United States
Environmental Protection
Agency
Analytical Protocol
(GC/ECNIMS) for OSWER's
Response to OIG Report
(2005-P-00022) on
Toxaphene Analysis
RESEARCH AND DEVELOPMENT
-------
EPA/600/R-08/048
May 2008
www.epa.gov
Analytical Protocol
(GC/ECNIMS) for OSWER's
Response to OIG Report
(2005-P-00022) on
Toxaphene Analysis
Prepared by
William C; Brumley
U.S. Environmental Protection Agency
Office of Research and Development
National Exposure Research Laboratory
Environmental Sciences Division
Environmental Chemistry Branch
944 E. Harmon Ave.
Las Vegas, NV 89119
Notice: Although this work was reviewed by EPA and approved for publication, it may not necessarily reflect official
Agency policy. Mention of trade names and commercial products does not constitute endorsement or
recommendation for use.
U.S. Environmental Protection Agency
Office of Research and Development
Washington, DC 20460 077ecb08
-------
Analytical Protocol (GC/ECNIMS) for OSWER's Response to OIG Report
(2005-P-00022) on Toxaphene Analysis
Prepared by William C. Brumley
13 February 2008
Abbreviations
ASE: accelerated solvent extraction, Dionex instrument; NIMS: electron capture negative ion
mass spectrometry, IS: internal standard; MDLs: method detection limits; MQLs: method
quantitation limits; OCPs: organochlorine pesticides; OIG: Office of Inspector General; OSW:
Office of Solid Waste; ppb: parts per billion (u.g/kg); ppt: parts per trillion (ng/kg); SPE-Si: solid
phase extraction using silica; TIC: total ion chromatogram
Background
This document offers a GC/MS protocol (attached as a text file and with supplementary data) for
updating Method 808 la with (electron capture and dissociative electron capture) negative ion
mass spectrometry (NIMS) for the determination/confirmation of selected analytes. The scope of
the protocol covers most of the existing analytes in 8081a (first listing in section 1.1). This
approach was developed in response to the OIG Report on Toxaphene [1] and to a specific
request from Barry Lesnick, OSW [2]. The approach discussed here divides the analytes into
four classes for either monitoring or method performance evaluation purposes: chlordane,
toxaphene, organochlorine pesticides, and toxaphene congeners. The two complex mixtures of
chlordane (chlordanes and related compounds heptachlor and nonachlor) and toxaphene
(polychlorinated camphenes and bomanes) involve monitoring a series of ions representing
various congener groups found in the mixtures and integrating all of these signals for a total
toxaphene or chlordane response. In the case of the organochlorine pesticides (OCPs) and the
toxaphene congeners, individual compounds are quantitated separately and reported separately.
Although the protocol does not address all of the 800-plus congeners that comprise toxaphene,
additional toxaphene congeners can be added to the method by simply identifying retention time
windows and associated responses as the additional congeners with the caveat that the responses
are resolved from other congeners (arguably, a difficult procedure). The PCB congener #204
(2,2',3,4,4',5,6,6'-octachlorobiphenyl, not found in the Aroclors) originally used by Swackhamer
et al. [3] was retained as internal standard although a number of different compounds could be
used as internal standard (e.g., dlO-chlorpyrifos). The methodology for toxaphene and chlordane
was also published as a peer-reviewed article in our earlier work performed at NERL-Las Vegas
page 1 of 15 13 February 2008
-------
[4,5].
The compounds 4,4'-DDD, 4,4'-DDE, and 4,4'-DDT, among the analytes of Method 808 la, do
not respond sensitively under NIMS conditions and should continue to be confirmed/quantitated
by GC/MS using El mass spectrometry and GC/ECD. The data we have obtained indicate that
the oxygen reaction observed with PCBs that gives rise to ions potentially interfering with
toxaphene determination (i.e., ions at the same nominal mass but not the same elemental
composition) is completely eliminated in modern instruments under appropriate conditions, and
the chosen internal standard serves to monitor this situation by the absence of (M - Cl + O)" ions
(e.g., m/z 411) at its retention time (less than 0.5% possible attributable response). The protocol
depends necessarily on the proper extraction, cleanup, concentration, and separations to achieve
the quantitations and confirm the target analytes.
