525.3

- 1 

### EPA Document #: EPA/600/R-12/010

METHOD 52 5.3 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)

Dav id 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 45268525.3

- 2 

### METHOD 52 5.3

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 water s for the compounds listed in the table below. This method was

initially developed with full scan GC/MS, but performa nce has also been demonstrated

in the selected ion monitoring ( SIM ) mode using a subset of analytes. SIM is useful

when enhance d sensitivity is desirable. An example chromatogram which includes the

entire analyte list is shown in Fig s. 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

Benz o [ 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

Chlor o neb 2675

- 77

- 6

Chlorobenzilate 510

- 15

- 6525.3

- 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 p arathion 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

- 7525.3

- 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 p arathion 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

Nitro f en 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

P ro meton 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

- 8525.3

- 5 

### Analyte Chemical Abstract

Services Registry

Number (CASRN)

Vernolate 1929

- 77

- 7

Vinclozolin 50471

- 44

- 8

P olychlorinated 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 percen t 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 require ments 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 full525.3

- 6 

### scan mode (T able 1 5 ) 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 Analyst s 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 m ass . Using the

instrument parameters in Method 525.3, techn ical 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 cal ibration 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 - and525.3

- 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 M ETHOD 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 m ade to sample collection and preservation (Sect. 8), sample

extraction (Sect. 11) or to the Q uality Control (QC) requirements (Sect. 9). Method

modifications should be considered only to improve method performance.

Modifications that are introduced in th e 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

.

N ote : The above method flexibility section is intended as an abbreviated summation

of method flexibility. Sect s. 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 Sect s. 4-

12, Sect s. 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 (Sect s. 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, c oncentrated by evapor ation with nitrogen gas

, and then adjusted to a 1- mL volume with ethyl acetate after adding the internal

standard s. A splitless injection is made into a GC equipped with a high-resolution

fused silica capillary column that is interfac ed 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 t he 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

(Sect s. 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. 3.1 4 ), when analyzed at low concentrations. Refer to525.3

- 8 

### the “comments” section of Table 1 for potentially affected analytes, and to Sect. 13

for information regard ing 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 matri x-matched standards (Sect. 3.1 5 )

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 meth od 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 an alyte

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 M atrix, 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

estim a te 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 sta ndard

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 de termine 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 f ortified, 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 concen tration for whic h 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 p roperties, 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 me thod 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

- in duced response enhancement effects and improves the

quantitative accuracy of sample results

. 1 2,13



### 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 prepar ed 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 s olution prepared using a PDS of

method ana lytes obtained from a source external to th e 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 t he characteristic ions of the

analyte s , SUR s and IS s 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 analyte s , SUR s and IS s 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 proc essing

hardware that lead to discrete artifacts and/or elevated baselines in the chromato

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

interferences (less than 1 

### / 3 

### the MRL for each target analyte) under the conditions of

t he 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 baseline s 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. Interfer ences from these sources should be monitored by analysis of

laboratory reagent blanks, par ticularly 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 lo ts

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 to525.3

- 12 

### ensure that accurate values are obtained for the next sample. The analyst should be

especially careful to check for carryover of poly cyclic 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 i on 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 a re 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,

esp ecially from plastics and chemicals that may have been stored in plastic

containers. If phthala tes 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 th e media to be come 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, s ample 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 all525.3

- 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

R eferences to specific brands or catalog numbers are included for illustrat ion 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 s orbents 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 determin e. 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 sorb ent materials m ust be addressed to the Office of

Ground Water and Drinking Water Alternate Test Procedure Coordinator. 19



### 6.1. SAMPLE CONTAINERS - 1-L or 1 -qt amber glass bottles fitted with

polytetrafluoroethylene (PTFE)- lined screw caps are preferred. Clear glass bottles

with PTFE

- lined screw caps may be substituted if sample bottles are wrapped with

foil, stored in boxes, or otherwise protected from light during sample shipping and

storage.

6.2. VIALS

- Various sizes of amber glass vials with PTFE -lined screw caps for storing

standard solutions and extracts. Amber glass 2- mL autosampler vials with PTFE

faced septa.

6.3. VOLUMETRIC FLASKS - Class A, suggested sizes include 1, 5, and 10 mL for

preparation of standards and dilution of extract to final volume.

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

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

1000 μL.

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

anhydrous sodiu m sulfate (Na 2 

### SO 4 

### ). 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

closel y 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 ma y be modified to

a chieve 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 qualit y. 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 tra pped 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 H 2 

### O 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. Al l 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 b e 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. SP E 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) -

d ivinylbenzene N -vinylpyrrolidone copolymer

6.11.1.2. J.T. Baker Speedisk Column H 2 

### O Phobic DVB , 200 mg (# 8109-09) - divinylbenzene polymer

6.11.2. VACUUM EXTRACTION MANIFOL D - Equipped with flow/vacuum

control (Supelco #57030-U or equivalent).525.3

- 16 

### 6.11.3. SAMPLE DELIVERY SYSTEM

- Use of a transfer t ube 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 Sec t. 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 possibl e 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 m ay 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 - U nited Chemical Technologies (U CT ) 525 Universal

cartridge, #ECUNI525, 1500 mg octadecyl unendcapped bonded silica,

carbon loading 15-18%, surface area approximately 500 m 2 

### /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 man ual procedure. The solvents

used for washing, conditioning, and sample elution must be the same as525.3

- 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 t imes. 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 USIN G 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 SPECTROMETE R (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 equiva lent). Any capillary column that

provides adequate capacity, resolution, accuracy, and precision m ay 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 inject ion port. This

problem is exacerbated when the injector and/or the injection port liner is525.3

- 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 w ere 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 i nterface 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 solu tion containing 5 ng (or less) of

decafluorotriphenylphos phine (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 integrati on 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 i ntended 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 (EtOA c) (CASRN 141 -78- 6) - High purity,

demonstrated to be free of ana lytes 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

equiva lent).

