525.3-1 

 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
 

525.3-2 

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. Accuracy 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. 1a-1d. 

Analyte 

Chemical Abstract 

Services Registry 

Number (CASRN)

Acenaphthylene 208-96-8

Acetochlor 34256-82-1

Alachlor 15972-60-8

Aldrin 309-00-2

Ametryn 834-12-8

Anthracene 120-12-7

Atraton 1610-17-9

Atrazine 1912-24-9

Benzo[a]anthracene 56-55-3

Benzo[b]fluoranthene 205-99-2

Benzo[k]fluoranthene 207-08-9

Benzo[a]pyrene 50-32-8

Benzo[g,h,i]perylene 191-24-2

Bromacil 314-40-9

Butachlor 23184-66-9

Butylate 2008-41-5

Butylated hydroxytoluene (BHT) 128-37-0

Butylbenzylphthalate 85-68-7

Chlordane (tech grade) 12789-03-6

 cis-chlordane 5103-71-9

 trans-chlordane 5103-74-2

 trans-nonachlor 39765-80-5

Chlorfenvinphos 470-90-6

Chloroneb 2675-77-6

Chlorobenzilate 510-15-6
 

525.3-3 

Analyte 

Chemical Abstract 

Services Registry 

Number (CASRN)

Chloropropham 101-21-3

Chlorothalonil 1897-45-6

Chlorpyrifos 2921-88-2

Chrysene 218-01-9

Cyanazine 21725-46-2

Cycloate 1134-23-2

Dacthal (DCPA) 1861-32-1

DDD, 4,4′- 72-54-8

DDE, 4,4′- 72-55-9

DDT, 4,4′- 50-29-3

DEET (N,N-Diethyl-meta-toluamide) 134-62-3

Dibenz[a,h]anthracene 53-70-3

Di-n-butylpthalate 84-74-2

Dichlorvos 62-73-7

Dieldrin 60-57-1

Diethylphthalate 84-66-2

Di(2-ethylhexyl)adipate 103-23-1

Di(2-ethylhexyl)phthalate 117-81-7

Diisopropyl methylphosphonate (DIMP) 1445-75-6

Dimethipin 55290-64-7

Dimethylphthalate 131-11-3

Dinitrotoluene, 2,4- 121-14-2

Dinitrotoluene, 2,6- 606-20-2

Diphenamid 957-51-7

Disulfoton 298-04-4

Endosufan I 959-98-8

Endosufan II 33213-65-9

Endosufan sulfate 1031-07-8

Endrin 72-20-8

EPTC (S-Ethyl dipropylthiocarbamate) 759-94-4

Ethion 563-12-2

Ethoprop 13194-48-4

Ethyl parathion 56-38-2

Etridiazole 2593-15-9

Fenarimol 60168-88-9

Fluorene 86-73-7

Fluridone 59756-60-4

Heptachlor 76-44-8

Heptachlor epoxide 1024-57-3

Hexachlorobenzene (HCB) 118-74-1

Hexachlorocyclohexane, alpha (α-HCH) 319-84-6

Hexachlorocyclohexane, beta (β-HCH) 319-85-7
 

525.3-4 

Analyte 

Chemical Abstract 

Services Registry 

Number (CASRN)

Hexachlorocyclohexane, delta (δ-HCH) 319-86-8

Hexachlorocyclohexane, gamma (γ-HCH) (Lindane) 58-89-9

Hexachlorocyclopentadiene (HCCPD) 77-47-4

Hexazinone 51235-04-2

Indeno[1,2,3-c,d]pyrene 193-39-5

Isophorone 78-59-1

Methoxychlor 72-43-5

Methyl parathion 298-00-0

Metolachlor 51218-45-2

Metribuzin 21087-64-9

Mevinphos 7786-34-7

MGK 264 113-48-4

Molinate 2212-67-1

Napropamide 15299-99-7

Nitrofen 1836-25-5

Norflurazon 27314-13-2

Oxyfluorfen 42874-03-3

Pebulate 1114-71-2

Pentachlorophenol 87-86-5

Phenanthrene 85-01-8

Permethrin, cis- 54774-45-7

Permethrin, trans- 51877-74-8

Prometon 1610-18-0

Phorate 298-02-2

Phosphamidon 13171-21-6

Profenofos 41198-08-7

Prometryn 7287-19-6

Pronamide 23950-58-5

Propachlor 1918-16-7

Propazine 139-40-2

Pyrene 129-00-0

Simazine 122-34-9

Simetryn 1014-70-6

Tebuconazole 107534-96-3

Tebuthiuron 34014-18-1

Terbacil 5902-51-2

Terbutryn 886-50-0

Tetrachlorvinphos 22248-79-9

Tribufos 78-48-8

Toxaphene 8001-35-2

Triadimefon 43121-43-3

Trifluralin 1582-09-8
 

525.3-5 

Analyte 

Chemical Abstract 

Services Registry 

Number (CASRN)

Vernolate 1929-77-7

Vinclozolin 50471-44-8

Polychlorinated Biphenyl (PCB) Congeners (IUPAC #)

 2-chlorobiphenyl (1) 2051-60-7

 4-chlorobiphenyl (3) 2051-62-9

 2,4′-dichlorobiphenyl (8) 34883-43-7

 2,2′,5-trichlorobiphenyl (18) 37680-65-2

 2,4,4′-trichlorobiphenyl (28) 7012-37-5

 2,2′,3,5′-tetrachlorobiphenyl (44) 41464-39-5

 2,2′,5,5′-tetrachlorobiphenyl (52) 35693-99-3

 2,3′,4′,5-tetrachloroobiphenyl (70) 32598-11-1

 2,3,3′,4′,6-pentachlorobiphenyl (110) 38380-03-9

 2,3′,4,4′,5-pentachlorobiphenyl (118) 31508-00-6

 2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 35065-28-2

 2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 38380-04-0

 2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 35065-27-1

 2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 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 
 

525.3-6 

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 
 

525.3-7 

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 
 

525.3-8 

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. 
 

525.3-9 

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. 
 

525.3-10 

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.
 

525.3-11 

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 chromatograms. All items such as these must be routinely demonstrated to be free from 

interferences (less than 1/3 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. 

4.6. 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 
 

525.3-12 

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 
 

525.3-13 

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 PTFEfaced 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 μL. 

6.6. DRYING COLUMN - The drying column must be able to contain 10-12 g of 

anhydrous sodium sulfate (Na2SO4). 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. 
 

525.3-14 

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. 
 

525.3-15 

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). 
 

525.3-16 

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 
 

525.3-17 

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 μm bonded 

film of poly(dimethylsiloxy)poly(1,4-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 
 

525.3-18 

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 programmed 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.
 

525.3-19 

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 1

/3 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 
 

525.3-20 

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. 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 μg/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 μL of 

the PDS for ISs 1-3 and 4 μL of the PDS for IS 4 to fortify the final 1-mL 

extracts (Sect. 11.9) will yield a concentration of 5 μg/mL each for ISs 1-3 

and 4 μg/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 μg/mL. The IS 4 concentration remained at 4 μg/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 CASRN Solvent PDS conc.

acenaphthene-d10 (IS 1) 15067-26-2 acetone 500 μg/mL 

phenanthrene-d10 (IS 2) 1517-22-2 acetone 500 μg/mL 

chrysene-d12 (IS 3) 1719-03-5 acetone 500 μg/mL 

13C-pentachlorophenol (IS 4) 85380-74-1 methanol 1000 μg/mL 

7.2.2. 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 
 

525.3-21 

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 oC or less. For full scan analysis, 10 μL 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 μg/L of each 

SUR. For SIM analyses the QC and Field Samples were fortified such that 

the expected final extract concentration was 1 μg/L for each SUR. 

 

Surrogates CASRN Solvent PDS conc.

1,3-dimethyl-2-nitrobenzene (SUR 1) 81-20-9 acetone 500 μg/mL 

triphenyl phosphate (SUR 2) 115-86-6 acetone 500 μg/mL 

benzo[a]pyrene-d12 (SUR 3) 63466-71-7 acetone 500 μg/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 μL) 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 
 

525.3-22 

weighed amount can be used without correction to calculate the 

concentration of the solution. Store at 4 oC 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 μg/mL for most compounds) - 

Prepare the 50-μg/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-μg/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 μL) needs to be 
 

525.3-23 

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., ≥ 5μg/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/μL are 
 

525.3-24 

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/μL 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 SUR PDSs (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 oC 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-

11.9). 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 μg/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/μL 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. 
 

525.3-25 

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.

8.1.2. 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 Amount Purpose

L-Ascorbic acid 0.10 g/L Dechlorination

Ethylenediaminetetraacetic acid, trisodium 

salt

0.35 g/L Inhibit metal-catalyzed 

hydrolysis of targets

Potassium dihydrogen citrate 9.4 g/L pH 3.8 buffer, 

microbial inhibitor

8.1.2.1. Residual chlorine must be reduced at the time of sample collection with 

100 mg of ascorbic acid per liter.21

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 
 

525.3-26 

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 oC 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. 
 

525.3-27 

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 

 HR S PIR = 3.963

 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 + HRPIR) meet the upper and lower 

recovery limits as shown below: 
 

525.3-28 

 The Upper PIR Limit must be ≤150 percent recovery. 

 ≤× 150% %100 +

FortifiedConcentration

Mean HRPIR

 

 The Lower PIR Limit must be ≥ 50 percent recovery. 

 ≥× 50% %100 −

FortifiedConcentration

Mean HRPIR

9.2.4.3. 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. 

9.2.4.4. 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 if DL 

determination is required based upon the intended use of the data.
 

525.3-29 

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. 11 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: 

 

 =−− )99.01 ,1( ×=

n α

DL ts

 

 where:

 t (n-1, 1-α=0.99) = 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 1

/3

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 
 

525.3-30 

than 1/3 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 calibration (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 samples 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 
 

525.3-31 

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 

 % ×100 

 



 = B

A R

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 
 

525.3-32 

acceptable, extraction of the sample should be repeated provided 

the sample is still available and within the holding time. If the reextracted 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 

 ( ) % ×100 − = C

BA R

 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 
 

525.3-33 

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 

 ( ) 100

2/21

21

×

+

− = FDFDFDFD

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 

( ) 100

2/

×

+

− = LFSM LFSMDLFSM LFSMD

RPD

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 
 

525.3-34 

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).
 

525.3-35 

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/μL, and acquire data in the full scan mode 
 

525.3-36 

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 = 

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

 ∑ 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 1-μL aliquot into a hot, splitless injection 

port held at 275 oC 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 oC, hold for 1.5 min, ramp at 10 oC/min to 200 

oC, ramp at seven oC/min to a final temperature of 320 oC 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 
 

525.3-37 

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 
 

525.3-38 

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 
 

525.3-39 

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 
 

525.3-40 

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-μL aliquot of each of the 500-μg/mL SUR
 

525.3-41 

PDSs (Sect. 7.2.2) was added to 1 L samples for a final concentration of 

5.0 μg/L.

11.2.3. 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. 

11.2.4. 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. 6.11 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 H2O 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 
 

525.3-42 

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 10 mL MeOH to 

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 
 

525.3-43 

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 10 mL MeOH. 

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 
 

525.3-44 

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 
 

525.3-45 

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.
 

525.3-46 

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 
 

525.3-47 

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. 
 

525.3-48 

Step # Description Solvent Soak Time

(mm:ss)

Air Dry Time

(mm:ss)

1 Prewet EtOAc 1:00 0:30

2 Prewet DCM 1:00 0:30

3 Prewet MeOH 1:00 0.00

4 Prewet LRW 0.05 0.00

5 Sample Load

6* Wash LRW 0:10 0:30

7* Wash LRW 0:10 0:30

8 Air Dry 1:00

9 Rinse EtOAc 1:30 0:30

10 Rinse DCM 1:30 0:30

11 Rinse DCM 1:30 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 o

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 oC 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 
 

525.3-49 

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 1g/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 1a-1d. 

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 chromatogram.

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 
 

525.3-50 

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 multicomponent 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. In validating 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. 
 

525.3-51 

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 
 

525.3-52 

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. 
 

525.3-53 

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 μm 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 μm 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 RXI5sil-MS 30 m x 0.25 mm x 0.25 μm 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 μm 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 
 

525.3-54 

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 H2OPhobic 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. LCMRLs and DLs

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. 
 

525.3-55 

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 oC, followed by storage at 6 oC 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 oC 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 
 

525.3-56 

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. 

13.6.2. 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. PENTACHLOROPHENOL - Pentachlorophenol is 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 
 

525.3-57 

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.
 

525.3-58 

14. POLLUTION PREVENTION

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 liquidliquid 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. High Resol. 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 
 

525.3-59 

Tubular Column Gas Chromatography with Splitless or Hot On-Column Injection and Flame 

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. High Resol. 

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. High Resol. 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 

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and Health Administration, OSHA 2206, (Revised, July 2001).

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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 

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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. 
 

525.3-60 

20. Pepich, B.V., Prakash, B., Domino, M.M., Dattilio, T.A., Munch, D.J., Price, E.K., 

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). 

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(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 

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Registry (1999). Available at http://www.atsdr.cdc.gov/ToxProfiles/tp112.pdf (accessed 

October 5, 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. Food Chem., 

1976, 24, 721-723. 

31. Pawlecki-Vonderheide, A.M., Munch, D.J., Method 515.3. Determination of Chlorinated 
 

525.3-61 

Acids in Drinking Water by Liquid-Liquid Extraction, Derivatization and Gas 

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 

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33. Standard Operating Procedure for Disinfectant Sample Preparation, SOP MB-22-00, 2008. 

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Available on-line at http://www.epa.gov/pesticides/methods/atmpmethods/MB-22-00.pdf 

(access November 10, 2011). 
 

525.3-62 

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

RT (min) Internal Standards, Analytes and 

Surrogates

IS Ref. 

# 

QI (m/z) Confirmation 

Ion(s) (m/z) 

Comments

15 13.21 acenaphthene-d10 (IS 1) 162 164 a 

41 16.35 13C-pentachlorophenol (IS 4) 276 -- b,c,d

47 16.73 phenanthrene-d10 (IS 2) 188 160* a 

116 24.29 chrysene-d12 (IS 3) 240 236* a 

1 7.24 DIMP 1 97 123 b 

2 8.20 isophorone 1 82 138* a 

3 9.13 1,3-dimethyl-2-nitrobenzene (SUR) 1 77 134 a 

4 9.97 dichlorvos 1 109 185* a,d,e

5 11.21 HCCPD 1 237 235, 239 a 

6 11.53 EPTC 1 128 86 a 

7 12.44 mevinphos 1 127 109*, 192* a,d,e,f

8 12.48 butylate 1 57 146, 156 a 

9 12.71 vernolate 1 128 86 a

10 12.74 dimethylphthalate 1 163 77* a

11 12.77 etridiazole 1 211 183 a

12 12.84 2,6-dinitrotoluene 1 165 63, 89 a

13 12.87 acenaphthylene 1 152 -- a

14 12.88 pebulate 1 128 57, 72 a

16 13.43 2-chlorobiphenyl 1 188 152 a 

17 13.45 BHT 1 205 220 b,g

18 13.47 chloroneb 1 193 191 a 

19 13.69 tebuthiuron 1 156 171 a 

20 13.79 2,4-dinitrotoluene 1 165 63, 89 a 

21 13.92 molinate 1 126 55 a 

22 14.31 DEET 1 119 91, 190 b 

23 14.44 diethylphthalate 1 149 177* a,g

24 14.46 4-chlorobiphenyl 1 188 152 a 

25 14.53 fluorene 1 165 166 a 

26 14.68 propachlor 1 120 77, 176 a 
 

525.3-63 

Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested 

Confirmation Ions, and Suggested Internal Standard Reference

Peak 

Identification 

#, Figure 1

RT (min) Internal Standards, Analytes and 

Surrogates

IS Ref. 

# 

QI (m/z) Confirmation 

Ion(s) (m/z) 

Comments

27 15.00 ethoprop 1 97 126, 139, 158 a,d

28 15.03 cycloate 1 83 55, 154 a 

29 15.27 chlorpropham 1 213 127 a 

30 15.34 trifluralin 1 264 306 a,d

31 15.66 phorate 1 75 121 b,d 

32 15.75 α-HCH 1 181 109, 183, 219 a 

33 15.81 2,4'-dichlorobiphenyl 1 222 152, 224 a 

34 15.83 hexachlorobenzene 1 284 142, 249 a 

35 16.08 atraton 2 196 169, 211 a 

36 16.20 simazine 2 201 173, 186 a 

37 16.21 prometon 2 225 168, 210 a 

38 16.28 dimethipin 2 54 53 b 

39 16.29 atrazine 2 200 215 a 

40 16.30 β-HCH 2 181 109, 183, 219 a 

42 16.35 pentachlorophenol 4 266 264, 268 a,c,d

43 16.36 propazine 2 214 58, 229 a 

44 16.46 γ-HCH (lindane) 2 183 109, 181, 219 a,e

45 16.66 pronamide 2 173 145 a 

46 16.69 2,2',5-trichlorobiphenyl 2 256 186 a 

48 16.79 phenanthrene 2 178 152* a 

49 16.81 chlorothalonil 2 266 264, 268 a,e

50 16.91 disulfoton 2 88 61*, 97* a 

51 16.91 anthracene 2 178 -- a 

52 17.01 terbacil 2 117 161 a,d

53 17.06 δ-HCH 2 181 109, 183, 219 a 

54 17.53 phosphamidon 2 127 72, 264 b,d

55 17.68 acetochlor 2 146 59, 162, 223 a 

56 17.71 metribuzin 2 198 -- a 

57 17.73 2,4,4'-trichlorobiphenyl 2 186 256 a,e

58 17.79 vinclozolin 2 212 124, 285 b,e
 

525.3-64 

Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested 

Confirmation Ions, and Suggested Internal Standard Reference

Peak 

Identification 

#, Figure 1

RT (min) Internal Standards, Analytes and 

Surrogates

IS Ref. 

# 

QI (m/z) Confirmation 

Ion(s) (m/z) 

Comments

59 17.84 methyl parathion 2 109 125, 263 b,d

60 17.87 alachlor 2 188 160 a 

61 17.96 simetryn 2 213 155, 170 a 

62 18.04 ametryn 2 227 212 a 

63 18.05 heptachlor 2 100 272, 274 a 

64 18.10 prometryn 2 241 184, 226 a 

65 18.39 terbutryn 2 226 170, 185, 241 a 

66 18.47 2,2',5,5'-tetrachlorobiphenyl 2 220 290, 292 a 

67 18.53 dibutyl phthalate 2 149 -- a 

68 18.56 bromacil 2 205, 207 207, 205 a 

69 18.72 metolachlor 2 162 238 a 

70 18.76 chlorpyrifos 2 97 197, 199 a,e

71 18.84 aldrin 2 66 79, 263 a 

72 18.87 cyanazine 2 225 68, 172, 198 a 

73 18.87 dacthal (DCPA) 2 301 332 a 

74 18.91 2,2',3,5'-tetrachlorobiphenyl 2 220 255, 292 a 

75 18.92 ethyl parathion 2 109 97, 291 b,d

76 19.01 triadimefon 2 208 57 a,d,e

77 19.27 diphenamid 2 72 167, 239* a 

78 19.30 MGK 264(a) 2 164 66, 111 a,h

79 19.59 MGK 264(b) 2 164 66, 111 a,h

80 19.72 heptachlor epoxide 2 353 81, 355 a,e

81 19.74 chlorfenvinphos 2 267 269, 323 b,d

82 19.85 2,3',4',5-tetrachlorobiphenyl 2 220 110, 292 a 

83 20.27 trans-chlordane 2 375 237, 272 a 

84 20.38 tetrachlorvinphos 2 109 329, 331 a,d

85 20.46 butachlor 2 176 57, 160 a,d

86 20.54 pyrene 2 202 -- a 

87 20.58 cis-chlordane 2 375 373, 377 a 

88 20.59 endosulfan I 2 241 195, 207 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

RT (min) Internal Standards, Analytes and 

Surrogates

IS Ref. 

# 

QI (m/z) Confirmation 

Ion(s) (m/z) 

Comments

89 20.65 trans-nonachlor 2 409 407, 411 a 

90 20.76 napropamide 2 72 100, 128 a,d

91 21.00 profenofos 2 339 97, 139, 208 b,d

92 21.12 4,4'-DDE 2 246 176, 318 a 

93 21.17 tribufos (+merphos) 2 57 169 b,d,i

94 21.23 dieldrin 2 79 81 a,e

95 21.25 oxyfluorfen 2 252 63, 361 b,d

96 21.26 2,3,3',4',6-pentachlorobiphenyl 2 326 184, 254 a 

97 21.69 nitrofen 2 283 139, 202 b,d

98 21.72 endrin 2 263 81, 281 a 

99 21.81 2,2',3,4',5',6-hexachlorobiphenyl 2 360 218, 290 a 

100 21.90 chlorobenzilate 2 251 111, 139 a 

101 21.91 2,3',4,4',5-pentachlorobiphenyl 2 326 184, 254 a 

102 21.99 endosulfan II 2 195 207, 241 a 

103 22.11 4,4'-DDD 2 235 165 a,d

104 22.11 ethion 2 231 97, 153 b,d,e

105 22.40 2,2',4,4',5,5'-hexachlorobiphenyl 2 360 218, 290 a 

106 22.82 norflurazon 2 145 102, 303 a,d

107 22.91 butylbenzylphthalate 2 149 91, 206 a,g

108 22.91 endosulfan sulfate 2 272 237, 387 a,e

109 23.03 4,4'-DDT 2 235 165 a,e

110 23.06 2,2',3,4,4',5'-hexachlorobiphenyl 2 360 218, 290 a 

111 23.17 hexazinone 2 171 83* a,d

112 23.38 di(2-ethylhexyl)adipate 3 129 57, 70 a,g

113 23.39 tebuconazole 3 125 83, 250 b,d,e

114 23.48 triphenyl phosphate (SUR) 3 77 169, 326 a,e

115 24.26 benzo[a]anthracene 3 228 226* a 

117 24.37 chrysene 3 228 226* a 

118 24.40 methoxychlor 3 227 -- a,d

119 24.67 2,2',3,4,4',5,5'-heptachlorobiphenyl 3 394 252, 324 a 
 

525.3-66 

Table 1. Retention Times (RTs), Suggested Quantitation Ions (QIs), Suggested 

Confirmation Ions, and Suggested Internal Standard Reference

Peak 

Identification 

#, Figure 1

RT (min) Internal Standards, Analytes and 

Surrogates

IS Ref. 

