EPA Document #: EPA/600/R-12/010
METHOD 525.3 DETERMINATION OF SEMIVOLATILE ORGANIC CHEMICALS IN
               DRINKING WATER BY SOLID PHASE EXTRACTION AND
               CAPILLARY COLUMN GAS CHROMATOGRAPHY/ MASS
               SPECTROMETRY (GC/MS)
                                 Version 1.0
                               February, 2012
Jean W. Munch and Paul E. Grimmett (U.S. EPA, Office of Research and Development,
National Exposure Research Laboratory)

David J. Munch and Steven C. Wendelken (U.S. EPA, Office of Water, Office of Ground
Water and Drinking Water, Technical Support Center)

Mark M. Domino (Industrial and Environmental Services, LLC)

Alan D. Zaffiro and Michael L. Zimmerman (Shaw Environmental and Infrastructure,
Inc.)
              NATIONAL EXPOSURE RESEARCH LABORATORY
                 OFFICE OF RESEARCH AND DEVELOPMENT
               U. S. ENVIRONMENTAL PROTECTION AGENCY
                          CINCINNATI, OHIO 45268
                                   525.3-1

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                                  METHOD 525.3
  DETERMINATION OF SEMIVOLATILE ORGANIC CHEMICALS IN DRINKING
    WATER BY SOLID PHASE EXTRACTION AND CAPILLARY COLUMN GAS
             CHROMATOGRAPHY/ MASS SPECTROMETRY (GC/MS)

1.  SCOPE AND APPLICATION

   1.1.   This is a gas chromatography/mass spectrometry (GC/MS) method for the
         determination of selected semivolatile organic compounds in drinking waters.  Accu-
         racy and precision data have been generated in reagent water, and in finished ground
         and surface waters for the compounds listed in the table below. This method was
         initially developed with full scan GC/MS, but performance has also been demonstrated
         in the selected ion monitoring (SIM) mode using a subset of analytes.  SIM is useful
         when enhanced sensitivity is desirable.  An example chromatogram which includes the
         entire analyte list is shown in Figs, la-Id.
Analyte
Acenaphthylene
Acetochlor
Alachlor
Aldrin
Ametryn
Anthracene
Atraton
Atrazine
B enzo [a] anthracene
Benzo[&]fluoranthene
B enzo [k] fluoranthene
Benzo[a]pyrene
Benzo[g,/7,/']perylene
Bromacil
Butachlor
Butylate
Butylated hydroxytoluene (BHT)
Butylbenzylphthalate
Chlordane (tech grade)
cis-chlordane
trans-chlordane
trans-nonachlor
Chlorfenvinphos
Chloroneb
Chlorobenzilate
Chemical Abstract
Services Registry
Number (CASRN)
208-96-8
34256-82-1
15972-60-8
309-00-2
834-12-8
120-12-7
1610-17-9
1912-24-9
56-55-3
205-99-2
207-08-9
50-32-8
191-24-2
314-40-9
23184-66-9
2008-41-5
128-37-0
85-68-7
12789-03-6
5103-71-9
5103-74-2
39765-80-5
470-90-6
2675-77-6
510-15-6
                                       525.3-2

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Analyte
Chloropropham
Chlorothalonil
Chlorpyrifos
Chrysene
Cyanazine
Cycloate
Dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET(N,N-Diethyl-meta-toluamide)
Dibenz[a,/z]anthracene
Di-n-butylpthalate
Dichlorvos
Dieldrin
Diethylphthalate
Di(2-ethylhexyl)adipate
Di(2-ethylhexyl)phthalate
Diisopropyl methylphosphonate (DIMP)
Dimethipin
Dimethylphthalate
Dinitrotoluene, 2,4-
Dinitrotoluene, 2,6-
Diphenamid
Disulfoton
Endosufan I
Endosufan II
Endosufan sulfate
Endrin
EPTC (S-Ethyl dipropylthiocarbamate)
Ethion
Ethoprop
Ethyl parathion
Etridiazole
Fenarimol
Fluorene
Fluridone
Heptachlor
Heptachlor epoxide
Hexachlorobenzene (HCB)
Hexachlorocyclohexane, alpha (a-HCH)
Hexachlorocyclohexane, beta (P-HCH)
Chemical Abstract
Services Registry
Number (CASRN)
101-21-3
1897-45-6
2921-88-2
218-01-9
21725-46-2
1134-23-2
1861-32-1
72-54-8
72-55-9
50-29-3
134-62-3
53-70-3
84-74-2
62-73-7
60-57-1
84-66-2
103-23-1
117-81-7
1445.75.6
55290-64-7
131-11-3
121-14-2
606-20-2
957-51-7
298-04-4
959-98-8
33213-65-9
1031-07-8
72-20-8
759-94-4
563-12-2
13194-48-4
56-38-2
2593-15-9
60168-88-9
86-73-7
59756-60-4
76-44-8
1024-57-3
118-74-1
319-84-6
319-85-7
525.3-3

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Analyte
Hexachlorocyclohexane, delta (5-HCH)
Hexachlorocyclohexane, gamma (y-HCH) (Lindane)
Hexachlorocyclopentadiene (HCCPD)
Hexazinone
Indeno [\.,2,3-c,d] pyrene
Isophorone
Methoxychlor
Methyl parathion
Metolachlor
Metribuzin
Mevinphos
MGK 264
Molinate
Napropamide
Nitrofen
Norflurazon
Oxyfluorfen
Pebulate
Pentachlorophenol
Phenanthrene
Permethrin, cis-
Permethrin, trans-
Prometon
Phorate
Phosphamidon
Profenofos
Prometryn
Pronamide
Propachlor
Propazine
Pyrene
Simazine
Simetryn
Tebuconazole
Tebuthiuron
Terbacil
Terbutryn
Tetrachlorvinphos
Tribufos
Toxaphene
Triadimefon
Trifluralin
Chemical Abstract
Services Registry
Number (CASRN)
319-86-8
58-89-9
77-47-4
51235-04-2
193-39-5
78-59-1
72-43-5
298-00-0
51218-45-2
21087-64-9
7786-34-7
113-48-4
2212-67-1
15299-99-7
1836-25-5
27314-13-2
42874-03-3
1114-71-2
87-86-5
85-01-8
54774-45-7
51877-74-8
1610-18-0
298-02-2
13171-21-6
41198-08-7
7287-19-6
23950-58-5
1918-16-7
139-40-2
129-00-0
122-34-9
1014-70-6
107534-96-3
34014-18-1
5902-51-2
886-50-0
22248-79-9
78-48-8
8001-35-2
43121-43-3
1582-09-8
525.3-4

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Analyte
Vernolate
Vinclozolin
Polychlorinated Biphenyl (PCB) Congeners (IUPAC #)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2, 2 ', 3 , 5 '-tetrachlorobiphenyl (44)
2,2',5,5'-tetrachlorobiphenyl(52)
2, 3 ',4 ', 5 -tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (110)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Chemical Abstract
Services Registry
Number (CASRN)
1929-77-7
50471-44-8

2051-60-7
2051-62-9
34883-43-7
37680-65-2
7012-37-5
41464-39-5
35693-99-3
32598-11-1
38380-03-9
31508-00-6
35065-28-2
38380-04-0
35065-27-1
35065-29-3
1.2.    The Minimum Reporting Level (MRL) is the lowest analyte concentration that meets
       Data Quality Objectives (DQOs) that are developed based on the intended use of this
       method.  The single laboratory lowest concentration MRL (LCMRL) (Sect. 3.12) is
       the lowest true concentration for which the future recovery is predicted to fall, with
       high confidence (99 percent), between 50 and 150 percent recovery.  The LCMRL is
       compound dependent and is also dependent on extraction efficiency,  sample matrix,
       fortification concentration, and instrument performance.  The procedure used to
       determine the LCMRL is described elsewhere.1;2 During method development,
       LCMRLs were determined by two laboratories from the results of laboratory
       fortified blanks (LFBs) in full scan mode for all method analytes. LCMRLs were
       also determined for selected analytes in the SIM mode.  These LCMRLs are
       provided in Tables 15  and 23 for full scan  and SIM analyses, respectively.

1.3     Laboratories using this method are not required to determine the LCMRL for this
       method, but will need to demonstrate that their laboratory MRL for this method
       meets the requirements described in Sect. 9.2.4.

1.4     Determining the Detection Limit (DL) for  analytes in this method is optional
       (Sect. 9.2.6). Detection limit is defined as the statistically calculated minimum
       concentration that can be measured with 99% confidence that the reported value is
       greater than zero.3  The DL is compound dependent and is also dependent on
       extraction efficiency, sample matrix, fortification concentration, and instrument
       performance. DLs have been determined for all analytes in two laboratories in full
                                     525.3-5

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       scan mode (Table 15) and by a single laboratory for selected analytes in SIM mode
       (Table 23).

1.5     This method is intended for use by analysts skilled in solid phase extractions, the
       operation of GC/MS instruments, and the interpretation of the associated data.

1.6     Analysts and laboratory managers are advised that analyzing for all of the method
       analytes on a continuing basis while maintaining quality control criteria may be
       difficult. It is highly recommended that analysts and laboratory managers consider
       analyzing a subset of the analyte list that will meet their data collection needs.

1.7     Multi-Component Analytes

       1.7.1    Toxaphene is a pesticide manufactured by the chlorination of camphene.
               Over 1000 individual congeners, mainly chlorinated bornanes,  have been
               identified in the technical mixture, although over 30,000 are theoretically
               possible.  The most abundant of the individual components of the technical
               mixture are typically less than 1% by weight of the total mass.  Using the
               instrument parameters in Method 525.3, technical toxaphene elutes as a
               poorly defined group of peaks between 21 and 26 min (Fig. 2).
               Toxaphene's complex composition introduces the potential for interferences
               that could negatively affect the method performance for other analytes.
               Therefore, all calibration standards and quality control procedures for
               toxaphene must be prepared and analyzed in separate samples from all the
               other method analytes.  Toxaphene may be analyzed using this method in
               either full scan or SIM mode. However, the authors have demonstrated the
               method in SIM mode only.  At the time of method development, the
               enhanced sensitivity provided by SIM  was necessary to meet the drinking
               water monitoring trigger of 0.001 mg/L [40CFR 141.24 (h)(18)] and
               maximum contaminant level (MCL) of 0.003 mg/L [40CFR 141.61 (c)].
               Detailed instructions for the identification and quantitation of toxaphene are
               in Sect. 12.3.3.

       1.7.2    Aroclors - The PCB congeners selected as analytes in this method are
               representative of the major components (by weight percent) of Aroclors
                1016, 1221, 1232,  1242, 1248, 1254, and  1260.4'5 Analyzing for these
               specific congeners allows the analyst to screen samples for possible Aroclor
               contamination without complex pattern recognition protocols.  This method
               is designed for Aroclor screening only and not for qualitative or quantitative
               analyses of specific Aroclors.

       1.7.3    Technical chlordane - Technical chlordane is a multi-component analyte
               regulated under the Safe Drinking Water Act (SDWA) at the time of
               publication of this  method.  It contains at least 140 chlorinated components.
               At the concentrations likely to be encountered in drinking water samples,
               only two or three major components will typically be identified: cis- and

                                      525.3-6

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                   trans-chlordane and trans-nonachlor.  These major components are listed as
                   method analytes along with technical chlordane. Specific instructions for
                   quantification of technical chlordane are provided in Sect.  12.3.1.

    1.8     METHOD FLEXIBILITY - In recognition of technological advances in analytical
           systems and techniques, the laboratory is permitted to modify the GC inlet, inlet
           conditions,  column, injection parameters, and all other GC and MS  conditions.
           Changes may not be made  to sample collection and preservation (Sect. 8), sample
           extraction (Sect. 11) or to the Quality Control (QC) requirements (Sect. 9).  Method
           modifications should be considered only to improve method performance.
           Modifications that are introduced in the interest of reducing cost or  sample
           processing time, but result  in poorer method performance, should not be used.  In all
           cases where method modifications are proposed, the analyst must perform the
           procedures  outlined in the initial demonstration of capability (IDC,  Sect. 9.2), verify
           that all QC  acceptance criteria in this method (Sect. 9) are met, and  that method
           performance in real sample matrices  is equivalent to that demonstrated for
           Laboratory  Fortified Sample Matrices (LFSMs) in Sect. 17.

           Note:  The  above method flexibility section is intended as an abbreviated summation
           of method flexibility.  Sects. 4-12 provide detailed information of specific portions
           of the method that may be modified.  If there is any perceived conflict between the
           general method flexibility statement in Sect. 1.8 and specific information in Sects. 4-
           12, Sects. 4-12 supersede Sect. 1.8.

2.  SUMMARY OF METHOD

    2.1.    A 1-liter water sample is fortified with surrogate analytes and passed through a solid
           phase extraction (SPE) device (Sects. 6.9-6.13) to extract the target  analytes and
           surrogates.  The compounds are eluted from the solid phase with a small amount of
           two or more organic solvents. The solvent extract is dried by passing it through a
           column of anhydrous sodium sulfate, concentrated by evaporation with nitrogen gas,
           and then adjusted to a  1-mL volume with ethyl acetate after adding the internal
           standards. A splitless injection is made into a GC equipped with a high-resolution
           fused silica capillary column that is interfaced to an MS. The analytes are separated
           and identified by comparing the acquired mass spectra and retention times to
           reference spectra and retention times for calibration standards acquired under
           identical GC/MS conditions. The GC/MS may be operated in the full scan, SIM, or
           selected ion storage (SIS) mode (Sects 3.19 and 3.20). The GC/MS may be
           calibrated using standards prepared in solvent or using matrix-matched standards
           (Sects. 3.15 and 7.2.4). The concentration of each analyte is calculated by using its
           integrated peak area and the internal  standard technique. Surrogate analytes are
           added to all Field and Quality Control (QC) Samples to monitor the performance of
           each extraction and overall method performance.

    2.2     Some analytes in this method can be  affected by matrix induced chromatographic
           response enhancement (Sect. 3.14), when analyzed at low concentrations.  Refer to

                                         525.3-7

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           the "comments" section of Table 1 for potentially affected analytes, and to Sect. 13
           for information regarding method performance.

3. DEFINITIONS

   3.1.     ANALYSIS BATCH - A set of samples that is analyzed on the same instrument
           during a 24-hour period that begins and ends with the analysis of the appropriate
           Continuing Calibration Check (CCC) Standards. Additional CCCs may be required
           depending on the length of the analysis batch and/or the number  of Field Samples.

   3.2.     CALIBRATION STANDARD (CAL) - A solution prepared from the primary
           dilution standard solution or stock standard solution(s) and the internal standards and
           surrogate analytes.  The CAL solutions are used to calibrate the instrument response
           with respect to analyte concentration. In this method, traditional CAL standards
           prepared in ethyl acetate may be used or matrix-matched standards (Sect. 3.15)
           prepared in a concentrated laboratory reagent water (LRW) extract may be used.
           This procedure is described in Sect. 7.2.4.2.

   3.3.     CONTINUING CALIBRATION CHECK (CCC) STANDARD - A calibration
           standard containing one or more method analytes, which is analyzed periodically to
           verify the accuracy of the existing calibration for those analytes.

   3.4.     DETECTION LIMIT (DL) - The minimum concentration of an analyte that can be
           identified, measured and reported with 99% confidence that the analyte
           concentration is greater than zero.  This is a statistical determination (Sect. 9.2.6),
           and accurate quantitation is not expected at this level.3

   3.5.     EXTRACTION BATCH - A set of up to 20 Field Samples (not including QC
           samples) extracted together by the same person(s) during a work day using the same
           lot of solid phase extraction devices, solvents, surrogate solution, and fortifying
           solutions.  Required QC samples include Laboratory Reagent Blank, Laboratory
           Fortified Blank, Laboratory Fortified Sample Matrix, and either a Field Duplicate or
           Laboratory Fortified Sample Matrix Duplicate.

   3.6.     FIELD DUPLICATES (FD1 and FD2) - Two separate samples collected at the same
           time and place under identical circumstances, and treated exactly the same
           throughout field and laboratory procedures.  Analyses of FD1 and FD2 provide an
           estimate of the precision associated with sample collection, preservation, and
           storage, as well as with laboratory procedures.

   3.7.     INTERNAL STANDARD (IS) - A pure compound added to an extract or standard
           solution in a known amount and used to measure the relative responses of the
           method analytes and surrogates. In this method, the internal standards are
           isotopically labeled analogues of selected method analytes.
                                         525.3-8

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3.8.    LABORATORY FORTIFIED BLANK (LFB) - An aliquot of reagent water or other
       blank matrix to which known quantities of the method analytes and all the
       preservation compounds are added. The LFB is processed and analyzed exactly like
       a sample, and its purpose is to determine whether the methodology is in control, and
       whether the laboratory is capable of making accurate and precise measurements.

3.9.    LABORATORY FORTIFIED SAMPLE MATRIX (LFSM) - An aliquot of a Field
       Sample to which known quantities of the method analytes and all the preservation
       compounds are added.  The LFSM is processed and analyzed exactly like a sample,
       and its purpose is to determine whether the sample matrix contributes bias to the
       analytical results. The background concentrations of the analytes in the sample
       matrix must be determined in a separate aliquot and the measured values in the
       LFSM corrected for background concentrations.

3.10.   LABORATORY FORTIFIED SAMPLE MATRIX DUPLICATE (LFSMD) - A
       duplicate Field Sample used to prepare the LFSM, which is fortified, extracted and
       analyzed identically to the LFSM. The LFSMD is used instead of the Field
       Duplicate to assess method  precision and accuracy when the occurrence of a method
       analyte is infrequent.

3.11.   LABORATORY REAGENT BLANK (LRB) - An aliquot of reagent water that is
       treated exactly as a sample including exposure to all glassware, equipment, solvents,
       reagents, sample preservatives, internal standards, and surrogates that are used in the
       extraction batch. The LRB is used to determine if method analytes or other
       interferences are present in the laboratory environment, the reagents, or the
       extraction apparatus.

3.12.   LOWEST CONCENTRATION MINIMUM REPORTING LEVEL (LCMRL) - The
       single-laboratory LCMRL is the lowest true concentration for which the future
       recovery is predicted to fall, with high confidence (99 percent), between 50 and 150
       percent recovery.1'2

3.13.   MATERIAL SAFETY DATA SHEET (MSDS) - Written information provided by
       vendors concerning a chemical's toxicity, health hazards, physical properties, fire,
       and reactivity data including storage, spill, and handling precautions.

3.14.   MATRIX-INDUCED CHROMATOGRAPHIC RESPONSE ENHANCEMENT -
       This phenomenon occurs when, in the absence of matrix components, method
       analytes in calibration solutions are degraded or absorbed in the GC injector or
       column, resulting in poor peak shapes and low response. When subsequent sample
       extracts containing the analytes and components from a complex sample matrix are
       injected, peak shape and response improve.  In this situation, quantitative data for
       field samples may exhibit a high bias.6"13 Generally, overestimation of results is
       more pronounced at low analyte concentrations.
                                    525.3-9

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3.15.   MATRIX-MATCHED CALIBRATION STANDARD - A calibration standard that
       is prepared by adding method analytes to a concentrated extract of a matrix (reagent
       water is used for this method) that has been prepared following all the extraction and
       sample preparation steps of the analytical method.  The material extracted from the
       matrix reduces matrix-induced response enhancement effects and improves the
       quantitative accuracy of sample results.12'13

3.16.   MINIMUM REPORTING LEVEL (MRL) - The minimum concentration that can be
       reported by a laboratory as a quantitated value for a method analyte in a sample
       following analysis. This concentration must meet the criteria defined in Sect. 9.2.4
       and must not be any lower than the concentration of the lowest continuing calibration
       check standard for that analyte. The MRL may be determined by the laboratory
       based upon project objectives, or may be set by a regulatory body as part of a
       compliance monitoring program.

3.17.   PRIMARY DILUTION STANDARD SOLUTION  (PDS) - A solution containing
       method analytes, internal standards, or surrogate analytes prepared in the laboratory
       from stock standard solutions and diluted as needed to prepare calibration solutions
       and other analyte solutions.

3.18.   QUALITY CONTROL SAMPLE (QCS) - A solution prepared using a PDS of
       method analytes obtained from a source external to the laboratory and different from
       the source of calibration standards. The second source PDS and the surrogate PDS
       are used to fortify the QCS at a known concentration. The QCS is used to verify the
       accuracy of the primary calibration standards.

3.19.   SELECTED ION MONITORING (SIM) - An MS technique where only one or a
       few ions are monitored for each target analyte.  When used with gas
       chromatography, the set of ions monitored is usually changed periodically
       throughout the chromatographic run, to correlate with the characteristic ions of the
       analytes, SURs and ISs  as they elute from the chromatographic column.  The
       technique is often used to increase sensitivity.  Throughout this document, the term
       "SIM" will be used to include both SIM as described here and SIS as described in
       Sect. 3.20.

3.20.   SELECTED ION STORAGE (SIS) - An MS technique typically used with ion trap
       mass spectrometers where only one or a few ions are stored at any given time point.
       When used with gas chromatography, the set of ions stored is usually changed
       periodically throughout the chromatographic run, to correlate with the characteristic
       ions of the analytes, SURs and ISs  as they elute from the chromatographic column.
       SIS can be used to enhance sensitivity. Throughout this document the term "SIM"
       will be used to include both SIM (Sect. 3.19) and SIS.

3.21.   STOCK STANDARD SOLUTION (SSS) - A concentrated solution containing one
       or more method analytes prepared in the  laboratory using assayed reference materials
       or purchased  from a reputable commercial source.

                                    525.3-10

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   3.22.   SURROGATE ANALYTE (SUR) - A pure analyte, which is extremely unlikely to
           be found in any sample, and which is added to a sample aliquot in a known amount
           before extraction or other processing, and is measured with the same procedures used
           to measure other sample components.  The purpose of the SUR is to monitor method
           performance with each sample.

4.  INTERFERENCES

   4.1.     All glassware must be meticulously cleaned. Wash glassware with detergent and tap
           water, rinse with tap water, followed by reagent water. Rinse with methanol and/or
           acetone. Non-volumetric glassware may be heated in a muffle furnace at 400 °C for
           two hours as a substitute for solvent rinsing.  Volumetric glassware should not be
           heated in an oven above 120 °C.

   4.2.     Method interferences may be caused by contaminants in solvents, reagents
           (including reagent water), sample bottles and caps, and other sample processing
           hardware that lead to discrete artifacts and/or elevated baselines in the chromato-
           grams.  All items such as these must be routinely demonstrated to be free from
           interferences (less than Vs the MRL for each target analyte) under the conditions of
           the analysis by analyzing laboratory reagent blanks as described in Sect. 9.3.1.
           Subtracting blank values from sample results is not permitted.

   4.3.     Matrix interferences may be caused by contaminants that are co-extracted from the
           sample.  The extent of matrix interferences will vary considerably from source to
           source, depending upon the nature of the water.  Water samples high in total organic
           carbon (TOC) may have elevated baselines or interfering peaks.  Matrix components
           may directly interfere by producing a signal at or near the retention time of an
           analyte peak.  They can also enhance the signal of method analytes (Sect. 3.14).
           Analyses of LFSMs are useful in identifying matrix interferences.

   4.4.     Relatively large quantities of the buffer and preservatives  (Sect. 8.1.2) are added to
           sample bottles.  The potential exists for trace-level organic contaminants in these
           reagents. Interferences from these sources should be monitored by analysis of
           laboratory reagent blanks, particularly when new lots of reagents are acquired.

   4.5.     Solid phase extraction media have been observed to be a source of interferences.14
           The analysis of field and laboratory reagent blanks can provide important
           information regarding the presence or absence of such interferences. Brands and lots
           of solid phase extraction devices should be tested to ensure that contamination does
           not preclude analyte identification and quantitation.

           Analyte carryover may occur when a relatively "clean" sample is analyzed
           immediately after a sample (or standard) that contains relatively high concentrations
           of compounds.  Syringes and GC injection port liners must be cleaned carefully or
           replaced as needed. After analysis of a sample (or standard) that contains high
           concentrations of compounds, a laboratory reagent blank should be analyzed to

                                         525.3-11

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           ensure that accurate values are obtained for the next sample. The analyst should be
           especially careful to check for carryover of polycyclic aromatic hydrocarbons
           (PAHs) and PCBs.

   4.7.     Silicone compounds may be leached from punctured autosampler vial septa,
           particularly when particles of the septa sit in the vial. This can occur after repeated
           injections from the  same autosampler vial.  These silicone compounds, which appear
           as regularly spaced chromatographic peaks with similar MS fragmentation patterns,
           can unnecessarily complicate the total ion chromatograms and may cause
           interferences at high levels.

   4.8.     Quantitation of bromacil should be reviewed for potential common interferences.
           The quantitation ion (QI) m/z 205 suggested in Table 1 can be found in SPE media;
           therefore, method blanks should be carefully examined for this potential interference.
           The ion at m/z 207 may be used as an alternate QI; however, this ion is associated
           with column bleed. Laboratories should select the QI depending on the sorbent
           being used and the amount of bleed associated with the GC column. If both types of
           interferences are present, some laboratories may not be able to analyze for bromacil
           at low concentrations.  Manual inspection of all bromacil data reported in field
           samples is mandatory.

   4.9.     There are many potential sources of phthalate  contamination in the laboratory,
           especially from plastics and chemicals that may have been stored in plastic
           containers. If phthalates are to be reported as  method analytes, care must be taken to
           minimize sources of contamination, and the QC criteria for LRBs must be met
           (Sect. 9.3.1).  Special precautions must also be taken when creating calibration
           curves for analytes  consistently found in LRBs (Sect. 10.2.5).

   4.10.   In cases where the SPE disks or cartridges  are dried by pulling room air through the
           media using vacuum, it may be possible for the media to  become contaminated by
           components in room air. This was not observed during method development.  If
           laboratories encounter  contamination problems associated with room air, compressed
           gas cylinders of high purity nitrogen may be used for drying SPE media during
           sample processing.

   4.11.   If samples are to be analyzed for DEET,  sample collection personnel should be
           cautioned against the use of insect repellents containing DEET.

5.  SAFETY

   5.1.     The toxicity or carcinogenicity of each reagent used in this method has not been
           precisely defined.  Each chemical should be treated as a potential health hazard, and
           exposure to these chemicals should be minimized.  Each laboratory is responsible for
           maintaining an awareness  of OSHA regulations regarding safe handling of chemicals
           used in this method. A reference file of MSDSs should be made available to all
                                         525.3-12

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           personnel involved in the chemical analysis. Additional references to laboratory
           safety are available.15"17

   5.2.     Pure standard materials and stock standard solutions of these compounds should be
           handled with suitable protection to skin and eyes, and care should be taken not to
           breathe the vapors or ingest the materials.

6.  EQUIPMENT AND SUPPLIES

   References to specific brands or catalog numbers are included for illustration only, and do
   not imply endorsement of the product. Other brands of equivalent quality may be used. The
   SPE sorbents described in Sects. 6.9-6.11 are proprietary products that have been fully
   evaluated for use in this method by two laboratories. The sorbents described in Sects. 6.12
   and 6.13 are proprietary products with demonstration data provided by the vendor. Due to
   their proprietary status,  some aspects of the chemistry of all of these sorbents are unknown
   making equivalency difficult to determine. The EPA document "Technical Notes on
   Drinking Water Methods"18 provides criteria for judging equivalency of SPE products.
   Before analyses are performed  for compliance under the Safe Drinking Water Act, questions
   regarding equivalency of alternate sorbent materials must be addressed to the Office of
   Ground Water and Drinking Water Alternate Test Procedure Coordinator.19

   6.1.     SAMPLE CONTAINERS - 1 -L or 1 -qt amber glass bottles fitted with
           polytetrafluoroethylene (PTFE)-lined screw caps are preferred.  Clear glass bottles
           with PTFE-lined screw caps may be  substituted if sample bottles are wrapped with
           foil, stored in boxes, or otherwise protected from light during sample shipping and
           storage.

   6.2.     VIALS - Various sizes of amber glass vials with PTFE-lined screw caps for storing
           standard solutions and  extracts.  Amber glass 2-mL autosampler vials with PTFE-
           faced septa.

   6.3.     VOLUMETRIC FLASKS - Class A, suggested sizes include 1, 5, and 10 mL for
           preparation of standards and dilution of extract to final volume.

   6.4.     GRADUATED CYLINDERS -  Suggested sizes include 5, 10, 250 and 1000 mL.

   6.5.     MICRO SYRINGES -  Suggested sizes include 10, 25, 50, 100, 250, 500, and
           1000 |iL.

   6.6.     DRYING COLUMN -  The drying column must be able to contain 10-12 g of
           anhydrous sodium sulfate (Na2SO/t).  The drying column should not leach interfering
           compounds or irreversibly adsorb method  analytes. Any small glass or
           polypropylene column  may be used,  such as Supelco #57176.
                                        525.3-13

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6.7.    COLLECTION TUBES - 15 to 50 mL, conical tubes (Fisher #05-569-6C) or other
       glassware suitable for collection of the eluent from the solid phase after extraction
       and for collecting extract from drying tube.

6.8.    ANALYTICAL BALANCE - Capable of weighing to the nearest 0.0001 g.

6.9.    SPE APPARATUS USING PTFE DISKS; MANUAL EXTRACTION

       6.9.1.   SPE DISKS - 47-mm diameter and 0.5-mm thick, manufactured with a
               styrene divinylbenzene (SDVB) sorbent (Empore SDB-XC, #2240 or
               equivalent).

               Note:  Several brands of SDVB and modified SDVB media in cartridge
               format were evaluated during method development and did not provide
               satisfactory performance. Therefore, SDVB  cartridges are not included in
               this method.

       6.9.2.   SPE DISK EXTRACTION GLASSWARE - glass funnel, PTFE-coated
               support screen, PTFE gasket, base, and clamp used to support SPE disks
               and contain samples during extraction. May be purchased as a set
               (Fisher #K971100-0047, Kontes #971000-6047, or equivalent) or
               separately.

       6.9.3.   VACUUM EXTRACTION MANIFOLD - Designed to accommodate
               extraction glassware and disks (Kontes #971000-6047, or UCT
               #ECUCTVAC6, or equivalent).

       6.9.4.   An automatic or robotic system designed for use with PTFE disks may be
               used if all quality control requirements discussed in Sect. 9 are met.
               Automated systems may use either vacuum or positive pressure to process
               samples and solvents through the disk. All sorbent washing, conditioning.
               sample loading, rinsing, drying and elution steps must be performed as
               closely as possible to the manual procedure.  The solvents used for washing.
               conditioning,  and sample elution must be the same as those used in the
               manual procedure: however, the amount used may be increased as
               necessary to achieve the required data quality. Solvent amounts may not be
               decreased.  Sorbent drying times prior to elution may be modified to
               achieve the required data quality. Caution should be exercised when
               increasing solvent volumes.  Increased extract volume will likely
               necessitate the need for additional sodium sulfate drying, and extended
               evaporation times which may compromise data quality.  Caution should
               also be exercised when modifying sorbent drying times.  Excessive  drying
               may cause losses due to analyte volatility, and excessive contact with room
               air may oxidize some method analytes. Insufficient drying may leave
               excessive water trapped in the disk and lead to poor recoveries.
                                    525.3-14

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6.10.   SPE APPARATUS USING SPEEDISKS; MANUAL EXTRACTION

       6.10.1.  SPEEDISKS - J.T. Baker H2O Phobic Divinylbenzene (DVB) Speedisk,
               regular capacity (part #8068-06).

       6.10.2.  VACUUM EXTRACTION MANIFOLD - J.T. Baker #8095-06

       6.10.3.  An automatic or robotic system designed for use with SPEEDISKS may be
               used if all quality control requirements discussed in Sect. 9 are met.
               Automated systems may use either vacuum or positive pressure to process
               samples and solvents through the disk. All sorbent washing, conditioning,
               sample loading, rinsing, drying and elution steps must be performed as
               closely as possible to the manual procedure.  The solvents used for washing,
               conditioning, and sample elution must be the same as those used in the
               manual procedure: however, the amount used may be increased as
               necessary to achieve the required data quality.  Solvent amounts may not be
               decreased. Sorbent drying times prior to elution may be modified to
               achieve the required data quality.  Caution should be exercised when
               increasing solvent volumes. Increased extract volume will likely
               necessitate the need for additional sodium  sulfate drying, and extended
               evaporation times which may compromise data quality.  Caution should
               also be exercised when modifying sorbent drying times. Excessive drying
               may cause losses due to analyte volatility,  and excessive contact with room
               air may oxidize some method analytes. Insufficient drying may leave
               excessive water trapped in the disk and lead to poor recoveries.

6.11.   SPE APPARATUS USING SPE CARTRIDGES (6-mL COLUMNS); MANUAL
       EXTRACTION

       6.11.1.  SPE CARTRIDGES - Modified DVB polymer (not SDVB polymer-see
               note below).

               Note:  Several brands of SDVB and modified SDVB media in cartridge
               format were evaluated during method development and did not provide
               satisfactory performance.  Therefore, SDVB cartridge products are not
               included in this method.

             6.11.1.1.  Waters Oasis HLB, 500 mg (Waters #186000115) -
                      divinylbenzene N-vinylpyrrolidone copolymer

             6.11.1.2.  J.T.  Baker Speedisk Column H2O Phobic DVB, 200 mg
                      (#8109-09) - divinylbenzene polymer

       6.11.2.  VACUUM EXTRACTION MANIFOLD - Equipped with flow/vacuum
               control (Supelco #57030-U or equivalent).
                                    525.3-15

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       6.11.3.  SAMPLE DELIVERY SYSTEM - Use of a transfer tube system (Supelco
               "Visiprep", #57275 or equivalent), which transfers the sample directly from
               the sample container to the SPE cartridge is recommended.

       6.11.4.  An automatic or robotic system designed for use with SPE cartridges may
               be used if all quality control requirements discussed in Sect. 9 are met.
               Automated systems may use either vacuum or positive pressure to process
               samples and solvents through the cartridge. All sorbent washing,
               conditioning, sample loading, rinsing, drying and elution steps must be
               performed as closely as possible to the manual procedure. The solvents
               used for washing, conditioning, and sample elution must be the same as
               those used in the manual procedure: however, the amount used may be
               increased as necessary to achieve the required data quality. Solvent
               amounts may not be decreased.  Sorbent drying times prior to elution may
               be modified to achieve the required data quality. Caution should be
               exercised when increasing solvent volumes. Increased extract volume will
               likely necessitate the need for additional sodium sulfate drying, and
               extended evaporation times which may compromise data quality.  Caution
               should also be exercised when modifying sorbent drying times. Excessive
               drying may cause losses due to analyte volatility, and excessive contact
               with room air may oxidize some method analytes.  Insufficient drying may
               leave excessive water trapped in the disk and lead to poor recoveries.

