DETERMINATION OF VOLATILE ORGANIC COMPOUNDS
IN SOILS USING EQUILIBRIUM HEADSPACE ANALYSIS AND
CAPILLARY COLUMN GAS CHROMATOGRAPHY/NASS SPECTROMETRY
EVALUATION OF THE TEKMAR 7000 HA ANALYZER
Pedro Flores
Thomas A. Bellar
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Environmental Monitoring Systems
Laboratory — Cincinnati, U.S. Environmental Protection Agency, and approved for
publication. Mention of trade names or commercial products does not constitute
endorsement or recommendation of use.
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FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of waste effluents. The Environmental
Monitoring Systems Laboratory — Cincinnati (EMSL—Cincinnati) conducts research
to:
o Develop and evaluate analytical methods to identify and measure
the concentration of chemical pollutants in drinking waters,
surface waters, groundwaters, wastewaters, sediments, sludges, and
solid wastes.
o Investigate methods for the identification and measurement of
viruses, bacteria and other microbiological organisms in aqueous
samples and to determine the responses of aquatic organisms to
water quality.
o Develop and operate a quality assurance program to support the
achievement of data quality objectives in measurements of
pollutants in drinking water, surface water, groundwater,
wastewater, sediment and solid waste.
o Develop methods and models to detect and quantify responses in
aquatic and terrestrial organisms exposed to environmental
stressors and to correlate the exposure with effects on chemical
and virological indicators.
This report, “Determination of Volatile Organic Compounds In Soils Using
Equilibrium Headspace Analysis and Capillary Column Gas Chromatography!
Mass Spectronietry,’ 1 presents methodology which is more accurate and precise in
determining volatile organics in soils than any existing methodology. It
addresses several problems including preserving the integrity of the sample
from collection to analysis, and efficiently extracting a broad spectrum of
volatile compounds. EMSL—Cincinnati is pleased to provide this report and
believes it will be of value to public and private laboratories involved in
soil analysis.
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ABSTRACT
Existing methods for determination of volatile organic compounds (VOCs)
in soil matrices using the purge and trap technique with gas chromatography/
mass spectrometry (GCIMS) have several problems, which include preserving
sample integrity from collection to analysis and efficiently extracting a
broad spectrum of VOCs from the soil matrix. This investigation was
undertaken using the Tekinar 7000 headspace autosampler to evaluate Its ability
to resolve these problems. The objective of this study was to optimize
analytical conditions and then to study the efficiency of the headspace
technique to extract VOCs from soils. Variations of sample preparation
procedures were studied, and method analytes were identified and measured
using internal standard calibration GC/MS. Using these data, relative
standard deviations and percent recoveries are reported for 59 analytes in
four different types of soil matrices: sand, clay, garden soil, and hazardous
waste landfill soil. The most accurate and precise results are obtained with
sand. Method detection limits (MDLs), ranging from 0.2 to 7.9 pg/kg, were
calculated for all analytes (Table 47), using results of replicate analyses of
sand, the matrix that had the least matrix effect. It is concluded that the
7000—HA headspace analyzer can be used to determine VOCs in soils.
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Disclaimer
Foreword
Abstract
Introduction
Conclusion
Recommendations
Materials and Conditions
Experimental Procedures
Results and Discussion
References
Table 1 Molecular Weights and Characteristic Ions
Table 2 Determination of Autosampler Precision 25 ng Analyte
Response In Reagent Water
Table 3 Evaluation of the Matrix Modifying Solution 25 ng Analyte
Response in Sodium Sulfate Solution
Table 4 Evaluation of the Matrix Modifying Solution 25 ng Analyte
Response in Calcium Chloride Solution
Table 5 Verification of Fortifying Procedure 25 ng Analyte
Response in Sand
Table 6 25 ng Analyte Response in Reagent Water
Table 7 25 ng Analyte Response in the MMS Solution .
Table 8 25 ng Analyte Response in Water/Sand
Table 9 25 ng Analyte Response in MMS/Sand
Table 10 Comparison of Four Fortified Matrices
Table 1125 ng Analyte Response in MMS/Sand
Table 1225 ng Analyte Response in MMS/Clay
Table 13 25 ng Analyte Response in MMS/Garden Soil .
Table 14 25 ng Analyte Response in MMS/Horizon—C Soil
Table 15 Relative Analyte Recoveries for Four Matrices
Table 16 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Fluorobenzene .
Table 17 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Fluorobenzene .
Table 18 Determination of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard Fluorobenzene
Table 19 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Benzene—d6
Table 20 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Benzene—d6
Table 21 Determination of Percent Recovery 25 ng Fortified
tillS/Garden Soil Internal Standard Benzene—d6
Table 22 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Toluene—d8
Table 23 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Toluene—d8
Table 24 Determination of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard Toluene-d8
Table 25 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Chloroform-d . .
CONTENTS
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• • • 35
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CONTENTS (Continued)
Table 26 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Chloroform—d 36
Table 27 Determination of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard Chloroform—d 37
Table 28 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Bromochloromethane—d2 38
Table 29 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Bromochloromethane-d2 39
Table 30 Determination of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard
Bromochloromethane—d2 40
Table 31 Determination of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard Bromobenzene—d5 41
Table 32 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard Bromobenzene—d5 . 42
Table 33 DeterminatIon of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard Bromobenzene--d5 . . . . 43
Table 34 DeterminatIon of Percent Recovery 25 ng Fortified
MMS/Sand Internal Standard 2—Bromo—1—Chloropropane—d6 . . 44
Table 35 Determination of Percent Recovery 25 ng Fortified
MMS/Clay Internal Standard 2—Bromo—1—Chloropropane—d6 . . 45
Table 36 Determination of Percent Recovery 25 ng Fortified
MMS/Garden Soil Internal Standard
2—Bromo—1—chloropropane—d6 46
Table 37 Evaluation of Analyte Recoveries in Garden Soil
Using Multiple Internal Standard 47
Table 38 Difference Headspace Volume Recoveries 25 ng -
Analyte Response Using 10 mL of MMS Vial -
Pressure 7.5 PSI 48
Table 39 Different Fleadspace Volume Recoveries 25 ng
Analyte Response Using 10 mL MMS and 5 mL
Glass Beads Vial Pressure 7.5 PSI 49
Table 40 Different Headspace Volume Recoveries 25 ng
Analyte Response Using 10 mL of MMS and
10 mL of Glass Beads Vial Pressure 7.5 PSI . . 50
Table 41 Different Headspace Volume Recoveries 25 ng
Analyte Response Usihg 10 niL of MMS and
15 mL Glass Beads Vial Pressure 7.5 PSI 51
Table 42 Comparison of Headspace Volume Recoveries
Three Replicates of Each Experiment Vial
Pressure 7.5 PSI 52
Table 43 Different MMS Amounts at Constant Headspace
Volume 25 ng Analyte Response Using 10 mL
of MMS Vial Pressure 7.5 PSI 53
Table 44 Different MMS Amounts at Constant Headspace
Volume 25 ng Analyte Response Using 7.2 mL
of MMS and 5 mL of the Beads Vial Pressure 7.5 PSI . . . . 54
Table 45 Different MMS Amounts at Constant Headspace
Volume 25 ng Analyte Response Using 4.5 ml
of MMS and 10 niL of the Beads Vial Pressure 7.5 PSI . . . 55
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CONTENTS (Continued)
Table 46 Comparison of 25 ng Analyte Recoveries for
Different MMS Amounts at Constant Headspace
Volume Vial Pressure 7.5 PSI . 56
Table 47 Determination of MDLs 25 ng Fortified tillS/Sand . . 57
Figure 1 Effect of Different Headspace Volumes on
Analyte Recovery . . 58
Figure 2 Effect of Different MMS Volume on Analyte
Recovery of Six Compounds . . 59
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DETERMINATION OF VOLATILE ORGANIC COMPOUNDS
IN SOILS USING EQUILIBRIUM HEADSPACE ANALYSIS AND
CAPILLARY COLUMN GAS CHROMATOGRAPHY/MASS SPECTROMETRY
INTRODUCTION
An accurate and precise procedure is needed to effectively remove
volatile organic compounds (VOCs) from soils for Identification and
measurement using gas chromatography/mass spectrometry (GC/MS). Ten years
ago, the number of VOCs that could be determined by GC/MS was limited by
packed column GC technology. The least volatile compounds included toluene
and ethyl benzene. Currently, with capillary column capabilities, the scope
of VOCs in aqueous samples has been expanded for a single column analysis to
include non—polar compounds with boiling points ranging from —30°C to >220°C.
Heated purge and trap methodology has also been applied to soil samples
utilizing capillary column technology (1). The results illustrated that many
compounds currently determined in water matrices can be included in the list
of compounds determined in soil matrices. However, the method was subjected
to matrix effects, particularly for those compounds with high boiling points.
In this work, we evaluated the capability of the Tekmar 7000 Headspace
Autosampler (7000—HA) to effectively introduce VOCs partitioned from soil
matrices Into a fused silica capillary column using the static headspace
technique. The integral features of the procedure evaluated include sample
fortification, different 7000—HA extraction parameters for a wide variety of
volatile compounds, and the quantitative capabilities of the method using
different soil matrices and different internal standards.
The 7000—HA was chosen for evaluation because of its potential to
include the VOCs contained in the headspace of the sample collection vials and
extract VOCs from a soil into the gas volume above the sample, as well as its
ability to permit analysis with a minimal amount of sample preparation. The
analytes used for the evaluation and their characteristic Ions are listed in
Table 1. The results of this evaluation are discussed in the following
sections of this report.
CONCLUS IONS
The’ following conclusions were made from evaluation of study results.
1. The accuracy and precision of the 7000—HA were acceptable when
used to determine VOCs in water, the matrix modifying solution
(MMS), and sand. The 7000—HA produced somewhat lower recoveries
from other tested soil matrices. However, these lower recoveries
were not due to inefficient headspace analysis, but tostronger
adsorption capacity of soil. This is the matrix effect. The
results obtained with the 7000—HA are equivalent or better than
current methodology for volatiles in soil.
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2. The matrix fortifying procedure was found to be reproducible for
all the compounds evaluated.
3. Comparing recoveries obtained in the different experiments for
different matrices, indicated a definite matrix effect.
4. In an attempt to correct for the matrix effect, seven internal
standards were evaluated. Results suggest that the use of one
internal standard improved data quality but did not completely
overcome the matrix effect problem. Adding additional internal
standards with chemical and physical properties similar to those
of the problem compounds helped resolve this problem.
5. The less volatile compounds, such as trichlorobenzenes, did not
appear to be good candidates for accurate measurement using the
headspace technique with a single internal standard.
6. Headspace volume had a definite effect on the sensitivity of the
method. When headspace volume is decreased, sensitivity
increases. This effect is greater as the volatility of the
compound decreases.
7. The amount of the matrix modifying solution added to the matrix
had little effect on analyte recovery. The percent difference
between experiments was within the experimental error.
8. This work pointed out the definite need to develop a mechanism to
collect an exact predetermined sample size and establish the
hermetic seal In the field. Until this is done, this method
cannot be used to its fullest potential.
RECOMMENDATIONS
The linear dynamic range of this method extends from the MDL of each
analyte to approximately 1000 x the MDL. Because vial contents cannot be
diluted or sub—sampled after the vial is sealed without losing headspace, for
high concentration samples multiple static headspace analysis techniques (2)
should be investigated to complement the single headspace evaluations reported
here. The 7000—HA has the capacity to perform this type of analysis, and
further investigation is encouraged. Moreover, work must continue on
developing multiple internal standard methods to correct for matrix effects in
soil.
MATERIALS AND CONDITIONS
Apparatus and Equipment
Tekmar 7000 Equilibrium Headspace Autosampler and Tekmar 7050 Carousel
(Tekmar Company, 7143 East Road Cincinnati, OH 45249).
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Soil vials — 20-mL clear Tekmar vials with crimp—seal open—toD septum
cap (14—4440—024).
Gas Chromato ra h — Carlo Erba HRGC Mega Series (Carlo Erba Instruments,
123 McClellan Dr., Pittsburgh, PA 15236) equipped with cryogenic cooling
capable of maintaining subambient temperatures.
GC Column — J&W Scientific, DB—624, Megabore, fused silica, 3 pm
thickness, 0.53 mm ID, 75 m length.
Mass Snectrometer — Finnigan MAT Ion Trap Detector 700, updated to 800
series (Finnigan MAT, 355 River Oaks Parkway, San Jose, CA 95134) equipped
with an open split Interface.
Reagents
Methyl alcohol, sodium sulfate (Na 2 SO 4 ), sodium phosphate dibasic
(Na 2 HPO 4 ), potassium phosphate monobasic (KH 2 PO 4 ), calcium chloride (CaC1 2 ) and
phosphoric acid (H 3 P0 4 ) — ACS Reagent Grade
Standards
Standard materials were obtained In flame sealed ampules containing 150,
1000, 2000, 5000 or 10000 pg of pure compound per ml of methanol from Supelco,
Inc., Supelco Park, Bellefonte, PA 16823—0048 or NSI Environmental Solutions,
Research Triangle Park, NC 27709.
Reagent Water
Reagent water was generated using a Standard 4—Bowl Milli—Q System
including an Organex Cartridge (Millipore Corp., 34 Maple St.,
Milford, MA 01757).
Matrix Modifying Solution (MMS)
The MMS was prepared by adding 120 g of Na 2 SO 4 , 0.75 g of Na 2 HPO 4 , and
4.8 g of KH 2 PO 4 to 300 ml of pH 2 reagent water wliich was prepared by adding
phosphoric acid to reagent water until a pH of 2 was measured by a pH meter.
Samples
Inert Sand — Approximately 30 mesh sand, rinsed with reagent water and
allowed to air dry.
Clay — Soil obtained from a shallow excavation at the EPA facilities in
Cincinnati was used as collected without any processing.
Garden Soil — Top soil obtained from Springdale, OH, and air dried.
Horizon—C Soil — An integrated core sample, primarily clay, collected
between 5 and 10 feet below the surface uphill from a hazardous waste
landfill, used as collected without further processing.
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Gas Chromatographic Conditions
The helium gas flow was adjusted to 9.6 mL/min. The column temperature
program was started at 25°C, held for 8 mm from injection, ramped to 200°C at
10°C/mm, and then held for 10 mm. Each total analyses time was
approximately 35 mm.
Plass Spectrometer Conditions
The ion trap detector (ITO) was scanned from 49 to 300 amu each second
with 6 inicroscans per scan. The electron multiplier voltage was varied from
1550 to 2050 volts depending on lTD tuning. The transfer line between the gas
chromatograph and the LTD was maintained at 250°C, the open—split interface
and the exit nozzle approximately 240°C and the trap manifold approximately
220°C. The characteristic ions used are listed in Table 1.
EXPERIMENTAL PROCEDURES
Each sample was prepared by adding 5.0 g of a soil matrix to a 20—mL
7000—HA crimp—seal glass headspace vial. In rapid succession, each soil
sample was fortified with the target analytes in methanol, the matrix modifier
solution (MMS) was added, and the vial was sealed. The purpose of the matrix
modifier solution was to increase the efficiency of the headspace analysis by
providing a salting—out effect and to minimize dehydrohalogenation reactions
through pH adjustment (2). The vials were placed in the autosampler carousel
and maintained at room temperature. Approximately 1 h prior to analysis, the
individual vials were moved to a heating zone and allowed to equilibrate for
50 mm at 85°C. The sample was then mixed by mechanical vibration for 8 mm
while the temperature was maintained at 85°C. The autosampler then raised the
vial causing a stationary needle to puncture the septum and pressurize the
vial with helium at 7.5 psi. The vial was allowed to pressure equilibrate for
a 0.10 mm to ensure complete mixing of the pressurization gas with the vial
headspace. The pressurized headspace was then vented through a 2 ml sample
loop to the atmosphere for 15 sec. In this manner, a representative volume of
headspace was isolated within the ioop. Finally the carrier gas, at a flow
rate of 9.5 mL/min, backflushed the sample loop, sweeping the sample through
the heated transfer line into the GC/MS system for separation, identification,
and measurement of the method analytes.
Precision of the Tek,nar 7000 Headspace Autosampler
To determine the precision of the Tekmar 7000 HA, the following
experiment was performed.
All operational parameters on the headspace analyzer were set within
manufacturer’s recommendations. Six 1O—mL reagent water samples in 20—mL
glass vials were sequentially adjusted to pH 2 with 85% phosphoric acid,
fortified with 5 4 uj.. of a 5 ng/jiL solution containing all analytes in Table 2,
and sealed. This aqueous standard preparation procedure has been demonstrated
to be accurate and precise for purge and trap methods (3). The vials were
placed in the 7000—HA and automatically submitted to the entire analytical
procedure. After each analysis, analyte peak integration areas were recorded
to determine precision.
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Preliminary work demonstrated that significant losses of the halogenated
alkanes occurred during sample equilibration periods when the pH was
maintained at 7 (1). These losses were due to dehydrohalogenation reactions
which occur readily at elevated temperatures with haloalkanes at a pH of 7 or
higher. Further results showed that these losses were avoided when the sample
pH was reduced to 2. Therefore, all matrices studied in this work were
adjusted to a pH of 2.
Selection of the Matrix Modified Solution
Two experiments were performed to determine an appropriate matrix
modifier solution which Is a salt solution that would help optimize accuracy
and precision of test compound determinations in a variety of soils. The
first MIIS contained an acidified saturated solution of Na 2 SO 4 and the second
contained an acidified saturated solution of CaCL 2 . Ten mL of the MMS were
added to vials, each fortified with 5 p1 of a solution of 5 ng/pL of analytes
in Table 3, sealed and submitted to the experimental procedure. These
experiments were carried out in an attempt to shift the equilibrium of the
analytes to the gas phase in order to improve sensitivity without sacrificing
precision and to determine If the MMS can be fortified and sealed before
losses occur. Addition of the MMS will also compensate for the varying salt
content that may be encountered in solid samples.
Verification of the Fortifying Procedure
To verify reproducible fortification of solid samples, five 5.0 g
portions of sand were placed Into individual vials. Each was then fortified
with 5 pL of a 5 ng/ uL solution containing the analytes, and followed by the
addition of the selected MMS, Na 2 SO 4 . The Na 2 SO 4 MMS was chosen because it
showed the better performance (see results). The vials were sealed, placed in
the 7000—HA and submitted to the analysis as previously described. Sand was
chosen over other solid matrices because it was believed that shifts of
equilibrium of the volatile analytes to the gas phase should be higher in this
relatively low surface area matrix.
Assessment of Analyte Recoveries Using the Matrix Modifying Solution
These experiments were performed to measure the increase in analyte
recoveries, based on analyte absolute integrated peak areas, when the MMS was
added to the same matrix. Experiments were carried out comparing recoveries
from the different matrices using a constant headspace volume. Five 10 mL
reagent water samples in individual vials at pH 2 were fortified with 5 pL of
a 5 ng/pL solution containing all the method analytes. They were sealed
immediately, and submitted to the analysis previously described.
Five 10 mL pH 2 Na 2 SO 4 MMS samples in individual vials were fortified
with 5 p1 of a 5 ng/pL solution containing all the method analytes, and
sealed. The vials were submitted to the analysis previously described.
Five 5.0 g samples of sand were placed in individual vials, and
fortified as above. It was independently determined that 5 g of sand
displaces approximately 2 mL of water. Therefore, an 8.0 ml aliquot of pH 2
reagent water was added to each in order to maintain a constant headspace
volume for all samples in the experiment. The vials were sealed, and the
samples were analyzed as described.
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Four 5.0 g sample of sand were treated as above, this time adding 8.0 mL
of the MMS instead of water.
Analyte Recoveries From Various Soil Matrices
These experiments were carried out to compare analyte recovery, based on
analyte absolute integrated peak areas, when the MMS is added to different
types of soil matrices. Three 10—mL Na 2 SO 4 MMS samples were fortified in
vials with 5 p1 of the 5 ng/pL analyte fortification solution, sealed, and
analyzed as described. These samples were used as the control samples.
Three 5.0 g samples of sand, three 5.0 g samples of clay, three 5.0 g
samples of garden soil, and three 5.0 g samples of horizon—c soil were placed
In individual vials, fortified as above, 8—mL of Na 2 SO 4 MMS added and analyzed
as described previously.
Analyte Recoveries From Various Soil Matrices Utilizing Internal Standard
Cal i brati on
These experiments were carried out to determine the percent recoveries
of the method analytes from the different matrices using different internal
standards (IS). The ISs evaluated were: fluorobenzene, benzene—d6, toluene-
d8, chloroform—d, 2—bromo—1—chloropropane—d6, bromobenzene—d5 and
bromochl oromethane-d2.
Three individual 10—mL Na 2 SO 4 MMS samples were fortified with 5, 25 and
50 ng of each analyte and 25 ng of each IS. These standards were analyzed to
create a concentration calibration curve for each analyte. Three different
sets of three samples each were prepared using sand, clay and garden soil.
The horizon—c soil sample was discarded for this experiment because it was
contaminated with the test analytes. Each sample was fortified with 25 ng of
each analyte, 25 ng of each IS and 8—mLof the Na 2 SO 4 MMS. The vials were
sealed and submitted to the complete analysis. These samples were used to
calculate the percent recovery.
Different Headspace Volume Recovery Experiment
To evaluate the effect of the headspace volume on the method
sensitivity, the following experiments were performed.
Three 10 mL aliquots of MMS were fortified with 5 pL of a 5 ng/pL
solution containing each analyte. The vials were sealed and analyzed as
described previously.
To vary the headspace volume, three more vials were filled with 5 mL of
5 mm diameter glass beads (enough glass beads to fill a 5 mL graduated
cylinder) and 10 mL of MMS. These were fortified as described, sealed and
analyzed. In exactly the same manner, two additional experiments were carried
out, filling the v als with 10 mL of the Na 2 SO 4 MMS and 15 mL of the beads,
respectively.
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Different MMS Volume at Constant Headspace Volume Recovery Experiments
To determine if the MMS volume affected analyte recovery, three
experiments were carried out with constant headspace volume.
First, three 1O-mL MMS samples at pH 2 were fortified in vials with 5 pL
of the 5 ng/pL analyte fortification solution. The vials were immediately
sealed and analyzed as described above.
In a second experiment three vials were filled with 5 mL of the glass
beads described above. Then an exact volume of MMS was added to each vial so
that exactly the same headspace volume would be contained in all vials as
compared with the previous experiment. The samples were fortified as above,
sealed and submitted to the entire analysis procedure. A third experiment was
performed adding 1O—mL of glass beads instead of 5 ml and the Na 2 SO 4 MMS to
the vials.
RESULTS AND DISCUSSION
Precision of the Tekmar 7000 Headspace Autosampler
Six replicate samples of fortified reagent water acidified to pH 2 were
analyzed to determine the reproducibility of the 7000—HA. Reagent water was
used so that results from headspace analysis could be compared to those
obtained using standard purge and trap technology. This would demonstrate
whether the headspace analyzer methodology could generate data of equal
quality to current EPA methodology (3). Only one relative standard deviation
(RSD) of all listed in Table 2 was greater than 13%. These RSDs were
comparable to purge and trap methodology utilizing similar matrices (1,3).
Selection of the Matrix Modifier Solution
Results from the experiments to evaluate the use of a matrix modifier
solution to improve the precision and sensitivity of the headspace analysis
are listed in Tables 3 and 4. Saturated solutions of pH adjusted Na 2 SO 4 and
CaC1 2 were used in this study. The RSDs calculated from the analyte
integrated peak areas obtained with Na 2 SO 4 solution (Table 3) ranged from 2%
to 22% with a mean of 8%. The RSDs for the CaC1 2 solution (Table 4) ranged
from 4% to 66% with a mean of 13%, indicating that the Na 2 SO 4 solution was a
suitable matrix modifier solution. Comparison of the average areas in Tables
2, 3, and 4 indicated that addition of salt to a sample matrix significantly
improves recoveries of the higher boiling compounds. The poor recoveries and
precision associated with the CaC1 2 solution may indicate that volatility
losses were significant before the vials could be sealed when using the CaC1 2
MMS. At this point in the study, it was decided to discontinue the use of
CaC1 2 , and use only the Na 2 SO 4 solution as the modifier.
The data in Tables 2, 3, and 4 appear in the same chronological order as
the-analyses were carried out. The storage time for each successive sample
was approximately 60 mm or longer than its predecessor; therefore, if
dehydrohalogenation reactions were occurring, they should be apparent by the
systematic loss of the haloalkanes and the corresponding increase of the
alkenes. Comparison of the areas of the alkanes (tetrachioroethane, 1,1,1—
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trichioroethane, and 1,1—dichioroethane) most prone to dehydrohalogenation
reactions and their corresponding products (1,1,2—trichioroethene, 1,1
dichloroethene, and chioroethene) indicated that no reactions were occurring
which could significantly affect the quality of the data.
Verification of the Fortifying Procedure
Having established the precision capabilities of the 7000—HA when
analyzing a simple aqueous matrix, an experiment was carried out to evaluate
the precision of the soil matrix fortifying procedure. Results from the
analyses of five replicate samples were compared, and RSDs of the integrated
analyte peak areas were calculated. RSDs from this experiment (Table 5)
ranged from 3% to 13% with a mean of 8% for all analytes. The similarity of
these RSDs to those In Table 2 indicated acceptable precision and a
reproducible fortifying procedure.
Assessment of Analyte Recoveries Using the Matrix Modifying Solution
Experiments were performed to measure the increase In analyte
recoveries, comparing the analyte absolute integrated peak areas when the MMS
was added to the soil matrices. In these experiments, the headspace volume
was controlled by adjusting the volume of the liquid added to the vial.
Analyte peak areas from reagent water, Na 2 SO 4 MMS, water/sand, and MMS/sand
are presented in Tables 6, 7, 8 and 9, respectively. Table 10 compares the
data in the four previous tables. It indicates that the Na 2 SO 4 MMS was
successful in increasing the shift of the analytes to the gas phase, and
produced higher recoveries for almost all analytes when compared to the
recoveries from reagent water. In addition, when the recoveries from reagent
water/sand and the MMS/sand samples were compared recoveries increased with
addition of the MMS. Clearly, the matrix modifying solution will increase
analyte recoveries. The data in Tables 6 — 9 also indicate no significant
losses within experimental error due to dehydrohalogenation reactions.
When matrix modifier solution results were compared with MMS/sand
results analyte recoveries decreased slightly in the samples with sand. This
indicates some matrix effect from the sand and inhibits removal of the
analytes from that matrix.
Analyte Recoveries From Various Soil Matrices
These experiments were performed to compare analyte recoveries, based on
analyte absolute integrated peak areas, when the MMS is added to a variety of
matrices and to assess the degree of matrix effect caused by each matrix.
Four different kinds of soil were studied: sand, clay, garden soil, and
horizon—c soil. The results obtained from the fortified control solution (10
mL of MMS) were used to establish baseline recoveries. Tables 11, 12, 13, and
14 show those results obtained with sand, clay, garden soil, and horizon—c
soil, respectively. Table 15 summarizes the results showing the relative
percent recovery obtained from each matrix. This relative percent recovery
was obtained by dividing the peak area of each analyte in the soil samples by
the respective analyte peak area in the fortified MMS sample, and multiplying
by 100. High ratios are indicative of high recoveries. Analyte relative
percent recoveries were higher for sand samples, followed by horizon—c and
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clay samples, and finally garden soil samples. These data indicated that
serious matrix effects can be experienced from one sample type to another.
With fortified clay samples containing a high percentage of large particles
(i.e., 20 mesh) recovery and precision is better than with fortified clay
samples containing mainly fine particles (i.e., <20 mesh).
Analyte Recoveries From Various Soil Matrices Utilizing Internal Standard
Cal I brat i on
Seven different commonly used purge and trap internal standards (IS)
were tested with sand, clay, and garden soil matrices. Tables from 16 to 36
show the results based on internal standard calibration for each matrix.
It can be concluded by observing these tables of data that, regardless
of the internal standard compound evaluated, analyte recoveries were highest
for sand, the matrix demonstrating little or no matrix effects. For sand, the
average percent recoveries for the seven internal standards were all >80%,
except for bromobenzene—d5 at 74%. Fluorobenzene is the internal standard of
choice in other analytical methods (1,3) used to determine VOCs in other
matrices, and produced similar results in this method as the internal
standard.
The results of the experiment utilizing garden soil indicated matrix
effects could be minimized if internal standards that have similar chemical
and physical properties to the target compound are added to the sample prior
to extraction. Table 37 demonstrates the use of multiple internal standards
in garden soil. The internal standards benzene—d6, toluene—d8, and
bromobenzene—d5 were observed to enhance the recoveries of most of the
analytes to near 100%. Due to the volatile nature of chloroethane and the
reactivity of styrene and dichloroethene, the recoveries for these analytes
were low with all the internal standards. Bromobenzene—d5 produced low
recoveries for the dichioro and trichlorobenzenes; however, 1,2—
dichlorobenzene—d4 could be used to enhance the recoveries of these compounds
to near 100%. The background concentration of toluene in garden soil was well
in excess of the fortified concentration; thus even though the toluene
response was corrected for the background contamination, its recovery was
still in excess of 100%.
Different Headspace Volume Recovery Experiments
Results of the studies to assess the effect of the headspace volume on
the method sensitivity are listed in Tables 38, 39, 40, and 41. The volume of
headspace was varied by adding glass beads to the sample vials as discussed in
the experimental section. Table 42 summarizes the previous three tables.
For this method, headspace volume was controlled by the volume of the
vial, the volume of MMS and the volume of solids added to the vial. Both the
volume of the vial and the volume of the MMS added can be accurately
maintained in the analytical laboratory and in the field. However, it is
extremely difficult to accurately sample a constant volume of a solid,
especially considering that the longer the soil sample is exposed to the air
the more significant the errors become because of volatility losses. The data
in Table 42 indicates the magnitude of the error that may be encountered if
the volume of sample added to the vial is not held constant. If the method
9
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specified a volume of sample equivalent to 10 ml of glass beads (Table 43),
then the headspace volume would be 6.8 mL. Decreasing the headspace volume by
approximately 2.6 mL (Table 42, column 4) would Increase the recovery by an
average of 37%. In addition, Increasing the headspace volume by 2.6 mL (Table
42, column 2) would decrease the recovery by an average of 11%.
Figure 1 illustrates results obtained for selected compounds chosen to
represent the complete method analyte list. Figure 1 demonstrates that
decreasing the sample headspace volume, while maintaining a constant MMS
volume, will increase the concentration of the analyte In the gas phase, and
therefore Introduce error into the method if the headspace volume is not held
constant. Figure 1 also shows that the increase in response due to decreased
headspace volume Is much more pronounced for the less volatile compounds. The
samples containing the largest volume of glass beads and therefore the
smallest headspace volume showed proportionally higher recoveries for 1,3,5—
trlmethylbenzene than for dichiorodifluoromethane.
Different MMS Volume at Constant Headspace Volume Recovery Experiments
These experiments were performed to study the effect of varying the
volume of MMS on the recoveries of the analytes from the matrix. Tables 43,
44, and 45 show the results obtained using a different volume of MMS, and
table 46 summarizes them.
The responses of six selected compounds, in order of their increasing
boilup point are depicted in Figure 2. It appears that 7 ml of the MMS
produced the optimum response, however, ±3 niL on either side of the optimum
MMS volume has only a slight effect (average % difference of 12) on the
response of the selected compounds. -
The volume of the MMS added to the sample is not as determinant as the
headspace volume of It. This indicates that the 7000 HA will only work
consistently if sample sizes are collected the same and therefore the
headspace column kept constant.
REFERENCES
1. G. Plemmons—Ruesink, USEPA, Development and Validation of a Sample
Preparation Procedure for the Analysis of Organic Compounds in Soil and
Solid Matrices: Evaluation of Dynatech PTA—30 W/S Autosampler, November
1990.
2. B.V. loffe and A.G. Vitenberg, IIeadspace Analysis and Related Methods in
Gas Chromatography, John Wiley and Sons, 1984.
3. J.W. Eichelberger and W.L. Budde, U.S. EPA Method 524.2, Office of
Research and Development, Measurement of Purgeable Organic Compounds in
Water by Capjllary Column Gas Chromatography/Mass Spectrometry.
Revision 3.0, 1989.