# 

QI (m/z) Confirmation 

Ion(s) (m/z) 

Comments

120 24.93 di(2-ethylhexyl)phthalate 3 149 167 a,g 

121 25.79 fenarimol 3 107 139, 219 a 

122 26.64 cis-permethrin 3 183 163* a,d,e

123 26.82 trans-permethrin 3 183 163* a,d,e

124 27.49 benzo[b]fluoranthene 3 252 126* a 

125 27.54 benzo[k]fluoranthene 3 252 126* a 

126 28.22 benzo[a]pyrene-d12 (SUR) 3 264 132* a 

127 28.28 benzo[a]pyrene 3 252 126* a 

128 28.50 fluridone 3 328 329 a,c,d

129 30.72 indeno[1,2,3-c,d]pyrene 3 276 138* a 

130 30.80 dibenzo[a,h]anthracene 3 278 139* a 

131 31.20 benzo[g,h,i]perylene 3 276 138* 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/μL. 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.
 

525.3-67 

Table 2. Ion Abundance Criteria for Decafluorotriphenyl Phosphine (DFTPP)a

Mass (m/z) Relative Abundance Criteria Purpose of Checkpointb 

68 < 2% of m/z 69 Low-mass resolution

69 present Low-mass resolution

70 < 2% of m/z 69 Low-mass resolution

197 < 2% of m/z 198 Mid-mass resolution

198 present c Mid-mass resolution and sensitivity 

199 5-9% of m/z 198 Mid-mass resolution and isotope ratio 

365 >1% of base peak Baseline threshold

441 < 150% of m/z 443 High-mass resolution

442 present c High-mass resolution and sensitivity

443 15-24% of m/z 442 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. 
 

525.3-68 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 87.1 2.8 95.8 2.2 88.7 1.7

acetochlor 102 4.6 108 6.8 95.2 2.0

alachlor 106 3.6 107 5.6 102 3.0

aldrin 96.2 2.0 87.1 6.2 86.4 2.0

ametryn 105 4.6 102 7.1 95.0 3.0

anthracene 90.1 4.6 98.5 2.7 98.4 0.66

atraton 108 11 109 6.6 99.9 1.3

atrazine 103 1.3 106 7.2 102 1.1

benzo[a]anthracene 90.9 7.0 104 2.8 89.2 0.75

benzo[a]pyrene 95.4 5.5 96.4 5.7 89.0 5.1

benzo[b]fluoranthene 98.2 3.1 96.8 3.8 90.8 2.4

benzo[g,h,i]perylene 97.0 13 94.9 5.6 90.3 5.9

benzo[k]fluoranthene 103 5.6 102 4.5 92.8 3.3

BHT NDe NDe 92.8 1.3

bromacil 119 2.1 103 12 99.5 1.4

butachlor 106 4.8 106 3.5 94.5 2.5

butylate 91.2 4.2 104 6.0 88.6 1.9

butylbenzylphthalate 105 5.9 123 7.4 92.9 2.2

chlordane, cis 99.1 2.9 105 3.7 99.8 0.86

chlordane, trans 91.7 1.4 99.3 3.6 105 3.8

chlorfenvinphos 101 6.8 105 3.9 108 2.6

chlorobenzilate 109 1.1 109 4.5 96.8 2.0

chloroneb 91.8 5.5 97.5 5.0 94.9 2.4

chlorothalonil 102 2.7 101 2.9 106 2.6

chlorpropham 119 11 105 5.6 92.7 2.0

chlorpyrifos 112 13 99.8 6.3 94.4 2.3

chrysene 95.6 8.3 107 2.3 89.8 0.39

cyanazine 107 9.4 111 6.3 95.5 1.0
 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

cycloate 90.4 2.7 99.6 5.0 90.7 1.8

dacthal (DCPA) 91.5 7.3 103 4.4 101 1.5

DDD, 4,4′- 101 6.0 103 5.7 92.5 0.70 

DDE, 4,4′- 98.1 1.2 100 5.9 95.0 2.4

DDT, 4,4′- 106 5.0 104 6.1 95.7 0.80 

DEET 102 4.1 101 2.9 94.2 0.81 

di(2-ethylhexyl)adipate 106 5.2 104 3.2 94.9 3.9

di(2-ethylhexyl)phthalate 144 27 112 4.6 91.3 1.8

dibenzo[a,h]anthracene 97.3 17 83.9 11 98.6 5.8

dibutyl phthalate 81.0 11 119 6.8 104 2.8

dichlorvos 101 9.2 98.3 5.9 91.2 2.5

dieldrin 97 2.0 100 5.0 91.6 2.1

diethylphthalate 108 7.2 104 2.6 94.2 1.4

dimethipin 107 15 95.2 5.5 61.1 7.3

dimethylphthalate 99.3 3.0 101 3.6 95.5 1.1

DIMP 104 5.3 96.2 1.6 90.6 2.1

dinitrotoluene, 2,4- 109 6.7 96.8 4.4 91.1 0.59

dinitrotoluene, 2,6- NDf 110 5.2 90.7 2.4

diphenamid 104 4.4 109 6.6 93.0 1.4

disulfoton 85.2 1.3 85.6 4.9 89.3 1.9

endosulfan I 101 13 101 6.0 97.9 1.7

endosulfan II 106 7.0 113 9.6 93.9 0.70 

endosulfan sulfate 98.7 6.2 106 6.2 96.5 1.5

endrin 94.7 14 107 5.9 95.8 3.2

EPTC 87.9 1.8 99.8 6.9 91.1 1.5

ethion 103 6.0 104 3.6 93.0 0.59

ethoprop 109 21 103 8.6 92.1 2.1

ethyl parathion 101 16 89.8 3.8 95.8 1.6
 

525.3-70 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

etridiazole 97.7 4.6 96.0 4.7 93.7 0.41 

fenarimol 108 14 112 7.5 95.6 1.2

fluorene 92.6 3.2 97.1 2.2 88.5 1.8

fluridone 116 2.6 95.9 11 122 3.5

HCCPD 61.7 12 80.6 4.2 79.4 1.4

HCH, α 101 1.9 101 6.1 93.8 2.7

HCH, β 103 4.4 106 4.5 98.9 1.4

HCH, δ 104 8.3 104 6.0 98.0 2.1

HCH, γ (lindane) 96.7 3.6 104 5.6 98.7 4.0

heptachlor 83.5 5.0 108 9.7 92.1 1.2

heptachlor epoxide 106 6.5 104 4.7 99.9 1.9

hexachlorobenzene 59.5 15 88.1 2.8 86.5 1.6

hexazinone 107 10 113 6.8 94.4 1.3

indeno[1,2,3-c,d]pyrene 101 23 90.8 12 84.9 7.1

isophorone 97.4 3.1 99.7 4.0 90.0 1.2

methoxychlor 100 6.9 108 3.7 98.0 1.1

methyl parathion 97.9 11 98.6 5.8 97.4 0.07

metolachlor 93.4 1.7 104 5.0 97.5 1.2

metribuzin 104 2.6 96.3 6.7 98.9 2.6

mevinphos 103 8.5 95.5 5.8 90.3 2.5

MGK 264(a) 95.7 11 104 5.4 98.6 2.5

MGK 264(b) 99 5.8 103 9.0 98.6 5.5

molinate 84.8 11 99.0 5.2 83.8 2.4

napropamide 103 3.2 109 6.8 92.1 1.3

nitrofen 102 13 102 3.0 92.7 1.6

nonachlor, trans 91.4 11 104 5.4 102 0.55

norflurazon 103 9.2 101 8.7 92.3 1.3

oxyfluorfen 106 2.6 107 2.9 91.6 0.23 
 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

pebulate 92.2 2.7 101 4.3 92.7 1.1

pentachlorophenol 92.9 5.6 85.8 5.5 93.9 2.7

permethrin, cis 101 5.4 109 5.2 88.5 3.2

permethrin, trans 100 5.1 101 4.5 90.5 1.6

phenanthrene 84.2 7.7 101 2.2 95.6 1.1

phorate 95.8 5.3 89.8 2.4 91.0 1.5

phosphamidon 112 7.8 112 4.2 97.8 2.0

profenofos 104 16 109 7.1 99.7 0.92 

prometon 93.5 13 110 7.5 92.4 2.1

prometryn 109 8.7 104 6.7 101 3.6

pronamide 102 2.4 104 6.8 100 1.9

propachlor 102 7.6 103 4.4 92.9 1.2

propazine 99.6 5.1 107 4.4 99.2 2.8

pyrene 95.7 2.6 102 2.4 93.6 1.3

simazine 96 1.2 84.8 5.2 100 2.7

simetryn 107 4.7 107 6.7 107 1.3

tebuconazole 105 1.6 107 5.0 96.1 0.87

tebuthiuron 105 4.0 109 5.0 96.8 2.1

terbacil 95.9 6.2 104 7.1 98.7 3.4

terbutryn 111 4.6 107 5.8 100 1.4

tetrachlorvinphos 109 6.3 104 7.8 94.8 2.4

triadimefon 99.6 7.5 110 6.8 98.0 2.7

tribufos+merphos 111 2.8 105 4.2 99.1 1.3

trifluralin 94.4 1.1 104 5.2 90.7 0.72 

vernolate 95.3 1.6 96.5 5.1 92.3 0.82 

vinclozolin 94.9 7.3 99.7 4.7 96.9 2.2

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 83.4 3.2 92.6 5.4 88.6 1.5
 

525.3-72 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

4-chlorobiphenyl (3) 82.4 3.0 94.0 4.4 86.2 1.0

2,4′-dichlorobiphenyl (8) 78.5 3.5 92.2 4.7 90.8 2.1

2,2′,5-trichlorobiphenyl (18) 83.4 11 94.1 4.2 92.5 2.8

2,4,4′-trichlorobiphenyl (28) 83.2 6.0 93.6 6.9 90.3 1.1

2,2′,3,5′-tetrachlorobiphenyl (44) 91.2 5.3 99.4 4.3 94.6 1.8

2,2′,5,5′-tetrachlorobiphenyl (52) 84.3 4.4 102 3.7 94.5 1.5

2,3′,4′,5-tetrachloroobiphenyl (70) 89.9 7.3 98.5 5.2 95.0 0.73 

2,3,3′,4′,6-pentachlorobiphenyl (110) 98.2 6.7 98.1 4.3 94.6 0.60 

2,3′,4,4′,5-pentachlorobiphenyl (118) 92.5 5.1 99.3 4.4 96.2 1.5

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 94.5 4.0 98.7 5.0 95.1 1.3

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 96.1 5.8 103 4.5 97.6 0.74 

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 92.2 0.9 101 4.3 99.1 2.0

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 88.5 4.1 107 3.6 100 3.0

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 91.5 3.7 94.0 2.5 91.3 1.7

benzo[a]pyrene-d12 101 4.7 86.5 3.5 91.2 3.0

triphenyl phosphate 102 2.8 105 3.2 88.3 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 μg/L, pentachlorophenol 

is 1.0 μg/L, tebuconazole is 1.2 μg/L, c-permethrin is 0.14 μg/L, t-permethrin is 0.36 μg/L, MGK 264(a) is 0.20 

μg/L and MGK 264(b) is 0.050 μg/L. 

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, tebuconazole is 10.0 μg/L, c-permethrin is 1.1μg/L, t-permethrin is 2.9μg/L, and MGK 264(a) is 1.6

μg/L and MGK 264(b) is 0.40 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20.0 μg/L, tebuconazole is 25.0 μg/L, c-permethrin is 2.8 μg/L, t-permethrin is 7.2 μg/L, and MGK 264(a) is 

4.0μg/L and MGK 264(b) is 1.0 μg/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.
 

525.3-73 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 90.5 1.7 99.3 2.5

acetochlor 2.0 102 3.8 128 2.3

alachlor 2.0 104 6.2 115 3.8

aldrin 2.0 80.3 3.2 91.6 2.0

ametryn 2.0 91.8 6.7 97.8 4.7

anthracene 2.0 96.5 1.3 101 3.3

atraton 2.0 96.5 1.8 94.1 4.7

atrazine 2.0 100 2.2 106 3.6

benzo[a]anthracene 2.0 99.1 4.0 104 3.7

benzo[a]pyrene 2.0 91.1 4.2 99.9 1.2

benzo[b]fluoranthene 2.0 93.9 3.3 105 3.4

benzo[g,h,i]perylene 2.0 95.3 5.9 113 2.9

benzo[k]fluoranthene 2.0 97.2 2.7 96.7 4.6

BHT 2.0 NDe ND d

bromacil 2.0 89.4 2.3 108 2.9

butachlor 2.0 102 4.0 117 4.8

butylate 2.0 101 1.9 114 2.6

butylbenzylphthalate 2.0 110 4.7 99.8 4.0

chlordane, cis- 2.0 96.9 3.9 112 2.4

chlordane, trans 2.0 92.0 4.0 106 3.3

chlorfenvinphos 2.0 104 3.3 102 3.6

chlorobenzilate 2.0 105 4.1 116 4.0

chloroneb 2.0 87.9 3.7 95.5 2.3

chlorothalonil 2.0 98.1 3.4 108 2.2

chlorpropham 2.0 100 2.3 120 5.2

chlorpyrifos 2.0 97.7 3.1 110 3.7

chrysene 2.0 102 3.1 104 3.1

cyanazine 2.0 103 2.7 102 1.8

cycloate 2.0 92.9 2.2 105 2.0
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

dacthal (DCPA) 2.0 98.7 2.8 108 2.7

DDD, 4,4′- 2.0 95.2 2.8 105 2.9

DDE, 4,4′- 2.0 93.7 3.5 104 2.7

DDT, 4,4′- 2.0 102 4.5 117 2.2

DEET 2.0 103 1.7 103 2.4

di(2-ethylhexyl)adipate 2.0 101 2.9 106 3.8

di(2-ethylhexyl)phthalate 2.0 101 3.7 99.8 6.3

dibenzo[a,h]anthracene 2.0 85.6 5.8 102 2.4

dibutyl phthalate 2.0 114 4.5 109 8.5

dichlorvos 2.0 94.3 1.6 118 2.2

dieldrin 2.0 96.0 3.0 101 3.8

diethylphthalate 2.0 90.5 1.2 102 2.5

dimethipin 2.0 94.9 6.7 85.3 2.9

dimethylphthalate 2.0 97.7 2.7 108 2.5

DIMP 2.0 93.4 2.0 98.4 4.5

dinitrotoluene, 2,4- 2.0 100 0.40 115 2.9

dinitrotoluene, 2,6- 2.0 103 2.6 124 3.8

diphenamid 2.0 102 3.1 109 4.1

disulfoton 2.0 73.0 5.1 82.6 5.9

endosulfan I 2.0 99.4 3.2 109 3.2

endosulfan II 2.0 106 2.8 108 4.0

endosulfan sulfate 2.0 94.3 9.1 102 2.9

endrin 2.0 107 5.2 118 2.0

EPTC 2.0 96.1 1.2 110 2.6

ethion 2.0 104 3.7 105 2.4

ethoprop 2.0 97.9 2.4 122 2.3

ethyl parathion 2.0 87.1 4.0 93.8 10

etridiazole 2.0 98.8 2.0 121 4.1

fenarimol 2.0 101 3.0 112 4.1
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

fluorene 2.0 94.9 1.1 100 3.8

fluridone 2.0 88.8 3.9 116 4.4

HCCPD 2.0 99.1 2.8 111 4.3

HCH, α 2.0 96.3 2.6 111 2.9

HCH, β 2.0 86.8 2.6 110 2.8

HCH, δ 2.0 93.8 1.7 95.1 0.6

HCH, γ (lindane) 2.0 98.6 2.7 111 7.2

heptachlor 2.0 105 4.3 113 2.6

heptachlor epoxide 2.0 100 1.7 110 1.8

hexachlorobenzene 2.0 81.5 2.6 95.3 3.0

hexazinone 2.0 98.5 3.6 108 1.9

indeno[1,2,3-c,d]pyrene 2.0 96.0 4.8 111 1.1

isophorone 2.0 92.4 1.2 106 3.2

methoxychlor 2.0 102 1.8 120 4.4

methyl parathion 2.0 102 3.3 108 4.2

metolachlor 2.0 102 1.6 114 2.7

metribuzin 2.0 89.4 5.9 92.1 6.2

mevinphos 2.0 94.9 3.2 116 2.9

MGK 264(a) 1.6 98.1 3.0 110 2.7

MGK 264(b) 0.4 97.8 4.0 110 3.6

molinate 2.0 91.3 3.5 107 4.7

napropamide 2.0 103 1.3 112 3.3

nitrofen 2.0 96.8 3.5 102 3.4

nonachlor, trans 2.0 96.7 4.2 107 3.6

norflurazon 2.0 92.5 4.6 114 1.7

oxyfluorfen 2.0 106 4.1 112 3.0

pebulate 2.0 95.9 2.3 109 1.9

pentachlorophenol 8.0 81.9 13 96.3 7.3

permethrin, trans 1.1 95.8 3.0 107 2.9
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

permethrin, trans 2.9 93.2 4.3 104 3.3

phenanthrene 2.0 97.0 2.5 99.6 3.7

phorate 2.0 92.5 2.3 96.9 1.5

phosphamidon 2.0 108 5.6 103 3.4

profenofos 2.0 105 2.5 110 4.3

prometon 2.0 94.7 1.9 88.3 5.5

prometryn 2.0 96.9 3.2 100 3.7

pronamide 2.0 101 2.8 114 2.8

propachlor 2.0 99.5 1.9 114 2.7

propazine 2.0 101 2.0 105 3.5

pyrene 2.0 97.1 4.3 100 3.2

simazine 2.0 78.9 2.0 79.9 2.9

simetryn 2.0 96.9 3.2 99.8 2.0

tebuconazole 10.0 112 1.1 107 1.2

tebuthiuron 2.0 105 2.5 106 3.3

terbacil 2.0 108 3.9 121 6.5

terbutryn 2.0 101 4.5 106 4.7

tetrachlorvinphos 2.0 102 4.2 110 4.4

triadimefon 2.0 104 3.1 109 3.7

tribufos+merphos 2.0 105 2.4 110 1.9

trifluralin 2.0 101 2.4 116 3.2

vernolate 2.0 91.3 0.8 106 2.6

vinclozolin 2.0 98.8 2.9 99.5 2.9

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 85.8 1.2 97.0 2.3

4-chlorobiphenyl (3) 2.0 96.0 1.7 99.5 4.4

2,4-dichlorobiphenyl (8) 2.0 87.8 2.3 96.6 3.3

2,2′,5-trichlorobiphenyl (18) 2.0 86.2 3.5 94.8 5.2

2,4,4′-trichlorobiphenyl (28) 2.0 87.8 7.4 100 2.8
 

525.3-77 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 93.6 3.4 105 2.7

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 104 4.7 103 3.7

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 92.8 1.8 103 2.1

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 93.2 2.6 102 2.0

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 91.2 3.7 102 4.4

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 88.2 6.7 97.5 4.2

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 95.7 0.8 106 4.2

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 93.1 5.2 103 3.1

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 97.7 1.8 107 2.5

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene (SUR) 5.0 92.3 1.7 97.9 2.8

benzo[a]pyrene-d12 5.0 88.4 3.2 88.0 3.9

triphenyl phosphate (SUR) 5.0 108 2.5 103 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.
 