This report includes detailed data concerned with calibrations and separation conditions as well
as ions monitored for each analyte class. Attached compressed files include the complete
protocol from the method print out in text format and full size screen captures of the calibration
plots with some data pairs visible. This method can be implemented directly by the user and
enables complete reproduction of the experiments provided the instrumentation is available.
Some performance data is included here for spiked soil for each of the analyte classes to assess
the performance of the protocol in a realistic setting. The protocol exhibits acceptable stability
normally spanning several weeks for a given calibration and excellent precision for the
determinative step (replicate injections of a given sample extract) of about 2%. Variations in the
replicates for spiked soil are chiefly the result of variability in the two concentration steps
performed (one following ASE extraction, and one following SPE-Si cleanup) since the
determinative step is tightly reproducible. The emphasis with the performance data is on
assessing overall reproducibility, ruggedness, and applicability because recoveries are not the
focus of this GC/MS protocol. Recoveries would be an appropriate emphasis for a complete new
method development for SW-846. Thus, the GC/MS protocol here is an additional
confirmation/quantitation option for the existing Method.
Experimental approach
Note regarding nomenclature: For the background regarding the term "parlars", see: [6]. The Hx-
Sed and Hp-Sed congeners specifically mentioned in the OIG Report refer to the two
environmentally significant toxaphene congeners, hexa- and hepta-chlorobornane, which had
been isolated from sediment; see [7, 8, 9].
Analytical standards: The OCPs, toxaphene, and chlordane standards were purchased from
Supelco (Bellafonte, PA, USA). The toxaphene congener solutions were purchased from LGC
PromoChem (United Kingdom). The sediment mix was DE-TOX 484 and contained 2-endo,3-
exo,6-exo,8,9,10-hexachlorobornane, 2-endo,3-exo,5-endo,6-exo,8,9,10-heptachlorobomane
(Hp-Sed), 2-exo,3-endo,6-exo,8,9,10-hexachlorobornane (Hx-Sed), 2-exo,3-endo,5-exo,6-
exo,8,9,10-heptachlorobornane (designated PI in this discussion). The important isomer mix
page 2 of 15 13 February 2008
-------
(parlars) was DE-TOX 483 and contained 2-exo,3-endo,5-exo,6-exo,8,9,10,10-
heptachlorobornane (designated P2 in this discussion), 2-endo,3-exo,5-endo,6-exo,8,8,10,10-
octachlorobornane(T2, parlar 26), 2,2,5,5,9,9,10,10-octachloroboraane (parlar 38), 2-endo,3-
exo,5-endo,6-exo,8,9,10,10-octachlorobomane (parlar 40), 2-exo,3-endo,5-exo,6-
exo,8,9,9,10,10-octachlorobomane (parlar 41), 2-exo, 5,5,8,9,9,10,10-octachlorobornane (parlar
44), 2-endo,3-exo,5-endo,6-exo,8,8,9,10,10-nonachlorobornane (T12, parlar 50),
2,2,5,5,8,9,9,10,10-nonachlorobornane (parlar 62). The first mix identities were deduced from
literature and analysis. The second mix contained only 5 distinct peaks for 8 components listed
and were partially deduced from literature and analysis with coelution assumed among the
remaining observed peaks which appeared to be multicomponent (i.e., parlars 38,40,41 and 50,
62).