6.12.   SPE APPARATUS USING SPE CARTRIDGES (83-mL COLUMNS); MANUAL
       EXTRACTION

       6.12.1.  SPE CARTRIDGES - United Chemical Technologies (UCT) 525 Universal
               cartridge, #ECUNI525, 1500 mg octadecyl unendcapped bonded silica,
               carbon loading 15-18%, surface area approximately 500  m2/g, or
               equivalent.

       6.12.2.  VACUUM EXTRACTION MANIFOLD - Designed to accommodate
               extraction glassware and cartridges (Varian #1214-6001  or
               UCT # ECUCTVAC6 or equivalent).

       6.12.3.  CARTRIDGE ADAPTER - UCT #ECUCTADP

       6.12.4.  BOTTLE HOLDER - UCT #ECUNIBHD

       6.12.5.  An automatic or robotic system designed for use with SPE cartridges may
               be used if all quality control requirements discussed in Sect. 9 are met.
               Automated systems may use either vacuum or positive pressure to process
               samples and solvents through the cartridge. All sorbent washing.
               conditioning, sample loading, rinsing, drying and elution steps must be
               performed as closely as possible to the manual procedure. The solvents
               used for washing, conditioning, and sample elution must be the same as

                                    525.3-16

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               those used in the manual procedure: however, the amount used may be
               increased as necessary to achieve the required data quality. Solvent
               amounts may not be decreased.  Sorbent drying times prior to elution may
               be modified to achieve the required data quality. Caution should be
               exercised when increasing solvent volumes.  Increased extract volume will
               likely necessitate the need for additional sodium sulfate drying, and
               extended evaporation times which may compromise data quality.  Caution
               should also be exercised when modifying sorbent drying times. Excessive
               drying may cause losses due to analyte volatility, and excessive contact
               with room air may oxidize some method analytes.  Insufficient drying may
               leave excessive water trapped in the disk and lead to poor recoveries.

6.13.   SPE APPARATUS USING HORIZON ATLANTIC DVB DISKS  WITH
       AUTOMATED OR MANUAL EXTRACTION

       6.13.1.  SPE DISKS - Horizon Atlantic DVB disk, 50 mm diameter, 4mm thick,
               #47-2346-06, or equivalent

       6.13.2.  DISK HOLDER ASSEMBLY - 50 mm disk holder with extended riser,
               Horizon #50-2629 or equivalent

       6.13.3.  VACUUM EXTRACTION MANIFOLD - Equipped with flow/vacuum
               control (Supelco #57030-U) or equivalent

       6.13.4.  SPE-DEX 4790 Automated Extraction System, Horizon Technology

6.14.   EXTRACT CONCENTRATION SYSTEM - Extracts are concentrated by
       evaporation with nitrogen gas using a water bath set at 40 °C (N-Evap, Model 11155,
       Organomation Associates, Inc., or equivalent).

6.15.   LABORATORY OR ASPIRATOR VACUUM SYSTEM - Sufficient capacity to
       maintain a vacuum of approximately 15 to 25  inches of mercury.

6.16.   GAS CHROMATOGRAPH/MASS SPECTROMETER (GC/MS)  SYSTEM

       6.16.1.  FUSED  SILICA CAPILLARY GC COLUMN - 30 m x 0.25-mm inside
               diameter (i.d.) fused silica capillary column coated with a 0.25 jim bonded
               film of poly(dimethylsiloxy)poly(l,4-bis(dimethylsiloxy)phenylene)-
               siloxane (Restek RXI-5sil-MS or equivalent). Any capillary column that
               provides adequate capacity, resolution, accuracy, and precision may be
               used. A nonpolar, low-bleed column is recommended for use with this
               method to provide adequate resolution and minimize column bleed.

       6.16.2.  GC INJECTOR AND OVEN - Some of the target compounds included in
               this method  are subject to thermal breakdown in the GC injection port. This
               problem is exacerbated when the injector and/or the injection port liner is

                                    525.3-17

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                   not properly deactivated or is operated at excessive temperatures. The
                   injection system must not allow analytes to contact hot stainless steel or
                   other metal surfaces that promote decomposition. The performance data in
                   Sect. 17 were obtained using hot, splitless injection using a 4 or 5-mm i.d.
                   glass deactivated liner. Other injection techniques such as temperature pro-
                   grammed injections, cold on-column injections and large volume injections
                   may be used if the QC criteria in Sect. 9 are met.  Equipment designed
                   appropriately for these alternate types of injections must be used if these
                   options are employed.

           6.16.3.  GC/MS INTERFACE - The interface should allow the capillary column or
                   transfer line exit to be placed within a few millimeters of the ion source.
                   Other interfaces are acceptable as long as the system has adequate
                   sensitivity and QC performance criteria are met.

           6.16.4.  MASS  SPECTROMETER (MS) - Any type of MS may be used (i.e.,
                   quadrupole, ion trap, time of flight, etc.) with electron impact ionization.
                   The instrument may be operated in full scan mode or in SIM mode for
                   enhanced sensitivity.  The minimum scan range capability of the MS must
                   be 45 to 450 m/z, and  it must  produce a full scan mass spectrum that meets
                   all criteria in Table 2 when a solution containing 5 ng (or less) of
                   decafluorotriphenylphosphine (DFTPP) is injected into the GC/MS
                   (Sect. 10.2.1).

           6.16.5.  DATA SYSTEM - An interfaced data system is required to acquire, store,
                   and output MS data. The computer software should have the capability of
                   processing stored GC/MS data by recognizing a GC peak within a given
                   retention time window. The software must allow integration of the ion
                   abundance of any specific ion between specified time or scan number
                   limits.  The software must be able to construct linear regressions and
                   quadratic calibration curves, and calculate analyte concentrations.

7.  REAGENTS AND STANDARDS SUPPLIES (References to specific brands or catalog
   numbers are included for illustration only,  and do not imply endorsement of the product.)

   7.1.     REAGENTS AND SOLVENTS - Reagent grade or better chemicals should be used
           in all tests.  Unless otherwise indicated, it is intended that all reagents will conform
           to the  specifications of the Committee on Analytical Reagents of the American
           Chemical Society (ACS), where such specifications are available.  Other grades may
           be used, if the reagents are demonstrated free of analytes and interferences, and all
           method requirements in the Initial Demonstration of Capability (IDC) are met.

           7.1.1.    HELIUM - 99.999 %  or better, GC carrier gas.
                                        525.3-18

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       7.1.2.   LABORATORY REAGENT WATER (LRW) - Purified water which does
               not contain any measurable quantities of any target analytes or interfering
               compounds at or above Vs the MRL for each compound of interest.

       7.1.3.   METHANOL (MeOH) (CASRN 67-56-1) - High purity, demonstrated to be
               free of analytes and interferences (Fisher Optima or equivalent).

       7.1.4.   ETHYL ACETATE (EtOAc) (CASRN 141-78-6) - High purity,
               demonstrated to be free of analytes and interferences (Tedia Absolv or
               equivalent).

       7.1.5.   DICHLOROMETHANE (DCM) (CASRN 75-09-02) - High purity,
               demonstrated to be free of analytes and interferences (Fisher GC Resolv or
               equivalent).

       7.1.6.   ACETONE (CASRN 67-64-1) - High purity,  demonstrated to be free of
               analytes and interferences (Tedia Absolv or equivalent).

       7.1.7.   SODIUM SULFATE (Na2SO4), ANHYDROUS (CASRN 7757-82-6) -
               Soxhlet extracted with DCM for a minimum of four hours or heated to
               400 °C for two hours in a muffle  furnace. An  "ACS grade, suitable for
               pesticide residue analysis," is recommended.

       7.1.8.   SAMPLE PRESERVATION REAGENTS - The following preservatives
               are solids at room temperature  and may be added to the sample bottle before
               shipment to the field.

             7.1.8.1.   POTASSIUM DIHYDROGEN CITRATE (CASRN 866-83-1) -
                      The sample must be buffered to pH 3.8 to inhibit microbial growth
                      and analyte degradation.20

             7.1.8.2.   L-ASCORBIC ACID  (CASRN 50-81-7) - Ascorbic acid reduces
                      free chlorine at the time of sample collection (ACS Reagent Grade
                      or equivalent).21

             7.1.8.3.   ETHYLENEDIAMINE TETRAACETIC ACID (EDTA),
                      TRISODIUM SALT (CASRN 10378-22-0) - Trisodium EDTA is
                      added to inhibit metal-catalyzed hydrolysis of analytes.20'21

7.2.    STANDARD SOLUTIONS - Standard solutions of internal standards, surrogates
       and method analytes may be prepared gravimetrically or from commercially
       available stock solutions.  When a compound purity is assayed to be 96% or greater,
       the weight can be used without correction to calculate the concentration of a
       gravimetrically prepared stock standard. Solution concentrations listed in this
       section were those used to develop this method and are included as an example only.
       Solution preparation steps may be modified as needed to meet the needs of the

                                   525.3-19

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laboratory.  Often, standard mixes appropriate to the method become commercially
available subsequent to method publication.  Even though stability times for
standard solutions are suggested in the following sections, laboratories should
use standard QC practices to determine when their standards need to be
replaced.  In addition, signs of evaporation and/or discoloration are indicators
that a standard should be replaced.
7.2.1.
7.2.2.
INTERNAL STANDARD (IS) SOLUTIONS - This method uses four IS
compounds listed in the table below. ISs 1-3 are the same as those used in
previous versions of this method and are available individually and as a
mixture from many commercial sources.  A commercial mixture of ISs 1-3
was used for method development, and it is highly recommended that other
analysts use a commercial mix as well. However, if an analyst chooses to
prepare a gravimetric stock solution, it should be prepared in acetone using
a procedure similar to the preparation of analyte stocks as outlined in Sect.
7.2.3.1. The PDS mix for ISs 1-3 has been shown to be stable for at least
one year when stored in amber glass screw cap vials at -5 °C or less. The
PDS for IS  4, 13C-pentachlorophenol, was prepared from neat material  in
methanol at 1000 jig/mL. The neat material was obtained from CDN
Isotopes. This IS PDS has been shown to be stable for at least nine months
when stored in amber glass screw cap vials at -5 °C or less. Using 10 jiL of
the PDS for ISs  1-3 and 4 |iL of the PDS for IS 4 to fortify the final 1-mL
extracts (Sect. 11.9) will yield a concentration of 5 |ig/mL each for ISs 1-3
and 4 |ig/mL of  IS 4 for full scan analysis. Lower concentrations of ISs 1-3
should be used for SIM analysis.  For SIM analysis  during method
development, ISs 1-3 were added to extracts such that their final
concentration was 1 |ig/mL. The IS 4 concentration remained at 4 |ig/mL
for most analyses due to the low abundance of the m/z 276 QI. IS 4 should
be omitted if pentachlorophenol is not being measured as an analyte.

Note:  Stock standard solutions  and PDSs should be brought to room
temperature and sonicated for few minutes prior to use.  This ensures that
components are  dissolved and the solution is homogeneous.
Internal Standards
acenaphthene-t/io (IS 1)
phenanthrene-t/io (IS 2)
chrysene-t/i2 (IS 3)
13C-pentachlorophenol (IS 4)
CASRN
15067-26-2
1517-22-2
1719-03-5
85380-74-1
Solvent
acetone
acetone
acetone
methanol
PDS cone.
500 |ig/mL
500 |ig/mL
500 |ig/mL
1000 |ig/mL
SURROGATE ANALYTE STANDARD SOLUTIONS - The surrogate
analytes used in this method are listed in the table below. All SUR PDSs
were used at the same concentration and were prepared in acetone.  The
                             525.3-20

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        SURs may be prepared or purchased (if available from commercial
        suppliers) as individual PDSs or a single PDS.  The SUR PDSs have been
        shown to be stable for at least one year when stored in amber glass screw
        cap vials at -5 °C or less.  For full scan analysis, 10 jiL of each of these
        solutions was added to each 1L aqueous QC and Field Sample prior to
        extraction, for an expected final extract concentration of 5 jig/L of each
        SUR.  For SIM analyses the QC and Field Samples were  fortified such that
        the expected final extract concentration was 1 |ig/L for each SUR.
Surrogates
l,3-dimethyl-2-nitrobenzene (SUR 1)
triphenyl phosphate (SUR 2)
benzo[a]pyrene-t/i2 (SUR 3)
CASRN
81-20-9
115-86-6
63466-71-7
Solvent
acetone
acetone
acetone
PDS cone.
500 ng/mL
500 ng/mL
500 ng/mL
        Notes:
        •  Stock standard solutions and PDSs should be brought to room
           temperature and sonicated for a few minutes prior to use.  This ensures
           that components are dissolved and the solution is homogeneous.
        •  Stock standard solutions that will be used for aqueous sample
           fortification generally should be prepared at a concentration such that
           only a small volume (e.g., 5-100 jiL) needs to be added to achieve the
           desired final concentration. This will minimize the quantity of organic
           solvent added to aqueous samples.

7.2.3.   ANALYTE STOCK SOLUTIONS

      7.2.3.1.    ANALYTE STOCK STANDARD SOLUTIONS (SSS)
                (0.5-5.0 mg/mL) - Analyte standards may be purchased
                commercially as ampulized solutions prepared from neat materials.
                Commercially prepared SSSs are widely available for most method
                analytes.  Exceptions are DIMP, which at the time of method
                development was available only from Cerilliant, and the 14 PCB
                congeners. During method development, custom PCB mixes were
                obtained from Accustandard  and Chem Service, Inc. Many groups
                of analytes can also be purchased as PDSs, making the preparation
                of individual SSSs unnecessary.  To prepare gravimetric stock
                standard solutions, add 10  mg (weighed on analytical balance to
                0.1 mg) of the pure material to 1.9 mL of solvent in a 2-mL
                volumetric flask, dilute to the mark, and transfer the  solution to an
                amber glass vial.  The suggested solvent for each analyte is
                identical to the PDS solvent listed in the "comments" portion of
                Table 1.  If the neat material  is only available in quantities less
                than 10 mg, reduce the volume of solvent accordingly. If
                compound purity is confirmed by the supplier to be > 96%, the
                             525.3-21

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          weighed amount can be used without correction to calculate the
          concentration of the solution.  Store at 4 °C or less to guard against
          degradation and evaporation.

          Note: Stock standard solutions and PDSs should be brought to
          room temperature and sonicated for a few minutes prior to use.
          This ensures that components are dissolved and the solution is
          homogeneous.
7.2.3.2.    ANALYTE PRIMARY DILUTION STANDARD / ANALYTE
          FORTIFICATION SOLUTION (50 jig/mL for most compounds) -
          Prepare the 50-|ig/mL Analyte PDS by volumetric dilution of the
          Analyte Stock Standard Solutions (Sect. 7.2.3.1) in acetone or
          methanol (see notes below) to make a 50-|ig/mL solution. Analyte
          PDSs containing PCBs, PAHs, and other nonpolar compounds
          must be diluted in acetone rather than methanol. The PDS can be
          used to fortify the LFBs and LFSMs with method analytes and to
          prepare calibration solutions.  Care should be taken during storage
          to prevent evaporation. The Analyte PDS/Analyte Fortification
          Solutions used during method development were stable for
          6 months when prepared in the solvents indicated in the
          "comments" portion of Table  1,  and stored in an amber glass screw
          cap vials at -5 °C or less.

          Notes:
          •  It may be necessary to prepare multiple Analyte PDS mixtures
             based on the laboratory's specific compounds of interest. For
             example, the method was developed using an Analyte PDS  mix
             containing analytes from Method 525.2 in acetone, a PCB PDS
             mix in acetone, a PDS mix containing analytes from EPA's
             Drinking Water Contaminant Candidate List 3 (CCL 3) in
             methanol, and a PDS mix containing the remaining analytes in
             methanol.  The solvent used  for the PDS solution for each
             analyte is listed in the "comments" portion of Table 1.
          •  During method development, PDS solutions contained most
             analytes at the same concentration. However, analytes can be
             combined in PDS solutions at any desired concentrations. It
             may be desirable to include some analytes at increased
             concentrations if they have a relatively low instrument
             response compared with other analytes. For example, during
             method development, pentachlorophenol was added to PDS
             solutions at four times the concentration of most other analytes.
          •  Standard solutions that will be used for aqueous sample
             fortification generally should be prepared at a concentration
             such that only a small volume (e.g., 5-100 jiL) needs to be

                       525.3-22

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                   added to achieve the desired final concentration.  This will
                   minimize the quantity of organic solvent added to aqueous
                   samples.
                •  Stock standard solutions and PDSs should be brought to room
                   temperature and sonicated for a few minutes prior to use.  This
                   ensures that components are dissolved and the solution is
                   homogeneous.

7.2.4.   CALIBRATION SOLUTIONS - Calibration standards may be prepared in
        EtOAc or as matrix-matched calibration standards (Sect. 3.15).  This option
        is provided so that the analyst has the flexibility to prepare calibration
        curves that will be appropriate for the various types of analytes and the
        calibration range of interest. If the analyses to be performed include only
        those analytes that are not susceptible to matrix induced response
        enhancement, and/or the concentrations to be measured are relatively high
        (e.g., > 5|ig/L), it is likely that accurate data can be obtained with the use of
        traditional CAL standards prepared in EtOAc.  If low concentrations of
        analytes susceptible to matrix induced response enhancement need to be
        measured, it is likely that matrix-matched standards will be required to
        obtain accurate quantitative data. Whichever type of CAL solutions are
        selected, those CAL solutions should be used for all calibration and QC
        procedures described in the method.

        Note: Analytes observed to be susceptible to matrix induced response
        enhancement during method development are indicated in the "comments"
        portion of Table  1. However, the occurrence and degree of enhancement
        will depend upon the GC injector design, and the history of the injector,
        injector liner and GC column.  It is highly recommended that prior to the
        initial demonstration of capability, separate calibration curves be generated
        using EtOAc CALs and matrix-matched CALs for each analyte to be
        measured. A careful evaluation of the relative peak areas using each type of
        CAL, especially low concentration CALs, can serve as a guide to the
        possible occurrence and extent of matrix enhancement, and thus an
        indicator of which type of standards should be used.

        Note: Technical toxaphene CAL standards must be prepared so that they
        contain only technical toxaphene and ISs and SURs.  Do not mix technical
        toxaphene with other analytes.

      7.2.4.1.   CALIBRATION SOLUTIONS PREPARED IN SOLVENT -
                Prepare a series of six concentrations of calibration solutions  in
                EtOAc,  which contain the analytes of interest. The suggested
                concentrations in this paragraph are a description of the
                concentrations used during method development, and may be
                modified to conform with instrument sensitivity.  For full scan
                analyses, concentrations ranging from 0.10-5.0 ng/uL are

                              525.3-23

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                           suggested for each analyte, with IS and SUR concentrations as
                           described in Sect. 7.2.1 and 7.2.2. For SIM analysis, six
                           concentrations in the range of 0.005-0.5 ng/uL are suggested, with
                           reduced concentrations of the ISs and  SURs (Sect. 7.2.1 and 7.2.2).
                           The six CAL standards (CAL1 through CAL6) are prepared by
                           combining appropriate aliquots of the  Analyte PDS  solution (Sect.
                           7.2.3.2) and the IS and SURPDSs (Sects. 7.2.1. and 7.2.2). All
                           calibration solutions should contain at least 60% EtOAc to avoid
                           gas chromatographic anomalies such as poor peak shape,  split
                           peaks, etc. During method development, all analytes were
                           prepared in a single set of calibration solutions. However, multiple
                           sets of calibration standards may be prepared at the discretion of
                           the analyst if more separation of the analytes is desired.
                           Calibration solutions were stable for six months when stored at
                           -5 °C in amber screw top vials.

                 7.2.4.2.    MATRIX-MATCHED CALIBRATION SOLUTIONS - Prepare a
                           series of six calibration solutions in the same manner as in Sect.
                           7.2.4.1, but instead of preparation in EtOAc, calibration solutions
                           are prepared in final solvent extracts derived from laboratory
                           reagent water. One-liter aliquots of reagent water with sample
                           preservatives added, are extracted using the sorbent selected for
                           sample analysis, dried with sodium sulfate, and evaporated to <1
                           mL following the same procedure used for samples (Sects. 11.3-
                           119)  However, the ISs, SURs, and  analyte PDSs are added to
                           the extract at appropriate concentrations immediately before
                           the adjustment of the extract to 1 mL, i.e., they are not
                           extracted.

           7.2.5.    GC/MS TUNE CHECK SOLUTION (5  |ig/mL or less)
                   (CASRN 5074-71-5) - Prepare  a DFTPP solution in DCM. DFTPP is more
                   stable in DCM than in acetone or EtOAc. Store this solution in an amber
                   glass screw cap vial at 4 °C or less.

           7.2.6.    4,4'-DDT BREAKDOWN CHECK SOLUTION (5ng/|iL in EtOAc) -
                   Prepare a solution of 4,4'-DDT in EtOAc. Store this solution in an amber
                   glass screw cap vial at 4 °C or less.  The solution is  used for the DDT
                   breakdown check described in Sect. 10.2.2.

8.  SAMPLE COLLECTION. PRESERVATION. AND STORAGE

   8.1.     SAMPLE BOTTLE PREPARATION

      8.1.1.  Grab samples must be collected using 1 -liter or 1 -quart sample bottles that meet
             the requirements in Sect. 6.1.
                                        525.3-24

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          Note: Larger samples must not be collected. The performance of this method has
          not been verified with sample volumes greater than 1L. Samples larger than 1L
          may not be portioned or split because some analytes may adhere to the glass
          surface. These analytes are recovered in the SPE procedural steps that solvent
          rinse the sample bottle and include that rinsate in the extract. If only a partial
          sample were to be analyzed, the resulting data would be biased high if the bottle
          rinsate were added to the extract, and biased low if it was not.

     . 1.2.  Preservation reagents, listed in the table below, are added to each sample bottle  as
          dry solids prior to shipment to the field (or prior to sample collection).
Compound
L-Ascorbic acid
Ethylenediaminetetraacetic acid, trisodium
salt
Potassium dihydrogen citrate
Amount
O.lOg/L
0.35 g/L
9.4 g/L
Purpose
Dechlorination
Inhibit metal -catalyzed
hydrolysis of targets
pH 3. 8 buffer,
microbial inhibitor
       8.1.2.1.  Residual chlorine must be reduced at the time of sample collection with
                                              01
                100 mg of ascorbic acid per liter.

       8.1.2.2.  Trisodium EDTA must be added to inhibit metal-catalyzed hydrolysis of
               method analytes, principally, chlorpyrifos, parathion, vinclozolin, atrazine,
               and propazine.20"22  There may be additional method analytes that also
               benefit from addition of EDTA.

       8.1.2.3.  The sample must be buffered to pH 3.8 using potassium dihydrogen citrate.
               This is added to inhibit microbial degradation of analytes, and to reduce
               base catalyzed hydrolysis of some of the method analytes.20

8.2.       SAMPLE COLLECTION

       8.2.1.   Open the tap and allow the system to flush until the water temperature has
               stabilized (usually 3-5 min). Collect samples from the flowing system.

       8.2.2.   Fill sample bottles, taking care not to flush out the sample preservation
               reagents.  Samples do not need to be collected headspace free.

       8.2.3.   After collecting the sample, cap the bottle and agitate by hand until
               preservatives are dissolved.  Immediately place in ice or refrigerate.

8.3.    SHIPMENT AND STORAGE - Samples must be chilled during shipment and must
       not exceed 10 °C during the first 48 hours after collection. Sample temperature must
       be confirmed to be at or below 10 °C when they are received at the laboratory, with
                                     525.3-25

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           the following exception.  Samples arriving at the laboratory on the day of sampling
           may not have had time to achieve a temperature of less than 10 °C.  This is
           acceptable as long as the cooling process has begun.  Samples stored in the lab must
           be held at or below 6 °C until extraction, but should not be frozen. Sample holding
           time data are discussed in Sect. 13.4.

           Note: Samples that are significantly above 10 °C at the time of collection,  may need
           to be iced or refrigerated for a period of time, in order to chill them prior to shipping.
           This will allow them to be shipped with sufficient ice to meet the above
           requirements.

   8.4.     SAMPLE AND EXTRACT HOLDING TIMES - Water samples should be extracted
           as soon as possible after collection but must be extracted within  14 days of
           collection.  Exceptions to the 14 day sample holding time are samples being
           analyzed for dichlorvos and/or cyanazine which must be extracted within 7 days. All
           extracts must be stored at -5 °C or less, protected from light and analyzed within 28
           days after extraction (Sect.  13.5).

9.   QUALITY CONTROL

   9.1.     QC requirements include the Initial Demonstration of Capability (IDC) and ongoing
           QC requirements that must be met when preparing and analyzing Field Samples.
           This section  describes QC parameters, their required frequency,  and the  performance
           criteria that must be met in order to meet EPA quality objectives. The QC criteria
           discussed in the following sections are summarized in Tables 24 and 25. These QC
           requirements are considered the minimum acceptable QC criteria.  Laboratories are
           encouraged to institute additional QC practices to meet their specific needs.

           Note: If toxaphene is being measured by this method in addition to other analytes,
           all QC steps  described in Sect. 9 must be performed for toxaphene in fortified
           samples that are prepared and analyzed separately from other analytes. The
           frequency of each  QC requirement and the acceptance criteria for toxaphene  are the
           same as the general criteria for other analytes.  Measured values for technical
           toxaphene to meet QC criteria should be obtained as described in Sect. 12.3.3.

   9.2.     INITIAL DEMONSTRATION OF CAPABILITY - The IDC must be successfully
           performed prior to analyzing any Field Samples.  Prior to conducting the IDC, the
           analyst must first generate an acceptable Initial Calibration following the procedure
           outlined in Sect. 10.2.  The IDC must be repeated if the laboratory changes the
           type or brand of SPE sorbent being used.

           9.2.1.    INITIAL DEMONSTRATION OF LOW SYSTEM BACKGROUND -
                   Any time a new lot of SPE cartridges or disks is used, it must be
                   demonstrated that a Laboratory Reagent Blank is reasonably free  of
                   contamination and that the criteria in Sect. 9.3.1 are met.
                                        525.3-26

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9.2.2.   INITIAL DEMONSTRATION OF PRECISION (IDP) - Prepare, extract,
        and analyze four to seven replicate LFBs fortified near the midrange of the
        initial calibration curve according to the procedure described in Sect. 11.
        Sample preservatives as described in Sect. 8.1.2 must be added to these
        samples.  The relative standard deviation (RSD) of the results of the
        replicate analyses must be < 20%.

9.2.3.   INITIAL DEMONSTRATION OF ACCURACY - Using the same set of
        replicate data generated for Sect. 9.2.2, calculate average recovery. The
        average recovery expressed as the mean of the replicate values must be
        within 70-130 % of the true value for all analytes except dimethipin,
        HCCPD and HCB which may be within 60-130% of the true value.

9.2.4.   MINIMUM REPORTING LEVEL (MRL) CONFIRMATION - Establish a
        target concentration for the MRL based on the intended use of the method.
        The MRL may be established by a laboratory for their specific purpose or
        may be set by a regulatory agency. Establish an Initial Calibration
        following the procedure outlined in Sect. 10.2. The lowest calibration
        standard used to establish the Initial Calibration (as well as the low-level
        Continuing Calibration Check standard) must be at or below the
        concentration of the MRL. Establishing the MRL concentration too low
        may cause repeated failure of ongoing QC requirements. Confirm the MRL
        following the procedure outlined below.

        Note:  Setting an MRL for method analytes that are consistently present in
        the background (e.g., phthalates) is particularly important so that false
        positive data are not reported for Field Samples. See Sect. 9.3.1 for
        guidance in setting an MRL for these analytes.

      9.2.4.1.    Fortify, extract, and analyze seven replicate Laboratory Fortified
                Blanks (LFBs) at the proposed MRL concentration.  These LFBs
                must contain all method preservatives described in Sect. 8.1.2.
                Calculate the mean and standard deviation for these replicates.
                Determine the Half Range for the Prediction Interval of Results
                (HRpiR) using the equation below

                                HRpm  =3.9638

                where:

                S = the standard  deviation, and 3.963 is a constant value for seven
                replicates.1

      9.2.4.2.    Confirm that the upper and lower limits for the Prediction Interval
                of Result (PIR = Mean + HR.PIR) meet the upper and lower
                recovery limits as shown below:

                              525.3-27

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                      The Upper PIR Limit must be <150 percent recovery.

                             Mean + HRnrD
                                              -xlOO%<150%
                         Fortified Concentrat ion


                      The Lower PIR Limit must be > 50 percent recovery.


                             Mean~HR^	x looo/o > 500/c
                         FortifiedConcentrat ion

      9.2 A3.   The MRL is validated if both the Upper and Lower PIR Limits
                meet the criteria described above (Sect. 9.2.4.2).  If these criteria
                are not met, the MRL has been set too low by the laboratory and
                must be demonstrated again at a higher concentration.  If a
                required MRL set by a regulatory body has not been met, the
                analyst should evaluate possible problems in the execution of the
                extraction steps, and/or possible problems with instrument
                sensitivity. Reattempt MRL validation at the required MRL after
                problems have been addressed.

      9.2 A A.   Confirmation of the MRL Using Fortified Matrix Samples
                (optional)- This validation procedure may  be used in addition to
                the reagent water confirmation described above.  It may be useful
                in assessing any matrix induced quantitative bias at the MRL.

                Obtain replicate 1 L aliquots of a water sample similar in nature to
                the ones planned for analysis. If tap waters from both ground and
                surface water sources are to be analyzed, it  is recommended that a
                surface water sample be selected for verification. Analyze one
                aliquot using the procedures in this method to verify the absence of
                analytes of interest.  Fortify seven remaining aliquots with the
                analytes to be measured near the expected MRL, and verify the
                MRL as described in Sects. 9.2.4.1 through 9.2.4.3.

9.2.5.   CALIBRATION CONFIRMATION - Analyze a Quality Control Sample as
        described in Sect. 9.3.9 to confirm the accuracy of the standards/calibration
        curve.

9.2.6.   DETECTION LIMIT DETERMINATION (optional) - While DL
        determination is not a specific requirement  of this method, it may be
        required by various regulatory bodies associated with compliance
        monitoring. It is the responsibility of the laboratory to determine ifDL
        determination is required based upon the intended use of the data.
                              525.3-28

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               Replicate analyses for this procedure should be done over at least three days
               (both the sample extraction and the GC analyses should be done over at
               least three days).  Prepare at least seven replicate LFBs at a concentration
               estimated to be near the DL. This concentration may be estimated by
               selecting a concentration at 2-5 times the noise level. The DLs in Tables 15
               and 23 were calculated from LFBs fortified at various concentrations as
               indicated in the table. The appropriate fortification concentrations will be
               dependent upon the sensitivity of the GC/MS system used.  All preservation
               reagents listed in Sect.  8.1.2 must also be added to these samples.  Analyze
               the seven (or more) replicates through all steps of Sects. 1 1  and 12.

               Note: If an MRL confirmation data set meets these requirements, a DL may
               be calculated from the MRL confirmation data, and no  additional analyses
               are necessary.

               Calculate the DL using the following equation:
                              = sxt(n-l,l-a=0.99)
               where:
                  t (n-i, i-a=o.99) = Student's t value for the 99% confidence level with n-1
                  degrees of freedom
                  n = number of replicates
                  s = standard deviation of replicate analyses.

               Note: Do not subtract blank values when performing DL calculations.

9.3 .    ONGOING QC REQUIREMENTS - This section summarizes the ongoing QC
       criteria that must be followed when processing and analyzing Field Samples.

       9.3.1.   LABORATORY REAGENT BLANK (LRB) - An LRB is required with
               each extraction batchto confirm that potential background contaminants are
               not interfering with the identification or quantitation of target analytes. If
               the LRB produces a peak within the retention time window of any analyte
               that would prevent the determination of that analyte,  locate the source of
               contamination and eliminate the interference before processing samples.
               Background contamination must be reduced to an acceptable level before
               proceeding. Background from method analytes or other contaminants that
               interfere with the measurement of method analytes must be at or below l/j
               of the MRL. Blank contamination may be estimated by extrapolation, if the
               concentration is below the lowest calibration standard. Although this
               procedure is not allowed for sample results as it may not meet data quality
               objectives, it can be useful in estimating background  concentrations. If any
               of the method analytes are detected in the LRB at concentrations greater

                                     525.3-29

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        than Vs of the MRL, then all data for the problem analyte(s) must be
        considered invalid for all samples in the extraction batch.

        Note: It is extremely important to evaluate background values of analytes
        that commonly occur in LRBs.  The MRL must be set at a value greater
        than three times the mean concentration observed in replicate LRBs.  If
        LRB values are highly variable, setting the MRL to a value greater than the
        mean LRB concentration plus three times the standard deviation may
        provide  a more realistic MRL.

9.3.2.   CONTINUING CALIBRATION CHECK (CCC) - CCC Standards are
        analyzed at the beginning of each analysis batch, after every ten Field
        Samples, and at the end of the analysis batch. See Sect. 10.3 for
        concentration requirements and acceptance criteria.

9.3.3.   LABORATORY FORTIFIED BLANK (LFB) - An LFB is required with
        each extraction batch. The fortified concentration of the LFB must be
        rotated between low, medium, and high concentrations from batch  to batch.
        The low concentration LFB must be as near as practical to, but no more
        than two times the MRL. Similarly, the high concentration LFB should be
        near the high end of the calibration range established during the initial cal-
        ibration  (Sect. 10.2). Results of the low-level LFB analyses must be
        50-150% of the true value.  Results of the medium and high-level LFB
        analyses must be 70-130%  of the true value for all analytes except
        dimethipin, HCCPD and HCB, which may be between 60-130% of the true
        value. If the LFB results do not meet these criteria for target analytes, then
        all data for the problem  analyte(s) must be considered invalid for all sam-
        ples in the extraction batch.

9.3.4.   MS TUNE CHECK - A complete description of the MS Tune  Check is
        found in Sect. 10.2.1. The acceptance criteria for the MS Tune Check are
        summarized  in Table 2.  The MS Tune Check must be performed each time
        a major  change is made to the mass spectrometer, and prior to  establishing
        and/or re-establishing an initial calibration (Sect. 10.2). Daily DFTPP
        analysis is not required.

        Note: The tune check is performed in full scan mode, even if samples will
        be analyzed in SIM mode.

9.3.5.   INTERNAL STANDARDS (IS) - The analyst must monitor the peak areas
        of the ISs in  all injections during each analysis day.  The peak area for each
        IS in any chromatographic run must not deviate by more than ±50% from
        the mean response in the CAL solutions analyzed for the initial analyte
        calibration.  In addition, the peak areas of ISs 1-3 must not deviate by more
        than ± 30% from the most recent CCC.  IS 4, 13C-pentachlorophenol, is
        expected to have greater area count variability, and therefore is not subject

                              525.3-30

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        to the most recent CCC criterion.  If the IS areas in a chromatographic run
        do not meet these criteria, inject a second aliquot of that standard or extract.