525.3-78 

Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE Columns (Cartridges); Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 84.9 1.9 88.2 2.4 90.7 1.8

acetochlor 102 4.0 94.7 1.9 97.0 3.0

alachlor 96.0 5.0 94.6 2.2 103 3.2

aldrin 95.6 2.5 88.3 7.1 96.5 4.5

ametryn 97.6 3.2 95.7 3.9 96.0 4.1

anthracene 89.4 3.2 91.1 2.9 104 2.7

atraton 107 12 101 3.3 97.9 2.5

atrazine 100 6.7 99.3 1.0 100 3.4

benzo[a]anthracene 89.1 0.43 95.8 2.9 92.4 1.9

benzo[a]pyrene 89.9 11 89.7 5.2 100 3.5

benzo[b]fluoranthene 94.1 2.6 97.6 3.8 96.6 0.81

benzo[g,h,i]perylene 89.9 10 92.8 9.0 98.7 5.1

benzo[k]fluoranthene 92.5 7.4 92.9 3.9 99.7 1.6

BHT 81.7 11 86.0 3.2 86.0 0.53

bromacil 104 8.2 97.5 17 97.7 2.9

butachlor 103 2.1 92.0 2.2 99.6 1.3

butylate 91.0 2.6 95.5 1.6 92.7 0.59

butylbenzylphthalate 103 5.8 96.5 3.1 101 4.3

chlordane, cis 97.2 5.2 97.9 2.6 103 2.2

chlordane, trans 93.7 5.3 106 2.3 105 1.2

chlorfenvinphos 92.7 5.3 99.1 4.6 98.9 3.3

chlorobenzilate 99.9 4.7 98.2 3.7 102 3.8

chloroneb 92.9 2.9 95.9 2.5 95.2 1.9

chlorothalonil 90.9 5.6 97.6 2.8 99.5 3.2

chlorpropham 97.9 12 98.9 2.9 93.3 2.2

chlorpyrifos 92.2 13 94.7 2.2 99.5 4.4

chrysene 90.4 7.9 96.2 3.8 94.7 1.6

cyanazine 93.2 6.4 19.2 3.8 99.1 3.7
 

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 H2O Phobic DVB 

SPE Columns (Cartridges); Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

cycloate 86.1 3.4 93.8 1.7 94.6 1.9

dacthal (DCPA) 91.2 8.3 100 3.0 99.6 2.8

DDD, 4,4′- 98.4 1.2 98.1 2.9 98.5 3.2

DDE, 4,4′- 90.9 4.9 93.4 2.5 103 2.8

DDT, 4,4′- 99.7 4.0 99.1 2.0 98.7 2.8

DEET 95.9 4.8 97.9 2.1 93.9 2.2

di(2-ethylhexyl)adipate 96.2 7.8 101 6.2 95.2 1.3

di(2-ethylhexyl)phthalate NDe 106 9.1 92.5 3.0

dibenzo[a,h]anthracene 85.8 14 89.7 10 101 5.6

dibutylphthalate 94.7 32 105 4.2 102 3.3

dichlorvos 94.4 5.0 101 2.0 93.8 4.9

dieldrin 94.8 7.8 98.2 3.6 101 1.2

diethylphthalate 88.4 5.5 98.6 1.4 94.1 0.60

dimethipin 85.1 17 36.8 6.5 25.2 1.8

dimethylphthalate 97.6 6.7 96.8 1.8 95.1 2.6

DIMP 98.1 2.5 92.7 3.3 91.7 2.1

dinitrotoluene, 2,4- ND 97.9 4.1 92.1 1.3

dinitrotoluene, 2,6- ND 95.7 1.7 92.1 3.1

diphenamid 101 4.4 95.3 3.4 98.5 3.2

disulfoton 90.7 5.5 73.9 6.0 94.2 5.1

endosulfan I 98.5 2.6 95.3 4.2 100 2.5

endosulfan II 98.8 4.2 91.6 4.9 104 2.4

endosulfan sulfate 98.2 7.5 97.6 4.4 99.7 4.6

endrin 86.8 8.6 101 4.8 101 4.5

EPTC 88.2 5.7 96.5 2.6 92.8 1.3

ethion 97.5 7.0 94.0 3.0 97.4 3.8

ethoprop 85.9 4.2 98.6 3.1 93.3 3.3

ethyl parathion 79.2 14 99.9 2.4 96.1 3.0
 

525.3-80 

Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE Columns (Cartridges); Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

etridiazole 97.8 4.0 93.6 2.3 93.7 0.94

fenarimol 101 3.1 94.4 3.4 96.0 5.6

fluorene 84.0 4.0 92.2 1.7 93.3 0.71

fluridone 110 13 98.2 6.1 104 1.4

HCCPD 58.3 13 75.0 3.5 80.4 2.0

HCH, α 95.3 4.5 101 1.7 100 2.7

HCH, β 98.7 4.6 100 2.8 101 3.4

HCH, δ 98.0 2.6 97.5 2.8 105 2.2

HCH, γ (lindane) 98.1 5.6 97.4 3.2 101 1.7

heptachlor 85.6 4.6 89.2 3.6 95.5 2.3

heptachlor epoxide 97.5 3.2 99.2 3.5 102 0.66

hexachlorobenzene 68.1 5.9 90.0 3.3 95.6 0.80

hexazinone 98.8 9.7 96.4 3.2 99.3 2.0

indeno[1,2,3-c,d]pyrene 102 17 91.8 9.3 96.1 3.8

isophorone 90.6 2.0 93.1 2.3 93.7 1.6

methoxychlor 96.8 6.5 102 3.0 95.1 1.3

methyl parathion 93.8 8.3 98.2 3.2 95.6 4.0

metolachlor 91.1 6.4 95.3 2.0 99.6 2.4

metribuzin 110 3.2 87.4 5.6 97.2 3.8

mevinphos 94.3 10 97.7 1.4 91.3 1.7

MGK 264(a) 100 5.2 94.1 2.9 105 5.5

MGK 264(b) 92.5 4.4 93.9 8.0 104 5.3

molinate 77.2 9.8 88.8 2.1 92.1 2.7

napropamide 91.0 5.3 94.2 2.3 97.4 2.6

nitrofen 90.2 9.1 98.1 4.0 94.9 3.7

nonachlor, trans 84.5 3.7 98.0 4.2 102 2.7

norflurazon 94.1 10 93.0 4.8 99.9 4.3

oxyfluorfen 89.9 8.3 99.7 1.9 96.7 2.2
 

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 H2O Phobic DVB 

SPE Columns (Cartridges); Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

pebulate 90.3 3.3 92.9 2.2 92.5 2.3

pentachlorophenol 85.8 6.0 95.4 2.5 98.5 4.5

permethrin, cis 91.6 4.4 99.3 3.2 91.2 2.8

permethrin, trans 93.6 3.8 92.8 3.2 92.2 1.7

phenanthrene 86.9 1.1 94.9 2.8 96.3 2.0

phorate 90.4 1.6 87.1 2.1 90.0 1.7

phosphamidon 109 8.6 97.2 4.0 95.2 2.8

profenofos 99.9 11 95.6 6.9 102 4.1

prometon 83.1 4.0 98.6 2.8 90.4 4.2

prometryn 103 4.7 99.8 2.5 99.3 2.5

pronamide 94.1 6.0 99.1 2.2 95.8 1.6

propachlor 94.5 0.94 98.6 1.2 96.5 0.77

propazine 107 4.1 98.9 2.2 97.3 3.3

pyrene 92.0 2.7 96.0 2.3 100 2.3

simazine 88.0 9.3 98.3 2.2 96.4 1.7

simetryn 92.4 6.0 97.3 2.1 108 3.5

tebuconazole 106 3.2 96.9 2.8 94.2 1.1

tebuthiuron 91.7 5.6 97.0 2.5 95.2 2.3

terbacil 82.6 9.0 102 5.7 97.7 3.0

terbutryn 99.4 2.8 99.0 1.7 100 3.1

tetrachlorvinphos 96.8 5.6 88.6 3.3 99.1 3.3

triadimefon 102 11 112 3.4 96.4 4.1

tribufos+merphos 119 2.2 90.4 2.7 100 3.4

trifluralin 92.5 3.3 98.9 1.3 93.9 0.71

vernolate 92.0 1.2 96.7 2.0 94.0 0.71

vinclozolin 98.8 6.6 101 3.1 97.9 3.8

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 84.7 4.6 92.9 2.4 90.5 0.78
 

525.3-82 

Table 5. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE Columns (Cartridges); Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

4-chlorobiphenyl (3) 81.8 6.5 92.8 2.2 90.0 1.2

2,4′-dichlorobiphenyl (8) 85.4 5.6 93.8 1.7 91.5 1.0

2,2′,5-trichlorobiphenyl (18) 80.4 2.3 93.9 3.9 92.9 4.2

2,4,4′-trichlorobiphenyl (28) 85.0 7.6 91.5 4.8 94.9 3.9

2,2′,3,5′-tetrachlorobiphenyl (44) 88.7 4.2 91.6 3.5 101 2.9

2,2′,5,5′-tetrachlorobiphenyl (52) 84.5 3.6 93.4 2.7 98.5 3.3

2,3′,4′,5-tetrachloroobiphenyl (70) 89.2 3.5 94.6 2.1 101 2.3

2,3,3′,4′,6-pentachlorobiphenyl (110) 93.6 3.0 99.1 1.8 102 2.0

2,3′,4,4′,5-pentachlorobiphenyl (118) 92.8 4.1 99.2 1.6 104 4.5

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 94.0 0.77 99.8 3.5 103 3.7

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 94.6 4.2 100 3.1 104 3.3

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 97.5 2.5 99.3 3.5 104 2.9

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 93.6 9.9 102 5.9 99.9 1.1

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 88.3 1.0 92.5 1.5 95.7 1.0

benzo[a]pyrene-d12 92.2 3.7 88.8 4.3 94.6 3.9

triphenyl phosphate 99.7 2.2 94.0 2.2 91.1 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 μg/L, pentachlorophenol 

is 1.0 μg/L, tebuconazole is 1.2 μg/L, c-permethrin is 0.14 μg/L, t-permethrin is 0.36 μg/L, MGK 264(a) is 0.20 

μg/L and MGK 264(b) is 0.05 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, tebuconazole is 10.0 μg/L, c-permethrin is 1.1μg/L, t-permethrin is 2.9μg/L, and MGK 264(a) is 1.6 

μg/L and MGK 264(b) is 0.4 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20.0 μg/L, tebuconazole is 25.0 μg/L, c-permethrin is 2.8 μg/L, t-permethrin is 7.2 μg/L, and MGK 264(a) is 

4.0μg/L and MGK 264(b) is 1.0 μg/L.

e. ND = Not determined. Analyte could not be determined because of the low concentration.
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 84.8 1.5 91.5 2.0

acetochlor 2.0 106 2.2 103 2.7

alachlor 2.0 108 3.4 104 1.0

aldrin 2.0 90.6 4.0 85.5 4.2

ametryn 2.0 92.2 6.5 87.5 5.3

anthracene 2.0 97.7 3.2 99.3 2.8

atraton 2.0 94.2 2.7 86.0 4.8

atrazine 2.0 97.3 2.4 90.9 2.0

benzo[a]anthracene 2.0 101 2.6 96.4 2.3

benzo[a]pyrene 2.0 105 4.8 97.5 6.0

benzo[b]fluoranthene 2.0 101 3.1 100 2.1

benzo[g,h,i]perylene 2.0 121 2.4 118 3.2

benzo[k]fluoranthene 2.0 106 3.5 102 1.7

BHT 2.0 96.4 1.6 109 2.0

bromacil 2.0 104 2.2 123 16

butachlor 2.0 103 3.1 104 2.8

butylate 2.0 100 1.6 97.8 2.8

butylbenzylphthalate 2.0 116 3.9 208 94

chlordane, cis- 2.0 99.5 2.4 98.3 3.5

chlordane, trans 2.0 92.6 2.8 93.0 3.2

chlorfenvinphos 2.0 101 2.6 102 5.4

chlorobenzilate 2.0 106 3.9 105 5.8

chloroneb 2.0 84.4 1.0 83.4 1.8

chlorothalonil 2.0 97.2 1.8 96.2 3.2

chlorpropham 2.0 89.7 3.3 100 2.2

chlorpyrifos 2.0 104 6.4 99.9 4.4

chrysene 2.0 105 3.2 101 2.8

cyanazine 2.0 108 1.2 98.0 3.0
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

cycloate 2.0 97.0 1.9 94.4 1.3

dacthal (DCPA) 2.0 96.0 4.0 97.8 2.0

DDD, 4,4′- 2.0 97.5 3.4 98.2 3.4

DDE, 4,4′- 2.0 94.4 1.8 95.0 3.7

DDT, 4,4′- 2.0 109 3.6 109 3.5

DEET 2.0 101 2.9 97.5 0.63

di(2-ethylhexyl)adipate 2.0 99.7 3.8 123 24

di(2-ethylhexyl)phthalate 2.0 106 1.7 126 29

dibenzo[a,h]anthracene 2.0 116 3.8 102 7.2

dibutyl phthalate 2.0 122 3.7 114 2.7

dichlorvos 2.0 82.3 3.2 92.1 2.0

diethylphthalate 2.0 94.3 3.5 94.4 3.5

dimethipin 2.0 49.2 11 34.9 4.6

dimethylphthalate 2.0 92.7 1.4 94.1 2.7

DIMP 2.0 91.2 2.3 87.7 1.9

dinitrotoluene, 2,4- 2.0 78.9 3.8 96.3 3.1

dinitrotoluene, 2,6- 2.0 102 4.8 111 4.7

diphenamid 2.0 109 3.9 98.2 4.7

disulfoton 2.0 81.4 2.4 74.5 1.9

endosulfan I 2.0 97.8 5.1 95.8 4.0

endosulfan II 2.0 98.9 3.0 103 8.3

endosulfan sulfate 2.0 101 4.8 98.6 3.7

endrin 2.0 105 5.7 110 6.2

EPTC 2.0 92.6 2.9 91.9 0.36

ethion 2.0 106 3.3 106 4.1

ethoprop 2.0 97.2 0.57 93.2 4.3

ethyl parathion 2.0 87.4 4.1 88.0 4.8

etridiazole 2.0 100 3.4 103 2.4
 

525.3-85 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

fenarimol 2.0 100 3.2 98.6 1.9

fluorene 2.0 93.1 1.1 95.9 1.6

fluridone 2.0 94.4 5.8 98.0 1.8

HCCPD 2.0 105 2.4 105 5.2

HCH, α 2.0 97.9 0.92 95.5 2.9

HCH, β 2.0 101 3.4 97.0 2.9

HCH, δ 2.0 95.1 2.0 88.2 2.1

HCH, γ (lindane) 2.0 95.7 3.1 96.4 2.2

heptachlor 2.0 111 3.3 105 1.4

heptachlor epoxide 2.0 94.6 4.2 99.0 1.9

hexachlorobenzene 2.0 87.6 1.6 85.8 2.8

hexazinone 2.0 110 6.7 100 2.8

indeno[1,2,3-c,d]pyrene 2.0 115 1.5 112 4.8

isophorone 2.0 90.7 2.6 90.2 1.8

methoxychlor 2.0 99.0 2.2 106 2.0

methyl parathion 2.0 101 4.1 104 3.0

metolachlor 2.0 105 3.4 102 2.7

metribuzin 2.0 74.7 2.9 76.0 2.8

mevinphos 2.0 84.2 2.6 93.7 3.1

MGK 264(a) 1.6 102 4.0 102 3.1

MGK 264(b) 0.4 100 5.1 104 3.2

molinate 2.0 90.6 2.0 88.6 2.3

napropamide 2.0 105 2.4 102 6.2

nitrofen 2.0 105 4.7 107 7.1

nonachlor, trans 2.0 99.0 3.3 95.9 1.0

norflurazon 2.0 83.2 8.1 97.5 6.4

oxyfluorfen 2.0 109 3.0 110 4.1

pebulate 2.0 94.5 4.0 92.4 2.7
 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

pentachlorophenol 8.0 87.7 3.9 92.5 2.6

permethrin, cis 1.1 95.7 0.88 102 2.8

permethrin, trans 2.9 94.4 2.0 97.8 2.1

phenanthrene 2.0 98.6 2.4 98.5 1.5

phorate 2.0 89.1 0.39 97.3 2.7

phosphamidon 2.0 106 4.8 105 5.6

profenofos 2.0 109 3.8 102 13

prometon 2.0 92.1 3.9 83.6 3.2

prometryn 2.0 95.5 3.4 89.3 2.2

pronamide 2.0 105 2.5 99.8 1.6

propachlor 2.0 100 1.8 97.6 1.4

propazine 2.0 102 2.2 93.3 3.1

pyrene 2.0 105 5.6 102 4.0

simazine 2.0 75.4 0.82 74.0 2.1

simetryn 2.0 93.0 3.2 90.7 5.3

tebuconazole 10.0 108 3.9 108 1.9

tebuthiuron 2.0 92.1 2.5 84.2 2.8

terbacil 2.0 105 4.8 108 6.9

terbutryn 2.0 101 3.3 94.5 4.3

tetrachlorvinphos 2.0 98.9 2.7 101 4.3

triadimefon 2.0 102 3.7 99.1 5.5

tribufos+merphos 2.0 108 4.0 110 4.6

trifluralin 2.0 100 2.6 103 2.3

vernolate 2.0 92.9 0.68 90.4 2.1

vinclozolin 2.0 98.7 2.7 100 0.61

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 83.5 1.0 83.8 2.0

4-chlorobiphenyl (3) 2.0 91.9 2.6 89.3 2.3
 

525.3-87 

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

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

2,4′-dichlorobiphenyl (8) 2.0 85.1 1.8 87.4 1.8

2,2′,5-trichlorobiphenyl (18) 2.0 89.5 3.9 90.9 2.8

2,4,4′-trichlorobiphenyl (28) 2.0 91.6 2.6 88.9 2.0

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 96.9 3.6 96.2 2.0

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 93.5 1.9 93.5 2.4

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 95.6 2.6 96.1 2.3

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 93.5 1.6 92.2 3.1

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 92.0 2.5 94.9 3.5

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 93.4 2.7 93.5 4.6

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 97.9 1.2 101 2.2

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 97.0 3.3 97.2 2.5

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 89.1 3.3 99.0 4.9

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 5.0 83.3 6.4 91.4 0.40

benzo[a]pyrene-d12 5.0 94.0 4.2 90.5 2.6

triphenyl phosphate 5.0 104 4.0 107 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. 
 

525.3-88 

Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE; Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 87.9 1.9 84.6 5.1 90.4 1.8

acetochlor 110 4.0 99.4 3.5 105 3.1

alachlor 107 5.0 92.5 3.8 110 2.4

aldrin 92.7 2.5 82.2 3.8 104 3.5

ametryn 96.6 3.2 89.5 7.3 99.2 5.7

anthracene 85.6 3.2 86.7 4.3 104 2.4

atraton 96.4 12 92.1 4.9 100 2.0

atrazine 96.8 6.7 94.2 2.6 103 2.9

benzo[a]anthracene 85.6 0.43 94.0 4.9 90.1 0.88

benzo[a]pyrene 94.5 11 81.3 5.9 94.6 3.5

benzo[b]fluoranthene 90.2 2.6 88.6 6.5 94.3 2.5

benzo[g,h,i]perylene 89.5 10 93.0 7.5 96.6 3.8

benzo[k]fluoranthene 103 7.4 90.1 4.7 94.1 2.8

BHT 50.4 11 107 2.6 85.4 1.8

bromacil 102 8.2 99.6 28 106 1.8

butachlor 103 2.1 95.5 2.7 105 2.0

butylate 91.5 2.6 87.6 3.6 95.8 1.4

butylbenzylphthalate 91.3 5.8 121 5.7 108 1.5

chlordane, cis 106 5.2 94.9 4.9 105 4.3

chlordane, trans 101 5.3 89.6 5.2 104 4.4

chlorfenvinphos 106 5.3 99.3 2.7 104 0.78 

chlorobenzilate 106 4.7 96.7 4.4 107 1.7

chloroneb 95.5 2.9 82.0 6.0 94.3 1.8

chlorothalonil 96.0 5.6 83.8 5.6 103 2.5

chlorpropham 77.3 12 88.7 11 102 1.4

chlorpyrifos 101 13 98.7 4.2 110 3.0

chrysene 96.5 7.9 95.4 5.2 94.2 0.73 

cyanazine 101 6.4 91.8 6.7 106 2.5
 

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 H2O Phobic DVB 

SPE; Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

cycloate 94.0 3.4 89.1 2.4 98.8 1.7

dacthal (DCPA) 93.2 8.3 89.8 3.5 101 1.9

DDD, 4,4′- 95.8 1.2 94.5 3.5 102 2.2

DDE, 4,4′- 95.2 4.9 89.2 3.2 106 3.4

DDT, 4,4′- 98.2 4.0 86.5 6.5 104 3.0

DEET 98.7 4.8 89.4 6.0 99.3 0.64 

di(2-ethylhexyl)adipate 96.1 7.8 105 8.3 97.6 0.91 

di(2-ethylhexyl)phthalate NDe 104 9.3 94.4 3.7

dibenzo[a,h]anthracene 101 14 90.9 10 106 3.1

dibutylphthalate 99.1 32 110 3.5 107 2.9

dichlorvos 109 5.0 100 9.5 102 2.3

dieldrin 106 7.8 95.9 3.9 109 4.6

diethylphthalate 90.8 5.5 87.7 4.8 98.8 1.0

dimethipin 83.7 17 76.1 5.5 64.6 4.1

dimethylphthalate 93.3 6.7 87.2 5.8 96.2 1.2

DIMP 101 2.5 84.6 7.2 97.0 0.36

dinitrotoluene, 2,4- 77.5 3.3 87.4 16 99.8 3.5

dinitrotoluene, 2,6- NDf 97.3 14 92.2 1.1

diphenamid 105 4.4 95.4 4.9 108 1.9

disulfoton 80.0 5.5 80.4 10 96.7 2.7

endosulfan I 109 2.6 92.3 5.6 107 2.4

endosulfan II 99.6 4.2 96.8 3.7 110 2.3

endosulfan sulfate 96.6 7.5 90.0 5.7 103 2.0

endrin 110 8.6 120 8.4 107 2.5

EPTC 93.8 5.7 85.0 5.7 94.8 0.59

ethion 98.4 7.0 98.7 2.8 101 1.1

ethoprop 108 4.2 95.9 7.7 103 2.8

ethyl parathion 90.6 14 90.0 9.6 104 2.3
 

525.3-90 

Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE; Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

etridiazole 88.8 4.0 84.5 11 96.8 1.9

fenarimol 123 3.1 103 6.7 101 1.6

fluorene 82.5 4.0 85.5 5.2 94.1 0.86

fluridone 108 13 87.2 16 110 4.5

HCCPD 67.5 13 77.7 12 88.4 2.1

HCH, α 101 4.5 88.2 4.9 102 0.18

HCH, β 99.4 4.6 92.1 5.5 105 2.9

HCH, δ 104 2.6 91.4 5.0 112 2.6

HCH, γ (lindane) 95.1 5.6 92.9 3.2 104 1.9

heptachlor 87.3 4.6 91.1 5.8 104 2.9

heptachlor epoxide 98.9 3.2 98.0 5.2 104 2.6

hexachlorobenzene 79.4 5.9 76.4 5.6 95.7 0.52 

hexazinone 107 9.7 89.1 4.2 103 1.3

indeno[1,2,3-c,d]pyrene 87.8 17 94.9 4.5 98.1 2.9

isophorone 96.4 2.0 85.1 4.3 97.5 0.52 

methoxychlor 97.4 6.5 98.7 9.8 96.3 0.80 

methyl parathion 103 8.3 92.1 4.2 102 3.5

metolachlor 99.0 6.4 94.4 4.5 106 2.7

metribuzin 93.7 3.2 81.0 2.8 99.8 2.5

mevinphos 94.2 10 88.3 13 100 3.9

MGK 246(a) 105 5.2 92.2 4.5 110 2.2

MGK 264(b) 95.5 4.4 98.0 5.0 107 2.2

molinate 93.2 9.8 87.2 4.8 98.4 3.6

napropamide 106 5.3 90.6 4.2 107 1.6

nitrofen 103 9.1 97.4 8.3 99.4 3.5

nonachlor, trans 90.1 3.7 86.0 4.5 103 1.5

norflurazon 102 10 96.1 14 110 0.76

oxyfluorfen 98.3 8.3 93.2 4.6 101 1.2
 

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 H2O Phobic DVB 

SPE; Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

pebulate 95.0 3.3 84.6 3.4 94.2 1.8

pentachlorophenol 93.5 6.0 111 3.9 101 4.2

permethrin, cis 89.5 4.4 96.3 7.0 93.8 1.5

permethrin, trans 91.6 3.8 90.4 6.7 96.1 2.7

phenanthrene 87.8 1.1 93.4 3.3 98.1 2.5

phorate 86.5 1.6 86.3 2.5 94.4 1.2

phosphamidon 103 8.6 105 4.3 108 1.9

profenofos 116 11 99.0 5.2 104 2.1

prometon 76.7 4.0 97.3 4.6 91.7 4.7

prometryn 99.7 4.7 91.4 5.0 101 2.4

pronamide 96.8 6.0 95.6 3.7 101 2.7

propachlor 98.3 0.9 88.0 4.4 103 1.0

propazine 95.0 4.1 88.5 3.9 102 2.6

pyrene 99.2 2.7 98.0 2.3 103 0.91 

simazine 89.5 9.3 83.8 5.8 99.6 3.7

simetryn 99.1 6.0 91.2 3.9 112 2.9

tebuconazole 107 3.2 100 8.2 100 0.91 

tebuthiuron 94.1 5.6 84.1 4.0 101 0.19

terbacil 98.2 9.0 95.1 3.6 110 2.6

terbutryn 103 2.8 91.2 4.7 105 2.9

tetrachlorvinphos 108 5.6 97.5 4.0 110 3.8

triadimefon 110 11 94.4 4.9 103 3.4

tribufos+merphos 126 2.2 96.3 5.3 107 2.0

trifluralin 84.3 3.3 89.6 8.7 95.5 0.67 

vernolate 97.2 1.2 85.9 5.8 95.0 2.8

vinclozolin 95.0 6.6 96.1 3.5 102 1.4

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 90.2 4.6 78.9 4.7 91.0 2.2
 

525.3-92 

Table 7. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent 

Water at Three Concentrations and Extracted Using J.T. Baker Speedisk H2O Phobic DVB 

SPE; Full Scan GC/MS Analysesa 

Analytes

Fortified Conc.