10
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TABLE 1
MOLECULAR WEIGHTS AND CHARACTERISTIC IONS
Conpound MoLecular Weight Quantitatlon Ions
Internal Standards
FLU OROBENZENE 96 96
BROMOCHLOROMETKANE-d2 130 51
CHLOROF ORM-d 119 84
BENZENE-d6 84 84
TOLUENE-d8 100 98
2-BRON O-1-CHLOROPROPANE-d6 163 82
BROMO8ENZENE- 162 82
Surrogates
4•BRCWFLUOROSENZENE 174 95
1,2-DICHLOR OBENZENE-d4 150 150
Analytes
BENZENE 78 78
BROMCBENZENE 157 77
BRONOCHLOROMETHANE 128 49
BR ICHL0R0METHANE 162 83
BROMOFORM 250 173
BW ONETHANE 94 94
n-BUTYLBENZENE 134 91
sec-BUTYLBENZENE 134 105
tert-BUTYLBENZENE 134 119
CARBON TETRACHLORIDE 152 117
CHLORO8ENZENE 112 77
CHLOROETHA NE 64 49
CHLOROFORM 118 83
CHLOROI4ETHANE 50 50
2-CHLOROTOLUENE 126 91
4-CHLOROT0LUENE 126 91
DIBROKOCHLOROMETHANE 206 129
1,2-DIBRON O-3-CHLOROPR OPANE 234 75
1,2-DIBROMOMETHANE 186 107
DIBROMOMETNAME 172 93
1 1 2-D ICHLOR O SENZENE 146 146
1,3-DICHLOROSENZENE 146 146
1,4-DICHLORO SENZENE 146 146
DICHLORO DIFLUOROMETNANE 120 85
1,1-DICHLOROETHANE 98 63
1.2DICHLOROETHANE 98 62
1 l-DICHLOROETHENE 96 61
C S-1,2-0ICHLOR0ETHEHE 96 61
trans-1,2-DICHLOROETHENE 96 61
1,2-OICHLOROPROPANE 112 63
1,3-OICHLOR OPROPANE 112 76
2,2-DICHLOROPROPANE 112 77
1,1-DICHLOROPROPENE 110 75
ETHYLBENZENE 106 91
HEXACHLOROSUTADIENE 258 225
ISOPROPYLBENZENE 120 105
4-ISOPROPYLTOLUENE 134 119
METHYLENE CHLORIDE 84 49
NAPHTHALENE 128 128
n-PROPYLBENZENE 120 91
STYRENE 104 104
1,1,1,2-TETRACHL OROETHAIIE 166 131
112,2-TETRACNLOR OETHANE 166 83
TETRACHLOROETHENE 164 129
TOLUENE 92 91
1 ,2,3-TRICHLOROBENZENE 180 180
1 1 2,4-TRICHLOROBENZENE 180 180
1,1,1-TRICHLOR OETHANE 132 97
1,1,2-TR CHLOR0ETHANE 132 83
TRICHL OROETHENE 130 95
TRICHLOROFLUOROMETHANE 136 101
1,2,3-TRICHI OROPROPAIIE 146 75
1 2 4-TRIMETHYLBENZENE 120 105
1 3,5-TRIMETHYLBENZENE 120 105
VINYL CHLORIDE 62 62
o -XYLENE 106 91
p-XYLENE 106 106
11
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TABLE 2
DETERMINATION OF AUTOSAMPLER PRECISION
25 ng ANALYTE RESPONSE IN REAGENT WATER
Sacpte 1 Sai pLe 2 SanpLe 3 Saupte 4 Saupte 5 Saupte 6 AVG RSD
ANALYTE Area Area Area Area Area Area Area (%)
VINYL CHLORIDE 2026 2264 2052 1901 1950 1682 1979 9
TRICHLOROFLUOROMETHANE 2215 2306 2156 2216 2404 2052 2225 5
1,1-DICHLOROETHENE 1125 1321 1126 1267 1292 1091 1204 8
NETHYLENE CHLORIDE 3237 3506 3214 3399 3535 2964 3309 6
trans-1,2-DICHLOR OETHENE 809 716 729 749 802 692 750 6
1,1-DICHLOROETHANE 3189 3403 3170 3088 3435 2963 3208 5
cis-1,2-DICHL OROETHENE 971 1116 1016 915 1046 965 1002 7
BRONOCHLORONETHANE 1233 1253 1294 1251 1441 1169 1274 7
CHLOROFORM 3140 3699 3239 3482 3820 2989 3395 9
1,1,1-TRICKLOROETHANE 3351 3597 3252 3221 3553 2815 3298 8
CARBON TETRACHLORIDE 2792 2918 2939 2724 3009 2544 2821 6
BENZENE 4296 5309 4749 5016 5299 4360 4838 8
TRICHLOROETHYLENE 1162 1238 1084 1108 1327 1012 1155 9
1,2 -DICHLORO?ROPAJIE 1609 1649 1555 1464 1781 1457 1586 7
DIBRONONETHANE 1321 1441 1254 1328 1356 1256 1326 5
BRON ICHLORO4ETHANE 2171 2052 1927 1770 2434 1787 2024 11
TOLUEIIE 5808 6179 6114 5632 6975 5073 5964 10
1,1,2-TRICHLOROETHAIIE 1006 916 971 875 924 739 905 9
TETRACHLOROETHYLENE 1070 1087 993 1058 1161 830 1033 10
1,3-DICHLOROPR OPAIIE 2337 2213 2273 2166 2482 2069 2257 6
DI BRONOCHLORONETHAIIE 889 844 885 879 1075 731 884 11
CHLOROBENZENE 2478 2579 2464 2377 2898 2275 2512 8
1,11,2-TETRACHLOROETHANE 1237 1046 1216 925 1223 937 1097 12
ETHYL BENZENE 6813 6557 6501 5847 7761 5528 6501 11
p-XYLENE 6252 6106 5813 5489 6527 5567 5959 6
o-XYLENE 6156 5082 4585 5132 6180 6585 5287 12
STYRENE 2655 2673 2581 2395 2703 1879 2481 12
BROMOFORN 390 399 333 361 474 337 382 12
ISOPROPYLBENZENE 7724 8169 7403 7145 7337 6009 7298 9
p-BROMOFLIJOROBENZEME 2400 2575 2250 2478 3206 2027 2489 15
BRONOSEN2ENE 928 939 802 903 907 854 889 5
1 ,1 ,2 ,2-TETRACHLOR OETI1AWE 1501 1953 1935 1468 1451 1555 1644 13
1,2 ,3-TRICHLOROPROPANE 1309 1346 1274 1209 1594 1259 1332 9
n-PROPYL BENZENE 11768 10588 9143 10098 11607 9266 10412 10
2-CHLOROTOLUENE 1204 1093 982 1141 1127 774 1054 13
4-CHLORDTOLUENE 1182 1181 962 1080 1186 936 1088 10
1 ,3,5-TRIMETHYLBENZENE 7476 7610 6739 6917 7269 6256 7045 7
sec-BUTYI. BENZENE 10657 10862 8835 9836 10943 9212 10058 8
1,2,4-TRIMETHYLBENzENE 2006 1954 1583 1768 2122 1595 1838 11
1,3-DICHLOROBENZENE 1875 1634 1588 1672 1970 1732 1779 7
p-ISOPROPYL TOLUENE 6668 6520 5737 5454 7022 5893 6216 9
1,4-DICHLOROBENZENE- 1919 1876 - 1695 1672 2034 1636 1805 8
1,2-DICHL OR OBENZENE-d4 1633 1620 1349 1461 1857 1451 1562 11
1 ,2-DICHLORO SENZENE 1525 1477 147? 1386 1545 1282 1449 6
n-BJJTYL BENZENE 9584 10564 8057 8734 10159 8776 9312 9
1,2,4-TRICHLORO SENZENE 1011 1063 903 892 1226 870 994 13
HEXACHLORO SUTADIENE 1335 1204 1199 1174 1270 972 1192 9
NAPHTHALENE 1969 1766 1953 1826 1895 1755 1861 5
1,2,3-TRICHLORO SENZENE 922 968 781 821 922 719 856 10
12
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TABLE 3
EVALUATION OF THE MATRIX MODIFYING SOLUTION
25 ng ANALYTE RESPONSE IN SODIUM SULFATE SOLUTION
San Le 1 Sanpte 2 Seapte 3 Saapte 4 AVG RSD
ANALYTE Area Area Area Area Area CX)
VINYL CHLORIDE 731 952 857 1148 922 17
TRICHLOROFLUORONETHANE 1748 1783 1522 1806 1715 7
1,1-DICHLOROETHENE 955 804 844 893 874 6
METHYLENE CHLORIDE 5343 4722 4762 4427 4814 7
trans-1,2-DICHLOROETHENE 691 767 614 623 674 9
1 1-DICHLOROETHANE 3974 3928 3790 3321 3753 7
cis-1 2-DICHLOROETHENE 1340 1229 1164 1080 1203 8
BROMOCNLORONETHANE 2840 2770 2481 2316 2602 8
CHLOROFORM 3674 3731 3597 3116 3530 7
1,11-TRICHLOROETHANE 3144 3056 2949 2509 2915 8
CARBON TETRACHLORIDE 2219 1962 2105 2223 2127 5
BENZENE 5421 5268 4860 4290 4960 9
TRICKLOROETHYLENE 1134 1169 1048 1128 1120 4
1 1 2-DICHLOROPROPANE 2561 2431 2415 2070 2369 8
DIBRONONETNANE 3330 3267 3061 2496 3039 11
BRONODICHL OR OMETHANE 3397 3426 3195 2653 3168 10
TOLUEHE 6924 6613 6731 5871 6535 6
1,1 .2-TRICHLOROETHANE 1706 1832 1551 1299 1597 12
TETRACHLOROETHYLENE 875 793 705 660 758 11
1,3-DICHLOROPROPANE 5006 4871 5528 4340 4936 9
DIBROMOCHLORONETHANE 1862 1927 1770 1664 1806 5
CHLOROBEMZENE 3381 3058 3151 2736 3094 7
1,1,1,2-TETRACHLOROETHANE 1335 731 1367 1153 1147 22
ETHYL BENZENE 5936 6285 6079 5940 6060 2
p-XYLENE 5951 6099 5834 5930 5954 2
o-XYLEME 5091 5353 4574 5069 5022 6
STYRENE 2702 2668 2522 2817 2677 4
BRONOFORM 1182 1245 1096 1110 1158 5
ISOPROPYLBENZENE 6212 5248 5701 5571 5683 6
p-BRONOFLUOR OBENZENE 2717 3514 2895 2881 3002 10
BRONOBENZENE 1313 844 1308 974 1110 19
1 1,2,2-TETRACHLOROETHANE 3232 3949 3317 3453 3488 8
1,2,3-TRICHLOROPROPANE 3151 3904 3373 3596 3506 8
n-PROPYL BENZENE 8237 9359 8567 9407 8893 6
2-CHLOROTOLUENE 1107 1029 1154 1070 1090 4
4-CHLOROTOLUENE 1194 1434 1169 1051 1212 11
1,3,5-TRIMETHYLBENZENE 6289 5415 6149 5348 5800 7
sec-BUTYL BENZENE 8151 7241 8137 7330 7715 6
1,2 1 4-TRIMETHYLBENZENE 1851 1927 1948 1788 1879 3
1,3-DICHLORO BENZENE 2234 2079 2228 2026 2142 4
pISOPROPYL TOLUENE 4993 5156 4648 4361 4790 6
1,4-DICHLOR OBENZENE 2234 2340 2474 2444 2373 4
1,2-DICHLOROBENZENE-d4 2423 2270 2207 2084 2246 5
1,2-DICHLOR OBENZENE 2080 2047 2150 2070 2087 2
n-BUTYL BENZENE 6476 7898 6424 7622 7105 9
1,2,4-TRICHL OROBEIIZENE 1620 1492 1389 1192 1423 11
HEXACHLOROBUTADIENE 932 971 778 858 885 8
NAPHTHALENE 5626 5925 5898 5016 5616 7
1,2,3-TRICHLORO BENZENE 1510 1547 1537 1398 1498 4
13
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TABLE 4
EVALUATION OF THE MATRIX MODIFYING SOLUTION
25 ng AIIALYTE RESPONSE IN CALCIUM CHLORIDE SOLUTION
Sa rpLe 1 S&Tpte 2 Sairpte 3 Sanpte 4 Saq,te 5 AVG RSD
ANALYTE Area Area Area Area Area Area (%)
VINYL CHLORIDE 978 547 821 923 889 832 18
TRICHLOROFLUOROMETHANE 1200 1133 1171 1204 1276 1197 4
1,1-DICHLOROETHENE 806 510 735 364 639 611 26
METHYLENE CHLORIDE 3553 2988 2674 2853 3014 3016 10
trans-1,2-DICHLOROETHENE 519 489 487 514 461 494 4
1,1-DICHLOROETHANE 2916 2541 2315 2676 2726 2635 8
cis l,2-DICHLOROETHENE 930 873 610 803 748 793 14
BROMOCHLORCMETHANE 1486 1383 1134 1251 1313 1313 9
CHLOROFORM 2677 2434 2235 2565 2614 2505 6
1,1,1-TRICHLOR OETHAWE 2234 2110 1865 2182 2225 2123 6
CARBON TETRACHLORIDE 2189 1903 1855 1819 1972 1948 7
BENZENE 3736 3511 2996 3528 3618 3478 7
TRICHLOROETHYLENE 1039 950 907 975 1031 980 5
1,2-DICHLOROPROPAIIE 1426 1385 1173 1107 1355 1289 10
DIBRONONETHANE 1384 1255 1081 1173 1326 1244 9
BRONODICHLORa1ETHAIIE 2339 1934 2010 1952 1879 2023 8
TOLUENE 2156 1901 1652 1839 1959 1901 9
1,1,2-TRICKLOROETHANE 688 565 636 573 581 609 8
TETRACHLOROETHYLENE 735 772 695 760 735 739 4
1,3-DICKLOROPROPANE 2397 2024 2041 1945 2031 2088 8
DI BRONOCHLORONETHAME 1407 1372 1025 1151 1196 1230 12
CHLORO SENZENE 2465 2586 1872 2443 2868 2447 13
1 ,1,1,2-TETRACHLOROETHAWE 708 1042 644 959 964 863 18
ETHYL BENZENE 4837 4275 3833 4531 4497 4395 8
p-XYLENE 4628 3838 3554 3458 3595 3815 11
o-XYLENE 4525 4013 4012 3589 4309 4090 8
STYRENE 1217 469 261 225 530 540 66
BROMOFORM 1385 1114 781 942 889 1022 21
ISOPROPYLBENZENE 5477 5488 4403 6074 6028 5494 11
p-BRONOFLUOROBENZENE 2091 1478 1326 1467 1580 1588 17
BROMOSENZENE 832 780 757 798 851 804 4
1,1,2,2-TETRACHLOR OETHANE 1676 1408 1162 1156 1173 1311 16
1,2.3-TRICHLCR OPROPAI IE 1636 1524 1171 1151 1106 1318 17
n-PROPYL BENZENE 6488 5437 5442 6387 6545 6060 8
2-CHLOROTOLUENE 864 1007 797 1066 1009 949 11
4-CHLOROTOLUENE 614 763 727 952 1070 825 20
1,3,5-TRINETIIYLBENZENE 3674 3176 2433 4627 6152 4012 32
sec-BUTYL BEUZENE 6593 7285 5237 7946 8870 7186 17
12,4-TRIMETHYLBENZENE 1135 1243 943 1328 1780 1286 22
1,3-DICHL OROBENZENE 1505 1446 1098 1552 1704 1461 14
p-ISOPROPYL TOLUENE 4081 6228 3133 4177 5090 4142 15
1,4 -DICHL OROSENZENE 1789 1643 1098 1552 1739 1564 16
1,2-OICHLOROBENZENE-d4 1646 1317 1173 1481 1589 1401 10
1,2-DICHLOROBENZENE 1227 1153 987 1365 1413 1229 12
n-BUTYL BENZENE 6458 5456 5814 5308 6136 5834 7
1 ,2,4-TRICHLOR OBENZENE 863 831 798 720 735 789 7
HEXACHLOROSIJTADIENE 687 677 603 612 798 675 10
NAPHTHALENE 2530 2475 1961 1918 1909 2159 13
1,2,3-TRICHLORC SENZENE 1045 758 671 556 418 690 31
14
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TABLE 5
VERIFICATION OF FORTIFYING PROCEDURE
25 ng ANALYTE RESPONSE IN SAND
Sa ipLe I SairpLe 2 SampLe 3 SampLe 4 SampLe 5 AVG RSD
ANALYTE Area Area Aera Area Area Area (%)
VINYL CHLORIDE 1610 1746 1774 1686 1670 1697 3
TRICHLOROFLUORONETHANE 1975 1904 1970 2136 2243 2046 6
1,1-DICNLOROETHENE 1277 1340 1594 1568 1599 1476 9
NETHYLENE CHLORIDE 7647 8437 8722 9153 9798 8751 8
trans-1,2-DICH I OROETHENE 1098 1160 1325 1121 1241 1189 7
1 1-DICHLOROETHANE 5532 5936 6189 6600 7277 6307 9
cts-1,2-DICHL OROETHENE 2134 2265 2206 2435 2746 2357 9
BRONOCKLORONETHANE 3931 4481 4397 4618 4931 4472 7
CHLOROFORM 5477 6498 6402 7016 7260 6531 9
1,1,1•TRICHLOROETHANE 4239 4769 5061 4922 5564 6911 9
CARBON TETRACHLORIDE 3475 3787 4325 4068 4793 4090 11
BENZENE 8817 8966 9244 10993 10033 9611 8
TRICHLOROETHYLENE 1859 2041 2067 2115 2380 2092 8
1,2-DICHL OR OPROPANE 3378 3846 4037 4133 4381 3955 8
DIBRONONETHANE 4602 5189 5313 5319 5360 5157 5
BRONODICHLORONETHANE 5000 5624 5496 5729 5562 5482 5
TOLUENE 11974 12766 13745 15946 14852 13857 10
1,1 2-TRICHLOROETHANE 2491 2719 2781 2820 2947 2752 5
TETRACHL OROETHYLENE 1492 1319 1626 1596 1626 1532 8
1 3-DICHLOROPROPANE 9496 9821 9671 11693 9882 10113 8
OIBROMOCHLOR ONETHANE 2878 3017 3095 3406 3447 3169 7
CHLORO BENZENE 5594 6285 6113 6565 6398 6191 5
1,1,1,2-TETRACHLOROETHANE 2894 2848 2808 2867 3282 2940 6
ETHYL BENZENE 13857 16503 13259 15808 14342 14754 8
p-XYLENE 12852 13419 12651 14986 12365 13255 7
o-XYLENE 12224 13593 11178 14658 14149 13160 10
STYRENE 2401 2251 2520 2165 1854 2238 10
BRONOFORM 1723 1969 1733 2038 1917 1876 7
ISOPR OPYLBENZENE 11758 11532 11208 13739 11974 12042 7
p- BRONOFLUOROBENZENE 5337 6182 5793 6114 5657 5817 5
BRON OBEMZENE 2118 2354 2157 2935 2374 2388 12
1,1,2,2-TETRACHLOR OETHANE 5812 6249 6407 8103 7868 6888 13
1,2 1 3-TRICHLOROPROPANE 7339 8454 6432 8923 7452 7720 11
n-PROPYL BENZENE 18223 20182 18641 21490 17960 19299 7
2-CHLOROTOLUENE 1932 2594 2406 2688 2331 2390 11
4-CHLOROT OLUENE 2136 2229 2161 2710 2311 2309 9
1,3 5-TRI NETHYLBENZENE 11177 13723 11797 13208 12225 12426 7
sec-BUTYL BENZENE 12405 16124 13677 16185 13063 14291 11
1,2 4-TRIMETHYLBENZENE 3145 3985 3227 4171 3985 3703 12
1,3-D ICHLORO BENZENE 3508 4195 3759 6809 4195 4093 11
p-ISOPROPYL TOLUENE 7989 8985 8822 10411 8985 9038 9
14-DICHL OROBENZENE 3772 4355 4404 4809 4355 4339 8
12-DICHLOROSENZENE-d4 3894 4826 4265 5007 4826 4564 9
1,2-DICHLOROBENZENE 3351 4013 3888 4367 4013 3926 8
n-BUTYL BENZENE 12550 13891 14133 14168 13891 13727 4
1,2,4-TRICHL OROBENZENE 1868 2401 1786 2309 2401 2153 13
HEXACHLOR OBUTADIENE 1005 1202 987 1092 1202 1098 8
NAPHTHALENE 7649 9800 8636 9603 9800 9098 9
1 .2,3-TRICHL OR OBENZENE 1797 2226 2Q32 2232 2226 2103 8
FILE SOIRE 107
15
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TABLE 6
25 rig AMALYTE RESPONSE IN REAGENT WATER
Sanpte 1 Saripte 2 SairpLe 3 Sarrpte 4 Saripte 5 AVG RSD
ANALYTE Area Area Area Area Area Area (%)
VINYL CHLORIDE 2416 2333 2265 2205 2149 2274 4
TRICHLOROFLUORCMETHANE 4002 3984 4054 3967 3770 3955 2
1,1 -DICHLOROETHENE 1570 1631 1633 1544 1622 1600 2
NETHYLENE CHLORIDE 2770 2781 2803 2812 2828 2799 1
trans-1,2-DICHLOROETHENE 1443 1400 1525 1460 1372 1440 4
1 1-DtCHL0R0ETHANE 3505 3542 3686 3648 3665 3609 2
c ls -1,2 -DICHLOROETHENE 1300 1337 1277 1244 1326 1297 3
BROMOCHLORONETHANE 1513 1464 1442 1629 1493 1508 4
CHLOROFORM 3929 3856 3851 3737 3824 3839 2
1,1,1-TRICHLOROETHANE 3715 3452 3559 3500 3508 3547 3
CARBON TETRACHLORIDE 3336 3248 3510 3321 3368 3357 3
BENZENE 5422 5575 5897 5459 5589 5588 3
TRICHLOROETHYLENE 1469 1501 1583 1488 1542 1517 3
1 ,2-DICHLOROPRCPANE 1671 1651 1765 1607 1720 1683 3
DIBRONOMETHANE 801 869 848 903 851 854 4
BROMODICHLOROMETHANE 2398 2276 2253 2151 2105 2237 5
TOLUENE 6838 6898 6854 6568 6483 6728 3
1,1,2-TRICHLOROETHANE 692 700 674 698 737 700 3
TETRACHLOROETHYLENE 1251 1237 1265 1329 1216 1260 3
1,3-DICHLOROPROPANE 1312 1393 1310 1417 1428 1372 4
DIBRO4OCHLOROMETHANE 917 953 1028 995 994 977 4
CHLORO8ENZENE 2891 2955 3079 3073 3153 3030 3
1,1,1,2-TETRACHLOROETHANE 1126 1310 1277 1267 1271 1250 5
ETHYL BENZENE 7933 7883 7742 7682 7632 7774 1
p -XYLENE 11999 12653 11334 12379 12284 12130 4
o-XYLENE 5358 5511 5328 5785 5677 5532 3
STYRENE 2475 2526 2579 2636 2835 2610 5
BRONOFORM 435 451 496 419 466 453 6
ISOPROPYLBEN ZENE 7218 7502 8399 7228 8550 7779 7
p-BRO IOFLUORO8EN ZENE 1922 1646 2140 2336 2575 2124 15
BRONOBENZENE - NI NI HI NI NI - -
1,1,2,2-TETRACHLOROETHANE 1369 1484 1485 1511 1366 1443 4
1,2 ,3 -TRICHLOROPROPANE 482 667 442 440 510 508 16
n-PROPYL BENZENE 9839 10928 10681 10793 10347 10518 4
2-CHLOROTOLUENE 1373- 1370 1395 1356 1401 1379 1
4-CHLOROTOLUENE 1306 1392 1343 1346 1271 1332 3
1,3,5-TRIMETHYLBEN ZENE 7202 7495 7792 7780 8217 7697 4
sec-BUTYL BENZENE 9589 9864 10863 10126 11470 10382 7
1,2,4 -TRIMETHYLBENZEHE 2728 2719 2921 2798 3091 2351 5
1,3-DICHLORO8ENZENE 2151 2199 2117 2253 2195 2183 2
p-I SOPROPYL TOLUENE 6746 6926 6881 7146 7329 7006 3
1,4-DICHLORO8ENZENE 2317 2052 2328 2158 2227 2216 5
1 ,2-DICHLORO8EHZENE-d4 1764 1726 1628 1772 1804 1739 3
1,2-DICHLORO8EHZEHE 1792 1810 1862 1759 1777 1800 2
n-BUTYL BEHZENE 8916 9342 10769 9347 9728 9620 7
1,2,4-TRICHLOROBENZEHE 1228 1332 1242 1404 1377 1317 5
HEXACHLORO8UTADIENE 1286 1254 1431 1278 1375 1325 5
NAPHTHALENE 2229 2205 2188 2394 2424 2288 4
1 .2 9 3-TRICHLOROBENZENE 1000 1096 1098 1092 1074 1072 3
HI=not IncLuded
16
-------
TABLE 7
25 ng ANALYTE RESPONSE IN THE S SOLUTION
San (e I Saupte 2 Sai Le 3 Sanpte 4 SaITpte 5 AVG RSD
ANALYTE Area Area Area Area Area Area (Z)
VINYL CHLORIDE 2374 2372 2559 2492 2161 2392 6
TRICHLOROFLUOROMETHANE 3721 3810 4013 3840 3460 3769 5
1,1DICHL O R OETHENE 1680 1806 1829 1871 1621 1761 5
NETHYLENE CHLORIDE 4672 4958 4934 5110 4697 4874 3
traflS•1,2•DICHLOROETHENE 1885 1978 2126 2038 1889 1983 5
1 1-DICHLOROETHANE 5432 5635 5827 5889 5288 5614 4
cls1 ,2-DICHL0R0 THENE 1976 2068 2161 2065 2028 2059 3
BRONOCHLORONETHANE 2991 3136 3156 3084 3098 3093 2
CHLOROFORM NI 5311 5347 5464 5078 5300 3
1,1,1-TRICHLOROETHANE 3837 4140 4647 4695 3822 4228 9
CARBON TETRACHLORIDE 3399 3550 4038 4185 3516 3738 8
BENZENE 7875 7881 8068 7938 7863 7925 1
TRICHLOROETHYLENE 1897 2109 2238 2263 2001 2102 7
1,2-DICHLOROPR OPANE 2880 3177 3222 3248 3118 3129 4
DIBRO 1ETHAIIE 1777 1801 1845 1935 1788 1829 3
BR OMODICHLORONETHANE 6279 4189 4235 4102 4113 4584 19
TOLUENE 9204 9436 10049 9961 9193 9569 4
11,2-TRICHIOROETHANE 1635 1648 1660 1736 1704 1677 2
TETRACHIOROETHYLENE 1303 1289 1581 1541 1306 1404 9
1,3-DICHLOROPROPANE 3060 3224 3384 3273 3226 3233 3
DIBRONOCHIORONETHANE 2958 2143 2117 2269 2175 2332 14
CHLOR OBENZENE 4791 4431 4920 4724 4263 4626 5
1,1,1,2-TETRACHLOROETHANE 1837 1908 1966 2016 1746 1895 5
ETHYL BENZENE 9228 9453 9984 10548 9200 9683 5
p-XYLENE 15815 18263 18872 17803 15756 17302 7
o-XYLENE 7278 8749 9138 9702 8318 8637 9
STYRENE 4365 4581 4765 4910 4487 4622 4
BRONOFORN 1304 1217 1282 1271 1194 1254 3
ISOPROPYLBENZENE 8861 9550 9248 9826 7879 9073 7
p-BROROFLUORO8ENZENE 3865 4212 4201 4469 4113 4172 5
BRONO SENZENE NI NI NI NI NI
1,1,2,2-TETRACHLOROETHANE 3628 4040 3885 3900 3845 3860 3
1,2,3-TRICHLOR OPROPANE 3416 3566 3385 3819 3388 3515 5
n-PROPYL BENZENE 11930 12270 13191 13047 11189 12325 6
2-CHL OROTOLUENE 1811 1858 2023 1921 1668 1856 6
4CHLOROTOLUENE 1950 1959 2001 2084 1840 1967 4
1,3,5-TRIMETHYLBENZENE 8000 8922 10053 9845 8452 9054 9
sec-BUTYL BENZENE 10779 11491 11774 11046 9911 11000 6
1I2,4-TRIMETHYLBENZENE 3295 3698 3701 3517 3187 3480 6
13•DICHLORO SENZENE 3494 3576 3452 3279 3243 3409 4
p-ISOPROPYL TOLUENE 8403 7341 8703 8317 7547 8062 7
1 ,4-DICHLOR OBENZENE 3563 3755 3922 3807 3623 3734 3
1,2-DICHLOR O BENZEHE-d4 3200 3224 3247 3244 2927 3168 4
1,2-DICHLORO SENZENE 3316 3222 3351 3216 3119 3245 3
n-B*JTYL BENZENE 10840 12244 12373 11640 9894 11398 8
1,2,4•TRICHLOR OBENZENE 2328 2475 2634 2589 2300 2465 5
HEXACHLOR OBUTADIENE 1294 1465 1594 1712 1483 1510 9
NAPHTHALENE 7057 7428 8050 7694 7518 7549 4
1 ,2,3-TRICHLOR OBENZENE 2186 2385 2507 2332 2316 2345 4
NI not included
17
-------
TABLE 8
25 ng ANALYTE RESPONSE IN WATER/SAND
Sanpte 1 San Le 2 Sanpte 3 Sarpte 4 Sanpte 5 AVG RSO
ANALYTE Area Area Area Area Area Area (%)
VINYL CHLORIDE 993 1157 1Q80 980 1011 1044 6
TR ICHLOROFLUOROMETHANE 1862 2376 2280 2213 2266 2199 8
1 ,1-DICHLOROETHENE 926 1107 1136 1077 1015 1052 7
METHYLENE CHLORIDE 1960 2503 2476 2410 2367 2339 9
trans-1,2-DICHLOROETHENE 946 1147 1228 1161 1194 1135 9
1,1-DICHLOROETHAME 2519 3147 3108 3268 3211 3051 9
c le-1,2-OICHL OROETHENE 888 1205 1197 1223 1233 1149 11
BROROCKLORONETHANE 1219 1558 1554 1454 1491 1455 9
CHLOROFORM 2781 3627 3647 3532 3637 3445 10
1,1,1-TRICHLOROETHANE 2078 2748 2774 2746 2818 2633 11
CARBON TETRACHLORIDE 1917 2389 2539 2443 2578 2373 10
BENZENE 4225 5298 5340 5759 5149 5154 10
TRICHLOROETHYLENE 1384 1314 1267 1264 1347 1315 4
1,2-DICHLOROPROPANE 1301 1579 1655 1589 1640 1553 8
DIBRC4ONETHANE 705 864 808 904 837 824 8
BRON ICHL0RONETHANE 1717 2293 2275 2255 2151 2138 10
TOt.UENE 4969 7011 6859 6820 7116 6555 12
1,1,2-TRICHLOROETHANE 729 758 735 763 802 757 3
TETRACHL OROETHYLENE 1063 1050 1080 1082 1101 1071 2
1 1 3-DICHLOROPROPANE 1194 1509 1517 1501 1429 1430 9
DI BRONOCHLOROMETHANE 815 1005 1034 1025 1069 990 9