      9.3.5.1.    If the reinjected aliquot produces acceptable internal standard
                 responses, report results for that aliquot.

      9.3.5.2.    If the reinjected aliquot is a sample extract and fails again, the
                 analyst should check the calibration by evaluating the CCCs within
                 the analysis batch.  If the CCCs are acceptable, extraction of the
                 sample may need to be repeated provided the sample is still
                 available and within the holding time.  Otherwise, report results
                 obtained from the reinjected extract, but annotate as suspect.
                 Alternatively, collect a new sample and reanalyze.

      9.3.5.3.    If the reinjected aliquot is a CAL standard, take remedial action
                 (Sect.  10.3.3).

9.3.6.   SURROGATE RECOVERY - Surrogate standards are fortified into the
        aqueous portion of all samples,  LRBs, CCCs, LFSMs, and LFSMDs prior to
        extraction. They are also added to the calibration standards.  The surrogates
        are a means of assessing  method performance from extraction to final
        chromatographic measurement. Calculate the recovery (%R) for each
        surrogate using the equation

                            ( A\
                      %R =  —  xlOO
                            UJ

        where:

        A  = calculated surrogate concentration for the QC or Field Sample, and
        B  = fortified concentration of the surrogate.

      9.3.6.1.    Surrogate recovery must be with 70-130% of the true value.  When
                 surrogate recovery from a sample,  blank, or CCC is less than 70%
                 or greater than 130%, check 1) calculations to locate possible
                 errors, 2) the integrity of the surrogate analyte solution, 3)
                 contamination, and 4) instrument calibration.  Correct the problem
                 and reanalyze the extract.

      9.3.6.2.    If the extract reanalysis meets the surrogate recovery criterion,
                 report only data for the reanalyzed extract.

      9.3.6.3.    If the extract reanalysis fails the 70-130% recovery criterion, the
                 analyst should check the calibration by evaluating the CCCs within
                 the analysis batch.  If the CCCs fail the criteria of Sect. 9.3.6.1,
                 recalibration is in order per Sect. 10.2. If the calibration standard is

                              525.3-31

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                      acceptable, extraction of the sample should be repeated provided
                      the sample is still available and within the holding time. If the re-
                      extracted sample also fails the recovery criterion, report all data for
                      that sample as suspect/surrogate recovery to inform the data user
                      that the results are suspect due to surrogate recovery.

9.3.7.   LABORATORY FORTIFIED SAMPLE MATRIX (LFSM) -  Within each
        analysis batch, analyze a minimum of one LFSM. The native concentrations of
        the analytes in the sample matrix must be determined in a second duplicate
        sample and subtracted from the measured values in the LFSM. If a variety of
        different sample matrices are analyzed regularly, for example, drinking water
        from ground water and surface water sources, performance data must be collected
        for each source.

            9.3.7.1.    Prepare the LFSM by fortifying a Field Duplicate with an
                      appropriate amount of analyte PDS (Sect. 7.2.3.2).  Select a
                      fortification concentration that is greater than or equal to the matrix
                      background concentration, if known.  Selecting a duplicate sample
                      that has already been analyzed aids in the selection of an
                      appropriate fortification concentration. If this is not possible, use
                      historical data.  If historical data are unavailable, rotate the
                      fortifying concentrations for LFSMs between low, medium and
                      high concentrations based on the calibration range.

            9.3.7.2.    Calculate the percent recovery (%R) for each analyte using the
                      equation
                                            C
                      where:

                      A = measured concentration in the fortified sample
                      B = measured concentration in the unfortified sample
                      C = fortification concentration.

                      Note: LFSMs and LFSMDs fortified at concentrations near the
                      MRL, where the associated Field Sample contains native analyte
                      concentrations above the DL but below the MRL, should be
                      corrected for the native levels in order the obtain meaningful %R
                      values. This example, and the LRB extrapolation (Sect. 9.3.1), are
                      the only permitted uses of analyte results below the MRL.

            9.3.7.3.    Analyte recoveries may exhibit matrix bias. For samples fortified
                      at or above their native concentration, recoveries should be within
                      70-130% (60-130% for dimethipin, HCCPD and HCB), except for

                                    525.3-32

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                low-level fortification near or at the MRL (within a factor of two
                times the MRL concentration) where 50-150% recoveries are
                acceptable. If the accuracy of any analyte falls outside the
                designated range, and the laboratory performance for that analyte
                is shown to be in control in the CCCs, the recovery is judged to be
                matrix biased.  The quantitative result for that analyte in the
                unfortified sample is labeled "suspect/matrix" to inform the data
                user that the quantitative results may be suspect due to matrix
                effects.

9.3.8.   FIELD DUPLICATE OR LABORATORY FORTIFIED SAMPLE
        MATRIX DUPLICATE (FD or LFSMD) - Within each extraction batch,
        analyze a minimum of one Field Duplicate (FD) or Laboratory Fortified
        Sample Matrix Duplicate (LFSMD). Duplicates check the precision
        associated with sample collection, preservation, storage, and laboratory
        procedures.  If target analytes are not routinely observed in Field Samples,
        an LFSMD should be analyzed rather than an FD.

      9.3.8.1.    Calculate the relative percent difference (RPD) for duplicate
                measurements (FD1 and FD2) using the equation

                                  FD1-FD2
                         RPD =
      9.3.8.2.    RPDs for Field Duplicates should be < 30 %. Greater variability
                may be observed when Field Duplicates have analyte
                concentrations that are within two times the MRL. At these
                concentrations, Field Duplicates should have RPDs that are < 50%.
                If the RPD of any analyte falls outside the designated range, and
                the laboratory performance for that analyte is shown to be in
                control in the CCC, the recovery is judged to be affected by the
                matrix. The result for that analyte in the unfortified sample is
                labeled "suspect/matrix" to inform the data user that the
                quantitative results may be  suspect due to matrix effects.

      9.3.8.3.    If an LFSMD is analyzed instead of a Field Duplicate, calculate the
                relative percent difference (RPD) for duplicate LFSMs (LFSM and
                LFSMD) using the equation

                                    \LFSM -LFSMDl
                                  - -
                                  - -
                                   IFSM + LFSMD J2

      9.3.8.4.    RPDs for duplicate LFSMs should be < 30% for samples fortified
                at or above their native concentration.  Greater variability may be
                observed when LFSMs are fortified at analyte concentrations that

                             525.3-33

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                        are within two times the MRL. LFSMs fortified at these
                        concentrations should have RPDs that are < 50% for samples
                        fortified at or above their native concentration.  If the RPD of any
                        analyte falls outside the designated range, and the laboratory
                        performance for that analyte is shown to be in control in the CCC,
                        the recovery is judged to be affected by the matrix.  The result for
                        that analyte in the unfortified sample is  labeled  suspect/matrix to
                        inform the data user that the quantitative results may be suspect
                        due to matrix effects.

       9.3.9.   QUALITY CONTROL SAMPLES (QCS) - As part of the IDC (Sect. 9.2),
               each time a new Analyte PDS (Sect. 7.2.3.2) is prepared, or at least
               quarterly, analyze a QCS sample from a source different from the source of
               the calibration standards. If a second vendor is not available then a different
               lot of the standard should be used. The QCS should be prepared and
               analyzed just like a CCC. Acceptance criteria for the QCS are identical to
               the CCCs; the calculated amount for each analyte must be ± 30% of the
               expected value.  If measured analyte concentrations are not of acceptable
               accuracy, check the entire analytical procedure to locate and correct the
               problem. If the discrepancy is not resolved, one  of the standard  materials
               may be degraded or otherwise compromised and a third standard must be
               obtained.

9.4.    METHOD MODIFICATION QC REQUIREMENTS - The analyst is permitted to
       modify GC columns, GC conditions, GC injection techniques, extract evaporation
       techniques, MS conditions and QIs.  However, each time  such method modifications
       are made, the analyst must repeat the procedures of the IDC (Sect. 9.2).

       9.4.1.   Each time method modifications are made, the analyst must repeat the
               procedures of the IDC (Sect. 9.2) and verify that all QC criteria can be met
               in ongoing QC samples (Sect. 9.3).

       9.4.2.   Each time method modifications are made, the analyst is also required to
               evaluate and document method performance for the proposed method
               modifications in real matrices that span the range of waters that the
               laboratory analyzes.  This additional step is required because modifications
               that perform acceptably in the IDC, which is conducted in reagent water,
               can fail ongoing method QC requirements in real matrices.  This is
               particularly important for methods subject to matrix effects.  If, for
               example, the laboratory analyzes finished waters from both  surface and
               groundwater municipalities, this requirement can be accomplished by
               assessing precision and accuracy (Sects. 9.2.2 and 9.2.3) in an analyte
               fortified surface water with moderate to high TOC (e.g., 2 mg/L or greater)
               and an analyte fortified hard groundwater (e.g., 250 mg/L or greater as
               calcium carbonate).
                                     525.3-34

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           9.4.3.    The results of Sects. 9.4.1 and 9.4.2 must be appropriately documented by
                   the analyst and should be independently assessed by the laboratory's
                   Quality Assurance (QA) officer prior to analyzing Field Samples. When
                   implementing method modifications, it is the responsibility of the
                   laboratory to closely review the results of ongoing QC, and in particular, the
                   results associated with the LFSMs (Sect. 9.3.7), FDs or LFSMDs
                   (Sect. 9.3.8), CCCs (Sect. 9.3.2), and the IS area counts (Sect. 9.3.5). If
                   repeated failures are noted, the modification must be abandoned.

10. CALIBRATION AND STANDARDIZATION

   10.1.    Demonstration and documentation of acceptable mass spectrometer tune and initial
           calibration is required before performing the IDC and prior to analyzing Field
           Samples. The MS tune check and initial calibration must be repeated each time a
           major instrument modification is made,  or maintenance is performed.

   10.2.    INITIAL CALIBRATION

           10.2.1.   MS TUNE/MS TUNE CHECK - Calibrate the mass and abundance scales
                   of the MS with calibration compounds and procedures prescribed by the
                   manufacturer with any modifications necessary to meet tuning
                   requirements. Inject 5 ng or less of the DFTPP solution (Sect. 7.2.5) into
                   the GC/MS system. Acquire a mass spectrum that includes data for m/z 45
                   to 450.  The scan time should be set so that a minimum of five scans are
                   acquired during the elution of the chromatographic peak.  Seven to ten
                   scans per chromatographic peak are recommended.  Use a single spectrum
                   at the apex of the DFTPP peak, an average spectrum of the three highest
                   points of the peak, or an average spectrum across the entire peak to evaluate
                   the performance of the system. If the DFTPP mass spectrum does not meet
                   all criteria in Table 2, the MS must be retuned and adjusted to meet all
                   criteria before proceeding with the initial calibration. The tune check
                   should be conducted as described above for both full scan and SIM MS
                   operation.

           10.2.2.   DDT BREAKDOWN CHECK -

                   Note:  This procedure is only required if the DDT degradation products
                   DDD and DDE are being reported.  The DFTTP tune check and the DDT
                   degradation check may be performed simultaneously with a single injection
                   of a standard containing both analytes.

                   4,4'-DDT is subject to thermal  degradation in the GC. Because the thermal
                   degradation products 4,4'-DDE and 4,4'-DDD are also environmental
                   contaminants and method analytes, it is important to determine their source
                   if they are observed in sample chromatograms.  Inject a standard of 4,4'-
                   DDT at a concentration near 5  ng/jiL, and acquire data in the full scan mode

                                        525.3-35

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        using instrument conditions similar to those in Sect. 10.2.3.  Evaluate the
        chromatogram for the presence of 4,4'-DDE and 4,4'-DDD using the
        retention times and ions listed in Table 1 as a guide. If either 4,4'-DDE or
        4,4'-DDD are observed, calculate the percentage breakdown of 4,4'-DDT
        using peak areas from the Total Ion Current (TIC) with the following
        equation:

        % DDT breakdown =

        X TIC area of DDT degradation peaks (DDE+DDD)  X 100
        X TIC area of total DDT peaks (DDT+DDE+DDD)

        If the degradation of 4,4'-DDT exceeds 20%,  perform  maintenance on the
        GC injection port and possibly other areas of the GC prior to proceeding
        with the calibration.  If GC maintenance does not correct the problem, a
        new 4,4'-DDT standard should be obtained from a different source to ensure
        that the standard material has not degraded.

10.2.3.  INSTRUMENT CONDITIONS - Operating conditions used during method
        development are described below. Conditions different from those
        described may be used if QC criteria in Sect.  9 are met. Different
        conditions include alternate GC columns, temperature  programs, MS
        conditions, and injection techniques and volumes, such as cold on-column
        and large volume injections.  Equipment specifically designed for alternate
        types of injections must be used if these alternate options are selected.

      10.2.3.1.   GC Conditions - Inject a l-|iL aliquot into a hot, splitless injection
                port held at 275 °C with a pressure pulse of 30 psi and a split delay
                of 1 min. The temperature program is as follows: initial oven
                temperature of 70 °C, hold for 1.5 min, ramp  at 10 °C/min to 200
                °C, ramp at seven °C/min to a final temperature of 320 °C and hold
                for 3 min.  The GC was operated at a constant flow rate of
                1.2 mL/min. Total run time is approximately 32 min. Begin data
                acquisition at about seven min.

      10.2.3.2.   Full Scan MS Acquistion Parameters - Select a scan range that
                allows the acquisition of a mass spectrum for each of the method
                analytes, which includes all of the major fragments m/z 45 and
                above.  Adjust the cycle time to measure at least five spectra
                during the elution of each GC peak.  Seven to ten scans across each
                GC peak are recommended. The chromatogram may be divided
                into time windows, also known as segments or periods, with
                different scan ranges for each time window. Minimizing the scan
                range for each time window may enhance sensitivity. If the
                chromatogram is divided into time windows,  the laboratory must
                ensure that each method analyte elutes entirely within the proper

                             525.3-36

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          window during each analysis.  This can be achieved by carefully
          monitoring the retention times of all ISs and SURs in each sample,
          and carefully monitoring the retention times of all method analytes
          in CCCs, LFBs and LFMs. This requirement does not preclude
          continuous operation by sequencing multiple analysis batches;
          however, the entire analysis batch is invalid if one or more analyte
          peaks have drifted outside of designated time windows in the CCC
          at the beginning or end of the analysis batch.

10.2.3.3.   SIM MS Acquistion Parameters - Prior to selecting SIM
          parameters, analyze a mid- to high-concentration CAL in full scan
          mode.  Select one primary QI and at least one secondary ion for
          confirmation. If possible, select a second confirmation ion.
          Suggested QIs and secondary ions for all method analytes are
          designated in Table 1, but these may be modified.  An internal
          standard for each analyte is also designated in Table 1. Verify that
          the primary ion is free from interferences due to an identical
          fragment ion in any overlapping peak(s).  Selection of the QI
          should be based on the best compromise between the intensity of
          the signal for that ion and the likelihood and intensity of
          interferences. The most intense ion may not be the best QI.
          Adjust the cycle time to measure at least five spectra during the
          elution of each GC peak. If the chromatogram is divided into time
          windows, the laboratory must ensure that each method analyte
          elutes entirely within the proper window during each analysis.
          This can be achieved by carefully monitoring the retention times of
          all ISs and SURs in each sample, and carefully monitoring the
          retention times of all method analytes  in CCCs, LFBs and LFMs.
          This requirement does not preclude continuous operation by
          sequencing multiple analysis batches;  however, the entire analysis
          batch is invalid if one or more analyte peaks have drifted outside of
          designated time windows in the CCC at the beginning or end of the
          analysis batch. The SIM parameters used during method
          development for selected analytes are  provided in Table 16 as an
          example.

10.2.3.4.   Alternating Full and SIM Scan Modes - Alternating full and  SIM
          scan modes during a single sample acquisition is permitted if the
          minimum number of scans across each GC peak acquired in each
          mode is maintained (as specified in Sect.  10.2.3.2 and 10.2.3.3),
          i.e., a minimum of five scans in full scan mode and a minimum of
          five scans in SIM mode. If the chromatogram is divided into time
          windows, the laboratory must ensure that each method analyte
          elutes entirely within the proper window during each analysis.
          This can be achieved by carefully monitoring the retention times of
          all ISs and SURs in each sample, and carefully monitoring the

                       525.3-37

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                retention times of all method analytes in CCCs, LFBs and LFMs.
                This requirement does not preclude continuous operation by
                sequencing multiple analysis batches; however, the entire analysis
                batch is invalid if one or more analyte peaks have drifted outside of
                designated time windows in the CCC at the beginning or end of the
                analysis batch.

10.2.4.  CALIBRATION SOLUTIONS - To establish a calibration range extending
        two orders of magnitude, prepare a set of at least six calibration standards as
        described in Sect. 7.2.4. The lowest concentration CAL must be at or below
        the MRL for each method analyte. The MRL must be confirmed using the
        procedure outlined  in Sect. 9.2.4 after establishing the initial calibration.

        Note: This method contains many analytes that vary widely with regard to
        instrument sensitivity. If the analytes of interest differ in response, and the
        CAL standards have been prepared such that all analytes are at the same
        concentration, more standards may be needed to obtain the minimum five
        CAL points for each analyte. Analytes with poor response may not be
        observed in the low concentration standards, and the most responsive
        analytes may saturate the detector at the higher concentrations.  It is likely
        that the calibration  range for all analytes will not be the same.  The use of
        custom calibration  standards with varying analyte concentrations based on
        their relative instrument response is a possible alternative.

10.2.5.  CALIBRATION - Calibrate the GC/MS system using the  internal standard
        technique in either  full scan, SIM or alternating full scan/SIM mode.
        Subsequent sample analysis must be performed in the same calibration
        mode using identical instrument conditions  and parameters.  Internal
        standard designations and suggested QIs for all method analytes are listed in
        Table 1. Table 16 contains example scanning parameters for selected
        analytes in SIM mode. Linear or quadratic  calibrations may be used.
        Weighting may be used at the discretion of the analyst. In general, forcing
        zero as part of the calibration is not recommended. However, zero must be
        forced for all analytes that are routinely observed as contaminants in
        LRBs. Forcing zero allows for a better estimate of the background level of
        contaminants in the blank.  An accurate estimate of background
        contamination is necessary to set MRLs for method analytes when blank
        levels are problematic (Sect. 9.3.1).  For example, phthalates are a chemical
        class which is typically problematic with regard to background
        contamination.

      10.2.5.1.   Toxaphene calibration - Analyze a minimum of five calibration
                standards of technical toxaphene.   These calibrations standards
                must contain only toxaphene and the ISs and SURs. Select a
                minimum  of four chromatographic peaks from the toxaphene
                chromatograms to use for calibration. See Fig. 2 as  an example of

                             525.3-38

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                        suggested peak selection, and Table 16 as an example of suggested
                        SIM parameters.  Create a calibration curve for each selected peak,
                        using the total technical toxaphene concentration in each CAL
                        standard as the calibration concentration.  See Sect. 12.3.3 for
                        utilizing the curves to calculate the concentration of toxaphene in
                        CCCs, LFBs, Field Samples, LFSMs, QCSs, FDs, and LFSMDs.

       10.2.6.  CALIBRATION ACCEPTANCE CRITERIA - Validate the initial
               calibration curves by using the regression equations to calculate the
               concentration of each analyte as an unknown in each of the analyses used to
               generate the curves.  Calibration points that are < MRL must calculate to be
               within ± 50% of their true value.  All other calibration points must calculate
               to be within ± 30% of their true value.  If these criteria cannot be met, the
               analyst may eliminate either the highest or lowest point on the curve and
               reassess the acceptance criteria. If the  acceptance criteria still cannot  be
               met, the analyst will have difficulty meeting ongoing QC criteria.  It is
               highly recommended that corrective action be taken before proceeding.
               This may include one or more of the following actions: analyze the
               calibration standards,  further restrict the range of calibration, or select an
               alternate method of calibration. The data presented in this method were
               obtained using either linear regression  or quadratic fits. Quadratic fit
               calibrations should be used with caution, because the non-linear area of the
               curve may not be reproducible.

10.3.   CONTINUING CALIBRATION CHECK (CCC) - Analyze a CCC to verify the
       initial calibration at the beginning of each analysis batch, after every tenth Field
       Sample, and at the end of each analysis batch.  The beginning CCC for each analysis
       batch must be at or below the MRL. This CCC verifies instrument sensitivity prior
       to the analysis of samples. Alternate subsequent CCCs between the remaining
       calibration levels.

       Notes:
           •  If standards have been prepared  such that all analytes are not in the same
              calibration standard (or all low CAL points are not in the same CAL
              standard), it may be necessary to analyze more than one CCC to meet this
              requirement. Alternatively, it may be cost effective to prepare or obtain a
              customized standard to meet this criterion.
           •  Separate CCCs must be analyzed for toxaphene if it is one  of the analytes
              being measured.  The frequency of analysis, the concentration rotation
              requirements and acceptance criteria are the same for toxaphene as for  other
              analytes.

       10.3.1.  Verify that the peak area of the QI of each IS has not changed by more than
               ± 50% from the mean peak area measured for that IS during initial
               calibration.  In addition, verify that the peak area of the QI of each of the
               ISs 1-3 are within ± 30% from the most recently analyzed CCC.  If these

                                     525.3-39

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                   limits are exceeded, remedial action must be taken (Sect. 10.3.3). Control
                   charts are useful aids in documenting system sensitivity changes.

           10.3.2.  Calculate the concentration of each analyte and surrogate in the CCC. The
                   calculated amount for each analyte for medium and high level CCCs must
                   be ± 30% of the true value. The calculated amount for the lowest
                   calibration level for each analyte must be within ± 50% of the true value.  If
                   these criteria are not met, then all data for the problem analyte must be
                   considered invalid, and remedial action (Sect. 10.3.3) must be taken.
                   Recalibration may be required.  Any Field Sample extracts that have been
                   analyzed since the last acceptable calibration verification should be
                   reanalyzed after adequate calibration has been restored, with the following
                   exception. If the CCC at the end of an analysis batch fails because the
                   calculated concentration is greater than 130% (150% for the low-level
                   CCC) for a particular target analyte, and Field Sample extracts show no
                   detection for that target compound, non-detects may be reported without
                   reanalysis.

           10.3.3.  REMEDIAL ACTION - Failure to meet CCC QC performance criteria may
                   require remedial action. Major maintenance such as cleaning an ion source,
                   cleaning the  mass analyzer, replacing filament assemblies, or replacing the
                   GC column,  etc., will likely require returning to the initial calibration step
                   (Sect. 10.2).

11. PROCEDURE

    11.1.   This section describes the procedures for sample preparation, SPE, final extract
           preparation and storage, and extract analysis.  Important aspects of this analytical
           procedure include proper preparation of laboratory glassware, sample containers
           (Sect.  4.1), and sample collection and storage (Sect. 8). Procedures for data analysis
           and calculations are described in Sect. 12.

    11.2.      SAMPLE PREPARATION

           11.2.1.  Samples are  preserved, collected and stored as described in Sect. 8.  All
                   field and QC samples,  including LRBs and LFBs, must contain the
                   preservatives listed in Sect. 8.1.2. Before extraction, verify that the  sample
                   pH is < 4.  If the sample pH does not meet this requirement, discard the
                   sample.  If the  sample pH is acceptable, proceed with the analysis. Mark
                   the level of the sample on the outside of the sample bottle for later sample
                   volume determination. If using weight to determine volume (Sect. 11.10),
                   weigh the bottle and sample contents before extraction.

           11.2.2.  Add an aliquot of the SUR PDS(s) to each sample to be extracted. For
                   method development work, a 10-jiL aliquot of each of the 500-|ig/mL SUR
                                         525.3-40

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                PDSs (Sect. 7.2.2) was added to 1 L samples for a final concentration of
               5.0
       1 1.2.3.  If the sample is an LFB, LFSM, or LFSMD, add the necessary amount of
               Analyte Fortification Solution(s) (Sect. 7.2.3.2). Swirl each sample to
               ensure all components are mixed.

       1 1.2.4.  Proceed with sample extraction using one of the SPE options described in
               Sects. 11.3-11.7.

11.3.   CARTRIDGE SPE (6 mL) PROCEDURE - This cartridge extraction procedure may
       be carried out in a manual mode or by using a robotic or automatic sample
       preparation device. This section describes the SPE procedure using the equipment
       outlined in Sect. 6. 1 1 in its simplest, least expensive mode without the use of a
       robotic system. The manual mode described below was used to collect data presented
       in  Sect. 17. The extraction steps are written for an individual sample, but multiple
       samples may be extracted simultaneously depending upon the extraction equipment
       used.

       Automated systems may use either vacuum or positive pressure to process samples
       and solvents through the cartridge. All sorbent washing, conditioning, sample
       loading, rinsing, drying and elution steps must be performed as closely as possible to
       the manual procedure. The solvents used for washing, conditioning, and sample
       elution must be the same as those used in the manual procedure: however, the
       amount used may be increased as necessary to achieve the required data quality.
       Solvent amounts may not be decreased. Sorbent drying times prior to elution may be
       modified to achieve the required data quality. Caution should be exercised when
       increasing solvent volumes.  Increased extract volume will likely necessitate the
       need for additional sodium sulfate drying, and extended evaporation times which
       may compromise data quality. Caution should also be exercised when modifying
       sorbent drying times. Excessive drying may cause losses due to analyte volatility,
       and excessive contact with room air may oxidize some method analytes. Insufficient
       drying may leave excessive water trapped in the cartridge and lead to poor
       recoveries. Compressed gas cylinders of high purity nitrogen may be used with
       systems that use positive pressure for sample processing.

       11.3.1.  CARTRIDGE CLEANUP - Install the SPE cartridge (Oasis HLB or J.T.
               Baker H^O Phobic DVB as described in Sect. 6.11.1) into the vacuum
               manifold.  Wash the cartridge with 5 mL of EtOAc by adding the solvent to
               the cartridge; draw about half through the sorbent, soak for about one min,
               then draw the remaining solvent through the cartridge.

       11.3.2.  CARTRIDGE CONDITIONING - Polymeric SPE sorbents are water
               wettable (unlike C-18 SPE sorbents). Many manufacturers of polymeric
               SPE media suggest that their products do not need to be kept wet during
               conditioning and sample processing. However, little data have been shown

                                     525.3-41

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               to demonstrate performance under those conditions for the wide variety of
               environmental contaminants using these media.  Therefore, in the interest of
               providing a single procedure for the sorbents and analytes in this method,
               the authors chose to use procedures similar to those used with C-18 where
               the sorbent is kept wet.

             11.3.2.1.  CONDITIONING WITH METHANOL - Add lOmLMeOHto
                       the  cartridge and allow it to soak for about one min.  Then draw
                       most of the MeOH through. A layer of MeOH must be left on the
                       surface of the cartridge. Do NOT let the cartridge go dry from this
                       point on until the end of sample extraction, otherwise recondition
                       the  cartridge with 10 mL MeOH.

             11.3.2.2.  CONDITIONING WITH WATER - Rinse the cartridge by adding
                       10 mL of reagent water to the cartridge and drawing most through,
                       again leaving a layer on the surface  of the cartridge.  Do NOT let
                       the  cartridge go dry from this point on until the end of sample
                       extraction, otherwise recondition the cartridge starting with step
                       11.3.2.1.

       11.3.3.  SAMPLE EXTRACTION - Attach a PTFE transfer line to the top of the
               cartridge.  Insert the opposite end of the transfer  line into the sample to be
               extracted. Apply vacuum to begin the extraction. Adjust the vacuum so
               that the sample passes through the cartridge at a  rate of about  10 mL/min.
               Pass the entire sample volume through the cartridge, draining  as much
               water from the sample container as possible.  Rinse the bottle with 10 mL
               LRW and transfer to the cartridge under full vacuum.  Rinsing the sorbent
               with LRW prior to drying helps remove  sample preservatives from the
               sorbent so they are not transferred to the extract. Remove the sample
               transfer line  from the cartridge and dry by maintaining vacuum for about
               10 min.

       11.3.4.  CARTRIDGE ELUTION - Remove the  manifold lid (but do not remove  the
               cartridge) and insert a suitable collection tube to contain the eluent (15 mL
               collection vial). Reassemble the apparatus.  Add 5 mL of EtOAc to the
               sample bottle, and rinse the inside walls thoroughly. Allow the solvent to
               settle to the bottom of the bottle, and then transfer to the cartridge by
               applying vacuum. Draw about half of the solvent through the cartridge, cut
               off vacuum at the cartridge, and allow the cartridge to soak for one min.
               Draw the remaining solvent through the  cartridge.  Repeat the above step
               with DCM.  Shut off vacuum, remove the transfer line, and remove the
               collection vial. Proceed to Sects. 11.8 and 11.9 to dry and concentrate the
               extract.

11.4.   CARTRIDGE SPE (83 ML) PROCEDURE - This cartridge extraction  procedure
       may be carried out in a manual mode or by using  a robotic or automatic sample

                                    525.3-42

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preparation device. This section describes the SPE procedure using the equipment
outlined in Sect. 6.12 in its simplest, least expensive mode without the use of a
robotic system. The manual mode described below was used to collect data presented
in Sect. 17.

Automated systems may use either vacuum or positive pressure to process samples
and solvents through the cartridge. All sorbent washing, conditioning, sample
loading, rinsing, drying and elution steps must be performed as closely as possible to
the manual procedure. The solvents used for washing, conditioning, and sample
elution must be the same as those used in the manual procedure: however, the
amount used may be increased as necessary to achieve the required data quality.
Solvent amounts may not be decreased.  Sorbent drying times prior to elution may be
modified to achieve the required data quality. Caution should be exercised when
increasing solvent volumes. Increased extract volume will likely necessitate the
need for additional sodium sulfate drying, and extended evaporation times which
may compromise data quality. Caution should also be exercised when modifying
sorbent drying times.  Excessive drying may cause losses due to analyte volatility,
and excessive contact with room air may oxidize some method analytes. Insufficient
drying may leave excessive water trapped in the cartridge and lead to poor
recoveries.  Compressed gas cylinders of high purity nitrogen may be used with
systems that use positive pressure for sample processing.

11.4.1.  CARTRIDGE CLEANUP - Assemble the extraction system by adding
        cartridge adaptors, UCT Universal 525 cartridges and bottle holders to the
        six station manifold. Wash the bottle holders and cartridges with 5  mL 1:1
        EtOAc:DCM, draw half through, soak the sorbent for one min, then draw
        the remaining solvent through, maintaining the vacuum for two additional
        min.

11.4.2.  CARTRIDGE CONDITIONING

      11.4.2.1.   CONDITIONING WITH METHANOL - Add 10 mL MeOH to
                each cartridge. Soak for one min. Then draw most of the MeOH
                through, leaving a thin layer of MeOH on the surface of the
                cartridge. Do NOT let the cartridge go dry from this point on until
                the end of sample extraction, otherwise recondition the cartridge
                with lOmLMeOH.

      11.4.2.2.   CONDITIONING WITH WATER - Add 10  mL LRW to each
                cartridge. Then draw most through, leaving a thin layer on the
                surface of the cartridge. Do NOT let the cartridge go dry from this
                point on until the end of sample extraction, otherwise recondition
                the cartridge starting with step 11.4.2.1.

11.4.3.  SAMPLE EXTRACTION - Load the sample bottles onto the bottle holders.
        Turn on the vacuum; adjust the  flow at a fast drop-wise fashion.  A  flow

                              525.3-43

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               rate of 10 mL/min provides optimum recoveries.  After passing the entire
               volume of each sample through the cartridges, add 10 mL LRW to the
               sample bottle, rinse and pass the water through the cartridges. Rinsing the
               sorbent with LRW prior to drying helps remove sample preservatives from
               the sorbent so they are not transferred to the extract.  Remove the sample
               bottles. Dry the cartridges under full vacuum for 10 min.

       11.4.4.  CARTRIDGE ELUTION - Remove cartridge adaptors and insert 40-mL
               glass vials into the manifold to collect the eluent.  Replace the cartridge
               adaptors, cartridges and bottle holders on the manifold. Rinse each bottle
               holder and cartridge with 5 mL EtOAc, draw half through the sorbent, soak
               one min,  then draw the remaining through. Repeat with 5 mL DCM. Again,
               rinse each sample bottle thoroughly with 5 mL EtOAc. Then pour the
               rinsing solvent into the cartridge. Repeat with 5 mL DCM. Proceed to
               Sects. 11.8 and  11.9 to dry and concentrate the extract.

11.5.   SPEEDISK SPE PROCEDURE - The Speedisk extraction procedure may be carried
       out in a manual mode or by using a robotic or automatic sample preparation device.
       This section describes the SPE procedure using the equipment outlined in Sect. 6.10
       in its simplest, least expensive mode without the use of a robotics system. The
       manual mode described below was used to collect data presented in Sect. 17. The
       extraction steps are written for an individual sample, but multiple samples may be
       extracted simultaneously depending upon the extraction equipment used.

        Note: All automated extraction systems may not be suitable for use with Speedisks.
        See the warning concerning excessive water content in extracts in Sect. 13.6.6.

        Automated systems may use either vacuum or positive pressure to process samples
        and solvents through the disk.  All sorbent washing, conditioning, sample loading.
        rinsing, drying and elution steps must be performed as closely as possible to the
        manual procedure.  The solvents used for washing, conditioning, and sample elution
        must be the same as those used in the manual procedure: however, the amount used
        may be increased as necessary to achieve the  required data quality. Solvent
        amounts may not be decreased. Sorbent drying times prior to elution may  be
        modified to achieve the  required data quality.  Caution should be exercised when
        increasing solvent volumes.  Increased extract volume will likely necessitate the
        need for additional sodium sulfate drying, and extended evaporation times which
        may compromise data quality.  Caution should also be exercised when modifying
        sorbent drying times.  Excessive drying may cause losses due to analyte volatility,
        and excessive contact with room air may oxidize some method analytes.
        Insufficient drying may  leave excessive water trapped in the disk and lead  to poor
        recoveries. Compressed gas cylinders of high purity nitrogen may be used with
        systems that use positive pressure  for sample processing.

       11.5.1.  SPEEDISK CLEANUP - Insert a J.T. Baker Speedisk disk (DVB H2O
               Phobic, 55 mm) onto a J.T. Baker Speedisk manifold apparatus. Wash the

                                     525.3-44

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        disk with 5 mL of EtOAc by adding the solvent to the disk, drawing about
        half through the disk, allowing it to soak the disk for about one min, then
        drawing the remaining solvent through the disk.

11.5.2.  SPEEDISK CONDITIONING

      11.5.2.1.   CONDITIONING WITH METHANOL  - Pre-wet the disk with
                10 mL MeOH by adding the MeOH to the disk and allowing it to
                soak for about one min, then drawing most of the remaining
                MeOH through. A layer of MeOH must be left on the surface of
                the disk, which should not be allowed to go dry from this point
                until the end of the sample extraction. Note that it may be
                necessary to briefly remove the disk from the manifold to prevent
                residual vacuum from pulling the remaining MeOH through and
                unintentionally allowing the disk to dry out.

