)
WA45-318
(FBK2 C FHR)
WA45-317(F)
WA45-320
(FBK2 C BHR)
WA45-319
(FBK2 C TRAP)
Amount Surrogate
Acetonitrile Recovery
(Total me) (%)
<0.01
<0.02a
<0.03
<0.04a
0.0797b
<0.05a
<0.01
<0.02a
<0.02
<0.02a
0.0756b
<0.03a
<0.01
55
90
90
86
81
90
60
94
78
92
73
91
52
-------
Table F-7. (Continued)
WA 45 Field Train Blank Results
Amount Surrogate
Acetonitrile Recovery
Sample (Total mg) (%)
WA45-321 <0.03 89
(FBK2 C COND)
Field Train Blank 2 D
WA45-409 <0.02 90
(FBK2 PR D)
WA45-324 <0.02 82
(FBK2 D FHR)
WA45-323 (F) 0.0720b 82
WA45-326 <0.04 86
(FBK2 D BHR)
WA45-325 <0.01 65
(FBK2 D TRAP)
WA45-327 (FBK O.03 83
2 D COND)
Detection Limit = (l/5)(lowest standard concentration)(total sample volume)
"Twenty samples were analyzed between second source calibration check standards.
b Sample results were corrected by subtracting the field trip blank results.
The trap broke during shipment to the laboratory. The contents were emptied into another
sorbent module and extracted.
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Table F-8. WA 45 Field Reagent and Field Trip Blank Results
Sample
Sorbent Trip Blanks
WA45-329 (ACN-TB1)
WA45-330 (ACN-TB2)
Filter Trip Blanks
WA45-331
WA45-332
Water Reagent Blanks
WA45-343 (RBI H20)
WA45-344 (RB2 H20)
Methanol Reagent Blanks
WA45-340 (RBI MeOH)
WA45-341 (RB2 MeOH)
DCM Reagent Blanks
WA45-337 (RBl-MeCl2)
WA45-338 (RB2-MeCl2)
Detection Limit = (l/5)(lowest standard
Amount
Acetonitrile
(Total mg)
<0.01
0.0435
0.0333"
0.03393
<0.03
<0.03
<0.03
<0.03
<0.12
<0.08
concentration)(total sample volume)
Surrogate
Recovery
(%)
55
47"
81
80
91
90
80
98
80
81
"Samples were blank corrected by substracting the laboratory method blank results.
bOutside quality control limits of 50 to 150%.
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TECHNICAL REPORT DATA
1. REPORT NO.
600/R-97/140 .
4. TITLE AND SUBTITLE
Acetonitrile Field Test
5.REPORT DATE
October 1997
6.PERFORMING ORGANIZATION CODE
7. AUTHOR (S)
Joette L. Steger and Joan T. Bursey
8.PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Eastern Research Group
P.O. Box 2010
Morrisville, NC 27560-2010
10.PROGRAM ELEMENT NO.
23 E3428
11. CONTRACT/GRANT NO.
68-D4-0022
12. SPONSORING AGENCY NAME AND ADDRESS
National Exposure Research Laboratory
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
13.TYPE OF REPORT AND PERIOD COVERED
Research, 2/21/96-9/30/96
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
Field experiments were conducted at a hazardous waste incinerator. The ability of a specially-
designed sampling train to quantitatively collect acetonitrile was evaluated. Ten quadruple runs were
conducted. Each run consisted of four acetonitrile sampling trains sampling simultaneously. The
sampling and analytical methods were evaluated using Method 301 ("Protocol for the Field Validation of
Emission Concentrations from Stationary Sources") statistical procedures.
The acetonitrile sampling train was based on the Method 0010 train which collects semivolatile
compounds on Amberlite XAD-2* sorbent. The Method 0010 train was modified by replacing the Amberlite
XAD-2* with Carboxenw-1000. Forty-eight grams of 45/60 mesh Carboxen"-1000 was used. Carboxen""-1000 is
a spherical carbon molecular sieve with an average pore diameter of 70 angstroms and a surface area
greater than 1200 square meters per gram.
The acetonitrile sampling train was evaluated in the field to demonstrate its ability to
determine acetonitrile in the gaseous waste stream from a hazardous waste incinerator. Two of the
quadruple trains were dynamically spiked with an aqueous solution of acetonitrile. Method 301
statistical analysis was performed. The mean recovery for the 20 spiked trains was 100*. The relative
standard deviation in the measured acetonitrile for the 20 spiked trains was 13%. The relative standard
deviation for the 20 unspiked trains was 17*. Both relative standard deviations were therefore within
the Method 301 criteria of <50*. The calculated bias was insignificant; therefore, a bias correction
factor was not needed.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
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328
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