CHLORO BENZENE 2220 2694 2785 2832 2759 2658 8
1,1,1,2•TETRACHLOROETHANE 999 1118 1163 1152 942 1075 8
ETHYL BENZENE 5852 7500 7522 7011 7053 6988 9
pXYLENE 8732 11018 11404 11574 11866 10919 10
o-XYLENE 6513 5578 5846 5417 5635 5398 9
STYRENE 1976 2225 2084 1885 2035 2041 6
BRONOFORM 390 516 522 467 543 488 11
ISOPROPYLBEUZENE 5075 6509 6925 6408 6516 6287 10
pBR 40FLU0RO8ENZENE 1576 2269 1942 1928 2145 1972 12
BRONO8ENZENE NI NI NI NI NI - -
1 1 1 1 2,2-TETRACHLOROETHANE 1285 1595 1647 1749 1608 1577 10
1,2,3-TRICHLOROPROPANE 947 1266 1354 1121 1489 1235 15
n-PROPYI. BENZENE 7358 9181 9488 9741 9470 9048 10
2-CHLOROTOLuENE 987 1309 1262 1273 1053 1177 11
4-CHIOROTOLUENE 1000 1291 1365 1294 1338 1258 10
1,3,5-TRIMETHYLBENZENE 5573 6299 6603 6409 6669 6311 6
sec-BUTYI. BENZENE 6718 8223 8085 7615 8663 7862 8
12 1 4-TRINETHYLBENZENE 2159 2666 2508 2529 2749 2522 8
1,3-DICHLOR O8ENZENE 1665 2219 2018 1992 1991 1977 9
p-ISOPROPYL TOLUEWE 4944 6195 5719 5685 5859 5680 7
1,4-DICHLOROSENZENE 1680 2183 2194 2039 2185 2056 10
1,2-DICHLOROBEHZENE-d4 1419 1932 1771 1560 1824 1701 11
1,2-DICHLORO BENZENE 1487 1877 1892 1625 1833 1743 9
n-8UTYL BENZENE 6947 8217 7838 7849 9014 7973 8
1,2,4-TRICHLOR O8ENZENE 897 1301 1274 1326 1467 1253 15
HEXACHLORO8UTADIENE 863 1159 1135 1112 1315 1117 13
NAPHTHALENE 2207 2761 2817 2694 2909 2678 9
1,2,3-TRICHLORO BENzE NE 956 1216 1135 1082 803 1038 14
NI:not IncLuded
18
-------
TABLE 9
25 ng ANALYTE RESPONSE IN P4MSISAND
San Le 1 SanpLe 2 Sairpte 3 SanVLe 4 AVG RSD
AMALYTE Area Area Area Area Area ( )
VINYL CHLORIDE 1602 1652 1636 144.8 1585 5
TRIC 1L0R0FLUOR0METHANE 2648 2831 2863 2580 2731 4
1,1-DICHLOR OETHENE 1358 1408 1336 1288 1348 3
METHYLENE CHLORIDE 4188 4110 4167 4193 4160 1
trans-1,2-OICHLOROETKENE 1120 1541 1613 1563 1459 14
1,1-DICHLOR OETHAME 4475 4507 4732 4724 4610 3
cls-1,2-DICHLOR OETHENE 1793 1785 1733 1843 1789 2
BRONOCHLOROHETHANE 2824 2798 2924 2755 2825 2
CHLOROFORM 4377 4448 4615 4605 4511 2
1,1,1-TRICHL OROETHANE 3318 3481 3570 3688 3514 4
CARBON TETRACHLORIDE 2863 3162 3144 3085 3064 4
BENZENE 6811 7059 7150 7470 7123 3
TRICHLOR OETHYLENE 1595 1646 1722 1781 1686 4
12DICHLOR OPR OPANE 2646 2690 2647 2845 2707 3
DIBRONONETHAME 1864 1789 1771 1825 1812 2
BROMODICHLORONETHAWE 3596 3671 3802 3880 3737 3
TOLLIENE 8994 9243 9736 9725 9425 3
1,1,2•TRICHLOR OETHANE 1539 1566 1683 1754 1636 5
TETRACHLOROETHYLENE 1237 1331 1300 1266 1284 3
1,3DICHLOROPROPANE 3162 3199 3204 3135 3175 1
DIBRCKOCHLORONETHANE 1922 1985 2010 1963 1970 2
CHLORO8ENZENE 4663 4203 4156 6456 4315 3
1,1 1,2-TETRACHL0R0ET}4ANE 1761 1638 1669 1711 1695 3
ETHYL BENZENE 8607 8766 9223 10278 9219 7
p-XYLENE 13736 14974 15156 16326 15048 6
o-XYLENE 7716 8008 7921 8058 7926 2
STYRENE 2977 2525 2605 2740 2712 6
BRONOFORM 1193 1150 1282 1270 1224 4
ISOPROPYLBENZENE 8118 8545 8271 8475 8352 2
p-BROMOFLUOROBENZENE 3466 3366 3812 3605 3562 5
BR OMOBEHZENE NI MI NI MI
1,1 1 2,2TETRACHLOROETHANE 3788 3713 4027 4014 3886 4
1,2,3-TR ICHLCROPR OPANE 3695 3695 3311 3731 3608 5
n-PROPYL BENZENE 11040 11275 10941 11411 11167 2
2-CHLOROTOLUENE 1678 1563 1633 1595 1617 3
4-CHLOROTOLUENE 1681 1685 1728 1743 1709 2
1 8 3 5-TRIHETHYLBENZENE 8018 7819 8068 7763 7917 2
sec-BUTYL BENZEME 9557 9984 9953 9985 9870 2
1,2 4•TRIMETHYLBEN2ENE 3259 3431 3391 3309 3348 2
1,3-DICHLOROBEMZENE 2872 2710 3096 2793 2868 5
p-ISOPROPYL TOLUENE 6939 - 6951 7287 7113 7073 2
1,4-DICHLOR OSENZENE 3056 3351 3227 3326 3260 4
1,2-DICHL ORO SENZENE-d4 2810 2897 2824 2838 2842 1
1,2-DICHL OROSENZENE 2869 2834 2698 2908 2827 3
n-BUTYL BENZENE 9601 9961 10031 10724 10079 4
12,4-TRICHLOROBENZENE 1916 1885 2020 2178 2000 6
HEXACHLOROBUTADIENE 1290 1370 1492 1547 1425 7
NAPHTHALENE 6229 6642 6843 7807 6880 8
1 1 2,3-TRICHLOR OBENZEME 1750 1801 2070 2080 1925 B
MI not included
19
-------
TABLE 10
COMPARISON OF FOUR FORTIFIED IATRICES
IFF(2)
ANALYTE
REAGENT WATER
104S
WATER SAND
MSS/SAND
Area
Area
Area
Area
AVG
RSD
AVG RSO IFF(1)
AVG RSD
AVG RSD
VINYL CHLORIDE
2274
4
2392 6
5
1044 6
1587 5
41
TRICHLOROFLUOROMETHANE
3955
2
3769 5
5
2188 8
2731 4
22
1,1-DICHLOROETHENE
1600
2
1761 5
10
1052 7
1348 3
25
NETHYLENE CHLORIDE
2799
1
4874 3
54
2339 9
4160 1
56
trans-1 1 2-DICHL.OROETHENE
1440
4
1983 5
32
1135 9
1459 14
25
1 1-DICHLOROETHANE
cis-1,2-DICHL ORCETHENE
3609
1297
2
3
5614 4
2059 3
44
45
3051 9
1159 11
4610 3
1789 2
34
43
BROMOCHLOROMETKANE
1508
4
3093 2
70
1455 9
2825 2
64
CHLOROFORM
3839
2
5300 3
32
3445 10
4511 2
27
1,1,1-TRICHLORQETHANE
3547
3
4228 9
18
2633 11
3514 4
29
CARBON TETRACHLORIDE
3357
3
3738 8
11
2373 10
3064 4
25
BENZEME
5588
3
7925 1
35
5154 10
7123 3
32
TRICHLOROETHYLEIIE
1517
3
2102 7
32
1315 6
1686 4
25
1,2-DICHLOROPROPANE
1683
3
3129 4
60
1553 8
2707 3
54
DIBROMOMETHANE
854
4
1829 3
73
824 8
1612 23
74
BRONODICHLORCNETHANE
2237
5
4584 19
70
2138 10
3737 3
54
TOLUENE
6728
3
9569 4
30
6555 12
9425 3
36
1,1,2-TRICHLOROETHAIIE
700
3
1677 2
82
757 3
1636 5
73
TETRACHLOROETHYLENE
1260
3
1404 9
12
1071 2
1284 3
18
1,3-DICHLOROPROPANE
1372
4
3233 3
81
1430 9
3175 1
76
DIBRONOCHLOROMETHAHE
977
4
2332 14
82
990 9
1970 2
66
CHLORO8ENZENE
3030
3
4626 5
42
2658 8
4315 3
48
1,1,1,2-TETRACHLOROETHAPIE
1250
5
1895 5
41
1075 8
1695 3
45
ETHYL BENZENE
7774
1
9683 5
22
6988 9
9219 7
28
p-XYLENE
12130
4
17302 7
35
10919 10
15048 6
32
o-XYLENE
5532
3
8637 9
44
5398 9
7926 2
38
STYRENE
2610
5
4622 6
56
2041 6
2712 6
28
BROMOFORM
453
6
1254 3
94
488 11
1224 4
86
ISOPROPYLBENZENE
7779
7
9073 7
15
6287 10
8352 2
28
p-BROflOFLUOROSEUZENE
2124
15
4172 5
65
1972 12
3562 5
57
BRONOBEN2ENE
NI
•
NI •
-
NI -
NI -
11,2,2-TETRACHL O ROETHA IiE
1443
4
3869 3
91
1577 10
3806 4
84
1,2,3-TRICHL OROPROPANE
508
16
3515 5
149
1235 15
3608 5
98
n-PROPYL BENZENE
10518
4
12325 6
16
9048 10
11167 2
21
2-CHLOROTOLUENE
1379
1
1856 6
30
1177 11
1617 3
31
4-CHLOROTOLUENE
1332
3
1967 4
38
1258 10
1709 2
30
1,3,5-TRIMETHYLBENZENE
7697
4
9054 9
16
6311 6
7917 2
23
sec-BUTYL BENZENE
10382
7
11000 6
6
7862 8
9870 2
23
-
1.2,4-TRINETHYLBENzENE
2851
5
.3480 6
20
2522 8
3348 2
28
1 3-DICHLORO8ENZENE
2183
2
3409 4
44
1977 9
2868 5
37
p-ISOPROPYL TOLUENE
7006
3
8062 7
14
5680 7
7073 2
22
1 ,4-DICHLOROBENZENE
2216
5
3734 3
51
2056 10
3240 4
45
1,2-DICHLORO BEMZENE-d4
1739
3
3168 4
58
1701 11
2842 1
50
1,2-DICHLORO BEMZENE
1800
2
3245 3
57
1743 9
2827 3
47
n-BUTYL BENZENE
9620
7
11398 8
17
7973 8
10079 4
23
1 ,2,4-TRICHLOROBENZENE
1317
5
2465 5
61
1253 15
2000 6
46
HEXACHLOROSLJIADIENE
1325
5
1510 9
13
1117 13
1425 7
24
NAPHTHALENE
2288
4
7549 4
107
2678 9
6880 8
84
1,2,3-TRICHLOROBENZENE
1072
3
2345 4
74
1038 14
1925 8
60
NI=not Inctt ed
(1) FIRST TWO COLUM$
(2) LAST TWO COLUIINS
20
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TABLE 11
25 ng ANALYTE RESPONSE IN P4NS/SAND
San Le 1 Swipte 2 Safl te 3 AVG R
AHALYTE Area Area Area Area CX)
DICHLOR IFLUOR IETHANE 82 258 151 166 44
CHLOROMETHANE 852 668 806 775 10
VINYL CHLORIDE 1688 1822 1459 1656 9
BR ONETNANE 223 72 150 148 42
CHLOROETHANE 589 566 645 600 6
TRICHLOROFLUORONETHAJIE 4083 3656 3543 3761 6
1,1DICHLOROETHENE 6739 6309 5729 6259 7
METHYLENE CHLORIDE 7643 7563 7500 7569 1
trans-1,2-DICHLOR OETHENE 6551 5755 5698 6001 6
1,1- OICHLOROETHANE 9769 9366 8685 9273 5
2 2-DICHLOROPROPANE 4931 3963 3816 4237 12
c%a-1 1 2-DICHLOR OETHENE 7150 7058 6946 7051 1
BROMOCHLOROMETHANE 5329 5737 5349 5472 3
CHLOROFORM 8750 8086 8325 8387 3
1,1,1-TRICHLOROETHANE 6805 6446 6341 6531 3
1,1-DICHLOROPROPENE 6132 5805 5789 5909 3
CARBON TETRACHLORIDE 5708 5335 5605 5549 3
BENZENE 15299 14146 14786 14743 3
1,2-DICHLOROETHANE 9308 8752 9493 9186 3
TRICHLOROETHYLENE 6421 5939 6528 6296 4
1,2-DICHLOROPROPANE 5349 4496 4561 4802 8
DIBR CMETHANE 3556 3495 3548 3533 1
BROMODICHLOR ONETHANE 7622 7117 7190 7310 3
TOLUENE 20397 18327 19708 19477 4
1 .1,2-TRICHLOROETHANE 4181 3969 3800 3983 4
TETRACHLOR OETHYLENE 4209 4035 3255 3833 11
1,3DICHLOROPROPANE 7154 6112 6162 6476 7
DIBRONOCHLOROI ETHANE 5908 5462 5351 5574 4
1,2-DIBRONOETHANE 4657 4937 4583 4726 3
CHLORO SENZENE 10430 11200 11595 11075 4
1,1,1,2-TETRACHLOROETHANE 5368 5265 5319 5317 1
ETHYL BENZENE 25995 26912 25798 26235 2
p-XYLENE 18675 18564 16626 17955 5
0XYLENE 23613 22728 21699 22680 3
STYRENE 9049 8307 7687 8348 7
BRONOFORM 3662 3420 3003 3362 8
ISOPROPYLBENZENE 9882 9517 8603 9334 6
p-BRONOFLUORO8ENZENE NI NI NI - -
BRONOBENZENE 18570 16084 18089 17581 - 6
1 ,1,2,2-TETRACHL OROETHANE 8175 7677 8213 8022 3
1 ,2,3-TRICKLOROPROPANE 7252 9097 6120 7490 16
n-PROPYI. BENZENE 27842- 28635 24844 27107 6
2 -CHLOROT OLUENE 27058 24576 22656 24763 7
4-CHIOROTOLUENE 20708 21099 20823 20877 1
tert-BUTYLBEMZEWE 20485 22875 19601 20987 7
1 ,3 ,5 -TRIMETHYLBENZENE 25626 30146 24768 26847 9
sec-BUTYL BEN2ENE 33823 31628 29868 31773 5
1,2-DIBRONO-3-CHLOROPROPANE 4594 4131 4102 4276 6
1 ,2,4-TRIMETHYLBENZENE 27528 24130 26971 26210 6
1,3-DICHLOROBENZENE 8868 7822 7855 8182 6
p-ISOPROPYL TOLUENE 23443 20637 21930 22003 5
1,4-DICHLORO BENZENE 9325 9273 8473 9024 4
1,2-DICHLORO BENZENE-C14 NI NI NI -
1,2-DICHLOROBENZENE 10059 7476 7009 8181 16
n-BUTYL BENZENE 27842 28635 24844 27107 6
1,2,4-TRICHLOR O BENZENE 4914 5318 5528 5253 5
HEXACHLORO8UTADIENE 4157 3938 3560 3885 6
NAP IITHALENE 17748 15066 15512 16109 7
1,2 ,3-TRICHL OR O BENZENE 4770 4708 444-4 4641 3
NI not Included
21
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TABLE 12
25 ng ANALYTE RESPONSE IN MMS/CLAY
San Le 1 Sanpte 2 San te 3 AVG RSD
ANALYTE Area Area Area Area CX)
DICHL OROFLU ORONETHANE 935 702 623 753 18
CHLOR OMETHAIIE 911 910 834 885 4
VINYL CHLORIDE 1746 1700 1633 1693 3
BRONONETHANE 42 92 110 81 35
CHL OROETHANE 620 444 367 410 8
TRICHLOROFLUOROMETHANE 2435 2227 2268 2310 4
1,1-DICHIOROETHENE 4191 6003 4938 4377 9
METHYLENE CHLORIDE 4877 4746 5829 5151 9
trans-1,2 -DICHLOROETHENE 3575 3368 4165 3703 9
1,1-DICHLO ROETHANE 4880 4882 6409 5390 13
2 2-DICHLOROPROPAIIE 1912 1425 2251 1863 18
cls-1,2-DICHL O ROETHENE 3892 3732 5001 4208 13
BRONOCHLORONETHANE 2994 3074 4052 3373 16
CHLOROFORM 3983 3823 5579 6462 18
1,1,1-TRICHLOROETHA IIE 2791 2300 3780 2957 21
1,1-DICHLOROPROPENE 2702 2220 3637 2853 21
CARBON TETRACHLORIDE 2387 1862 3023 2424 20
BENZENE 5992 5820 8162 6658 16
1,2DICHLOROETHANE 4625 4688 6394 5236 16
TRICHLCROETHYLENE 2536 2009 3448 2664 22
1,2-DICHLOROPROPANE 2165 2213 3508 2629 24
DIBRON (ETNANE 1597 1808 2355 1920 17
BRONODICHLOR ONETHANE 3347 2995 5005 3782 23
TOLUENE 6159 4481 9570 6737 31
1,1,2-TRICHLOROETHANE 1786 1582 2707 2025 26
TETRACHLOROETHYLENE 983 500 1354 946 37
1,3-DICHLOROPROPANE 2998 2931 4653 3527 23
D IBRON OCHLOROMETHANE 1894 1682 3213 2263 30
1,2-DIBROMOETHANE 1743 1679 2753 2058 24
CHLORO BENZENE 3191 2021 5169 3460 38
1,1,1,2-TETRACHLOROETHANE 1565 1026 2404 1665 34
ETHYL BENZENE 5712 3003 8463 5726 39
p-XYLENE 3149 1635 6521 3102 38
o-XYLENE 4594 2671 7057 4774 38
STYRENE 2328 1087 2603 2006 33
BRONOFORM 996 865 1716 1192 31
ISCPROPYLBENZENE 2135 888 2381 1801 36
p-BROI4 OFLUORO SENZENE NI NI NI - -
BRON OSENZENE 4301 2806 - 7049 4719 37
1,1,2,2-TETRACHLOR OETHANE 3002 2563 5185 3583 32
1 ,2,3-TRICHLOROPROPANE 3507 3078 5840 4142 29
n-PROPYL BENZENE 6 037 1989 7072 5033 44
2-CHLOROTOLUENE 4570 1742 6124 4145 44
4-CHLOROTOLUENE 3746 1500 5279 3508 44
tert- BLJTYLBENZENE 3310 1135 3989 2811 43
1,3 ,5-TRIMETHYLBENZENE 4100 1483 4899 3494 42
sec-BUTYL BENZENE 4197 1262 4106 3188 43
1,2-DIBR ONO-3-CHLOROPR OPAJIE 1519 958 2576 1684 40
1,2 ,4-TRIMETHYLBENZENE 4667 2097 5901 4222 38
1,3-DICHL ORO SENZENE 1439 514 1845 1266 44
p-ISOPROPYL TOLUENE 2965 958 2937 2287 41
1,4 -DICHLORO BENZENE 1530 484 1960 1325 47
1,2-DICHLORO BENZENE-d4 NI NI NI - -
1,2-DICHLOROBENZENE 1386 507 2014 1302 47
n-BUTYL BENZENE 3644 1083 3274 2667 42
1,2,4-TRICHL ORO SENZENE 662 154 624 473 48
HEXACHLOROSUTADIENE 317 68 163 176 59
NAPHTHALENE 2980 1089 3843 2637 44
1 ,2 ,3-TRICHLORO BENZENE 634 137 613 461 50
NI not Included
22
-------
TABLE 13
25 n ANALYTE RESPONSE IN S/GARDEN SOIL
SaITpte 1 San Le 2 SaupLe 3 AVG RSD
ANALYTE Area Area Area Area (%)
DICHLOROOIFLUORONETHANE 154 126 203 161 20
CHLORONETHANE 577 210 420 402 37
VINYL CHLORIDE 530 453 455 479 7
BROMOMETHANE 33 141 33 69 74
CHLOROETHANE 44 209 56 103 73
TRICHLOROFLUOROMETHANE 2218 2154 2214 2195 1
11-DICHLOROETHENE 2875 2671 2974 2840 4
METHYLENE CHLORIDE 4.411 4194 4386 4330 2
trans-1,2-DICHLOROETHENE 1819 1491 1844 1718 9
1,1-DICHLOROETHANE 4188 3246 4439 3958 13
2 2-DICHLOROPROPANE 2830 1917 3501 2749 26
cla-1,2-DICHLOR OETHENE 819 521 2238 1193 63
BRON OCHLOROMETHANE 1285 932 1309 1175 15
CHLOROFORM 3440 2441 3824 3235 18
1,1,1-TRICHLOROETHANE 3524 2763 3873 3387 14
1,1-DICHLOROPROPENE 2273 1693 2191 2052 12
CARBON TETRACHLORIDE 3065 2062 3258 2795 19
BEMZENE 5556 4812 5556 5308 7
12-DICHLOROETHANE 1891 1267 2058 1739 20
TRICHLOROETHYLENE 2187 1526 1941 1885 14
1,2-DICHLOROPROPANE 1904 1364 1951 1740 15
DIBRONOMETHANE 852 502 881 745 23
BROM ICHLOROMETHANE 2479 1600 2736 2272 21
TOLUENE 6718 5343 7404 6488 13
1,1,2-TRICHLOROETHANE 1206 699 1416 1107 27
TETRACKLOROETNYLENE 1144 810 1205 1053 16
1,3-DICHLOROPROPANE 1158 657 1479 1098 31
DIBROMOCKLORONETHANE 1330 652 1441 1141 31
1,2•DIBROMOETNAIiE 609 584 958 717 24
CHLOROBENZENE 1192 803 1628 1208 28
1,1,1,2-TETRACHLOROETHANE 1285 720 1123 1043 23
ETHYL BENZENE 4499 2923 4703 4042 20
p-XYLENE 2866 1970 3066 2634 18
o-XYLENE 4600 2963 4450 4004 18
STYRENE 1199 572 35 602 79
BRO 0F0RN 534 353 661 516 24
ISOPROPYLBENZENE 2427 1586 2342 2118 18
p-BROMOFLUORO BENZENE NI NI NI - -
BROMO8ENZENE 2353 614 1577 1515 47
1,1,2 1 2-TETRACHLOROETHANE 2147 1303 2256 1902 22
1,2,3-TRICHLQROPROPANE 1555 885 1692 1377 53
n-PROPYL BENZENE 3916 2525 4291 3577 21
2-CHLOROTOLUENE 2497 191 2995 1894 64
4-CHLOROTOLUENE 1569 735 1507 1270 30
tert-BUTYLBENZENE 3010 1993 3658 2887 26
1,3,5-TRIMETHYLBENZENE 3522 2658 3514 3231 13
sec-BUTYL BENZEME 4034 2575 3694 3434 18
1,2-DIBRORO•3-CHLOROPROPANE 733 56 873 554 64
1,2 ,4-TRIMETHYLBEPIZENE 4747 4230 5409 4795 10
1,3-DICHLOROBENZENE 495 289 482 422 22
p-ISOPROPYL TOLUENE 2521 1533 2434 2163 21
1,4-DICHLOROBENZENE 653 392 647 564 22
1,2-DICHLOROBENZENE-d4 NI NI NI - -
1,2-DICHLORO BENZENE 400 379 420 400 4
n-BUTYL BENZENE 2607 1408 2203 2073 24
1,2,4-TRICHLORO BENZENE 77 • 73 75 47
HEXACHLOROSUTADIENE 123 92 62 92 27
NAPHTHALENE 1455 915 1826 1399 27
1,2,3-TRICHLORO8EUZENE 80 35 148 88 53
NI= not Included
23
-------
TABLE 14
25 ng ANALYTE RESPONSE IN MMS/HORIZION-C SOIL
SaITpLe 1 Sanpte 2 Sanpte 3 AVG RSD
ANALYTE Area Area Area Area (S)
DICHLORODIFLUOR 1ETHANE 51 109 122 94 33
CHL OROMETHAIIE 590 357 416 454 22
VINYL CHLORIDE 1484 1237 1269 1330 8
BRONONETHANE 45 60 54 53 12
CHIOROETNANE 531 639 258 476 34
TRICHLOROFLU OR ONETHANE 2973 3093 2841 2969 3
1 1-DICHLOROETHENE 5147 5031 4904 5027 2
METHYLENE CHLORIDE 6503 5884 5933 6107 5
trans•1,2-DICHLORO€THENE 5280 5537 4748 5188 6
1,1•DICHLOROETHANE 7717 7269 6967 7318 4
2 2-DICHLOROPROPAIIE 4395 4423 4075 4298 4
c s-1,2-DICHLOROETHENE 6128 5708 6097 5978 3
BRCIOCHIORONETHANE 4175 4627 44.62 4421 4
CHLOROFORM 7101 6989 6790 6960 2
1,1,1-TRICHLOROETHANE 5921 5410 5214 5515 5
1,1-DICHLOROPROPENE 4732 5131 4552 4805 5
CARBON TETRACHLOR IDE 4630 4799 4288 4572 5
BENZENE 10914 11000 10217 10710 3
1,2-DICHLOROETMAME 6530 6537 6075 6381 3
TRICHLOROETHYLENE 5060 5309 4769 5046 4
1 1 2-DICHLOROPR OPANE 4185 4071 3745 4000 5
DIBRONONETHAIIE 2758 2692 2772 2741 1
BRONODICHLORONETHANE 6084 5828 5761 5891 2
TOLUENE 13064 13635 11979 12893 5
1 1,2-TRICHLOROETHANE 2976 3217 3242 3145 4
TETRACHLOROETHYLENE 2425 2922 2464 2604 9
1,3-DICHLOROPROPANE 5192 4580 4607 4793 6
DIBRONOCHLORONETHANE 4098 4592 4018 4236 6
1,2-DIBRONOETHANE 3919 3831 3963 3904 1
CHLORO8ENZENE 8585 8665 6767 8006 11
1 1 1,2-TETRACHLOROETHANE 3772 3986 3629 3796 4
ETHYL BENZENE 19342 21042 17337 19260 8
p-XYLENE 14265 10995 8888 11383 19
o-XYLENE 20980 20474 15554 19003 13
STYRENE 9547 9390 6149 8362 19
BRONOFORM 2866 2868 2478 2737 7
ISOPROPYLBENZENE 7193 6592 5527 6437 11
p-BRONOFLUOR OBENZENE NI NI NI -
BRONOBENZENE 12040 12678 12464 12394 2
1,1,2,2-TETRACHLOROETHA NE 6324 6308 5747 6126 4
1,2,1-TRICHLOROPROPAIIE 5271. 4510 6852 5544 18
n-PROPYI. BENZENE 23135 23635 15424 20731 18
2-CHLOROTOLUENE 18909 18283 13328 16840 15
4-CHLOROTOLUENE 14206 13295 10874 12792 11
tert-BUTYLBENZENE 16483 12383 9723 12863 22
1,3,5-TRIMETHYLBENZENE 17519 16803 11909 15410 16
sec-SUTYL BENZENE 20807 17706 11795 16769 22
1,2-DIBRONO -3-CHLOROPROPANE 3514 3016 3163 3231 6
1,2,4-TRIHETHYLBENZENE 20414 16938 11426 16259 23
13-DICHLORO SENZENE 5902 5478 4115 5165 15
p-ISOPROPYL TOLUENE 13820 11720 8749 11430 18
1,4-DICHLOROSENZENE 6307 5594 4390 5430 15
1,2-DICHLORO SENZENE-d4 NI NI NI - -
1,2 -DICHLORO SENZENE 6359 5707 4312 5459 16
n-BUTYL BENZENE 16294 12648 9039 12660 23
1,2,4-TRICHLOROSENZENE 3503 2639 1919 2687 24
HEXACHLORO8UTADIENE 1958 1762 1131 1617 22
NAPHTHALENE 10866 9007 6559 8811 20
1,2,3-TRICHLOROBENZENE 3290 2899 1770 2653 24
NI= not IncLuded
24
-------
TABLE 15
RELATIVE ANALYTE RECOVERIES FOR FOUR MATRICES
PINS/SAND
AVG RSD RECOVERY
Area CX) CX)
PINS/GARDEN
AVG RSD RECOVERY
Area CX) (2)
PINS/HORIZON-C
AVG RSO RECOVERY
Area CX) CX)
PIllS/CLAY
AVG RSD RECOVERY
Area (2) (2)
DI CHLOROD I FLUOROMETHANE
CH L OR OM E I H ANE
VINYL CHLORIDE
BROMOIIETHANE
CHLOROETHANE
IR I CHLOROFLUOROMETHANE
1, 1-DICHLOROETHENE
METHYLENE CHLORIDE
trans-i ,2-DICHLOR0ETHENE
1,1 -DICHLOROETHAWE
2, 2-D I CHLOROPROPANE
C is-i, 2-0 ICHLOROETHENE
8ROM OCHLORONE THANE
CHLOROFORM
1,1, 1-TRICHLOROETHANE
1, 1-DICHLOROPROPENE
CARBON TETRACHLORIDE
BEN ZE NE
1,2-0! CHLOROETHAWE
IR ICHLOROETHYLENE
1, 2-D I CHLOROPROPANE
DI BROMOMETHANE
BROMOD I CHLOROMETHANE
TOLUENE
1,1 ,2-TRICHLOROETHANE
TETRACHIOROETHYLENE
1 ,3-DICHLOROPROPANE
DI BROMOCHLOROMETHANE
1,2-DIBROMOETHANE
CHLOROBENZENE
1,1,1 ,2-TETRACHLOROETHANE
ETHYL BENZENE
p- XYLE NE
o-XYLENE
STYRENE
BROMOFORM
I SOPROPYLBENZENE
p- BROMOFLUOROBENZENE
BR OMOBE N Z EN E
1,1,2, 2-TETRACIILOROETHAJIE
1 ,2,3-TRICHLOROPROPANE
n-PROPYL BENZENE
2-CHLOROTOLUENE
4-CHL OR OTOLUENE
tert-BUTYLBENZENE
1 ,3,5-TRIMETHYLBENZENE
sec-BUTYL BENZENE
1, 2-01 BROMO-3-CHLOROPROPANE
1 ,2,4-TRIMETHYLBENZENE
1 ,3-DICHLOROBENZENE
p ISOPROPYL TOLUENE
1, 4-0! CHLOROBENZENE
1,2-01 CHLOROBENZENE-d4
1 ,2-DICHLOROBEHZENE
n-BUTYL BENZENE
1 ,2,4-TRICHLOROBENZENE
HEXACHLOROBIJTAD IENE
WAPHIHALENE
1 ,2,3-TRICHLOROBENZENE
NI= not incLuded
164 44 33
775 10 65
1656 9 67
148 42 89
600 6 65
3761 6 71
6259 7 78
7569 1 85
6001 6 81
9273 5 87
4237 12 73
7051 1 77
5672 3 94
8387 3 88
6531 3 89
5909 3 84
5549 3 87
14743 3 87
9184 3 89
6296 4 81
4802 8 90
3533 1 98
7310 3 87
19677 4 164
3983 4 100
3833 11 90
6476 7 89
5574 4 98
4726 3 91
11075 4 83
5317 1 92
26235 2 85
17955 5 103
22680 3 80
8348 7 48
3362 8 89
9334 6 87
NI - -
17581 6 93
8022 3 95
7490 16 80
27107 6 87
24763 7 87
20877 1 95
20987 7 95
26847 9 90
31773 5 94
4276 6 92
26210 95
8182 6 80
22003 5 86
9024 4 91
NI - -
8181 16 86
27107 6 87
5253 5 75
3885 6 87
16109 7 77
4641 3 70
161 20
402 37
479 7
69 74
103 73
2195 1
2840 4
4330 2
1718 9
3958 13
2749 24
119363
1175 15
3235 18
3387 14
2052 12
2795 19
5308 7
1739 20
1885 14
1740 15
745 23
2272 21
6488 13
1107 27
1053 16
1098 31
1141 31
717 24
1208 28
1043 23
4042 20
2634 18
4004 18
602 79
516 24
2118 18
NI
1515 47
1902 22
1377 53
357•7 21
1894 64
1270 30
2887 24
3231 13
3434 18
554 64
4795 10
422 22
2163 21