      11.5.2.2.   CONDITIONING WITH WATER - Rinse the disk with 10 mL
                reagent water by adding the water to the disk and drawing most
                through, again leaving a layer on the surface of the disk. Add a
                sample reservoir adaptor to the top of the Speedisk.

11.5.3.  SAMPLE EXTRACTION - Add the water sample to the reservoir and
        apply full vacuum to begin the extraction. Particulate-free water may pass
        through the disk in as little as five min without reducing analyte recoveries.
        Pass the entire sample through the disk, draining as much water from the
        sample container as possible.  Rinse the bottle with 10 mL LRW and transfer
        to the disk under full vacuum. Rinsing the sorbent with LRW prior to
        drying helps remove sample preservatives from the sorbent so they are not
        transferred to the extract. Dry the disk by maintaining vacuum for about
        three min.

11.5.4.  SPEEDISK ELUTION - Remove the reservoir adaptor and Speedisk disk,
        and add the collection vial adaptor and insert a suitable collection tube to
        contain the eluent (40 to 60-mL collection vial). Reassemble the apparatus.
        Add ~2 mL of acetone to the  sample bottle, and rinse the  inside walls
        thoroughly. Allow the solvent to settle to the bottom of the bottle, then
        transfer it to the disk. Draw the solvent through the disk by applying
        vacuum.  Add 5 mL of EtOAc to the sample bottle, and rinse the inside
        walls thoroughly. Allow the solvent to settle to the bottom of the bottle,
        then transfer it to the Speedisk disk.  A disposable pipette  or syringe may be
        used to do this, rinsing the sides of the glass filtration reservoir in the
        process. Draw about half of the solvent through the disk, release the
        vacuum, and allow the disk to soak for one min. Draw the remaining
        solvent through the disk.  Repeat the above step with 5 mL DCM.  Proceed
        to Sects 11.8 and 11.9 to dry and concentrate the extract.
                             525.3-45

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11.6.   EMPORE DISK SPE PROCEDURE - The disk extraction procedure may be carried
       out in a manual mode or by using a robotic or automatic sample preparation device.
       This section describes the SPE procedure using the equipment outlined in Sect. 6.9 in
       its simplest, least expensive mode without the use of a robotics system. The manual
       mode described below was used to collect data presented in Sect. 17. The extraction
       steps are written for an individual sample, but multiple samples may be extracted
       simultaneously depending upon the extraction equipment used.

       Automated systems may use either vacuum or positive pressure to process samples
       and solvents through the disk.  All sorbent washing, conditioning, sample loading,
       rinsing, drying and elution steps must be performed as closely as possible to the
       manual procedure.  The solvents  used for washing, conditioning, and sample elution
       must be the same as those used in the manual procedure: however, the amount used
       may be increased as necessary to achieve the required data quality. Solvent amounts
       may not be decreased. Sorbent drying times prior to elution may be modified to
       achieve the required data quality.  Caution should be exercised when increasing
       solvent volumes. Increased extract volume will likely necessitate the need for
       additional sodium sulfate drying, and extended evaporation times which may
       compromise data quality.  Caution should also be exercised when modifying sorbent
       drying times.  Excessive drying may cause losses due to analyte volatility, and
       excessive contact with room air may oxidize some method analytes.  Insufficient
       drying may leave excessive water trapped in the disk and lead to poor recoveries.
       Compressed gas cylinders of high purity nitrogen may be used with systems that use
       positive pressure for sample processing.

       11.6.1.  EMPORE DISK CLEANUP - Insert the disk (3M SDB-XC, 47mm) into the
               filter manifold apparatus. Wash the disk with 5 mL EtOAc by adding the
               solvent to the disk, drawing about half through the disk, allowing it to soak
               the disk for about one min, then drawing the remaining solvent through the
               disk.

       11.6.2.  EMPORE DISK CONDITIONING

              11.6.2.1.  CONDITIONING WITH METHANOL - Pre-wet the disk with 10
                       mL MeOH by adding the MeOH to the disk and allowing it to soak
                       for about one min, then drawing most of the remaining MeOH
                       through. A layer of MeOH must be left on the  surface of the disk,
                       which should not be allowed to go dry from this point until the end
                       of the sample extraction.

              11.6.2.2.  CONDITIONING WITH WATER - Rinse the disk with 10 mL
                       reagent water by adding the water to the disk and drawing most
                       through, again  leaving a layer on the surface of the disk.

       11.6.3.  SAMPLE EXTRACTION - Add the water sample to the reservoir and
               apply full vacuum to begin the extraction. Particulate-free water may pass

                                     525.3-46

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               through the disk in as little as five min without reducing analyte recoveries.
               Pass the entire sample through the disk, draining as much water from the
               sample container as possible. Rinse the bottle with 10 mL LRW and transfer
               to the disk under full vacuum. Rinsing the sorbent with LRW prior to
               drying helps remove sample preservatives from the sorbent so they are not
               transferred to the extract. Dry the disk by maintaining vacuum for about 10
               min.

       11.6.4.  DISK ELUTION - Remove the filtration top (but do not disassemble the
               reservoir and fritted base) and insert a suitable collection tube to contain the
               eluent  (40-mL collection vial). Reassemble the apparatus.  Add 5 mL
               EtOAc to the sample bottle, and rinse the inside walls thoroughly. Allow
               the solvent to settle to the bottom of the bottle, then transfer it to the disk. A
               disposable pipette or syringe may be used to do this, rinsing the sides of the
               glass filtration reservoir in the process. Draw about half of the solvent
               through the disk, release the vacuum, and allow the disk to soak for one
               min. Draw the remaining solvent through the disk.  Repeat this step with
               DCM.  Using a syringe or disposable pipette, rinse the filtration reservoir
               with 5  mL 1:1 EtOAc:DCM. Draw the solvent through the disk and into the
               collection vial.  Proceed to Sects. 11.8 and 11.9 to dry and concentrate the
               extract.

11.7.  HORIZON ATLANTIC DVB DISK PROCEDURE - This extraction procedure may
      be carried out in a manual mode or by using a robotic or automatic sample
      preparation device.  The following section describes the SPE procedure using the
      automated extraction equipment outlined in Sect. 6.13.  The automated procedure
      described below was used to collect  data presented in Sect. 17. The use of a manual
      system is allowed; however, all sorbent washing, conditioning, sample loading.
      rinsing, drying and elution steps must be performed as closely as possible to the
      automated procedure. The solvents used for washing, conditioning, and sample
      elution must be the same as those used in the manual procedure: however, the amount
      used may be increased as necessary to achieve the required data quality.  Solvent
      amounts may not be decreased. Note that in the automated procedure each solvent
      "prewet" step is  approximately 10 mL and each solvent elution "rinse" is 4-5 mL.
      Sorbent drying times prior to elution may be modified to achieve the required data
      quality.  Caution should be exercised when increasing solvent volumes. Increased
      extract volume will likely necessitate the need for additional sodium sulfate drying,
      and extended evaporation times which may compromise data quality. Caution should
      also be exercised when modifying sorbent drying times. Excessive drying may cause
      losses due to analyte volatility, and excessive contact with room air may oxidize some
      method analytes. Insufficient drying may leave excessive water trapped in the disk
      and lead to poor recoveries.  Compressed gas cylinders of high purity nitrogen may
      be used with systems that use positive pressure for sample processing.
                                     525.3-47

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Step#
1
2
O
4
5
6*
7*
8
9
10
11
Description
Prewet
Prewet
Prewet
Prewet
Sample Load
Wash
Wash
Air Dry
Rinse
Rinse
Rinse
Solvent
EtOAc
DCM
MeOH
LRW

LRW
LRW

EtOAc
DCM
DCM
Soak Time
(mm:ss)
1:00
1:00
1:00
0.05

0:10
0:10

1:30
1:30
1:30
Air Dry Time
(mm:ss)
0:30
0:30
0.00
0.00

0:30
0:30
1:00
0:30
0:30
0:30
      * Steps 6 and 7 of this procedure were added subsequent to the collection of the data
       shown in Tables 13 and 14.  The procedure has been tested with these additional
       steps, with no negative effect on the resulting data.  These steps are optional, but
       highly recommended. Rinsing the sorbent with LRW before air drying and solvent
       elution removes any residual preservatives from the sorbent so that they are not
       eluted into the extract.

       Proceed to Sects. 11.8 and 11.9 to dry and concentrate the extract.

11.8.   DRYING THE EXTRACT - Transfer the combined eluent through a drying tube
       containing about 10 g of anhydrous sodium sulfate. Rinse the collection tube with
       5 mL DCM, and then put the DCM through the sodium sulfate. Collect the dried
       extract and DCM rinse in a clean collection tube (15- or 40-mL tube depending on
       the extract volume).

       Note:  Speedisk disk extracts may contain higher amounts of water due to the
       acetone in the elution steps.  If extracts appear wet after completing Sect. 11.8 or
       11.9, additional sodium sulfate may be used. If additional sodium sulfate is used the
       5 mL DCM rinse may need to be increased by a proportional amount.

11.9.   EXTRACT CONCENTRATION - Concentrate the extract to about 0.7 mL under a
       gentle stream of nitrogen gas in a warm water bath (at ~ 40 °C). Do not blow down
       samples to less than 0.5 mL, because the more volatile compounds will exhibit
       diminished recovery. Transfer the extract to a 1 -mL volumetric flask and add the
       internal standards (Sect. 7.2.1). Rinse the collection tube that held the dried extract
       with small amounts of EtOAc and add to the volumetric flask to bring the volume up
       to the 1-mL mark. Transfer to an autosampler vial. Store extracts at -5 °C or less
       until analysis.

11.10.  SAMPLE VOLUME OR WEIGHT DETERMINATION - Use a graduated cylinder
       to measure the volume of water required to fill the original sample bottle to the mark
       made prior to extraction (Sect. 11.2.1). Determine volume to the nearest 10 mL for
       use in the final calculations of analyte concentration (Sect. 12.2). If using weight to
                                     525.3-48

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           determine volume, reweigh the empty sample bottle. Subtract the empty bottle
           weight from the weight of the original combined bottle/sample weight measured in
           Sect. 11.2.1. To calculate the sample volume from its weight, assume a sample
           density of Ig/mL.  Use the calculated sample volume for analyte concentration
           calculations in Sect. 12.2.

   11.11.  ANALYSIS OF SAMPLE EXTRACTS

           11.11.1.  Establish operating conditions as described in Sect. 10.2.3.  Confirm that
                   compound separation and resolution are similar to those summarized in
                   Table 1 and Figures la-Id.

           11.11.2.  Establish a valid initial calibration following the procedures outlined in
                   Sect. 10.2 or confirm that the calibration is still valid by running a CCC as
                   described in Sect. 10.3.  If establishing an initial calibration for the first
                   time, complete the IDC as described in Sect. 9.2.

           11.11.3.  Analyze aliquots of Field and QC Samples at appropriate frequencies
                   (Sect. 9) with the GC/MS conditions used to acquire the initial calibration
                   and the CCC. At the conclusion of data acquisition, use the same software
                   that was used in the calibration procedure to tentatively identify peaks in
                   predetermined retention time windows of interest. Use the data system
                   software to examine the ion abundances of components of the chromato-
                   gram.

12. DATA ANALYSIS AND CALCULATIONS

   12.1.    COMPOUND IDENTIFICATION - Identify sample components by comparison of
           their retention times and mass spectra to the reference retention times and spectra in
           the user-created data base as follows:

           12.1.1.  Establish an appropriate retention time window for each analyte, internal
                   standard and surrogate analyte to identify them in QC and Field Sample
                   chromatograms. Ideally, the retention time window should be based on
                   measurements of actual retention time variation for each compound in
                   standard solutions collected on each GC/MS over the course of time. The
                   suggested variation is plus or minus three times the standard deviation of
                   the retention time for each compound for a series of injections.  The
                   injections from the initial calibration and from the IDC (Sect. 9.2) may be
                   used to calculate a suggested window size. However, the experience of the
                   analyst should weigh heavily on the determination of an appropriate
                   retention window size.

           12.1.2.  Each compound should be identified from its reference spectrum obtained
                   during the acquisition of the initial calibration curve.  The mass spectrum
                   used for identification of each compound may have been acquired in the full

                                        525.3-49

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               scan or SIM mode.  In general, all ions that are present above 30% relative
               abundance in the mass spectrum of the reference standard obtained during
               calibration should be present in the mass spectrum of the sample component
               and should agree within an absolute 20%. For example, if an ion has a
               relative abundance of 30% in the standard spectrum, its abundance in the
               sample spectrum should be in the range of 10-50%.

       12.1.3.  Identification is hampered when sample components are not resolved
               chromatographically and produce mass spectra containing ions contributed
               by more than one analyte.  When GC peaks obviously represent more than
               one sample component (i.e., broadened peak with shoulder(s) or valley
               between two or more maxima), appropriate analyte spectra and background
               spectra can be selected by examining plots of characteristic ions.
               Comparing a background subtracted spectrum to the reference spectrum is
               suggested. If two or more analytes coelute but only one GC peak is
               apparent, the identification criteria can be met but each analyte spectrum
               will contain extraneous ions contributed by the coeluting compound.
       12.1.4.  Structural isomers that produce very similar mass spectra can be explicitly
               identified only if they have sufficiently different GC retention times.
               Acceptable resolution is achieved if the height of the valley between two
               isomer peaks is < 25% of the average height of the two isomer peaks.
               Otherwise, combine the peak areas of the isomers and quantify and identify
               as an isomeric pair.

       12.1.5.  Tribufos is the oxidation product of merphos. When analyzed by GC/MS
               under the conditions used during method development, the retention time
               and mass  spectrum produced by merphos is identical to that of tribufos.
               Therefore, when tribufos is identified as a sample component in this
               method, it is possible that the original contaminant may have been merphos.

       12.1.6.  For specific instructions on identification and quantitation of the multi-
               component analytes chlordane  and toxaphene, and for instructions on
               screening for Aroclors, see Sect.  12.3.

12.2.   QUANTITATION AND CALCULATIONS

       12.2.1.  Calculate analyte and surrogate concentrations using the multipoint
               calibration established in Sect.  10.2.  Invalidating this method,
               concentrations were calculated by measuring the characteristic ions listed in
               Table  1. Other ions  may be selected at the discretion of the analyst. Do not
               use daily continuing calibration check data to quantitate analytes in
               samples.   Adjust the final analyte concentrations to reflect the actual sample
               volume determined  in Sect. 11.10. Field Sample extracts that require
               dilution should be treated as described in Sect. 12.2.2.
                                     525.3-50

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        12.2.2.  If the calculated amount of any analyte exceeds the calibration range of the
               curve, the extract must be diluted with EtOAc, with the appropriate amount
               of additional internal standard added to match the original concentration.
               Analyze the diluted extract. Acceptable surrogate performance (Sect. 9.3.6)
               should be determined from the undiluted sample extract. Incorporate the
               dilution factor into final concentration calculations. The resulting sample
               should be documented as a dilution, and MRLs should be adjusted
               accordingly.  If matrix-matched calibration standards are being used, the
               dilution may be made with EtOAc but care should be taken to dilute just
               enough to position the analyte within the calibration range. Excessive
               dilution and resulting low concentration may affect the accuracy of the final
               measurement.

        12.2.3.  Calculations must utilize all available digits of precision, but final reported
               concentrations should be rounded to an appropriate number of significant
               figures (one digit of uncertainty), typically two, and not more than three
               significant figures.

               Note:  Some data in Sect. 17 of this method are reported with more than two
               significant figures. This is done to better illustrate the method performance
               data.

12.3.   MULTI-COMPONENT ANALYTES

        12.3.1.  Technical Chlordane - Technical chlordane is a multi-component analyte
               regulated under the Safe Drinking Water Act (SDWA) at the time of
               publication of this method. It contains at least 140 chlorinated components.
               At the concentrations likely to be encountered in drinking water samples,
               only two or three major components will typically be identified: cis- and
               trans-chlordane and trans-nonachlor. If one or more of these components is
               identified in a Field Sample, and a quantitative value for technical
               chlordane is required, the analyst may choose from the following options:

               Option 1: Obtain a standard of technical chlordane  and use it to prepare
               calibration curves for each major component observed in the Field Sample.
               Assign the concentration of technical chlordane in the calibration standard
               to each peak selected for quantitation. Quantitate each of the major
               components observed in the Field Sample from the technical chlordane
               calibration and report a technical chlordane amount by averaging the values
               found  for the components.

               Option 2: If trans-chlordane is present as the major chlordane component,
               multiply the concentration of trans-chlordane (determined from calibration
               with a trans-chlordane standard) by seven to obtain a value for technical
               chlordane. (A multiplier of seven was determined from the average weight
               percent of trans-chlordane in multiple standards of technical chlordane.) If

                                      525.3-51

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                  trans-chlordane is not the major chlordane component observed, Option 1
                  must be used.

           12.3.2.  Aroclor screening - Aroclors are complex mixtures of polychlorinated
                  biphenyls (PCBs).  If any of the 14 PCB congeners in the analyte list are
                  identified in a Field Sample, presume that one or more Aroclors are present.
                  A quantitative value for "total PCBs" can be obtained by analyzing a
                  duplicate sample by Method 508A23.

           12.3.3.  Toxaphene - Identify the toxaphene peaks selected during calibration using
                  the procedures in Sects. 12.1.1 and 12.1.2. Use the calibration curves
                  created in Sect. 10.2.5.1 to quantitate each toxaphene peak.  If all four peaks
                  are present, use the mean concentration of the four as the reported
                  concentration of technical toxaphene.  All four peaks must be present in
                  calibration standards  and all fortified samples, i.e., LFBs and LFSMs. If
                  one or more, but not all of the selected component peaks are present in a
                  Field Sample, it may  be an indication that weathering has taken place.  In
                  this case, calculate the amount of technical toxaphene to be  reported as the
                  mean of ONLY the target peaks present (do not include any user-defined
                  value, or use zero in the mean calculation to represent missing peaks).
                  Annotate the reported technical toxaphene concentration with the range of
                  concentrations observed for the individual target peaks.

13. METHOD PERFORMANCE

   13.1.    METHOD DEVELOPMENT  AND PERFORMANCE DATA COLLECTION - This
           method was developed by USEPA's National Exposure Research Laboratory
           (NERL) chemists and staff from Shaw Environmental and Infrastructure, Inc.
           (SHAW) and Industrial and Environmental Services, LLC (IES) under contract to
           USEPA's Office of Ground Water and Drinking Water (OGWDW).  The method
           was developed using the four types of SPE media described in Sects. 6.9-6.11. Most
           data collected during the development phase of the method were duplicated in both
           the NERL lab and the SHAW/IES lab by different analysts using different
           instrumentation. This verified that the method procedures were transferable between
           labs.  The majority of the data presented in Sect. 17 were generated with these four
           types of SPE media. Subsequent to the method development, Horizon Technologies,
           Inc. and United Chemical Technologies (UCT) each generated data using the method
           procedures with additional types of SPE media (Sects. 6.12-6.13). These additional
           SPE products were added to the method to further extend the SPE options available
           for use with this method.  Data demonstrating the performance of these additional
           sorbents are in Tables  11-14.

           13.1.1.  GC/MS INSTRUMENTATION - The instruments described in this section
                  were used to collect method performance data as cross-referenced in the
                  footnotes of the tables in Sect. 17.
                                        525.3-52

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             13.1.1.1.  Thermo DSQ quadrupole mass spectrometer equipped with a
                       Thermo Trace Ultra GC and a Restek RXI-5sil-MS 30 m x 0.25
                       mm x 0.25 jam column. A 5-mm i.d. single gooseneck injection
                       port liner with Siltek deactivation was used (Restek #20946-214).
                       Calibration standards and sample extracts were injected in the hot,
                       splitless mode using a pressure pulse. See Sect. 10.2.3.1  for GC
                       oven temperature program.

             13.1.1.2.  Agilent 5975C MSD equipped with a 7890A GC and a Restek
                       RXI-5sil-MS 30 m x 0.25 mm x 0.25 jim column. A 4-mm i.d.
                       single gooseneck injection port liner with intermediate polarity
                       deactivation was used (Restek #20798). Calibration standards and
                       sample extracts were injected in the hot, splitless mode using a
                       pressure pulse.  See Sect. 10.2.3.1 for GC oven temperature
                       program.

             13.1.1.3.  Agilent 5973 MSD equipped with a 6890 GC and a Restek RXI-
                       5sil-MS 30 m x 0.25 mm x 0.25 |im column. A drilled Uniliner
                       (Restek #21055) was used in the injector, installed with the hole on
                       top. One microliter pulsed (1 min) splitless injections were made
                       with the injector at 275 °C. The GC oven temperature program
                       was as follows:  initial oven temperature 50 °C,  hold for 1.5  min,
                       ramp a 10 °C/min to 130 °C, ramp at 2 °C/min to 142 °C, ramp at
                       20 °C/min to 270 °C, ramp at 7 °C/min to 320 °C, hold for 1 min.

             13.1.1.4.  Agilent 5975C MSD with a 6890N GC, equipped with a Restek
                       RXI-5sil-MS 30m x 0.25 mm x 0.25 jim column. A 4-mm i.d.
                       splitless gooseneck injection port liner (UCT#GCLGN4MM) was
                       used, with the injection port at 250 °C.  One microliter injections
                       were made with a 1 min split delay. The GC oven temperature
                       program was as follows: initial oven temperature of 55 °C, hold for
                       1 min, ramp at 10 °C/min to 200 °C, ramp at 7 °C/min to a final
                       temperature of 320 °C, hold for 0.36 min.

13.2.   PRECISION AND ACCURACY DATA

       13.2.1.  FULL SCAN GC/MS - Precision and accuracy data were collected from
               LFBs at three concentration levels using each of the six sorbents described
               in Sects. 6.9-6.13.  Precision and accuracy data were also collected at a
               single fortified concentration using two challenging water matrices. Water
               matrices were selected to be representative of ground water with high
               mineral content and surface water with a moderate level of TOC. Precision
               and accuracy data in both fortified reagent water and fortified matrices are
               presented in Tables 3-14. These data were generated using matrix-matched
               calibration standards.  Performance is similar for most analytes on most
               sorbents, especially considering that the data were obtained by different

                                    525.3-53

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               analysts using different instrumentation. A notable exception is dimethipin.
               The data generated for dimethipin using the J.T. Baker H2O Phobic DVB
               Speedisk or the Oasis HLB cartridge provided the best performance.  The
               other sorbent options do not retain dimethipin sufficiently to meet the
               method acceptance criteria for recovery. If dimethipin data are to be
               reported, either the Oasis HLB cartridge or the J.T.  Baker H2O Phobic DVB
               Speedisk must be used.

       13.2.2.  SIM GC/MS  - The SIM GC/MS analysis option may be used with extracts
               from any of the options described in Sects. 6.9-6.13. To demonstrate the
               enhanced sensitivity and overall method performance using SIM, two
               sorbents were selected. Waters Oasis HLB cartridges and J.T. Baker H2O-
               Phobic DVB  Speedisks were specifically selected so that acceptable
               performance data could be obtained for dimethipin, a compound of
               particular interest to EPA at the time of method development.  Precision and
               accuracy data were collected by two laboratories using LFBs fortified at
               three concentration levels. Additional precision and accuracy data were
               collected by the same laboratories using LFSMs created by fortifying two
               challenging tap water matrices with selected analytes at either one or two
               concentrations. Tap water matrices were selected to be representative of
               ground water with high mineral content and surface water with a moderate
               level of TOC. Precision and accuracy data in both fortified reagent water
               and fortified matrices are presented in Tables 17-20. These data were
               generated using matrix-matched calibration standards.

       13.2.3.  Toxaphene data - Precision and accuracy data for toxaphene in the SIM
               mode was generated using five sorbent options in reagent water (Table 21)
               and using four sorbents in challenging drinking water matrices (Table 22).
               Toxaphene data were not generated in the full scan  mode due to poor
               sensitivity relative to regulatory requirements (Sect. 1.7).

13.3.   LCMRLsandDLs

       13.3.1.  FULL SCAN GC/MS - The values in Table 15 were generated by the
               NERL and SHAW/IES laboratories. Sorbents were selected based on their
               convenience of use by each of the laboratories.  The use of these specific
               brands of SPE media for generating LCMRLs and DLs does not imply any
               specific preference or endorsement of the products.  Because the data were
               generated in two laboratories by different personnel using different sorbent
               options and instrumentation,  minor variations between the data sets should
               be expected.

       13.3.2.  SIM GC/MS  - The values for DLs in Table 23 were generated by the NERL
               using Oasis HLB cartridges.  Table 23 also includes two sets of LCMRL
               data; one generated by NERL using Oasis HLB cartridges and one
               generated by  SHAW/IES using J.T. Baker H2O Phobic DVB Speedisks.

                                     525.3-54

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               These sorbents were selected because they provided acceptable performance
               data for dimethipin, a compound of particular interest to EPA at the time of
               method development.

13.4.   SAMPLE STORAGE STABILITY STUDIES - Drinking water samples from a
       chlorinated surface source were used as a representative matrix for an analyte
       holding time study in aqueous solution. Replicate samples in amber bottles were
       preserved as described in Sect. 8, fortified with method analytes, then stored for 48
       hours at 10 °C, followed by storage at 6 °C until analysis.  Randomly selected
       samples were analyzed in replicate (n=4) on day 0 and at several time points up to
       and beyond the 14 day holding time. Data from days 0, 7 and 14 are presented in
       Figs. 3a-3c. These data were used to establish the 14 day aqueous holding time for
       most method analytes (Sect. 8.4).

       Notes:
       •   Surrogate analytes were not stored in this study, but added at the time  of
           extraction.  The data in Figs. 3a-c for SURs are same day data,  obtained for QC
           purposes.
       •   Holding time studies conducted during method development indicated significant
           analyte losses (more than 20% in 14 days, with increasing loss at subsequent
           time points) for the two compounds listed below using the sample collection,
           preservation and holding time procedures in this method. Dichlorvos  exhibited a
           loss of 25% at 7 days, 39% at 14 days and 56% at 28 days. Cyanazine exhibited
           a loss of 16% at 7 days, 22% at 14 days, and 44% at 28 days. (All losses are
           relative to the day 0 measurement.) Degradation of these compounds  in aqueous
           samples has been previously reported.24"26
       •   Toxaphene holding time data were collected in separate LFSMs.  After 14 days
           of storage under the conditions described above, the toxaphene recovery was
           105% with an RSD of 7.1%. Aqueous holding time data for toxaphene are not
           shown  in Fig. 3.

13.5.   EXTRACT STORAGE STABILITY STUDIES - Replicate sample extracts (n=4)
       that were stored at -5 °C and protected from light, were analyzed on day 0, and at
       five additional time points up to and beyond 28 days. Data from these analyses
       validate the 28 day extract holding time and are presented in Figs. 4a-4c.  Extract
       holding time data for toxaphene were collected in separate sample extracts. After 28
       days of storage under the conditions described above, the recovery of toxaphene was
       104% with an RSD of 3.6. Extract holding time data for toxaphene are not shown in
       Fig. 4.

13.6.   POTENTIAL PROBLEMS/ PROBLEM COMPOUNDS

       13.6.1.   MATRIX INDUCED CHROMATOGRAPHIC RESPONSE
               ENHANCEMENT - Some method analytes have the potential to exhibit a
               high bias. This has been attributed to this phenomenon. Examples of this
               are shown in Table 20a for oxyfluorfen and tebuconazole, which have

                                    525.3-55

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        recovery data for a fortified tap water (from a surface water source) that is
        > 130% of the fortified amount. Data in Table 20b show that this
        phenomenon is related to analyte concentration, since the high bias is not
        observed at the higher fortified concentration.  Compounds with the
        potential for matrix induced chromatographic response enhancement are
        noted in Table 1.  Although the use of matrix-matched standards will
        improve quantitative accuracy for these analytes, a bias may still be
        observed. In addition to the use of matrix matched standards, "priming" the
        GC system by injecting one or more sample extracts at the beginning of
        each analytical sequence was found to reduce matrix enhancement effects.
        The data presented in Tables  19, 20a and 20b were obtained using this type
        of priming sequence.  Literature citations suggest that temperature
        programmed or cold injections may also reduce matrix enhancement,12'13'27
        although trials of these types of injections during method development
        showed little or no improvement.  The biased data was instrument
        dependent, and not related to the sorbent used.  Similar tap water extracts
        generated using different sorbent options listed in this  method, showed
        similarly high biased data on the same instrument.

        Depending upon the intended use of the data, the analyst should consider
        performing the MRL verification (Sect. 9.2.4.4) in fortified matrices similar
        to the samples being analyzed.

        HIGH BACKGROUND - Phthalates and adipates commonly appear in
        LRBs, either from their presence in laboratory reagent water, or in
        chemicals and solvents used in the sample preparation process.  BHT was
        also noted to have intermittently high background values during method
        development. Compounds observed to have high background values are
        noted in Table 1.

13.6.3.  HCCPD - This compound is sometimes recovered at lower rates than other
        method analytes.  It is known to be highly reactive, and degrades relatively
        quickly via photolysis and hydrolysis.28 The performance of this compound
        during method development was influential in establishing lower
        acceptance criteria for its recovery in LFBs.

13.6.4.  HCB -  This compound is sometimes recovered at lower rates than other
        method analytes.  Although there are literature references to
        photodegradtion of HCB29'30, there was no direct evidence during method
        development that this was the cause  of low recovery. The  performance of
        this compound during method development was influential in establishing
        lower acceptance criteria for its recovery in LFBs.

13.6.5.  PENT ACHLOROPHENOL - Pentachlorophenol i s prone to peak tailing
        and changes in response due to changes in the GC column  and injector.  In
        this method the isotopically labeled 13C-pentachlorophenol has been used as

                             525.3-56

-------
                  an internal standard for pentachlorophenol to minimize inaccuracies in
                  quantitation.  Assuming that there is not complete chromatographic
                  separation between pentachlorophenol and the isotopically-labeled IS, the
                  QI used for 13C-pentachlorophenol must be m/z 276 (Table 1).  Although
                  this ion has low abundance, it is the only ion free of interferences from the
                  chlorine isotope ions of pentachlorophenol.

                  Some GC/MS instrumentation may have too many active sites for
                  acceptable analysis of pentachloro-phenol by this method. Alternate
                  methods that employ derivatization procedures to methylate
                  pentachlorophenol to its methyl ether prior to analysis are available for
                  drinking water compliance monitoring.31'32

           13.6.6.  EXCESSIVE WATER CONTENT IN EXTRACTS - This is most often
                  seen using the Speedisk, and  is exacerbated by the use of some automated
                  extraction devices. Excessive water will typically result in low recoveries
                  of triazines.  Not all automated extraction systems may be suitable for use
                  with the Speedisk option.

           13.6.7.  OVERDRYING SPE MEDIA PRIOR TO ELUTION - If SPE media is
                  over dried between sample loading and solvent elution by drawing
                  excessive amounts of room air through the media, analytes that can undergo
                  oxidation may be observed to have low recoveries. Benzo(a) pyrene is an
                  example of an analyte that may be affected.

   13.7.    MULTIPLE LABORATORY DEMONSTRATION - In addition to the two
           laboratories in which this method was developed, the performance of this method in
           the SIM mode for a subset of analytes (those listed in Table 18) was demonstrated by
           three independent laboratories (two commercial laboratories and a drinking water
           utility laboratory).  These laboratories produced acceptable results and provided the
           authors with valuable comments and method performance data.  The authors wish to
           acknowledge the assistance of the analysts and managers  at the laboratories listed
           below for their participation in the multi-laboratory study.

           13.7.1.  Dr. Yongtao Li and Mr. William Davis of Underwriters Laboratories, South
                  Bend, IN.

           13.7.2.  Mr. Kevin Durk and Ms. Annmarie Walsh of Suffolk County Water
                  Authority, Hauppauge,  NY.

           13.7.3.  Dr. Andrew Eaton, Mr. Charles Grady, Mr. Ali Haghani and Mr. Patrick
                  Chapman of MWH Laboratories, Monrovia, CA.
14. POLLUTION PREVENTION


                                        525.3-57

-------
    14.1.   This method utilizes SPE to extract analytes from water. It requires the use of very
           small volumes of organic solvent and very small quantities of pure analytes, thereby
           minimizing the potential hazards to both the analyst and the environment as
           compared to the use of large volumes of organic solvents in conventional liquid-
           liquid extractions.

    14.2.   For information about pollution prevention that may be applicable to laboratory
           operations, consult "Less is Better:  Guide to Minimizing Waste in Laboratories"
           available on-line from the American Chemical Society at http://portal.acs.org/portal/
           fileFetch/C/WPCP_012290/pdf/WPCP_012290.pdf accessed November 8, 2011.

15. WASTE MANAGEMENT

    15.1.   The analytical procedures described in this method generate relatively small amounts
           of waste since only  small amounts of reagents and solvents are used. The matrices
           of concern are finished drinking water or source water.  However, the Agency
           requires that laboratory waste management practices be conducted consistent with all
           applicable rules and regulations, and that laboratories protect the air, water, and land
           by minimizing and controlling all releases from fume hoods and bench operations.
           Also, compliance is required with any sewage discharge permits and regulations,
           particularly the hazardous waste identification rules and land  disposal restrictions.

16. REFERENCES

1.   Winslow, S.D., Pepich, B.V., Martin, J.J., Hallberg, G.R., Munch, D.J., Frebis, C.P.,
    Hedrick, E. J., Krop, R. A., Statistical Procedures for Determination and Verification of
    Minimum Reporting Levels for Drinking Water Methods, Environ. Sci.  Technol., 2006, 40,
    281-288.

2.   Martin, J. J., Winslow, S.D., Munch, D.J., A New Approach to Drinking Water Quality Data:
    Lowest Concentration Minimum Reporting Level, Environ. Sci. Technol.., 2007,  41, 677-681.

3.   Glaser, J.A., Foerst, D.L., McKee, G.D., Quave, S.A., Budde, W.L., Trace Analyses for
    Wastewaters, Environ. Sci. Technol., 1981,  15, 1426-1435.

4.   Erikson, Mitchell D., Analytical Chemistry  of PCBs. Lewis Publishers,  CRC Press, 1997,
    584-585.

5.   Frame, G.M., Cochran, J.W., Bowadt, S.S.,  Complete PCB Congener Distributions for 17
    Aroclor Mixtures Determined by 3 HRGC Systems Optimized for Comprehensive,
    Quantitative, Congener Specific Analysis, J. HighResol. Chromatogr.,  1996, 19, 657-668.