GC/MS Protocol Features:
The protocols reported here were developed on an Agilent GC/MSD 7673 (analytes chlordane
and OCPs) and an Agilent GC/MSD 7675 (analytes toxaphene and toxaphene congeners) both
fitted with 6890 gas chromatographs. Thus, the protocol involves both the previous generation
and the latest generation of Agilent instruments, and both performed adequately. The column
parameters on the 7673 were injector 250°C, transfer 280°C, 0.5 mL/min flow rate, 40 m Agilent
J&W DB5MS, 0.18 mm ID, 0.18 nm film thickness. The column parameters used on the 7675
were injector 250 °C, transfer 280°C, 1.2 mL/min flow rate, 30 m Agilent HP5MSI, 0.25 mm ID,
0.25 um film thickness. The GC program was the same for the two instruments: 60°C for 1 min,
60°C to 150°C at 10°C/min, 150°C to 250°C at 4°C/min, 250°C to 300°C at 10°C/min and hold
for 6 min.
Ions monitored for the chlordane analysis: m/z 429.8 (IS); 303.9, 305.9, 337.9, 339.9, 341.9,
371.8, 373.8, 375.8, 407.8, 409.8, 411.8,441.8, 443.8, 445.8, and optional 321.9 (dlO-
chlorpyrifos) all for 25 msec dwell time. Quantitation was performed by using manual
integration of the total ion chromatogram (TIC) within the retention time window of chlordane.
Ions monitored for the OCPs analysis: m/z 429.8 (IS); Groupl: 252.9, 254.9, 256.9, 263.9, 265.9,
267.9, 297.9, 299.9, 301.9 and Group 2 (start 26.50 min): 234.9, 236.9, 238.9, 327.9, 329.9,
331.9, 377.9, 379.9, 381.9, 385.9, 387.9, 389.9, 403.7, 405.7, 407.7, 419.7, 421.7,423.7; and
optional 321.9 (dlO- chlorpyrifos) all for 25 msec dwell time. Quantitation was based on m/z
254.9 for a-BHC, 0-BHC, y-BHC, and 8-BHC; 299.9 for heptachlor; 329.9 for aldrin; 389.9 for
heptachlor epoxide; 405.8 for endosulfan I and II; 379.9 for dieldrin, endrin, and endrin
aldehyde; 421.7 for endosulfan sulfate. Alternatively, these ions can all be done in one group,
eliminating the need for defining a group break time.
Ions monitored for the toxaphene analysis: m/z 429.8 (IS); 306.9, 308.9, 310.9, 340.9, 342.9,
344.9, 376.9, 378.9, 380.9, 410.8, 412.8, 414.8, 444.8, 446.8, 448.8, and optional 321.9 (dlO-
chlorpyrifos) all for 25 msec .dwell time. Quantitation was performed by using manual
integration of the TIC within the retention tune window of toxaphene.
page 3 of 15 13 February 2008
-------
Ions monitored for the toxaphene congener analysis: m/z 429.8 (IS);306.9, 308^9, 3 10.9, 340.9,
342.9, 344.9, 376.9, 378.9, 380.9, 410.8, 412.8, 414.8, 444.8, 446.8, 448.8, and optional 321.9
(dlO- chlorpyrifos) all for 25 msec dwell time. Quantisation was based on m/z 308.9 for Hx-sed,
342.9 for Hp-sed, m/z 378.9 for parlar 26 and 38, 40, 41, m/z 412.8 for parlar 50,62.
The reagent gas, methane, was set at a flow setting of 40 which means 40% of 2 mL/min. A
number of other parameters characterize the conditions, some of which reside within the tune file
that contains the calibration data. The instrument temperatures for the GC/MSD 5975 were
150°C for both source and quadrupole region and for the GC/MSD 5973 were 150°C for the
source and 106°C for the quadrupole (these are the customary settings for each respective
instrument as recommended by the vendor). The emission current is set automatically during the
tune. The electron multiplier voltage was set at 2000V absolute. The appropriate tune file also is
created with the polarity negative as befits the technique. Attached to this document in a zip file
are the four acquisition file parameters as text files as put out by the data system for the four
classes of analytes.