564 22
NI -
400 4
2073 24
75 47
92 27
1399 27
88 53
33 94 33
34 454 22
19 1330 8
62 53 12
11 476 34
42 2969 3
35 5027 2
49 6107 5
23 5188 6
37 7318 6
48 4298 4
13 5978 3
20 4421 4
34 6960 2
46 5515 5
29 4805 5
44 4572 5
31 10710 3
17 6381 3
24 5046 4
33 4000 5
21 2741 1
27 5891 2
16 12893 5
28 3145 4
25 2604 9
15 4793 6
20 4236 6
14 3904 1
9 8006 11
18 3796 4
13 19240 8
15 11383 19
14 19003 13
3 8362 19
14 2737 7
20 6437 11
- NI -
8 12394 2
22 6126 4
15 642 126
9 20731 18
7 16840 15
6 12792 11
13 12863 22
11 15410 16
10 16769 22
12 3231 6
17 16259 23
4 5165 15
8 11430 18
6 5430 15
- NI -
4 5459 16
7 12660 23
1 2687 24
2 1617 22
7 8811 20
1 2653 24
AWALYTE
38
885
4
35
54
1693
3
44
32
81
35
43
52
410
8
48
56
2310
4
42
62
4377
9
47
67
5151
9
65
70
3703
9
48
69
5390
13
54
74
1863
18
40
66
4208
13
54
76
3373
14
67
73
4462
18
55
75
2957
21
47
68
2853
21
46
71
2424
20
43
63
6658
16
59
62
5236
16
82
65
2664
22
47
75
2629
24
57
76
1920
17
68
70
3782
23
59
119
6737
31
48
79
2025
24
64
61
946
37
32
66
3527
23
69
74
2263
30
61
75
2058
24
69
60
3460
38
43
66
1665
34
51
62
5726
39
40
65
3102
38
33
67
4774
38
39
48
2006
33
24
72
1192
31
63
60
1801
36
27
-
NI
-
-
65
4719
37
42
72
3583
32
57
59
4142
29
67
53
5033
44
25
59
4145
44
29
58
3508
44
25
58
2811
43
21
52
3494
42
20
49
3188
43
17
70
1684
40
62
59
4222
38
25
50
1266
44
23
45
2287
41
18
55
1325
47
23
-
NI
-
57
1302
47
25
41
2667
42
16
38
473
48
13
36
176
59
9
42
2637
44
24
40
461
50
13
25
-------
TABLE 16
DETERMINATION OF S RECOVERY
25 ng FORTIFIED NMSISAND
INTERNAL STANDARD FLUOROSENZENE
NO RECOVERED
RSD RECOVERY
AMALYTE Sanpte 1 Sanpte 2 Sanpte 3 AVG ( 5) ( 5)
DICHLORODIFLUORONETHANE 9.8 11.2 8.3 9.8 11.9 39.1
CHL OR OMETHANE 10.1 13.0 10.5 11.2 11.2 44.8
VINYL CHLORIDE 10.4 13.9 10.7 11.7 13.7 46.7
BROMONETHANE HF 13.7 6.9 10.3 33.1 41.2
CHLOROETHANE 11.7 15.3 10.4 12.5 16.8 49.8
TRICHLOROFLUOR OMETHANE 11.3 16.3 11.8 13.2 17.2 52.6
1,1-DICHLOROETHENE 11.4 11.6 10.8 11.2 2.8 45.0
METHYLENE CHLORIDE III NI NI -
trans-1,2•DICHLOR OETHENE 15.7 16.3 15.4 15.8 2.4 63.1
1,1-DICHLOROETHANE 16.5 17.0 16.9 16.8 1.3 67.3
2 2 -DICHLOROPROPANE 23.4 24.4 26.5 24.8 5.1 99.1
C%S-1,2-DICHLOROETHENE 18.0 19.1 19.3 18.8 3.2 75.2
BRCMOCHLORONETHAJIE 16.5 17.2 17.2 17.0 1.9 67.9
CHLOROFORM 19.9 21.5 20.6 20.7 3.3 82.6
1,1,1-TRICHLOROETHANE 19.8 21.7 20.8 20.8 3.8 83.1
1,1-DICHLOROPROPENE 20.0 21.1 20.1 20.4 2.5 81.6
CARBON TETRACHL0RIDE 20.6 20.7 20.6 20.6 0.2 82.4
BENZENE 25.9 27.5 26.8 26.7 2.5 106.9
1,2-DICHLOROETHA NE 24.3 26.8 26.5 25.9 4.4 103.4
TRICHLOROETNYLENE 22.0 23.4 22.6 22.7 2.4 90.6
1,2-DICHLOROPROPANE 21.3 23.8 23.3 22.8 4.7 91.2
DIBROMOMETHANE 19.6 22.9 21.4 21.3 6.3 85.2
BROMODICHLORONETHANE 23.2 26.3 25.6 25.0 5.3 100.1
TOLUENE 27.3 30.4 28.6 28.8 4.4 115.1
11,2-TRICHLOR OETHAiIE 23.3 25.3 25.5 24.7 4.0 98.8
TETRACHIOROETHYLENE 25.6 27.5 27.5 26.8 3.7 107,2
1,3-DICHLOR OPR OPANE 24.2 28.0 28.0 26.7 6.6 106.9
DIBROMOCHLOR OHETHA NE 22.3 24.6 24.7 23.9 4.6 95.5
1,2-DIBRONOETHANE 21.4 23.7 22.8 22.6 4.3 90.5
CHLOROBENZENE 25.1 28.0 27.4 26.8 4.6 107.3
1,1,1,2•TETRACHLOROETHANE 27.9 33.0 31.7 30.9 6.9 123.4
ETHYL BENZENE 32.1 35.7 34.3 34.1 4.3 136.2
p-XYLENE 31.0 34.8 34.9 33.6 5.4 134.3
o-XYLENE 29.6 32.7 32.7 31.7 4.6 126.7
STYRENE 22.1 22.6 20.4 21.7 4.2 86.8
BROMOFORN 24.0 26.1 28.0 26.0 6.2 104.1
ISOPROPYLBENZENE 30.2 34.1 33.2 32.5 5.1 129.8
p-BR OM OFLUOROBENZENE 28.3 30.3 29.5 29.4 2.7 117.4
BRCN08ENZENE 20.6 23.3 31.1 25.0 17.8 100.0
1,1 2,2-VETRACHL0R0ETHANE 20.9 - 22.9 29.3 24.4 14.6 97.4
1,2,3-TRICHL OROPROPANE 31.6 34.7 33.5 33.3 3.9 133.0
ri-PROPYL BENZENE 22.1 24.3 24.4 23.6 4.4 94.4
2-CHLOROTOLUENE 21.6 23.9 23.6 23.0 4.5 92.2
4-CHLOROTOLUENE 24.1 26.7 26.4 25.7 4.4 102.9
tert•BUTYLBENZEME 22.0 24.2 23.8 23.4 4.2 93.5
1,3 5-TRIMETHYLBENZENE 20.8 23.5 23.4 22.6 5.5 90.4
sec-BUTYL BENZENE 21.8 24.1 23.9 23.2 4.5 93.0
1,2-DIBROMO-3-CHLOROPROPANE 17.3 18.7 18.9 18.3 4.0 73.2
1,2,4-TRIMETHYLBENZENE 21.3 23.5 23.4 22.7 4.5 90.8
1,3-DICHLOR OBENZENE 21.1 24.0 23.7 23.0 5.6 91.8
pISOPROPYL TOLUENE 21.5 23.9 23.8 23.1 4.7 92.2
1,4-DICHLOROBENZENE 20.6 23.6 23.3 22.5 6.0 90.1
1,2-DICHL OROSENZENE -d6 14.3 17.4 15.3 15.7 8.3 62.7
1,2-OICHL OROBENZENE 21.1 23.1 23.6 22.6 4.8 90.4
n-BUTYL BENZENE 20.8 22.8 22.5 22.0 4.1 88.1
1,2,4-TRICHL OROBENZENE 20.7 22.5 21.9 21.7 3.3 86.8
HEXACHLOROBUTADIENE 19.7 22.2 20.6 20.8 5.0 83.4
NAPHTHALENE 21.2 23.3 23.3 22.6 4.5 90.4
1,2,3-TRICHLOROBENZENE 18.9 21.1 19.9 20.0 4.6 79.9
NF not fotx d
NI not r cLuded
26
-------
TABLE 17
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/CLAY
INTERNAL STANDARD FLUOROBENZENE
HG RECOVERED
RSD RECOVERY
ANALYTE Sauple 1 Sanpte 2 Sanple 3 AVG (%) (%)
DICHLORODIFLUORCMETHAHE 14.8 13.4 14.3 14.2 4.1 56.6
CHLORONETHANE 26.6 21.1 30.4 26.0 14.6 104.2
VINYL CHLORIDE 19.0 17.5 19.6 18.7 4.7 74.9
BR 4OMETHANE HF HF HF -
CHLOROETHANE 19.9 19.3 18.5 19.3 2.9 79.2
TRICHLOROFLUORONETHANE 22.3 19.0 17.8 19.7 9.7 78.8
1,1-DICHLOROETHENE 15.7 12.2 7.7 11.9 27.3 47.4
METHYLENE CHLORIDE NI NI NI -
trans-12 -DICHLOROETHENE 18.9 14.8 16.1 16.6 10.3 66.5
1,1-DICHLOROETHANE 22.8 16.9 20.0 19.9 12.1 79.5
2 2-DICHLOROPROPAJIE 21.9 21.2 23.6 22.2 4.6 88.9
cls-1,2-DICHLOR OETHENE 23.1 18.1 20.1 20.4 10.0 81.7
BROMOCHLOROMETHAIIE 26.3 19.2 23.1 22.9 12.6 91.5
CHLOROFORM 26.4 21.2 22.9 23.5 9.2 93.9
1,1,1-TRICHLOROETHANE 23.2 17.7 21.0 20.7 11.0 82.6
1 1 1-DICHLOROPROPENE 19.4 16.0 17.3 17.6 8.0 70.4
CARBON TETRACHLORIDE 17.8 15.8 15.3 16.3 6.7 65.3
BEHZENE 29.2 22.7 25.7 25.9 10.2 103.5
1 1 2-DICHLOROETHANE 37.4 29.6 32.4 33.1 9.7 132.6
TRICHLOR OETHYLENE 21.2 18.7 18.3 19.4 6.6 77.5
1,2-DICHLOROPROPANE 30.2 23.6 26.6 26.8 10.1 107.2
DIBRONOMETHANE 32.9 25.2 29.5 29.2 10.7 116.8
BROMODICHLORONETHANE 30.8 26.3 29.5 28.8 6.5 115.4
TOLUENE 23.6 22.8 22.2 22.9 2.6 91.5
1,1,2-TRICHLOROETHAHE 34.0 28.1 35.2 32.5 9.6 129.9
TETRACHIOROETHYLEHE 15.2 16.1 15.9 15.7 2.6 62.9
1 3-DICHLOROPROPANE 32.7 29.3 32.1 31.4 4.8 125.5
DIBROMOCHIORONETHANE 26.8 24.5 26.8 26.0 4.2 104.1
1,2-DIBROMOETHANE 28.4 24.5 26.4 26.4 6.0 105.6
CHLOROBEMZENE 17.0 19.1 18.4 18.2 4.9 72.6
1,1 .1,2-TETRACHL OROETHANE 22.1 23.4 22.8 22.8 2.2 91.1
ETHYL BENZENE 17.3 20.1 19.5 18.9 6.6 75.7
p-XYLEME 16.9 20.5 18.5 18.7 7.8 74.6
o-XYLENE 17.2 19.2 18.6 18.3 4.6 73.3
STYRENE 2.2 3.1 2.5 2.6 13.7 10.4
BRONOFORM 26.3 26.3 27.2 26.6 1.6 106.5
ISOPROPYLBENZENE 11.6 14.9 13.4 13.3 10.1 53.2
p-BR ONOFLUOROBENZENE 15.3 16.8 17.3 16.5 5.3 65.8
BRONO BENZEHE 17.4 20.3 20.9 19.5 7.8 78.2
1,1,2,2-TETRACHLOROETHANE 28.8 - 26.9 30.4 28.7 4.9 114.8
1,2,3 -TRICHL OROPR OPAHE 39.6 18.3 43.2 33.7 32.6 134.8
n-PROPYL SENZEME 9.1 12.9 11.7 11.2 14.0 44.8
2-CHLOROTOLUENE 11.1 15.5 13.7 13.4 13.5 53.6
4-CHLOROT OLUENE 12.4 17.3 12.4 14.0 16.7 56.1
tert-BUTYLBENZENE 8.1 11.0 10.9 10.0 13.5 40.0
1,3,5-TRIMETHYLBENZENE 9.3 12.1 10.9 10.8 10.8 43.1
sec-BUTYL BENZENE 7.1 9.4 8.5 8.3 11.1 33.3
1 1 2-DIBR ONO-3-CHLOROPROPANE 22.3 22.0 29.9 24.7 14.7 98.9
1,2,4 -TRIMETHYLBENZENE 12.1 14.7 14.2 13.7 8.1 54.7
1,3-DICHL OROBEMZENE 7.6 12.2 9.8 9.9 18.8 39.6
p-ISOPROPYL TOLUENE 6.7 8.3 8.6 7.9 10.7 31.4
1,4-DICHLORO SENZENE 7.5 12.0 9.7 9.7 18.8 38.9
1 1 2-DICHLOROBENZENE-d4 4.0 5.8 4.5 4.8 16.2 19.1
1,2-DICHLOROBENZENE 8.9 10.9 11.5 10.5 10.6 41.9
n-BUTYL BENZENE 5.4 6.5 6.5 6.1 8.6 24.5
1,2,4-TRICHLOROBENZEHE 2.8 5.6 4.1 4.2 26.6 16.7
HEXACHLOROBUTADIENE 1.5 3.0 3.6 2.7 32.6 10.9
NAPHTHALENE 7.8 9.8 10.9 9.5 13.4 37.9
1,2,3-TRCCHLOROBENZENE 2.7 5.3 4.4 4.1 26.3 16.5
NF not found
HI’ not incLuded
27
-------
TABLE 18
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MNS/GARDEH SOIL
INTERNAL STANDARD FLUOROBENZENE
NG RECOVERED
RSD RECOVERY
ANALYTE Sanpte 1 SaITpte 2 SanpLe 3 AVG (%) (%)
DICHLOR IFLUORONETHANE 20.7 24.9 24.4 23.4 8.1 93.4
CHLORONETHANE 23.4 28.0 29.9 27.1 10.0 108.4
VINYL CHLORIDE 19.6 26.5 26.5 24.2 13.4 96.8
BROMONETHANE HF HF HF - - -
CHLOROETHANE 2.4 10.4 16.3 9.7 58.7 38.7
TRICHL OROFLUOROMETHAHE 25.3 33.5 33.2 30.6 12.4 122.6
1 1-DICHLOROETHENE 18.7 22.5 23.0 21.4 9.0 85.6
NETHYLENE CHLORIDE NI NI NI NI
trans-1 1 2-DICHLOROETHENE 10.1 13.8 13.5 12.5 13.7 49.8
1,1-DICHLOROETHANE 22.5 29.9 27.4 26.6 11.5 106.4
2 2-DICHLOROPROPANE 36.5 44.5 41.3 40.7 8.1 163.0
c s -1,2-DICHLOROETHENE 17.1 23.1 20.6 20.3 12.1 81.1
BROROCHLOR OMETHANE 13.6 19.9 15.0 16.1 16.7 64.6
CHLOROFORM 21.6 32.8 25.5 26.6 17.5 106.5
1,1,1-TRICHLOROETHANE 33.1 41.6 35.3 36.7 9.8 146.6
1,1-DICKLOROPROPENE 17.9 25.7 22.1 21.9 14.6 87.6
CARBON TETRACKLORIDE 21.6 27.5 23.8 24.3 10.0 97.1
BENZENE 21.9 32.9 24.6 26.5 17.7 105.9
1,2-DICKLOROETHAIIE 19.2 29.1 21.6 23.3 18.1 93.1
TRICKLOROETHYLENE 14.9 20.1 17.4 17.5 12.2 69.9
1,2-DICHLOROPROPANE 22.7 35.2 24.9 27.6 19.8 110.3
DIBROMOMETHANE 13.3 20.4 15.0 16.2 18.8 65.0
BROM ICHLOR0NETHANE 17.1 23.3 19.0 19.8 13.0 79.2
TOLUENE 23.0 38.7 22.2 28.0 27.2 111.8
1,1,2-TRICHL OROETHAHE 17.0 25.3 20.8 21.0 16.1 84.1
TETRACKLOROETHYLEHE 16.4 21.5 19.1 19.0 10.9 76.1
1,3-DICHLOR OPROPANE 12.4 18.2 14.3 14.9 16.2 59.8
DIBROMOCKLOROMETHANE 11.0 15.0 11.6 12.5 14.0 50.1
1,2-DIBROMOETI4ANE 9.0 12.3 9.1 10.1 15.3 40.4
CHLORO BENZENE 6.7 8.5 6.0 7.1 15.3 28.2
1 ,1 ,1 ,2-TETRACHLOROETHANE 22.5 23.4 22.0 22.6 2.6 90.5
ETHYL BENZENE 16.4 21.5 15.0 17.7 15.8 70.6
p-XYLENE 16.2 22.0 13.4 17.2 20.8 68.8
o-XYLENE 13.0 17.4 10.5 13.6 21.0 54.5
STYRENE 4.9 3.5 2.8 3.7 23.6 15.0
BRONOFORM 9.9 13.3 10.1 11.1 14.1 44.4
IS OPROPYLBENZEHE 13.9 16.7 12.4 14.3 12.4 57.2
p-BRON OFLU OROBENZENE 4.8 7.2 5.9 6.0 17.0 23.8
BRONOBENZEME 5.7 6.9 6.2 6.2 7.6 25.0
1,1,2 ,2-TETRACHLOROETHANE 172 21.1 16.3 18.2 11.5 72.8
1,2,3-TRICKLOROPROPANE 20.7 - 21.0 16.9 19.5 9.6 78.1
n-PROPYL BENZENE 8.8 12.7 8.8 10.1 18.3 40.2
2-CHLOROTOLUENE 13.1 16.6 12.1 13.9 13.6 55.7
4-CHLOROTOLUENE 14.7 18.5 13.6 15.6 • 13.5 62.5
tert-8UTYLBEHZENE 122 11.9 12.5 12.2 1.9 48.8
1,3,5-TRIMETHYLBENZENE 12.0 13.5 11.5 12.3 6.7 49.3
SecBUTYL BENZENE 12.5 13.4 9.8 11.9 12.9 47.6
1,2-DIBROMO-3-CHLOROPROPANE 16.8 17.5 11.6 15.3 17.2 61.3
1,2 1 4-TRIMETHYLBENZENE 13.9 16.2 7.0 12.4 31.5 49.4
1,3-DICHL ORO8EHZENE 4.0 5.0 2.9 4.0 22.5 15.9
p-ISOPROPYL TOLUENE 9.6 12.5 8.6 10.2 16.4 40.9
1,4-DICHLOROBENZENE 4.0 5.0 3.7 4.2 12.5 16.9
1,2-DICHLORO BENZEHE-d4 1.8 1.7 1.2 1.6 16.8 6.2
1,2-DICHLORO SENZENE 4.3 4.6 3.8 4.2 7.3 17.0
n-BUTYL BENZENE 8.2 10.9 6.1 8.4 23.5 33.6
1 ,2,4-TRICHLOROBENZEHE 4.8 6.3 3.5 4.8 23.5 19.3
HEXACHLOROSUTADIENE 1.5 3.2 1.9 2.2 33.1 8.9
NAPHTHALENE 9.9 12.2 9.5 10.5 11.3 42.2
1,2,3-TRICHLOROBENZENE 1.0 3.9 1.9 2.3 52.4 9.0
NF=not fow d
NI not incLuded
28
-------
TABLE 19
DETERMINATION OF RECOVERY
25 ng FORTIFIED MNS/SAND
INTERNAL STAJITARD BENZENE-d6
HG RECOVERED
RSO RECOVERY
ANALYTE Sanpte 1 Sanpte 2 SanpLe 3 AVG ( ) (X)
DICHLORODIFLUOROMETHANE 10.3 11.5 8.7 10.2 11.0 40.6
CHLORONETNANE 13.1 15.5 12.7 13.8 8.8 55.0
VINYL CHLORIDE 11.3 8.8 11.0 10.4 11.1 41.5
BROMONETHANE 17.3 8.0 12.6 37.0 50.4
CHL OROETHANE 12.1 15.6 10.8 12.8 15.8 51.3
TRICHLOROFLUORONETHANE 12.6 17.1 12.9 14.2 14.2 56.8
1,1-DICHLOROETHENE 12.0 12.0 11.5 11.9 2.1 47.4
METHYLENE CHLORIDE NI NI NI - - -
trans -1,2-DICHLOROETHENE 16.6 16.9 16.3 16.6 1.3 66.5
1,1-DICHLOROETHAME 17.4 17.6 17.9 17.6 1.1 70.5
2 2 -DICHLOROPROPANE 24.2 26.9 27.3 25.5 5.3 101.9
c s-1,2-DICHLOR0ETHENE 18.8 19.7 20.3 19.6 3.1 78.5
BROMOCHLORCNETHANE 17.5 17.8 18.2 17.8 1.7 71.3
CHLOROFORM 21.1 22.3 21.9 21.8 2.3 87.0
1 1 1,1-TRICHLOROETHANE 20.8 21.3 21.9 21.3 2.2 85.3
1 1 1-DICHLOROPROPENE 21.0 21.8 21.2 21.3 1.5 85.3
CARBON TETRACHLORIDE 21.9 21.6 22.0 21.8 0.8 87.2
BENZENE 27.0 28.1 28.0 27.7 1.9 110.9
1,2-DICHLOROETHANE 25.4 27.5 27.8 26.9 4.0 107.5
TRICHLOROETHYLENE 23.1 24.0 23.7 23.6 1.6 94.3
1 2DICHLOROPROPANE 22.4 24.4 24.5 23.8 4.2 95.1
DIBRONOHETHANE 20.6 23.5 22.6 22.2 5.5 88.9
BROMODICHLORONETHANE 24.3 27.0 26.8 26.0 4.7 104.1
TOLUENE 28.5 31.1 30.0 29.9 3.6 119.4
1,1,2-TRICHLOR OETHANE 24.4 25.9 26.8 25.7 3.8 102.9
TETRACHLOROETIIYLENE 26.6 28.2 28.8 27.8 3.4 111.4
1,3-DICHLOROPROPANE 25.4 28.6 29.3 27.8 6.2 111.1
DI8RONOCHLOROMETHANE 23.3 25.2 25.9 24.8 4.4 99.2
1 1 2-DI BRONOETHANE 22.4 24.4 24.0 23.6 3.6 94.2
CHLOROBENZENE 26.3 28.6 28.7 27.9 6.1 111.4
1,1 1 1,2-TETRACHLOROETHANE 29.2 33.6 33.2 32.0 6.2 128.1
ETHYL BEHZENE 33.4 36.3 35.7 35.1 3.6 140.5
p-XYLENE 32.4 35.7 36.6 34.9 5.1 139.7
o-XYLENE 30.8 33.4 34.0 32.7 4.3 130.8
STYRENE 23.1 23.2. 21.5 22.6 3.4 90.5
BRONOFORM 25.0 26.7 29.2 27.0 6.3 107.9
ISOPROPYLBENZENE 31.4 34.7 34.6 33.6 4.5 134.3
p-BROMOFLUOR OBENZENE 29.5 30.9 30.8 30.4 2.1 121.6
BROMOBENZENE 21.6 24.0 32.5 26.0 18.0 104.0
1,1,2,2-TETRACHLOROETHANE 22.0 23.5 30.6 25.4 14.8 101.4
1,2,3-TRICHLOROPROPANE 32.8 35.3 34.9 34.3 3.2 137.3
n-PROPYL BENZEHE 23.2 24.9 25.5 24.5 6.1 98.2
2-CHLOROT OLUENE 22.6 24.6 24.8 24.0 4.1 96.0
4-CHLOROT OLUENE 25.2 27.4 27.6 26.7 4.0 107.0
tert-BUTYLBENZENE 23.1 24.9 25.1 24.3 3.7 97.4
1,3,5-TRIMETHYLBENZENE 21.8 24.1 24.5 23.5 5.2 93.9
sec-BUTYL BENZENE 22.8 24.7 25.1 24.2 4.1 96.8
1 2-DIBRONO-3 -CHLOROPROPANE 18.0 19.2 19.8 19.0 3.9 76.1
1,2,4-TRIMETHYLBENZENE 22.2 24.0 24.5 23.6 4.3 94.4
1 9 3-DICHL OROBENZENE 22.2 24.7 26.9 23.9 5.2 95.6
p-ISOPROPYL TOLUENE 22.6 24.5 25.0 24.0 4.4 96.1
1,4-DICHLOROBE HZENE 21.6 24.3 24.5 23.5 5.6 93.9
1 2-DICHLOROBENZENE-d4 15.7 18.3 16.9 17.0 6.4 67.9
1,2-DICHLOROBENZENE 22.1 23.8 24.7 23.5 4.7 94.1
n-BUTYL BENZENE 21.8 23.5 23.7 23.0 3.6 91.9
1,2,4-TRICHL OROBENZENE 21.7 23.1 23.0 22.6 2.8 90.4
HEXACHLOROBUTADIENE 20.7 22.8 21.7 21.7 6.1 86.9
NAPHTHALENE 22.2 23.9 24.5 23.5 4.2 94.1
1,2,3-TRICHLOROBENZENE 19.8 21.7 20.9 20.8 3.8 83.1
NF not foi. d
NI not included
29
-------
TABLE 20
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMSICLAT
INTERNAL STANDARD BENZENE-d6
HG RECOVERED
RSD RECOVERY
ANALYTE Sanpte 1 SairpLe 2 Saffpte 3 AVG CX) CX)
DICKLORCOIFLUORONETHANE 14.2 13.4 13.4 13.7 2.7 56.8
CHLORONETHANE 25.6 21.1 28.5 25.1 12.1 100.2
VINYL CHLORIDE 18.5 17.4 16.9 17.6 3.7 70.4
BROMOMETHANE HF HF HF
CHLOROETHANE 18.9 19.1 17.1 18.3 4.9 73.4
TRICHLOROFLUORONETHANE 21.5 19.0 16.8 19.1 10.2 76.5
1,1-DICHLOROETHEME 15.1 12.3 7.3 11.6 27.8 46.2
METHYLENE CHLORIDE NI NI NI - -
trans-1 2•DICHLOR0ETHENE 18.1 14.9 15.0 16.0 9.3 64.0
1,1-DICHLOR OETHANE 21.9 16.9 18.8 19.2 10.7 76.9
2 2-DICHLOROPROPANE 21.3 21.2 22.6 21.7 3.0 86.9
cls-1,2-DICHLO ROETHENE 22.3 18.1 19.0 19.8 9.0 79.1
BRONOCHLORONETHANE 26.9 19.2 21.4 21.8 10.8 87.4
CHLOROFORM 24.6 21.0 20.8 22.2 7.9 88.6
1,1 1 1-TRICHLOROETHANE 22.3 17.7 19.7 19.9 9.4 79.6
1,1-DICHLOROPROPENE 18.7 16.1 16.2 17.0 7.0 67.9
CARBON TETRACKLORIDE 17.3 15.9 14.4 15.9 7.4 63.5
BENZENE 27.9 22.6 24.0 24.8 8.9 99.3
1,2-DICKLOROETHANE 35.4 29.4 30.0 31.6 8.6 126.3
TRICHLOROETHYLENE 20.4 18.7 17.2 18.8 6.9 75.0
12-DICHLOR OPR OPANE 28.7 23.5 24.6 25.6 8.7 102.4
DIBRONOMETHANE 31.2 25.1 27.3 27.9 9.0 111.5
BRONODICHLORONETIIANE 29.3 26.1 27.4 27.6 4.7 110.4
TOLUENE 22.6 22.6 20.6 21.9 4.3 87.7
1,1,2-TRICHLOROETHANE 32.3 27,9 32.6 30.9 6.8 123.4
TETRACHLOROETHYLEHE 14.6 16.2 14.9 15.2 4.3 61.0
1,3-DICHLOROPROPAHE 31.1 24.4 29.7 28.4 10.2 113.7
DIBROMOCHLORONETHANE 25.7 24.4 25.1 25.1 2.2 100.3
1,2-DIBROIIOETHANE 27.1 24.4 24.6 25.4 5.0 101.5
CHLOROBENZENE 16.4 19.1 17.2 17.6 6.5 70.3
1,11,2-TETRACHLOROETHANE 21.1 23.2 21.1 21.8 4.6 87.3
ETHYL BENZEHE 16.7 20.1 18.2 18.3 7.6 73.3
p-XTLEHE 16.3 20.5 17.3 18.0 9.9 72.1
o-XYLENE 16.6 19.2 17.5 17.7 6.0 71.0
STYRENE 2.1 3.1 2.3 2.5 16.2 10.0
BROMOFORM 25.4 26.2 25.5 25.7 1.5 102.8
ISOPROPYLBENZENE 11.2 15.0 12.6 12.9 11.9 51.7
p-BROMOFLUOROBENZEHE 16.8 16.8 16.3 15.9 5.4 63.8
BROMOBENZENE 16.8 20.3 19.6 18.9 7.9 75.5
1,1,2,2-TETRACHLOR OETHANE 27.5 26.8 28.2 27.5 2.1 110.0
1,2 ,3-TRICHL.OROPROPANE 37.8 - 18.2 40.2 32.1 30.8 128.3
n-PROPYL BENZENE 8.8 12.9 11.0 10.9 15.3 43.7
2-CHLOROTOLUENE 10.7 15.5 12.9 13.0 15.1 52.2
4-CHLOROTOLUENE 12.0 17.4 11.6 13.7 19.2 54.7
tert-BUTYLBENZEHE 7.9 11.1 10.2 9.7 14.1 38.9
1,3,5-TRINETHYLBENZENE 9.0 12.2 10.2 10.5 12.6 42.0
sec-BUTYL BENZENE 6.9 9.5 8.0 8.1 12.7 32.5
1,2-DIBRONO-3-CHL OROPR OPANE 21.4 21.9 27.6 23.6 11.8 94.5
1,2,4-TRINETHYLBENZENE 11.7 14.8 13.3 13.3 9.3 53.1
1,3-DICHLORO BENZENE 7.4 12.3 9.3 9.7 20.6 38.7
p-ISOPROPYL TOLUENE 6.5 8.4 8.1 7.7 10.8 30.6
1,4-DICHLOROSENZENE 7.3 12.1 9.1 9.5 20.7 38.0
1,2-DICHLORQBENZENE-d4 3.9 6.0 4.2 4.7 19.1 18.8
1 ,2-DICHL OROBENZENE 8.7 11.0 10.9 10.2 10.5 40.8
n-BtJTYL BENZENE 5.2 6.5 6.2 6.0 9.2 23.9
12 ,4-TRICHLOROBENZENE 28 5.6 3.9 41 28.6 16.4
HEXACHLOR OBUTADIEHE 1.5 3.0 3.4 2.7 31.9 10.6
NAPHTHALEHE 7.6 9.9 10.2 9.2 12.8 36.9
1,2,3-TRICHLORO BENZENE 2.6 5.4 4.2 4.0 27.7 16.2
NF not fotuid
NI not incLuded
30
-------
TABLE 21
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMSIGARDEN SOIL
INTERNAL STANDARD BENZENE-d6
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUOROMETHANE 21.4 25.1 24.4 23.7 6.7 94.6
CHLOROMETHANE 23.8 28.1 29.8 27.2 9.3 108.9
VINYL CHLORIDE 19.9 26.6 26.5 24.3 12.9 97.2
BRONOMETHANE NF NF NF - — -
CHLOROETHANE 2.4 11.5 16.1 10 0 56.8 40.0
TRICHLOROFLUOROMETHANE 25.6 33.5 33 0 30.7 11.7 122.8
1,1-DICHIOROETHENE 19.1 22.7 23.0 21.6 8.3 86.4
METHYLENE CHLORIDE NI NI NI — - —
trans-1 ,2-DICHLOROETHENE 10.4 14.1 13.6 12.7 13.0 50.7
1.1-DICHLOROETHANE 22.9 30.0 27.4 26.7 10.9 106.9
2.2-DICHLOROPROPANE 36.7 44.6 41.2 40.9 7.9 163.4
cls-1,2—DICHLOROETHEHE 17.5 23.3 20.7 20.5 11.6 81.9
BROMOCHLCROMETKANE 13.9 20.1 15.1 16.4 16.3 65.5
CHLOROFORM 21.9 32.6 25.3 26.6 16.7 106.4
1,1 ,1-TRICHLOROETHANE 33.5 41.8 35.2 36.8 9.7 147.4
1 ,1-DICHLOROPROPENE 18.3 25.9 22.1 22.1 14.0 88.3
CARBON TETRACKLORIDE 22.2 28.1 24.2 24.8 9.9 99.4
BENZENE 22.2 33.1 24.6 26.6 17.6 106.5
1.2-DICHLOROETHANE 19.6 29.2 21.6 23.5 17.6 93.8
TRICHIOROETHYLENE 15.2 20.3 17.5 17.7 11.7 70.8
1.2-DICHLOROPROPANE 23.0 35.1 24.9 27.6 19.1 110.6
DIBROMOMETHANE 13.6 20.6 15.1 16.5 18.4 65.8
BRONOOICHLOR OMETHANE 17.5 23 5 19.1 20.0 12 7 80.0
TOLLJENE 23.2 38.8 22.1 28.1 27 2 112.3
1 ,1.2-TRICHLOROETHANE 17.3 25.4 20.9 21.2 15.6 84.9
TETRACHLOROETHYLENE 16.6 21 6 19.1 19.1 10.6 76 4
1 ,3-DICHLOROPROPANE 12.7 18.4 14.4 15.2 15.8 60.6
DI BROM OCHLOROMETHANE 11.3 15.2 11.7 12.7 13.7 51.0
1,2-DIBROMOETHANE 9.2 12.5 9.2 10.3 15.1 41.2
CHLOROBENZENE 6.7 8.6 6.0 7.1 15.4 28.4
1 ,1,1 ,2-TETRACKLOROETHANE 22.9 23.6 22.0 22.8 2.8 91.2
ETHYL BEMZENE 16.6 21.6 15.0 17.8 15.9 71.0
p—XYLENE 16.5 22.1 13.3 17.3 21.0 69.2
o—XYLENE 13.1 17.5 10 5 13.7 21.2 54.8
STYRENE 5 0 3.6 2.8 3.8 24.2 15.1
BROMOFORM 10.1 13.5 10.3 11.3 14.0 45.2
ISOPROPYLBENZENE 14.1 16.8 12.3 14.4 12.6 57.6
p-BROMOFLUOROBENZENE 4.9 7.4 6.0 6.1 16 7 24.4
BR ONOBENZENE 5.9 7.0 6.3 6.4 7.3 25.6
1.1.2,2-TETRACHLOROETHANE 17.6 21.3 16.4 18.4 11.4 73.7
1 ,2.3-TRICHLOROPROPANE 21.1 21.2 17.0 19.8 9.9 79.1
n—PROPYL BENZENE 8.9 12.7 8.7 10 1 18.3 40.4
2-CHLOROTOLUENE 13.4 16.8 12.3 14.2 13.6 56.6
4-CHLOROTOIUENE 15.0 18.8 13.7 15.8 13.5 63.3
tert-BUTYLBENZENE 12.3 12.0 12.5 12.3 1.6 49.1
1.3,5-TRIMETHYLBENZENE 12.2 13.5 11.5 12.4 6.8 49.6
sec-BUTYL BENZENE 12.8 13.6 9.9 12.1 13.1 48.5
1 ,2-DIBROMO-3-CHLOROPROPANE 17.2 17.8 11.7 15.6 17.5 62.3
1.2.4-TRIMETHYIBENZENE 14.1 16.3 7.0 12.4 31.8 49 8
1.3-DICHLOROBENZENE - 4.2 5.2 2.9 4.1 22.7 16.3
p—ISOPROPYL TOLUENE 9.9 12.7 8 7 10.4 16.4 41.7
1,4-DICHLOROBENZENE 4.1 5.1 3.8 4.3 12.5 17.3
1 ,2-DICHLOROBENZENE-d4 1.9 1.8 1.2 1.6 17.3 6.6
1.2-DICHLDROBENZENE 4.5 4.7 3.9 4.3 7.7 17.4
n-BUTYL BENZENE 8.3 11.0 6.1 8.5 23.7 33.8
1 ,2,4-TRICHLOR OBENZENE 4.9 6.4 3.5 4.9 23.6 19.8
HEXACHLOROBUTADIENE 1.6 3.3 1.9 2.3 33.0 9.1