0.25 μg/Lb 

n=4

Fortified Conc.

2.0 μg/Lc 

n=8

Fortified Conc.

5.0 μg/Ld 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

4-chlorobiphenyl (3) 87.9 6.5 80.5 5.8 92.7 0.82 

2,4-dichlorobiphenyl (8) 85.3 5.6 78.6 5.5 94.2 1.5

2,2′,5-trichlorobiphenyl (18) 90.7 2.3 85.9 4.7 94.9 4.0

2,4,4′-trichlorobiphenyl (28) 93.2 7.6 90.0 6.7 103 2.1

2,2′,3,5′-tetrachlorobiphenyl (44) 97.5 4.2 89.5 3.9 108 2.4

2,2′,5,5′-tetrachlorobiphenyl (52) 89.0 3.6 95.0 3.1 103 1.7

2,3′,4′,5-tetrachloroobiphenyl (70) 102 3.5 89.6 3.8 106 3.6

2,3,3′,4′,6-pentachlorobiphenyl (110) 98.0 3.0 89.1 2.7 102 2.4

2,3′,4,4′,5-pentachlorobiphenyl (118) 96.0 4.1 90.3 3.5 105 1.6

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 93.7 0.8 90.9 3.3 105 3.4

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 96.4 4.2 92.4 2.0 103 2.8

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 98.3 2.5 90.0 5.3 104 3.5

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 87.2 9.9 88.4 6.5 95.3 2.2

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 98.0 1.0 95.5 3.9 102 2.4

benzo[a]pyrene-d12 101 3.7 82.1 3.1 91.9 2.2

triphenyl phosphate 103 2.2 110 3.8 97.0 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 μg/L, pentachlorophenol 

is 1.0 μg/L, tebuconazole is 1.2 μg/L, c-permethrin is 0.14 μg/L, t-permethrin is 0.36 μg/L, MGK 264(a) is 0.20 

μg/L and MGK 264(b) is 0.05 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, tebuconazole is 10.0 μg/L, c-permethrin is 1.1μg/L, t-permethrin is 2.9μg/L, and MGK 264(a) is 1.6 

μg/L and MGK 264(b) is 0.4 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20.0 μg/L, tebuconazole is 25.0 μg/L, c-permethrin is 2.8 μg/L, t-permethrin is 7.2 μg/L, and MGK 264(a) is 

4.0μg/L and MGK 264(b) is 1.0 μg/L.

e. ND = Not determined. Analyte could not be determined because of the low fortified concentration relative to 

the LRB.

f. ND = Not determined. Analyte could not be determined due to poor instrument sensitivity at this concentration.
 

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 

Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 98.8 2.4 87.5 1.1

acetochlor 2.0 123 4.2 101 4.4

alachlor 2.0 116 5.8 91.6 3.8

aldrin 2.0 102 3.1 80.5 4.3

ametryn 2.0 113 2.0 82.7 2.0

anthracene 2.0 103 3.2 88.6 3.9

atraton 2.0 114 4.3 83.0 6.4

atrazine 2.0 119 5.9 93.0 4.8

benzo[a]anthracene 2.0 93.6 2.6 95.2 2.1

benzo[a]pyrene 2.0 80.2 4.5 85.6 11

benzo[b]fluoranthene 2.0 89.5 2.8 88.8 6.1

benzo[g,h,i]perylene 2.0 90.7 3.5 92.9 5.0

benzo[k]fluoranthene 2.0 88.6 2.3 87.8 3.4

BHT 2.0 121 3.6 109 0.46

bromacil 2.0 99.1 2.6 115 4.4

butachlor 2.0 114 3.3 99.1 5.6

butylate 2.0 104 4.0 92.0 4.6

butylbenzylphthalate 2.0 115 2.4 95.9 4.4

chlordane, cis- 2.0 118 7.2 93.1 6.0

chlordane, trans 2.0 114 4.3 85.1 4.4

chlorfenvinphos 2.0 116 3.7 95.9 7.4

chlorobenzilate 2.0 123 2.9 95.2 5.5

chloroneb 2.0 95.8 2.1 82.9 2.5

chlorothalonil 2.0 102 4.8 82.8 5.0

chlorpropham 2.0 100 5.5 99.3 1.1

chlorpyrifos 2.0 123 2.5 88.4 3.3

chrysene 2.0 95.0 6.3 93.9 2.9

cyanazine 2.0 121 4.4 84.4 6.2
 

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 

Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

cycloate 2.0 105 3.2 91.9 1.9

dacthal (DCPA) 2.0 116 4.2 89.9 4.6

DDD, 4,4′- 2.0 119 3.4 94.1 4.9

DDE, 4,4′- 2.0 113 4.1 87.4 5.2

DDT, 4,4′- 2.0 112 3.5 87.5 6.0

DEET 2.0 106 1.9 95.4 1.2

di(2-ethylhexyl)adipate 2.0 112 6.4 102 1.9

di(2-ethylhexyl)phthalate 2.0 113 7.4 108 5.2

dibenzo[a,h]anthracene 2.0 90.4 3.8 90.0 5.3

dibutyl phthalate 2.0 132 4.2 102 5.1

dichlorvos 2.0 116 4.2 112 2.7

dieldrin 2.0 126 4.0 101 5.8

diethylphthalate 2.0 103 3.8 89.1 1.7

dimethipin 2.0 98.6 7.0 77.8 3.1

dimethylphthalate 2.0 103 4.1 89.1 2.6

DIMP 2.0 111 4.7 88.7 4.9

dinitrotoluene, 2,4- 2.0 87.9 3.7 100 4.9

dinitrotoluene, 2,6- 2.0 110 7.9 110 1.3

diphenamid 2.0 121 5.1 95.5 5.3

disulfoton 2.0 91.9 4.8 84.9 1.8

endosulfan I 2.0 121 1.7 90.4 5.8

endosulfan II 2.0 117 6.1 93.9 12

endosulfan sulfate 2.0 112 5.1 84.9 6.0

endrin 2.0 103 8.8 115 3.3

EPTC 2.0 100 3.1 89.5 3.1

ethion 2.0 112 1.4 102 4.4

ethoprop 2.0 112 2.3 104 1.2

ethyl parathion 2.0 95.4 5.7 99.8 1.1
 

525.3-95 

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 

Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

etridiazole 2.0 105 2.9 90.5 2.8

fenarimol 2.0 99.3 4.8 111 2.8

fluorene 2.0 99.6 3.5 88.9 1.6

fluridone 2.0 86.3 3.5 82.8 2.4

HCCPD 2.0 96.6 2.5 82.9 6.3

HCH, α 2.0 105 3.5 90.0 1.1

HCH, β 2.0 111 3.7 88.7 4.2

HCH, δ 2.0 107 5.2 84.4 5.2

HCH, γ (lindane) 2.0 118 4.3 86.3 2.7

heptachlor 2.0 116 5.1 84.5 7.2

heptachlor epoxide 2.0 121 3.4 93.0 2.8

hexachlorobenzene 2.0 94.8 4.0 78.1 2.8

hexazinone 2.0 104 4.1 79.3 5.6

indeno[1,2,3-c,d]pyrene 2.0 87.3 4.3 103 7.7

isophorone 2.0 103 3.7 89.8 3.1

methoxychlor 2.0 109 3.2 102 3.8

methyl parathion 2.0 107 4.7 100 5.0

metolachlor 2.0 120 3.0 94.9 4.2

metribuzin 2.0 101 5.0 80.6 2.7

mevinphos 2.0 94.3 2.6 94.2 2.6

MGK 246(a) 1.6 116 5.6 94.7 5.5

MGK 264(b) 0.4 114 4.3 89.4 9.9

molinate 2.0 101 3.6 89.3 1.8

napropamide 2.0 112 3.9 87.1 6.4

nitrofen 2.0 121 1.8 101 5.6

nonachlor, trans 2.0 108 3.9 83.8 3.4

norflurazon 2.0 106 2.4 102 6.8

oxyfluorfen 2.0 114 1.9 101 5.6
 

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 

Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

pebulate 2.0 98.0 4.6 84.4 1.7

pentachlorophenol 8.0 118 2.3 110 3.8

permethrin, cis 1.1 93.9 4.8 93.4 4.8

permethrin, trans 2.9 94.8 4.7 92.7 2.5

phenanthrene 2.0 110 5.1 92.2 4.0

phorate 2.0 94.8 3.7 89.1 2.4

phosphamidon 2.0 126 5.2 97.6 3.9

profenofos 2.0 120 4.8 97.7 8.0

prometon 2.0 117 4.6 82.6 3.5

prometryn 2.0 118 3.7 86.2 4.9

pronamide 2.0 119 3.7 94.6 4.4

propachlor 2.0 104 1.9 94.2 1.3

propazine 2.0 113 4.1 85.2 3.2

pyrene 2.0 119 2.1 96.8 4.3

simazine 2.0 103 2.4 81.6 6.7

simetryn 2.0 116 4.0 88.3 6.5

tebuconazole 10.0 105 2.6 97.8 4.2

tebuthiuron 2.0 101 4.3 81.9 3.7

terbacil 2.0 120 4.1 101 4.7

terbutryn 2.0 113 2.5 85.9 3.6

tetrachlorvinphos 2.0 115 5.6 95.8 6.0

triadimefon 2.0 121 3.4 93.9 5.4

tribufos+merphos 2.0 121 2.1 102 6.1

trifluralin 2.0 110 2.7 94.8 2.7

vernolate 2.0 105 2.2 91.0 1.1

vinclozolin 2.0 117 4.6 96.1 5.1

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 94.2 2.8 81.3 2.0
 

525.3-97 

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 

Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

4-chlorobiphenyl (3) 2.0 92.9 1.3 85.3 1.9

2,4-dichlorobiphenyl (8) 2.0 93.2 1.9 80.4 1.2

2,2′,5-trichlorobiphenyl (18) 2.0 109 4.7 86.4 4.9

2,4,4′-trichlorobiphenyl (28) 2.0 118 8.4 88.3 4.4

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 112 3.2 89.1 6.3

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 121 2.4 95.4 5.3

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 114 4.2 91.4 6.2

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 113 3.7 88.3 4.5

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 113 3.1 89.2 5.9

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 116 3.6 88.3 6.8

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 119 3.1 93.8 4.1

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 112 5.2 88.4 5.3

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 90.9 7.7 83.8 3.4

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 5.0 111 3.3 102 1.5

benzo[a]pyrene-d12 5.0 79.8 3.4 86.0 2.8

triphenyl phosphate 5.0 115 3.7 115 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. 
 

525.3-98 

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 Analysesa 

Analytes 

Fortified Conc.

0.20 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 90.0 4.5 87.9 2.6 86.4 5.4

acetochlor 106 4.5 94.5 2.6 90.0 7.6

alachlor 98.8 6.4 92.0 1.9 92.3 8.2

aldrin 91.3 5.2 80.5 3.1 86.6 7.1

ametryn 106 5.9 90.8 4.6 94.3 9.2

anthracene 98.8 4.8 91.1 2.3 89.4 5.7

atraton 109 4.4 90.2 2.3 91.8 7.3

atrazine 105 3.9 91.1 3.5 91.6 8.0

benzo[a]anthracene 95.0 4.3 91.6 1.9 91.0 5.1

benzo[a]pyrene 96.3 7.8 88.0 3.5 88.9 5.9

benzo[b]fluoranthene 106 5.9 90.6 1.5 91.9 6.2

benzo[g,h,i]perylene 108 6.0 87.0 5.4 89.4 6.9

benzo[k]fluoranthene 111 4.3 89.4 1.6 89.4 5.6

BHT 97.5 8.9 81.0 4.4 81.7 7.0

bromacil 124 2.0 90.2 3.5 96.4 7.2

butachlor 115 3.5 92.1 3.7 93.2 8.0

butylate 100 4.1 88.6 3.6 87.1 6.9

butylbenzylphthalate 131 6.5 94.1 3.3 96.3 7.4

chlordane, cis 96.3 5.0 90.7 2.9 88.8 7.9

chlordane, trans 96.3 5.0 90.8 3.0 89.3 7.3

chlorfenvinphos 123 2.4 92.4 3.5 95.9 7.0

chlorobenzilate 105 3.9 92.9 3.7 92.9 8.4

chloroneb 283 10 101 4.1 96.6 7.1

chlorothalonil 98.8 2.5 88.6 2.8 88.4 7.3

chlorpropham 113 5.7 90.5 3.0 90.2 6.7

chlorpyrifos 96.3 5.0 93.3 3.1 89.6 7.3

chrysene 72.5 12 89.2 5.7 89.4 5.2

cyanazine 101 4.7 88.8 5.8 90.5 9.0

cycloate 90.0 4.5 90.1 0.99 91.6 7.1
 

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 Analysesa 

Analytes 

Fortified Conc.

0.20 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

dacthal (DCPA) 95.0 4.3 92.7 2.7 89.6 7.5

DDD, 4,4′- 92.5 3.1 93.3 2.7 88.7 7.9

DDE, 4,4′- 98.8 6.4 90.8 2.8 90.5 7.2

DDT, 4,4′- 113 4.4 87.8 2.7 92.5 7.9

DEET 103 4.9 92.7 2.9 90.1 7.2

di(2-ethylhexyl)adipate 129 4.9 90.9 3.4 96.4 9.0

di(2-ethylhexyl)phthalate 160 5.1 98.9 2.7 102 8.5

dibenzo[a,h]anthracene 104 4.6 90.7 4.2 90.2 7.9

dibutyl phthalate 741 9.8 105 2.9 125 7.5

dichlorvos 101 4.7 86.6 3.3 88.6 6.5

dieldrin 103 4.9 91.0 3.0 90.4 7.7

diethylphthalate 97.5 6.6 90.7 3.0 88.6 7.3

dimethipin 23.8 11 8.52 9.0 6.7 11

dimethylphthalate 90.0 4.5 90.2 3.2 87.0 7.4

DIMP 103 6.3 64.0 3.5 67.8 6.1

dinitrotoluene, 2,4- 116 5.4 90.5 2.2 90.4 6.7

dinitrotoluene, 2,6- 108 6.0 88.9 3.3 90.1 6.7

diphenamid 111 4.3 93.3 2.9 92.2 7.3

disulfoton 98.8 4.8 87.1 4.1 85.4 7.2

endosulfan I 77.5 3.7 92.8 2.9 89.5 8.1

endosulfan II 83.8 5.7 93.5 3.7 91.0 7.3

endosulfan sulfate 104 4.6 90.9 3.3 90.0 8.1

endrin 111 5.7 94.5 1.8 93.4 7.0

EPTC 100 4.1 89.0 3.1 88.2 6.8

ethion 120 3.4 94.2 3.1 93.7 8.1

ethoprop 114 2.2 94.0 2.5 92.3 6.5

ethyl parathion 121 3.9 91.2 3.0 93.1 7.8

etridiazole 110 3.7 90.2 1.7 87.1 7.1

fenarimol 123 5.3 93.0 4.9 95.7 7.3
 

525.3-100 

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 Analysesa 

Analytes 

Fortified Conc.

0.20 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

fluorene 90.0 4.5 89.8 2.6 86.6 5.6

fluridone 116 5.4 94.1 2.3 100 8.5

HCCPD 75.0 5.4 78.3 2.6 70.5 6.3

HCH, α 88.8 2.8 88.7 2.7 85.9 7.2

HCH, β 95.0 6.1 91.9 3.3 89.4 8.2

HCH, δ 101 2.5 89.9 3.6 89.0 7.6

HCH, γ (lindane) 93.8 6.7 91.8 2.5 88.2 7.4

heptachlor 86.3 5.6 88.4 4.4 86.4 8.0

heptachlor epoxide 98.8 2.5 92.5 1.9 90.2 7.7

hexachlorobenzene 82.5 7.8 87.2 1.8 83.7 5.4

hexazinone 121 3.9 92.2 2.4 97.0 7.7

indeno[1,2,3-c,d]pyrene 111 4.3 87.7 4.3 91.9 7.1

isophorone 98.8 8.6 82.9 4.2 82.3 5.7

methoxychlor 118 4.3 92.3 3.2 93.1 6.9

methyl parathion 123 5.3 91.5 3.2 92.8 7.6

metolachlor 109 5.8 93.1 3.1 92.9 7.9

metribuzin 113 4.4 90.9 3.3 90.9 7.2

mevinphos 118 5.5 80.6 4.9 87.8 6.4

MGK 264(a) 128 4.8 89.6 4.8 91.3 8.1

MGK 264(b) 123 6.1 92.4 2.9 93.6 7.6

molinate 103 2.8 90.7 2.6 88.3 6.7

napropamide 111 4.3 94.1 3.4 94.9 8.0

nitrofen 111 2.2 91.4 1.7 93.6 6.9

nonachlor, trans 93.8 6.7 90.6 2.9 88.6 8.0

norflurazon 123 5.3 89.9 4.2 95.8 9.0

oxyfluorfen 110 3.7 95.4 2.9 94.3 7.8

pebulate 101 4.7 89.9 3.6 87.6 6.5

pentachlorophenol 95.0 5.4 95.1 4.0 88.2 6.7

permethrin, cis 112 6.3 92.2 3.4 99.7 7.5
 

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 Analysesa 

Analytes 

Fortified Conc.

0.20 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

permethrin, trans 107 4.1 92.8 2.8 91.8 7.5

phenanthrene 95.0 4.3 92.2 2.1 90.0 5.9

phorate 121 3.9 88.2 2.1 85.7 7.5

phosphamidon 126 3.8 94.7 3.8 99.7 6.1

profenofos 125 3.3 93.4 2.5 94.9 7.3

prometon 111 5.7 91.4 3.1 93.5 7.7

prometryn 111 4.3 92.3 3.3 92.0 8.1

pronamide 118 5.5 94.4 3.6 93.9 7.6

propachlor 96.3 5.0 91.2 2.7 87.7 7.0

propazine 103 6.3 91.5 3.1 91.4 7.5

pyrene 98.8 4.8 92.5 2.1 91.0 6.0

simazine 108 2.7 90.7 3.3 91.0 7.9

simetryn 119 5.3 93.6 3.1 93.6 7.9

tebuconazole 126 2.0 89.5 1.5 95.6 9.9

tebuthiuron 116 7.3 94.0 4.4 100 5.0

terbacil 120 3.4 92.3 3.4 95.2 7.8

terbutryn 111 4.3 93.0 2.7 93.1 7.9

tetrachlorvinphos 125 3.3 92.1 3.4 97.4 7.2

triadimefon 105 8.7 93.9 2.4 94.5 7.6

tribufos+merphos 116 3.7 93.6 2.8 100 7.3

trifluralin 109 2.3 88.1 2.6 86.5 7.4

vernolate 100 4.1 90.0 2.9 87.2 6.9

vinclozolin 105 3.9 89.3 3.4 89.8 7.7

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 85.0 4.8 88.4 2.9 84.8 6.2

4-chlorobiphenyl (3) 90.0 4.5 89.2 2.6 85.6 6.1

2,4′-dichlorobiphenyl (8) 88.8 7.1 88.8 2.0 86.1 6.5

2,2′,5-trichlorobiphenyl (18) 82.5 6.1 90.3 3.1 88.3 6.8

2,4,4′-trichlorobiphenyl (28) 91.3 6.9 90.4 2.3 89.4 6.7
 

525.3-102 

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 Analysesa 

Analytes 

Fortified Conc.