Spiked Soil Extractions/Cleanup:
A large number of development runs were made to somewhat refine the sample handling part of
the methodology and ensure greater reproducibility, but no exhaustive attempt was made to
reduce variations further. Seven replicates of soil (25 ppb toxaphene, 50 ppb chlordane, 50 ppb
each of the OCPs, and 500 ppt each of the toxaphene congeners) were analyzed treating each
class of analytes independently (total of 28 data sets reported). In each case 5 g of soil was
spiked and extracted using ASE. The soil was New England Horizan A, sifted and homogenized
.(obtained from Dr. Brian Schumacher, EPA). The solvent was 50/50 acetone/methylene chloride
and the conditions were 5 min equilibration, 1 5 min static extraction at 80°C, and 2500 psi
pressure. The extract was then concentrated just to dryness under a gentle nitrogen stream and
redissolved in hexane using sonication (not all components redissolve, presumably more polar
analytes do not) with hexane for SPE cleanup. The 3 mL SPE Si cartridges were rinsed with 6
mL of hexane. The sample was applied in 1 mL of hexane and eluted with 3 mL hexane. The
OCPs and parlars were not fully recovered with hexane elution and SPE cartridges were further
subjected to 2 mL hexane/methylene chloride followed by 2 mL of methyl ene chloride. All
eluants were combined and concentrated to about 1 mL. The internal standard was added and the
sample extract was placed in a GC vial for analysis with the internal standard concentration at 10
Calibrations
Calibration plots are included within the document and attached separately as *.png files (in the
attached zip file) for all of the compounds. Calibrations were generally linear with r2 of 0.98 or
0.99. The plots contain a visible tabulation of 3 or 7 pairs of the data that are used as area ratios
versus amount ratios where the internal standard amount or area is the divisor. Additional data
pairs may not be visible in the screen captures. These are captured plots afforded directly by the
data system (EnviroQuant ChemStation version B.01.00 and Enhanced MSD ChemStation
page 4 of 15 13 February 2008
-------
D.02.00.275) . As such they give an idea of the linearity and intercept of the plots, and,
additionally, show the equation and some of the raw data.
By using the lowest calibration point as the method detection limit, estimates of achievable
detections in samples can be obtained. Detection limits are strongly dependent on sample and
matrix interferences. Additional cleanup may be needed when multiple analyte classes and
additional contaminants are present in real samples.
Results from Spiked Soils
In general the spiked soil results were reproducible within the 15-20% relative standard deviation
range. There were some notable exceptions (certain OCPs) among the analytes that exhibited
higher standard deviations and some obviously low recoveries. Method variability less than 10%
is a desired goal but since the reproducibility of the determinative step is 2%, attempts at further
refinement in the overall methodology is not germane to this report.
Table 1 lists the values obtained for determining toxaphene in spiked soils. The average recovery
and percent relative standard deviation were 38.7 ppb for a 25 ppb spike and 17.8% relative
standard deviation. There was a toxaphene-like background (appropriate ions in the retention
time window) in the soil although the pattern was different from the standard. All soils available
to us exhibited a background response for toxaphene ions. The reagent blank for toxaphene was
10 ppb while the unspiked soil contained 13 ppb level of toxaphene-like response that may
indicate as much as a 25 ppb level of background when corrected for recovery. The background
level and reagent blank thus explains the high recovery from the 25 ppb spike. In the face of a
lack of a clean laboratory facility and the lack of a true blank media, it was not deemed essential
to try to further improve the results reported here for spiked soils involving toxaphene.
Table 1 also lists the values obtained for determining chlordane. The average recovery and
percent relative standard deviation were 31.5 ppb for a 50 ppb spike and 16.7% relative standard
deviation. The chlordane blank soil response was about 10 ppb.
Table 2 tabulates values for the toxaphene congeners. The congeners were essentially not
detected in blanks. The results are fairly consistent with the overall work reproducibility here
with precision between 10% to 20% relative standard deviation.