NAPHTHALENE 10.2 12.4 9.6 10.7 11.3 43.0
1.2.3-TRICHLOROBENZENE 1.1 4.0 1.9 2.3 52.3 9 2
NF not found
NI not Included
31
-------
TABLE 22
DETERMINATION OF S RECOVERY
25 ng FORTIFIED MMS/SAND
INTERNAL STANDARD TOLUENE-d8
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG ( 5) (5)
DICHLORODLFLUOROMETHANE 9.7 10.8 7.9 9.5 12.8 37.9
CHLORONETHANE 12.5 14.7 11.6 12.9 10.1 51.8
VINYL CHLORIDE 10.8 8.3 10.0 9.7 10.6 38.8
BROMOMETHANE 15.7 NF 6.1 10.9 59.2 43.6
CHLOROETHANE 11.7 15.1 10.0 12.3 17.3 49.0
TRICHLOROFLUOROMETHANE 10.5 14.8 10.5 11.9 17.2 47.7
1,1—DICHLOROETHENE 11.4 11.4 10.4 11.1 4.1 44.3
METHYLENE CHLORIDE NI NI NI — - -
trans—1,2-DICHLOROETHENE 15.7 15.9 14.7 15.4 3.5 61.7
1.1—DICHLOROETHANE 16.6 16.7 16.3 16.5 1.1 66.1
2,2—DICHLOROPROPANE 23.5 24.2 25.9 24.5 4.1 98.2
cls—1.2-DICHLOROETHENE 18.0 18.8 18.6 18.4 1.9 73.8
BROMOCHLOROMETHANE 16.5 16.8 16.4 16.6 1.2 66.2
CHLOROFORM 19.6 20.7 19.3 19.8 3.1 79.4
1.1,1—TRICHLOROETHANE 19.7 20.2 19.9 20.0 1.1 79.8
1.1—DIC1ILOROPROPENE 19.9 20.6 19.1 19.9 3.0 79.5
CARBON TETRACHLORIDE 21.4 21.1 20.4 21.0 2.0 83.9
BENZENE 25.6 26.7 25.5 25.9 2.1 103.7
1,2—DICHLOROETHANE 24.1 26.0 25.2 25.1 3.2 100.3
TRICHL OROETHYLENE 21.9 22.8 21.6 22.1 2.3 88.3
1,2—DICHLOROPROPANE 21.2 23.1 22.1 22.1 3.6 88.5
DIBROMONETHANE 19.5 22.3 20.4 20.7 5.6 82.9
BROMODICHLORONETHANE 23.0 25.6 24.3 24.3 4.2 97.2
TOLUENE 27.1 29.5 27.2 27.9 4.0 111.6
1.1.2—TRICHLOR OETHANE 23.1 24.5 24.2 24.0 2.5 95.8
TETRACHLOROETHYLENE 25.2 26.7 26.0 26.0 2.4 103.9
1,3—OICHLOR OPROPANE 24.0 27.1 26.5 25.9 5.2 103.6
DIBROMOCHLOROMETHANE 22.2 24.0 23.6 23.3 3.3 93.1
1,2-DIBROMOETHANE 21.3 23.1 21.8 22.1 3.6 88.3
CHLOROBENZENE 24.8 27.1 25.9 25.9 3.5 103.7
1.1.1,2-TETRACHLOROETftANE 27.5 31.6 29.6 29.6 5.6 118.2
ETHYL BENZENE 31.6 34.4 32.4 32.8 3.6 131.2
p-XYLENE 29.7 31.4 29.1 30.1 3.2 120.3
o-XYLENE 29.3 31.7 31.0 30.7 3.4 122.6
STYRENE 21.9 22.0 19.5 21.2 5.4 84.7
BROMOFORM 23.9 25.5 26.7 25.4 4.6 101.5
ISOPROPYLBENZENE 29.8 32 8 31.3 31.3 4.0 125.2
p-BRON DFLUOROB(NZENE 28.0 29.4 28.0 28.5 2.3 113.9
BROMOBENZENE 20.5 22.7 29.5 24.2 15.7 96.9
1.1,2,2-TETRACHLOROETHANE 20.8 22.3 27.7 23.6 12.6 94.5
1.2.3—TRICHLOROPROPANE 31.1 33.5 31.6 32.0 3.2 128.2
n-PROPYL BENZENE 22.0 23.7 23.3 23.0 3.1 92.0
2—CHLOROTOLUENE 21.5 23.3 22.5 22.4 3.3 89.7
4-CHLOROTOLUENE 24.0 26.0 25.1 25.1 3.4 100.2
tert-BUTYLBENZENE 21.9 23.6 22.7 22.7 3.1 90.9
1.3.5—TRIMETHYLBENZENE 20.6 22.8 22.2 21.9 4.3 87.6
sec—BUTYL BENZENE 21.7 23.5 22.8 22.6 3.3 90.5
1.2—DIBRONO-3—CHLOROPROPANE 17.1 18.2 18.0 17.8 2.6 71.0
1.2.4—TRINETHYIBENZENE 21.1 22.8 22.2 22.0 3.3 88.1
1.3-DICHLOROBENZENE 21.0 23.4 22.6 22.4 4.4 89.4
p-ISOPROPYL TOLUENE 21.4 23.2 22.6 22.4 3.4 89.7
1.4-DICHLOROBENZENE 20.5 23.1 22.3 22.0 4.8 87.8
1.2—DICHLOROBENZENE-d4 14.1 16.3 13.9 14.7 7.3 58.9
1.2—DICHLOROBENZENE 21.0 22.6 22.5 22.0 3.3 88.2
n-BUTYL BENZENE 20.7 22.2 21.4 21.4 3.0 85.7
1.2.4—TRICHLOROBENZENE 20.7 21.9 21.0 21.2 2.6 84.7
HEXACHLOROBUTADIENE 19.6 21.1 19.7 20.4 4.7 81.4
NAPHTKALENE 21.1 22.8 22.3 22.1 3.2 88.2
1.2.3—TRICHLOROBENZENE 18.9 20.7 19.2 19.6 4.2 78.3
NF=not found
NI not Included
32
-------
TABLE 23
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/CLAY
INTERNAL STANDARD TOLUENE-d8
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUDROHETHANE 19.0 14.5 17.8 17.1 11.2 68.5
CHLOROHETHANE 32.5 22.5 35.7 30.3 18.6 121.0
VINYL CHLORIDE 24.2 18.7 22.0 21.7 10.6 86.6
BROMOMETHANE NF NF NF - — -
CHLOROETHANE 25.4 20.9 22.8 23.0 7.9 92.1
TRICHLOROFLUOROMETHANE 27.4 20.3 21.4 23.0 13.5 92.1
1,1-DICHLOROETHENE 20.1 13.2 9.6 14.3 30.3 57.2
NETHYLENE CHLORIDE NI NI NI — — -
trans—1,2-DICHLOROETHENE 24.7 16.1 20.2 20.3 17.3 81.3
1.1-DICHLOROETHANE 28.2 18.1 24.2 23.5 17.7 94.1
2.2—DICHLOROPROPANE 25.6 22.4 26.9 25.0 7.7 99.9
cls—1.2-DICHLOROETHENE 28.4 19.4 24.2 24.0 15.4 96.0
8ROMOCHLORONETHANE 33.7 20.7 28.6 27.7 19.4 110.7
CHLOROFORM 36.2 23.0 29.8 29.7 18.2 118.6
1.1.1—TRICHLOROETHANE 29.1 19.0 25.5 24.6 17.0 98.3
1,1—DICHLOROPR OPENE 24.9 17.3 21.4 21.2 14.6 84.7
CARBON TETRACHI.ORIDE 24.2 17.6 19.7 20.5 13.6 81.9
BENZENE 36.3 24.3 31.1 30.6 16.2 122.2
1.2—DICHLOROETHANE 46.6 31.5 39.1 39.1 15.7 156.2
TRICHLOROETHYLENE 26.4 20.0 22.2 22.9 11.6 91.5
1,2-DICHLOROPROPANE 38.1 25.2 32.4 31.9 16.5 127.6
DIBROMONETHANE 41.4 27.0 35.9 34.7 17.1 139.0
BROMODICHLOROMETKANE 38.5 28.0 35.7 34.1 13.0 136.3
TOLIJENE 29.7 24.3 26.9 27.0 8.2 107.8
1,1,2-TRICHIOROETHANE 42.7 29.9 42.5 38.4 15.5 153.5
TETRACHLOROETHYLENE 19.3 17.4 19.5 18.7 5.2 75.0
1.3-DICHLOROPROPANE 41.0 31.2 38.9 37.0 11 4 148.0
DIBROHOCHIOROHETHANE 33.0 26.0 32.0 30.4 10.1 121.4
1 ,2-DIBROMOETHANE 35.2 26.1 31.7 31.0 12.0 124.0
CHLOROBENZENE 21.6 20.5 22.6 21.6 3.8 86.2
1 ,1,1 ,2—TETRACHLOROETHANE 28.5 25.1 28.3 27.3 5.8 109.3
ETHYL BENZENE 21.9 21.5 23.7 22.4 4.3 89.5
p—XYLENE 21.6 22.0 22.8 22.1 2.2 88.5
o—XYLENE 21.6 20.5 22.6 21.6 4.0 86.4
STYRENE 2.8 3.3 3.0 3.0 6.4 12.1
BROMOFORM 32.3 27.9 32.2 30.8 6.6 123.2
ISOPROPYLBENZENE 14.8 16.1 16.5 15.8 4.4 63.1
p- BROMOFLUOROBENZENE 19.3 18.0 21.1 19.5 - 6.6 78.0
BRONOBENZENE 22.1 21.7 25.5 23.1 7 3 92.4
1.1.2.2-TETRACHLOROETHANE 36.0 28.7 36.6 33.7 10.6 134.9
1.2.3—TRICHLOROPROPANE 49.7 19.5 52.5 40.6 35.8 162.3
n-PROPYL BENZENE 11.6 13.9 14.3 13.3 9.0 53.0
2-CHIOROTOLUENE 14.1 16.7 16.7 15.8 7.8 63.3
4-CHIOROTOLUENE 15.7 18.6 15.1 16.5 9 3 65 9
tert- BUTYL BENZENE 10.4 11.9 13.4 11.9 10.5 47.6
1.3 ,5-TRIMETHYLBENZENE 11.9 13.1 13.4 12.8 5.2 51.1
sec-BUTYL BENZENE 9.1 10.2 10.4 9.9 5.7 39.6
1 ,2—DI BROMO-3-CHLOROPROPANE 28.4 23.6 36.4 29.5 17.9 117.8
1 ,2 ,4-TRIMETHYLBENZENE 15.5 15.9 17.5 16.3 5.3 65.1
1 ,3—DICHL OR OBENZENE 9.8 13.2 12 1 11.7 12.2 46.8
p—ISOPROPYL TOLUENE 8.6 9.0 10.6 9.4 9.4 37.6
1 ,4-DICHLOROBENZENE 9.6 13.0 11.9 11.5 12.2 46.0
1 ,2—DICHLCROBENZENE-d4 5.7 6 6 6.0 6,1 6.4 24.5
1.2—OICHLCROBENZENE 11.4 11.8 14.1 12.4 9.8 49.7
n—BUTYI BENZENE 6.9 7.0 8.1 7.3 7.3 29.3
1,2 ,4—TRICHLOROBENZENE 3.6 6.0 5.1 4.9 20.1 19.7
HEXACHLOROBIJTADIENE 2.0 3.3 4.5 3.2 32.1 12.9
NAPHTHALENE 9.9 10.6 13.3 11.3 13.0 45.1
1,2,3—TRICHLOROBENZENE 3.4 5.8 5.4 4.9 21 0 19.5
NF not found
NI not included
33
-------
TABLE 24
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/GPRDEN SOIL
INTERNAL STANDARD TDLUENE—d8
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUOROMETHANE 28.7 37.9 35.7 34.1 11.4 136.4
CHLOROMETHANE 30.9 39.9 41.1 37.3 12.3 149.2
VINYL CHLORIDE 26.6 40.1 38.8 35.2 17.3 140.7
BRONONETHANE NF NF NF - — —
CKLOROETHANE 3.3 17.8 24.1 15.1 57.8 60.3
TRICHLOROFLUOROMETHANE 32.9 46.5 44.8 41.4 14.6 165.6
1,1—DICHLOROETHENE 26.0 35.1 34.5 31.9 13.1 127.4
METHYLENE CHLORIDE NI NI NI — — —
trans—1,2—DICHLOROETHENE 14.3 22.3 20.8 19.1 18.3 76.5
1.1—DICH 1.ORDETHANE 30.1 43.3 38.7 37.3 14.7 149.4
2,2-DICHLORDPROPANE 41.7 50.4 47.1 46.4 7.8 185.6
cls—1,2-D!CHLOROETHENE 22.9 33.5 29.2 28.5 15.3 114.2
BROMOCHLOROMETHANE 19.1 31.6 22.8 24.5 21.4 98.0
CHLOROFORM 32.9 63.8 44.4 47.0 27.1 188.2
1.1,1-TRICHLOR OETHANE 45.0 63.1 51.6 53.2 14.1 213.0
1.1—DICHLOROPROPENE 24.9 40.2 33.1 32.7 19.1 130.9
CARBON TETRACHLORIDE 33.1 51.2 40.8 41.7 17.8 166.8
BENZENE 29.7 49.9 36.0 38.6 21.9 154.3
1.2—DICHLOROETHANE 26.3 44.1 31.8 34.1 21.9 136.3
TRICKLOROETHYLENE 20.2 30.0 25.3 25.2 15.8 100.7
1.2—DICHLOROPROPANE 31.2 53.9 37.0 40.7 23.7 162.8
DIBROMOMETHANE 18.4 31.5 22.4 24.1 22.8 96.4
BROMODICHLOROMETHANE 23.5 35.4 28.0 29.0 17.0 115.9
TOLUENE 31.1 58.7 32.5 40.8 31.1 163.0
1.1.2—TRICHLOROETHANE 23.4 38.8 30.9 31.0 20.2 124.1
TETRACHLOROETHYLENE 22.4 32.7 28.0 27.7 15.2 110.8
1.3—DICHLOROPROPANE 17.1 27.9 21.2 22.1 20.2 88.2
DIBRONOCHLOROMETHANE 15.0 22.5 17.0 18.2 17.4 72.7
1.2—DIBROMOETHANE 9.0 13.0 8.8 10.3 18.7 41.0
CIILOROBENZENE 11.0 15.7 11.3 12.7 16.8 50.7
1.1.1.2-TETRACKLOROETHANE 31.7 37.5 33.7 34.3 7.0 137.1
ETHYL BENZENE 22.3 32.7 22.0 25.7 19.3 102.7
p—XYLEME 22.1 33.4 19.6 25.0 24.0 100.1
o—XYLENE 17.6 26.4 15.4 19.8 24.1 79.2
STYRENE 6.7 5.4 4.1 5.4 19.9 21.5
8ROMOFORM 13.4 19.9 14.8 16.0 17.4 64.2
ISOPROPYLBENZENE 18.9 25.3 18.1 20.8 15.5 83.1
p- BROMOFLUOROBENZENE 6.6 11.1 8.7 8.8 21.1 35.3
BROMO BENZ ENE 7.9 10.6 9.2 9.2 11.9 36.9
1.1.2.2-T TRACHLOR0ETHANE 23.5 - 32.0 24.0 26.5 14.7 106.0
1.2.3—TRICHLOROPR OPANE 28.2 31.8 24.8 28.3 10.1 113.2
n—PROPYI. BENZENE 11.9 19.2 12.8 14.6 22.2 58.6
2-CHLOROTOLUENE 17.9 25.2 17.9 20.4 16.8 81.4
4-CHLOROTOLUENE 20.0 28.1 20.0 22.7 16.8 90.9
tert- BUTYLBENZENE 16.6 18.1 18.3 17.7 4.5 70.7
1.3.5—TRIMETHYLBENZENE 16.3 20.4 16.9 17.9 10.2 71.5
sec-BUTYL BENZENE 17.2 20.5 14.5 17.4 14.0 69.6
I.2—DIBROMO—3—CHLOROPROPANE 23.3 27.2 17.4 22.6 17 9 90,6
1.2,4—TRIMETHYLBENZENE 12.6 16.4 6.8 11.9 32.9 47.8
1,3—DICHLOROBENZENE 5.6 7.8 4.3 5.9 24.7 23.6
p—ISOPROPYL TOLUENE 13.3 19.3 12.8 15.1 19.7 60.5
1.4-0ICHLOROBENZENE 5.5 7.7 5.6 6.3 15.9 25.0
1,2—DICHLORO BENZENE-d4 2.7 3.0 1.9 2.5 11.4 10.0
1.2-DICHLOROBENZENE 6.0 7.0 5.7 6.2 9.3 24.9
n—BUTYL BENZENE 11.2 16.6 8.9 12.2 26.3 48.9
1.2.4—TRICHLOR OBENZENE 6.6 9.6 5.2 7.1 26.0 28.5
HEXACHLOROBUTADIENE 2.1 5.0 2.8 3.3 36.9 13.3
NAPHTHALENE 13.6 18.6 14.0 15.4 14.6 61.5
1.2,3—TRICHLOROBENZENE 1.4 5.9 2.8 3.4 55.4 13.5
NF not found
NI included
34
-------
TABLE 25
DETERMINATION OF S RECOVERY
25 ng FORTIFIED MMS/SAND
INTERNAL STANDARD CHLOROFORN-d
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (5) (5)
DICHLORODIFLUORDMETUANE 10.7 11.4 8.7 10.2 11.0 40.9
CHLOROMETHANE 10.9 13.1 10.9 11.7 8.8 46.6
VINYL CHLORIDE 11.2 14.1 11.2 12.2 11.3 48.7
BROMOMETHANE 17.2 NF 8.0 12 6 55.9 50.4
CHLOROETHANE 12.3 15.1 10.5 12.7 15.0 50.6
TRICHLDROFLUOROMETHANE 13.1 16.9 12.9 14.3 12.9 57.1
1.1—DICHLOROETHENE 12.5 11.9 11.5 12.0 3.6 47.9
METHYLENE CHLORIDE NI NI NI — - —
trans-1.2-DICHLOROETHENE 17.3 16.7 16.3 16.8 2.6 67.1
1.1—DICHLOROETHANE 18.0 17.4 17.8 17.7 1.4 71.0
2,2—DICHLOROPROPANE 24.6 24.6 27.0 25.4 4.6 101.6
cls—1,2-OICHLOROETHENE 19.5 19.5 20.2 19.7 1.7 78.9
BROMOCHLOROMETHANE 18.2 17.7 18.1 18.0 1.3 72.0
CHLOROFORM 22.2 22.0 21.8 22.0 0.6 88.0
1.1,1—TRICHL OROETHANE 21.5 21.1 21.8 21.5 1.3 85.9
1,1—DICHLOROPROPENE 21.9 21.5 21.1 21.5 1.5 86.0
CARBON TETRACHLORIOE 21.8 20.5 21.0 21.1 2.5 84.5
BENZENE 28.0 27.8 27.9 27.9 0.2 111.4
1.2—DICHLOROETHANE 26.3 27.1 27.6 27.0 2.0 108.0
TRICHLORO [ THYLENE 23.9 23.7 23.6 23.7 0.6 94.9
1.2-DICHLOROPROPANE 23.3 24.2 24.4 23.9 2.0 95.7
DIBROKOMETHANE 21.4 23.2 22.5 22.4 3.4 89.4
BROMODICHLOROMETHANE 25.2 26.6 26.6 26.1 2.6 104.6
TOLUENE 29.5 30.7 29.8 30.0 1.7 120.0
I,1,2—TRICHLOROETHANE 25.3 25.6 26.6 25.9 2.1 103.4
TETRACHLOROETHYLENE 27.5 27.8 28.6 28.0 1.6 111.9
1.3—DICHLOROPROPANE 26.3 28 2 29.1 27.9 4.2 111.4
DIBROM OCHLOROI4ETHANE 24.1 25.0 25.7 24.9 2.6 99.7
1,2—DIBROMOETHANE 23.2 24.1 23.8 23.7 1.6 94.7
CHLOROBENZENE 27.3 28.3 28.5 28.0 2.0 112.1
1.1.1.2—TETRACHLOROETHANE 30.4 33.1 32.9 32.1 3.8 128.5
ETHYL BENZENE 34.5 35.8 35.3 35.2 1.5 140.7
p-XYLENE 33.6 35.3 36.3 35.0 3.2 140.1
o—XYLENE 31.7 32.9 33.7 32.8 2.4 131.1
STYRENE 23.9 23.0 21.4 22.8 4.6 91.1
BROMOFORM 25.8 26.4 28.9 27.1 5.0 108.2
ISOPROPYLBENZENE 32.5 34.1 34.2 33.6 2.4 134.4
p-BROM OFLUDROBENZENE 30.5 30.5 30.5 30.5 0.0 121.9
BROMOBENZENE 22.4 23.7 32.1 26.1 16.5 104.3
1,1,2,2-TETRACHLOROETHANE 22.8 23.2 30.3 25.5 13.6 101.8
1,2.3—TRICHLOROPROPANE 33.9 - 34 8 34.5 34.4 1.1 137.6
n-PROPYL BENZEHE 24.0 24.6 25.4 24.7 2.3 98.6
2—CHLOROTOLUENE 23.4 24.3 24.6 24.1 2.1 96.5
4—CHLOROTOLUENE 26.1 27 0 27.3 26.8 2 0 107.2
tert-BUTYLBENZENE 23.9 24.6 24.9 24.5 1.6 97.9
1.3.5—TRINETHYLBENZENE 22.5 23.8 24.4 23.6 3.2 94.2
sec-BUTYL BENZENE 23.6 24.4 24.9 24.3 2.2 97.3
1,2—OIBROM O-3-CHLOROPROPANE 18.7 19.0 19.7 19.1 2.3 76.6
1.2.4-TRIMETHYLBENZENE 23.0 23.7 24.3 23.7 2.3 94.7
1,3-DICHLOR OBENZENE 23.0 24.4 24.7 24.0 3.2 96.1
p-ISOPROPYL TOLUENE 23.4 24.2 24.8 24.1 2.4 96.6
1.4—DICH LOROBENZENE 22.4 24.0 24.3 23.6 3.5 94.3
1.2-DICHLOROBENZENE—d4 17.0 18.0 16.8 17.2 3.0 69.0
1,2-DICHLOROBENZENE 22.9 23.5 24.6 23.6 3.0 94.5
n-BUTYL BENZENE 22.6 23.2 23.5 23.1 1.6 92.4
1.2.4—TRICHLOROBENZENE 22.5 22.8 22.9 22.7 0.8 90.9
HEXACHLOROBUTADIENE 21.4 22.6 21.6 21.9 2.4 87.4
NAPHTHALENE 23.0 23.7 24.3 23.7 2.4 94.6
1,2,3—TRICHLOROBENZENE 20.4 21.5 20.8 20.9 2 1 83.5
NF not found
NI=not included
35
-------
TABLE 26
DETERMINATION OF X RECOVERY
25 ng FORTIFIED MMS/CLAY
INTERNAL STANDARD CHLOROFORM—d
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (X) CX)
DICHLORODIFLIJOROMETHANE 14.1 13.0 12.7 13.2 4.4 53.0
CHLOROMETHANE 25.3 20.4 27.1 24.3 11.7 97.1
VINYL CHLORIDE 18.2 16.8 17.4 17.5 3.4 69.9
BROMOMETHANE NF NF NF - — -
CHLOROETHANE 18.3 18.0 16.0 17.4 5.8 69.8
TRICHLOROFLUORONETHANE 21.3 18.4 16.0 18.5 11.7 74.2
1,1-DICHIOROETHENE 14.9 11.8 7.0 11.2 29.2 44.9
METHYLENE CHLORIDE NI NI NI — — -
trans—1.2—DICHLOROETHENE 17.9 14.3 14.2 15.5 11.0 61.8
1 ,1—DICHLOROETHANE 21.6 16.3 17.9 18.6 11.9 74.5
2,2—DICHLOROPROPANE 21.8 20.5 21.7 21.4 2.7 85.4
cls-1 ,2—D ICHLOROETHENE 22.0 17.5 18.0 19.2 10.3 76.7
BROMOCHLOR ONETHANE 24.6 18.5 20.2 21.1 12.2 84.4
CHLOROFORM 24.2 20.1 19.4 21.2 10.0 85.0
1,1.1—TRICHLOROETHANE 22.0 17.1 18.7 19.3 10.6 77.1
1,1-DICHLOROPROPENE 18.4 15.5 15.4 16.4 8.6 65.7
CARBON TETRACHLORIDE 16.7 15.2 13.6 15.1 8.5 60.6
BENZENE 27.5 21.8 22.7 24.0 10.3 96.0
1 ,2-DICHLOROETHANE 34.8 28.2 28.3 30.4 10.1 121.7
TRICKLOROETHYLENE 20.1 18.0 16.3 18.2 8.5 72.7
1,2-DICHLOROPROPANE 28.3 22.6 23.3 24.7 10.2 98.9
DIBROMOMETHANE 30.7 24.1 25.8 26.9 10.3 107.5
BROMODICHLORONETHANE 28.8 25.1 25.9 26.6 6.0 106.5
TOLUENE 22.2 21.8 19.5 21.2 5.6 84.7
1,1 ,2—TRICHLOROETHANE 31.7 26.8 30.6 29.7 7.1 118.9
TETRACHLOROETHYLENE 14.5 15.6 14.2 14.8 4.1 59.0
1,3-DICHLOROPROPANE 30.6 27.9 28,1 28.9 4.2 115.4
DI8ROMDCHLOROMETHANE 25.4 23.6 23.9 24.3 3.3 97.1
1,2-DIBRONOETHANE 26.7 23.5 23.4 24.5 6.4 98.1
CHLORO BENZENE 16.2 18.4 16.3 17.0 6.1 67.9
1,1,1,2—TETRACHLOROETHANE 20.8 22.3 19.9 21.0 4.6 84.1
ETHYL BENZENE 16.5 19.4 17.3 17.7 6.9 70.8
p-XYLENE 16.1 19.7 16.4 17.4 9.4 69.7
o-XYLENE 16.4 18.5 16.6 17.2 5.5 68.7
STYRENE 2.1 2.9 2.2 2.4 15.9 9.6
BROMOFORN 25.0 25.3 24.3 24.9 1.8 99.5
ISOPROPYLBENZENE 11.1 14.4 12.0 12.5 11.3 50.0
p-BROMOFLUOROBENZENE 14.6 16.2 15.5 15.4 4.3 61.7
BROMOBENZENE 16.6 19.5 18.6 18.2 6.7 73.0
1,1.2.2—TETRACHIOROETHANE 27.1 - 25.8 26.7 26.5 2.1 106.1
1,2,3—TRICHLOROPROPANE 37.2 17.5 38.0 30.9 30.7 123.6
n-PROPYL BENZENE 8.8 12.5 10.5 10.6 14.5 42.3
2-CHLOROTOLUENE 10.6 15.0 12.2 12.6 14.4 50.4
4-CHLOROTOLUENE 11.9 16.8 11.1 13.3 18.9 53.1
tert—BIJTYLBENZENE 7.8 10.7 9.7 9.4 13.0 37.7
1,3 ,5—TRINETHYLBENZENE 8.9 11.8 9.7 10.2 11.9 40.7
sec-BUTYL BENZENE 6.9 9.2 7.6 7.9 12.0 31.6
1 ,2-DIBROM O—3—CHLOROPROPANE 21.1 21.1 26.0 22.7 10.2 91.0
1 ,2,4-TRIMETHYL BENZENE 11.6 14.3 12.7 12.9 8.4 51.4
1,3-OICHLOROBENZENE 7.4 11.9 8.8 9.4 20.0 37.4
p-ISOPROPYL TOLUENE 6.5 8.1 7.7 7.4 9.6 29.7
1 ,4-DICHLOR OBENZENE 7.3 11.7 8.7 9.2 20.0 36.9
1,2-DICHLOROBENZENE-d4 3.9 5.7 3.9 4.5 18.5 18.0
1 ,2-DICHIOROBENZENE 8.6 10.7 10.4 9.9 9.1 39.5
n-BUTYL BENZENE 5.2 6.3 5.9 5.8 8.0 23.2
1.2 ,4—TRICHLOROBENZENE 2.8 5.5 3.7 4.0 28.0 15.9
HEXACHLOROBUTADIENE 1.5 2.9 3.3 2.6 30.7 10.3
NAPHTHAL(NE 7.5 9.5 9.8 8.9 11.3 35.7
1 ,2,3—TRICHL OROBENZENE 2.6 5.2 4.0 3.9 27.0 15.7
NF=not found
NI=not Included
36
-------
TABLE 27
DETERMINATION OF % RECOVERY
25 ng FORTIFIED NNS/GARDEN SOIL
INTERNAL STANDARD CHLOROFORM-d
NG RECOVERED
RSD RECOVERY
AIIALYTE Sample 1 Sample 2 Sample 3 AVG CX) (X i
DICHLORODIFLUOROMETHANE 16.6 19.2 20.8 18.9 9.3 75.5
CHLOROMETHANE 19.4 22.5 25.8 22.6 11.7 90 4
VINYL CHLORIDE 15.9 21.0 22.6 19.8 14.5 79.2
BROHOMETHANE NF NF NF - - —
CHLORCETHANE 1.9 8.8 13.5 8.1 59.0 32.3
TRECHLOROFLUOROMETKANE 21.0 27.1 28.8 25.6 13.1 102.5
1,1—DICHLOROETHENE 15.1 17.6 19.5 17.4 10.3 69.6
METHYLENE CHLORIDE NI NI NI - — —
trans—1.2-DICHLOROETHENE 8.2 10.8 11.5 10.2 14.0 40.7
1.1—DICHLOROETHANE 18.5 23.8 23.6 22.0 11.2 87.9
2.2—DICHLOROPROPANE 32.8 40.5 38.4 37.2 8.8 148.8
cls—1.2-DICHLOROETHENE 14.2 18.6 17.9 16.9 11.5 67.6
BROMOCHLORONETHANE 11.0 15.4 12.8 13.1 13.9 52.3
CHLOROFORM 16.5 23.1 20.5 20.0 13.5 80.1
1,1,1—TRICHIOROETHANE 26.1 31.9 29.3 29.1 8.1 116.4
1 ,1-DICHLOROPROPENE 14.5 20.0 18.7 17.7 13.1 71.0
CARBON TETRACHLORIDE 17.1 20.8 19.7 19.2 7.9 76.8
BENZENE 17.7 25.8 20.9 21.5 15.6 85.9
1.2—DICIILOROETHANE 15.6 22.8 18.5 18.9 15.5 75.8
TRICHLOROETHYLENE 12.3 16.0 15.1 14.4 11.1 57.8
1,2-DICIILOROPROPANE 18.3 27.1 21.1 22.1 16.5 88.6
DIBROMOMETHANE 10.9 16.1 12.9 13.3 16.1 53.1
BROM DDICHLOROMETHANE 14.0 18.3 16.3 16.2 11.0 64.8
TOLUENE 18.5 30.3 18.9 22.6 24.3 90.2
1.1.2—TRICHLOROETHANE 13.8 19.8 17.8 17.1 14.4 68.5
TETRACHLOROETHYLENE 13.3 16.9 16.3 15.5 10.2 61.9
1 ,3—DICHLOROPROPANE 10.2 14.4 12.3 12.3 14.1 49.2
DIBROMOCHIORONETHANE 9.1 12.0 10.1 10.4 11.7 41.6
1.2—DIBROMOETHANE 7.5 9.8 7.9 8.4 12.3 33.6
CHLOROBENZENE 5.4 6.7 5.1 5.7 12.3 22.9
1 ,1,1 ,2—TETRACHLOROETHANE 17.9 18.1 18.5 18.2 1.4 72.7
ETHYL BENZENE 13.2 16.9 12.8 14.3 12.8 57.2
p—XYLENE 13.1 17.2 11.3 13.9 17.7 55.6
o—XYLENE 10.5 13.6 8.9 11.0 17.9 44.0
STYRENE 4.0 2.8 2.4 3.0 22.4 12.1
BROMOFORM 8.2 10.7 8.8 9.2 11.8 37.0
ISOPROPYLBENZENE 11.2 13.1 10.5 11.6 9.3 46.4
p-BROM OFLUOROBENZENE 4.0 5.8 5.1 5 0 15.6 19.9
BROMOBENZENE 4.7 5.5 5.4 5.2 6.7 20.8
1,1,2,2—TETRACHLOROETHANE 14.1 16.7 14.0 14.9 8.4 59.8
1 ,2.3—TRICHLOROPROPANE 16.9 - 16.6 14.5 16.0 6.6 64.1
n—PROPYL BENZENE 7.1 9.9 7.4 8.1 15.6 32.5
2-CHIOROTOLUENE 10.8 13.2 10.5 11.5 10.5 45.9
4-CHLOROTOLUENE 12.1 14.8 11.8 12.9 10.4 51.6
tert-BUTYLBENZENE 9.8 9.4 10.6 9.9 5.3 39.7
1.3.5-TRIMETHYLBENZENE 9.7 10.6 9.8 10.0 3.9 40.1
sec—BUTYL BENZENE 10.3 10.7 8.5 9.8 9.7 39.4
1.2-DIBRONO-3-CHLOR DPROPANE 13.7 13.8 10.0 12.5 14.1 50.1
1.2,4—TRIMETHYL8ENZENE 11.2 12.7 6.0 9.9 29.1 39 8
1,3—DICHLOROBENZENE 3 4 4.1 2.5 3.3 19.4 13.2
p—ISOPROPYL TOLUENE 7.9 10.0 7.4 8.4 13.1 33.8
1 ,4—DICHL OROBENZENE 3.3 4.0 3.3 3.5 9.5 14.1
1.2-DICHLOROBENZENE-d4 1.5 1.4 1.1 1.3 13.8 5.2
1,2—DICHLOROBENZENE 3.6 3.7 3.3 3.5 4.1 14.2
n-BUTYL BENZENE 6.6 8.6 5.2 6.8 20.4 27.2
1 ,2.4—TRICHLOR OBENZENE 4.0 5.0 3.9 4.3 12.0 17.2
HEXACHLOROBUTADIENE 1.3 2.6 1.7 1.9 30.5 7.4
NAPHTHALENE 8.2 9.8 8.3 8.8 8.5 35.0
1,2 ,3—TRICHLORO BENZENE 0 9 3.1 1.6 1.9 49.9 7.5
NF=not found
NI=not included
37
-------
TABLE 28
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/SAND
INTERNAL STANDARD BROMOCHLOROMETHANE-d2
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (X) (%)
DICHLORODIFLUOROMETHANE 16.3 18.6 14.0 16.3 11.4 65.1
CHLORONETHANE 13 2 16.9 13.9 14.7 11.1 56.7
VINYL CHLORIDE 16.5 22.2 17.3 18 7 13.5 74.7
BROMOMETHANE 17.7 26.7 14.1 19.5 27.1 76.0
CHLOROETHANE 17.6 23.1 15.9 18.9 16.5 75.5
TRICHLOROFLUOROMETHANE 13.9 20.1 14.7 16.2 17.0 64.9
1,1-DICHLOROETHENE 15.1 15.4 14.6 15.0 2.1 60.1
METHYLENE CHLORIDE NI NI N E — - —
trans-1.2—DICHLOROETHENE 28.0 29.0 27.9 28.3 1.8 113.2
1.1-DICHIOROETHANE 21.0 21.7 21.8 21.5 1.8 86.1
2,2-DICHLOROPROPANE 19.6 21.0 24.2 21.6 9.0 86.3
cis-1.2—DICHLOROETHENE 22.6 24.3 24.8 23.9 3.9 95.7
BROMOCHLOROMETHANE 28.9 30.2 30.5 29.9 2.2 119.4
CHLOROFORM 37.4 39.9 39.1 38.8 2.6 155.3
1,1,1-TRICHLOROETHANE 25.5 26.7 27.2 26.5 2.8 105.9
1.1-OICHLOROPRDPENE 25.9 27.3 26.4 26.5 2.2 106.1
CARBON TETRACHLORIDE 26.1 26.3 26.5 26.3 0.6 105.2
BENZENE 33.3 35.4 35.0 34.6 2.7 138.3
1,2-DICHLOROETHANE 31.2 34.4 34.5 33.4 4.7 133.5
TRICHLOROETHYLENE 28.3 30.1 29.4 29.3 2.6 117.0
1,2-DICHLOROPROPANE 27.4 30.5 30.2 29.4 4.8 117.5
DIBROMOMETHANE 25.3 29.5 28.1 27.6 6.3 110.4
BROMODICHLOROMEThANE 29.8 33.8 33.3 32.3 5.5 129.4