0.20 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 91.3 6.9 91.1 3.1 89.9 7.6

2,2′,5,5′-tetrachlorobiphenyl (52) 95.0 4.3 90.6 2.9 89.6 6.6

2,3′,4′,5-tetrachloroobiphenyl (70) 91.3 6.9 91.1 2.9 90.5 7.0

2,3,3′,4′,6-pentachlorobiphenyl (110) 93.8 6.7 90.6 2.4 91.1 6.5

2,3′,4,4′,5-pentachlorobiphenyl (118) 97.5 6.6 91.2 2.3 91.4 6.7

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 90.0 4.5 91.3 3.1 91.1 7.6

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 93.8 5.1 91.1 3.0 91.5 7.0

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 95.0 4.3 91.2 1.7 91.6 7.6

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 88.8 5.4 92.5 1.9 90.9 5.2

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 93.8 3.6 93.3 3.5 87.9 7.1

benzo[a]pyrene-d12 79.6 3.8 90.2 2.0 91.2 4.2

triphenyl phosphate 86.4 5.2 102 4.2 94.9 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 μg/L, pentachlorophenol 

is 0.80 μg/L, MGK 246(a) is 0.067 μg/L, MGK 246(b) is 0.13 μg/L, tribufos+merphos is 0.40 μg/L, 

c-permethrin is 0.12 μg/L, and t-permethrin is 0.29 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, MGK 246(a) is 0.67 μg/L, MGK 246(b) is 1.3 μg/L, tribufos+merphos is 4.0 μg/L, c-permethrin is 

1.2 μg/L, and t-permethrin is 2.9 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20 μg/L, MGK 246(a) is 1.7 μg/L, MGK 246(b) is 3.3 μg/L, tribufos+merphos is 10 μg/L, c-permethrin is 

2.9 μg/L, and t-permethrin is 7.2 μg/L.
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 94.1 2.4 87.4 7.8

acetochlor 2.0 95.6 2.2 92.0 7.1

alachlor 2.0 98.1 3.3 92.4 7.2

aldrin 2.0 87.0 1.8 84.9 6.4

ametryn 2.0 101 2.2 92.0 9.2

anthracene 2.0 96.0 2.9 90.3 8.2

atraton 2.0 100 3.8 93.9 7.5

atrazine 2.0 99.1 3.1 91.4 7.1

benzo[a]anthracene 2.0 105 2.4 99.8 8.4

benzo[a]pyrene 2.0 95.1 3.4 91.5 9.8

benzo[b]fluoranthene 2.0 96.0 2.6 92.9 9.9

benzo[g,h,i]perylene 2.0 97.3 4.2 97.9 10

benzo[k]fluoranthene 2.0 124 3.5 118 8.2

BHT 2.0 91.3 3.7 87.5 7.3

bromacil 2.0 100 3.5 96.8 6.3

butachlor 2.0 98.3 2.5 94.3 6.9

butylate 2.0 96.4 3.0 90.5 7.8

butylbenzylphthalate 2.0 99.1 3.1 95.6 9.4

chlordane, cis- 2.0 94.9 2.3 89.6 6.7

chlordane, trans 2.0 94.0 2.6 89.8 6.3

chlorfenvinphos 2.0 102 3.5 96.8 8.0

chlorobenzilate 2.0 100 3.2 96.3 9.3

chloroneb 2.0 94.8 1.9 95.6 7.7

chlorothalonil 2.0 95.8 3.0 91.8 6.4

chlorpropham 2.0 97.4 2.8 91.9 7.5

chlorpyrifos 2.0 97.0 2.9 90.0 6.9

chrysene 2.0 84.8 2.8 79.5 9.3

cyanazine 2.0 101 2.3 79.4 4.9

cycloate 2.0 99.0 3.6 93.0 7.1
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

dacthal (DCPA) 2.0 95.4 3.2 89.4 7.1

DDD, 4,4′- 2.0 92.8 3.1 86.5 7.0

DDE, 4,4′- 2.0 94.9 2.7 90.0 6.4

DDT, 4,4′- 2.0 102 3.6 102 7.8

DEET 2.0 97.9 2.7 92.9 7.3

di(2-ethylhexyl)adipate 2.0 97.0 3.1 93.3 10

di(2-ethylhexyl)phthalate 2.0 109 2.9 104 6.3

dibenzo[a,h]anthracene 2.0 100 3.3 102 11

dibutyl phthalate 2.0 106 3.0 96.8 7.4

dichlorvos 2.0 96.8 2.6 90.9 7.1

dieldrin 2.0 96.8 3.2 92.6 6.5

diethylphthalate 2.0 96.1 2.6 89.9 8.5

dimethipin 2.0 9.0 24 8.50 25

dimethylphthalate 2.0 94.5 3.1 88.1 7.9

DIMP 2.0 87.3 3.1 76.6 6.5

dinitrotoluene, 2,4- 2.0 97.5 2.7 93.3 7.6

dinitrotoluene, 2,6- 2.0 96.1 2.3 90.6 8.0

diphenamid 2.0 100 3.4 94.6 7.2

disulfoton 2.0 91.6 2.5 81.5 7.2

endosulfan I 2.0 95.0 3.7 90.4 6.3

endosulfan II 2.0 93.5 2.9 88.4 7.5

endosulfan sulfate 2.0 96.4 4.5 91.4 8.1

endrin 2.0 104 3.3 101 8.0

EPTC 2.0 97.3 2.5 90.6 7.6

ethion 2.0 98.3 3.6 95.6 8.1

ethoprop 2.0 103 1.1 98.9 9.5

ethyl parathion 2.0 96.8 3.7 92.9 8.4

etridiazole 2.0 99.9 2.7 95.8 7.4

fenarimol 2.0 106 2.4 103 9.4
 

525.3-105 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

fluorene 2.0 94.4 2.3 88.5 8.0

fluridone 2.0 110 5.2 117 11

HCCPD 2.0 90.0 3.1 90.3 7.8

HCH, α 2.0 94.4 3.0 88.3 7.7

HCH, β 2.0 95.5 3.4 90.3 6.1

HCH, δ 2.0 96.4 2.9 92.3 6.6

HCH, γ (lindane) 2.0 95.4 3.3 91.3 5.6

heptachlor 2.0 93.1 3.5 88.5 6.9

heptachlor epoxide 2.0 95.8 3.3 90.6 8.0

hexachlorobenzene 2.0 90.0 2.1 84.0 7.5

hexazinone 2.0 102 3.2 100 9.2

indeno[1,2,3-c,d]pyrene 2.0 103 4.1 105 11

isophorone 2.0 93.4 2.7 86.9 7.2

methoxychlor 2.0 107 2.9 106 7.3

methyl parathion 2.0 98.8 3.0 94.5 6.9

metolachlor 2.0 98.6 3.2 93.1 6.6

metribuzin 2.0 98.4 2.9 89.9 6.7

mevinphos 2.0 99.8 3.4 97.0 8.2

MGK 264(a) 1.3 97.8 2.9 93.1 6.4

MGK 264(b) 0.67 96.9 4.4 95.4 6.8

molinate 2.0 97.6 2.8 91.3 7.6

napropamide 2.0 99.6 3.7 93.4 8.4

nitrofen 2.0 101 3.3 98.4 7.8

nonachlor, trans 2.0 94.4 2.9 89.4 7.4

norflurazon 2.0 102 4.4 99.6 8.8

oxyfluorfen 2.0 102 3.7 98.9 8.6

pebulate 2.0 96.8 2.9 90.4 7.7

pentachlorophenol 8.0 95.0 2.5 87.9 7.7

permethrin, cis 1.2 107 3.3 106 8.8
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

permethrin, trans 2.9 101 2.9 96.9 9.1

phenanthrene 2.0 93.0 2.7 87.5 7.8

phorate 2.0 96.0 2.8 90.9 7.0

phosphamidon 2.0 105 3.7 101 7.3

profenofos 2.0 100 2.7 96.3 8.5

prometon 2.0 99.3 3.1 92.6 7.5

prometryn 2.0 102 3.2 90.8 7.3

pronamide 2.0 101 3.0 95.9 6.9

propachlor 2.0 96.4 3.0 91.1 8.0

propazine 2.0 98.4 2.8 91.4 7.1

pyrene 2.0 95.5 2.9 91.0 7.8

simazine 2.0 98.5 3.3 91.0 6.3

simetryn 2.0 99.8 3.4 92.6 6.7

tebuconazole 2.0 110 4.5 112 9.8

tebuthiuron 2.0 105 3.9 96.1 9.3

terbacil 2.0 104 2.2 99.4 5.9

terbutryn 2.0 101 2.7 95.3 7.5

tetrachlorvinphos 2.0 105 3.6 100 7.0

triadimefon 2.0 102 3.7 96.6 7.2

tribufos+merphos 4.0 95.9 3.2 91.4 7.0

trifluralin 2.0 95.0 3.5 90.5 7.9

vernolate 2.0 95.9 3.1 89.5 7.6

vinclozolin 2.0 93.0 3.1 88.4 6.6

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 93.3 2.9 86.1 8.0

4-chlorobiphenyl (3) 2.0 93.1 2.4 86.5 8.0

2,4′-dichlorobiphenyl (8) 2.0 93.3 2.9 87.0 8.4

2,2′,5-trichlorobiphenyl (18) 2.0 94.8 3.1 87.3 8.7

2,4,4′-trichlorobiphenyl (28) 2.0 94.6 3.4 88.6 7.3
 

525.3-107 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 94.5 2.6 89.0 7.6

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 94.3 3.0 88.8 7.1

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 95.5 2.7 89.6 8.1

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 94.9 2.8 88.8 7.7

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 95.0 2.7 89.3 8.1

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 94.3 2.9 89.0 8.0

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 95.1 2.8 89.6 7.1

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 94.1 2.9 90.5 8.7

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 97.3 2.7 90.6 8.0

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 5.0 96.6 2.7 89.2 7.8

benzo[a]pyrene-d12 5.0 95.0 4.0 91.0 11

triphenyl phosphate 5.0 100 2.7 91.2 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.
 

525.3-108 

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 Analysesa 

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 101 2.0 93.6 0.51 99.8 0.88

acetochlor 99.0 3.9 93.6 2.1 104 2.1

alachlor 100 7.3 89.8 0.72 92.8 1.0

aldrin 77.0 5.0 78.4 2.9 85.0 3.4

ametryn 105 4.8 93.1 1.3 95.8 1.1

anthracene 106 3.8 92.3 1.0 104 0.71

atraton 112 2.9 90.3 4.1 96.8 2.2

atrazine 111 3.5 96.1 3.2 97.3 1.5

benzo[a]anthracene 112 5.1 99.1 3.8 112 3.6

benzo[a]pyrene 109 5.5 103 1.7 111 1.2

benzo[b]fluoranthene 119 5.0 102 1.2 114 2.4

benzo[g,h,i]perylene 112 2.9 102 4.3 113 2.8

benzo[k]fluoranthene 105 1.9 103 2.4 113 3.1

BHT NDe ND ND 

bromacil 102 9.3 98.9 0.86 103 2.1

butachlor 107 3.6 86.3 1.1 99.4 1.4

butylate 85.0 7.1 83.0 2.2 84.0 3.0

butylbenzylphthalate 122 1.9 95.9 3.7 114 3.6

chlordane, cis 98.0 5.3 102 2.5 101 1.3

chlordane, trans 103 1.9 103 2.3 96.6 0.71

chlorfenvinphos 113 1.8 110 2.5 111 3.9

chlorobenzilate 82.0 9.3 99.8 5.1 94.1 1.3

chloroneb 93.0 2.2 92.0 2.9 100 1.4

chlorothalonil 116 2.8 106 3.8 105 1.5

chlorpropham 109 3.5 93.1 2.5 98.6 1.1

chlorpyrifos 102 5.1 93.4 3.3 97.2 2.5

chrysene 117 1.7 97.1 1.7 114 2.1

cyanazine 99.0 3.9 88.1 4.9 106 2.4

cycloate 102 3.9 87.4 1.0 88.8 1.2
 

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 Analysesa 

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

dacthal (DCPA) 105 3.6 102 3.5 101 1.7

DDD, 4,4′- 107 3.6 85.8 0.75 105 1.4

DDE, 4,4′- 99.0 3.9 82.3 1.3 101 1.0

DDT, 4,4′- 116 2.8 87.6 2.8 112 0.83

DEET 103 1.9 98.3 3.2 104 2.0

di(2-ethylhexyl)adipate 112 4.1 96.6 3.1 111 1.8

di(2-ethylhexyl)phthalate 137 3.7 97.6 1.3 110 2.4

dibenzo[a,h]anthracene 110 3.6 95.4 2.5 109 1.5

dibutyl phthalate 115 3.3 101 1.5 114 2.6

dichlorvos 104 3.1 91.6 1.7 88.8 2.7

dieldrin 103 1.9 87.4 0.55 98.1 0.39

diethylphthalate 111 1.8 111 2.3 114 1.4

dimethipin 24.0 14 29.5 6.5 24.9 2.5

dimethylphthalate 110 3.6 113 0.25 113 0.78

DIMP 112 5.8 90.0 1.9 93.7 3.0

dinitrotoluene, 2,4- 126 1.8 105 2.6 113 2.5

dinitrotoluene, 2,6- 121 1.7 106 0.71 111 0.67

diphenamid 106 2.2 95.1 0.90 97.8 0.69

disulfoton 79.0 2.5 91.5 8.9 85.3 1.5

endosulfan I 95.0 5.3 88.4 1.3 101 1.0

endosulfan II 103 1.9 89.6 3.5 103 1.0

endosulfan sulfate 112 7.1 96.5 2.4 106 0.75

endrin 89.0 5.7 82.9 3.4 91.3 4.0

EPTC 89.0 2.2 88.0 0.80 85.8 0.60

ethion 106 2.2 100 2.7 108 3.1

ethoprop 110 2.1 91.3 1.6 96.2 1.4

ethyl parathion 117 4.3 97.6 2.3 105 3.5

etridiazole 118 3.4 90.6 2.2 101 1.5

fenarimol 110 4.7 87.1 2.0 91.7 3.4
 

525.3-110 

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 Analysesa 

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

fluorene 106 3.8 97.5 2.1 101 1.1

fluridone 92.0 5.0 103 4.9 98.6 2.9

HCCPD 92.0 3.5 65.6 1.7 68.0 5.8

HCH, α 101 3.8 92.5 1.3 95.2 0.47

HCH, β 101 3.8 94.0 4.0 102 1.7

HCH, δ 97.0 6.2 96.4 1.3 101 0.49

HCH, γ (lindane) 90.0 4.4 95.6 2.1 97.9 1.8

heptachlor 96.0 3.4 83.1 2.0 86.2 1.2

heptachlor epoxide 104 3.1 86.9 2.0 95.9 1.6

hexachlorobenzene 94.0 5.5 78.4 3.8 93.0 1.9

hexazinone 107 1.9 84.6 1.7 94.6 2.6

indeno[1,2,3-c,d]pyrene 113 4.5 95.0 2.1 112 2.4

isophorone 108 3.0 108 3.2 102 1.1

methoxychlor 122 1.9 89.9 1.5 109 0.72

methyl parathion 129 3.0 103 2.1 112 2.5

metolachlor 109 1.8 93.1 1.1 97.8 0.42

metribuzin 116 2.8 97.3 0.30 106 2.5

mevinphos 115 3.3 96.1 3.1 97.0 1.5

MGK 264(a) 94.0 2.5 75.5 1.9 88.3 4.1

MGK 264(b) 94.0 2.5 82.8 0.35 92.3 0.80

molinate 88.0 3.7 89.4 1.2 88.9 2.1

napropamide 105 3.6 89.9 2.4 99.2 1.5

nitrofen 129 3.0 106 2.7 113 3.9

nonachlor, trans 119 3.2 103 2.3 96.2 1.0

norflurazon 106 2.2 91.9 1.6 102 1.6

oxyfluorfen 129 1.6 93.9 2.9 111 3.5

pebulate 85.0 8.0 84.5 1.7 84.7 2.4

pentachlorophenol 104 4.1 100 1.3 96.0 3.6

permethrin, cis 110 3.6 107 1.3 107 2.2
 

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 Analysesa 

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

permethrin, trans 115 3.3 96.1 3.1 97.0 1.5

phenanthrene 94.0 2.5 75.5 1.9 88.3 4.1

phorate 94.0 2.5 82.8 0.35 92.3 0.80

phosphamidon 88.0 3.7 89.4 1.2 88.9 2.1

profenofos 105 3.6 89.9 2.4 99.2 1.5

prometon 129 3.0 106 2.7 113 3.9

prometryn 119 3.2 103 2.3 96.2 1.0

pronamide 106 2.2 91.9 1.6 102 1.6

propachlor 129 1.6 93.9 2.9 111 3.5

propazine 85.0 8.0 84.5 1.7 84.7 2.4

pyrene 104 4.1 100 1.3 96.0 3.6

simazine 110 3.6 107 1.3 107 2.2

simetryn 115 3.3 96.1 3.1 97.0 1.5

tebuconazole 94.0 2.5 75.5 1.9 88.3 4.1

tebuthiuron 94.0 2.5 82.8 0.35 92.3 0.80

terbacil 88.0 3.7 89.4 1.2 88.9 2.1

terbutryn 105 3.6 89.9 2.4 99.2 1.5

tetrachlorvinphos 129 3.0 106 2.7 113 3.9

triadimefon 119 3.2 103 2.3 96.2 1.0

tribufos+merphos 106 2.2 91.9 1.6 102 1.6

trifluralin 129 1.6 93.9 2.9 111 3.5

vernolate 85.0 8.0 84.5 1.7 84.7 2.4

vinclozolin 104 4.1 100 1.3 96.0 3.6

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 75.0 2.7 81.0 2.6 85.0 1.1

4-chlorobiphenyl (3) 85.0 2.4 84.4 2.8 88.9 1.5

2,4′-dichlorobiphenyl (8) 85.0 2.4 82.5 2.2 87.1 0.51

2,2′,5-trichlorobiphenyl (18) 104 3.1 89.3 2.9 95.3 4.0

2,4,4′-trichlorobiphenyl (28) 81.0 2.5 88.6 3.3 92.4 0.48
 

525.3-112 

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 Analysesa 

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 85.0 9.7 91.1 3.1 93.4 1.6

2,2′,5,5′-tetrachlorobiphenyl (52) 84.0 3.9 90.3 4.4 96.4 1.1

2,3′,4′,5-tetrachloroobiphenyl (70) 84.0 3.9 92.4 3.4 97.0 0.94

2,3,3′,4′,6-pentachlorobiphenyl (110) 81.0 2.5 94.3 3.2 97.1 0.90

2,3′,4,4′,5-pentachlorobiphenyl (118) 90.0 2.6 94.5 3.7 98.8 1.1

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 86.0 4.7 99.0 3.2 105 1.3

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 87.0 5.8 96.5 4.3 101 1.2

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 79.0 2.5 96.9 2.8 101 1.1

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 101 2.0 93.1 2.9 91.6 2.2

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 92.9 4.0 98.9 3.1 88.8 4.0

benzo[a]pyrene-d12 112 2.1 101 2.6 101 4.9

triphenyl phosphate 107 2.5 97.9 4.1 104 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 μg/L, pentachlorophenol 

is 1.0 μg/L, c-permethrin is 0.13 μg/L, t-permethrin is 0.38 μg/L, MGK 264 (a) is 0.085 μg/L and MGK 264 (b) 

is 0.17 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, c-permethrin is 1.0 μg/L, t-permethrin is 3.0 μg/L, MGK 264 (a) is 0.67 μg/L and MGK 264 (b) is 

1.3 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20.0 μg/L, c-permethrin is 2.5 μg/L, and t-permethrin is 7.5 μg/L, MGK 264 (a) is 1.7 μg/L and MGK 264 (b) 

is 3.3 μg/L.

e. ND = Not determined. Analyte could not be determined because of the low fortified concentration relative to the 

LRB. 
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 99.3 5.7 95.1 1.8

acetochlor 2.0 97.4 5.5 106 4.9

alachlor 2.0 93.5 3.5 95.0 3.3

aldrin 2.0 94.9 4.0 81.1 0.59

ametryn 2.0 98.9 5.7 93.4 6.2

anthracene 2.0 102 4.7 101 1.6

atraton 2.0 92.6 5.9 87.3 5.3

atrazine 2.0 100 4.6 95.6 1.5

benzo[a]anthracene 2.0 104 1.5 102 2.4

benzo[a]pyrene 2.0 106 3.2 100 2.7

benzo[b]fluoranthene 2.0 104 3.3 100 3.9

benzo[g,h,i]perylene 2.0 101 3.9 101 5.3

benzo[k]fluoranthene 2.0 103 3.0 101 2.6

BHT 2.0 95.5 1.2 114 1.9

bromacil 2.0 98.9 5.5 104 4.6

butachlor 2.0 96.4 2.9 95.6 3.3

butylate 2.0 87.6 3.2 83.6 1.8

butylbenzylphthalate 2.0 107 4.1 107 2.9

chlordane, cis- 2.0 96.1 6.2 98.0 5.9

chlordane, trans 2.0 94.5 5.9 98.3 7.3

chlorfenvinphos 2.0 93.1 3.9 111 3.4

chlorobenzilate 2.0 101 5.6 97.1 4.3

chloroneb 2.0 104 2.0 108 4.0

chlorothalonil 2.0 108 1.5 110 2.2

chlorpropham 2.0 95.9 5.6 98.1 2.4

chlorpyrifos 2.0 97.8 5.3 103 4.1

chrysene 2.0 106 2.2 100 3.2

cyanazine 2.0 97.4 5.2 91.0 11

cycloate 2.0 92.3 5.6 95.1 1.6
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

dacthal (DCPA) 2.0 92.1 7.3 107 4.3

DDD, 4,4′- 2.0 93.1 3.7 91.0 2.0

DDE, 4,4′- 2.0 90.0 3.6 85.6 2.7

DDT, 4,4′- 2.0 91.4 3.7 90.4 3.5

DEET 2.0 101 1.8 109 1.1

di(2-ethylhexyl)adipate 2.0 102 5.8 106 3.4

di(2-ethylhexyl)phthalate 2.0 107 2.7 104 2.2

dibenzo[a,h]anthracene 2.0 106 6.2 102 2.2

dibutyl phthalate 2.0 110 3.7 107 1.5

dichlorvos 2.0 90.4 7.3 88.8 2.3

dieldrin 2.0 96.0 5.4 96.3 2.6

diethylphthalate 2.0 110 2.5 107 1.1

dimethipin 2.0 29.4 8.7 38.1 4.2

dimethylphthalate 2.0 111 2.4 111 1.0

DIMP 2.0 89.6 5.9 99.6 5.9

dinitrotoluene, 2,4- 2.0 95.6 7.0 105 4.1

dinitrotoluene, 2,6- 2.0 95.6 6.2 101 5.0

diphenamid 2.0 98.5 5.6 101 2.3

disulfoton 2.0 79.6 5.9 103 6.3

endosulfan I 2.0 96.9 7.0 93.0 4.5

endosulfan II 2.0 98.5 5.7 94.3 4.1

endosulfan sulfate 2.0 102 2.8 100 2.1

endrin 2.0 97.9 2.6 88.1 3.4

EPTC 2.0 89.0 7.2 85.8 3.0

ethion 2.0 95.8 6.9 98.9 4.3

ethoprop 2.0 94.9 5.7 103 3.9

ethyl parathion 2.0 97.6 5.9 103 3.0

etridiazole 2.0 104 2.4 104 3.1

fenarimol 2.0 93.5 4.4 86.6 3.3
 

525.3-115 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

fluorene 2.0 101 5.1 104 1.8

fluridone 2.0 111 3.9 97.4 6.0

HCCPD 2.0 64.6 6.7 69.1 2.8

HCH, α 2.0 93.5 5.7 91.8 2.4

HCH, β 2.0 97.9 4.2 97.8 1.8

HCH, δ 2.0 102 6.4 94.3 3.7

HCH, γ (lindane) 2.0 100 6.8 90.0 2.1

heptachlor 2.0 91.0 3.0 86.1 1.5

heptachlor epoxide 2.0 98.3 6.2 91.6 1.6

hexachlorobenzene 2.0 90.4 4.0 89.0 2.7

hexazinone 2.0 93.4 3.1 97.0 8.1

indeno[1,2,3-c,d]pyrene 2.0 107 6.6 103 4.6

isophorone 2.0 104 3.9 101 2.6

methoxychlor 2.0 94.0 5.6 94.0 2.6

methyl parathion 2.0 100 3.7 110 2.5

metolachlor 2.0 97.5 5.6 97.8 2.1

metribuzin 2.0 102 2.6 120 0.77

mevinphos 2.0 89.9 5.3 96.3 4.5

MGK 264(a) 1.3 92.9 2.3 86.4 4.1

MGK 264(b) 0.67 95.9 4.1 92.6 3.9

molinate 2.0 94.9 5.0 89.1 2.3

napropamide 2.0 95.9 4.6 104 3.1

nitrofen 2.0 111 6.2 96.4 5.3

nonachlor, trans 2.0 105 4.0 98.4 5.3

norflurazon 2.0 98.1 3.8 101 6.4

oxyfluorfen 2.0 91.8 7.7 94.9 5.0

pebulate 2.0 89.3 4.4 84.3 1.0

pentachlorophenol 8.0 98.3 2.6 97.3 2.9

permethrin, cis 1.0 92.6 6.0 108 4.3
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

permethrin, trans 3.0 91.4 7.1 100 2.3

phenanthrene 2.0 106 3.7 104 2.5

phorate 2.0 95.5 2.0 98.9 4.8

phosphamidon 2.0 100 3.3 114 2.8

profenofos 2.0 98.4 4.4 108 1.7

prometon 2.0 96.9 2.1 88.4 5.7

prometryn 2.0 98.8 4.9 94.6 4.9

pronamide 2.0 95.1 5.5 96.6 3.4

propachlor 2.0 106 1.4 110 3.4

propazine 2.0 101 2.8 96.4 2.5

pyrene 2.0 106 1.2 107 2.2

simazine 2.0 101 3.7 96.1 3.0

simetryn 2.0 98.6 4.2 87.9 3.8

tebuconazole 2.0 94.4 5.4 96.0 5.2

tebuthiuron 2.0 88.5 7.1 101 1.8

terbacil 2.0 101 5.6 95.8 10

terbutryn 2.0 97.3 5.1 87.4 5.1

tetrachlorvinphos 2.0 97.5 6.6 104 5.4

triadimefon 2.0 99.3 2.1 101 3.0

tribufos+merphos 4.0 96.6 7.3 107 2.0

trifluralin 2.0 90.8 2.2 90.0 4.5

vernolate 2.0 88.0 6.0 88.3 1.8

vinclozolin 2.0 98.6 7.0 111 1.7

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 90.8 1.7 96.3 5.6

4-chlorobiphenyl (3) 2.0 96.1 0.65 99.9 5.4

2,4′-dichlorobiphenyl (8) 2.0 97.9 0.87 86.6 6.3

2,2′,5-trichlorobiphenyl (18) 2.0 101 3.8 90.9 7.5

2,4,4′-trichlorobiphenyl (28) 2.0 101 2.2 86.1 4.9
 

525.3-117 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 93.0 3.0 88.1 6.9

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 97.1 3.1 87.8 6.6

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 107 1.5 88.1 5.2

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 107 1.3 92.0 6.3

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 108 1.2 91.3 6.4

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 110 2.0 93.8 5.3

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 106 1.4 91.5 6.0

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 108 0.89 91.3 6.3

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 99.6 1.0 87.6 7.2

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 5.0 91.7 7.5 89.0 6.5

benzo[a]pyrene-d12 5.0 103 2.7 104 3.0

triphenyl phosphate 5.0 104 0.58 112 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.
 