6.   Erney, D.R., Gillespie, A.M., Gilvydis, D.M., Poole, C.F., Explanation of the Matrix-Induced
    Chromatographic Response  Enhancement of Organophosphorous Pesticides During Open
    Tubular Column Gas Chromatography with Splitless or Hot On-Column Injection and Flame

                                        525.3-58

-------
   Photometric Detection, J. Chromatogr., 1993, 638, 57-63.

7.  Mol, H.G.J., Althuizen, M., Janssen, H., Cramers, C.A., Brinkman, U.A.Th., Environmental
   Applications of Large Volume Injection in Capillary GC Using PTV Injectors, J. HighResol.
   Chromatogr., 1996, 19, 69-79.

8.  Erney, D.R., Pawlowski, T.M., Poole, C.F., Matrix Induced Peak Enhancement of Pesticides
   in Gas Chromatography, J. HighResol. Chromatogr., 1997, 20, 375-378.

9.  Hajslova, J., Holadova, K., Kocourek, V., Poustka, J., Godula, M., Cuhra, P., Kempny, M.,
   Matrix Induced Effects: A Critical Point in the Gas Chromatographic Analysis of Pesticide
   Residues, J. Chromatogr., 1998, 800, 283-295.

10. Wylie, P., Uchiyama, M., Improved Gas Chromatographic Analysis of Organophosphorous
   Pesticides with Pulsed Splitless Injection, J. AOAC International, 1996, 79, 571-577.

11. Hajslova, J., Zrostlikova, J., Matrix effects in (ultra) trace analysis of pesticide residues in
   food and biotic matrices, J. Chromatog. A, 2003, 1000,181-197.

12. Anastassiades, M., Mastovska, K., Lehotay, S.J., Evaluation of analyte protectants to
   improve gas Chromatographic analysis of pesticides, J. Chromatog. A, 2003, 1015,163-184.

13. Poole, C.F., Matrix induced response enhancement in pesticide residue analysis by gas
   chromatography, J. Chromatogr. A, 2007, 1158, 241-250.

14. Thurman, E.M., Mills, M.S., Solid Phase Extraction Principles and Practice. John Wiley and
   Sons, Inc.,  1998, p. 66.

15. Prudent Practices in the Laboratory: Handling and Disposal of Chemicals. National
   Academies Press (1995), available at http://www.nap.edu (accessed October 5, 2011).

16. OSHA Safety and Health Standards. General Industry. (29CFR1910), Occupational Safety
   and Health Administration, OSHA 2206, (Revised, July 2001).

17. Safety in Academic Chemistry Laboratories. American Chemical Society Publication,
   Committee on Chemical Safety, 7th Edition. Available online at http://portal.acs.org/portal/
   PublicWebSite/about/governance/committees/chemicalsafety/publications/WPCP_012294
   (accessed October 5, 2011).

18. Technical Notes on Drinking Water Methods, 1994, EPA Document #600/R-94/173.
   Available through EPA's digital publications National Environmental Publications Internet
   Site (NPEIS) database.

19. USEPA Office of Ground Water and Drinking Water, Technical Support Center, Alternate
   Test Procedure Coordinator, 26 W. Martin Luther King Dr., Cincinnati, OH, 45268.
20. Pepich, B.V., Prakash, B., Domino,  M.M., Dattilio, T.A., Munch, D.J., Price, E.K.,

                                        525.3-59

-------
   Development of USEPA Method 527 for the Analysis of Selected Pesticides and Flame
   Retardants in the UCMR Survey. Environ. Sci. TechnoL, 2005, 9, 4996-5004.

21. Winslow, S.D., Prakash, B., Domino, M.M., Pepich, B.V., Munch, D.J., Considerations in
   gathering Occurrence Data for Selected Unstable Compounds in the USEPA Unregulated
   Contaminant Candidate List in USEPA Method 526.  Environ. Sci. TechnoL, 2001, 5, 1851-
   1858.

22. Price, E.K., Prakash, B., Domino, M.M., Pepich, B.V., Munch, D.J., Method 527.
   Determination of Selected Pesticides and Flame Retardants in Drinking Water by Solid Phase
   Extraction and capillary Gas Chromatography/ Mass Spectrometry, 2005, EPA Document
   #815-R-05-005.  Available on-line at http://www.epa.gov/safewater/methods/pdfs/methods/
   met527.pdf (accessed October 5, 2011).

23. Bellar, T.A., Method 508A. Screening for Polychlorinated Biphenyls by Perchlorination and
   Gas Chromatography, 1989. In: Methods for the Determination of Organic Compounds in
   Drinking Water.  1989, revised 1991, EPA Document #600/4-88/039. Available on-line at
   http://www.nemi.gov (accessed October 5, 2011).

24. National Library of Medicine HSDB Database, Cyanazine. Available at
   http://toxnet.nlm.nih.gov (accessed October 5, 2011).

25. Dichlorvos Environmental Assessment, Australian Pesticides and Veterinary Medicines
   Authority, 2008. Available at http://www.apvma.gov.au (accessed October 5,  2011).

26. Dichlorovos, Extension Toxicology Network, 1993, Available at http://pmep.cce.cornell.edu
   (accessed October 5, 2011).

27. Szelewski, M., Environmental Semivolatiles Using an Agilent Multimode Inlet for
   Maximum Sensitivity -  Application Note. Agilent Technologies, Inc. 2850 Centerville Rd.,
   Wilmington, DE 19809-1610.

28. Toxicological Profile for Hexachlorocyclopentadiene (HCCPD), U.S. Department of Health
   and Human Services, Public Health Service, Agency for Toxic Substances and Disease
   Registry (1999).  Available at http://www.atsdr.cdc.gov/ToxProfiles/tpl 12.pdf (accessed
   Octobers, 2011).

29. Yamada, M., Naito, N, Takada, M., Nakai, S., Hosomi, M., Photodegradation of
   Hexachlorobenzene and Theoretical Prediction of its Degradation Pathways Using Quantum
   Chemical Calculation, Chemosphere, 2008, 70, 731-736.

30. Plimmer, J.R., Klingebiel, U.I., Photolysis of Hexachlorobenzene, J. Agric. FoodChem.,
   1976, 24, 721-723.

31. Pawlecki-Vonderheide, A.M., Munch, D.J., Method 515.3. Determination of Chlorinated
   Acids in Drinking Water by Liquid-Liquid Extraction, Derivatization and Gas

                                        525.3-60

-------
   Chromatography with Electron Capture Detection. 1996. Available on-line at
   http://www.nemi.gov (accessed October 5, 2011).

32. Wendelken, S.C., Bassett, M.V., Dattilio. T.A., Pepich, B.V., Method 515.4. Determination
   of Chlorinated Acids in Drinking Water by Liquid-Liquid Microextraction, Derivatization,
   and Fast Gas Chromatography with Electron Capture Detection. 2000.  Available on-line at
   http://www.nemi.gov (accessed October 5, 2011).

33. Standard Operating Procedure for Disinfectant Sample Preparation, SOP MB-22-00, 2008.
   USEPA, Office of Pesticide Programs, Environmental  Service Center, Ft. Meade, MD.
   Available on-line at http://www.epa.gov/pesticides/methods/atmpmethods/MB-22-00.pdf
   (access November 10, 2011).
                                        525.3-61

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17. TABLES, FIGURES AND VALIDATION DATA
Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested
Confirmation Ions, and Suggested Internal Standard Reference
Peak
Identification
#, Figure 1
15
41
47
116
1
2
o
J
4
5
6
7
8
9
10
11
12
13
14
16
17
18
19
20
21
22
23
24
25
26
RT (min)
13.21
16.35
16.73
24.29
7.24
8.20
9.13
9.97
11.21
11.53
12.44
12.48
12.71
12.74
12.77
12.84
12.87
12.88
13.43
13.45
13.47
13.69
13.79
13.92
14.31
14.44
14.46
14.53
14.68
Internal Standards, Analytes and
Surrogates
acenaphthene-^io (IS 1)
13C-pentachlorophenol (IS 4)
phenanthrene-^io (IS 2)
chrysene-^12 (IS 3)
DIMP
isophorone
l,3-dimethyl-2-nitrobenzene (SUR)
dichlorvos
HCCPD
EPTC
mevinphos
butylate
vernolate
dimethylphthalate
etridiazole
2,6-dinitrotoluene
acenaphthylene
pebulate
2-chlorobiphenyl
BHT
chloroneb
tebuthiuron
2,4-dinitrotoluene
molinate
DEBT
diethylphthalate
4 -chlorobiphenyl
fluorene
propachlor
IS Ref.
#




1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
QI (m/z)
162
276
188
240
97
82
77
109
237
128
127
57
128
163
211
165
152
128
188
205
193
156
165
126
119
149
188
165
120
Confirmation
Ion(s) (nt/z)
164
-
160*
236*
123
138*
134
185*
235,239
86
109*, 192*
146, 156
86
77*
183
63,89
-
57,72
152
220
191
171
63,89
55
91, 190
177*
152
166
77, 176
Comments
a
b,c,d
a
a
b
a
a
a,d,e
a
a
a,d,e,f
a
a
a
a
a
a
a
a
b,g
a
a
a
a
b
a,g
a
a
a
                                    525.3-62

-------
Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested
Confirmation Ions, and Suggested Internal Standard Reference
Peak
Identification
#, Figure 1
27
28
29
30
31
32
33
34
35
36
37
38
39
40
42
43
44
45
46
48
49
50
51
52
53
54
55
56
57
58
RT (min)
15.00
15.03
15.27
15.34
15.66
15.75
15.81
15.83
16.08
16.20
16.21
16.28
16.29
16.30
16.35
16.36
16.46
16.66
16.69
16.79
16.81
16.91
16.91
17.01
17.06
17.53
17.68
17.71
17.73
17.79
Internal Standards, Analytes and
Surrogates
ethoprop
cycloate
chlorpropham
trifluralin
phorate
a-HCH
2,4'-dichlorobiphenyl
hexachlorobenzene
atraton
simazine
prometon
dimethipin
atrazine
P-HCH
pentachlorophenol
propazine
y-HCH (lindane)
pronamide
2,2',5-trichlorobiphenyl
phenanthrene
chlorothalonil
disulfoton
anthracene
terbacil
5-HCH
phosphamidon
acetochlor
metribuzin
2,4,4'-trichlorobiphenyl
vinclozolin
IS Ref.
#
1
1
1
1
1
1
1
1
2
2
2
2
2
2
4
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
QI (m/z)
97
83
213
264
75
181
222
284
196
201
225
54
200
181
266
214
183
173
256
178
266
88
178
117
181
127
146
198
186
212
Confirmation
Ion(s) (m/z)
126, 139, 158
55, 154
127
306
121
109, 183,219
152, 224
142, 249
169,211
173, 186
168,210
53
215
109, 183,219
264, 268
58, 229
109, 181,219
145
186
152*
264, 268
61*, 97*
-
161
109, 183,219
72, 264
59, 162, 223
-
256
124, 285
Comments
a,d
a
a
a,d
b,d
a
a
a
a
a
a
b
a
a
a,c,d
a
a,e
a
a
a
a,e
a
a
a,d
a
b,d
a
a
a,e
b,e
                                      525.3-63

-------
Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested
Confirmation Ions, and Suggested Internal Standard Reference
Peak
Identification
#, Figure 1
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
RT (min)
17.84
17.87
17.96
18.04
18.05
18.10
18.39
18.47
18.53
18.56
18.72
18.76
18.84
18.87
18.87
18.91
18.92
19.01
19.27
19.30
19.59
19.72
19.74
19.85
20.27
20.38
20.46
20.54
20.58
20.59
Internal Standards, Analytes and
Surrogates
methyl parathion
alachlor
simetryn
ametryn
heptachlor
prometryn
terbutryn
2,2',5,5'-tetrachlorobiphenyl
dibutyl phthalate
bromacil
metolachlor
chlorpyrifos
aldrin
cyanazine
dacthal (DCPA)
2,2',3,5'-tetrachlorobiphenyl
ethyl parathion
triadimefon
diphenamid
MGK 264(a)
MGK 264(b)
heptachlor epoxide
chlorfenvinphos
2,3',4',5-tetrachlorobiphenyl
trans-chlordane
tetrachlorvinphos
butachlor
pyrene
cis-chlordane
endosulfan I
IS Ref.
#
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
QI (m/z)
109
188
213
227
100
241
226
220
149
205, 207
162
97
66
225
301
220
109
208
72
164
164
353
267
220
375
109
176
202
375
241
Confirmation
Ion(s) (m/z)
125, 263
160
155, 170
212
272, 274
184, 226
170, 185, 241
290, 292
-
207, 205
238
197, 199
79, 263
68, 172, 198
332
255, 292
97, 291
57
167, 239*
66, 111
66, 111
81,355
269, 323
110,292
237, 272
329,331
57, 160
-
373, 377
195, 207
Comments
b,d
a
a
a
a
a
a
a
a
a
a
a,e
a
a
a
a
b,d
a,d,e
a
a,h
a,h
a,e
b,d
a
a
a,d
a,d
a
a
a
                                      525.3-64

-------
Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested
Confirmation Ions, and Suggested Internal Standard Reference
Peak
Identification
#, Figure 1
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
117
118
119
RT (min)
20.65
20.76
21.00
21.12
21.17
21.23
21.25
21.26
21.69
21.72
21.81
21.90
21.91
21.99
22.11
22.11
22.40
22.82
22.91
22.91
23.03
23.06
23.17
23.38
23.39
23.48
24.26
24.37
24.40
24.67
Internal Standards, Analytes and
Surrogates
trans-nonachlor
napropamide
profenofos
4,4'-DDE
tribufos (+merphos)
dieldrin
oxyfluorfen
2,3,3',4',6-pentachlorobiphenyl
nitrofen
endrin
2,2',3,4',5',6-hexachlorobiphenyl
chlorobenzilate
2,3',4,4',5-pentachlorobiphenyl
endosulfan II
4,4'-DDD
ethion
2,2',4,4',5,5'-hexachlorobiphenyl
norflurazon
butylbenzylphthalate
endosulfan sulfate
4,4'-DDT
2,2',3,4,4',5'-hexachlorobiphenyl
hexazinone
di(2-ethylhexyl)adipate
tebuconazole
triphenyl phosphate (SUR)
benzo [a] anthracene
chrysene
methoxychlor
2,2',3,4,4',5,5'-heptachlorobiphenyl
IS Ref.
#
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
QI (m/z)
409
72
339
246
57
79
252
326
283
263
360
251
326
195
235
231
360
145
149
272
235
360
171
129
125
77
228
228
227
394
Confirmation
Ion(s) (m/z)
407,411
100, 128
97, 139, 208
176,318
169
81
63,361
184, 254
139, 202
81,281
218,290
111, 139
184, 254
207, 241
165
97, 153
218,290
102, 303
91,206
237, 387
165
218,290
83*
57,70
83, 250
169, 326
226*
226*
-
252, 324
Comments
a
a,d
b,d
a
b,d,i
a,e
b,d
a
b,d
a
a
a
a
a
a,d
b,d,e
a
a,d
a,g
a,e
a,e
a
a,d
a,g
b,d,e
a,e
a
a
a,d
a
                                      525.3-65

-------
Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested
Confirmation Ions, and Suggested Internal Standard Reference
Peak
Identification
#, Figure 1
120
121
122
123
124
125
126
127
128
129
130
131
RT (min)
24.93
25.79
26.64
26.82
27.49
27.54
28.22
28.28
28.50
30.72
30.80
31.20
Internal Standards, Analytes and
Surrogates
di(2-ethylhexyl)phthalate
fenarimol
cis-permethrin
trans-permethrin
benzo[6]fluoranthene
benzo [k] fluoranthene
benzo[a]pyrene-<5?i2 (SUR)
benzo[a]pyrene
fluridone
indeno[l,2,3-c,c/|pyrene
dibenzo[a,/z]anthracene
benzo [g, h, /'Jperylene
IS Ref.
#
3
3
3
3
3
3
3
3
3
3
3
3
QI (m/z)
149
107
183
183
252
252
264
252
328
276
278
276
Confirmation
Ion(s) (m/z)
167
139,219
163*
163*
126*
126*
132*
126*
329
138*
139*
138*
Comments
a,g
a
a,d,e
a,d,e
a
a
a
a
a,c,d
a
a
a
*  Confirmation ions may be at or below 30% relative abundance depending on instrument tune.
~  Compounds without values do not have qualifier ions of significant relative abundance.

Comment Key
a.  PDS solvent, acetone
b.  PDS solvent, methanol
c.  May exhibit peak tailing
d.  Potential to exhibit matrix induced chromatographic response enhancement was observed during method
   development. This assessment was done based on a peak area comparison of a standard prepared in solvent
   compared to a matrix-matched standard, both at a concentration of 0.2 ng/uL.  If the matrix-matched standard
   area was > 130% of the solvent prepared standard, the analyte was flagged as having the potential for matrix
   induced chromatographic response enhancement.
e.  Literature references 11 and 12 indicate that this compound may exhibit matrix induced response enhancement.
f  Mevinphos exists as two isomers, cis and trans that will partially or completely coelute in this method. Partial
   coelution results in distorted peak shape.
g.  Commonly occurs in LRBs
h.  MGK 264 consists of two isomers, endo and exo. In this method, a standard of mixed isomers was used.  The
   resulting chromatographic peaks have been designated by the authors as (a) and (b) throughout this document,
   where (a) is the first eluting isomer and (b) is the second eluting isomer. The amounts of each isomer listed in
   subsequent tables are based on the relative peak areas of the two isomers. Users of this method who need to
   specifically identify each isomer, must obtain and analyze standards of each isomer.
i.  Tribufos + merphos. Some fortified samples were fortified with tribufos and merphos together because of the
   configuration of standards used. Subsequent analysis of individual standards of merphos and tribufos  showed
   an identical retention time, mass spectrum and response for each compound when analyzed at the same
   concentration. The mass spectrum observed matched the NIST MS library for tribufos.
                                               525.3-66

-------
Table 2. Ion Abundance Criteria for Decafluorotriphenyl Phosphine (DFTPP)"
Mass (m/z)
68
69
70
197
198
199
365
441
442
443
Relative Abundance Criteria
< 2% of m/z 69
present
< 2% of m/z 69
<2%ofWzl98
present c
5-9% of m/z 198
>1% of base peak
< 150%ofWz443
present c
15-24% of m/z 442
Purpose of Checkpoint11
Low-mass resolution
Low-mass resolution
Low-mass resolution
Mid-mass resolution
Mid-mass resolution and sensitivity
Mid-mass resolution and isotope ratio
Baseline threshold
High-mass resolution
High-mass resolution and sensitivity
High-mass resolution and isotope ratio
a.  These ion abundance criteria have been developed specifically for target compound analysis
   as described in this method.  Adherence to these criteria may not produce spectra suitable for
   identifying unknowns by searching commercial mass spectral libraries. If the analyst intends
   to use data generated with this method to identify unknowns, adherence to stricter DFTPP
   criteria as published in previous methods22 is recommended.
b.  All ions are used primarily to check the mass accuracy of the mass spectrometer and data
   system, and this is the most important part of the performance test.  The three resolution
   checks, which include natural abundance isotope ratios,  constitute the next most important
   part of the performance test, followed by the correct setting of the baseline threshold, as
   indicated by the presence of m/z 365.
c.  Either m/z 198 or 442 is typically the base peak.
                                         525.3-67

-------
Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges; Full
Scan GC/MS Analyses"
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
87.1
102
106
96.2
105
90.1
108
103
90.9
95.4
98.2
97.0
103
NDe
119
106
91.2
105
99.1
91.7
101
109
91.8
102
119
112
95.6
107
RSD
2.8
4.6
3.6
2.0
4.6
4.6
11
1.3
7.0
5.5
3.1
13
5.6

2.1
4.8
4.2
5.9
2.9
1.4
6.8
1.1
5.5
2.7
11
13
8.3
9.4
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
95.8
108
107
87.1
102
98.5
109
106
104
96.4
96.8
94.9
102
NDe
103
106
104
123
105
99.3
105
109
97.5
101
105
99.8
107
111
RSD
2.2
6.8
5.6
6.2
7.1
2.7
6.6
7.2
2.8
5.7
3.8
5.6
4.5

12
3.5
6.0
7.4
3.7
3.6
3.9
4.5
5.0
2.9
5.6
6.3
2.3
6.3
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
88.7
95.2
102
86.4
95.0
98.4
99.9
102
89.2
89.0
90.8
90.3
92.8
92.8
99.5
94.5
88.6
92.9
99.8
105
108
96.8
94.9
106
92.7
94.4
89.8
95.5
RSD
1.7
2.0
3.0
2.0
3.0
0.66
1.3
1.1
0.75
5.1
2.4
5.9
3.3
1.3
1.4
2.5
1.9
2.2
0.86
3.8
2.6
2.0
2.4
2.6
2.0
2.3
0.39
1.0
                                      525.3-68

-------
Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges; Full
Scan GC/MS Analyses"
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
90.4
91.5
101
98.1
106
102
106
144
97.3
81.0
101
97
108
107
99.3
104
109
NDf
104
85.2
101
106
98.7
94.7
87.9
103
109
101
RSD
2.7
7.3
6.0
1.2
5.0
4.1
5.2
27
17
11
9.2
2.0
7.2
15
3.0
5.3
6.7

4.4
1.3
13
7.0
6.2
14
1.8
6.0
21
16
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
99.6
103
103
100
104
101
104
112
83.9
119
98.3
100
104
95.2
101
96.2
96.8
110
109
85.6
101
113
106
107
99.8
104
103
89.8
RSD
5.0
4.4
5.7
5.9
6.1
2.9
3.2
4.6
11
6.8
5.9
5.0
2.6
5.5
3.6
1.6
4.4
5.2
6.6
4.9
6.0
9.6
6.2
5.9
6.9
3.6
8.6
3.8
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
90.7
101
92.5
95.0
95.7
94.2
94.9
91.3
98.6
104
91.2
91.6
94.2
61.1
95.5
90.6
91.1
90.7
93.0
89.3
97.9
93.9
96.5
95.8
91.1
93.0
92.1
95.8
RSD
1.8
1.5
0.70
2.4
0.80
0.81
3.9
1.8
5.8
2.8
2.5
2.1
1.4
7.3
1.1
2.1
0.59
2.4
1.4
1.9
1.7
0.70
1.5
3.2
1.5
0.59
2.1
1.6
                                      525.3-69

-------
Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges; Full
Scan GC/MS Analyses"
Analytes
etridiazole
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges; Full
Scan GC/MS Analyses"
Analytes
pebulate
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
92.2
92.9
101
100
84.2
95.8
112
104
93.5
109
102
102
99.6
95.7
96
107
105
105
95.9
111
109
99.6
111
94.4
95.3
94.9

83.4
RSD
2.7
5.6
5.4
5.1
7.7
5.3
7.8
16
13
8.7
2.4
7.6
5.1
2.6
1.2
4.7
1.6
4.0
6.2
4.6
6.3
7.5
2.8
1.1
1.6
7.3

3.2
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
101
85.8
109
101
101
89.8
112
109
110
104
104
103
107
102
84.8
107
107
109
104
107
104
110
105
104
96.5
99.7

92.6
RSD
4.3
5.5
5.2
4.5
2.2
2.4
4.2
7.1
7.5
6.7
6.8
4.4
4.4
2.4
5.2
6.7
5.0
5.0
7.1
5.8
7.8
6.8
4.2
5.2
5.1
4.7

5.4
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
92.7
93.9
88.5
90.5
95.6
91.0
97.8
99.7
92.4
101
100
92.9
99.2
93.6
100
107
96.1
96.8
98.7
100
94.8
98.0
99.1
90.7
92.3
96.9

88.6
RSD
1.1
2.7
3.2
1.6
1.1
1.5
2.0
0.92
2.1
3.6
1.9
1.2
2.8
1.3
2.7
1.3
0.87
2.1
3.4
1.4
2.4
2.7
1.3
0.72
0.82
2.2

1.5
                                      525.3-71

-------
Table 3.  Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges;  Full
Scan GC/MS Analyses"
Analytes
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
82.4
78.5
83.4
83.2
91.2
84.3
89.9
98.2
92.5
94.5
96.1
92.2
88.5

91.5
101
102
RSD
3.0
3.5
11
6.0
5.3
4.4
7.3
6.7
5.1
4.0
5.8
0.9
4.1

3.7
4.7
2.8
Fortified Cone.
2.0 ug/Lc
n=8
Mean %
Recovery
94.0
92.2
94.1
93.6
99.4
102
98.5
98.1
99.3
98.7
103
101
107

94.0
86.5
105
RSD
4.4
4.7
4.2
6.9
4.3
3.7
5.2
4.3
4.4
5.0
4.5
4.3
3.6

2.5
3.5
3.2
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
86.2
90.8
92.5
90.3
94.6
94.5
95.0
94.6
96.2
95.1
97.6
99.1
100

91.3
91.2
88.3
RSD
1.0
2.1
2.8
1.1
1.8
1.5
0.73
0.60
1.5
1.3
0.74
2.0
3.0

1.7
3.0
1.8
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Exceptions to the stated concentration are as follows:  Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 1.0 ug/L, tebuconazole is 1.2 ug/L, c-permethrin is 0.14 ug/L, t-permethrin is 0.36 ug/L, MGK 264(a) is 0.20
   ug/L and MGK 264(b) is 0.050 ug/L.
c.  Exceptions to the stated concentration are as follows:  Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L, tebuconazole is 10.0 ug/L, c-permethrin is 1. lug/L, t-permethrin is 2.9ug/L, and MGK 264(a) is 1.6
   ug/L and MGK 264(b) is 0.40 ug/L.
d.  Exceptions to the stated concentration are as follows:  Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20.0 ug/L, tebuconazole is 25.0 ug/L, c-permethrin is 2.8 ug/L, t-permethrin is 7.2 ug/L, and MGK 264(a) is
   4.0ug/L and MGK 264(b) is 1.0 ug/L.
e.  ND = Not determined.  Analyte could not be determined because of high laboratory reagent blank values.
f.  ND = Not determined.  Analyte could not be determined because of the low concentration.
                                              525.3-72

-------
Table 4. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Oasis HLB SPE Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analysesa
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo [g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
90.5
102
104
80.3
91.8
96.5
96.5
100
99.1
91.1
93.9
95.3
97.2
NDe
89.4
102
101
110
96.9
92.0
104
105
87.9
98.1
100
97.7
102
103
92.9
RSD
1.7
3.8
6.2
3.2
6.7
1.3
1.8
2.2
4.0
4.2
3.3
5.9
2.7

2.3
4.0
1.9
4.7
3.9
4.0
3.3
4.1
3.7
3.4
2.3
3.1
3.1
2.7
2.2
Surface Water0
Mean %
Recoveryd
99.3
128
115
91.6
97.8
101
94.1
106
104
99.9
105
113
96.7
NDd
108
117
114
99.8
112
106
102
116
95.5
108
120
110
104
102
105
RSD
2.5
2.3
3.8
2.0
4.7
3.3
4.7
3.6
3.7
1.2
3.4
2.9
4.6

2.9
4.8
2.6
4.0
2.4
3.3
3.6
4.0
2.3
2.2
5.2
3.7
3.1
1.8
2.0
                                      525.3-73

-------
Table 4. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Oasis HLB SPE Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analysesa
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified
Cone. Qig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
98.7
95.2
93.7
102
103
101
101
85.6
114
94.3
96.0
90.5
94.9
97.7
93.4
100
103
102
73.0
99.4
106
94.3
107
96.1
104
97.9
87.1
98.8
101
RSD
2.8
2.8
3.5
4.5
1.7
2.9
3.7
5.8
4.5
1.6
3.0
1.2
6.7
2.7
2.0
0.40
2.6
3.1
5.1
3.2
2.8
9.1
5.2
1.2
3.7
2.4
4.0
2.0
3.0
Surface Water0
Mean %
Recoveryd
108
105
104
117
103
106
99.8
102
109
118
101
102
85.3
108
98.4
115
124
109
82.6
109
108
102
118
110
105
122
93.8
121
112
RSD
2.7
2.9
2.7
2.2
2.4
3.8
6.3
2.4
8.5
2.2
3.8
2.5
2.9
2.5
4.5
2.9
3.8
4.1
5.9
3.2
4.0
2.9
2.0
2.6
2.4
2.3
10
4.1
4.1
                                      525.3-74

-------
Table 4. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Oasis HLB SPE Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analysesa
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,t/|pyrene
isophorone
methoxychlor
methyl parathion
metolachlor
metribuzin
mevinphos
MGK 264(a)
MGK 264(b)
molinate
napropamide
nitrofen
nonachlor, trans
norflurazon
oxyfluorfen
pebulate
pentachlorophenol
permethrin, trans
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.6
0.4
2.0
2.0
2.0
2.0
2.0
2.0
2.0
8.0
1.1
Ground Water
Mean %
Recoveryd
94.9
88.8
99.1
96.3
86.8
93.8
98.6
105
100
81.5
98.5
96.0
92.4
102
102
102
89.4
94.9
98.1
97.8
91.3
103
96.8
96.7
92.5
106
95.9
81.9
95.8
RSD
1.1
3.9
2.8
2.6
2.6
1.7
2.7
4.3
1.7
2.6
3.6
4.8
1.2
1.8
o o
5.5
1.6
5.9
3.2
3.0
4.0
3.5
1.3
3.5
4.2
4.6
4.1
2.3
13
3.0
Surface Water0
Mean %
Recoveryd
100
116
111
111
110
95.1
111
113
110
95.3
108
111
106
120
108
114
92.1
116
110
110
107
112
102
107
114
112
109
96.3
107
RSD
3.8
4.4
4.3
2.9
2.8
0.6
7.2
2.6
1.8
3.0
1.9
1.1
3.2
4.4
4.2
2.7
6.2
2.9
2.7
3.6
4.7
3.3
3.4
3.6
1.7
3.0
1.9
7.3
2.9
                                      525.3-75

-------
Table 4. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Oasis HLB SPE Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analysesa
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified
Cone. (jig/L)
2.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
10.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
93.2
97.0
92.5
108
105
94.7
96.9
101
99.5
101
97.1
78.9
96.9
112
105
108
101
102
104
105
101
91.3
98.8

85.8
96.0
87.8
86.2
87.8
RSD
4.3
2.5
2.3
5.6
2.5
1.9
3.2
2.8
1.9
2.0
4.3
2.0
3.2
1.1
2.5
3.9
4.5
4.2
3.1
2.4
2.4
0.8
2.9

1.2
1.7
2.3
3.5
7.4
Surface Water0
Mean %
Recoveryd
104
99.6
96.9
103
110
88.3
100
114
114
105
100
79.9
99.8
107
106
121
106
110
109
110
116
106
99.5

97.0
99.5
96.6
94.8
100
RSD
3.3
3.7
1.5
3.4
4.3
5.5
3.7
2.8
2.7
3.5
3.2
2.9
2.0
1.2
3.3
6.5
4.7
4.4
3.7
1.9
3.2
2.6
2.9

2.3
4.4
3.3
5.2
2.8
                                      525.3-76

-------
Table 4.  Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Oasis HLB SPE Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analysesa
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
l,3-dimethyl-2-nitrobenzene (SUR)
benzo [a] pyrene-^i 2
triphenyl phosphate (SUR)
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

5.0
5.0
5.0
Ground Water
Mean %
Recoveryd
93.6
104
92.8
93.2
91.2
88.2
95.7
93.1
97.7

92.3
88.4
108
RSD
3.4
4.7
1.8
2.6
3.7
6.7
0.8
5.2
1.8

1.7
3.2
2.5
Surface Water0
Mean %
Recoveryd
105
103
103
102
102
97.5
106
103
107

97.9
88.0
103
RSD
2.7
3.7
2.1
2.0
4.4
4.2
4.2
3.1
2.5

2.8
3.9
2.7
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Tap water from a ground water source with high mineral content. Tap water hardness was 290 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.8 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
e.  ND= Not determined.  Analyte could not be determined because of high laboratory reagent blank values.
                                           525.3-77

-------
Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE Columns (Cartridges); Full Scan GC/MS Analyses'1
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
84.9
102
96.0
95.6
97.6
89.4
107
100
89.1
89.9
94.1
89.9
92.5
81.7
104
103
91.0
103
97.2
93.7
92.7
99.9
92.9
90.9
97.9
92.2
90.4
93.2
RSD
1.9
4.0
5.0
2.5
3.2
3.2
12
6.7
0.43
11
2.6
10
7.4
11
8.2
2.1
2.6
5.8
5.2
5.3
5.3
4.7
2.9
5.6
12
13
7.9
6.4
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
88.2
94.7
94.6
88.3
95.7
91.1
101
99.3
95.8
89.7
97.6
92.8
92.9
86.0
97.5
92.0
95.5
96.5
97.9
106
99.1
98.2
95.9
97.6
98.9
94.7
96.2
19.2
RSD
2.4
1.9
2.2
7.1
3.9
2.9
3.3
1.0
2.9
5.2
3.8
9.0
3.9
3.2
17
2.2
1.6
3.1
2.6
2.3
4.6
3.7
2.5
2.8
2.9
2.2
3.8
3.8
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
90.7
97.0
103
96.5
96.0
104
97.9
100
92.4
100
96.6
98.7
99.7
86.0
97.7
99.6
92.7
101
103
105
98.9
102
95.2
99.5
93.3
99.5
94.7
99.1
RSD
1.8
3.0
3.2
4.5
4.1
2.7
2.5
3.4
1.9
3.5
0.81
5.1
1.6
0.53
2.9
1.3
0.59
4.3
2.2
1.2
3.3
3.8
1.9
3.2
2.2
4.4
1.6
3.7
                                     525.3-78

-------
Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE Columns (Cartridges); Full Scan GC/MS Analyses'1
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutylphthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
86.1
91.2
98.4
90.9
99.7
95.9
96.2
NDe
85.8
94.7
94.4
94.8
88.4
85.1
97.6
98.1
ND
ND
101
90.7
98.5
98.8
98.2
86.8
88.2
97.5
85.9
79.2
RSD
3.4
8.3
1.2
4.9
4.0
4.8
7.8

14
32
5.0
7.8
5.5
17
6.7
2.5


4.4
5.5
2.6
4.2
7.5
8.6
5.7
7.0
4.2
14
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
93.8
100
98.1
93.4
99.1
97.9
101
106
89.7
105
101
98.2
98.6
36.8
96.8
92.7
97.9
95.7
95.3
73.9
95.3
91.6
97.6
101
96.5
94.0
98.6
99.9
RSD
1.7
3.0
2.9
2.5
2.0
2.1
6.2
9.1
10
4.2
2.0
3.6
1.4
6.5
1.8
o o
J.J
4.1
1.7
3.4
6.0
4.2
4.9
4.4
4.8
2.6
3.0
3.1
2.4
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
94.6
99.6
98.5
103
98.7
93.9
95.2
92.5
101
102
93.8
101
94.1
25.2
95.1
91.7
92.1
92.1
98.5
94.2
100
104
99.7
101
92.8
97.4
93.3
96.1
RSD
1.9
2.8
3.2
2.8
2.8
2.2
1.3
3.0
5.6
3.3
4.9
1.2
0.60
1.8
2.6
2.1
1.3
3.1
3.2
5.1
2.5
2.4
4.6
4.5
1.3
3.8
3.3
3.0
                                     525.3-79