TOLUENE 35.0 39.1 37.3 37.1 4.5 148.6
1,1,2-TRICHLOROETHANE 29.9 32.4 33.1 31.8 4.3 127.2
TETRACHLOROETHYIENE 32.6 35.3 35.7 34.5 4.0 138.0
1,3-DICHLOROPROPANE 31.1 35.8 36.4 34.4 6.9 137.8
DI BROMOCHLORONETHANE 28.6 31.8 32.4 31.0 5.4 123.8
1.2-DIBROMOETHANE 27.5 30.7 29.8 29.3 4.6 117.3
CHLOROBENZENE 32.1 35.7 35.4 34.4 4.8 137.5
1 ,1,1.2-TETRACHIOROETHANE 34.7 40.2 39.4 38.1 6.3 152.3
ETHYL BENZENE 41.2 45.9 44.7 43.9 4.5 175.7
p-XYLENE 39.9 44.9 45.6 43.5 5.8 173.9
o-XYLENE 38.4 42.7 43.2 41.4 5.3 165.7
STYRENE 28.4 29.2 26.8 28.1 3.6 112.4
BROMOFORM 30.9 34.0 37.2 34.0 7.5 136.1
ISOPROPYLBENZENE 38.4 - 43.2 42.7 41.4 5.2 165.7
p-BROMOFLUOROBENZENE 36.6 39.2 38.6 38.1 3.0 152.6
BROMOBENZENE 26.5 30.1 40.6 32.4 18.4 129.6
1 .1,2,2-TETRACHLOROETHANE 27.0 29.5 38.2 31.5 15.2 126.2
1.2,3-TRICKLOROPROPANE 40.5 44.6 43.6 42.9 4.1 171.5
n-PROPYL BENZENE 28.5 31.4 31.9 30.6 5.0 122.5
2-CHLOROT OLUENE 27.8 30.9 30.9 29.8 4.9 119.4
4-CHLOROTOLUENE 31.1 34.6 34.6 33.4 4.9 133.7
tert—BUTYLBENZENE 28.3 31.2 31.1 30.2 4.4 120.9
1 ,3 ,5-TRIMETHYLBENZENE 26.8 30.4 30.6 29.3 5.9 117.1
sec-BtJTYL BENZENE 28.0 31.1 31.3 30.1 4.9 120.5
1 ,2-DIBROMO—3—CHLOROPROPANE 22.0 23.9 24.5 23.5 4.5 93.8
1 ,2,4-TRIMETHYLBENZENE 27.2 30.1 30.4 29.2 5.0 116.9
1 ,3-DICHLOROBENZENE 27.2 31.0 31.0 29.7 6.0 119.0
p-ISOPROPYL TOLUENE 27.7 30.7 31.0 29.8 5.0 119.3
1.4-DICHL OROBEMZENE 26.6 30.6 30.5 29.2 6.4 116.9
1,2-DICHLOROBENZENE-d4 38.6 42.4 40.5 40.5 3.9 162.0
1,2-DICHLOROBENZENE 27.1 29.9 30.9 29.3 5.5 117.2
n—BUTYL BENZENE 26.8 29.4 29.4 28.5 4.3 114.1
1.2.4-TRICHLOROBENZENE 26.6 29.0 28.7 28.1 3.7 112.4
HEXACHLOROBUTADIENE 25.3 28.7 27.0 27.0 5.1 108.0
NAPHTHAIENE 27.2 30.1 30.6 29.3 5.1 117.2
1,2 ,3-TRICHLOROBENZENE 23.7 26.9 25.5 25.4 5.2 101.5
NI=not included
38
-------
TABLE 29
DETERMINATION OF X RECOVERY
25 ng FORTIFIED MMS/CIAY
INTERNAL STANDARD BROMOCHLORONETHANE—d2
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICIILORODIFLUOROMETHANE 20.4 22.4 19.6 20.8 5.8 83.2
CIILOROMETHANE 24.9 23.4 28.4 25.6 8.2 102.2
VINYL CHLORIDE 22.2 24,3 20.5 22.3 6.9 89.3
BRONOMETHANE NF NF NF - — —
CHLOROETHANE 21.6 25.4 19.8 22.3 10.4 89.1
TRICHLOROFLUOROMETHANE 20.5 20.8 15.8 19.0 12.1 76.0
1.1-DICHLOROETHENE 14.8 14.0 7.4 12.1 27.6 48.2
METHYLENE CHLORIDE NI NI NI - — —
trans-1,2-DICHLOROETHENE 23.8 23.1 20.3 22.4 6.6 89.7
1.1-DICHL OROETHANE 21.1 18.6 18.2 19.3 6.6 77.2
2.2-DICHLOR OPROPANE 12.7 14.6 14.1 13.8 5.8 55.3
cls-1,2-DICHLOROETHENE 21.4 19.8 18.2 19.8 6.7 79.2
BROMOCHIOROMETHANE 31.6 28.9 27.8 29.4 5.4 117.7
CHLOROFORM 33.1 34.2 29.6 32.3 6.1 129.2
1.1.1-TRICHLOROETHANE 21.6 19.8 19.2 20.2 4.9 80.8
1.1-OICHLOROPROPENE 18.2 18.3 16.1 17.5 5.8 70.0
CARBON TETRACHLORIOE 16.5 17.7 14.0 16.1 9.6 64.2
BENZENE 27.0 25.4 23.5 25.3 5.7 101.3
1,2-DICHLOROETHANE 34.2 32.9 29.3 32.1 6.4 128.5
TRICHL OROETHYLENE 19.6 20.7 16.6 19.0 9.2 75 9
l.2-DICHLOROPROPANE 27.4 26.2 23.9 25.9 5.5 103.4
DIBRONOMETHANE 29.8 28.1 26.5 28.2 4.8 112.6
BROMODICHIOROMETHANE 28.3 29,4 26.8 28.2 3.8 112.6
TOLUENE 21.9 25.4 20.2 22.5 9.7 90.0
1,1,2-TRICHLOROETHANE 30.9 31.1 31.4 31.1 0.7 124.5
TETRACHIOROETHYLENE 14.2 18.2 14.7 15.7 11.4 62.8
1.3—DICHLOROPROPANE 30.0 32.5 29.0 30.5 4.9 122.0
DIBRONOCHLOROMETHANE 25.1 27.5 24.7 25.7 4.8 103.0
1.2-DIBROMOETHANE 26.5 27.5 24.2 26.0 5.3 104,1
CHLOROBENZENE 15.9 21.5 16.9 18.1 13.5 72.3
1.1.1,2-T(TRACHLOROETHANE 20.4 25.8 20.7 22.3 11.2 89.2
ETHYL BENZENE 16.1 22.6 17.8 18.8 14.5 75.2
p—XYLENE 15.9 23.1 17.1 18.7 16.8 74.7
o—XYLENE 15.9 21.4 17.0 18.1 13.2 72.3
STYRENE 2.1 3.4 2.2 2.6 23.6 10.3
BROMOFORM 24.7 - 29.8 25.1 26.6 8.7 106.2
ISOPROPYL BENZENE 11.0 16.9 12.4 13.4 18.8 53.6
p—BRON OFLU OROBENZENE 14.2 18.8 15.8 16.2 11.7 65.0
BROMO BENZENE 16.2 22.8 19.1 19.4 13.8 77.5
1.1,2,2-TETRACHLOROETHANE 26.7 30.1 27.7 28.1 5.1 112.6
1.2.3-TRICHIOROPROPANE 36.7 20.5 39.4 32.2 26.0 128 7
n—PROPYL BENZENE 8.3 14.2 10.5 11.0 22.1 44.1
2—CHLOROTOLUENE 10.3 17.3 12.5 13.4 22.1 53.5
4—CIILOROTOLUENE 11.5 19.4 11.3 14.1 27.0 56.2
tert- BUTYLBENZENE 7.7 12.6 10.1 10.1 19.8 40.5
1,3.5-TRINETHYLBENZENE 8.6 13.6 9.9 10.7 19.7 42 9
sec—BUTYL BENZENE 6.6 10.5 7.8 8.3 19.7 33.2
1.2—DIBROMO-3-CHLOROPROPANE 20.7 24.6 26.7 24.0 10.4 96.0
1.2.4-TR IMETHYLBENZENE 11.5 16.7 13.2 13.8 15.8 55.1
l,3-OICIIL OROBENZENE 7.1 13.6 9.0 9.9 27.9 39.6
p—ISOPROPYL TOLUENE 6.4 9.5 8.0 8.0 16.1 31.8
1.4-OICHLORO BENZENE 7.0 13.4 8.8 9.8 27.9 39.0
1.2—DICHLOROBENZENE-d4 12.3 19.5 13.1 15.0 21.7 59.9
1.2—DICHLOR OBENZENE 8.2 12.1 10.4 10.2 15.6 40.9
n-BUTYL BENZENE 51 7.4 6.1 6.2 15.1 25.0
1.2.4—TRICHLOROBENZENE 2.6 6.1 3.7 4.2 35.7 16.6
HEXACHLOROBUTADIENE 1 4 3.3 3.3 2.7 33.8 10.7
NAPHTHALENE 7.1 10.8 9.8 9.2 16 B 36.8
1,2.3—TRICHLOROBENZENE 2.3 5.4 3 7 3.8 34.3 15 1
NF=not found
N1=not included
39
-------
TABLE 30
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/GARDEN SOIL
INTERNAl. STANDARD BROMOCHLORONETHANE-d2
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUOROMETHANE 35.7 38.9 42.6 39.1 7.3 156.2
CHLOROMETHANE 24.9 32.4 39.0 32.1 18.0 128.4
VINYL CHLORIDE 31.8 39.6 44.5 38.6 13.5 154.4
BROMOMETHANE NF NF NF — — —
CHLOROETHANE 3.7 16.4 25.8 15.3 59.3 61.2
TRICHLOROFLUOROMETKANE 33.3 42.3 47.0 40.8 13.9 163.4
1,1-DICHLOROETHENE 24.7 27.1 31.0 27.6 9.5 110.4
METHYLENE CHLORIDE MI NI NI — — -
trans-1.2—DICHLOROETHENE 19.0 23.5 25.7 22.8 12.2 91.0
1,1-DICHLOROETHANE 29.5 36.6 37.5 34.5 10.4 138.1
2,2-DICHL OR OPR OPANE 44.6 68.6 62.1 58.4 17.4 233.7
cls-1.2—DICH 1 .OROETHENE 21.9 27.9 27.7 25.8 10.8 103.3
BROM OCHLOROMETHANE 24.6 32.2 27.9 28.2 10.9 113.0
CHLOROFORM 40.6 50.0 47.4 46.0 8.6 184.0
1,1,1-TRICHLOROETHANE 43.4 50.3 47.9 47.2 6.1 188.8
1,1-DICHLOROPR OPENE 23.8 30.7 29.9 28.1 11.0 112.5
CARBON TETRACHLORIDE 27.8 32.1 31.6 30.5 6.3 122.0
BENZENE 28.7 39.8 33.4 34.0 13.4 135.8
1.2-DICHLOROETHANE 25.2 34.9 29.3 29.8 13.3 119.4
TRICHLOROETHYLENE 19.3 24.2 23.5 22.3 9.7 89.2
1.2-DICHLOROPROPANE 29.6 41.1 33.4 34.7 13.8 138.8
DIBROMOMETHANE 17.7 24.8 20.7 21.1 13.8 84.2
BROMODICHLOROMETHANE 22.6 28.1 25.8 25.5 9.0 102.1
TOLUENE 30.0 46.6 30.0 35.6 22.0 142.2
1.1.2-TRICHI .OROETHANE 22.5 30.4 28.3 27.0 12.4 108.2
TETRACHLOROETHYLENE 21.4 25.9 25.8 24.4 8.5 97.4
1.3-DICHI.OROPROPANE 16.4 22.1 19.5 19.4 12.0 77.5
DIBROMOCIILOROMETHANE 14.0 17.8 15.4 15.7 9.9 62.9
1.2-DIBROMOETHANE 11.6 14.7 12.2 12.8 10.6 51.4
CHLOROBENZENE 8.6 10.2 8.1 9.0 10.3 35.9
1.1.1,2—TETRACHLOROETHANE 29.3 28.0 29.7 29.0 2.5 115.9
ETHYL BENZENE 21.5 26.0 20.4 22.6 10.7 90.5
p-XYLENE 21.1 26.4 18.0 21.8 15.9 87.3
o-XYLENE 17.1 21.2 14.3 17.5 16.1 70.1
STYRENE 6.4 - 4.2 3.8 4.8 24.2 19.2
BROMOFORM 12.3 15.5 13.1 13.6 10.1 54.5
ISOPROPYL8ENZENE 18.1 20.0 16.7 18.3 7.6 73.1
p-8RONOFLUOR OBENZENE 6.2 8.7 7.9 7.6 13.8 30.5
BROM OBENZENE 7.5 8.3 8.5 8.1 5.2 32.5
1.1.2,2—TETRACHLOROETHANE 22.6 25.6 22.2 23.4 6.4 93.8
1,2,3—TRICHLOROPROPANE 27.2 25.4 23.0 25.2 6.9 100.8
n-PROPYL 8ENZENE 11.5 15.4 11.9 13.0 13.4 51.8
2-CHLORDTOLUENE 17.2 20.0 16.5 17.9 8.6 71.6
4-CHLOROTOLUENE 19.2 22.4 18.5 20.0 8.6 80.2
tert—BUTYLBENZENE 15.9 14.4 16.9 15.7 6.6 62.8
1.3.5-TRIMETHYLBENZENE 15.7 16.3 15.7 15.9 1.8 63.6
sec-BUTYL BENZENE 16.5 16.2 13.3 15.3 9.3 61.4
1,2-OIBROMO—3-CHLOROPROPANE 22.3 21.4 16.2 20.0 13.6 79.9
1,2,4-TRIMETHYLBENZENE 18.1 19.5 9.4 15.7 28.3 62.7
1,3-DICHLOROBENZ ENE 5.3 6.1 3.9 5.1 18.2 20.3
p-ISOPROPYL TOLUENE 12.8 15.4 11.9 13.4 11.1 53.5
1,4-DICHL OROBENZENE 5.2 6.0 5.1 5.4 7.5 21.7
1,2-DICHLOROBENZENE—d4 8.7 7.9 6.3 7.6 13.1 30.6
1,2-DICHLOROBENZENE 5.5 5.4 5.1 5.3 3.7 21.4
n-BUTYI BENZENE 10.7 13.1 8.2 10.7 18.8 42.7
1,2.4-TRICHLORO BENZENE 6.1 7.5 4.6 6.1 19.0 24.3
HEXACHLOROBUTADIENE 2.0 3.9 2.5 2.8 28.3 11.3
MAPHTHALENE 12.8 14.6 12.7 13.3 6.5 53.4
1,2.3-TRICHLORO8ENZENE 1.2 4.2 2.3 2.6 48.4 10.4
NF= not found
NI=not Included
40
-------
TABLE 31
DETERMINATION OF % RECOVERY
25 ng FORTIFIED NMS/SAND
INTERNAL STANDARD BROMOBENZENE-d5
MG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUOROMETHANE 9.3 9.4 5.4 8.0 23.3 32.1
CHLOROMETHANE 9.7 10.9 6 9 9.2 18.6 36.6
VINYL CHLORIDE 9.9 11.7 6 9 9.5 20.5 38.0
BROMONETHANE 15.3 20.2 8.2 14.6 34.0 58.3
CHLOROETHANE 11.6 13.4 7.0 1D.7 25.2 42.7
TRICHLOROFLUOROMETHANE 10.2 12.9 7.2 1D.1 23.1 40.4
l.1—DICHLOROETHENE 11.3 10.1 7.4 9.6 17.3 38.4
I1ETHYLENE CHLORIDE NI NI NI - — -
trans-1.2-DICHLOROETHENE 15.9 14.5 10.7 13.7 16.3 54.8
1.1-DICHLOROETHANE 15.5 14.1 10.8 13.5 14.6 53.8
2.2-D ICHLOROPR OPANE 12.7 12.0 10.6 11.8 7.7 47.0
cls-1,2-DICHLOROETHENE 16.6 15.6 12.2 14.8 12.7 59.3
BR OMOCHLORONETHANE 16.4 15.0 11.5 14.3 14.2 57.1
CHLOROFORM 24.9 23.3 17.4 21.9 14.7 87.6
1.1.1—TRICHLOROETHANE 18.9 17.4 13.6 16.6 13.6 66.6
1.1—DICHLOROPROPENE 19.4 18.0 13.3 16.9 15.6 67.6
CARBON TETRACHLORIDE 19.5 17.2 13.2 16.6 15.5 66.6
BENZENE 24.7 23.1 17.4 21.8 14.4 87.1
1.2—DICHLOROETHANE 23.3 22.5 17.3 21.0 12.7 84.1
TRICHLOROETHYLENE 20.9 19.5 14.6 18.4 14.8 73.4
1,2-DICHL OROPROPANE 20.5 20.1 15.2 18.6 13.0 74.4
DIBROMOMETHANE 18.9 19.4 14.1 17.5 13.8 69.8
BROMODICHLOROHETHANE 22.3 22.2 16.7 20.4 12.9 81.5
TOLUENE 26.1 25.6 18.6 23.4 14.5 93.7
1 ,1,2—TRICHIOROETHANE 22.4 21.3 16.6 20.1 12.5 80.4
TETRACHLOROETHYLENE 24.3 23.1 17.9 21.8 12.9 87.1
1,3—DICHLOROPROPANE 23.2 23.5 18.2 21.6 11.3 86.6
DIBRONOCHLOROMETHANE 21.1 20.6 16.0 19.2 12.0 77.0
1,2—DIBROMOETHANE 20.4 20.0 14.8 18.4 13.7 73.5
CHLOR OBENZENE 24.0 23.4 17.7 21.7 13.0 86.9
1.1 ,1.2-TETRACHLOR OETHANE 26.3 26.6 19.9 24.3 12.7 97.1
ETHYL BENZENE 30.7 30.0 22.3 27.7 13.8 110.6
p—XYLENE 29.7 29 3 22.7 27.3 11.8 109.0
o—XYLENE 28.4 27.8 21.4 25.9 12.2 103.6
STYRENE 21.2 19.1 13.4 17.9 18.5 71.4
BROMOFORM 22.7 21.9 18.3 21.0 9.2 83.8
ISOPROPYLEENZENE 28.7 - 28.4 21.4 26.1 12.9 104.6
p-BROM OFLUOROBENZENE 27.2 25.6 19.2 24.0 14.3 96.0
BROMOBENZENE 20 1 20.2 22.3 20.9 4.9 83.5
1.1,2.2—TETRACHLOROETHANE 20.1 19.3 19 0 19.5 2.3 77.9
1 ,2,3—TRICHLOROPROPANE 30.1 29.1 21.7 27.0 13.9 108.0
n-PROPYL BENZENE 21.1 20.4 15 8 19.1 12.2 76.5
2—CHLOROTOLUENE 20.7 20.2 15 4 18.7 12.7 74.9
4-CHLOROTOLUENE 23.2 22.6 17.2 21.0 12.7 84.0
tert-BUTYLBENZENE 21.2 20.5 15.6 19.1 13.1 76.4
1,3 ,5—TRIMETHYLBENZENE 20.0 19.8 15.3 18.3 11 9 73.4
sec—BUTYL BENZENE 20.9 20.3 15.6 18.9 12 5 75.7
1.2—DIBROMO-3-CHLOR OPROPANE 16 5 15.7 12.3 14.9 12.3 59.4
1,2,4—TRIMETHYLBENZENE 20.3 19.8 15.2 18 4 12.4 73.8
1.3—DICHLORO BENZENE 20.2 20.2 15.4 18.6 12.1 74.5
p-ISOPROPYI. TOLUENE 20.7 20.2 15.5 18.8 12.4 75.3
1,4—DICHLOROBENZENE 19.8 19.9 15.2 18.3 12.0 73.2
1,2—DICHLOROBENZENE-d4 26.1 25 2 18.4 23.3 14.9 93.0
1,2—DICHLCROBENZENE 20.1 19.4 15.3 18.3 11.5 73.2
n—BUTYL BENZENE 20.1 19.3 14.7 18.0 13.1 72 1
1,2,4—TRICHLOROBENZEHE 19.8 18.9 14.2 17.6 13 7 70.5
HEXACHLOROBUTADIENE 18.8 18.7 13.4 17.0 14.9 67.9
NAPHTHALENE 20.1 19.6 15.2 18.3 12.2 73.2
1,2.3—TRICHLORO8ENZENE 17.3 17.3 12.5 15.7 14.4 62.8
NI not included
41
-------
TABLE 32
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/CLAY
INTERNAL STANDARD BROMOBENZEME—d5
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 1 Sample 1 AVG (%) (%)
DICHLORODIFLIJOROMETI4ANE 18.3 11.5 17.7 15.8 19.3 63.3
CHLORONETHANE 29.8 16.0 34.2 26.7 29.2 106.7
VINYL CHLORIDE 21.6 13.6 20.2 18.5 19.0 73.9
BROMOMETHANE NF NF NF - - -
CHLOROETKANE 23.2 15.6 21.5 20.1 16.3 80.4
TRICHLOROFLUOROMETHANE 24.4 14.2 18.9 19.2 21.9 76.7
1,1—DICHLOROETHENE 18.1 9.8 9.1 12.3 33.0 49.4
METHYLENE CHLORIDE NI NI NI - - -
trans—1.2—DICHLOROETHENE 22.1 12.3 19.1 17.8 22.9 71.3
1,1—DICHLOROETHANE 25.4 12.8 22.1 20.1 26.4 80.3
2,2—DICHLOR OPROPANE 13.5 8.9 15.1 12.5 21.0 50.0
cls—1,2—DICHLOROETHENE 25.6 13.6 21.9 20.4 24.6 81.4
BROP4OCHLOROMETHANE 29.1 15.2 25.8 23.4 25.3 93.6
CHLOROFORM 35.9 21.2 32.4 29.8 21.0 119.4
1,1.1—TRICHL OROETHANE 26.1 13.8 23.5 21.1 25.2 84.5
1.1—DICHLOROPROPENE 22.2 12.8 19.8 18.3 21.9 73.2
CARBON TETRACIILORIDE 20.0 12.3 17.2 16.5 19.2 66.0
BENZENE 32.8 17.6 28.7 26.4 24.3 105.5
1,2-DICHLOROETHANE 41.5 22.9 36.0 33.5 23.3 133.9
TRICHLOROETHYLENE 23.6 14.3 20.2 19.4 19.8 77.5
1.2-DICHLOROPROPANE 33.5 18.3 29.5 27.1 23.6 108.5
DIBROMOMETHANE 36.4 19.6 32.7 29.6 24.4 118.3
BROMODICHLOROMETHANE 34 4 20.4 32.9 29.2 21.4 117.0
TOLLJENE 26.5 16.6 24.7 22.6 19.1 90.5
1,1.2—TRICHLOROETHANE 37.6 21.7 38.6 32.7 23.7 130.7
TETRACHLOROETHYLENE 17.3 12.7 18.0 16.0 14.8 64.0
1.3—DICHLOROPROPANE 36.5 22.7 35.6 31.6 20.0 126.4
DIBRONOCHLOROP4ETHANE 30.1 18.9 30.0 26.3 19.9 105.3
1.2—DI8ROMOETHANE 32.0 19.0 29.5 26.8 20.9 107.2
CHLOROBENZENE 19.3 15.0 20.8 18.4 13.4 73.4
1.1.1,2—TEIRACHLOROETHANE 25.1 18.2 25.7 23.0 14.7 92.0
ETHYL BENZENE 19.5 15.6 21.8 19.0 13.4 75.9
p-XYLENE 19.4 16.1 21.0 18.9 10.9 75.5
o—XYLENE 19.1 14.8 20.7 18.2 13.7 72.8
STYRENE 2.5 2.4 2.7 2.6 5.6 10.2
BR OM OFORM 29.5 - 20.4 30.3 26.8 16.9 107.0
ISOPROPYLBENZENE 13.3 11.8 15.2 13.5 10.5 53.8
p—BROMOFLU OROBENZENE 17.1 13.0 19.3 16.5 15.9 66.0
BR OHOBENZENE 25.5 18.4 26.5 23.5 15.4 93.9
1.1.2,2—TETRACHLOROETHANE 32.4 20.9 33.9 29.0 19.9 116.2
1.2,3—TRICHLOROPR OPANE 44.5 14.2 48.3 35.7 42.8 142.7
n—PROPYL BENZENE 10.0 9.8 12.8 10.9 12.5 43.6
2—CHLOROTOLUENE 12.4 12.0 15.3 13.2 10.9 53.0
4—CHIOROTOLUENE 13.9 13.5 13.8 13.7 1.4 55.0
tert-BUTYL BENZENE 9.4 8.8 12 4 10.2 15.8 40.8
1.3,5—TRINETHYLBENZENE 10.5 9.4 12.1 10.7 10.4 42.7
sec—BUTYL BENZENE 8.1 7.3 9.5 8.3 11.0 33.1
1,2—DIBROMO—3—CHLOROPROPANE 25.3 17.2 32.9 25.1 25.5 100.6
1,2,4-TRINETHYLBENZENE 14.0 11.6 16.2 13.9 13.4 55.8
1.3—DICHLOROBENZENE 8.6 9.5 11.0 9.7 10.2 38.7
p-ISOPROPYL TOLIJENE 7.7 6.6 9.9 8.1 16.6 32.3
1.4—DICHLOROBENZENE 8.5 9.3 10.8 9.5 10.2 38.1
1.2—DICHLOROBENZENE-d4 13.6 12.4 14.6 13.5 6.8 54.0
1.2—DICHLOROBENZENE 9.9 8.3 12.7 10.3 17.5 41.2
n—BUTYL BENZENE 6.3 5.2 7.6 6.3 15.2 25.4
1.2.4—TRICHLORORENZENE 3.1 4.2 4.5 4.0 15.3 15.9
HEXACKLOROBUTADIENE 1.7 2.3 4.0 2.7 36.9 10.7
NAPHTHALENE 8.6 7.4 11.9 9.3 20.4 37.2
1.2.3—TRICHLOROBENZENE 2.7 3 7 4.4 3.6 19.7 14.4
NF not found
NI not included
42
-------
TABLE 33
DETERMINATION OF X RECOVERY
25 ng FORTIFIED I4NS/GARDEN SOIL
INTERNAL STANDARD BROHOBENZENE-d5
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICHLORODIFLUOROMETHANE 43.9 66.1 61.8 57.2 16.8 229.0
CHLOR OMETHANE 48.1 74.6 76.6 66.4 19.5 265.8
VINYL CHLORIDE 40.8 70.3 67.3 59.4 22.3 237.8
BROMOHETKANE NF NF NF - - -
CHLOROETHANE 5.2 32.0 43.0 26.7 59.4 106.8
TRICHLOROFLUOROMETHANE 52.1 91.6 86.6 76.8 22.9 307.1
1,1—DICHLOROETHENE 39.7 60.3 58.9 53.0 17.7 211.9
NETHYLENE CHLORIDE NI NI NI — — —
trans-1,2-DICHLOROETHENE 23.2 39.7 37.0 33.3 21.6 133.3
1.1-DICHLOROETHANE 46.6 80.1 69.9 65.5 21.4 262.0
2.2—DICIILOROPROPANE 52.1 132.4 102.0 98.8 29.1 395.3
c1s—1 2-DfCHLOROETHENE 34.4 60.6 51.3 48.8 22.2 195.0
SROMOCHLOROMETHANE 29.8 53.9 39.8 41.2 24.0 164.7
CHLOROFORM 57.8 98.6 79.6 78.7 21.2 314.7
1.1,1-TRICHLOROETHANE 69.1 110.9 89.8 89.9 19.0 359.7
1.1—DICHLOROPROPENE 38.3 68.4 56.6 54.4 22.8 217.8
CARBON TETRACHIOBIDE 44.4 71.1 59.4 58.3 18.7 233.3
BENZENE 45.7 87.7 62.7 65.4 26.4 261.4
1.2—DICHLOROETHANE 40.4 77.3 55.2 57.6 26.3 230.5
TRICHLOROETHYLENE 30.6 53.0 43.8 42.5 21.7 169.8
1,2—DICHLOROPROPANE 47.5 91.3 63.3 67.4 26.9 269.5
DIBRONONETHANE 28.4 55.0 39.1 40.8 26.8 163 3
BROMODICHIOROMETHANE 36.0 62.2 48.7 49.0 21.8 195.9
TOLUENE 45.9 103.0 55.5 68.4 36 2 273.7
1.1.2-TRICHLOROETHANE 36.0 67.3 53.5 52.3 24.5 209.0
TETRACHLOROETHYLENE 34.3 57.3 48.7 46.8 20.3 187.2
1.3-DICHLOROPROPANE 26.3 49.0 36.8 37.4 24.8 149.5
DIBROMOCHLOROMETHANE 22.2 38.9 28.6 29.9 23.0 119.5
1,2-DIBROH0ETHANE 18 4 32.4 22.8 24 5 23.7 98.1
CHLOROBENZENE 13.8 22.7 15.2 17.3 22.6 69 0
1.1.1,2-TETRACHLOROETHANE 47.3 62.7 56.6 55.5 11.3 222.1
ETHYL BENZENE 34.3 57.3 38.3 43.3 23.3 173 2
p-XYLENE 33.9 58.6 34.0 42.2 27.5 168.7
o-XYLENE 27.1 46.5 26.8 33.4 27.5 133.8
STYRENE 10.2 9.4 7.1 8.9 15.2 35.7
BROMOFORM 19.3 - 33.7 24.3 25.8 23.2 103.1
ISOPROPTLBENZENE 29.0 44.4 31.4 35.0 19.3 139.8
p—8ROMOFLUOROBENZENE 9 9 19.2 14.9 14.7 26.0 58.7
BROMOBENZENE 16.9 19.8 21.3 19.3 9.4 77.4
1.1.2.2-TETRACHLOROETHANE 36.1 56.4 41.6 44.7 19.2 178.7
1,2.3—TRICHLOROPROPANE 43.4 56.1 43.1 47.5 12.7 190.1
n—PRDPYL BENZENE 18.3 33.8 22.3 24.8 26 5 99.2
2-CHLOROTOLUENE 27.3 44.2 30.9 34.1 21.2 135.6
4—CHLOROTOLUENE 30.6 49.5 34 7 38.3 21.2 153.1
tert-BUTYLBENZENE 25.4 31.8 31.8 29.7 10.2 118.8
1.3,5-TRIMETHYLBENZENE 25.1 35.9 29.4 30 1 14.8 120.5
sec-BUTYL BENZENE 26.3 35.8 25.0 29.0 16.6 116.1
1.2-DIBROMO-3-CHLOROPROPANE 35.9 47.7 30.6 38.0 18 8 152.1
1.2.4—TRIMETHYIBENZENE 29.0 43.1 17.8 30.0 34 5 119.9
1.3-DICHLOR OBENZENE 8.4 13.4 7.2 9.7 27.6 38.8
p—ISOPROPYL TOLUENE 20.6 34.1 22.4 26.7 23.3 102.7
1.4—DICHLOR OBENZENE 8.3 13.2 9.5 10.4 20.2 41.4
1.2—DICHLOROBENZENE—d4 12.7 15.9 10.8 13.1 16.0 52.4
1.2—DICHLOROBENZENE 8.8 11.9 9.5 10.1 13.1 40.2
n—BUTYL BENZENE 17 1 29.1 15.5 20.6 29.5 82.3
1.2.4—TRICHLOROBENZENE 9.8 16.4 8.7 11.6 29.4 46.4
HEXACHLOROBUTADIENE 3.2 8.6 4.8 5.5 41.1 22.1
NAPHIKALENE 20.2 32.0 23.7 25.3 19.5 101 3
1.2.3—TRICHLOROBENZENE 1.9 9.2 4.2 5 1 59.4 20 5
NF not found
NI=not included
43
-------
TABLE 34
DETERMINATION OF % RECOVERY
25 nq FORTIFIED MMS/SAND
INTERNAL STANDARD 2-BROMO-1-CHLOROPROPANE-d6
NG RECOVERED
RSD RECOVERY
ANALYTE Sample 1 Sample 2 Sample 3 AVG (%) (%)
DICRLORODIFLUOROMETHANE 9.4 9.8 7.2 8.8 13.0 35.2
CHLOROMETHANE 9.6 11.4 9.1 10.0 9.8 40.0
VINYL CHLORIDE 9.9 12.2 9.3 10.5 12.3 41.8
BROMOMETHANE 16.0 22.3 11.5 15.6 26.8 66.4
CHLOROETHANE 11.0 13.4 8.9 11.1 16.5 44.3
TRICHIOROFLUOROMETHANE 10.1 13.4 9.5 11.0 15.7 44.0
I.1—DICHL OROETHENE 11.3 10.6 9.8 10.6 5.8 42.4
NETHYLENE CHLORIDE NI NI N! - — —
trans—1.2-DICHLOROETHENE 16.0 15.3 14.3 15.2 4.6 60.8
1,1-DICHI.OROETHANE 15.4 14.7 14.3 14.8 2.9 59.2
2.2—DICHLOROPROPANE 12.1 12.0 13.4 12.5 5.2 50.0
cls—1.2-DICHLOROETHEN [ 16.4 16.2 16.1 16.3 0.7 65.1
BRONOCHLOROMETKANE 18.1 17.4 17.1 17.5 2.5 70.1
CHLOROFORM 23.7 23.3 22.2 23.1 2.8 92.2
1.1.1-TRIcHLaR OETHANE 18.8 18.2 18.0 18.4 1.9 73.4
1.1—DICHLOROPROPENE 19.4 18.9 17.7 18.7 3.8 74.6
CARBON TETRACKLORIDE 19.4 18.0 17.6 18.3 4.1 73.4
BENZENE 24.6 24.2 23.2 24.0 2.5 96.0
1.2—DICHLOROETHANE 23.2 23.6 23.0 23.2 1.1 92.9
TRICHLOROETHYLENE 20.8 20.4 19.4 20.2 3.0 80.8
1.2—DICHLOROPROPANE 20.5 21.0 20.3 20.6 1.6 82.4
DI8ROMOMETHANE 18.9 20.3 18.7 19.3 3.6 77.2
BRONODICHLOROMETHANE 22.2 23.2 22.2 22.5 2.1 90 0
TOLUENE 26.0 26.7 24.8 25.8 3.1 103.3
1.1,2—TRICHLOROETHANE 22.3 22.3 22.1 22.2 0.4 89.0
TETRACKLOROETHYLENE 24.2 24.2 23.8 24.1 0.9 96.2
1.3—DICHLOROPROPANE 23.1 24.6 24.2 24.0 2.5 95.9
DIBROMOCHLOROMETHANE 21.0 21.5 21.2 21.2 1.0 84.9
1.2—DIBROMOETHANE 20.2 20.8 19.7 20.2 2.3 81.0
CHLOROBENZENE 23.9 24.5 23.7 24.0 1.5 96.2
1,1.1.2—TETRACHLOROETHANE 26.2 28.0 26.6 27.0 2.8 107.8
ETHYL BENZENE 30.5 31.3 29.6 30.5 2.3 122.0
p-XYLENE 29.5 30.7 30.2 30.1 1.6 120.5
o—XYLENE 28.2 29.0 28.5 28.6 1.1 114.2
STYRENE 20.2 18.6 18.3 19.0 4.3 76.1
BRON OFORM 22.5 22.8 24.2 23.1 3.2 92.6
ISOPROP’YLBENZENE 28.6 29.7 28.4 28.9 1.9 115.6
p— BR OMOFLUOROBENZENE 27.0 26.7 25.5 26.4 2.4 105.6
BROMOBENzENE 19.6 20.6 26.9 22.4 14.4 89.5
1.1,2.2-TETRACHLOROETHANE 20.0 20.2 25.3 21.8 11.4 87.3
1.2.3—TRICHLOROPROPANE 30.0 30.5 28.9 29.8 2.2 119.1
n—PROPYL BEPIZENE 20.9 21.3 21.0 21.1 0.8 84.4
2—CHLOROTOLUENE 20.6 21.1 20.4 20.7 1.3 82.7
4—CHLOROTOLUENE 23.0 23.6 22.9 23.1 1.3 92.5
tert-BUTYLBENZEHE 21.1 21.4 20.7 21.1 1.3 84.3
- 1,3.5—TRIMETHY IBENZENE 19.8 2D.7 20.3 20.3 1.8 81.1
sec-BUTYL BENZENE 20.7 21.2 20.7 20.9 1.1 83.5
1.2—DIBROMO-3-CHLOROPR OPANE 16.4 16.5 16.4 16.4 0.2 65.7