525.3-118 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

acenaphthylene 87.3 3.4 86.6 1.1 90.5 1.3

acetochlor 92.3 4.0 93.9 2.6 95.2 1.4

alachlor 95.6 8.0 93.4 2.0 94.6 1.4

aldrin 85.6 1.2 84.7 5.7 90.4 1.2

ametryn 91.4 3.5 93.9 2.9 95.8 1.5

anthracene 87.2 4.6 90.2 2.2 92.9 1.4

atraton 93.2 5.2 94.9 5.3 98.5 2.4

atrazine 94.5 7.4 92.9 2.9 95.0 1.9

benzo[a]anthracene 93.6 2.5 90.6 2.1 91.3 1.7

benzo[a]pyrene 88.9 3.5 85.8 3.0 88.2 3.9

benzo[b]fluoranthene 87.9 3.6 85.1 3.0 89.0 4.0

benzo[g,h,i]perylene 88.3 4.2 79.8 3.9 84.5 3.8

benzo[k]fluoranthene 91.1 3.8 85.9 2.7 87.2 3.9

BHT 89.8 5.0 84.9 1.5 87.6 1.2

bromacil 96.9 1.9 94.3 2.8 96.6 3.6

butachlor 94.9 5.0 91.5 2.8 93.0 2.4

butylate 86.9 2.4 88.0 2.4 91.5 1.5

butylbenzylphthalate 104 19 94.5 3.9 93.6 1.2

chlordane, cis 92.1 6.5 89.2 4.9 89.7 2.5

chlordane, trans 91.2 5.0 89.4 4.2 88.9 2.3

chlorfenvinphos 89.1 7.7 94.0 4.3 95.3 2.4

chlorobenzilate 96.0 4.0 93.8 4.4 92.4 1.9

chloroneb 89.7 4.2 90.9 1.4 93.6 1.3

chlorothalonil 89.0 4.8 94.3 1.6 97.3 2.3

chlorpropham 93.7 7.7 92.5 2.3 95.8 0.75

chlorpyrifos 89.1 2.6 91.3 3.2 94.4 2.1

chrysene 90.7 2.3 92.0 2.6 90.9 1.4

cyanazine 101 8.6 108 3.3 114 3.7

cycloate 90.0 4.9 89.6 1.7 92.4 0.32
 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

dacthal (DCPA) 93.9 3.3 94.3 2.1 96.0 1.2

DDD, 4,4′- 91.0 3.4 91.8 3.4 88.3 1.8

DDE, 4,4′- 83.9 4.3 87.9 6.8 85.6 3.0

DDT, 4,4′- 88.8 6.0 88.3 4.2 86.4 2.4

DEET 91.6 5.5 92.9 2.0 94.5 0.82

di(2-ethylhexyl)adipate 84.1 8.6 76.2 3.3 76.5 3.1

di(2-ethylhexyl)phthalate NDe 77.0 2.7 72.7 2.8

dibenzo[a,h]anthracene 85.3 5.0 76.7 3.7 81.5 4.5

dibutyl phthalate ND 111 2.2 95.0 0.96

dichlorvos 93.2 4.4 86.7 0.98 89.3 2.3

dieldrin 93.6 9.2 91.3 6.2 91.1 2.8

diethylphthalate 93.6 5.4 91.4 2.2 94.2 0.90

dimethipin 36.0 13 32.8 25 28.4 9.6

dimethylphthalate 89.4 5.3 90.0 1.0 92.6 1.0

DIMP 89.9 5.3 83.9 2.7 86.8 1.8

dinitrotoluene, 2,4- 88.6 5.8 92.1 1.4 97.0 1.3

dinitrotoluene, 2,6- 89.3 5.7 89.1 2.1 94.0 0.67

diphenamid 93.8 3.2 94.7 2.1 96.2 1.4

disulfoton 71.0 5.0 77.4 4.9 77.8 4.8

endosulfan I 87.9 9.2 89.6 3.3 91.1 1.4

endosulfan II 94.8 5.8 91.5 6.7 90.6 3.0

endosulfan sulfate 95.1 4.8 93.4 2.7 93.4 1.7

endrin 88.1 2.1 92.5 4.7 93.0 2.3

EPTC 85.8 3.5 86.2 0.96 90.5 1.8

ethion 96.1 4.3 93.5 3.9 92.7 2.8

ethoprop 91.9 4.1 92.1 2.7 95.7 0.71

ethyl parathion 92.9 7.8 88.8 3.1 93.4 2.8

etridiazole 84.6 6.7 88.8 1.4 92.3 1.1

fenarimol 99.8 5.9 95.9 3.7 100 3.4
 

525.3-120 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

fluorene 86.6 4.4 88.1 1.2 92.5 0.53

fluridone 95.4 8.2 96.1 5.9 101 4.6

HCCPD 72.6 6.9 73.5 2.4 76.5 4.4

HCH, α 91.5 5.9 91.1 1.3 93.3 0.71

HCH, β 96.1 6.1 94.4 2.8 97.0 2.3

HCH, δ 88.5 5.7 90.6 3.4 93.4 1.5

HCH, γ (lindane) 89.4 4.0 92.1 3.0 92.3 0.85

heptachlor 91.9 9.9 89.8 3.2 92.6 0.26

heptachlor epoxide 86.8 3.3 91.3 5.7 92.8 2.4

hexachlorobenzene 86.8 6.1 89.5 1.9 90.5 1.1

hexazinone 95.0 3.8 97.8 1.8 100 1.7

indeno[1,2,3-c,d]pyrene 85.3 5.5 80.2 3.7 86.1 4.3

isophorone 88.2 6.0 87.4 1.3 87.1 1.5

methoxychlor 94.1 4.0 93.0 2.6 92.2 1.3

methyl parathion 90.3 3.8 93.6 3.1 95.4 0.43

metolachlor 90.3 5.0 93.9 3.2 96.6 1.6

metribuzin 93.3 4.7 94.8 1.5 95.4 2.0

mevinphos 90.1 4.7 89.4 1.6 93.2 0.92

MGK 264(a) 87.5 4.0 92.3 2.6 94.5 1.5

MGK 264(b) 86.3 7.9 94.4 3.9 96.3 2.5

molinate 90.5 6.9 89.2 1.1 91.6 1.4

napropamide 97.3 7.6 93.3 3.8 92.9 1.2

nitrofen 90.4 5.1 94.4 3.3 94.0 1.3

nonachlor, trans 86.7 4.2 86.8 2.4 86.0 3.3

norflurazon 97.0 3.8 95.1 2.3 98.9 3.3

oxyfluorfen 94.3 5.2 93.2 4.5 92.9 1.9

pebulate 90.5 3.7 88.4 1.6 90.9 2.0

pentachlorophenol 93.0 4.4 97.4 3.9 94.8 3.4

permethrin, cis 87.7 2.0 79.8 1.3 80.9 3.5
 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

permethrin, trans 89.3 3.2 82.3 2.2 83.2 2.0

phenanthrene 88.6 3.9 90.1 2.4 92.6 1.7

phorate 83.7 4.2 88.8 2.3 91.1 0.97

phosphamidon 98.3 6.5 95.2 2.9 95.5 2.0

profenofos 92.0 8.6 93.7 2.8 94.7 4.2

prometon 90.0 3.8 93.9 3.2 96.0 0.79

prometryn 94.0 2.0 98.9 3.9 102 2.2

pronamide 92.3 4.0 93.5 1.7 96.1 1.9

propachlor 88.8 5.2 91.5 2.8 94.7 0.89

propazine 95.5 3.3 93.5 2.6 95.7 0.55

pyrene 92.2 4.3 91.8 3.8 92.3 2.1

simazine 93.9 3.8 94.2 1.8 98.7 2.9

simetryn 95.1 2.1 93.8 2.8 95.4 1.0

tebuconazole 93.2 5.3 94.7 2.0 97.0 2.3

tebuthiuron 95.4 11 91.3 9.5 99.6 8.9

terbacil 91.4 6.1 94.5 1.9 96.2 2.9

terbutryn 96.5 5.1 93.7 3.0 95.5 1.5

tetrachlorvinphos 95.6 4.9 92.3 3.1 93.0 2.8

triadimefon 94.5 2.4 96.1 3.3 96.7 2.6

tribufos 82.0 5.2 95.8 4.4 93.7 1.6

trifluralin 91.0 5.8 91.2 2.1 95.9 0.75

vernolate 87.3 2.5 87.0 1.1 90.7 1.8

vinclozolin 94.3 8.5 94.7 4.6 94.9 2.2

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 85.3 5.2 87.2 1.8 90.0 0.53

4-chlorobiphenyl (3) 88.2 4.0 88.1 1.3 92.0 1.1

2,4′-dichlorobiphenyl (8) 87.1 5.8 90.8 2.0 92.5 0.43

2,2′,5-trichlorobiphenyl (18) 89.4 2.5 91.0 2.9 92.0 0.54

2,4,4′-trichlorobiphenyl (28) 84.4 6.8 90.6 3.1 90.8 0.41
 

525.3-122 

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 Analysesa

Analytes 

Fortified Conc.

0.25 μg/Lb

Fortified Conc.

2.0 μg/Lc

Fortified Conc.

5.0 μg/Ld

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 87.2 7.5 89.6 2.8 90.3 1.7

2,2′,5,5′-tetrachlorobiphenyl (52) 89.4 5.4 88.8 2.2 89.4 2.7

2,3′,4′,5-tetrachloroobiphenyl (70) 87.8 8.3 88.3 5.0 89.4 1.7

2,3,3′,4′,6-pentachlorobiphenyl (110) 87.1 3.2 90.5 4.1 88.5 3.4

2,3′,4,4′,5-pentachlorobiphenyl (118) 85.5 3.4 89.0 4.3 84.3 4.1

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 85.9 5.7 88.6 3.9 86.4 2.8

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 84.3 6.6 88.0 4.5 86.7 3.6

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 83.1 4.4 87.7 4.7 85.1 4.6

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 81.9 6.0 87.1 4.5 86.5 2.9

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 86.4 4.0 86.2 1.9 88.0 0.92

benzo[a]pyrene-d12 89.6 3.5 93.5 5.1 98.9 4.2

triphenyl phosphate 87.8 2.6 93.3 2.9 99.9 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 μg/L, pentachlorophenol 

is 1.0 μg/L, MGK 264 (a) is 0.200 μg/L and MGK 264 (b) is 0.050 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 8.0 μg/L, , MGK 264 (a) is 1.6 μg/L and MGK 264 (b) is 0.4 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 5.0 μg/L, pentachlorophenol 

is 20.0 μg/L, , MGK 264 (a) is 4.0 μg/L and MGK 264 (b) is 1.0 μg/L.

e. ND = Not determined. Analyte could not be determined because of high laboratory reagent blank values relative 

to the fortification concentration. 

 
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Synthetic Hard Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acenaphthylene 2.0 90.9 2.2 92.1 1.8

acetochlor 2.0 98.7 0.47 97.0 2.6

alachlor 2.0 96.9 1.2 95.0 1.6

aldrin 2.0 93.3 3.4 93.2 2.9

ametryn 2.0 90.8 4.2 90.0 3.2

anthracene 2.0 95.3 2.2 94.8 1.6

atraton 2.0 85.8 5.7 88.2 4.5

atrazine 2.0 92.2 3.2 93.3 0.82

benzo[a]anthracene 2.0 92.1 2.4 91.9 1.7

benzo[a]pyrene 2.0 87.4 2.3 86.8 2.4

benzo[b]fluoranthene 2.0 85.7 3.6 85.8 3.0

benzo[g,h,i]perylene 2.0 79.1 1.6 78.4 6.1

benzo[k]fluoranthene 2.0 87.9 3.3 85.1 3.5

BHT 2.0 92.6 1.6 93.8 2.4

bromacil 2.0 95.4 4.2 96.1 2.7

butachlor 2.0 93.5 3.6 93.4 2.1

butylate 2.0 95.0 2.0 95.8 3.4

butylbenzylphthalate 2.0 92.8 3.2 92.5 1.9

chlordane, cis- 2.0 89.0 1.7 89.8 2.3

chlordane, trans 2.0 89.7 1.6 90.3 1.3

chlorfenvinphos 2.0 95.2 4.1 95.1 2.3

chlorobenzilate 2.0 94.3 4.1 93.2 1.7

chloroneb 2.0 95.6 1.2 95.6 1.5

chlorothalonil 2.0 97.1 1.9 97.8 1.6

chlorpropham 2.0 97.1 1.4 97.4 2.0

chlorpyrifos 2.0 95.2 2.5 95.0 2.2

chrysene 2.0 94.8 2.7 91.8 2.3

cyanazine 2.0 98.7 7.1 97.4 5.4

cycloate 2.0 94.4 2.3 94.5 2.0
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Synthetic Hard Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

dacthal (DCPA) 2.0 97.5 1.7 98.0 0.56

DDD, 4,4′- 2.0 86.5 3.5 87.5 1.4

DDE, 4,4′- 2.0 83.6 1.7 84.2 2.6

DDT, 4,4′- 2.0 82.4 2.1 82.5 0.57

DEET 2.0 99.3 2.4 99.3 2.9

di(2-ethylhexyl)adipate 2.0 72.1 1.4 73.4 2.0

di(2-ethylhexyl)phthalate 2.0 73.0 3.6 74.7 3.1

dibenzo[a,h]anthracene 2.0 75.8 2.1 75.2 6.3

dibutyl phthalate 2.0 116 2.3 114 1.0

dichlorvos 2.0 90.0 3.6 91.4 2.2

dieldrin 2.0 90.4 4.9 88.3 1.8

diethylphthalate 2.0 96.7 2.3 96.4 1.1

dimethipin 2.0 45.0 24 34.8 17

dimethylphthalate 2.0 94.3 1.8 95.2 1.9

DIMP 2.0 84.6 3.5 88.3 5.1

dinitrotoluene, 2,4- 2.0 93.4 5.6 98.2 3.0

dinitrotoluene, 2,6- 2.0 92.9 3.3 95.5 1.1

diphenamid 2.0 95.5 2.6 95.2 1.8

disulfoton 2.0 80.0 5.1 73.4 10

endosulfan I 2.0 68.1 2.7 59.4 7.7

endosulfan II 2.0 90.6 6.2 89.7 4.8

endosulfan sulfate 2.0 92.6 3.2 92.1 2.4

endrin 2.0 90.6 3.4 93.0 2.5

EPTC 2.0 93.0 2.0 94.6 2.0

ethion 2.0 92.8 3.2 89.3 1.1

ethoprop 2.0 99.1 2.1 98.7 2.6

ethyl parathion 2.0 95.4 1.9 96.3 6.8

etridiazole 2.0 96.1 2.6 95.1 2.8

fenarimol 2.0 98.7 4.5 94.4 1.8
 

525.3-125 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Synthetic Hard Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

fluorene 2.0 93.3 1.7 93.0 2.4

fluridone 2.0 89.1 6.1 87.0 10

HCCPD 2.0 83.8 2.7 85.4 3.8

HCH, α 2.0 95.2 2.6 96.4 3.6

HCH, β 2.0 99.6 3.1 98.5 2.9

HCH, δ 2.0 94.8 3.3 94.2 2.4

HCH, γ (lindane) 2.0 92.8 1.8 94.1 2.8

heptachlor 2.0 90.5 3.7 91.4 3.7

heptachlor epoxide 2.0 95.4 4.5 92.3 3.0

hexachlorobenzene 2.0 93.6 1.3 92.8 1.8

hexazinone 2.0 95.1 1.6 94.9 4.4

indeno[1,2,3-c,d]pyrene 2.0 80.6 2.7 80.6 6.3

isophorone 2.0 90.9 2.3 91.9 1.4

methoxychlor 2.0 93.4 3.6 93.8 1.8

methyl parathion 2.0 95.4 2.6 98.3 4.9

metolachlor 2.0 97.0 1.6 98.0 1.6

metribuzin 2.0 93.7 0.99 93.6 1.5

mevinphos 2.0 95.0 2.5 95.6 1.3

MGK 264(a) 1.6 95.7 2.3 93.9 2.2

MGK 264(b) 0.4 98.4 3.6 98.1 4.0

molinate 2.0 93.9 2.2 94.5 1.7

napropamide 2.0 91.3 4.4 93.1 1.9

nitrofen 2.0 93.2 3.3 95.6 1.8

nonachlor, trans 2.0 86.7 3.7 86.3 2.9

norflurazon 2.0 97.1 3.1 96.0 1.5

oxyfluorfen 2.0 93.5 3.2 95.3 0.75

pebulate 2.0 92.8 2.3 94.3 2.4

pentachlorophenol 8.0 96.8 2.7 96.6 2.2

permethrin, cis 2.0 77.7 3.1 77.3 2.1
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Synthetic Hard Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

permethrin, trans 2.0 80.1 2.9 79.1 1.8

phenanthrene 2.0 93.8 1.2 94.3 2.3

phorate 2.0 92.0 1.5 93.0 4.1

phosphamidon 2.0 92.7 5.3 94.6 1.7

profenofos 2.0 94.2 2.9 95.7 2.0

prometon 2.0 87.4 6.1 86.1 3.6

prometryn 2.0 93.3 4.5 91.5 2.8

pronamide 2.0 95.7 2.3 96.4 1.7

propachlor 2.0 97.1 2.8 96.3 1.3

propazine 2.0 93.8 1.8 93.0 3.0

pyrene 2.0 93.0 2.5 93.7 1.4

simazine 2.0 91.8 2.7 92.9 2.7

simetryn 2.0 88.4 3.8 89.6 3.4

tebuconazole 2.0 97.0 2.3 96.8 2.4

tebuthiuron 2.0 97.7 6.1 98.8 8.0

terbacil 2.0 96.1 2.0 96.5 2.6

terbutryn 2.0 92.4 5.4 89.6 4.2

tetrachlorvinphos 2.0 91.7 3.9 91.8 3.1

triadimefon 2.0 97.6 3.9 93.8 4.2

tribufos 2.0 95.2 3.7 93.5 2.3

trifluralin 2.0 100 1.8 99.1 2.0

vernolate 2.0 92.6 2.4 94.0 2.5

vinclozolin 2.0 97.5 1.1 97.6 3.9

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 2.0 90.8 2.0 92.0 2.4

4-chlorobiphenyl (3) 2.0 91.8 2.3 92.4 3.2

2,4′-dichlorobiphenyl (8) 2.0 94.9 2.0 95.0 2.7

2,2′,5-trichlorobiphenyl (18) 2.0 95.2 2.2 94.4 1.8

2,4,4′-trichlorobiphenyl (28) 2.0 93.6 1.9 92.9 3.4
 

525.3-127 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Synthetic Hard Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

2,2′,3,5′-tetrachlorobiphenyl (44) 2.0 94.4 3.8 92.1 2.1

2,2′,5,5′-tetrachlorobiphenyl (52) 2.0 91.1 3.6 91.4 2.5

2,3′,4′,5-tetrachloroobiphenyl (70) 2.0 87.8 1.2 89.4 1.2

2,3,3′,4′,6-pentachlorobiphenyl (110) 2.0 86.6 1.3 88.0 1.8

2,3′,4,4′,5-pentachlorobiphenyl (118) 2.0 83.3 2.9 86.9 1.7

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 2.0 82.6 1.8 84.7 2.2

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 2.0 82.5 2.0 85.9 2.8

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 2.0 81.5 1.8 83.4 2.9

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 2.0 79.3 2.6 81.3 1.6

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 2.0 88.7 2.9 90.6 3.8

benzo[a]pyrene-d12 2.0 94.1 2.4 93.4 3.2

triphenyl phosphate 2.0 92.2 1.8 92.4 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.
 