-------
Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE Columns (Cartridges); Full Scan GC/MS Analyses'1
Analytes
etridiazole
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE Columns (Cartridges); Full Scan GC/MS Analyses'1
Analytes
pebulate
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
90.3
85.8
91.6
93.6
86.9
90.4
109
99.9
83.1
103
94.1
94.5
107
92.0
88.0
92.4
106
91.7
82.6
99.4
96.8
102
119
92.5
92.0
98.8

84.7
RSD
3.3
6.0
4.4
3.8
1.1
1.6
8.6
11
4.0
4.7
6.0
0.94
4.1
2.7
9.3
6.0
3.2
5.6
9.0
2.8
5.6
11
2.2
3.3
1.2
6.6

4.6
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
92.9
95.4
99.3
92.8
94.9
87.1
97.2
95.6
98.6
99.8
99.1
98.6
98.9
96.0
98.3
97.3
96.9
97.0
102
99.0
88.6
112
90.4
98.9
96.7
101

92.9
RSD
2.2
2.5
3.2
3.2
2.8
2.1
4.0
6.9
2.8
2.5
2.2
1.2
2.2
2.3
2.2
2.1
2.8
2.5
5.7
1.7
o o
J.J
3.4
2.7
1.3
2.0
3.1

2.4
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
92.5
98.5
91.2
92.2
96.3
90.0
95.2
102
90.4
99.3
95.8
96.5
97.3
100
96.4
108
94.2
95.2
97.7
100
99.1
96.4
100
93.9
94.0
97.9

90.5
RSD
2.3
4.5
2.8
1.7
2.0
1.7
2.8
4.1
4.2
2.5
1.6
0.77
3.3
2.3
1.7
3.5
1.1
2.3
3.0
3.1
3.3
4.1
3.4
0.71
0.71
3.8

0.78
                                     525.3-81

-------
Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE Columns (Cartridges); Full Scan GC/MS Analyses'1
Analytes
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
81.8
85.4
80.4
85.0
88.7
84.5
89.2
93.6
92.8
94.0
94.6
97.5
93.6

88.3
92.2
99.7
RSD
6.5
5.6
2.3
7.6
4.2
3.6
3.5
3.0
4.1
0.77
4.2
2.5
9.9

1.0
3.7
2.2
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
92.8
93.8
93.9
91.5
91.6
93.4
94.6
99.1
99.2
99.8
100
99.3
102

92.5
88.8
94.0
RSD
2.2
1.7
3.9
4.8
3.5
2.7
2.1
1.8
1.6
3.5
3.1
3.5
5.9

1.5
4.3
2.2
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
90.0
91.5
92.9
94.9
101
98.5
101
102
104
103
104
104
99.9

95.7
94.6
91.1
RSD
1.2
1.0
4.2
3.9
2.9
3.3
2.3
2.0
4.5
3.7
3.3
2.9
1.1

1.0
3.9
2.1
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 1.0 ug/L, tebuconazole is 1.2 ug/L, c-permethrin is 0.14 ug/L, t-permethrin is 0.36 ug/L, MGK 264(a) is 0.20
   ug/L and MGK 264(b) is 0.05  ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L, tebuconazole is 10.0 ug/L, c-permethrin is 1. lug/L, t-permethrin is 2.9ug/L, and MGK 264(a) is 1.6
   ug/L and MGK 264(b) is 0.4 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20.0 ug/L, tebuconazole is 25.0  ug/L, c-permethrin is 2.8 ug/L, t-permethrin is 7.2 ug/L, and MGK 264(a) is
   4.0ug/L and MGK 264(b) is 1.0 ug/L.
e.   ND = Not determined.  Analyte could not be determined because of the low concentration.
                                              525.3-82

-------
Table 6. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE Columns (Cartridges); N=4 for Each Matrix;
Full Scan GC/MS Analysesa
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo [g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Fortified
Cone. (fig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
84.8
106
108
90.6
92.2
97.7
94.2
97.3
101
105
101
121
106
96.4
104
103
100
116
99.5
92.6
101
106
84.4
97.2
89.7
104
105
108
RSD
1.5
2.2
3.4
4.0
6.5
3.2
2.7
2.4
2.6
4.8
3.1
2.4
3.5
1.6
2.2
3.1
1.6
3.9
2.4
2.8
2.6
3.9
1.0
1.8
3.3
6.4
3.2
1.2
Surface Water0
Mean %
Recoveryd
91.5
103
104
85.5
87.5
99.3
86.0
90.9
96.4
97.5
100
118
102
109
123
104
97.8
208
98.3
93.0
102
105
83.4
96.2
100
99.9
101
98.0
RSD
2.0
2.7
1.0
4.2
5.3
2.8
4.8
2.0
2.3
6.0
2.1
3.2
1.7
2.0
16
2.8
2.8
94
3.5
3.2
5.4
5.8
1.8
3.2
2.2
4.4
2.8
3.0
                                     525.3-83

-------
Table 6. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE Columns (Cartridges); N=4 for Each Matrix;
Full Scan GC/MS Analysesa
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
97.0
96.0
97.5
94.4
109
101
99.7
106
116
122
82.3
94.3
49.2
92.7
91.2
78.9
102
109
81.4
97.8
98.9
101
105
92.6
106
97.2
87.4
100
RSD
1.9
4.0
3.4
1.8
3.6
2.9
3.8
1.7
3.8
3.7
3.2
3.5
11
1.4
2.3
3.8
4.8
3.9
2.4
5.1
3.0
4.8
5.7
2.9
3.3
0.57
4.1
3.4
Surface Water0
Mean %
Recoveryd
94.4
97.8
98.2
95.0
109
97.5
123
126
102
114
92.1
94.4
34.9
94.1
87.7
96.3
111
98.2
74.5
95.8
103
98.6
110
91.9
106
93.2
88.0
103
RSD
1.3
2.0
3.4
3.7
3.5
0.63
24
29
7.2
2.7
2.0
3.5
4.6
2.7
1.9
3.1
4.7
4.7
1.9
4.0
8.3
3.7
6.2
0.36
4.1
4.3
4.8
2.4
                                     525.3-84

-------
Table 6. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE Columns (Cartridges); N=4 for Each Matrix;
Full Scan GC/MS Analysesa
Analytes
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 6. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE Columns (Cartridges); N=4 for Each Matrix;
Full Scan GC/MS Analysesa
Analytes
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
Fortified
Cone. (fig/L)
8.0
1.1
2.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
10.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
2.0
Ground Water
Mean %
Recoveryd
87.7
95.7
94.4
98.6
89.1
106
109
92.1
95.5
105
100
102
105
75.4
93.0
108
92.1
105
101
98.9
102
108
100
92.9
98.7

83.5
91.9
RSD
3.9
0.88
2.0
2.4
0.39
4.8
3.8
3.9
3.4
2.5
1.8
2.2
5.6
0.82
3.2
3.9
2.5
4.8
o o
J.J
2.7
3.7
4.0
2.6
0.68
2.7

1.0
2.6
Surface Water0
Mean %
Recoveryd
92.5
102
97.8
98.5
97.3
105
102
83.6
89.3
99.8
97.6
93.3
102
74.0
90.7
108
84.2
108
94.5
101
99.1
110
103
90.4
100

83.8
89.3
RSD
2.6
2.8
2.1
1.5
2.7
5.6
13
3.2
2.2
1.6
1.4
3.1
4.0
2.1
5.3
1.9
2.8
6.9
4.3
4.3
5.5
4.6
2.3
2.1
0.61

2.0
2.3
                                     525.3-86

-------
Table 6.  Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE Columns (Cartridges); N=4 for Each Matrix;
Full Scan GC/MS Analysesa
Analytes
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

5.0
5.0
5.0
Ground Water
Mean %
Recoveryd
85.1
89.5
91.6
96.9
93.5
95.6
93.5
92.0
93.4
97.9
97.0
89.1

83.3
94.0
104
RSD
1.8
3.9
2.6
3.6
1.9
2.6
1.6
2.5
2.7
1.2
o o
J.J
3.3

6.4
4.2
4.0
Surface Water0
Mean %
Recoveryd
87.4
90.9
88.9
96.2
93.5
96.1
92.2
94.9
93.5
101
97.2
99.0

91.4
90.5
107
RSD
1.8
2.8
2.0
2.0
2.4
2.3
3.1
3.5
4.6
2.2
2.5
4.9

0.40
2.6
1.9
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Tap water from a ground water source with high mineral content.  Tap water hardness was 342 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.8 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
                                          525.3-87

-------
Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE; Full Scan GC/MS Analyses"
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
87.9
110
107
92.7
96.6
85.6
96.4
96.8
85.6
94.5
90.2
89.5
103
50.4
102
103
91.5
91.3
106
101
106
106
95.5
96.0
77.3
101
96.5
101
RSD
1.9
4.0
5.0
2.5
3.2
3.2
12
6.7
0.43
11
2.6
10
7.4
11
8.2
2.1
2.6
5.8
5.2
5.3
5.3
4.7
2.9
5.6
12
13
7.9
6.4
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
84.6
99.4
92.5
82.2
89.5
86.7
92.1
94.2
94.0
81.3
88.6
93.0
90.1
107
99.6
95.5
87.6
121
94.9
89.6
99.3
96.7
82.0
83.8
88.7
98.7
95.4
91.8
RSD
5.1
3.5
3.8
3.8
7.3
4.3
4.9
2.6
4.9
5.9
6.5
7.5
4.7
2.6
28
2.7
3.6
5.7
4.9
5.2
2.7
4.4
6.0
5.6
11
4.2
5.2
6.7
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
90.4
105
110
104
99.2
104
100
103
90.1
94.6
94.3
96.6
94.1
85.4
106
105
95.8
108
105
104
104
107
94.3
103
102
110
94.2
106
RSD
1.8
3.1
2.4
3.5
5.7
2.4
2.0
2.9
0.88
3.5
2.5
3.8
2.8
1.8
1.8
2.0
1.4
1.5
4.3
4.4
0.78
1.7
1.8
2.5
1.4
3.0
0.73
2.5
                                     525.3-88

-------
Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE; Full Scan GC/MS Analyses"
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutylphthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
94.0
93.2
95.8
95.2
98.2
98.7
96.1
NDe
101
99.1
109
106
90.8
83.7
93.3
101
77.5
NDf
105
80.0
109
99.6
96.6
110
93.8
98.4
108
90.6
RSD
3.4
8.3
1.2
4.9
4.0
4.8
7.8

14
32
5.0
7.8
5.5
17
6.7
2.5
3.3

4.4
5.5
2.6
4.2
7.5
8.6
5.7
7.0
4.2
14
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
89.1
89.8
94.5
89.2
86.5
89.4
105
104
90.9
110
100
95.9
87.7
76.1
87.2
84.6
87.4
97.3
95.4
80.4
92.3
96.8
90.0
120
85.0
98.7
95.9
90.0
RSD
2.4
3.5
3.5
3.2
6.5
6.0
8.3
9.3
10
3.5
9.5
3.9
4.8
5.5
5.8
7.2
16
14
4.9
10
5.6
3.7
5.7
8.4
5.7
2.8
7.7
9.6
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
98.8
101
102
106
104
99.3
97.6
94.4
106
107
102
109
98.8
64.6
96.2
97.0
99.8
92.2
108
96.7
107
110
103
107
94.8
101
103
104
RSD
1.7
1.9
2.2
3.4
3.0
0.64
0.91
3.7
3.1
2.9
2.3
4.6
1.0
4.1
1.2
0.36
3.5
1.1
1.9
2.7
2.4
2.3
2.0
2.5
0.59
1.1
2.8
2.3
                                     525.3-89

-------
Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE; Full Scan GC/MS Analyses"
Analytes
etridiazole
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE; Full Scan GC/MS Analyses"
Analytes
pebulate
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
95.0
93.5
89.5
91.6
87.8
86.5
103
116
76.7
99.7
96.8
98.3
95.0
99.2
89.5
99.1
107
94.1
98.2
103
108
110
126
84.3
97.2
95.0

90.2
RSD
3.3
6.0
4.4
3.8
1.1
1.6
8.6
11
4.0
4.7
6.0
0.9
4.1
2.7
9.3
6.0
3.2
5.6
9.0
2.8
5.6
11
2.2
3.3
1.2
6.6

4.6
Fortified Cone.
2.0 jig/Lc
n=8
Mean %
Recovery
84.6
111
96.3
90.4
93.4
86.3
105
99.0
97.3
91.4
95.6
88.0
88.5
98.0
83.8
91.2
100
84.1
95.1
91.2
97.5
94.4
96.3
89.6
85.9
96.1

78.9
RSD
3.4
3.9
7.0
6.7
3.3
2.5
4.3
5.2
4.6
5.0
3.7
4.4
3.9
2.3
5.8
3.9
8.2
4.0
3.6
4.7
4.0
4.9
5.3
8.7
5.8
3.5

4.7
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
94.2
101
93.8
96.1
98.1
94.4
108
104
91.7
101
101
103
102
103
99.6
112
100
101
110
105
110
103
107
95.5
95.0
102

91.0
RSD
1.8
4.2
1.5
2.7
2.5
1.2
1.9
2.1
4.7
2.4
2.7
1.0
2.6
0.91
3.7
2.9
0.91
0.19
2.6
2.9
3.8
3.4
2.0
0.67
2.8
1.4

2.2
                                     525.3-91

-------
Table 7.  Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using J.T. Baker Speedisk HiO Phobic DVB
SPE; Full Scan GC/MS Analyses"
Analytes
4-chlorobiphenyl (3)
2,4-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified Cone.
0.25 jig/Lb
n=4
Mean %
Recovery
87.9
85.3
90.7
93.2
97.5
89.0
102
98.0
96.0
93.7
96.4
98.3
87.2

98.0
101
103
RSD
6.5
5.6
2.3
7.6
4.2
3.6
3.5
3.0
4.1
0.8
4.2
2.5
9.9

1.0
3.7
2.2
Fortified Cone.
2.0 ug/Lc
n=8
Mean %
Recovery
80.5
78.6
85.9
90.0
89.5
95.0
89.6
89.1
90.3
90.9
92.4
90.0
88.4

95.5
82.1
110
RSD
5.8
5.5
4.7
6.7
3.9
3.1
3.8
2.7
3.5
o o
J.J
2.0
5.3
6.5

3.9
3.1
3.8
Fortified Cone.
5.0 ng/Ld
n=4
Mean %
Recovery
92.7
94.2
94.9
103
108
103
106
102
105
105
103
104
95.3

102
91.9
97.0
RSD
0.82
1.5
4.0
2.1
2.4
1.7
3.6
2.4
1.6
3.4
2.8
3.5
2.2

2.4
2.2
2.1
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 1.0 ug/L, tebuconazole is 1.2 ug/L, c-permethrin is 0.14 ug/L, t-permethrin is 0.36 ug/L, MGK 264(a) is 0.20
   ug/L and MGK 264(b) is 0.05 ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L, tebuconazole is 10.0 ug/L, c-permethrin is 1. lug/L, t-permethrin is 2.9ug/L, and MGK 264(a) is 1.6
   ug/L and MGK 264(b) is 0.4 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20.0 ug/L, tebuconazole is 25.0 ug/L, c-permethrin is 2.8 ug/L, t-permethrin is 7.2 ug/L, and MGK 264(a) is
   4.0ug/L and MGK 264(b) is 1.0 ug/L.
e.   ND = Not determined. Analyte could not be determined because of the low fortified concentration relative to
    theLRB.
f.   ND = Not determined. Analyte could not be determined due to poor instrument sensitivity at this concentration.
                                              525.3-92

-------
Table 8. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE; N=4 for Each Matrix; Full Scan GC/MS
Analyses21
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo [g, h, /'Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
98.8
123
116
102
113
103
114
119
93.6
80.2
89.5
90.7
88.6
121
99.1
114
104
115
118
114
116
123
95.8
102
100
123
95.0
121
RSD
2.4
4.2
5.8
3.1
2.0
3.2
4.3
5.9
2.6
4.5
2.8
3.5
2.3
3.6
2.6
o o
J.J
4.0
2.4
7.2
4.3
3.7
2.9
2.1
4.8
5.5
2.5
6.3
4.4
Surface Water0
Mean %
Recoveryd
87.5
101
91.6
80.5
82.7
88.6
83.0
93.0
95.2
85.6
88.8
92.9
87.8
109
115
99.1
92.0
95.9
93.1
85.1
95.9
95.2
82.9
82.8
99.3
88.4
93.9
84.4
RSD
1.1
4.4
3.8
4.3
2.0
3.9
6.4
4.8
2.1
11
6.1
5.0
3.4
0.46
4.4
5.6
4.6
4.4
6.0
4.4
7.4
5.5
2.5
5.0
1.1
3.3
2.9
6.2
                                     525.3-93

-------
Table 8. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE; N=4 for Each Matrix; Full Scan GC/MS
Analyses21
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Water
Mean %
Recoveryd
105
116
119
113
112
106
112
113
90.4
132
116
126
103
98.6
103
111
87.9
110
121
91.9
121
117
112
103
100
112
112
95.4
RSD
3.2
4.2
3.4
4.1
3.5
1.9
6.4
7.4
3.8
4.2
4.2
4.0
3.8
7.0
4.1
4.7
3.7
7.9
5.1
4.8
1.7
6.1
5.1
8.8
3.1
1.4
2.3
5.7
Surface Water0
Mean %
Recoveryd
91.9
89.9
94.1
87.4
87.5
95.4
102
108
90.0
102
112
101
89.1
77.8
89.1
88.7
100
110
95.5
84.9
90.4
93.9
84.9
115
89.5
102
104
99.8
RSD
1.9
4.6
4.9
5.2
6.0
1.2
1.9
5.2
5.3
5.1
2.7
5.8
1.7
3.1
2.6
4.9
4.9
1.3
5.3
1.8
5.8
12
6.0
3.3
3.1
4.4
1.2
1.1
                                     525.3-94

-------
Table 8. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE; N=4 for Each Matrix; Full Scan GC/MS
Analyses21
Analytes
etridiazole
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 8. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE; N=4 for Each Matrix; Full Scan GC/MS
Analyses21
Analytes
pebulate
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
Fortified
Cone. (jig/L)
2.0
8.0
1.1
2.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
10.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
Ground Water
Mean %
Recoveryd
98.0
118
93.9
94.8
110
94.8
126
120
117
118
119
104
113
119
103
116
105
101
120
113
115
121
121
110
105
117

94.2
RSD
4.6
2.3
4.8
4.7
5.1
3.7
5.2
4.8
4.6
3.7
3.7
1.9
4.1
2.1
2.4
4.0
2.6
4.3
4.1
2.5
5.6
3.4
2.1
2.7
2.2
4.6

2.8
Surface Water0
Mean %
Recoveryd
84.4
110
93.4
92.7
92.2
89.1
97.6
97.7
82.6
86.2
94.6
94.2
85.2
96.8
81.6
88.3
97.8
81.9
101
85.9
95.8
93.9
102
94.8
91.0
96.1

81.3
RSD
1.7
3.8
4.8
2.5
4.0
2.4
3.9
8.0
3.5
4.9
4.4
1.3
3.2
4.3
6.7
6.5
4.2
3.7
4.7
3.6
6.0
5.4
6.1
2.7
1.1
5.1

2.0
                                     525.3-96

-------
Table 8.  Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using
J.T. Baker Speedisk H2O Phobic DVB SPE; N=4 for Each Matrix; Full Scan GC/MS
Analyses21
Analytes
4-chlorobiphenyl (3)
2,4-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

5.0
5.0
5.0
Ground Water
Mean %
Recoveryd
92.9
93.2
109
118
112
121
114
113
113
116
119
112
90.9

111
79.8
115
RSD
1.3
1.9
4.7
8.4
3.2
2.4
4.2
3.7
3.1
3.6
3.1
5.2
7.7

o o
J.J
3.4
3.7
Surface Water0
Mean %
Recoveryd
85.3
80.4
86.4
88.3
89.1
95.4
91.4
88.3
89.2
88.3
93.8
88.4
83.8

102
86.0
115
RSD
1.9
1.2
4.9
4.4
6.3
5.3
6.2
4.5
5.9
6.8
4.1
5.3
3.4

1.5
2.8
2.3
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Tap water from a ground water source with high mineral content. Tap water hardness was 342 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.8 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
                                           525.3-97

-------
Table 9. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Empore SDB-XC Disks; N=4 for Each
Concentration; Full Scan GC/MS Analyses'1
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified Cone.
0.20 jig/Lb
Mean %
Recovery
90.0
106
98.8
91.3
106
98.8
109
105
95.0
96.3
106
108
111
97.5
124
115
100
131
96.3
96.3
123
105
283
98.8
113
96.3
72.5
101
90.0
RSD
4.5
4.5
6.4
5.2
5.9
4.8
4.4
3.9
4.3
7.8
5.9
6.0
4.3
8.9
2.0
3.5
4.1
6.5
5.0
5.0
2.4
3.9
10
2.5
5.7
5.0
12
4.7
4.5
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
87.9
94.5
92.0
80.5
90.8
91.1
90.2
91.1
91.6
88.0
90.6
87.0
89.4
81.0
90.2
92.1
88.6
94.1
90.7
90.8
92.4
92.9
101
88.6
90.5
93.3
89.2
88.8
90.1
RSD
2.6
2.6
1.9
3.1
4.6
2.3
2.3
3.5
1.9
3.5
1.5
5.4
1.6
4.4
3.5
3.7
3.6
o o
J.J
2.9
3.0
3.5
3.7
4.1
2.8
3.0
3.1
5.7
5.8
0.99
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
86.4
90.0
92.3
86.6
94.3
89.4
91.8
91.6
91.0
88.9
91.9
89.4
89.4
81.7
96.4
93.2
87.1
96.3
88.8
89.3
95.9
92.9
96.6
88.4
90.2
89.6
89.4
90.5
91.6
RSD
5.4
7.6
8.2
7.1
9.2
5.7
7.3
8.0
5.1
5.9
6.2
6.9
5.6
7.0
7.2
8.0
6.9
7.4
7.9
7.3
7.0
8.4
7.1
7.3
6.7
7.3
5.2
9.0
7.1
                                      525.3-98

-------
Table 9. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Empore SDB-XC Disks; N=4 for Each
Concentration; Full Scan GC/MS Analyses'1
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified Cone.
0.20 jig/Lb
Mean %
Recovery
95.0
92.5
98.8
113
103
129
160
104
741
101
103
97.5
23.8
90.0
103
116
108
111
98.8
77.5
83.8
104
111
100
120
114
121
110
123
RSD
4.3
3.1
6.4
4.4
4.9
4.9
5.1
4.6
9.8
4.7
4.9
6.6
11
4.5
6.3
5.4
6.0
4.3
4.8
3.7
5.7
4.6
5.7
4.1
3.4
2.2
3.9
3.7
5.3
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
92.7
93.3
90.8
87.8
92.7
90.9
98.9
90.7
105
86.6
91.0
90.7
8.52
90.2
64.0
90.5
88.9
93.3
87.1
92.8
93.5
90.9
94.5
89.0
94.2
94.0
91.2
90.2
93.0
RSD
2.7
2.7
2.8
2.7
2.9
3.4
2.7
4.2
2.9
o o
J.J
3.0
3.0
9.0
3.2
3.5
2.2
o o
J.J
2.9
4.1
2.9
3.7
o o
5.5
1.8
3.1
3.1
2.5
3.0
1.7
4.9
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
89.6
88.7
90.5
92.5
90.1
96.4
102
90.2
125
88.6
90.4
88.6
6.7
87.0
67.8
90.4
90.1
92.2
85.4
89.5
91.0
90.0
93.4
88.2
93.7
92.3
93.1
87.1
95.7
RSD
7.5
7.9
7.2
7.9
7.2
9.0
8.5
7.9
7.5
6.5
7.7
7.3
11
7.4
6.1
6.7
6.7
7.3
7.2
8.1
7.3
8.1
7.0
6.8
8.1
6.5
7.8
7.1
7.3
                                      525.3-99

-------
Table 9. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Empore SDB-XC Disks; N=4 for Each
Concentration; Full Scan GC/MS Analyses'1
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 9. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Empore SDB-XC Disks; N=4 for Each
Concentration; Full Scan GC/MS Analyses'1
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified Cone.
0.20 jig/Lb
Mean %
Recovery
107
95.0
121
126
125
111
111
118
96.3
103
98.8
108
119
126
116
120
111
125
105
116
109
100
105

85.0
90.0
88.8
82.5
91.3
RSD
4.1
4.3
3.9
3.8
3.3
5.7
4.3
5.5
5.0
6.3
4.8
2.7
5.3
2.0
7.3
3.4
4.3
3.3
8.7
3.7
2.3
4.1
3.9

4.8
4.5
7.1
6.1
6.9
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
92.8
92.2
88.2
94.7
93.4
91.4
92.3
94.4
91.2
91.5
92.5
90.7
93.6
89.5
94.0
92.3
93.0
92.1
93.9
93.6
88.1
90.0
89.3

88.4
89.2
88.8
90.3
90.4
RSD
2.8
2.1
2.1
3.8
2.5
3.1
o o
J.J
3.6
2.7
3.1
2.1
o o
J.J
3.1
1.5
4.4
3.4
2.7
3.4
2.4
2.8
2.6
2.9
3.4

2.9
2.6
2.0
3.1
2.3
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
91.8
90.0
85.7
99.7
94.9
93.5
92.0
93.9
87.7
91.4
91.0
91.0
93.6
95.6
100
95.2
93.1
97.4
94.5
100
86.5
87.2
89.8

84.8
85.6
86.1
88.3
89.4
RSD
7.5
5.9
7.5
6.1
7.3
7.7
8.1
7.6
7.0
7.5
6.0
7.9
7.9
9.9
5.0
7.8
7.9
7.2
7.6
7.3
7.4
6.9
7.7

6.2
6.1
6.5
6.8
6.7
                                     525.3-101

-------
Table 9. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Empore SDB-XC  Disks; N=4 for Each
Concentration; Full Scan GC/MS Analyses'1
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.20 jig/Lb
Mean %
Recovery
91.3
95.0
91.3
93.8
97.5
90.0
93.8
95.0
88.8

93.8
79.6
86.4
RSD
6.9
4.3
6.9
6.7
6.6
4.5
5.1
4.3
5.4

3.6
3.8
5.2
Fortified Cone.
2.0 ug/Lc
Mean %
Recovery
91.1
90.6
91.1
90.6
91.2
91.3
91.1
91.2
92.5

93.3
90.2
102
RSD
3.1
2.9
2.9
2.4
2.3
3.1
3.0
1.7
1.9

3.5
2.0
4.2
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
89.9
89.6
90.5
91.1
91.4
91.1
91.5
91.6
90.9

87.9
91.2
94.9
RSD
7.6
6.6
7.0
6.5
6.7
7.6
7.0
7.6
5.2

7.1
4.2
7.3
a.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 0.80 ug/L, MGK 246(a) is 0.067 ug/L, MGK 246(b) is 0.13 ug/L, tribufos+merphos is 0.40 ug/L,
   c-permethrin is 0.12 ug/L, and t-permethrin is 0.29 ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L, MGK 246(a) is 0.67 ug/L, MGK 246(b) is 1.3 ug/L, tribufos+merphos is 4.0 ug/L, c-permethrin is
   1.2 ug/L, and t-permethrin is 2.9 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20 ug/L, MGK 246(a) is 1.7 ug/L, MGK 246(b) is 3.3 ug/L, tribufos+merphos is 10 ug/L, c-permethrin is
   2.9 ug/L, and t-permethrin is 7.2 ug/L.
                                             525.3-102

-------
Table 10. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Empore SDB-XC Disks; N=4 for Each Matrix; Full Scan GC/MS Analyses21
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
94.1
95.6
98.1
87.0
101
96.0
100
99.1
105
95.1
96.0
97.3
124
91.3
100
98.3
96.4
99.1
94.9
94.0
102
100
94.8
95.8
97.4
97.0
84.8
101
99.0
RSD
2.4
2.2
o o
J.J
1.8
2.2
2.9
3.8
3.1
2.4
3.4
2.6
4.2
3.5
3.7
3.5
2.5
3.0
3.1
2.3
2.6
3.5
3.2
1.9
3.0
2.8
2.9
2.8
2.3
3.6
Surface Water0
Mean %
Recoveryd
87.4
92.0
92.4
84.9
92.0
90.3
93.9
91.4
99.8
91.5
92.9
97.9
118
87.5
96.8
94.3
90.5
95.6
89.6
89.8
96.8
96.3
95.6
91.8
91.9
90.0
79.5
79.4
93.0
RSD
7.8
7.1
7.2
6.4
9.2
8.2
7.5
7.1
8.4
9.8
9.9
10
8.2
7.3
6.3
6.9
7.8
9.4
6.7
6.3
8.0
9.3
7.7
6.4
7.5
6.9
9.3
4.9
7.1
                                     525.3-103

-------
Table 10. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Empore SDB-XC Disks; N=4 for Each Matrix; Full Scan GC/MS Analyses21
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified
Cone. Qig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
95.4
92.8
94.9
102
97.9
97.0
109
100
106
96.8
96.8
96.1
9.0
94.5
87.3
97.5
96.1
100
91.6
95.0
93.5
96.4
104
97.3
98.3
103
96.8
99.9
106
RSD
3.2
3.1
2.7
3.6
2.7
3.1
2.9
3.3
3.0
2.6
3.2
2.6
24
3.1
3.1
2.7
2.3
3.4
2.5
3.7
2.9
4.5
o o
J.J
2.5
3.6
1.1
3.7
2.7
2.4
Surface Water0
Mean %
Recoveryd
89.4
86.5
90.0
102
92.9
93.3
104
102
96.8
90.9
92.6
89.9
8.50
88.1
76.6
93.3
90.6
94.6
81.5
90.4
88.4
91.4
101
90.6
95.6
98.9
92.9
95.8
103
RSD
7.1
7.0
6.4
7.8
7.3
10
6.3
11
7.4
7.1
6.5
8.5
25
7.9
6.5
7.6
8.0
7.2
7.2
6.3
7.5
8.1
8.0
7.6
8.1
9.5
8.4
7.4
9.4
                                     525.3-104

-------
Table 10. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Empore SDB-XC Disks; N=4 for Each Matrix; Full Scan GC/MS Analyses21
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 10. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Empore SDB-XC Disks; N=4 for Each Matrix; Full Scan GC/MS Analyses21
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified
Cone. (jig/L)
2.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
4.0
2.0
2.0
2.0

2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
101
93.0
96.0
105
100
99.3
102
101
96.4
98.4
95.5
98.5
99.8
110
105
104
101
105
102
95.9
95.0
95.9
93.0

93.3
93.1
93.3
94.8
94.6
RSD
2.9
2.7
2.8
3.7
2.7
3.1
3.2
3.0
3.0
2.8
2.9
o o
J.J
3.4
4.5
3.9
2.2
2.7
3.6
3.7
3.2
3.5
3.1
3.1

2.9
2.4
2.9
3.1
3.4
Surface Water0
Mean %
Recoveryd
96.9
87.5
90.9
101
96.3
92.6
90.8
95.9
91.1
91.4
91.0
91.0
92.6
112
96.1
99.4
95.3
100
96.6
91.4
90.5
89.5
88.4

86.1
86.5
87.0
87.3
88.6
RSD
9.1
7.8
7.0
7.3
8.5
7.5
7.3
6.9
8.0
7.1
7.8
6.3
6.7
9.8
9.3
5.9
7.5
7.0
7.2
7.0
7.9
7.6
6.6

8.0
8.0
8.4
8.7
7.3
                                     525.3-106

-------
Table 10. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Empore SDB-XC Disks; N=4 for Each Matrix; Full Scan GC/MS Analyses21
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

5.0
5.0
5.0
Ground Waterb
Mean %
Recoveryd
94.5
94.3
95.5
94.9
95.0
94.3
95.1
94.1
97.3

96.6
95.0
100
RSD
2.6
3.0
2.7
2.8
2.7
2.9
2.8
2.9
2.7

2.7
4.0
2.7
Surface Water0
Mean %
Recoveryd
89.0
88.8
89.6
88.8
89.3
89.0
89.6
90.5
90.6

89.2
91.0
91.2
RSD
7.6
7.1
8.1
7.7
8.1
8.0
7.1
8.7
8.0

7.8
11
8.4
a.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
b.  Tap water from a ground water source with high mineral content.  Tap water hardness was 334 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.8 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
                                          525.3-107

-------
Table 11. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4
for Each Concentration; Full Scan GC/MS Analyses21
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
101
99.0
100
77.0
105
106
112
111
112
109
119
112
105
NDe
102
107
85.0
122
98.0
103
113
82.0
93.0
116
109
102
117
99.0
102
RSD
2.0
3.9
7.3
5.0
4.8
3.8
2.9
3.5
5.1
5.5
5.0
2.9
1.9

9.3
3.6
7.1
1.9
5.3
1.9
1.8
9.3
2.2
2.8
3.5
5.1
1.7
3.9
3.9
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
93.6
93.6
89.8
78.4
93.1
92.3
90.3
96.1
99.1
103
102
102
103
ND
98.9
86.3
83.0
95.9
102
103
110
99.8
92.0
106
93.1
93.4
97.1
88.1
87.4
RSD
0.51
2.1
0.72
2.9
1.3
1.0
4.1
3.2
3.8
1.7
1.2
4.3
2.4

0.86
1.1
2.2
3.7
2.5
2.3
2.5
5.1
2.9
3.8
2.5
3.3
1.7
4.9
1.0
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
99.8
104
92.8
85.0
95.8
104
96.8
97.3
112
111
114
113
113
ND
103
99.4
84.0
114
101
96.6
111
94.1
100
105
98.6
97.2
114
106
88.8
RSD
0.88
2.1
1.0
3.4
1.1
0.71
2.2
1.5
3.6
1.2
2.4
2.8
3.1

2.1
1.4
3.0
3.6
1.3
0.71
3.9
1.3
1.4
1.5
1.1
2.5
2.1
2.4
1.2
                                      525.3-108