1.2.4-TRIMETHYLBENZENE 20.2 20.7 20.3 20.4 0.9 81.6
1,3-DICHLOR OBENZENE 20.1 21.1 20.5 20.6 2.1 82.3
p—ISOPROPYL TOLUENE 20.7 21.1 20.7 20.8 0.9 83.2
1.4—DICHLOROBENZENE 19.6 20.8 20.2 20.2 2.4 80.9
1.2—DICHL OROBENZENE—d4 24.9 25.2 23.4 24.5 3.2 98.0
1.2—DICHLOR OBENZENE 19.9 20.3 20.3 20.2 0.9 80.7
n-BUTYL BEHZENE 20.0 20.2 19.6 19.9 1.3 79.7
1.2.4—TRICHL OROBENZENE 19.6 19.7 18.9 19.4 1.9 77.6
HEXACHLOROBUTADIENE 18.7 19.5 17.8 18.7 3.8 74.7
NAPHIHALENE 20.0 20.4 20.1 20.2 0.9 80.7
1,2,3—TRICHLOROBENZ(N( 17.1 17.9 16.5 17.2 3.3 68.7
NI not Included
44
-------
TABLE 35
DETERMINATION OF S RECOVERY
25 ng FORTIFIED P4NS/CLAY
INTERNAL STANDARD 2-BR()IO- 1 -CHLOROPROPANE-d6
HG RECOVERED
RSD RECOVERY
ANALYTE Sanpte 1 SaupLe 2 Saupte 3 AVG CS) ( 5)
DICHLOR IFLUOROMETHANE 14.3 12.0 12.7 13.0 7.6 52.0
CHLOROMETHANE 23.1 16.4 24.3 21.3 16.3 85.0
VINYL CHLORIDE 16.8 14.0 14.7 15.2 7.9 60.7
BRONONETHANE NF HF NF - - -
CHLOROETHANE 17.2 15.3 14.6 15.7 7.1 62.8
TRICHLOROFLUOR ONETHANE 18.9 14.5 13.4 15.6 15.2 62.4
1,1-DICHLOROETHENE 14.1 10.2 6.5 10.3 30.2 41.0
NETHYLENE CHLORIDE NI NI NI . -
trans-12-DICHLOROETHENE 17.3 12.8 13.7 14.6 13.4 58.3
1,1-DICNLOROETI IANE 19.7 13.2 15.7 16.2 16.5 64.7
2 2-DICKLOROPROPANE 10.0 8.7 10.3 9.7 6.9 38.7
cls-1 ,2-DICHLOROETHENE 19.7 13.9 15.5 16.4 15.1 65.5
BRONOCHLORc1 ETHANE 25.1 17.6 20.4 21.0 15.0 84.0
CHLOROFORM 26.7 20.9 22.0 23.2 10.8 92.7
1,1,1-TRICHIOROETHANE 20.3 14.2 16.7 17.0 14.7 68.1
1 ,1-DICHLOROPROPENE 17.3 13.2 14.1 14.9 11.8 59.5
CARBON TETRACHLORIDE 15.5 12.7 12.2 13.5 10.9 53.9
8ENZENE 25.4 18.1 20.4 21.3 14.3 85.3
1,2 -DICHIOROETHANE 32.3 23.6 25.6 27.1 13.7 108.6
TRICHLOROETHYIENE 18.3 14.7 14.4 15.8 11.3 63.2
1 ,2-DICHLOR OPR OPANE 26.1 18.9 21.1 22.0 13.6 88.1
DIBRONOI4ETHANE 28.3 20.2 23.3 23.9 14.0 95.7
BRONODICHLOROHETHANE 26.8 21.0 23.4 23.7 9.9 94.8
TOLUENE 20.6 18.2 17.6 18.8 6.9 75.2
1,1 ,2-TRICHLOR OETHANE 29.3 22.4 27.5 26.4 11.1 105.6
TETRACHLOROETHYLENE 13.4 13.1 12.8 13.1 1.9 52.4
1,3-DICHLOROPROPA NE 28.4 23.3 25.3 25.7 8.0 102.7
DIBRONOCKLORONETNAME 23.3 19.4 21.2 21.3 7.5 85.3
1,2-DIBRONOETHANE 24.8 19.5 20.9 21.7 10.2 86.9
CHLOROBENZENE 15.1 15.5 14.8 15.1 1.8 60.4
1 ,1,1 ,2-TETRACHL OR OETHANE 19.6 18.8 18.3 18.9 2.8 75.7
ETHYL BENZENE 15.1 16.1 15.5 - 15.6 2.5 62.3
p-XYLEHE 15.1 16.6 15.0 15.6 4.8 62.2
o-XYLENE 14.8 15.2 14.7 14.9 1.4 59.5
STYRENE 2.0 - 2.5 1.9 2.1 11.3 8.5
BRONOFORN 22.8 20.9 21.5 21.7 3.7 86.9
ISOPROPYLBENZENE 10.4 12.1 10.8 11.1 6.7 44.4
p-BRONOFLUOROSENZENE 13.3 13.4 13.7 13.5 1.4 53.8
BRONO BENZENE 15.3 16.3 16.7 16.1 3.6 64.2
1,12,2-TETRACHLOROETHANE 25.1 21.5 24.1 23.6 6.4 94.3
1,2 ,3-TRICHLOR OPROPANE 34.5 14.6 34.3 27.8 33.6 111.2
n-PROPYL BENZENE 7.8 10.1 9.1 9.0 10.6 36.0
2-CHLOROTOLUENE 9.7 12.4 10.8 11.0 10.1 43.8
4-CHLOROTOLUENE 10.8 13.8 9.8 11.5 15.0 45.9
tert-BUTYLBENZENE 7.3 9.0 8.8 8.4 9.4 33.5
1 ,3 ,5-TRIMETHYLBENZENE 8.1 9.7 8.6 8.8 7.5 35.3
sec-BUTYL BENZENE 6.2 7.5 6.7 6.8 7.6 27.3
1 ,2-DIBR ONO-3-CHLOROPROPANE 19.7 17.8 23.5 20.3 11.7 81.2
1 ,2,4-TRINETHYLBENZEME 10.9 12.0 11.5 11.5 4.0 45.8
1,3-DICHLOROBENZENE 6.7 9.7 7.8 8.1 15.7 32.2
p-ISOPROPYL TOLUENE 6.0 6.8 7.0 6.6 6.5 26.5
1 ,4-DICHLORO BENZENE 6.6 9.6 7.7 7.9 15.7 31.8
1,2-DICHL OROBENZENE-d4 10.1 12.2 9.9 10.7 9.5 42.9
1,2-DICHLOROBENZENE 7.6 8.6 9.0 8.4 6.7 33.6
n-BUTYL BENZENE 4.9 5.4 5.4 5.2 4.4 20.8
1 ,2,4-TRICHLOR O SENZENE 2.4 4.4 3.2 3.3 23.8 13.3
HEXACHL OR O SUTADIENE 1.3 2.4 2.9 2.2 29.6 8.7
NAPHTHALENE 6.6 7.6 8.4 7.6 9.8 30.3
1,2,3-TRICHLORO BENZENE 2.1 3.8 3.1 3.0 23.6 12.0
NF not found
NI not incLuded
45
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TABLE 36
DETERMINATION OF % RECOVERY
25 ng FORTIFIED MMS/GARDEN SOIL
INTERNAL STANDARD 2 -BRaND-i -CHLOROPROPANE-d6
MG RECOVERED
RSD RECOVERY
ANALYTE San te 1 Sanpte 2 Sanpte 3 AVG (%) (%)
DICHLOROOIFIIJOROMETHANE 16.0 21.6 19.2 19.0 12.1 75.8
CHLORONETHA IIE 17.4 24.2 23.6 21.7 14.1 87.0
VINYL CHLORIDE 14.8 23.0 20.8 19.5 17.6 78.2
BRONOMETHANE HF HF HF -
CHLOROETHANE 1.8 9.9 2.7 4.8 76.0 19.2
TRICHLOROFLUORONETHANE 18.8 29.7 26.6 25.0 18.2 100.2
1,1-DICHLOROETHENE 14.5 19.7 18.2 17.5 12.5 69.9
NETHYLENE CHLORIDE N NI NI -
trens-1,2 -DICHLOR O€THEME 8.5 13.0 11.5 11.0 17.0 44.1
1,1-DICHL OROETHANE 16.9 26.0 21.5 21.5 17.3 85.9
2 2-DICHLOROPROPANE 21.6 41.2 30.1 30.9 25.9 123.8
cls-1,2-DICHL OR OETHENE 12.4 19.6 15.1 15.9 18.4 63.7
BRONUCHL O RONETHANE 12.0 19.5 13.1 15.1 21.2 60.3
CHLOROFORM 20.1 30.7 23.5 24.7 17.8 99.0
1,1,1-TRICHLOROETHANE 25.1 36.0 27.7 29.6 15.8 118.5
1,1-DICHLOROPROPENE 13.9 22.3 17.5 17.9 19.2 71.7
CARBON TETRACHLORIDE 16.2 23.1 18.4 19.2 15.1 76.9
BENZENE 16.6 28.5 19.4 21.5 23.7 86.0
1,2-DICHLOROETHANE 14.7 25.2 17.1 19.0 23.7 75.8
TRICHLOROETHYLENE 11.1 17.2 13.5 14.0 18.1 55.8
1,2-DICHLOROPROPANE 17.3 29.8 19.6 22.2 24.4 89.0
DIBRONONETHANE 10.3 17.9 12.1 13.4 24.1 53.8
BRONOOICHLORONETHANE 13.1 20.2 15.0 16.1 18.7 64.5
TOLUENE 17.4 33.5 17.4 22.8 33.3 91.1
1,1,2-TRICHLOROETHANE 13.1 21.9 16.5 17.2 21.2 68.8
TETRACHLOROETHYLENE 12.5 18.6 15.0 15.4 16.5 61.5
13-DICHLOROPROPANE 9.6 15.9 11.4 12.3 21.8 49.2
DI BRONOCHLORO NETHANE 8.0 12.6 8.8 9.8 20.4 39.3
1,2-DIBRONOETHANE 6.7 10.5 7.0 8.1 21.4 32.3
CHLOROSENZENE 5.0 7.4 4.7 5.7 21.0 22.9
1,1,1 1 2-TETRACHLOROETHANE 17.3 20.5 17.6 18.4 7.8 73.8
ETHYL BENZENE 12.4 18.6 11.8 14.3 21.6 57.2
p-XYLENE 12.3 19.1 10.5 14.0 26.4 55.9
o-XYLENE 9.8 15.1 8.2 11.1 26.5 44.2
STYRENE 3.7 - 3.1 2.2 3.0 21.2 12.0
BRONOFORM 7.0 10.9 75 8.4 20.8 33.8
ISOPROPYLBENZENE 10.5 16.4 9.7 11.6 17.8 46.3
p-BR ONOFLUOR O BENZENE 3.6 6.2 4.6 4.8 22.8 19.2
BRONOBENZEHE 4.4 6.0 4.9 5.1 13.3 20.3
1 1,2,2-TETRACHL0ROETI4ANE 13.1 18.3 12.8 14.8 17.1 59.0
1,2.3-TRICHLOROPROPANE 15.8 18.2 13.3 15.8 12.7 63.1
n-PROPYL BENZENE 6.6 11.0 6.9 8.2 24.4 32.6
2-CHLOROTOLUENE 9.9 14.4 9.6 11.3 19.4 45.1
4-CHLOROTOLUENE 11.1 16.1 10.7 12.6 19.4 50.4
tert-BUTYL BENZENE 9.2 10.4 9.8 9.8 4.7 39.2
1,3.5-TRIHETHYLBENZENE 9.1 11.7 9.1 9.9 12.3 39.8
sec-BUTYL BENZENE 9.5 11.6 77 9.6 16.6 38.5
1,2-DIBR ONO-3-CHLOROPR OPANE 13.1 15.5 9.5 12.7 19.7 50.8
1,2,4-TRIHETHYLBENZENE 10.5 14.0 5.5 10.0 34.9 40.1
1,3-DICHL OR OBENZENE 3.1 4.4 2.2 3.2 27.2 12.9
p-ISOPROPYL TOLUENE 7.5 11.1 6.9 8.5 21.8 34.0
1,4-DICHLOR O BENZENE 3.0 4.3 2.9 3.4 18.3 13.7
1,2-DICHLOROBENZENE-d4 6.4 4.9 3.2 4.2 17.5 16.7
1,2-DICHLOROBENZENE 3.2 3.9 2.9 3.3 11.8 13.3
n-BUTYL BENZENE 6.2 9.5 4.8 6.8 28.7 27.3
1,2 1 4-TRICHLOROBENZENE 3.5 5.3 2.7 3.8 28.7 15.4
HEXACHLOROBUTADIENE 1.2 2.8 13 1.8 39.2 7.2
NAPHTHALENE 7.3 10.4 7.3 8.3 17.3 33.4
1 1 2,3-TRICHLOROBENZENE 0.7 3.0 1.3 1.7 58.4 6.6
NF=not found
NI=not incLuded
46
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TABLE 37
EVALUATION OF ANALYTE RECOVERIES IN GARDEN SOIL
USING MULTIPLE INTERNAL STANDARD
ANALYTE IS PERCENT
SELECTED RECOVERY
DICHIORODIFLUORONETHANE BENZENE—d6 95
CHIOROMETHANE BENZENE—d6 109
VINYL CHLORIDE BENZENE-d6 97
BRONOMETHANE BENZENE-d6 NF
CHLOROETKANE BENZENE-d6 * 40
TR ICIILOROFLUOROMETHANE BENZENE-d6 123
1.1—DICHLOROETHENE BENZENE-d6 86
METHYLENE CHLORIDE BENZENE-d6 NF
trans—i .2—DICHLOROETHENE BENZENE—d6 51
1.1—DICHLOROETHANE BENZENE—d6 107
2,2—DICHLOROPROPANE BENZENE—d B 163
cis—1 • 2—DICHLOROETHENE BENZENE-d6 82
BROMOCHLOROMETHANE TOLtJENE-d8 98
CHLOROFORM BENZENE-d6 106
1. 1,1-TRICHLOROETHANE BENZENE—d6 147
1,1—DICHLOROPROPENE BENZENE—d6 88
CARBON TETRACIILORIDE BENZENE—d6 99
BENZENE BENZENE—d6 107
1.2—DICKLOROETHANE BENZENE-d6 94
TRICHLOROETHYLENE TOLUENE-d8 101
1, 2-DICHIOROPROPANE BENZENE-d6 111
DIBROMOMETHANE TOLUENE—d8 96
BROMODICHLOROMETHANE 8ENZENE-d6 80
TOLUENE TOLUENE—d8 163
1.1. 2—TRICHLOROETHANE TOLUENE—d8 124
TETRACHLOROETHYLENE TOLUENE—d8 111
1,3—DICHLOROPROPANE TOLUENE-d8 88
DIBROMOCHLOROHETHANE TOLUENE—d8 73
1, 2-DIBROMOETItANE BROMOBENZENE-d5 98
CHLOROBENZENE BROMO BENZENE-d5 69
1, 1.1.2-TETRACHIOROETHANE BENZENE-d6 91
ETHYL 8ENZENE TOLUENE-d8 103
p-XYLENE TOLUENE-d8 101
o-XYLENE TOLUENE—d8 79
STYRENE TOLUENE—d8 22
BROMOFORM BROMOBENZENE-d5 103
IS OPROPYLBENZENE TOLUENE-d8 83
p-BROMOFLUOROBENZENE BROMOBENZENE-d5 59
BROMOBENZENE BROMOBENZENE-d5 77
1, 1.2.2—TETRACHLOROETHANE TOLUENE-d8 106
1, 2.3—TRICHLOROPROPANE TOLUENE-d8 113
n-PROPYL BENZENE - BRONOBENZENE-d5 99
2-CHLOR OT OLUENE TOLUENE—d8 81
4-CHLOROTOLUENE TOLUENE-d8 91
tert—BUTYLBENZENE TOLUENE-d8 71
1,3,5—TRIMETHYLBENZENE TOLUENE-d8 72
sec-BUTYL BENZENE T OLUENE-d8 70
1, 2-DIBROMO-3—CHLOROPROPANE TOLUENE—d8 91
1.2.4-TRIHETHYLBENZENE BROMOBENZENE-d5 120
1,3-DICHLOROSENZENE BROMOBENZENE-d5 ** 39
p-ISOPROPYI. TOLUENE BROMO BENZENE-d5 103
1,4-DICHLOROBENZENE BROMOBENZENE-d5 ** 41
1 ,2-DICHLOROBENZENE-d4 BROMOBENZENE-d5 52
1,2-DICHLOROBENZENE BROMOBENZENE-d5 ** 40
n-BUTYL BENZENE BROM OBENZENE-dS 82
1,2.4—TRICHLORO BENZENE BROMOBENZENE-d5 ** 46
HEXACHLOROBUTADIENE BRONOBENZENE-d5 ** 22
NAPHTHALENE BROMOBENZENE-d5 101
1,2.3—TRICHLOROBENZENE BROMOBENZENE-dS ** 21
NI=NOT INCLUDED IN THIS STUDY
* BROMOMETHANE WAS ONLY FOUND IN THE SAND MATRIX
** 1,2-DICHLOROBENZENE-d4 IS RECOMMENDED AS AN ALTERNATE INTERNAL STANDARD
THESE ANALYTES WERE DETECTED IN THE UNFORTIFIED GARDEN SOIL SAMPLE
47
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TABLE 38
DIFFERENT HEADSPACE VOLUME RECOVERIES
25 ng ANALYTE RESPONSE USING 10 ml OF 14 )45
VIAL PRESSURE 7.5 PSI
Samp’e 1 Sample 2 Sample 3 AVG RSD
ANALYTE Area Area Area Area (%)
DICHLORODIFLUOROMETHANE 6611 5864 5622 6032 7
CHLOROMETHANE 2864 2833 2660 2786 3
VINYl CHLORIDE 7614 7900 8613 8042 5
BROMOMETHANE 2502 2994 2927 2808 8
CHLCROETHANE 1812 2112 2451 2125 12
TRICHLOROFLUOROMETHANE 15422 16457 17839 16573 6
1.1-DICHLOROETHENE 12277 12189 11855 12107 2
METHYLENE CHLORIDE 12993 13006 12055 12685 4
trans-1,2-DICH IOROETHENE 12540 13376 12801 12906 3
1.1-DICHLOROETHANE 13694 13134 13316 13381 2
2.2-DICHLOROPROPANE 8440 8459 6590 7830 11-
cls—1 ,2-DICHLOROETHENE 13047 12735 11454 12412 6
BROP4OCHL OROMETHANE 9151 8788 8336 8758 4
CHLOROFORM 12462 11873 12339 12225 2
1.1.1-TRICHLOR OETHANE 12761 12030 11940 12244 3
1.1-DICHLOROPROPENE 9410 9095 8662 9056 3
CARBON TETRACHLORIDE 13991 14700 14378 14356 2
BENZENE 19026 19068 18341 18812 2
1.2-DICHL OROETHANE 12216 12158 10854 11743 5
TRICHLOROETHYLENE 8327 7856 7025 7736 7
1,2-DICIILOROPROPANE 7378 7764 7101 7414 4
DIBROMONETHANE 5732 5324 5303 5453 4
BROHODICHLOROMETHANE 10337 10511 10665 10504 1
TOLUENE 25530 24195 23053 24259 4
1.1.2-TRICHLOROETHANE 6170 6050 5247 5822 7
TETRACHLOROETHYLENE 6785 7525 7065 7125 4
1.3-DICHLOROPROPANE 8097 7666 6841 7535 7
DIBROM OCHLOROMETHANE 10353 10620 10008 10327 2
1,2-DIBROMOETHANE 9379 9852 8922 9384 4
CHLORO BENZENE 12604 12069 12194 12289 2
1,1.1 ,2-TETRACHLOROETHANE 9551 10186 9296 9678 4
ETHYL BENZENE 24522 24702 22973 24066 3
p—XYLENE 26569 24137 27763 26156 6
o—XYLENE 24917 23808 21790 23505 6
STYRENE 20638 22441 21304 21461 3
BROMOFORM 6511 6377 6262 6383 2
ISOPROPYLBENZENE 39143 37637 38710 38497 2
p—BRONOFLUOROBENZENE 11665 10497 10313 10825 6
BROMOBENZENE 17357 20120 19285 18921 6
1.1.2.2-TETRACHL OR OETHANE 12130 11281 10966 11459 4
1,2 ,3-TRICHLOROPROPANE 12796 12441 13991 13076 5
n—PROPYL BENZENE 34929 31429 29584 31981 7
2—CHLOROTO IUENE 24730 25175 21045 23650 8
4-CHLOROTOLUENE 21736 22540 20940 21739 3
tert—BUTYLBENZEH E 27715 31621 30342 29893 5
I ,3,5-TRIMETHY IBENZENE 37027 38753 39782 38521 3
sec-BUTYL BENZENE 42213 41967 39755 41312 3
1.2-DIBROM O—3—CHL OR OPROPANE 6575 6478 6606 6553 1
1,2.4—TRIMETHY LBENZENE 38645 40168 38812 39208 2
1.3-DICHLOROBENZENE 16432 17884 16329 16882 4
p—ISOPROPYL TOLUENE 31083 32475 30033 31197 3
1,4-DICHLOROBENZENE 16049 17299 16165 16505 3
1.2-OICHLOROBENZENE-d4 16400 16768 16838 16669 1
1.2- OICHLOROBENZENE 15968 16348 16283 16200 1
n—BUTYL BENZEME 27498 24966 21889 24784 9
1.2.4-TRICHLOROBENZENE 11732 13097 11106 11978 7
HEXACHLORO BUTADIENE 8382 8220 7420 8007 5
NAPHTHALENE 32462 33868 33832 33387 2
1 ,2 ,3-TRICHLOROBEMZENE 10149 10637 10388 10385 2
48
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TABLE 39
DIFFERENT HEADSPACE VOLUME RECOVERIES
25 ng ANALYTE RESPONSE USING 10 ml P4MS AND 5 ml GLASS BEADS
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 Sample 3 AVG RSD
ANALYTE Area Area Area Area (%)
DICHLORODIFLU OROMETKANE 8125 8014 6488 7542 10
CHL OROMETHANE 3842 4125 3798 3922 4
VINYL CHLORIDE 10355 11104 9218 10226 8
BRONOMETHANE 3956 4934 2514 3801 26
CHLOROETHANE 2728 2610 2445 2594 4
TRICHLOROFLUOROMETHANE 22674 23310 20385 22123 6
1.1-DICHLOROETHENE 15598 16008 14659 15422 4
METHYLENE CHLORIDE 16007 16872 15266 16048 4
trans-1,2— OICHLOROETHENE 15720 16893 15613 16075 4
1.1-DICHLOROETHANE 16923 18508 16093 17175 6
2.2-DICHLOROPR OPANE 10284 12145 8999 10476 12
cls-1,2-DICHLOROETHENE 16282 17206 16068 16519 3
BROMOCHLOROMETHANE 10484 10796 9739 10340 4
CHLOROFORM 16501 14713 16420 15878 5
1.1 1-TRICHLOR0ETHANE 15456 17020 14563 15680 6
1,1-DICHLDROPROPENE 11809 12388 11360 11852 4
CARBON TETRACHLORIDE 20288 20996 19087 20124 4
BENZENE 24548 25647 23186 24460 4
1.2-DICHL OROETHANE 14855 15557 13128 14513 7
TRICHLOROETHYLENE 9832 10872 9393 10032 6
1.2-DICHLDROPROPANE 9237 9177 8844 9086 2
DIBROMOHEIHANE 6635 6373 6285 6431 2
BRONODICHLOROMETHANE 13406 13090 12117 12871 4
TOLUENE 30883 33401 29156 31147 6
1,1.2-TRICHLOROETHANE 6500 7148 5962 6537 7
TETRACHLOROETHYLENE 9965 10909 10866 10580 4
1.3-DICHLOROPROPANE 9578 10250 9405 9744 4
DIBROMOCHLOROMETHANE 14526 13987 12654 13722 6
1.2-DIBROMOETHANE 11893 11634 11359 11629 2
CHLOROBENZENE 17149 17508 16661 17106 2
1,1.1,2-TETRACHLOROETHANE 14102 13947 12643 13564 5
ETHYL BENZENE 32862 39245 34849 35652 7
p-XY 1ENE 40467 17155 37039 31554 33
o-XYLENE 31830 35088 29839 32252 7
STYRENE 30567 32296 27161 30008 7
BROMOFORM 8598 8907 7584 8363 7
ISOPROPYLBENZENE 56044 58074 54961 56360 2
p—BRON OFLUOROBENZENE 14199 14520 13587 14102 3
BROMOBENZENE 21852 28681 24177 24903 11
1.1.2,2-TETRACHLOROETHANE 3437 13744 12845 13342 3
1,2.3-TRICHLOROPROPANE 10432 14309 10089 11610 16
n—PROPYL BENZENE 43713 48370 40174 44086 8
2-CHLOROTOLUENE 32816 35686 30970 33157 6
4—CHLOROTOLUENE 28420 32262 29459 30047 5
tert—BUTYLBENZENE 44517 48902 42801 45407 6
1,3.5-TRIMETHYL8ENZENE 57887 65734 58713 60778 6
sec-BUTYL BENZENE 56397 64541 53599 58179 8
1,2-DIBR OMO-3-CHLOR OPROPANE 7566 6130 6123 6606 10
1,2.4-TRIMETHYLBENZENE 57398 67028 54111 59512 9
1.3-DICHLOROBENZENE 25751 25987 24080 25273 3
p—ISOPROPYL TOLUENE 45674 51946 42947 46856 8
1.4-DICHLOROBENZENE 25657 24718 22499 24291 5
1.2—DICHLOROBENZENE—d4 23135 26715 22323 24058 8
1.2—DICHLOROBENZENE 21562 26992 21981 23512 10
n—BUTYL BENZENE 32988 36873 31202 33688 7
1.2.4-TRICHLOROBENZENE 17003 18432 16842 17426 4
HEXACKLOROBUTADIENE 9981 12071 9701 10584 10
NAPHTHALENE 49234 47039 44236 46836 4
1.2,3-TRICHLOROBENZENE 15506 15857 15253 15539 2
49
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TABLE 40
DIFFERENT HEADSPACE VOLUME RECOVERIES
25 ng ANALYTE RESPONSE USING 10 ml OF MNS AND 10 ml OF GLASS BEADS
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 Sample 3 AVG RSD
AMALYTE Area Area Area Area (%)
DICHLORODIFLUOROMETHANE 8318 7718 7085 7707 7
CKLOROMETKANE 3685 4115 3770 3857 5
VINYL CHLORIDE 11873 11294 10696 11288 4
BROMONETHANE 3280 3999 3223 3501 10
CHLOROETHANE 3281 2907 2898 3029 6
TRICHLOROFLUOROMETHANE 27284 25819 24355 25819 5
1,1-DICHLOROETHENE 19108 17475 16826 17803 5
METHYLENE CHLORIDE 17357 16549 15586 16497 4
TRANS—1.2—DICHLOROETHENE 18268 17963 17447 17893 2
1.1—DICHLOROETHANE 20970 19258 18679 19636 5
2,2—DICHLOROPROPANE 12032 12492 10151 11558 9
CIS—1.2—DICHLOROETHENE 19660 18534 16457 18217 7
BROMOCHLOROMETHANE 11813 9660 9565 10346 10
CHLOROFORM 19543 18657 16967 18389 6
1.1,1—TRICHLOROETHANE 18976 18014 15909 17633 7
1,1—DICKLOROPROPENE 14562 13202 13664 13809 4
CARBON TETRACHLORIDE 25406 22362 21917 23228 7
BENZENE 31201 28669 28300 29390 4
1,2—DICHLOROETHANE 15646 14791 13179 14539 7
TRICHLOROETHYLENE 12302 12009 11179 11830 4
1,2—DICHLOROPROPANE 11052 10591 9604 10416 6
DIBROMOMETHANE 7064 5820 5658 6181 10
BROHODICIILOROMETHANE 13895 14468 12061 13475 8
TOLUENE 38485 38210 34809 37168 4
1.1,2—TRICHLOROETKANE 7663 7101 6444 7069 7
TETRACHLOROETHYLENE 14616 12535 12068 13073 8
1,3—DICHLOROPROPANE 10506 10536 9342 10128 5
DIBROM OCHLOROMETHANE 16073 14411 12416 14300 10
1 ,2—DIBROHOETHANE 13037 11509 10968 11838 7
CHLOROBENZENE 21443 19956 19184 20194 5
1,1 ,1,2—TETRACHLOROETHANE 17293 15184 14483 15653 8
ETHYL BENZENE 48232 42488 40310 43677 8
P-XYLENE 49392 48485 44836 47571 4
O-XYLENE 21740 24051 23070 22954 4
STYRENE 33724 35260 35084 34689 2
BROMOFORM 9231 8439 7909 8526 6
IS OPROPYLBENZENE 73506 72482 68917 71635 3
P-BROMOFLUOROBENZENE 18391 16425 15050 16622 8
BROMOBENZENE 26846 28662 26995 27501 3
1,1 ,2.2—TETRACHLOROETHANE 14636 1380? 12354 13597 7
1 ,2.3—TRICHLOROPROPANE 13008 12225 11336 12190 6
N-PROPYt BENZENE 57912 54999 49581 54164 6
2-CHLOR OTOLUENE 42142 41437 39107 40895 3
4-CHLOROTOLUENE 38823 36210 33817 36283 6
TER- BUTYLBENZENE 65410 59357 53252 59340 8
1,3.5-TRIMETHYLBENZENE 81294 68508 64784 71529 10
SEC-BUTYL BENZENE 81131 80833 59876 77280 7
1,2-DIBROMD-3-CHLOROPR OPANE 6928 6478 6305 6570 4
1.2.4—TRIMETHYLBENZENE 81267 68736 68058 72687 8
1,3-DICHLOR OBENZENE 34192 31423 26789 30801 10
P-ISOPROPYL TOLUENE 61698 59901 56488 59362 4
1,4- DICHLOR OBENZENE 27929 27314 27388 27544 1
D4 1,2-DICHLOROBENZENE 33456 27869 28032 29786 9
1,2-DICHLOROBENZENE 30944 27016 27243 28401 6
N-BUTYLBENZENE 44471 41361 37183 41005 7
1 ,2,4—TRICHLOROBENZENE 22155 19725 18537 20139 7
HEXACHIOROBUTADIENE 13841 13783 12575 13400 4
NAPHTHALENE 54983 52167 47855 51668 6
1,2,3-TRICHLOROBENZENE 19623 17914 17199 18245 6
50
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TABLE 41
DIFFERENT HEADSPACE VOLUME RECOVERIES
25 ng ANALYTE RESPONSE USING 10 m l . OF MMS AND 15 ml. GLASS BEADS
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 Sample 3 AVG RSD
ANALYTE Area Area Area Area (%)
DICHLORODIFLUOROMETHANE 9794 9871 8544 9403 6
CHLOROHETHANE 5038 5095 4422 4852 5
VINYL CHLORIDE 7635 13306 7776 9572 28
BROHOMETHANE 3555 3158 2926 3213 8
CHLOROETHANE 4102 4041 3854 3999 3
TRICHLOROFLUOR OMETHANE 35146 36912 36629 36229 2
1,1—DICHLOROETHENE 25070 24111 23869 24350 2
METHYLENE CHLORIDE 20230 21403 20165 20599 3
trans—1.2—DICHLOROETHENE 23115 24732 23319 23722 3
1 ,1—DICKLOROETHANE 26960 27634 26621 27072 2
2,2-DICHIOROPROPANE 14513 15960 14575 15016 4
cls—1 ,2—DICHLOROETHENE 23319 24509 23848 23892 2
BROMOCHLOROMETHANE 13240 12461 11745 12482 5
CHLOROFORM 23609 23001 23188 23266 1
1,1.1—TRICHLOROETHANE 23385 25620 23928 24311 4
1,1—DICHLOROPROPENE 19460 19801 20856 20039 3
CARBON TETRACHLORIDE 32930 34820 36939 34896 5
BENZENE 38122 40322 40034 39493 2
1,2-OICHLOROETHANE 18482 18184 17215 17960 3
TRICHLOROETHYL€NE 15994 16553 15595 16047 2
1,2—DICKLOROPROPANE 13522 14544 13750 13939 3
DIBROMOMETHANE 6442 7681 7821 7315 8
BROMODICHLOROMETHANE 16855 17803 16039 16899 4
TOLUENE 51831 54405 53153 53130 2
1.1.2—TRICHLOROETHANE 8746 9289 9398 9144 3
TETRACHLOROETHYLENE 20553 20571 22642 21255 5
1.3—DICHIOROPROPANE 13300 13287 12299 12962 4
DIBROMOCKLOROMETHANE 18674 18825 18986 18828 1
1.2—DI8ROM OETHANE 14168 15548 14305 14674 4
CHLOPOBENZENE 26195 29966 30228 28796 6
1,1.1,2—TETRACHLOROETHANE 24041 24311 23427 23926 2
ETHYL BENZENE 61526 65634 66498 64553 3
p-XYLENE 66020 69074 78679 71258 8
o—XYLENE 38983 33355 30764 34367 10