525.3-128 

Table 15. DLs and LCMRLs (μg/L) Calculated from Replicate Analyses of Fortified 

Reagent Water Samples Analyzed in Full Scan GC/MS Mode

Analytes 

Laboratory 1

Oasis HLB SPEa,b

Laboratory 2

Empore PSDVB SPEc

DL

Fortified 

conc. of 

DL 

replicates

LCMRL DL

Fortified 

conc. of 

DL 

replicates

LCMRL

acenaphthylene 0.015 0.050 NCd 0.0029 0.025 0.028

acetochlor 0.037 0.050 0.19 0.011 0.025 0.054

alachlor 0.035 0.10 0.25 0.0084 0.025 0.097

aldrin 0.056 0.10 0.30 0.010 0.025 0.420

ametryn 0.038 0.050 0.17 0.017 0.025 0.12

anthracene 0.018 0.050 0.12 0.0078 0.025 0.059

atraton 0.016 0.10 0.12 0.0055 0.025 0.12

atrazine 0.030 0.050 0.29 0.010 0.025 0.086

benzo[a]anthracene 0.021 0.050 0.12 0.0062 0.025 0.043

benzo[a]pyrene 0.043 0.050 0.18 0.035 0.025 0.11

benzo[b]fluoranthene 0.031 0.050 0.14 0.013 0.050 0.11

benzo[g,h,i]perylene 0.021 0.10 0.31 0.011 0.025 0.047

benzo[k]fluoranthene 0.048 0.050 0.18 0.026 0.025 0.190

BHT 0.092 0.10 0.32 0.0064 0.025 0.50

bromacil NDe 0.31 0.037 0.050 0.10

butachlor 0.028 0.050 0.39 0.0043 0.025 0.089

butylate 0.024 0.050 0.16 0.0053 0.025 0.089

butylbenzylphthalate 0.068 0.10 0.40 0.016 0.025 0.20

chlordane, cis 0.10 0.10 0.33 0.0094 0.025 0.068

chlordane, trans 0.027 0.050 0.28 0.010 0.025 0.043

chlorfenvinphos 0.095 0.10 0.52 0.0062 0.025 0.098

chlorobenzilate 0.034 0.050 0.30 0.0042 0.025 0.091

chloroneb 0.068 0.10 0.16 0.19 0.025 0.90

chlorothalonil 0.036 0.10 0.17 0.0074 0.025 0.11

chlorpropham 0.026 0.050 0.21 0.013 0.025 0.14

chlorpyrifos 0.091 0.10 0.45 0.026 0.025 0.076

chrysene 0.017 0.050 0.15 0.010 0.050 0.035

cyanazine 0.032 0.050 0.33 0.19 0.050 0.15
 

525.3-129 

Table 15. DLs and LCMRLs (μg/L) Calculated from Replicate Analyses of Fortified 

Reagent Water Samples Analyzed in Full Scan GC/MS Mode

Analytes 

Laboratory 1

Oasis HLB SPEa,b

Laboratory 2

Empore PSDVB SPEc

DL

Fortified 

conc. of 

DL 

replicates

LCMRL DL

Fortified 

conc. of 

DL 

replicates

LCMRL

cycloate 0.039 0.050 0.27 0.018 0.025 0.14

dacthal (DCPA) 0.018 0.050 0.44 0.0055 0.025 0.040

DDD, 4,4′- 0.019 0.050 0.35 0.0031 0.025 0.092

DDE, 4,4′- 0.033 0.050 0.32 0.0023 0.025 0.088

DDT, 4,4′- 0.036 0.050 0.25 0.022 0.025 0.12

DEET 0.019 0.050 0.14 0.0042 0.025 0.066

di(2-ethylhexyl)adipate 0.079 0.10 0.38 0.013 0.025 0.083

di(2-ethylhexyl)phthalate ND 0.050 0.29 0.020 0.025 0.40

dibenzo[a,h]anthracene 0.014 0.050 0.30 0.014 0.025 0.14

dibutyl phthalate ND 0.050 0.88 0.13 0.025 1.4

dichlorvos 0.021 0.050 0.46 0.0051 0.025 0.081

dieldrin 0.064 0.10 0.28 0.017 0.025 0.084

diethylphthalate 0.037 0.050 0.074 0.018 0.025 0.13 

dimethipin 0.045 0.050 0.27 ND 0.025 NC

dimethylphthalate 0.026 0.050 0.11 0.0048 0.025 0.046

DIMP 0.039 0.050 0.19 0.0036 0.025 >5.0

dinitrotoluene, 2,4- 0.026 0.050 0.23 0.0076 0.025 0.19 

dinitrotoluene, 2,6- 0.056 0.10 0.31 0.053 0.075 0.20

diphenamid 0.033 0.050 0.29 0.010 0.025 0.089

disulfoton 0.12 0.10 0.12 0.0066 0.025 0.11 

endosulfan I 0.039 0.050 0.62 0.015 0.050 0.11

endosulfan II 0.14 0.10 0.38 0.024 0.050 NC

endosulfan sulfate 0.068 0.10 0.39 0.025 0.050 0.12

endrin 0.045 0.050 0.40 0.033 0.050 0.12

EPTC 0.037 0.050 0.13 0.0048 0.025 0.068

ethion 0.010 0.050 0.29 0.013 0.025 0.13

ethoprop 0.13 0.10 0.39 0.0048 0.025 0.12

ethyl parathion 0.15 0.10 0.46 0.013 0.050 0.19
 

525.3-130 

Table 15. DLs and LCMRLs (μg/L) Calculated from Replicate Analyses of Fortified 

Reagent Water Samples Analyzed in Full Scan GC/MS Mode

Analytes 

Laboratory 1

Oasis HLB SPEa,b

Laboratory 2

Empore PSDVB SPEc

DL

Fortified 

conc. of 

DL 

replicates

LCMRL DL

Fortified 

conc. of 

DL 

replicates

LCMRL

etridiazole 0.024 0.050 0.24 0.012 0.025 0.17

fenarimol 0.10 0.10 0.28 0.041 0.050 0.20

fluorene 0.016 0.050 0.08 0.0058 0.025 0.051

fluridone 0.11 0.10 0.33 0.045 0.050 0.27

HCCPD 0.012 0.050 0.24 0.0066 0.025 0.084

HCH, α 0.036 0.050 0.31 0.0037 0.025 0.062

HCH, β 0.10 0.10 0.24 0.021 0.050 0.11 

HCH, δ 0.019 0.050 0.31 0.015 0.025 0.099

HCH, γ (lindane) 0.036 0.050 0.24 0.014 0.025 0.078

heptachlor 0.034 0.050 0.27 0.0032 0.025 0.029

heptachlor epoxide 0.039 0.10 0.11 0.0053 0.025 0.063

hexachlorobenzene 0.016 0.050 0.40 0.0094 0.025 0.087

hexazinone 0.025 0.050 0.26 0.012 0.025 0.14

indeno[1,2,3-c,d]pyrene 0.11 0.10 0.40 0.039 0.025 0.20

isophorone 0.014 0.050 0.11 0.0043 0.025 0.063

methoxychlor 0.024 0.050 0.23 0.0064 0.025 0.061

methyl parathion 0.036 0.050 0.28 0.0088 0.050 0.16

metolachlor 0.019 0.050 0.11 0.0042 0.025 0.14

metribuzin 0.036 0.050 0.076 0.0070 0.025 0.11

mevinphos 0.035 0.10 0.21 0.0040 0.025 0.093

MGK 264(a) 0.072 0.080 0.32 0.0026 0.025 0.031

MGK 264(b) 0.023 0.020 0.09 0.0096 0.025 0.083

molinate 0.062 0.10 0.29 0.0036 0.025 0.074

napropamide 0.077 0.10 0.44 0.025 0.050 0.11

nitrofen 0.093 0.10 0.39 0.042 0.050 0.13

nonachlor, trans 0.035 0.050 0.35 0.0062 0.025 0.049

norflurazon 0.057 0.10 0.26 0.062 0.050 0.14

oxyfluorfen 0.037 0.050 0.34 0.015 0.050 0.28
 

525.3-131 

Table 15. DLs and LCMRLs (μg/L) Calculated from Replicate Analyses of Fortified 

Reagent Water Samples Analyzed in Full Scan GC/MS Mode

Analytes 

Laboratory 1

Oasis HLB SPEa,b

Laboratory 2

Empore PSDVB SPEc

DL

Fortified 

conc. of 

DL 

replicates

LCMRL DL

Fortified 

conc. of 

DL 

replicates

LCMRL

pebulate 0.020 0.050 0.20 0.0053 0.025 0.040

pentachlorophenol 0.060 0.20 0.56 0.069 0.025 0.16

permethrin, cis 0.015 0.028 0.13 0.0026 0.025 0.036

permethrin, trans 0.031 0.072 0.10 0.012 0.025 0.087

phenanthrene 0.025 0.10 0.097 0.0069 0.025 0.51

phorate 0.032 0.050 0.20 0.052 0.050 0.15 

phosphamidon 0.040 0.10 0.23 0.0029 0.025 0.11 

profenofos 0.11 0.10 0.31 0.055 0.050 0.11 

prometon 0.065 0.10 0.22 0.010 0.025 0.12

prometryn 0.021 0.050 0.24 0.012 0.025 0.10

pronamide 0.017 0.050 0.13 0.0077 0.025 0.13

propachlor 0.029 0.050 0.27 0.0076 0.025 0.068

propazine 0.023 0.050 0.20 0.0065 0.025 0.055

pyrene 0.013 0.050 0.17 0.0045 0.025 0.062

simazine 0.023 0.050 0.12 0.0059 0.025 0.083

simetryn 0.037 0.050 0.28 0.013 0.025 0.12

tebuconazole 0.24 0.50 2.1 0.053 0.050 0.18 

tebuthiuron 0.027 0.050 0.21 0.060 0.075 0.13

terbacil 0.082 0.10 0.41 0.039 0.075 0.13

terbutryn 0.029 0.050 0.18 0.0051 0.025 0.093

tetrachlorvinphos 0.048 0.10 0.35 0.0042 0.025 0.14 

triadimefon 0.053 0.050 0.35 0.048 0.050 0.11

tribufos+merphos 0.12 0.10 0.53 0.013 0.025 0.18 

trifluralin 0.027 0.050 0.28 0.019 0.025 0.12

vernolate 0.038 0.050 0.11 0.0051 0.025 0.080

vinclozolin 0.029 0.050 0.34 0.016 0.050 0.12

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 0.021 0.050 0.14 0.0061 0.025 0.054
 

525.3-132 

Table 15. DLs and LCMRLs (μg/L) Calculated from Replicate Analyses of Fortified 

Reagent Water Samples Analyzed in Full Scan GC/MS Mode

Analytes 

Laboratory 1

Oasis HLB SPEa,b

Laboratory 2

Empore PSDVB SPEc

DL

Fortified 

conc. of 

DL 

replicates

LCMRL DL

Fortified 

conc. of 

DL 

replicates

LCMRL

4-chlorobiphenyl (3) 0.019 0.050 0.24 0.0059 0.025 0.065

2,4′-dichlorobiphenyl (8) 0.024 0.050 0.18 0.0037 0.025 0.088

2,2′,5-trichlorobiphenyl (18) 0.024 0.050 0.086 0.028 0.025 0.14

2,4,4′-trichlorobiphenyl (28) 0.036 0.050 0.069 0.0073 0.025 0.036

2,2′,3,5′-tetrachlorobiphenyl (44) 0.029 0.050 0.23 0.0079 0.025 0.041

2,2′,5,5′-tetrachlorobiphenyl (52) 0.043 0.10 0.092 0.0055 0.025 0.078

2,3′,4′,5-tetrachloroobiphenyl (70) 0.043 0.050 0.30 0.0044 0.025 0.046

2,3,3′,4′,6-pentachlorobiphenyl (110) 0.026 0.050 0.36 0.0030 0.025 0.084

2,3′,4,4′,5-pentachlorobiphenyl (118) 0.046 0.050 0.36 0.0050 0.025 0.095

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 0.19 0.10 0.41 0.0071 0.025 0.058

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 0.020 0.050 0.37 0.0039 0.025 0.056

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 0.029 0.050 0.38 0.0033 0.025 0.092

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 0.058 0.10 0.31 0.0066 0.025 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.
 

525.3-133 

Table 16. Example SIM Parameters for Selected Method Analytes

SIM 

Segment Compound

RT 

(min)

QI 

(m/z)

Confirmation 

Ion(s) (m/z)

Dwell 

Time 

(ms)

Scan 

Time

(sec/scan)

# 1 1,3-dimethyl-2-nitrobenzene (SUR) 8.94 77 134 80 0.49

HCCPD 11.03 237 235, 239

# 2

acenaphthene-d10 (IS #1) 13.05 162 164

80 0.58

2-chlorobiphenyl 13.26 188 152

# 3 molinate 13.72 126 55 225 0.49

# 4

4-chlorobiphenyl 14.26 188 152

100 0.59

ethoprop 14.81 97 139, 158

# 5

α-HCH 15.55 181 183, 219

2,4'-dichlorobiphenyl 15.61 222 152, 224 50 0.60

hexachlorobenzene 15.62 284 142, 249

# 6

simazine 15.99 201 173, 186

25 0.57

dimethipin 16.04 54 53

atrazine 16.10 200 215

pentachlorophenol 16.15 266 264, 268

13C-pentachlorophenol (IS #4) 16.17 276 --

γ-HCH (lindane) 16.27 183 181, 219

# 7

2,2',5-trichlorobiphenyl 16.50 256 186

75 0.37

phenanthrene-d10 (IS #2) 16.55 188 160*

# 8

acetochlor 17.48 146 162, 223

40

 

 

 

0.62

 

 

 

2,4,4'-trichlorobiphenyl 17.52 186 256

vinclozolin 17.59 212 124

alachlor 17.66 188 160

heptachlor 17.84 100 272

# 9

2,2',5,5'-tetrachlorobiphenyl 18.25 220 292

60 0.61 metolachlor 18.50 162 238

2,2',3,5'-tetrachlorobiphenyl 18.69 220 255, 292

# 10

heptachlor epoxide 19.50 353 81, 355

50 0.47

2,3',4',5-tetrachlorobiphenyl 19.62 220 292

# 11

trans-chlordane 20.02 375 373, 377

50 

 

0.60 

 

cis-chlordane 20.35 375 373, 377

trans-nonachlor 20.42 409 407, 411
 

525.3-134 

Table 16. Example SIM Parameters for Selected Method Analytes

SIM 

Segment Compound

RT 

(min)

QI 

(m/z)

Confirmation 

Ion(s) (m/z)

Dwell 

Time 

(ms)

Scan 

Time

(sec/scan)

# 12

 

 

profenofos 20.77 339 97, 139

45

 

 

0.61

 

 

tribufos 20.91 57 169

oxyfluorfen 21.02 252 361

2,3,3',4',6-pentachlorobiphenyl 21.03 326 254, 256

# 13

 

 

 

 

endrin 21.46 263 81, 281

50

 

 

 

 

 

0.60

 

 

 

 

2,2',3,4',5',6-hexachlorobiphenyl 21.57 360 218, 290

2,3',4,4',5-pentachlorobiphenyl 21.68 326 254, 256

toxaphene, peak 1 21.74 159 125, 305*

2,2',4,4',5,5'-hexachlorobiphenyl 22.18 360 218, 290

toxaphene, peak 2 22.47 305 125

toxaphene, peak 3 22.67 159 125, 305* 

2,2',3,4,4',5'-hexachlorobiphenyl 22.81 360 218, 290

# 14

 

tebuconazole 23.12 125 83, 250

50

 

0.60

 

di(2-ethylhexyl)adipate 23.17 129 57, 70

triphenyl phosphate (SUR) 23.26 77 169, 325

# 15

 

chrysene-d12 (IS #3) 24.03 240 236*

75

 

0.55

 

methoxychlor 24.18 227 --

2,2',3,4,4',5,5'-heptachlorobiphenyl 24.44 394 252, 324

# 16

 

 

toxaphene, peak 4 24.55 159 125, 305* 

125

 

 

0.57

 

 

di(2-ethylhexyl)phthalate 24.72 149 167

c-permethrin 26.42 183 163*

t-permethrin 26.60 183 163*

# 17

benzo(a)pyrene-d12 (SUR) 27.90 264 132*

125 0.57

benzo(a)pyrene 28.03 252 126*

* Confirmation ions may be at or below 30% relative abundance depending on instrument tune. 
 

525.3-135 

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 Analysesa 

Analytes 

Fortified Conc.

0.025 μg/Lb

n=4

Fortified Conc.

0.10 μg/Lc

n=4

Fortified Conc.

0.25 μg/Ld

n=4

Mean % 

Recovery RSD Mean % Recovery

Mean % 

Recovery

Mean % 

Recovery RSD

acetochlor 103 1.8 109 1.9 105 2.2

alachlor 114 2.7 112 1.1 104 3.1

atrazine 117 5.7 118 3.6 111 1.8

benzo[a]pyrene 81.0 4.8 103 2.2 97.4 7.5

chlordane, cis 110 4.1 102 2.9 100 3.0

chlordane, trans 89.9 1.4 99.4 5.3 100 2.8

di(2-ethylhexyl)adipate NDe 114 4.2 111 1.7

di(2-ethylhexyl)phthalate ND 113 33 118 7.8

dimethipin 91.5 4.1 108 7.4 112 3.2

endrin 97.5 6.1 105 3.7 100 1.6

ethoprop 89.4 19 109 3.2 112 1.7

HCCPD 102 7.6 108 1.2 100 4.3

HCH, α 112 5.6 114 3.3 99.6 4.5

HCH, γ (lindane) 104 6.9 110 2.0 100 6.2

heptachlor 104 9.3 99.9 3.4 89.2 2.7

heptachlor epoxide 108 3.8 103 4.6 98.2 3.3

hexachlorobenzene 90.2 9.6 95.3 2.1 90.6 2.7

methoxychlor 113 8.4 116 2.8 104 1.6

metolachlor 114 1.0 115 4.3 107 1.7

molinate 104 5.7 109 2.3 109 1.4

nonachlor, trans 98.9 2.8 96.4 5.5 99.9 3.4

oxyfluorfen 114 12 115 5.2 124 6.3

pentachlorophenol 79.0 7.9 96.3 6.7 97.2 2.0

permethrin, cis 91.5 9.7 113 3.2 105 2.0

permethrin, trans 94.6 2.5 104 2.0 103 1.5

profenofos 102 8.4 92.0 2.3 112 1.7

simazine 85.2 12 101.3 13.0 124 1.9

tebuconazole 82.6 7.4 116.0 1.9 117 0.69

tribufos 96.2 7.8 101.2 3.5 105 3.9

vinclozolin 93.1 4.4 110 2.0 104 2.4
 

525.3-136 

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 Analysesa 

Analytes 

Fortified Conc.

0.025 μg/Lb

n=4

Fortified Conc.

0.10 μg/Lc

n=4

Fortified Conc.

0.25 μg/Ld

n=4

Mean % 

Recovery RSD Mean % Recovery

Mean % 

Recovery

Mean % 

Recovery RSD

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 99.9 2.7 106 1.1 98.8 2.6

4-chlorobiphenyl (3) 96.8 4.8 105 1.0 109 1.8

2,4′-dichlorobiphenyl (8) 109 12 110 7.1 102 2.4

2,2′,5-trichlorobiphenyl (18) 101 6.1 106 3.0 99.9 0.82

2,4,4′-trichlorobiphenyl (28) 90.8 10.0 105 1.7 101 1.3

2,2′,3,5′-tetrachlorobiphenyl (44) 94.5 4.2 108 5.7 98.5 3.1

2,2′,5,5′-tetrachlorobiphenyl (52) 97.0 4.6 105 1.3 101 2.5

2,3′,4′,5-tetrachloroobiphenyl (70) 88.3 15 103 6.5 100 2.5

2,3,3′,4′,6-pentachlorobiphenyl (110) 92.0 3.7 99.9 4.9 99.2 1.6

2,3′,4,4′,5-pentachlorobiphenyl (118) 86.2 8.8 96.5 3.7 97.6 2.5

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 86.7 3.7 96.1 4.4 96.3 1.5

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 95.3 4.7 97.4 3.1 95.4 2.3

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 86.8 2.0 98.7 0.79 97.2 1.4

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 99.7 9.5 97.6 4.3 95.7 2.0

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 101 2.2 105 3.6 93.6 4.4

benzo[a]pyrene-d12 87.9 3.0 92.1 2.4 94.5 8.8

triphenyl phosphate 103 1.9 106 3.2 101 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 μg/L, pentachlorophenol 

is 0.10 μg/L, tebuconazole is 0.12 μg/L, c-permethrin is 0.014 μg/L, and t-permethrin is 0.036 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 μg/L, pentachlorophenol 

is 0.40 μg/L, tebuconazole is 0.50 μg/L, c-permethrin is 0.056 μg/L, and t-permethrin is 0.144 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 μg/L, pentachlorophenol 

is 1.0 μg/L, tebuconazole is 1.02 μg/L, c-permethrin is 0.14 μg/L, and t-permethrin is 0.36 μg/L. 

e. ND = Not determined. Analyte could not be determined because of the low concentration relative to the LRB.
 