-------
Table 11. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4
for Each Concentration; Full Scan GC/MS Analyses21
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
105
107
99.0
116
103
112
137
110
115
104
103
111
24.0
110
112
126
121
106
79.0
95.0
103
112
89.0
89.0
106
110
117
118
110
RSD
3.6
3.6
3.9
2.8
1.9
4.1
3.7
3.6
3.3
3.1
1.9
1.8
14
3.6
5.8
1.8
1.7
2.2
2.5
5.3
1.9
7.1
5.7
2.2
2.2
2.1
4.3
3.4
4.7
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
102
85.8
82.3
87.6
98.3
96.6
97.6
95.4
101
91.6
87.4
111
29.5
113
90.0
105
106
95.1
91.5
88.4
89.6
96.5
82.9
88.0
100
91.3
97.6
90.6
87.1
RSD
3.5
0.75
1.3
2.8
3.2
3.1
1.3
2.5
1.5
1.7
0.55
2.3
6.5
0.25
1.9
2.6
0.71
0.90
8.9
1.3
3.5
2.4
3.4
0.80
2.7
1.6
2.3
2.2
2.0
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
101
105
101
112
104
111
110
109
114
88.8
98.1
114
24.9
113
93.7
113
111
97.8
85.3
101
103
106
91.3
85.8
108
96.2
105
101
91.7
RSD
1.7
1.4
1.0
0.83
2.0
1.8
2.4
1.5
2.6
2.7
0.39
1.4
2.5
0.78
3.0
2.5
0.67
0.69
1.5
1.0
1.0
0.75
4.0
0.60
3.1
1.4
3.5
1.5
3.4
                                      525.3-109

-------
Table 11. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4
for Each Concentration; Full Scan GC/MS Analyses21
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 11. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4
for Each Concentration; Full Scan GC/MS Analyses21
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
115
94.0
94.0
88.0
105
129
119
106
129
85.0
104
110
115
94.0
94.0
88.0
105
129
119
106
129
85.0
104

75.0
85.0
85.0
104
81.0
RSD
3.3
2.5
2.5
3.7
3.6
3.0
3.2
2.2
1.6
8.0
4.1
3.6
3.3
2.5
2.5
3.7
3.6
3.0
3.2
2.2
1.6
8.0
4.1

2.7
2.4
2.4
3.1
2.5
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
96.1
75.5
82.8
89.4
89.9
106
103
91.9
93.9
84.5
100
107
96.1
75.5
82.8
89.4
89.9
106
103
91.9
93.9
84.5
100

81.0
84.4
82.5
89.3
88.6
RSD
3.1
1.9
0.35
1.2
2.4
2.7
2.3
1.6
2.9
1.7
1.3
1.3
3.1
1.9
0.35
1.2
2.4
2.7
2.3
1.6
2.9
1.7
1.3

2.6
2.8
2.2
2.9
3.3
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
97.0
88.3
92.3
88.9
99.2
113
96.2
102
111
84.7
96.0
107
97.0
88.3
92.3
88.9
99.2
113
96.2
102
111
84.7
96.0

85.0
88.9
87.1
95.3
92.4
RSD
1.5
4.1
0.80
2.1
1.5
3.9
1.0
1.6
3.5
2.4
3.6
2.2
1.5
4.1
0.80
2.1
1.5
3.9
1.0
1.6
3.5
2.4
3.6

1.1
1.5
0.51
4.0
0.48
                                      525.3-111

-------
Table 11.  Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4
for Each Concentration;  Full Scan GC/MS Analyses21
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
85.0
84.0
84.0
81.0
90.0
86.0
87.0
79.0
101

92.9
112
107
RSD
9.7
3.9
3.9
2.5
2.6
4.7
5.8
2.5
2.0

4.0
2.1
2.5
Fortified Cone.
2.0 ug/Lc
Mean %
Recovery
91.1
90.3
92.4
94.3
94.5
99.0
96.5
96.9
93.1

98.9
101
97.9
RSD
3.1
4.4
3.4
3.2
3.7
3.2
4.3
2.8
2.9

3.1
2.6
4.1
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
93.4
96.4
97.0
97.1
98.8
105
101
101
91.6

88.8
101
104
RSD
1.6
1.1
0.94
0.90
1.1
1.3
1.2
1.1
2.2

4.0
4.9
3.2
a.  Data obtained on the instrumentation described in Sect. 13.1.1.4.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 1.0 ug/L, c-permethrin is 0.13 ug/L, t-permethrin is 0.38 ug/L, MGK 264 (a) is 0.085 ug/L and MGK 264 (b)
   is 0.17  ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L, c-permethrin is 1.0 ug/L, t-permethrin is 3.0 ug/L, MGK 264 (a) is 0.67 ug/L and MGK 264 (b) is
   1.3 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20.0  ug/L, c-permethrin is 2.5 ug/L, and t-permethrin is 7.5 ug/L, MGK 264 (a) is 1.7 ug/L and MGK 264 (b)
   is 3.3 ug/L.
e.  ND = Not determined. Analyte could not be determined because of the low fortified concentration relative to the
   LRB.
                                             525.3-112

-------
Table 12. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
99.3
97.4
93.5
94.9
98.9
102
92.6
100
104
106
104
101
103
95.5
98.9
96.4
87.6
107
96.1
94.5
93.1
101
104
108
95.9
97.8
106
97.4
92.3
RSD
5.7
5.5
3.5
4.0
5.7
4.7
5.9
4.6
1.5
3.2
3.3
3.9
3.0
1.2
5.5
2.9
3.2
4.1
6.2
5.9
3.9
5.6
2.0
1.5
5.6
5.3
2.2
5.2
5.6
Surface Water0
Mean %
Recoveryd
95.1
106
95.0
81.1
93.4
101
87.3
95.6
102
100
100
101
101
114
104
95.6
83.6
107
98.0
98.3
111
97.1
108
110
98.1
103
100
91.0
95.1
RSD
1.8
4.9
3.3
0.59
6.2
1.6
5.3
1.5
2.4
2.7
3.9
5.3
2.6
1.9
4.6
3.3
1.8
2.9
5.9
7.3
3.4
4.3
4.0
2.2
2.4
4.1
3.2
11
1.6
                                     525.3-113

-------
Table 12. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified
Cone. Qig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
92.1
93.1
90.0
91.4
101
102
107
106
110
90.4
96.0
110
29.4
111
89.6
95.6
95.6
98.5
79.6
96.9
98.5
102
97.9
89.0
95.8
94.9
97.6
104
93.5
RSD
7.3
3.7
3.6
3.7
1.8
5.8
2.7
6.2
3.7
7.3
5.4
2.5
8.7
2.4
5.9
7.0
6.2
5.6
5.9
7.0
5.7
2.8
2.6
7.2
6.9
5.7
5.9
2.4
4.4
Surface Water0
Mean %
Recoveryd
107
91.0
85.6
90.4
109
106
104
102
107
88.8
96.3
107
38.1
111
99.6
105
101
101
103
93.0
94.3
100
88.1
85.8
98.9
103
103
104
86.6
RSD
4.3
2.0
2.7
3.5
1.1
3.4
2.2
2.2
1.5
2.3
2.6
1.1
4.2
1.0
5.9
4.1
5.0
2.3
6.3
4.5
4.1
2.1
3.4
3.0
4.3
3.9
3.0
3.1
3.3
                                     525.3-114

-------
Table 12. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 12. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified
Cone. (jig/L)
3.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
4.0
2.0
2.0
2.0

2.0
2.0
2.0
2.0
2.0
Ground Waterb
Mean %
Recoveryd
91.4
106
95.5
100
98.4
96.9
98.8
95.1
106
101
106
101
98.6
94.4
88.5
101
97.3
97.5
99.3
96.6
90.8
88.0
98.6

90.8
96.1
97.9
101
101
RSD
7.1
3.7
2.0
3.3
4.4
2.1
4.9
5.5
1.4
2.8
1.2
3.7
4.2
5.4
7.1
5.6
5.1
6.6
2.1
7.3
2.2
6.0
7.0

1.7
0.65
0.87
3.8
2.2
Surface Water0
Mean %
Recoveryd
100
104
98.9
114
108
88.4
94.6
96.6
110
96.4
107
96.1
87.9
96.0
101
95.8
87.4
104
101
107
90.0
88.3
111

96.3
99.9
86.6
90.9
86.1
RSD
2.3
2.5
4.8
2.8
1.7
5.7
4.9
3.4
3.4
2.5
2.2
3.0
3.8
5.2
1.8
10
5.1
5.4
3.0
2.0
4.5
1.8
1.7

5.6
5.4
6.3
7.5
4.9
                                     525.3-116

-------
Table 12. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

5.0
5.0
5.0
Ground Waterb
Mean %
Recoveryd
93.0
97.1
107
107
108
110
106
108
99.6

91.7
103
104
RSD
3.0
3.1
1.5
1.3
1.2
2.0
1.4
0.89
1.0

7.5
2.7
0.58
Surface Water0
Mean %
Recoveryd
88.1
87.8
88.1
92.0
91.3
93.8
91.5
91.3
87.6

89.0
104
112
RSD
6.9
6.6
5.2
6.3
6.4
5.3
6.0
6.3
7.2

6.5
3.0
3.5
a.  Data obtained on the instrumentation described in Sect. 13.1.1.4.
b.  Tap water from a ground water source with high mineral content.  Tap water hardness was 300 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.4 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
                                          525.3-117

-------
Table 13. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Horizon Atlantic DVB Disks; N=5 for
Each Concentration; Full Scan GC/MS Analyses21
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /'Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
87.3
92.3
95.6
85.6
91.4
87.2
93.2
94.5
93.6
88.9
87.9
88.3
91.1
89.8
96.9
94.9
86.9
104
92.1
91.2
89.1
96.0
89.7
89.0
93.7
89.1
90.7
101
90.0
RSD
3.4
4.0
8.0
1.2
3.5
4.6
5.2
7.4
2.5
3.5
3.6
4.2
3.8
5.0
1.9
5.0
2.4
19
6.5
5.0
7.7
4.0
4.2
4.8
7.7
2.6
2.3
8.6
4.9
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
86.6
93.9
93.4
84.7
93.9
90.2
94.9
92.9
90.6
85.8
85.1
79.8
85.9
84.9
94.3
91.5
88.0
94.5
89.2
89.4
94.0
93.8
90.9
94.3
92.5
91.3
92.0
108
89.6
RSD
1.1
2.6
2.0
5.7
2.9
2.2
5.3
2.9
2.1
3.0
3.0
3.9
2.7
1.5
2.8
2.8
2.4
3.9
4.9
4.2
4.3
4.4
1.4
1.6
2.3
3.2
2.6
3.3
1.7
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
90.5
95.2
94.6
90.4
95.8
92.9
98.5
95.0
91.3
88.2
89.0
84.5
87.2
87.6
96.6
93.0
91.5
93.6
89.7
88.9
95.3
92.4
93.6
97.3
95.8
94.4
90.9
114
92.4
RSD
1.3
1.4
1.4
1.2
1.5
1.4
2.4
1.9
1.7
3.9
4.0
3.8
3.9
1.2
3.6
2.4
1.5
1.2
2.5
2.3
2.4
1.9
1.3
2.3
0.75
2.1
1.4
3.7
0.32
                                     525.3-118

-------
Table 13. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Horizon Atlantic DVB Disks; N=5 for
Each Concentration; Full Scan GC/MS Analyses21
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
93.9
91.0
83.9
88.8
91.6
84.1
NDe
85.3
ND
93.2
93.6
93.6
36.0
89.4
89.9
88.6
89.3
93.8
71.0
87.9
94.8
95.1
88.1
85.8
96.1
91.9
92.9
84.6
99.8
RSD
3.3
3.4
4.3
6.0
5.5
8.6

5.0

4.4
9.2
5.4
13
5.3
5.3
5.8
5.7
3.2
5.0
9.2
5.8
4.8
2.1
3.5
4.3
4.1
7.8
6.7
5.9
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
94.3
91.8
87.9
88.3
92.9
76.2
77.0
76.7
111
86.7
91.3
91.4
32.8
90.0
83.9
92.1
89.1
94.7
77.4
89.6
91.5
93.4
92.5
86.2
93.5
92.1
88.8
88.8
95.9
RSD
2.1
3.4
6.8
4.2
2.0
3.3
2.7
3.7
2.2
0.98
6.2
2.2
25
1.0
2.7
1.4
2.1
2.1
4.9
o o
J.J
6.7
2.7
4.7
0.96
3.9
2.7
3.1
1.4
3.7
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
96.0
88.3
85.6
86.4
94.5
76.5
72.7
81.5
95.0
89.3
91.1
94.2
28.4
92.6
86.8
97.0
94.0
96.2
77.8
91.1
90.6
93.4
93.0
90.5
92.7
95.7
93.4
92.3
100
RSD
1.2
1.8
3.0
2.4
0.82
3.1
2.8
4.5
0.96
2.3
2.8
0.90
9.6
1.0
1.8
1.3
0.67
1.4
4.8
1.4
3.0
1.7
2.3
1.8
2.8
0.71
2.8
1.1
3.4
                                     525.3-119

-------
Table 13. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Horizon Atlantic DVB Disks; N=5 for
Each Concentration; Full Scan GC/MS Analyses21
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 13. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Horizon Atlantic DVB Disks; N=5 for
Each Concentration; Full Scan GC/MS Analyses21
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
89.3
88.6
83.7
98.3
92.0
90.0
94.0
92.3
88.8
95.5
92.2
93.9
95.1
93.2
95.4
91.4
96.5
95.6
94.5
82.0
91.0
87.3
94.3

85.3
88.2
87.1
89.4
84.4
RSD
3.2
3.9
4.2
6.5
8.6
3.8
2.0
4.0
5.2
3.3
4.3
3.8
2.1
5.3
11
6.1
5.1
4.9
2.4
5.2
5.8
2.5
8.5

5.2
4.0
5.8
2.5
6.8
Fortified Cone.
2.0 jig/Lc
Mean %
Recovery
82.3
90.1
88.8
95.2
93.7
93.9
98.9
93.5
91.5
93.5
91.8
94.2
93.8
94.7
91.3
94.5
93.7
92.3
96.1
95.8
91.2
87.0
94.7

87.2
88.1
90.8
91.0
90.6
RSD
2.2
2.4
2.3
2.9
2.8
3.2
3.9
1.7
2.8
2.6
3.8
1.8
2.8
2.0
9.5
1.9
3.0
3.1
o o
J.J
4.4
2.1
1.1
4.6

1.8
1.3
2.0
2.9
3.1
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
83.2
92.6
91.1
95.5
94.7
96.0
102
96.1
94.7
95.7
92.3
98.7
95.4
97.0
99.6
96.2
95.5
93.0
96.7
93.7
95.9
90.7
94.9

90.0
92.0
92.5
92.0
90.8
RSD
2.0
1.7
0.97
2.0
4.2
0.79
2.2
1.9
0.89
0.55
2.1
2.9
1.0
2.3
8.9
2.9
1.5
2.8
2.6
1.6
0.75
1.8
2.2

0.53
1.1
0.43
0.54
0.41
                                     525.3-121

-------
Table 13.  Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent
Water at Three Concentrations and Extracted Using Horizon Atlantic DVB Disks; N=5 for
Each Concentration;  Full Scan GC/MS Analyses21
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.25 jig/Lb
Mean %
Recovery
87.2
89.4
87.8
87.1
85.5
85.9
84.3
83.1
81.9

86.4
89.6
87.8
RSD
7.5
5.4
8.3
3.2
3.4
5.7
6.6
4.4
6.0

4.0
3.5
2.6
Fortified Cone.
2.0 ug/Lc
Mean %
Recovery
89.6
88.8
88.3
90.5
89.0
88.6
88.0
87.7
87.1

86.2
93.5
93.3
RSD
2.8
2.2
5.0
4.1
4.3
3.9
4.5
4.7
4.5

1.9
5.1
2.9
Fortified Cone.
5.0 ng/Ld
Mean %
Recovery
90.3
89.4
89.4
88.5
84.3
86.4
86.7
85.1
86.5

88.0
98.9
99.9
RSD
1.7
2.7
1.7
3.4
4.1
2.8
3.6
4.6
2.9

0.92
4.2
1.8
a.  Data obtained on the instrumentation described in Sect. 13.1.1.3.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 1.0 ug/L, MGK 264 (a) is 0.200 ug/L and MGK 264 (b) is 0.050 ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 8.0 ug/L,, MGK 264 (a) is 1.6 ug/L and MGK 264 (b) is 0.4 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 ug/L, pentachlorophenol
   is 20.0 ug/L,, MGK 264 (a) is 4.0 ug/L and MGK 264 (b) is 1.0 ug/L.
e.  ND = Not determined. Analyte could not be determined because of high laboratory reagent blank values relative
   to the fortification concentration.
                                             525.3-122

-------
Table 14. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /Jperylene
benzo [k] fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis-
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
cycloate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Synthetic Hard Waterb
Mean %
Recoveryd
90.9
98.7
96.9
93.3
90.8
95.3
85.8
92.2
92.1
87.4
85.7
79.1
87.9
92.6
95.4
93.5
95.0
92.8
89.0
89.7
95.2
94.3
95.6
97.1
97.1
95.2
94.8
98.7
94.4
RSD
2.2
0.47
1.2
3.4
4.2
2.2
5.7
3.2
2.4
2.3
3.6
1.6
o o
5.5
1.6
4.2
3.6
2.0
3.2
1.7
1.6
4.1
4.1
1.2
1.9
1.4
2.5
2.7
7.1
2.3
Surface Water0
Mean %
Recoveryd
92.1
97.0
95.0
93.2
90.0
94.8
88.2
93.3
91.9
86.8
85.8
78.4
85.1
93.8
96.1
93.4
95.8
92.5
89.8
90.3
95.1
93.2
95.6
97.8
97.4
95.0
91.8
97.4
94.5
RSD
1.8
2.6
1.6
2.9
3.2
1.6
4.5
0.82
1.7
2.4
3.0
6.1
3.5
2.4
2.7
2.1
3.4
1.9
2.3
1.3
2.3
1.7
1.5
1.6
2.0
2.2
2.3
5.4
2.0
                                     525.3-123

-------
Table 14. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
etridiazole
fenarimol
Fortified
Cone. Qig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Synthetic Hard Waterb
Mean %
Recoveryd
97.5
86.5
83.6
82.4
99.3
72.1
73.0
75.8
116
90.0
90.4
96.7
45.0
94.3
84.6
93.4
92.9
95.5
80.0
68.1
90.6
92.6
90.6
93.0
92.8
99.1
95.4
96.1
98.7
RSD
1.7
3.5
1.7
2.1
2.4
1.4
3.6
2.1
2.3
3.6
4.9
2.3
24
1.8
3.5
5.6
3.3
2.6
5.1
2.7
6.2
3.2
3.4
2.0
3.2
2.1
1.9
2.6
4.5
Surface Water0
Mean %
Recoveryd
98.0
87.5
84.2
82.5
99.3
73.4
74.7
75.2
114
91.4
88.3
96.4
34.8
95.2
88.3
98.2
95.5
95.2
73.4
59.4
89.7
92.1
93.0
94.6
89.3
98.7
96.3
95.1
94.4
RSD
0.56
1.4
2.6
0.57
2.9
2.0
3.1
6.3
1.0
2.2
1.8
1.1
17
1.9
5.1
3.0
1.1
1.8
10
7.7
4.8
2.4
2.5
2.0
1.1
2.6
6.8
2.8
1.8
                                     525.3-124

-------
Table 14. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,
-------
Table 14. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
2.0
2.0
2.0
2.0
Synthetic Hard Waterb
Mean %
Recoveryd
80.1
93.8
92.0
92.7
94.2
87.4
93.3
95.7
97.1
93.8
93.0
91.8
88.4
97.0
97.7
96.1
92.4
91.7
97.6
95.2
100
92.6
97.5

90.8
91.8
94.9
95.2
93.6
RSD
2.9
1.2
1.5
5.3
2.9
6.1
4.5
2.3
2.8
1.8
2.5
2.7
3.8
2.3
6.1
2.0
5.4
3.9
3.9
3.7
1.8
2.4
1.1

2.0
2.3
2.0
2.2
1.9
Surface Water0
Mean %
Recoveryd
79.1
94.3
93.0
94.6
95.7
86.1
91.5
96.4
96.3
93.0
93.7
92.9
89.6
96.8
98.8
96.5
89.6
91.8
93.8
93.5
99.1
94.0
97.6

92.0
92.4
95.0
94.4
92.9
RSD
1.8
2.3
4.1
1.7
2.0
3.6
2.8
1.7
1.3
3.0
1.4
2.7
3.4
2.4
8.0
2.6
4.2
3.1
4.2
2.3
2.0
2.5
3.9

2.4
3.2
2.7
1.8
3.4
                                     525.3-126

-------
Table 14. Precision and Accuracy Data Obtained for Method Analytes Fortified into
Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using
Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses'1
Analytes
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-c/i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0

2.0
2.0
2.0
Synthetic Hard Waterb
Mean %
Recoveryd
94.4
91.1
87.8
86.6
83.3
82.6
82.5
81.5
79.3

88.7
94.1
92.2
RSD
3.8
3.6
1.2
1.3
2.9
1.8
2.0
1.8
2.6

2.9
2.4
1.8
Surface Water0
Mean %
Recoveryd
92.1
91.4
89.4
88.0
86.9
84.7
85.9
83.4
81.3

90.6
93.4
92.4
RSD
2.1
2.5
1.2
1.8
1.7
2.2
2.8
2.9
1.6

3.8
3.2
1.7
a.  Data obtained on the instrumentation described in Sect. 13.1.1.3.
b.  A synthetic hard water sample was prepared as described in Sect. 16, Reference 33 by adding calcium carbonate,
   magnesium carbonate, and sodium bicarbonate to tap water.  The resulting synthetic hard water was > 350 mg/L
   as calcium carbonate.
c.  Tap water from a surface water source. TOC of 2.6 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
                                           525.3-127

-------
Table 15. DLs and LCMRLs (ug/L) Calculated from Replicate Analyses of Fortified
Reagent Water Samples Analyzed in Full Scan GC/MS Mode
Analytes
acenaphthylene
acetochlor
alachlor
aldrin
ametryn
anthracene
atraton
atrazine
benzo [a] anthracene
benzo[a]pyrene
benzo[6]fluoranthene
benzo \g, h, /Jperylene
benzo[&]fluoranthene
BHT
bromacil
butachlor
butylate
butylbenzylphthalate
chlordane, cis
chlordane, trans
chlorfenvinphos
chlorobenzilate
chloroneb
chlorothalonil
chlorpropham
chlorpyrifos
chrysene
cyanazine
Laboratory 1
Oasis HLB SPEab
DL
0.015
0.037
0.035
0.056
0.038
0.018
0.016
0.030
0.021
0.043
0.031
0.021
0.048
0.092
NDe
0.028
0.024
0.068
0.10
0.027
0.095
0.034
0.068
0.036
0.026
0.091
0.017
0.032
Fortified
cone, of
DL
replicates
0.050
0.050
0.10
0.10
0.050
0.050
0.10
0.050
0.050
0.050
0.050
0.10
0.050
0.10

0.050
0.050
0.10
0.10
0.050
0.10
0.050
0.10
0.10
0.050
0.10
0.050
0.050
LCMRL
NCd
0.19
0.25
0.30
0.17
0.12
0.12
0.29
0.12
0.18
0.14
0.31
0.18
0.32
0.31
0.39
0.16
0.40
0.33
0.28
0.52
0.30
0.16
0.17
0.21
0.45
0.15
0.33
Laboratory 2
Empore PSDVB SPEC
DL
0.0029
0.011
0.0084
0.010
0.017
0.0078
0.0055
0.010
0.0062
0.035
0.013
0.011
0.026
0.0064
0.037
0.0043
0.0053
0.016
0.0094
0.010
0.0062
0.0042
0.19
0.0074
0.013
0.026
0.010
0.19
Fortified
cone, of
DL
replicates
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.050
0.025
0.025
0.025
0.050
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.050
0.050
LCMRL
0.028
0.054
0.097
0.420
0.12
0.059
0.12
0.086
0.043
0.11
0.11
0.047
0.190
0.50
0.10
0.089
0.089
0.20
0.068
0.043
0.098
0.091
0.90
0.11
0.14
0.076
0.035
0.15
                                     525.3-128

-------
Table 15. DLs and LCMRLs (ug/L) Calculated from Replicate Analyses of Fortified
Reagent Water Samples Analyzed in Full Scan GC/MS Mode
Analytes
cycloate
dacthal (DCPA)
ODD, 4,4'-
DDE, 4,4'-
DDT, 4,4'-
DEET
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dibenzo[a,/z]anthracene
dibutyl phthalate
dichlorvos
dieldrin
diethylphthalate
dimethipin
dimethylphthalate
DIMP
dinitrotoluene, 2,4-
dinitrotoluene, 2,6-
diphenamid
disulfoton
endosulfan I
endosulfan II
endosulfan sulfate
endrin
EPTC
ethion
ethoprop
ethyl parathion
Laboratory 1
Oasis HLB SPEab
DL
0.039
0.018
0.019
0.033
0.036
0.019
0.079
ND
0.014
ND
0.021
0.064
0.037
0.045
0.026
0.039
0.026
0.056
0.033
0.12
0.039
0.14
0.068
0.045
0.037
0.010
0.13
0.15
Fortified
cone, of
DL
replicates
0.050
0.050
0.050
0.050
0.050
0.050
0.10
0.050
0.050
0.050
0.050
0.10
0.050
0.050
0.050
0.050
0.050
0.10
0.050
0.10
0.050
0.10
0.10
0.050
0.050
0.050
0.10
0.10
LCMRL
0.27
0.44
0.35
0.32
0.25
0.14
0.38
0.29
0.30
0.88
0.46
0.28
0.074
0.27
0.11
0.19
0.23
0.31
0.29
0.12
0.62
0.38
0.39
0.40
0.13
0.29
0.39
0.46
Laboratory 2
Empore PSDVB SPEC
DL
0.018
0.0055
0.0031
0.0023
0.022
0.0042
0.013
0.020
0.014
0.13
0.0051
0.017
0.018
ND
0.0048
0.0036
0.0076
0.053
0.010
0.0066
0.015
0.024
0.025
0.033
0.0048
0.013
0.0048
0.013
Fortified
cone, of
DL
replicates
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.075
0.025
0.025
0.050
0.050
0.050
0.050
0.025
0.025
0.025
0.050
LCMRL
0.14
0.040
0.092
0.088
0.12
0.066
0.083
0.40
0.14
1.4
0.081
0.084
0.13
NC
0.046
>5.0
0.19
0.20
0.089
0.11
0.11
NC
0.12
0.12
0.068
0.13
0.12
0.19
                                     525.3-129

-------
Table 15. DLs and LCMRLs (ug/L) Calculated from Replicate Analyses of Fortified
Reagent Water Samples Analyzed in Full Scan GC/MS Mode
Analytes
etridiazole
fenarimol
fluorene
fluridone
HCCPD
HCH, a
HCH, (3
HCH, 5
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
hexazinone
indeno[l,2,3-c,c/|pyrene
isophorone
methoxychlor
methyl parathion
metolachlor
metribuzin
mevinphos
MGK 264(a)
MGK 264(b)
molinate
napropamide
nitrofen
nonachlor, trans
norflurazon
oxyfluorfen
Laboratory 1
Oasis HLB SPEab
DL
0.024
0.10
0.016
0.11
0.012
0.036
0.10
0.019
0.036
0.034
0.039
0.016
0.025
0.11
0.014
0.024
0.036
0.019
0.036
0.035
0.072
0.023
0.062
0.077
0.093
0.035
0.057
0.037
Fortified
cone, of
DL
replicates
0.050
0.10
0.050
0.10
0.050
0.050
0.10
0.050
0.050
0.050
0.10
0.050
0.050
0.10
0.050
0.050
0.050
0.050
0.050
0.10
0.080
0.020
0.10
0.10
0.10
0.050
0.10
0.050
LCMRL
0.24
0.28
0.08
0.33
0.24
0.31
0.24
0.31
0.24
0.27
0.11
0.40
0.26
0.40
0.11
0.23
0.28
0.11
0.076
0.21
0.32
0.09
0.29
0.44
0.39
0.35
0.26
0.34
Laboratory 2
Empore PSDVB SPEC
DL
0.012
0.041
0.0058
0.045
0.0066
0.0037
0.021
0.015
0.014
0.0032
0.0053
0.0094
0.012
0.039
0.0043
0.0064
0.0088
0.0042
0.0070
0.0040
0.0026
0.0096
0.0036
0.025
0.042
0.0062
0.062
0.015
Fortified
cone, of
DL
replicates
0.025
0.050
0.025
0.050
0.025
0.025
0.050
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.050
0.025
0.025
0.025
0.025
0.025
0.025
0.050
0.050
0.025
0.050
0.050
LCMRL
0.17
0.20
0.051
0.27
0.084
0.062
0.11
0.099
0.078
0.029
0.063
0.087
0.14
0.20
0.063
0.061
0.16
0.14
0.11
0.093
0.031
0.083
0.074
0.11
0.13
0.049
0.14
0.28
                                     525.3-130

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Table 15. DLs and LCMRLs (ug/L) Calculated from Replicate Analyses of Fortified
Reagent Water Samples Analyzed in Full Scan GC/MS Mode
Analytes
pebulate
pentachlorophenol
permethrin, cis
permethrin, trans
phenanthrene
phorate
phosphamidon
profenofos
prometon
prometryn
pronamide
propachlor
propazine
pyrene
simazine
simetryn
tebuconazole
tebuthiuron
terbacil
terbutryn
tetrachlorvinphos
triadimefon
tribufos+merphos
trifluralin
vernolate
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
Laboratory 1
Oasis HLB SPEab
DL
0.020
0.060
0.015
0.031
0.025
0.032
0.040
0.11
0.065
0.021
0.017
0.029
0.023
0.013
0.023
0.037
0.24
0.027
0.082
0.029
0.048
0.053
0.12
0.027
0.038
0.029

0.021
Fortified
cone, of
DL
replicates
0.050
0.20
0.028
0.072
0.10
0.050
0.10
0.10
0.10
0.050
0.050
0.050
0.050
0.050
0.050
0.050
0.50
0.050
0.10
0.050
0.10
0.050
0.10
0.050
0.050
0.050

0.050
LCMRL
0.20
0.56
0.13
0.10
0.097
0.20
0.23
0.31
0.22
0.24
0.13
0.27
0.20
0.17
0.12
0.28
2.1
0.21
0.41
0.18
0.35
0.35
0.53
0.28
0.11
0.34

0.14
Laboratory 2
Empore PSDVB SPEC
DL
0.0053
0.069
0.0026
0.012
0.0069
0.052
0.0029
0.055
0.010
0.012
0.0077
0.0076
0.0065
0.0045
0.0059
0.013
0.053
0.060
0.039
0.0051
0.0042
0.048
0.013
0.019
0.0051
0.016

0.0061
Fortified
cone, of
DL
replicates
0.025
0.025
0.025
0.025
0.025
0.050
0.025
0.050
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.050
0.075
0.075
0.025
0.025
0.050
0.025
0.025
0.025
0.050

0.025
LCMRL
0.040
0.16
0.036
0.087
0.51
0.15
0.11
0.11
0.12
0.10
0.13
0.068
0.055
0.062
0.083
0.12
0.18
0.13
0.13
0.093
0.14
0.11
0.18
0.12
0.080
0.12

0.054
                                     525.3-131

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Table 15.  DLs and LCMRLs (ug/L) Calculated from Replicate Analyses of Fortified
Reagent Water Samples Analyzed in Full Scan GC/MS Mode
Analytes
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Laboratory 1
Oasis HLB SPEab
DL
0.019
0.024
0.024
0.036
0.029
0.043
0.043
0.026
0.046
0.19
0.020
0.029
0.058
Fortified
cone, of
DL
replicates
0.050
0.050
0.050
0.050
0.050
0.10
0.050
0.050
0.050
0.10
0.050
0.050
0.10
LCMRL
0.24
0.18
0.086
0.069
0.23
0.092
0.30
0.36
0.36
0.41
0.37
0.38
0.31
Laboratory 2
Empore PSDVB SPEC
DL
0.0059
0.0037
0.028
0.0073
0.0079
0.0055
0.0044
0.0030
0.0050
0.0071
0.0039
0.0033
0.0066
Fortified
cone, of
DL
replicates
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
0.025
LCMRL
0.065
0.088
0.14
0.036
0.041
0.078
0.046
0.084
0.095
0.058
0.056
0.092
0.036
a.  DL calculated from eight replicates.
b.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
c.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
d.  NC= Not calculated.  A sufficient number of data points were not available to calculate a valid LCMRL.
e.  ND= Not determined.  DLs were not determined when a response was not detected in all replicates at a given
   concentration, or when a high background concentration or an interference was present that prevented accurate
   quantitation at the fortified concentration.
                                             525.3-132

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Table 16. Example SIM Parameters for Selected Method Analytes
SIM
Segment
# 1
#2
#3
#4
#5
#6
#7
#8
#9
# 10
#11
Compound
l,3-dimethyl-2-nitrobenzene (SUR)
HCCPD
acenaphthene-
-------
 Table 16. Example SIM Parameters for Selected Method Analytes
SIM
Segment
#12
# 13
#14
#15
# 16
#17
Compound
profenofos
tribufos
oxyfluorfen
2,3,3',4',6-pentachlorobiphenyl
endrin
2,2',3,4',5',6-hexachlorobiphenyl
2,3',4,4',5-pentachlorobiphenyl
toxaphene, peak 1
2,2',4,4',5,5'-hexachlorobiphenyl
toxaphene, peak 2
toxaphene, peak 3
2,2',3,4,4',5'-hexachlorobiphenyl
tebuconazole
di(2-ethylhexyl)adipate
triphenyl phosphate (SUR)
chrysene-^2 (IS #3)
methoxychlor
2,2',3,4,4',5,5'-heptachlorobiphenyl
toxaphene, peak 4
di(2-ethylhexyl)phthalate
c-permethrin
t-permethrin
benzo(a)pyrene-<5?i2 (SUR)
benzo(a)pyrene
RT
(min)
20.77
20.91
21.02
21.03
21.46
21.57
21.68
21.74
22.18
22.47
22.67
22.81
23.12
23.17
23.26
24.03
24.18
24.44
24.55
24.72
26.42
26.60
27.90
28.03
Qi
(m/z)
339
57
252
326
263
360
326
159
360
305
159
360
125
129
77
240
227
394
159
149
183
183
264
252
Confirmation
Ion(s) (m/z)
97, 139
169
361
254, 256
81,281
218,290
254, 256
125, 305*
218,290
125
125, 305*
218,290
83, 250
57,70
169, 325
236*
-
252, 324
125, 305*
167
163*
163*
132*
126*
Dwell
Time
(ms)
45
50
50
75
125
125
Scan
Time
(sec/scan)
0.61
0.60
0.60
0.55
0.57
0.57
* Confirmation ions may be at or below 30% relative abundance depending on instrument tune.
                                         525.3-134

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Table 17. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified in
Reagent Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges;
SIM GC/MS Analyses21
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
tribufos
vinclozolin
Fortified Cone.
0.025 jig/Lb
n=4
Mean %
Recovery
103
114
117
81.0
110
89.9
NDe
ND
91.5
97.5
89.4
102
112
104
104
108
90.2
113
114
104
98.9
114
79.0
91.5
94.6
102
85.2
82.6
96.2
93.1
RSD
1.8
2.7
5.7
4.8
4.1
1.4