STYRENE 57152 51797 46628 51859 8
BROMOFORM 10611 11369 10107 10696 5
ISOPROPYLBENZENE 103999 119132 109681 110937 6
p—BROM OFLU OROBENZENE 22033 23382 22861 22759 2
BROMOBENZENE 42145 41191 39988 41108 2
1,1.2,2—TETRACHLOROETHANE 17068 17675 17485 17409 1
1,2.3—TRICKLOROPROPANE 15433 15923 16375 15910 2
n—PROPYL BENZENE 81130 82380 83046 82185 1
2—CHLOROTOLUENE 59234 60006 58781 59340 1
4-CHLOROTOLUENE 51148 53144 52324 52205 2
tert—BUTYLBENZENE 86219 99233 91977 92476 6
1.3.5-TRIMETHYLBENZENE 108576 109704 114631 110970 2
sec—BUTYL BENZENE 118000 117052 118862 117971 1
1,2-DIBROMO-3—CHLOR OPR OPANE 7555 7816 7050 7474 4
1.2.4—TRIMETHYLBENZENE 104627 115845 110816 110429 4
1.3-OICHLOROBENZENE 41114 46494 41868 43159 6
p-ISOPROPYL TOLUENE 87497 96265 91767 91843 4
l.4—OICHLOROBENZENE 41114 46498 40388 42667 6
1.2-DICHLOROBENZENE-d4 42301 42397 42037 42245 0
1.2—DICHLOROBENZENE 41414 43148 40419 41660 3
n-BUTYL BENZENE 59364 61787 59277 60143 2
1.2.4—TRICHLOROBENZENE 29074 32342 29469 30295 5
HEXACHLOROBUTADIENE 19205 20823 19736 19921 3
NAPHTHALENE 69496 72652 68996 70381 2
1.2.3—TRICHLOROBENZENE 26038 26821 26214 26358 1
51
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TABLE 42
COMPARISON OF HEADSPACE VOLUME RECOVERIES
THREE REPLICATES OF EACH EXPERIMENT
VIAL PRESSURE 7.5 PSI
MMS 14J4S/SmL BEADS NMS/1 rL BEADS MMS/lSniL BEADS % DIF X DIF
ANALYTE AVG AREA RSD AVG AREA RSD AVG AREA RSD AVG AREA RSD 5 mL 15 mL
(%) (%) (s) (%)
DICHLORODIFLUOROMETHANE 6032 7 7542 10 7707 7 9403 6 98 122
CHLOROMETHANE 2786 3 3922 4 3857 5 4852 6 102 126
VINYL CHLORIDE 8042 5 10226 8 11288 4 9572 28 91 85
BROMOMETHANE 2808 8 3801 26 3501 10 3213 8 109 92
CHLOROETHANE 2125 12 2594 4 3029 6 3999 3 86 132
TRICHLOROFLUOROHETHANE 16573 6 22123 6 25819 5 36229 2 86 140
1,1-DICHLOROETHENE 12107 2 15422 4 17803 5 24350 2 87 137
METHYLENE CHLORIDE 12685 4 16048 4 16497 4 20599 3 97 125
TRANS-1.2-DICHLOR OETHENE 12906 3 16075 4 17893 2 23722 3 90 133
1,1-D ICHLOROETHANE 13381 2 17175 6 19636 5 27072 2 87 138
2.2-DICHLOROPROPANE 7830 11 10476 12 11558 9 15016 4 91 130
CIS-1,2-DICHLOROETHENE 12412 6 16519 3 18217 7 23892 2 91 131
BROMOCHLOROMETHANE 8758 4 10340 4 10346 10 12482 5 100 121
CHLOROFORM 12225 2 15878 5 18389 6 23266 1 86 127
1.1.1-TRICHL OROETHANE 12244 3 15680 6 17633 7 24311 4 89 138
1.1-DICHLOROPROPENE 9056 3 11852 4 13809 4 20039 3 86 145
CARBON TETRACHLORIDE 14356 2 20124 4 23228 7 34896 5 87 150
BENZENE 18812 2 24460 4 29390 4 39493 2 83 134
1.2-O ICHLOROETHANE 11743 5 14513 7 14539 7 17960 3 100 124
TRICHLOROETHYLENE 7736 7 10032 6 11830 4 16047 2 85 136
1,2-DICHLOROPROPANE 7414 4 9086 2 10416 6 13939 3 87 134
DIBROMOMETHANE 5453 4 6431 2 6181 10 7315 8 104 118
BROMODICHLOROMETIIANE 10504 1 12871 4 13475 8 16899 4 96 125
TOLUENE 24259 4 31147 6 37168 4 53130 2 84 143
1.1,2—TRICHL OROETHANE 5822 7 6537 7 7069 7 9144 3 92 129
TETRACHL OROETHYLENE 7125 4 10580 4 13073 8 21255 5 81 163
1,3-OICHLOROPROPANE 7535 7 9744 4 10128 5 12962 4 96 128
D IBROMOCHLOROMETHANE 10327 2 13722 6 14300 10 18828 1 96 132
1,2-DIBROMOETHANE 9384 4 11629 2 11838 7 14674 4 98 124
CHLOROBENZENE 12289 2 17106 2 20194 5 28796 6 85 143
1,1,1.2-TETRACHLOROETHANE 9678 4 13564 5 15653 8 23926 2 87 153
ETHYL BENZENE 24066 3 35652 7 43677 8 64553 3 82 148
p-XYLENE 26156 6 31554 33 47571 4 71258 8 66 150
o-XYLENE 23505 6 32252 7 22954 4 34367 10 141 150
STYRENE 21461 3 30008 7 34689 2 51859 8 87 149
BROMOFORM 6383 2 8363 7 8526 6 10696 5 98 125
ISOPROPYLBENZENE 38497 2 56360 2 71635 3 110937 6 79 155
p-BROMOFLUOR OBENZENE 10825 6 14102 3 16622 8 22759 2 85 137
BROMOBENZENE 18921 6 24903 11 27501 3 41108 2 91 149
1,1,2,2-TETRACHLOROETHANE - 11459 4 13342 - 3 13597 7 17409 1 98 128
1,2,3—TRICHL OR OPROPANE 13076 5 11610 16 12190 6 15910 2 95 131
n-PROPYL BENZENE 31981 7 44086 8 54164 6 82185 1 81 152
2-CHLOROTOLUENE 23650 8 33157 6 40895 3 59340 1 81 145
4-CHLOROTOLUENE 21739 3 30047 5 36283 6 52205 2 83 144
t-BUTYLBENZENE 29893 5 45407 6 59340 8 92416 6 77 156
1,3 .5-TRIMETHYLBENZENE 38521 3 60778 6 71529 10 110970 2 85 155
sec-OUTYL BENZENE 41312 3 58179 8 77280 7 117971 1 75 153
1,2-OIBROMO-3—CHLOROPROPANE 6553 1 6606 10 6570 4 7474 4 101 114
1,2.4-TRIMETHYLBENZENE 39208 2 59512 9 72687 8 110429 4 82 152
1.3-OICHLOROBENZENE 16882 4 25273 3 30801 10 43159 6 82 140
p-ISOPROPYL TOLUENE 31197 3 46856 8 59362 4 91843 4 79 155
1.4-OICHLOROBENZENE 16505 3 24291 5 27544 1 42667 6 88 155
d4 1.2-DICHLOROBENZENE 16669 1 24058 8 29786 9 42245 0 81 142
1.2-DICHLOROBENZENE 16200 1 23512 10 28401 6 41660 3 83 147
n-BUTYL BENZENE 24784 9 33688 7 41005 7 60143 2 82 147
1,2 .4-TRICHLOROBENZENE 11978 7 17426 4 20139 7 30295 5 87 150
HEXACHLOROBUTA DIENE 8007 5 10584 10 13400 4 19921 3 79 149
NAPHTHALENE 33387 2 46836 4 51668 6 70381 2 91 136
1.2.3-TRICHL OROBENZENE 10385 2 15539 2 18245 6 26358 1 85 144
AVG 89 137
APPROXIMATE HEADSPACE VOLUME 12 mL 9.4 niL 6.8 ml. 4.2 mL
52
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TABLE 43
DIFFERENT 14145 AMOUNTS AT CONSTANT HEADSPACE VOLUME
25 ng ANALYTE RESPONSE USING 10 m l. OF 14145
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 Sample 3 AVG RSD
ANALYTE Area Area Area Area (%)
DICHLORODIFLUOROMETHANE 775 825 1060 887 14
CHLOROMETHANE 842 977 1070 963 10
VINYL CHLORIDE 4774 4343 4235 4451 5
BROMOMETHANE 1690 1743 1582 1672 4
CHLOROETHANE 1546 1534 1529 1536 0
TRICHLOROFLUOROHETHANE 11729 11095 12912 11912 6
1.1-DICHLOROETHENE 9999 9392 10182 9858 3
METHYLENE CHLORIDE 11008 11118 11305 11144 1
trans—1,2—DICHLOR OETHENE 11417 11224 11691 11444 2
1,1-DICHLOROETHANE 12137 12357 12203 12232 1
2,2-DICHLOROPROPANE 7697 8116 8443 8085 4
cls—1.2—DICHLOROETHENE 12730 13154 12711 12865 2
BROM OCHLOROMETHANE 7892 7592 7621 7702 2
CHLOROFORM 12048 12184 12869 12367 3
1.1.1-TRICHLOROETI IANE 11280 11890 11910 11693 3
1.I—DICHLOROPROPENE 8509 8144 8702 8452 3
CARBON TETRACHLOR IDE 13243 13426 14426 13698 4
BENZENE 17680 17822 18359 17954 2
1.2— OICHLOROETHANE 10394 10040 10781 10405 3
TRICHLOROETHYLENE 7095 7125 7223 7148 1
1.2-DICHIOROPROPANE 7050 6972 7463 7162 3
DIBROMOMETHANE 4562 4629 5019 4737 4
BROMODICHLOR OMETHANE 9522 10329 10270 10040 4
TOLUENE 24326 24399 25441 24722 2
1.1,2—TRICHLOR OETHANE 5350 5608 4926 5295 5
TETRACHL OR OETHYLENE 7293 7403 7929 7542 4
1,3-DICHLOROPR OPANE 7598 7490 7448 7512 1
DIBROMOCHL OR OMETHANE 9798 9484 9455 9579 2
1.2-DIBROMOETHANE 8078 7965 7830 7958 1
CHLOROBENZENE 13526 14187 13640 13784 2
1,1.1.2—TETRACHL OROETKANE 9337 10545 11784 10555 9
ETHYL BENZENE 25807 25074 27869 26250 5
p-XYLENE 28624 28390 30810 29275 4
o-XYLENE 22488 24972 28442 25301 10
STYRENE 21395 22781 24036 22737 5
BROMOFORM 5964 5773 5782 5840 2
ISOPROPYLBENZENE 41420 43072 46134 43542 4
p—BROMOFLUOROBENZENE 11134 11171 10948 11084 1
BR OMOBENZENE 18519 20073 20627 19740 5
1.1.2.2—TETRACHL OROETHANE 11389 10984 10323 10899 4
1.2.3-TRICHLOR OPROPANE 8062 7619 8563 8081 5
n—PROPYL BENZENE 34062 36553 38223 36279 5
2-CHIOROTOLUENE 24519 25648 27527 25898 5
4-CHIOROTOLUENE 22637 25515 24774 24309 5
tert-BUTYLBENZENE 34178 35724 36403 35435 3
1.3.5-TRIHETHYLBENZENE 43199 44975 46886 45020 3
sec-BUTYL BENZENE 45214 44987 53873 48025 9
1.2—DIBRONO-3—CHLOROPROPANE 5426 4929 4656 5004 6
1,2,4—TRIMETHYLBENZENE 46431 42709 48617 45919 5
1,3—OICHLOROBENZENE 17486 19132 20422 19013 6
p—ISOPROPYL TOLUENE 36161 37118 38983 37421 3
1.4—DICHIOROBEPIZENE 17646 18420 19123 18396 3
1.2-DICHLOROBENZENE-d4 17602 19073 19312 18662 4
1.2—DICHLOROBENZENE 17865 18577 18669 18370 2
n-BUTYL BENZENE 26883 27737 29712 28111 4
1.2,4-TRICHLOR OBENZENE 13794 13945 14244 13994 1
HEXACHIOROBUTADIENE 8853 8590 9489 8977 4
NAPHTHALENE 35739 36000 36964 36234 1
1.2.3—TRICHLOROBENZENE 11630 11949 12433 12004 3
53
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TABLE 44
DIFFERENT MMS AMOUNTS AT CONSTANT HEADSPACE VOLUME
25 ng ANALYTE RESPONSE USING 7.2 ml. OF ME AND 5 Ml OF THE BEADS
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 AVG RSD
ANALYTE Area Area Area (%)
DICHLORODIFLUORONETHANE 1206 811 1009 20
CHLOROMETI1ANE 1034 925 980 6
VINYL CHLORIDE 4365 4596 4481 3
BROMOMETHANE 1478 1367 1423 4
CHLOROETHANE 1780 1723 1752 2
TRICHL OROFLUOROMETHANE 13739 12977 13358 3
1,1-DICHLOROETHENE 10786 11031 10909 1
METHYLENE CHLORIDE 12537 12381 12459 1
trans-1,2-DICHLOROETHENE 12853 13508 13181 2
1,1-DICHLOROETHANE 13810 13592 13701 1
2 ,2-DICHLOROPROPANE 9173 9292 9233 1
cis-1,2-DICHLOROETHENE 13591 14525 14058 3
BROMOCHLOROMETHANE 8821 8640 8731 1
CHLOROFORM 13398 13955 13677 2
1,1,1—TRICHLOROETHANE 13600 13949 13775 1
1,1-OICHLOROPROPENE 9963 9960 9962 0
CARBON TETRACHLORIDE 15446 15624 15535 1
BENZENE 21227 20749 20988 1
1,2-DICHLOROETHANE 11750 11165 11458 3
TRICHLOROETHYLENE 8472 8651 8562 1
1.2-OICHLOROPROPANE 8145 8387 8266 1
DIBROMOMETHANE 5244 4906 5075 3
BROMODICHLOROMETHANE 10912 11209 11061 1
TOLUENE 29408 29785 29597 1
1.1,2-TRICHLOROETHANE 5592 5747 5670 1
TETRACHLOROETHYLENE 8632 9175 8904 3
1,3-DICHLOROPROPANE 8135 8497 8316 2
DI BRONOCHLOROMETHANE 11168 11122 11145 0
1.2-DIBROMOETHANE 8784 9124 8954 2
CHLOROBENZENE 15708 15326 15517 1
1.1.1,2-TETRACHLOROETHANE 12134 11460 11797 3
ETHYL BENZENE 32377 33818 33098 2
p-XYLENE 37960 38953 38457 1
o-XYLENE 32293 31310 31802 2
STYRENE 28080 29977 29029 3
BROMOFORM 6747 7044 6896 2
ISOPROPYLBENZENE 52798 51877 52338 1
p-BROMOFLUOROBENZENE 12649 13349 12999 3
BRONQBENZENE 20559 22967 21763 6
1,1,2,2-TETRACHLOROETHANE 12090 11807 11949 1
1,2,3-TRICHLOROPROPANE - 9188 9590 9389 2
n-PROPYL BENZENE 42872 44610 43741 2
2-CHLOROTOLUENE 31451 31158 31305 0
4-CHLOROTOLUENE 29023 29927 29475 2
tert—BUTYLBENZENE 43874 44250 44062 0
1,3,5-TRIHETHYLBENZENE 56006 58388 57197 2
sec-BUTYL BENZENE 57026 60602 58814 3
1,2-DIBROM O-3-CHLOR OPROPAN( 5789 5633 5711 1
1,2,4-TRIHETHYLBENZENE 56175 55410 55793 1
1.3-DICHLOROBENZENE 21672 22567 22120 2
p-ISOPROPYL TOLUENE 42884 44041 43463 1
1,4—DICHLOROBENZENE 23353 23094 23224 1
1,2-DICHLOROBEHZENE-d4 22842 21605 22224 3
1,2-DICHLOROBENZENE 21722 20765 21244 2
n-BUTYL BENZENE 32925 34170 33548 2
1,2,4-TRICHLOROBENZENE 16888 16338 16613 2
HEXACHLOROBUTADIENE 10759 11412 11086 3
NAPHTHALENE 41621 39900 40761 2
1,2,3-TRICHLOROBENZENE 13879 14396 14138 2
NF not found
54
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TABLE 45
DIFFERENT NMS AMOUNTS AT CONSTANT HEADSPACE VOLUME
25 ny ANALYTE RESPONSE USING 4.5 nil. OF MMS AND 10 nil. OF THE BEADS
VIAL PRESSURE 7.5 PSI
Sample 1 Sample 2 AVG RSD
ANALYTE Area Area Area (%)
DICHLORODIFLUOROMETHANE 907 984 946 4
CHLOROHETHANE 974 884 929 5
VINYL CHLORIDE 3285 3215 3250 1
BROMOMETHANE 1236 1369 1303 5
CHLOROETHANE 1214 1327 1271 4
TRICHIOROFLUOROMETHANE 9638 9428 9533 1
1,1-DICHLOROETHENE 5349 4996 5173 3
METHYLENE CHLORIDE 10235 9742 9989 2
trans-1,2-DICHLOROETHENE 10316 9080 9698 6
1 ,1-DICULOROETHAtIE 11000 10316 10658 3
2 ,2- OICHLOROPR OPANE 7868 8193 8031 2
cls-1,2-DICHLOROETHENE 11786 11518 11652 1
BR OMOCHLOROMETHANE 7502 6934 7218 4
CHLOROFORM 11673 10799 11236 4
1,1,1-TRICHL OROETHANE 10942 10759 10851 1
1,1-DICHLOROPROPENE 7384 7533 7459 1
CARBON TETRACHLORIDE 11861 11534 11698 1
BENZENE 17213 16791 17002 1
1,2-DICHLOROETHANE 10244 9441 9843 4
TRICHIOROETHYLENE 6786 6926 6856 1
1.2-DICHLOROPROPANE 6777 6349 6563 3
DIBROMOMETHANE 4864 4124 4494 8
BROMODICHLOROMETHANE 9483 9131 9307 2
TOLUENE 24163 22777 23470 3
1.1.2-TRICHLOROETHANE 5418 4860 5139 5
TETRACHLOROETHYLENE 6988 6613 6801 3
1 ,3-DICHLOROPROPANE 7781 6919 7350 6
DIBROMOCHLOROHETHANE 9770 8850 9310 5
1,2-DIBROMOETHANE 8299 7619 7959 4
CHLOROBENZENE 12907 11982 12445 4
1,1,1,2-TETRACHLOROETHANE 9804 9195 9500 3
ETHYL BENZENE 26068 25374 25721 1
p-XYLENE 29839 26669 26254 6
o-XYLENE 26021 23948 24985 4
STYRENE 21716 21139 21428 1
BROMOFORM 6429 5422 5926 8
ISOPROPYLBENZENE 40922 39100 40011 2
p-BROMOFLUOROBENZENE 10778 10636 10707 1
BRONOBENZENE 19604 17754 18679 5
1 ,1,2,2-T(TRACHLOROETHANE 11505 10153 10829 6
1.2 ,3-TRICHLOROPROPANE - 8139 7644 7892 3
n-PROPYL BENZENE 34969 34278 34624 1
2-CIILOROTOLUENE 25390 23492 24441 4
4-CIILOROTOLUENE 22681 22381 22531 1
tert—BUTYLBENZENE 34921 32522 33722 4
1,3,5-TRINETHYLBENZENE 43411 40034 41723 4
sec-BUTYL BENZENE 48129 45396 46763 3
1.2-DIBROMO-3-CHLOROPROPANE 5987 5559 5773 4
1,2,4-TRIMETHYLBENZENE 43111 39730 41421 4
1,3-DICHLOROBENZENE 17328 17391 17360 0
p-ISOPROPYL TOLUENE 35433 33510 34472 3
1,4-DJCHLOROBENZENE 16307 16285 16296 0
1,2-DICHLOROBENZENE-d4 16749 17278 17014 2
1,2-DICHLOROBENZENE 17094 16548 16821 2
n-BUTYL BENZENE 26772 27096 26934 1
1,2,4-TRICHLOROBENZENE 13473 12590 13032 3
HEXACHLOROBUTADIENE 9378 8759 9069 3
NAPHTHALENE 37329 32729 35029 7
1,2,3-TRICHLOROBENZENE 11781 11232 11507 2
NF not found
55
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TABLE 46
COMPARISON OF 25 ng ANALYTE RECOVERIES FOR
DIFFERENT NMS AMOUNTS AT CONSTANT HEADSPACE VOLUME
VIAL PRESSURE 7.5 PSI
10 niL MNS 7mL MMS/5mL BEADS 4.SmL MNS/1 nL BEADS
ANALYTE AVG AREA RSD AVG AREA RSD AVG AREA RSD
(%) (%) (%)
DICHLORODIFLU OROMETHANE 887 14 1009 20 946 4
CHL OROMETHANE 963 10 980 6 929 5
VINYL CHLORIDE 4451 5 4481 3 3250 1
BROMOMETHANE 1672 4 1423 4 1303 5
CHLOROETHANE 1536 0 1752 2 1271 4
TRICHLOROFLUOROMETHANE 11912 6 13358 3 9533 1
1.1-DICHLOROETHENE 9858 3 10909 1 5173 3
METHYLENE CHLORIDE 11144 1 12459 1 9989 2
trans-1.2—DICHLOROETHENE 11444 2 13181 2 9698 6
1.1-OICHI. OROETHANE 12232 1 13701 1 10658 3
2.2-DICHL OROPROPA ME 8085 4 9233 1 8031 2
cis-1,2—DICHLOROETRENE 12865 2 14058 3 11652 1
BROMOCHLOROMETHANE 7702 2 8731 1 7218 4
CHLOROFORM 12367 3 13677 2 11236 4
1.1.1—TRICH 1.OROETHANE 11693 3 13775 1 10851 1
1.1-DICHLOROPR OPENE 8452 3 9962 0 7459 1
CARBON TETRACHLORIDE 13698 4 15535 1 11698 1
BENZENE 17954 2 20988 1 17002 1
1,2-DICHLOROETHANE 10405 3 11458 3 9843 4
TRICHLOROETHYLENE 7148 1 8562 1 6856 1
1,2-DICHLOROPROPANE 7162 3 8266 1 6563 3
DIBROMOMETHANE 4737 4 5075 3 4494 8
BR OMODICHLOROMETHANE 10040 4 11061 1 9307 2
TOLUENE 24722 2 29597 1 23470 3
1.1.2—TRICHLOROETHANE 5295 5 5670 1 5139 5
TETRACHLOR OETHYLENE 7542 4 8904 3 6801 3
1.3-DICHLOROPROPANE 7512 1 8316 2 7350 6
DIBROMOCHLOROMETHANE 9579 2 11145 0 9310 5
1.2-DIBROMOETHANE 7958 1 8954 2 7959 4
CHLDROBENZENE 13784 2 15517 1 12445 4
1.1.1.2—TETRACHLOROETHANE 10555 9 11797 3 9500 3
ETHYL BENZENE 26250 5 33098 2 25721 1
p-XYLENE 19275 6 38457 1 28254 6
o-XYLENE 25301 10 31802 2 24985 4
STYRENE 22737 5 29029 3 21428 1
BROMOFORM 5840 2 6896 2 5926 8
ISOPRDPYLBENZENE 43542 4 52338 1 40011 2
p-BROMOFLUOROBENZENE 11084 1 12999 3 10707 1
BROMDBENZENE 19740 5 21763 6 18679 5
1,1,2 .2—TETRACHLOROETHANE 10899 4 11949 1 10829 6
1,2,3—TRICHLOROPROPANE 8081 S 9389 2 7892 3
n-PROPYL BENZENE 36279 5 43741 2 34624 1
2-CHLDROTOLUENE 25898 5 31305 0 24441 4
4-CHLOROTOLUENE 24309 5 29475 2 22531 1
tert-BUTYLBENZENE 35435 3 44062 0 33722 4
1.3,5—TRIHETHYLBENZENE 45020 3 57197 2 41723 4
sec-BUTYL BENZENE 48025 9 58814 3 46763 3
1,2-DIBROMO—3—CHLOROPROPANE 5004 6 5711 1 5773 4
1.2.4—TRIMETHYL8ENZENE 45919 5 55793 1 41421 4
1,3-DICHLORO8ENZENE 19013 6 22120 2 17360 0
p-ISOPROPYL TOLUENE 37421 3 43463 1 34472 3
1.4-DICHLOROBENZENE 18396 3 23224 1 16296 0
1.2-DICHLOROBENZENE—d4 18662 4 22224 3 17014 2
1.2-DICHLOROBENZENE 18370 2 21244 2 16821 2
n-BUTYL BENZENE 28111 4 33548 2 26934 1
1.2.4-TRICHLOROBENZENE 13994 1 16613 2 13032 3
HEXACHLORO BUTADIENE 8977 4 11086 3 9069 3
NAPHIHALENE 36234 1 40761 2 35029 7
1.2.3—TRICHLOROBENZENE 12004 3 14138 2 11507 2
DECREASING MMS VOLUME
56
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TABLE 67
DETERMINATION OF NDLs
25 ng FORTIFIED MMS/SAND
MG RECOVERED
RSD RECOVERY MDL
ANALYTE Sa te I Saupte 2 Sanp(e 3 AVG CX) CX) (ug/Kg)
DICHLORODIFLUOROMETHA NE 10.3 11.5 8.7 10.2 11.0 40.6 1.6
CHLOROMETHANE 13.1 15.5 12.7 13.8 8.8 55.0 1.7
VINYL CHLORIDE 11.3 8.8 11.0 10.4 11.1 41.5 1.6
BROMOMETHANE 17.7 26.7 14.1 19.5 27.1 78.0 7.4
CHLOROETHANE 17.6 23.1 15.9 18.9 16.5 75.5 4.3
TRICHLOROFLUORONETHANE 12.6 17.1 12.9 16.2 14.2 56.8 2.8
1,1-DICHLOROETHENE 15.1 15.4 16.6 15.0 2.2 60.1 0.5
trans-1,2-DICHLOROETHENE 28.0 29.0 27.9 28.3 1.8 113.2 0.7
1,1-DICHLOROETHAJIE 17.4 17.6 17.9 17.6 1.1 70.5 0.3
2.2-DICHLOROPROPAME 24.2 24.9 27.3 25.5 5.3 101.9 1.9
ds-1,2-DICHLOROETHENE 22.6 24.3 24.8 23.9 3.9 95.6 1.3
BROMOCHIOROMETHANE 28.9 30.2 30.5 29.9 2.3 119.5 1.0
CHLOROFORM 21.1 22.3 21.9 21.8 2.3 87.0 0.7
1,1 ,1-TRICHLOROETHA NE 20.8 21.3 21.9 21.3 2.2 85.3 0.7
1,1-DICHLOROPROPENE 25.9 27.3 26.4 26.5 2.2 106.1 0.8
CARBON TETRACHLORIDE 21.9 21.6 22.0 21.8 0.8 87.2 0.2
BENZENE 27.0 28.1 28.0 27.7 1.9 110.9 0.7
1,2-DICHLOROETHANE 25.4 27.5 27.8 26.9 4.0 107.5 1.5
TRICHLOROETHYLENE 21.9 22.8 21.6 22.1 2.3 88.4 0.7
1,2-DICKLOROPROPANE 22.4 24.4 24.5 23.8 4.2 95.1 1.4
DIBRONOMETHANE 25.3 29.5 28.1 27.6 6.3 110.5 2.4
BROI400ICHLORONETHANE 24.3 27.0 26.8 26.0 4.7 104.1 1.7
TOLUEME 27.1 29.5 27.2 27.9 4.0 111.7 1.5
1 ,1,2-TRICHLOROETMANE 24.4 25.9 26.8 25.7 3.8 102.9 1.4
TETRACHLOROETHTLENE 25.2 26.7 26.0 26.0 2.4 103.9 0.9
1,3-DICHLOR OPR OPANE 24.0 27.1 26.5 25.9 5.2 103.5 1.9
DIBROMOCHLOROMETHANE 23.3 25.2 25.9 24.8 4.4 99.2 1.5
1,2-DIBROMOETHANE 20.4 20.0 14.8 18.4 13.9 73.6 3.6
CHLOROBENZENE 24.8 27.1 25.9 25.9 3.6 103.7 1.3
1,1,1,2-TETRACHL OROETHAHE 29.2 33.6 33.2 32.0 6.2 128.1 2.8
ETHYL BENZENE 31.6 34.4 32.4 32.8 3.6 131.2 1.6
p-XYLEWE 29.7 31.4 29.1 30.1 3.2 120.3 1.4
o-XYLENE 29.3 31.7 31.0 30.7 3.3 122.7 1.4
STYREME 21.9 22.0 19.5 21.1 5.5 84.5 1.6
BRONOFORM 22.7 21.9 18.3 21.0 9.1 83.9 2.7
ISOPROPYLBENZENE 29.8 32.8 31.3 31.3 3.9 125.2 1.7
p-BROMOFLUOROBENZENE 27.2 25.6 19.2 24.0- 14.4 96.0 4.8
BRONOSENZENE 20.1 20.2 22.3 20.9 4.9 83.5 1.4
1,12,2-TETRACHLOROETHANE 22.0 23.5 30.6 25.4 14.8 101.4 5.2
1,2,3-TRIcHL0R0PR0PANE - 32.8 35.3 -34.9 34.3 3.2 137.3 1.5
n-PROPYL BENZENE 21.1 20.4 15.8 19.1 12.3 76.4 3.3
2-CHLOR OTOLUENE 21.5 23.3 22.5 22.4 3.3 89.7 1.0
4-CHL OROTOLUENE 24.0 26.0 25.1 25.0 3.3 100.1 1.1
tert-BUTYLBENZENE 21.9 23.6 22.7 22.7 3.1 90.9 1.0
1,3,5-TRIMETHYLBENZENE 20.6 22.8 22.2 21.9 4.2 87.5 1.3
sec-BUTYL BENZENE 21.7 23.5 22.8 22.7 3.3 90.7 1.0
1,2-DIBROMO-3-CHLOROPROPANE 22.0 23.9 24.5 23.5 4.5 93.9 1.5
1,2,4-TRIMETHYLBENZENE 20.3 19.8 15.2 18.4 12.5 73.7 3.2
1,3-DICHIOROSENZENE 20.2 20.2 15.4 18.6 12.2 74.4 3.2
p-ISOPROPYL TOLUENE 20.7 20.2 15.5 18.8 12.5 75.2 3.3
1,4-DICHLOROBEN2ENE 19.8 19.9 15.2 18.3 12.0 73.2 3.1
1,2-DICHLOROBENZENE-d4 26.1 25.2 18.4 23.2 14.8 92.9 4.8
1,2-DICHLORO BENZENE 20.1 19.4 15.3 18.3 11.6 73.1 2.9
n-BUTYL BENZENE 20.1 19.3 14.7 18.0 13.2 72.1 3.3
1 ,2,4-TRICHLORO BENZENE 19.8 18.9 14.2 17.6 13.9 70.5 3.4
HEXACHLOROSUTADIENE 19.6 21.7 19.7 20.3 4.8 81.3 1.3
NAPHTHALENE 20.1 19.6 15.2 18.3 12.0 73.2 3.1
1,2,3-TRICHLOROBENZENE 17.3 17.3 12.5 15.7 14.4 62.8 3.2
57
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Area (thousands)
120
100
80
60
I ”
40
20
0
decreasing headspace vo’ume ->
DCDFMETHANE I CHLOROFORM * BENZENE
0 CHLOROBENZENE > < 135TRIMETHYLBEN 0 NAPHTHALENE
Figure 1. Effect of Different Headspace Volumes
On Analyte Recovery
x
I I I
-------
Compound
__ 7mL MMS
. 1 4.5mL MMS
Effect of Different MMS Volumes On
Analyte Recovery of Six Compounds
Area (thousands)
60
50
40
30
20
10-
0—
1. Dlchlorodlfluorobenzene
2. Chloroform
3. Benzene
4. Chlorobenzene
5. 1,35-Trimethylbenzene
8. Naphthalene
n
H .
1 2
3 4
lOmL MMS
Figure 2.
5 6
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