525.3-137 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

acetochlor 0.10 109 9.6 NAe 

alachlor 0.10 110 5.9 112 3.6

atrazine 0.10 112 11 101 0.45

benzo[a]pyrene 0.10 86.3 2.7 104 7.6

chlordane, cis 0.10 98.1 3.4 97.9 3.9

chlordane, trans 0.10 101 4.3 102 3.7

di(2-ethylhexyl)adipate 0.10 116 7.4 114 4.8

di(2-ethylhexyl)phthalate 0.10 NDf ND

dimethipin 0.10 96.0 7.4 103 18

endrin 0.10 112 4.4 107 3.3

ethoprop 0.10 111 9.6 102 3.6

HCCPD 0.10 122 7.4 82.8 7.3

HCH, α 0.10 111 8.4 84.5 7.2 

HCH, γ (lindane) 0.10 100 5.5 108 4.6

heptachlor 0.10 90.9 5.9 85.3 5.8

heptachlor epoxide 0.10 96.5 4.5 103 1.4

hexachlorobenzene 0.10 90.4 4.9 83.8 3.3

methoxychlor 0.10 116 4.1 128 1.3

metolachlor 0.10 112 6.3 NA

molinate 0.10 120 7.2 NA

nonachlor, trans 0.10 93.3 3.8 NA

oxyfluorfen 0.10 122 6.5 123 4.6

pentachlorophenol 0.40 90.5 8.2 94.9 0.88

permethrin, cis 0.06g 106 5.0 102 5.1

permethrin, trans 0.14h 101 3.6 108 3.0

profenofos 0.10 107 3.5 110 6.8

simazine 0.10 101 10 105 3.0

tebuconazole 0.50 115 5.6 99.9 4.5

tribufos 0.10 107 5.9 110 3.5
 

525.3-138 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recoveryd RSD

vinclozolin 0.10 103 8.3 104 4.2

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 0.10 87.8 9.6 95.8 4.5

4-chlorobiphenyl (3) 0.10 104 6.4 96.5 3.5 

2,4′-dichlorobiphenyl (8) 0.10 110 5.9 90.0 4.9 

2,2′,5-trichlorobiphenyl (18) 0.10 93.0 4.0 92.7 3.2

2,4,4′-trichlorobiphenyl (28) 0.10 97.2 6.1 91.4 2.1

2,2′,3,5′-tetrachlorobiphenyl (44) 0.10 96.8 3.9 81.6 5.2

2,2′,5,5′-tetrachlorobiphenyl (52) 0.10 94.2 4.4 95.3 5.0

2,3′,4′,5-tetrachloroobiphenyl (70) 0.10 95.4 4.9 98.8 0.85

2,3,3′,4′,6-pentachlorobiphenyl (110) 0.10 92.8 4.6 97.5 3.0

2,3′,4,4′,5-pentachlorobiphenyl (118) 0.10 91.5 5.6 92.3 3.0

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 0.10 101 4.6 96.9 3.5

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 0.10 93.6 4.4 96.6 1.5

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 0.10 92.1 4.8 94.5 0.86

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 0.10 92.1 3.7 92.6 2.1

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 1.0 106 5.4 95.3 5.7

benzo[a]pyrene-d12 1.0 84.4 2.6 100 5.6 

triphenyl phosphate 1.0 103 2.7 106 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 μg/L.

h. The concentration in ground water is as listed in the table. The concentration in surface water is 0.070 μg/L.
 

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 H2O Phobic 

Speedisks; SIM GC/MS Analysesa

Analytes 

Fortified Conc.

0.025μg/Lb

n=4

Fortified Conc.

0.10 μg/Lc

n=4

Fortified Conc.

0.25 μg/Ld

n=4

Mean % 

Recovery RSD Mean % Recovery

Mean % 

Recovery

Mean % 

Recovery RSD

acetochlor 99.0 1.7 98.7 1.9 98.8 0.67

alachlor 111 2.3 100 1.1 100 1.0

atrazine 106 5.0 98.6 6.0 99.3 1.2

benzo[a]pyrene 89.6 2.4 93.3 2.9 91.8 2.3

chlordane, cis 100 1.3 98.0 2.4 99.2 1.6

chlordane, trans 100 0.60 96.5 2.5 97.5 1.6

di(2-ethylhexyl)adipate 102 1.1 94.9 5.1 96.2 2.8

di(2-ethylhexyl)phthalate NDe ND ND

dimethipin 86.0 9.9 105 6.9 98.8 1.5

endrin 105 3.6 105 1.5 104 0.76

ethoprop 104 4.1 101 2.7 98.0 1.0

HCCPD 85.8 5.1 86.6 3.5 87.4 1.3

HCH, α 101 2.0 96.8 2.0 96.2 2.0

HCH, γ (lindane) 102 1.8 96.3 3.3 97.0 2.1

heptachlor 96.7 3.2 90.6 3.4 89.9 1.5

heptachlor epoxide 103 2.0 99.3 1.9 101 1.9

hexachlorobenzene 94.7 2.1 88.0 2.2 91.2 1.8

methoxychlor 104 2.9 101 4.0 101 2.1

metolachlor 104 1.5 101 2.3 101 1.3

molinate 110 13 95.7 2.6 96.1 1.3

nonachlor, trans 99.5 1.0 97.3 2.6 97.4 1.6

oxyfluorfen 107 1.4 107 5.7 105 2.2

pentachlorophenol 99.5 1.4 93.6 2.4 92.8 1.6

permethrin, cis 97.0 5.0 95.6 5.4 93.1 2.4

permethrin, trans 95.8 2.5 95.5 5.1 96.0 2.1

profenofos 109 1.7 105 3.6 105 1.5

simazine 105 0.71 99.7 5.1 100 0.74

tebuconazole 125 2.8 114 4.1 112 2.3

tribufos 95.0 5.2 96.9 4.3 98.7 1.2

vinclozolin 89.2 6.7 82.7 6.3 87.1 6.6
 

525.3-140 

Table 19. Precision and Accuracy Data Obtained for Selected Method Analytes Fortified in 

Reagent Water at Three Concentrations and Extracted Using J.T. Baker H2O Phobic 

Speedisks; SIM GC/MS Analysesa

Analytes 

Fortified Conc.

0.025μg/Lb

n=4

Fortified Conc.

0.10 μg/Lc

n=4

Fortified Conc.

0.25 μg/Ld

n=4

Mean % 

Recovery RSD Mean % Recovery

Mean % 

Recovery

Mean % 

Recovery RSD

PCB congeners (by IUPAC#) 96.4 1.6 94.5 2.8 95.3 2.9

2-chlorobiphenyl (1) 97.3 1.7 93.4 2.5 93.2 1.1

4-chlorobiphenyl (3) 95.0 1.8 93.2 2.9 92.4 1.8

2,4′-dichlorobiphenyl (8) 97.2 2.0 94.6 2.7 93.7 1.5

2,2′,5-trichlorobiphenyl (18) 94.8 1.2 92.9 2.3 94.8 1.3

2,4,4′-trichlorobiphenyl (28) 98.4 2.2 94.3 2.3 95.5 1.7

2,2′,3,5′-tetrachlorobiphenyl (44) 96.5 2.2 93.6 2.4 95.2 1.5

2,2′,5,5′-tetrachlorobiphenyl (52) 97.6 1.8 95.7 2.4 96.8 3.6

2,3′,4′,5-tetrachloroobiphenyl (70) 98.7 1.4 95.0 2.3 96.1 1.4

2,3,3′,4′,6-pentachlorobiphenyl (110) 97.9 1.5 95.4 2.5 96.3 1.7

2,3′,4,4′,5-pentachlorobiphenyl (118) 101 1.1 91.9 2.3 94.6 2.8

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 96.8 1.3 94.7 2.4 95.2 1.7

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 95.9 1.0 94.2 2.4 94.5 1.9

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 92.8 1.5 87.9 2.1 87.1 2.6

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180)

Surrogate Analytes

2.5 96.4 1.2 95.4 2.4

1,3-dimethyl-2-nitrobenzene 89.0 2.2 92.0 1.8 91.6 2.1

benzo[a]pyrene-d12 100 2.6 101 2.0 100 2.9

triphenyl phosphate 99.0 1.7 98.7 1.9 98.8 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 μg/L, pentachlorophenol 

is 0.10 μg/L, c-permethrin is 0.014 μg/L, and t-permethrin is 0.036 μg/L.

c. Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 μg/L, pentachlorophenol 

is 0.40 μg/L, c-permethrin is 0.058 μg/L, and t-permethrin is 0.14 μg/L.

d. Exceptions to the stated concentration are as follows: Surrogate concentrations are 1.0 μg/L, pentachlorophenol 

is 1.0 μg/L, c-permethrin is 0.14 μg/L, and t-permethrin is 0.36 μg/L.

e. ND = Not determined. Matrix spike recovery could not be determined due to the low fortification concentration 

relative to the background concentration.

96.2
 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recovery c RSD

acetochlor NAd

alachlor 0.10 90.4 6.6 104 1.4

atrazine 0.10 112 5.3 125 0.94

benzo[a]pyrene 0.10 84.8 5.1 83.1 6.1

chlordane, cis 0.10 91.0 4.5 98.4 1.8

chlordane, trans 0.10 90.4 4.1 98.5 1.8

di(2-ethylhexyl)adipate 0.10 67.0 7.9 81.0 8.2

di(2-ethylhexyl)phthalate 0.10 NDe NDe

dimethipin 0.10 69.6 9.7 70.8 6.7

endrin 0.10 95.3 4.2 108 2.9

ethoprop 0.10 91.0 4.4 109 1.8

HCCPD 0.10 82.4 8.9 163 4.2

HCH, α 0.10 90.9 4.2 96.9 1.7

HCH, γ (lindane) 0.10 88.2 4.8 91.9 0.73

heptachlor 0.10 90.6 5.1 101 1.3

heptachlor epoxide 0.10 93.8 4.3 104 1.5

hexachlorobenzene 0.10 87.3 5.6 90.8 1.9

methoxychlor 0.10 98.9 5.6 121 1.8

metolachlor NA

molinate NA

nonachlor, trans NA

oxyfluorfen 0.10 100 6.2 141 1.3

pentachlorophenol 0.40 90.2 5.5 89.0 1.8

permethrin, cis 0.058 87.1 4.5 108 4.3

permethrin, trans 0.14 86.3 4.9 105 3.5

profenofos 0.10 96.8 5.5 119 2.1

simazine 0.10 84.9 7.1 97.2 2.7

tebuconazole 0.50 109 5.6 138 2.5

tribufos 0.10 95.9 9.0 117 3.2
 

525.3-142 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recovery c RSD

vinclozolin 0.10 90.3 4.9 104 1.5

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 0.10 85.8 4.7 88.1 1.4

4-chlorobiphenyl (3) 0.10 85.3 4.8 89.1 1.7

2,4′-dichlorobiphenyl (8) 0.10 87.0 4.7 89.9 1.8

2,2′,5-trichlorobiphenyl (18) 0.10 90.2 2.2 90.4 1.3

2,4,4′-trichlorobiphenyl (28) 0.10 87.7 4.3 91.0 1.8

2,2′,3,5′-tetrachlorobiphenyl (44) 0.10 87.7 3.9 89.9 2.0

2,2′,5,5′-tetrachlorobiphenyl (52) 0.10 87.3 4.0 90.8 1.8

2,3′,4′,5-tetrachloroobiphenyl (70) 0.10 84.1 3.6 88.2 2.1

2,3,3′,4′,6-pentachlorobiphenyl (110) 0.10 84.8 3.4 88.7 2.2

2,3′,4,4′,5-pentachlorobiphenyl (118) 0.10 83.6 2.4 88.1 3.1

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 0.10 77.4 2.6 79.9 4.3

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 0.10 81.6 2.7 84.7 3.6

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 0.10 76.9 2.9 77.8 4.7

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 0.10 67.9 4.4 67.9 8.7

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 1.0 102 1.0 109 0.60

benzo[a]pyrene-d12 5.0 119 2.0 112 5.0

triphenyl phosphate 1.0 99.1 3.4 110 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.
 

525.3-143 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recovery c RSD

acetochlor NAd

alachlor 0.50 90.8 1.1 95.8 3.3

atrazine 0.50 90.5 0.85 92.1 3.7

benzo[a]pyrene 0.50 92.3 2.8 79.6 6.6

chlordane, cis 0.50 92.5 1.1 94.6 2.8

chlordane, trans 0.50 91.9 0.98 94.1 2.6

di(2-ethylhexyl)adipate 0.50 73.5 1.1 76.3 9.9

di(2-ethylhexyl)phthalate 0.50 NDe NDe

dimethipin 0.50 72.3 6.0 69.7 7.8

endrin 0.50 96.1 1.3 102 3.0

ethoprop 0.50 91.7 1.6 97.7 2.9

HCCPD 0.50 89.1 2.2 114 1.6

HCH, α 0.50 92.4 1.4 92.6 3.6

HCH, γ (lindane) 0.50 91.3 1.0 90.7 3.0

heptachlor 0.50 92.8 1.2 97.7 2.3

heptachlor epoxide 0.50 94.6 1.4 97.6 2.7

hexachlorobenzene 0.50 89.3 1.7 90.0 3.2

methoxychlor 0.50 99.7 1.3 104 2.6

metolachlor NA

molinate NA

nonachlor, trans NA

oxyfluorfen 0.50 93.0 0.83 107 2.7

pentachlorophenol 2.0 92.3 1.3 89.7 2.8

permethrin, cis 0.15 81.1 1.4 86.1 4.4

permethrin, trans 0.35 82.2 0.97 84.9 3.8

profenofos 0.10 93.3 2.1 99.4 3.0

simazine 0.50 82.8 1.0 85.0 3.3

tebuconazole 2.5 96.5 1.3 103 2.7

tribufos 0.50 91.4 1.0 98.0 2.5
 

525.3-144 

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 Analysesa

Analytes

Fortified 

Conc. (μg/L)

Ground Waterb Surface Waterc

Mean % 

Recoveryd RSD Mean % Recovery c RSD

vinclozolin 0.50 91.3 1.0 94.7 2.7

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 0.50 89.7 1.8 87.8 4.7

4-chlorobiphenyl (3) 0.50 87.7 1.9 87.5 3.7

2,4′-dichlorobiphenyl (8) 0.50 89.7 1.9 89.4 3.3

2,2′,5-trichlorobiphenyl (18) 0.50 90.9 1.5 90.2 3.0

2,4,4′-trichlorobiphenyl (28) 0.50 90.6 1.1 90.8 2.9

2,2′,3,5′-tetrachlorobiphenyl (44) 0.50 90.5 1.1 90.0 3.1

2,2′,5,5′-tetrachlorobiphenyl (52) 0.50 90.2 1.4 90.1 2.9

2,3′,4′,5-tetrachloroobiphenyl (70) 0.50 90.6 1.7 88.8 3.2

2,3,3′,4′,6-pentachlorobiphenyl (110) 0.50 88.5 2.2 86.6 3.7

2,3′,4,4′,5-pentachlorobiphenyl (118) 0.50 86.1 1.2 86.0 3.2

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 0.50 80.6 0.86 78.9 3.1

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 0.50 83.5 0.84 81.5 3.0

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 0.50 79.1 0.82 76.1 3.2

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 0.50 71.0 0.72 64.9 2.8

Surrogate Analytes

1,3-dimethyl-2-nitrobenzene 1.0 103 0.65 108 0.93

benzo[a]pyrene-d12 5.0 117 2.6 112 5.1

triphenyl phosphate 1.0 102 1.8 112 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.
 

525.3-145 

Table 21. Precision and Accuracy Data for Toxaphene Extracted from Fortified Reagent 

Water; Sample Extracts Analyzed in SIM GC/MS Mode 

Sorbent

Fortified Conc.

1.0 μg/L 

n=4

Fortified Conc.

10 μg/L

n=4

Fortified Conc.

25 μg/L 

n=4

Mean % 

Recovery RSD Mean % Recovery RSD Mean % Recovery RSD

Oasis-HLBa 82.9 5.0 101 3.3 89.5 8.8

J.T. Baker H2O Phobic 

cartridgea 100 3.63 104 3.8 98.5 1.7

J.T. Baker H2O Phobic 

Speediskb 114 1.0 103 3.4 98.5 2.8

Empore SDB-XCa 107 5.3 111 2.1 101 0.15

UCT 525 Universal 

Cartridgea NAc 111 1.8 NA

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 μg/L. 

Table 22. Precision and Accuracy Data for Toxaphene Extracted from Fortified Drinking 

Water Samples; Sample Extracts Analyzed in SIM GC/MS Mode

Sorbent

Ground Water a

Fortified Conc.

10 μg/L, n=4

Surface Water b

Fortified Conc.

10 μg/L, n=4

Mean % Recovery RSD Mean % Recovery RSD

Oasis-HLBc 95.4 3.7 94.2 5.9

J.T. Baker H2O Phobic 

cartridgec 102 5.6 103 3.5

J.T. Baker H2O Phobic 

Speediskd 120 2.4 124 1.9

Empore SDB-XCc 106 4.6 104 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.
 

525.3-146 

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 H2O Phobic Speedisks, 

All Samples Analyzed in SIM Mode, All concentrations in μg/L

Analytes

Oasis HLBa Baker Speediskb

DLc Fortified conc. of 

DL replicates LCMRL LCMRL

acetochlor 0.0047 0.010 0.011 0.0091

alachlor 0.0045 0.010 0.016 0.013

atrazine 0.0062 0.010 0.023 0.015

benzo[a]pyrene 0.0069 0.010 0.036 0.0060

chlordane, cis 0.0016 0.010 0.0073 0.0039

chlordane, trans 0.0028 0.010 0.0097 0.0020

di(2-ethylhexyl)adipate NDd 0.38 0.020

di(2-ethylhexyl)phthalate ND 0.43 ND

dimethipin 0.0093 0.010 0.022 0.065

endrin 0.0081 0.010 0.014 0.011

ethoprop 0.0082 0.010 0.036 0.0084

HCCPD 0.0055 0.010 0.014 0.0026

HCH, α 0.0068 0.010 0.021 0.0040

HCH, γ (lindane) 0.0040 0.010 0.031 0.0071

heptachlor 0.0034 0.010 0.010 0.0024

heptachlor epoxide 0.0026 0.010 0.017 0.0031

hexachlorobenzene 0.0092 0.010 0.014 0.0065

methoxychlor 0.0025 0.010 0.021 0.0011

metolachlor 0.0035 0.010 0.019 0.004

molinate 0.0057 0.010 0.010 0.029

nonachlor, trans 0.0029 0.010 0.0061 0.0066

oxyfluorfen 0.0038 0.010 0.035 0.031

pentachlorophenol 0.047 0.100 0.068 0.0086

permethrin, cis 0.0041 0.006 0.012 0.0015

permethrin, trans 0.0080 0.014 0.020 0.0023

profenofos 0.0081 0.010 0.029 0.012

simazine 0.010 0.025 0.048 0.018

tebuconazole 0.042 0.12 0.20 0.037
 

525.3-147 

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 H2O Phobic Speedisks, 

All Samples Analyzed in SIM Mode, All concentrations in μg/L

Analytes

Oasis HLBa Baker Speediskb

DLc Fortified conc. of 

DL replicates LCMRL LCMRL

toxaphene 0.32 1.0 1.4 NFe 

tribufos 0.0033 0.010 0.023 0.0063

vinclozolin 0.0064 0.010 0.0098 0.095

PCB congeners (by IUPAC#)

2-chlorobiphenyl (1) 0.0024 0.010 0.0080 0.0063

4-chlorobiphenyl (3) 0.0049 0.010 0.0073 0.0056

2,4′-dichlorobiphenyl (8) 0.0045 0.010 0.023 0.0022

2,2′,5-trichlorobiphenyl (18) 0.0038 0.010 0.013 0.0012

2,4,4′-trichlorobiphenyl (28) 0.0056 0.010 0.014 0.0084

2,2′,3,5′-tetrachlorobiphenyl (44) 0.0063 0.010 0.025 0.0020

2,2′,5,5′-tetrachlorobiphenyl (52) 0.0027 0.010 0.0078 0.0012

2,3′,4′,5-tetrachloroobiphenyl (70) 0.013 0.025 0.036 0.0022

2,3,3′,4′,6-pentachlorobiphenyl (110) 0.0030 0.010 0.0092 0.0035

2,3′,4,4′,5-pentachlorobiphenyl (118) 0.0077 0.010 0.013 0.0026

2,2′,3,4,4′,5′-hexachlorobiphenyl (138) 0.0081 0.010 0.016 0.015

2,2′,3,4′,5′,6-hexachlorobiphenyl (149) 0.0063 0.010 0.012 0.0021

2,2′,4,4′,5,5′- hexachlorobiphenyl (153) 0.0092 0.010 0.013 0.0038

2,2′,3,4,4′,5,5′-heptachlorobiphenyl (180) 0.0029 0.010 0.015 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.
 

525.3-148 

Table 24. Initial Demonstration of Capability (IDC) and Quality Control (QC) Requirements (Summary)

Method 

Reference

Requirement Specification and Frequency Acceptance Criteria

Sect. 9.2.1

& 9.3.1

Initial Demonstration of 

Low Background

Analyze LRB prior to any other IDC steps. When a new 

lot of SPE media is obtained, verify that background is 

at acceptable limits.

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.

Sect. 9.2.2 Initial Demonstration of 

Precision (IDP)

Analyze 4-7 replicate LFBs fortified near the midrange 

calibration concentration.

%RSD must be ≤ 20%

Sect. 9.2.3 Initial Demonstration of 

Accuracy (IDA)

Calculate average recovery for replicates used in IDP. 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

Sect. 9.2.4 Minimum Reporting 

Limit (MRL) 

Confirmation 

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. 

Upper PIR ≤ 150%

Lower PIR ≥ 50% 

Sect. 9.2.5 

& 9.3.9

Calibration Confirmation,

Quality Control Sample 

(QCS)

Analyze a standard from a second source (QCS) to 

verify the initial calibration curve.

± 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.
 

525.3-149 

Table 25. Ongoing Quality Control (QC) Requirements (Summary) 

Method 

Reference

Requirement Specification and Frequency Acceptance Criteria

Sect. 8.4 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.

Sect. 8.4 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 ≤ 1/3 the MRL, and confirm that possible 

interferences do not prevent quantification. If the 

background concentration exceeds 1

/3 the 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 CAL 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.
 

525.3-150 

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.
 

525.3-151 

Figure 1a. Example chromatogram of a calibration standard (concentration of 5 ng/μL injected for most analytes). Peak 

identification numbers correspond to those in Table 1. 
 

525.3-152 

Figure 1b. Example chromatogram of a calibration standard (concentration of 5 ng/μL injected for most analytes). Peak 

identification numbers correspond to those in Table 1. 
 

525.3-153 

Figure 1c. Example chromatogram of a calibration standard (concentration of 5 ng/μL injected for most analytes). Peak 

identification numbers correspond to those in Table 1. 
 

525.3-154 

Figure 1d. Example chromatogram of a calibration standard (concentration of 5 ng/μL injected for most analytes). Peak 

identification numbers correspond to those in Table 1. 
 

525.3-155 

Figure 2. Example extracted ion current profiles of toxaphene at m/z 125, 305, and 159. 
 

525.3-156 

Figure 3a. Results of Aqueous Holding Time Study (Sect. 13.4) 

 
 

525.3-157 

Figure 3b. Results of Aqueous Holding Time Study (Sect. 13.4) 
 

525.3-158 

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

525.3-159 

Figure 4a. Results of Extract Holding Time Study (Sect. 13.5) 
 

525.3-160 

Figure 4b. Results of Extract Holding Time Study (Sect. 13.5) 

 
 

525.3-161 

Figure 4c. Results of Extract Holding Time Study (Sect. 13.5)