Table 3 summarizes data for the OCPs. The OCPs were absent in soil and reagent blanks. The
• levels were consistent with the reproducibility found in this work with the exception of the
endosulfan I and n and endrin aldehyde. These compounds are obviously subject to greater
recovery variability than the other OCPs. It was first supposed that the P-BHC compound was
coalescing with the y-BHC peak at lower levels and the two compounds would be combined.
Later it was realized that the P-BHC was indeed distinct but exhibited a response between 10 to
15 tunes less than that of y-BHC and disappeared below the 250 pg/uL level. Distinct
observations of P-BHC in spiked soils allowed requantitation from a limited but applicable
page 5 of 15 . 13 February 2008
-------
calibration response. A calibration plot derived from a new calibration involving higher values
for P-BHC has been included. All of the BHC isomers exhibited poor chromatographic peak
shape with pronounced tailing.
Method Quantitation Limits (MQLs)
Based on the lowest calibration point in the calibration data, the MQL (simple estimate of lowest
reliable quantitation) for toxaphene is 50 pg/|J.L or 10 ppb for a 5 g soil sample. A similar
approach for chlordane yields an MQL of 125 pg/fiL or 25 ppb for a 5 g soil sample. The
toxaphene congeners were responsive to at least 625 fg/p.L which would be 125 ppt for a 5 g soil
•sample. The OCPs were calibrated to 12.5 pg/jiL (except for P-BHC) resulting in a 2.5 ppb
level per component in a 5 g soil sample. A more conservative estimate of MQLs can be based
on the spiked soil data provided in this report. Method detection limits (MDLs) have not been
determined in accordance with SW-846 guidance because the request for a GC/MS protocol was
not linked to specific matrices, and performance data as would be required for a full method
development were not obtained.
Concluding Remarks
The determination of the complex analytes chlordane and toxaphene was approached by using a
number of ion groups spanning the congeners present. This ensures that transformation products
will be included in the integrated signal in the context of a real-world analysis. The total ion
current integration across the entire response envelop for the composite analyte is the most
simple approach but tends to overemphasize the amount present in a real sample in some cases
where there may be matrix contributions to monitored ions. In other cases where weathering or
transformations have occurred, the comparison of sample signal to the response of a laboratory
standard is inaccurate and likely to be inconsistent between NIMS and GC/ECD.
Because of environmental transformations of the multicomponent analytes, congener specific
analysis is the more defensible form of determination. Weathered toxaphene determinations
suffer from a lack of an appropriate standard to derive meaningful results. Some effort was made
to develop macros to use more sophisticated integration but the results were not different enough
to justify the increased complexity. The ChemStation software does not handle
multiresponse/multicomponent analytes directly as it is optimized for a quantitation ion or a total
ion current in the form of a peak at a given retention time. The approach described here thus
requires manual intervention (or macro construction) and review, but review is essential even in
trivial analyses which must be checked for proper integration and assignment in any serious
quality control framework. The current application of the official Method by GC/ECD already
integrates the signal over a window so that this approach is consistent with current practice. It
should be further emphasized that the oxygen reaction with PCBs has been eliminated as a
concern in toxaphene analysis by GC/NIMS, and the presence of internal standard PCB#204
ensures that this is properly demonstrated by monitoring m/z 411 at the retention time of the
internal standard when it is run separately.
page 6 of 15 13 February 2008
-------
page 7 of 15 13 February 2008
-------
Notice
The United States Environmental Protection Agency through its Office of Research and
Development funded and managed the research described here. It has been subjected to Agency's
peer and administrative review and approved for publication as an EPA document.
References
1. OIG Report on Toxaphene, http://www. epa.gov/oig/reports/2006/20051216-2006-P-
00007.pdf.
2. email, Barry Lesnick, 11/02/2005.
3. D. L. Swackhamer, M. J. Charles and R. A. Kites, "Quantitation of Toxaphene in
Environmental Samples Using Negative Ion Chemical lonization Mass Spectrorrietry," Anal.
Chem., 59, 913-917(1987).