4.1
6.1
19
7.6
5.6
6.9
9.3
3.8
9.6
8.4
1.0
5.7
2.8
12
7.9
9.7
2.5
8.4
12
7.4
7.8
4.4
Fortified Cone.
0.10 fig/Lc
n=4
Mean %
Recovery
109
112
118
103
102
99.4
114
113
108
105
109
108
114
110
99.9
103
95.3
116
115
109
96.4
115
96.3
113
104
92.0
101.3
116.0
101.2
110
Mean %
Recovery
1.9
1.1
3.6
2.2
2.9
5.3
4.2
33
7.4
3.7
3.2
1.2
o o
5.5
2.0
3.4
4.6
2.1
2.8
4.3
2.3
5.5
5.2
6.7
3.2
2.0
2.3
13.0
1.9
3.5
2.0
Fortified Cone.
0.25 jig/Ld
n=4
Mean %
Recovery
105
104
111
97.4
100
100
111
118
112
100
112
100
99.6
100
89.2
98.2
90.6
104
107
109
99.9
124
97.2
105
103
112
124
117
105
104
RSD
2.2
3.1
1.8
7.5
3.0
2.8
1.7
7.8
3.2
1.6
1.7
4.3
4.5
6.2
2.7
3.3
2.7
1.6
1.7
1.4
3.4
6.3
2.0
2.0
1.5
1.7
1.9
0.69
3.9
2.4
                                     525.3-135

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Table 17.  Precision and Accuracy Data Obtained for Selected Method Analytes Fortified in
Reagent Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges;
SIM GC/MS Analyses21
Analytes
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.025 jig/Lb
n=4
Mean %
Recovery

99.9
96.8
109
101
90.8
94.5
97.0
88.3
92.0
86.2
86.7
95.3
86.8
99.7

101
87.9
103
RSD

2.7
4.8
12
6.1
10.0
4.2
4.6
15
3.7
8.8
3.7
4.7
2.0
9.5

2.2
3.0
1.9
Fortified Cone.
0.10 fig/Lc
n=4
Mean %
Recovery

106
105
110
106
105
108
105
103
99.9
96.5
96.1
97.4
98.7
97.6

105
92.1
106
Mean %
Recovery

1.1
1.0
7.1
3.0
1.7
5.7
1.3
6.5
4.9
3.7
4.4
3.1
0.79
4.3

3.6
2.4
3.2
Fortified Cone.
0.25 jig/Ld
n=4
Mean %
Recovery

98.8
109
102
99.9
101
98.5
101
100
99.2
97.6
96.3
95.4
97.2
95.7

93.6
94.5
101
RSD

2.6
1.8
2.4
0.82
1.3
3.1
2.5
2.5
1.6
2.5
1.5
2.3
1.4
2.0

4.4
8.8
1.4
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 0.10 ug/L, tebuconazole is 0.12 ug/L, c-permethrin is 0.014 ug/L, and t-permethrin is 0.036 ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 0.40 ug/L, tebuconazole is 0.50 ug/L, c-permethrin is 0.056 ug/L, and t-permethrin is 0.144 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 1.0 ug/L, tebuconazole is  1.02 ug/L, c-permethrin is 0.14 ug/L, and t-permethrin is 0.36 ug/L.
e.  ND = Not determined. Analyte could not be determined because of the low concentration relative to the LRB.
                                              525.3-136

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Table 18. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using Oasis HLB SPE Cartridges; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
tribufos
Fortified
Cone. (jig/L)
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.40
0.06g
0.14h
0.10
0.10
0.50
0.10
Ground Water
Mean %
Recoveryd
109
110
112
86.3
98.1
101
116
NDf
96.0
112
111
122
111
100
90.9
96.5
90.4
116
112
120
93.3
122
90.5
106
101
107
101
115
107
RSD
9.6
5.9
11
2.7
3.4
4.3
7.4

7.4
4.4
9.6
7.4
8.4
5.5
5.9
4.5
4.9
4.1
6.3
7.2
3.8
6.5
8.2
5.0
3.6
3.5
10
5.6
5.9
Surface Water0
Mean %
Recoveryd
NAe
112
101
104
97.9
102
114
ND
103
107
102
82.8
84.5
108
85.3
103
83.8
128
NA
NA
NA
123
94.9
102
108
110
105
99.9
110
RSD

3.6
0.45
7.6
3.9
3.7
4.8

18
3.3
3.6
7.3
7.2
4.6
5.8
1.4
3.3
1.3



4.6
0.88
5.1
3.0
6.8
3.0
4.5
3.5
                                     525.3-137

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Table 18.  Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using Oasis HLB SPE Cartridges; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
0.10

0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10

1.0
1.0
1.0
Ground Water
Mean %
Recoveryd
103

87.8
104
110
93.0
97.2
96.8
94.2
95.4
92.8
91.5
101
93.6
92.1
92.1

106
84.4
103
RSD
8.3

9.6
6.4
5.9
4.0
6.1
3.9
4.4
4.9
4.6
5.6
4.6
4.4
4.8
3.7

5.4
2.6
2.7
Surface Water0
Mean %
Recoveryd
104

95.8
96.5
90.0
92.7
91.4
81.6
95.3
98.8
97.5
92.3
96.9
96.6
94.5
92.6

95.3
100
106
RSD
4.2

4.5
3.5
4.9
3.2
2.1
5.2
5.0
0.85
3.0
3.0
3.5
1.5
0.86
2.1

5.7
5.6
2.0
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Tap water from a ground water source with high mineral content.  Tap water hardness was 393 mg/L as calcium
   carbonate.
c.  Tap water from a surface water source. TOC of 2.0 mg/L.
d.  Recoveries have been corrected to reflect the native amount in the unfortified matrix water.
e.  NA = Not analyzed. Matrix sample was not fortified with this analyte.
f.  ND = Not determined. Recovery could not be determined because high LRB concentrations were observed
   relative to the fortified concentration.
g.  The concentration in ground water is as listed in the table.  The concentration in surface water is 0.030 ug/L.
h.  The concentration in ground water is as listed in the table.  The concentration in surface water is 0.070 ug/L.
                                             525.3-138

-------
Table 19. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified in
Reagent Water at Three Concentrations and Extracted Using J.T. Baker HiO Phobic
Speedisks; SIM GC/MS Analyses"
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
tribufos
vinclozolin
Fortified Cone.
0.025jig/Lb
n=4
Mean %
Recovery
99.0
111
106
89.6
100
100
102
NDe
86.0
105
104
85.8
101
102
96.7
103
94.7
104
104
110
99.5
107
99.5
97.0
95.8
109
105
125
95.0
89.2
RSD
1.7
2.3
5.0
2.4
1.3
0.60
1.1

9.9
3.6
4.1
5.1
2.0
1.8
3.2
2.0
2.1
2.9
1.5
13
1.0
1.4
1.4
5.0
2.5
1.7
0.71
2.8
5.2
6.7
Fortified Cone.
0.10 fig/Lc
n=4
Mean %
Recovery
98.7
100
98.6
93.3
98.0
96.5
94.9
ND
105
105
101
86.6
96.8
96.3
90.6
99.3
88.0
101
101
95.7
97.3
107
93.6
95.6
95.5
105
99.7
114
96.9
82.7
Mean %
Recovery
1.9
1.1
6.0
2.9
2.4
2.5
5.1

6.9
1.5
2.7
3.5
2.0
3.3
3.4
1.9
2.2
4.0
2.3
2.6
2.6
5.7
2.4
5.4
5.1
3.6
5.1
4.1
4.3
6.3
Fortified Cone.
0.25 jig/Ld
n=4
Mean %
Recovery
98.8
100
99.3
91.8
99.2
97.5
96.2
ND
98.8
104
98.0
87.4
96.2
97.0
89.9
101
91.2
101
101
96.1
97.4
105
92.8
93.1
96.0
105
100
112
98.7
87.1
RSD
0.67
1.0
1.2
2.3
1.6
1.6
2.8

1.5
0.76
1.0
1.3
2.0
2.1
1.5
1.9
1.8
2.1
1.3
1.3
1.6
2.2
1.6
2.4
2.1
1.5
0.74
2.3
1.2
6.6
                                     525.3-139

-------
Table 19.  Precision and Accuracy Data Obtained for Selected Method Analytes Fortified in
Reagent Water at Three Concentrations and Extracted Using J.T. Baker HiO Phobic
Speedisks; SIM GC/MS Analyses"
Analytes
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3 ',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified Cone.
0.025jig/Lb
n=4
Mean %
Recovery
96.4
97.3
95.0
97.2
94.8
98.4
96.5
97.6
98.7
97.9
101
96.8
95.9
92.8

96.2
89.0
100
99.0
RSD
1.6
1.7
1.8
2.0
1.2
2.2
2.2
1.8
1.4
1.5
1.1
1.3
1.0
1.5

2.5
2.2
2.6
1.7
Fortified Cone.
0.10 fig/Lc
n=4
Mean %
Recovery
94.5
93.4
93.2
94.6
92.9
94.3
93.6
95.7
95.0
95.4
91.9
94.7
94.2
87.9

96.4
92.0
101
98.7
Mean %
Recovery
2.8
2.5
2.9
2.7
2.3
2.3
2.4
2.4
2.3
2.5
2.3
2.4
2.4
2.1

1.2
1.8
2.0
1.9
Fortified Cone.
0.25 jig/Ld
n=4
Mean %
Recovery
95.3
93.2
92.4
93.7
94.8
95.5
95.2
96.8
96.1
96.3
94.6
95.2
94.5
87.1

95.4
91.6
100
98.8
RSD
2.9
1.1
1.8
1.5
1.3
1.7
1.5
3.6
1.4
1.7
2.8
1.7
1.9
2.6

2.4
2.1
2.9
0.67
a.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
b.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 0.10 ug/L, c-permethrin is 0.014 ug/L, and t-permethrin is 0.036 ug/L.
c.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 0.40 ug/L, c-permethrin is 0.058 ug/L, and t-permethrin is 0.14 ug/L.
d.  Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 ug/L, pentachlorophenol
   is 1.0 ug/L, c-permethrin is 0.14 ug/L, and t-permethrin is 0.36 ug/L.
e.  ND = Not determined. Matrix spike recovery could not be determined due to the low fortification concentration
   relative to the background concentration.
                                              525.3-140

-------
Table 20a. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using J.T. Baker H2O Phobic Speedisks; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
tribufos
Fortified
Cone. (jig/L)
NAd
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
NA
NA
NA
0.10
0.40
0.058
0.14
0.10
0.10
0.50
0.10
Ground Water
Mean %
Recoveryd

90.4
112
84.8
91.0
90.4
67.0
NDe
69.6
95.3
91.0
82.4
90.9
88.2
90.6
93.8
87.3
98.9



100
90.2
87.1
86.3
96.8
84.9
109
95.9
RSD

6.6
5.3
5.1
4.5
4.1
7.9

9.7
4.2
4.4
8.9
4.2
4.8
5.1
4.3
5.6
5.6



6.2
5.5
4.5
4.9
5.5
7.1
5.6
9.0
Surface Water0
Mean %
Recovery °

104
125
83.1
98.4
98.5
81.0
NDe
70.8
108
109
163
96.9
91.9
101
104
90.8
121



141
89.0
108
105
119
97.2
138
117
RSD

1.4
0.94
6.1
1.8
1.8
8.2

6.7
2.9
1.8
4.2
1.7
0.73
1.3
1.5
1.9
1.8



1.3
1.8
4.3
3.5
2.1
2.7
2.5
3.2
                                     525.3-141

-------
Table 20a. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using J.T. Baker H2O Phobic Speedisks; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
0.10

0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10

1.0
5.0
1.0
Ground Water
Mean %
Recoveryd
90.3

85.8
85.3
87.0
90.2
87.7
87.7
87.3
84.1
84.8
83.6
77.4
81.6
76.9
67.9

102
119
99.1
RSD
4.9

4.7
4.8
4.7
2.2
4.3
3.9
4.0
3.6
3.4
2.4
2.6
2.7
2.9
4.4

1.0
2.0
3.4
Surface Water0
Mean %
Recovery °
104

88.1
89.1
89.9
90.4
91.0
89.9
90.8
88.2
88.7
88.1
79.9
84.7
77.8
67.9

109
112
110
RSD
1.5

1.4
1.7
1.8
1.3
1.8
2.0
1.8
2.1
2.2
3.1
4.3
3.6
4.7
8.7

0.60
5.0
2.6
a.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
b.  Tap water from a ground water source with high mineral content. Tap water hardness was 325 mg/L as calcium
   carbonate, TOC was 0.73 mg/L.
c.  Tap water from a surface water source. Tap water hardness was 137 mg/L as calcium carbonate, TOC was 2.52
   mg/L.
d.  NA = Not analyzed. Matrix sample was not fortified with this analyte.
e.  ND = Not determined. Recovery could not be determined because high LRB concentrations were observed
   relative to the fortified concentration.
                                           525.3-142

-------
Table 20b.  Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using J.T. Baker H2O Phobic Speedisks; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
tribufos
Fortified
Cone. (jig/L)
NAd
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
NA
NA
NA
0.50
2.0
0.15
0.35
0.10
0.50
2.5
0.50
Ground Water
Mean %
Recoveryd

90.8
90.5
92.3
92.5
91.9
73.5
NDe
72.3
96.1
91.7
89.1
92.4
91.3
92.8
94.6
89.3
99.7



93.0
92.3
81.1
82.2
93.3
82.8
96.5
91.4
RSD

1.1
0.85
2.8
1.1
0.98
1.1

6.0
1.3
1.6
2.2
1.4
1.0
1.2
1.4
1.7
1.3



0.83
1.3
1.4
0.97
2.1
1.0
1.3
1.0
Surface Water0
Mean %
Recovery °

95.8
92.1
79.6
94.6
94.1
76.3
NDe
69.7
102
97.7
114
92.6
90.7
97.7
97.6
90.0
104



107
89.7
86.1
84.9
99.4
85.0
103
98.0
RSD

3.3
3.7
6.6
2.8
2.6
9.9

7.8
3.0
2.9
1.6
3.6
3.0
2.3
2.7
3.2
2.6



2.7
2.8
4.4
3.8
3.0
3.3
2.7
2.5
                                     525.3-143

-------
Table 20b. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified
into Finished Drinking Waters from Ground and Surface Water Sources, and Extracted
Using J.T. Baker H2O Phobic Speedisks; N=4 for Each Matrix; SIM GC/MS Analyses'1
Analytes
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Surrogate Analytes
1 , 3 -dimethyl-2 -nitrobenzene
benzo [a] pyrene-^i 2
triphenyl phosphate
Fortified
Cone. (jig/L)
0.50

0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50

1.0
5.0
1.0
Ground Water
Mean %
Recoveryd
91.3

89.7
87.7
89.7
90.9
90.6
90.5
90.2
90.6
88.5
86.1
80.6
83.5
79.1
71.0

103
117
102
RSD
1.0

1.8
1.9
1.9
1.5
1.1
1.1
1.4
1.7
2.2
1.2
0.86
0.84
0.82
0.72

0.65
2.6
1.8
Surface Water0
Mean %
Recovery °
94.7

87.8
87.5
89.4
90.2
90.8
90.0
90.1
88.8
86.6
86.0
78.9
81.5
76.1
64.9

108
112
112
RSD
2.7

4.7
3.7
3.3
3.0
2.9
3.1
2.9
3.2
3.7
3.2
3.1
3.0
3.2
2.8

0.93
5.1
0.84
a.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
b.  Tap water from a ground water source with high mineral content. Tap water hardness was 325 mg/L as calcium
   carbonate, TOC was 0.73 mg/L.
c.  Tap water from a surface water source. Tap water hardness was 137 mg/L as calcium carbonate, TOC was
   2.52 mg/L.
d.  NA = Not analyzed. Matrix sample was not fortified with this analyte.
e.  ND = Not determined. Recovery could not be determined because high LRB concentrations were observed
   relative to the fortified concentration.
                                           525.3-144

-------
Table 21.  Precision and Accuracy Data for Toxaphene Extracted from Fortified Reagent
Water; Sample Extracts Analyzed in SIM GC/MS Mode
Sorbent
Oasis-HLBa
J.T. Baker H2O Phobic
cartridge3
J.T. Baker H2O Phobic
Speediskb
Empore SDB-XC3
UCT 525 Universal
Cartridge3
Fortified Cone.
l.Ofig/L
n=4
Mean %
Recovery
82.9
100
114
107
NAC
RSD
5.0
3.63
1.0
5.3

Fortified Cone.
lOfig/L
n=4
Mean %
Recovery
101
104
103
111
111
RSD
3.3
3.8
3.4
2.1
1.8
Fortified Cone.
25u£/L
n=4
Mean %
Recovery
89.5
98.5
98.5
101
NA
RSD
8.8
1.7
2.8
0.15

a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
c.  NA = Not analyzed. Data using the UCT 525 Universal cartridge was obtained at a single concentration of
   10 ug/L.
Table 22.  Precision and Accuracy Data for Toxaphene Extracted from Fortified Drinking
Water Samples; Sample Extracts Analyzed in SIM GC/MS Mode
Sorbent
Oasis-HLBc
J.T. Baker H2O Phobic
cartridge0
J.T. Baker H2O Phobic
Speediskd
Empore SDB-XCC
Ground Water a
Fortified Cone.
10 jig/L, n=4
Mean % Recovery
95.4
102
120
106
RSD
3.7
5.6
2.4
4.6
Surface Water b
Fortified Cone.
10 jig/L, n=4
Mean % Recovery
94.2
103
124
104
RSD
5.9
3.5
1.9
0.46
a.  Tap water from a ground water source with high mineral content.  Hardness was determined to be 323-360 mg/L
   as calcium carbonate.
b.  Tap water from surface water sources.  Fortified water samples extracted on Oasis-HLB cartridges had a TOC of
   2.05 mg/L. Fortified water samples extracted on other sorbents had a TOC of 3.12 mg/L.
c.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
d.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
                                            525.3-145

-------
Table 23. DLs and LCMRLs Calculated from Replicate Analyses of Fortified Reagent Water
Samples Extracted on Oasis HLB Cartridges, and LCMRLs Calculated from Replicate
Analyses of Fortified Reagent Water Samples Extracted on J.T. Baker HiO Phobic Speedisks,
All Samples Analyzed in SIM Mode, All concentrations in ug/L
Analytes
acetochlor
alachlor
atrazine
benzo[a]pyrene
chlordane, cis
chlordane, trans
di(2-ethylhexyl)adipate
di(2-ethylhexyl)phthalate
dimethipin
endrin
ethoprop
HCCPD
HCH, a
HCH, y (lindane)
heptachlor
heptachlor epoxide
hexachlorobenzene
methoxychlor
metolachlor
molinate
nonachlor, trans
oxyfluorfen
pentachlorophenol
permethrin, cis
permethrin, trans
profenofos
simazine
tebuconazole
Oasis HLBa
DLC
0.0047
0.0045
0.0062
0.0069
0.0016
0.0028
NDd
ND
0.0093
0.0081
0.0082
0.0055
0.0068
0.0040
0.0034
0.0026
0.0092
0.0025
0.0035
0.0057
0.0029
0.0038
0.047
0.0041
0.0080
0.0081
0.010
0.042
Fortified cone, of
DL replicates
0.010
0.010
0.010
0.010
0.010
0.010


0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.100
0.006
0.014
0.010
0.025
0.12
LCMRL
0.011
0.016
0.023
0.036
0.0073
0.0097
0.38
0.43
0.022
0.014
0.036
0.014
0.021
0.031
0.010
0.017
0.014
0.021
0.019
0.010
0.0061
0.035
0.068
0.012
0.020
0.029
0.048
0.20
Baker Speedisk"
LCMRL
0.0091
0.013
0.015
0.0060
0.0039
0.0020
0.020
ND
0.065
0.011
0.0084
0.0026
0.0040
0.0071
0.0024
0.0031
0.0065
0.0011
0.004
0.029
0.0066
0.031
0.0086
0.0015
0.0023
0.012
0.018
0.037
                                     525.3-146

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Table 23.  DLs and LCMRLs Calculated from Replicate Analyses of Fortified Reagent Water
Samples Extracted on Oasis HLB Cartridges, and LCMRLs Calculated from Replicate
Analyses of Fortified Reagent Water Samples Extracted on J.T. Baker HiO Phobic Speedisks,
All Samples Analyzed in SIM Mode, All concentrations in ug/L
Analytes
toxaphene
tribufos
vinclozolin
PCB congeners (by IUPAC#)
2-chlorobiphenyl (1)
4-chlorobiphenyl (3)
2,4'-dichlorobiphenyl (8)
2,2',5-trichlorobiphenyl (18)
2,4,4'-trichlorobiphenyl (28)
2,2',3,5'-tetrachlorobiphenyl(44)
2,2',5,5'-tetrachlorobiphenyl(52)
2,3 ',4',5-tetrachloroobiphenyl (70)
2,3,3',4',6-pentachlorobiphenyl (1 10)
2,3',4,4',5-pentachlorobiphenyl (118)
2,2',3,4,4',5'-hexachlorobiphenyl(138)
2,2',3,4',5',6-hexachlorobiphenyl(149)
2,2',4,4',5,5'- hexachlorobiphenyl (153)
2,2',3,4,4',5,5'-heptachlorobiphenyl(180)
Oasis HLBa
DLC
0.32
0.0033
0.0064

0.0024
0.0049
0.0045
0.0038
0.0056
0.0063
0.0027
0.013
0.0030
0.0077
0.0081
0.0063
0.0092
0.0029
Fortified cone, of
DL replicates
1.0
0.010
0.010

0.010
0.010
0.010
0.010
0.010
0.010
0.010
0.025
0.010
0.010
0.010
0.010
0.010
0.010
LCMRL
1.4
0.023
0.0098

0.0080
0.0073
0.023
0.013
0.014
0.025
0.0078
0.036
0.0092
0.013
0.016
0.012
0.013
0.015
Baker Speedisk"
LCMRL
NFe
0.0063
0.095

0.0063
0.0056
0.0022
0.0012
0.0084
0.0020
0.0012
0.0022
0.0035
0.0026
0.015
0.0021
0.0038
0.0026
a.  Data obtained on the instrumentation described in Sect. 13.1.1.1.
b.  Data obtained on the instrumentation described in Sect. 13.1.1.2.
c.  DL calculated from eight replicates.
d.  ND = Not determined. DLs and LCMRLs were not determined when a high background concentration or an
   interference was present that prevented accurate quantitation at the fortified concentration.
e.  NF = Not fortified.
                                          525.3-147

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Table 24. Initial Demonstration of Capability (IDC) and Quality Control (QC) Requirements (Summary)
Method
Reference
Sect. 9.2.1
& 9.3.1
Sect. 9.2.2
Sect. 9.2.3
Sect. 9.2.4
Sect. 9.2.5
&9.3.9
Requirement
Initial Demonstration of
Low Background
Initial Demonstration of
Precision (IDP)
Initial Demonstration of
Accuracy (IDA)
Minimum Reporting
Limit (MRL)
Confirmation
Calibration Confirmation,
Quality Control Sample
(QCS)
Specification and Frequency
Analyze LRB prior to any other IDC steps. When a new
lot of SPE media is obtained, verify that background is
at acceptable limits.
Analyze 4-7 replicate LFBs fortified near the midrange
calibration concentration.
Calculate average recovery for replicates used in IDP.
Fortify, extract and analyze 7 replicate LFBs at the
proposed MRL concentration. Calculate the mean,
standard deviation and HRPIR for each analyte. Confirm
that the upper and lower limits for the Prediction
Interval of Result (Upper PIR, and Lower PIR, Sect.
9.2.4.2) meet the recovery criteria.
Analyze a standard from a second source (QCS) to
verify the initial calibration curve.
Acceptance Criteria
Demonstrate that the method analytes are < 1/3 the
MRL, and that possible interferences from
extraction media do not prevent the identification
and/or quantification of any analytes, SURs or ISs.
Note: This includes the absence of interferences at
both the QIs and confirmation ions at the RTs of
interest.
%RSDmustbe<20%
Mean recovery ± 30% of the true value for all
analytes except dimethipin, HCCPD and HCB
which must be within 60-130% of the true value
Upper PIR < 150%
Lower PIR > 50%
± 30% of the expected value.
 NOTE: Table 24 is intended as an abbreviated summary of QC requirements provided as a convenience to the method user. Because the information has been
 abbreviated to fit the table format, there may be issues that need additional clarification, or areas where important additional information from the method text
 is needed. In all cases, the full text of the QC in Sect. 9 supersedes any missing or conflicting information in this table.
                                                                525.3-148

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Table 25.  Ongoing Quality Control (QC) Requirements (Summary)
  Method
  Reference
Requirement
Specification and Frequency
Acceptance Criteria
                Sample Holding Time
                          14 days for most analytes with appropriate preservation
                          and storage as described in Sects. 8.1-8.3. See Sect 8.4
                          for exceptions.	
                                                     Sample results are valid only if samples are
                                                     extracted within sample hold time.
                Extract Holding Time
                          28 days stored at -5 °C and protected from light
                                                     Sample results are valid only if extracts are
                                                     analyzed within extract hold time.
  Sect. 9.3.1
Laboratory Reagent Blank
(LRB)
One LRB with each extraction batch of up to 20 Field
Samples.
Demonstrate that the method analyte concentration
is < V3 the MRL, and confirm that possible
interferences do not prevent quantification. If the
background concentration exceeds V3the MRL,
results for the extraction batch are invalid.
  Sect. 9.3.3
Laboratory Fortified
Blank (LFB)
One LFB is required for each extraction batch of up to
20 Field Samples. Rotate the fortified concentrations
between low, medium, and high amounts.
Results of LFB analyses at medium and high
fortifications must be ± 30% of the true value for all
analytes except dimethipin, HCCPD and HCB
which may be 60-130% of the true value. Results
of the low-level LFB must be ± 50% of the true
value.
  Sect. 9.3.5
Internal Standard (IS)
Compare IS area to the mean IS area from the analysis
of each C AL in the initial calibration and the area in the
most recent CCC.
Peak area counts for all ISs in all injections must be
within ± 50% of their mean peak area calculated
during the initial calibration.  Peak areas of ISs 1-3
must also be ± 30% from the most recent CCC. If
the ISs do not meet these criteria, target analyte
results are invalid.  Consult Sect. 9.3.5 for further
information.
  Sect. 9.3.6
Surrogate (SUR)
Standards
The SUR standards are added to all calibration standards
and samples, including QC samples prior to extraction.
Calculate SUR recoveries.
SUR recovery must be ± 30% of the true value. If
any SUR fails this criterion, report all results for
sample as suspect/SUR recovery.
  Sect. 9.3.7
Laboratory Fortified
Sample Matrix (LFSM)
Analyze one LFSM per extraction batch (of up to 20
Field Samples) fortified with the method analytes at a
concentration close to but greater than the native
concentration. Calculate LFSM recoveries.
See Sect. 9.3.7.3 for instructions on the
interpretation of LFSM results.
                                                                   525.3-149

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Table 25.   Ongoing Quality Control (QC) Requirements (Summary) (Continued)
  Sect. 9.3.8
Laboratory Fortified
Sample Matrix Duplicate
(LFSMD) or Field
Duplicates (FD)
Extract and analyze at least one FD or LFSMD with
each extraction batch of up to 20 Field Samples.  An
LFSMD may be substituted for a FD when the
frequency of detects for analytes  of interest are low.
Calculate RPDs.
Method analyte RPDs for the LFSMD or FD should
be < 30% at mid and high levels of fortification and
< 50% at concentrations within 2 times the MRL.
Failure to meet this criterion may indicate a matrix
effect.
  Sect. 9.3.9
Quality Control Sample
(QCS)
Analyze a QCS during the IDC, and each time new CAL
solutions or PDSs are prepared. A QCS must be
analyzed at least quarterly.	
Results must be ±30% of the expected value.
  Sect. 10.2
Initial Calibration
Use the IS calibration technique to generate a linear or
quadratic calibration curve for each analyte. A
minimum of six standards should be used for a
calibration range of two orders of magnitude.  Suggested
concentrations can be found in Sect. 7.2.4.  Check the
calibration curve against the acceptance criteria in Sect.
10.2.6.
When each calibration standard is calculated as an
unknown using the calibration curve, the result
should be ± 30% of the true value for all except the
lowest standard, which should be ± 50% of the true
value. If this criterion is not met, reanalyze CALs,
select a different method of calibration or
recalibrate over a shorter range.
  Sects. 10.1
  and 10.2.1
MS Tune Check
Analyze DFTPP to verify the MS tune after instrument
maintenance and each time the instrument is mass
calibrated. The MS tune must also be verified prior to
analyzing CAL stds and establishing calibration curves
for method analytes.
Acceptance criteria are given in Table 2.
  Sect. 10.3
Continuing Calibration
Check (CCC)
Verify initial calibration by analyzing a calibration
standard at the beginning of each analysis batch prior to
analyzing samples, after every 10 Field Samples, and
after the last sample of each analysis batch. The first
CCC daily must be at or below the MRL.  Subsequent
CCCs alternate between medium and high
concentrations.

Low CCC - at or below the MRL concentration
Mid CCC - near midpoint in the initial calibration curve
High CCC - near the highest calibration standard.
                                                                                              Low: ±50% of true value
                                                                                              Mid: ±30% of true value
                                                                                              High: ±30% of true value
Note: Table 25 is intended as an abbreviated summary of QC requirements provided as a convenience to the method user.  Because the information has been
abbreviated to fit the table format, there may be issues that need additional clarification, or areas where important additional information from the method text is
needed. In all cases, the full text of Sects. 8-10 in the method supersedes any missing or conflicting information in this table.
                                                                   525.3-150

-------
Figure la. Example chromatogram of a calibration standard (concentration of 5 ng/uL injected for most analytes). Peak
identification numbers correspond to those in Table 1.
105^
100E
95 E
90-E
85E:
80 E
75^
8 65|
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1 55EE
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1 1 1 ! ' 1 1 i > 1 < I ! 1 ' I ! 1 i 1 I 1 1 1 ' ] < 1 i 1 1 1 1 1 1 	 1 ' 1 I I 1 1 1 1 1 i i 1 i ] I
6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0
Time (min)
                                                       525.3-151

-------
Figure Ib. Example chromatogram of a calibration standard (concentration of 5 ng/uL injected for most analytes). Peak
identification numbers correspond to those in Table 1.
                                                                                                   41-43
   CU
   ce
100-
95^
90-
85i
75^
65^
55^
5CH
45^
40^
35 ^E
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22
21

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52
/I
U

U' y i'
1 i '
12.5       13.0       13.5       14.0
                                                           14.5      15.0
                                                           Time (min)
15.5       16.0       16.5       17.0
                                                        525.3-152

-------
Figure Ic. Example chromatogram of a calibration standard (concentration of 5 ng/uL injected for most analytes).  Peak
identification numbers correspond to those in Table 1.

ioo^

 90^
 85^
 80^
 75^
 70-E

 60^
  -S  45-
  o:
40-
35-
30
25-
20
15-
10-
                     62,63
                                67,68  72, 73
               56,57
                                                             82
                                                    80,81
                                                       79
                                                                           87,88
                                                                         85
                                                                           86
                                                                     83
                                                                       84
                                                                                         94-96
                                                                                        93
                                                                                      92
                                                                              89
                                                                                90
                                                                                91
                                                                                                         103,104
                                                                                                    100,101
                                                                                                     99
                                                                                                   98
                                                                                                  97
                                                                                                     102
                                                                                                                  105
            17.5       18.0       18.5
                                        19.0      19.5       20.0
                                                       Time (min)
                                                                       20.5       21.0       21.5      22.0
                                                        525.3-153

-------
Figure Id. Example chromatogram of a calibration standard (concentration of 5 ng/uL injected for most analytes). Peak
identification numbers correspond to those in Table 1.
J
"55
cc
    10O—

     95^:

     90^

     85-
70-

65^E



55^



45-E



35^



25^

20
              112,113
          107,108
             109,
             110'
         106
               111
                        115,116
                   114
                               119
                                                      123
23
                       24
                                                   122
                                              ptTp-t-rprrr-prtrp-rT-, n T| rr Ty

                                               26         27
                                                                       128
                                                         124,125
                                                       126,
                                                       127
        28
Time (min)
29
                                                                                              129,
                                                                                              130   131
                                                                                     30
31
                                                                                                              32
                                                         525.3-154

-------
Figure 2. Example extracted ion current profiles of toxaphene at m/z 125, 305, and 159.
 RT: 20.71 -25.66
     40000-
   _a
                            Peak 1
                           RT:21.72
                                               Peak 3
                                              RT: 22.66
                                                                                   Peak 4
                                                                                  RT: 24.52
               21.0      21.5      22.0       22.5       23.0      23.5
                                                        Time (min)
24.0
24.5
25.0
                                   Base Peak
                                   m/z=
                                   158.50-159.50
                                                                                                             Base Peak
                                                                                                             m/z=
                                                                                                             304.50-305.50
                                                                                                             Base Peak
                                                                                                             m/z=
                                                                                                             124.50-125.50
25.5
                                                           525.3-155

-------
Figure 3a. Results of Aqueous Holding Time Study (Sect. 13.4)
 140%
 120%
                                                   •II ill ill ill ill ill ill ill ill ill ill
         ?££////////./££/.//£/*
         f */////////j ///*//
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                                 525.3-156

-------
Figure 3b. Results of Aqueous Holding Time Study (Sect. 13.4)
  140%
  120%

                                                      525.3-157

-------
 Figure 3c. Results of Aqueous Holding Time Study (Sect. 13.4)
o>

o
o
CD
CO
CD

E
   140%
   120%
   100%
            hi
                 i
                                                       mi
I
                                                 mini
     ////*
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-------
  Figure 4a. Results of Extract Holding Time Study (Sect. 13.5)
CO
CD
    140%
    120%
    100%
     80%
     60%
     40%
     20%
      0%
                                                                                                              •t=0 days(n=4)
                                                                                                              •t=7 days(n=4)
                                                                                                              •t=14days(n=4)
                                                                                                              Dt=21 days(n=4)
                                                                                                              •t=28 days(n=4)
                                                               525.3-159

-------
Figure 4b. Results of Extract Holding Time Study (Sect. 13.5)
  140%
  120%
                                                                                                              •t=0 days(n=4)
                                                                                                              •t=7 days(n=4)
                                                                                                              •t=14days(n=4)
                                                                                                              Dt=21 days(n=4)
                                                                                                              •t=28 days(n=4)
                                                              525.3-160

-------
 Figure 4c. Results of Extract Holding Time Study (Sect. 13.5)
   140%
   120%
100%
 80%
    60%
    40%
    20%
                            i
o>
o
o
CD
to
CD
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