4. W. C. Brumley, E. Latorre, V. Kelliher, A. Marcus, and D. Knowles, "Determination of
Chlordane in Soil by LC/GC/ECD and GC/EC NIMS.with Comparison of ASE, SFE, and
Soxhlet Extraction" J. Liq. Chromatogr., 21, 1199-1216 (1998).
5. W. C. Brumley, C. M. Brownrigg, and A. H. Grange, "Determination of Toxaphene in Soil by
Electron-capture Negative Ion Mass Spectrometry after Fractionation by High-performance Gel
Permeation Chromatography," J. Chromatogr., 633, 177-183 (1993).
6. http://l92.129.24.144/licensed_materials/0698/papers/0003k/0003k0237.pdf
7. G. A Stem, M. D. Loewen, B. M. Miskimmin, D. C. G. Muir, and J. B.Westmore,
"Characterization of Two Major Toxaphene Components in Treated Lake Sediment," Environ.
Sci. Technol, 30, 2251-2258 (1996).
8. http://pubs.acs.org/cgi-bin/article.cgi/esthag/1996/30/i07/pdf7es950622y.pdf.
9. L. Kimmel, D. Angerhoefer, U. Gill, M. Coelhan, and H. Parlar, "HRGC-ECD and HRGC-
ECNI-SIM-HRMs Quantification of Toxaphene Residues by Six Environmentally Relevant
Chlorobornanes as Standard," Chemosphere, 37(3), 549-558 (1998).
page 8 of 15 13 February 2008
-------
Table 1. Quantitations of spiked soil for toxaphene (25 ppb, 5 g sample) and chlordane (50 ppb,
5 g sample).
Replicate no.
1
2
3
4
5
6
7
avg
% rel std dev
Toxaphene in ppb
34.2
46.4
42.7
35.0
27.0
42.0
43.9
38.7
17.8
Chlordane in ppb
31.4
35.2
29.4
41.6
27.0
27.8
28.0
31.5
16.7
page 9 of 15
13 February 2008
-------
Table 2. Quantitations of spiked soil for toxaphene congeners (500 ppt, 5 g sample).
Replicate no.
1
2
3
4
5
6
7
avg
rel std dev %
Hx-Sed
468
690
768
688
780
778
672
692
15.8
Hp-Sed
532
722
746
724
752
786
784.
720
12.1
PI
454
698
720
742
758
756
782
702
16.0
Parlar 26
552
788
778
808
804
822
706
752
12.7
P2
542
894
836
910
942
928
1032
870
17.9
Replicate no.
1
2
3
4
5
6
7
avg
rel std dev %
Parlar
38,40,41
508
792
808
856
860
826
866
788
16.1
Parlar 44
696
930
876
1016
986
942
1266
958
17.8
Parlar 50,62
544
812
702
844
790
750
772
744
13.4
page 10 of 15
13 February 2008
-------
Table 3. Quantitations of spiked soil for OCPs (50 ppb, 5 g sample).
Replicate
no.
1
2
3
4
5
6
7
avg
% rel std
dev
alphaBHC
28.0
40.6
33.0
27.0
42.4
43.2
37.6
36.0
18.7
betaBHC
52.0
57.6
46.4
71.6
71.4
64.4
43.2
58.0
19.9
deltaBHC
39.8
50.0
37.8
40.4
53.4
51.2
32.2
43.6
18.3
heptachlor
34.8
44.6
35.4
28.2
49.2
53.0
49.0
42.0
22.0
aldrin
40.8
53.4
42.0
34.4
56.6
59.8
53.0
48.6
19.5
heptachlor
epoxide
51.2
53.0
46.2
51.8
59.6
62.4
54.2
54.0
10.0
Replicate
no.
1
2
3
4
5
6
7
avg
% rel std
dev
endosulfan
I
16.8
21.4
37.8
51.0
25.2
20.4
13.0
26.6
50.1
dieldrin
73.8
70.4
61.2
69.6
74.4
74.2
62.8
69.4
7.9
endrin
73.6
72.6
63.6
68.6
72.8
70.6
66.6
69.8
5.3
endosulfan
n
17.7
29.4
38.4
43.0
37.8
.29.8 .
11.1
29.6
39.2
endrin
aldehyde
26.0
44.6
19.7
25.6
44.2
42.8
37.8
34,4
30.1
endosulfan
sulfate
36.6
47.4
37.6
42.8
51.0
52.4
46.2
44.8
13.8
page 11 of 15
13 February 2008
-------
Attachments imbedded:
Calibrations plots
Attachments as zip file
Calibrations plots (full size)
Method ouputs as text files
C-U
page 12 of 15
13 February 2 00 8
-------
page 13 of 15
13 February 2008
-------
SW-846 Format for NIMS Confirmation/Quantitation Draft Form
7.7 NIMS GC/MS confirmation/quantitation may be used in conjunction with either
single-column or dual-column analysis.
7.7.1 Selected ion monitoring NIMS GC/MS is capable of reaching similar
detection limits to those of GC/ECD. The ions monitored and quantitation ions are given
in Table 1.
7.7.2 The NIMS GC/MS must be calibrated for the specific target pesticides when
it is used for quantitative analysis.
7.7.3 NIMS GC/MS may not be used for quantitation when concentrations are
below MDLs.
7.7.4 NIMS GC/MS confirmation should be accomplished by analyzing the same
extract that is used for GC/ECD analysis and the extract of the associated method blank.
7.7.5 The base/neutral/acid extract and the associated blank may be used for
NIMS GC/MS confirmation if the surrogates and internal standard do not interfere and if
it is demonstrated that the analyte is stable during acid/base partitioning. However, if the
compounds are not detected in the base/neutral/acid extract, then GC/MS analysis of the
pesticide extract should be performed..
7.7.6 A QC reference sample containing the compound must also be analyzed by
GC/MS. The concentration of the QC reference sample must demonstrate that those
pesticides identified by GC/ECD can be confirmed by NIMS GC/MS or EMS GC/MS.
page 14 of 15 13 February 2008
-------
Table 1. Selected Ion monitoring for analytes by GC/NIMS
Compound
toxaphene
chlordane
alpha-BHC
beta-BHC
gamma-BHC
delta-BHC
beptachlor
aldrin
heptacblor epoxide
endosulfan I, D
dieldrin
endrin
endrin aldehyde
endosulfan sulfate
parlar 26,38
parlar 38,40,41
parlar 50,62
Hx-Sed
Hp-Sed
IS, PCB#204
Quantitation ion
TIC
TIC
254,9
254.9
254.9
254.9
299.9
329.9
389.8
405.7
379.9
379.9
379.9
421.7
378.9
378.9
412.8
308.9
342.9
429.8
Other ions
306.9,308.9,310.9,340.9,342.9,344.9,37
6.9,378.9,380.9,410.8,412.8,414.8,444.8
446.8,448.8
303.9,305.9,337.9,339.9,341.9,371.8,37
3.8,375.8,407.8,409.8,411.8,441.8,443.8
445.8
252.9,254.9,256.9
252.9,254.9,256.9
252.9,254.9,256.9
252.9,254.9,256.9
297.9,299.9,301.9,263.9,265.9,267.9
327.9,329.9,331.9
387.9,389.9,391.9
403.7,405.7,407.7
377.9,379.9,381.9
377.9,379.9,381.9
377.9,379.9,381.9
419.7,421.7,423.7
toxaphene ions
toxaphene ions
toxaphene ions
toxaphene ions
toxaphene ions
410.8
Comments
Manual integration
Manual integration
Group 1
Group 1
Group 1
Group 1
Group 1
Group2 (26.5 min)
Group2 (26.5 min)
Group2 (26.5 min)
Group2 (26.5 min)
Group2 (26.5 min)
Group2 (26.5 min)
Group2 (26.5 min)
Monitor oxygen reaction
page 15 of 15
13 February 2008
------- |