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 (Na 2 

### SO 4 

### ), 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

ship ment 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 ana lytes 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 o f a gravimetrically prepared s tock 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 the525.3

- 20 

### laborato ry. 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 ot her

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, 13 

### C-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 th e 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 wer e 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

- d 10 

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

phenanthrene- d 10 

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

chrysene

- d 12 

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

13 

### C- pen ta chlorophenol (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. The525.3

- 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 S amp le prior to

extraction, for an expected final extract concentration of 5 μg/L of each

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

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

Surrogates CASRN Solvent PD S 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

- d 12 

### (SUR 3) 63466-71-7 acetone 500 μg/mL

Note s:

• 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 sho uld 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

c ommercially 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%, the525.3

- 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 SOLUTIO N (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.

Note s:

• It may be nece ssary to prepare multiple A nalyte PDS mixtures

based on the laboratory’s specific compounds of interest. For

example, the method was developed using an A nalyte PDS mix

containing analytes from Method 525.2 in acetone, a PCB PDS

mix in acetone, a PDS mix c ontaining 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 “ c omments ” 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

concentrat ions 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 be525.3

- 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 analyte s 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 likel y 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. H owever, 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 a nd 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 concentration s 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 are525.3

- 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 co ncentrations 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 (Sect s. 7.2.1. and 7.2.2 ). All

calibration solutions should contain at least 6 0% 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

se ts 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 s tore d 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 reage nt 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 , SUR s, 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 am ber

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. S AMPLE BOTTLE PREPARATION

8.1.1. Grab samples must be collected using 1

- liter or 1 -quart sample bottle s that meet

the requirements in Sect. 6.1.525.3

- 25 

### Note: Larger sample s 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 A mount 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 p otassium 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 r efrigerate

.

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, with525.3

- 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 o r 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

e xtracts 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 require ments that must be met when preparing and analyzing Field Samples.

This section describes QC parameter s, 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 ac ceptable 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

foll owing the procedure outlined below.

Note: Setting an MRL for m ethod 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 R esults

(HR PIR 

### ) 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 + HR PIR 

### ) meet the upper and lower

recovery limits as shown below:525.3

- 28 

### The Upper PIR Limit must be ≤150 percent recovery.

150% %100 ≤× +

ion Concentrat Fortified HR Mean

PIR



### The Lower PIR Limit must be ≥ 50 percent recovery.

50% %100 ≥× −

ion Concentrat Fortified HR Mean

PIR



### 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

re quired 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 quan titative 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 verif y 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 a nalyses 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 conce ntration 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 S ects. 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(

=−− ×=

α n ts DL

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 require d with

each extraction batch to 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 conta minants that

inter fere 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 greater525.3

- 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 r equired 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. S imilarly, 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- le vel 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). D aily DFTPP

analysis is not required.

Note: The tune check is perfor med in full s can 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, 13 

### C-pentachlorophenol, is

expected to have greater area count variability, and therefore is not subject525.3

- 31 

### to the most recent CCC criterion. If the IS area s 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

th e 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 - S urrogate standard s 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 equatio n

100 % ×      

= B A R



### w here :

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 is525.3

- 32 

### acceptable, extraction of the sample should be repeated provided

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

extracted sample also fails the recovery criterion, report all data for

that sample as suspect/surrogate recovery to inform the data user

that the results are suspect due to surrogate recovery.

9.3.7. LABORATORY FORTIFIED SAMPLE MATRIX (LFSM)

- Within each

analysis batch , analyze a minimum of one LFSM. The native concentrations of

the analytes in the sample matrix must be determined in a second duplicate

sample and subtracted from the measured values in the LFSM. If a variety of

different sample matrices are analyzed regularly, for example, drinking water

from ground water and surface water sources, performance data must be collected

for each source.

9.3.7.1. Prepare the LFSM by fortifying a Field Duplicate with an

appropriate amount of analyte PDS (Sect. 7.2.3.2). Select a

fortification concentration that is greater than or equal to the matrix

background concentration, if known. Selecting a duplicate sample

that has already been analyzed aids in the selection of an

appropriate fortification concentration. If this is not possible, u se

historical data . If historical data are unavailable, rotate th e 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 th e fortified sample

B = measured concentration in the unfortified sample

C = fortification concentration.

N ote: 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 for525.3

- 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

ma trix 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 Ma trix 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. Ca lculate the relative percent difference ( RPD ) for duplicate

measurements ( FD1 and FD2 ) using the equation



# ( ) 100

2/21

21

×

+ −

= FDFD FDFD

RPD

9.3.8.2. RPDs for Field Duplicates should be ≤ 30 % . Greater variabil ity

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/ ×

+ −

= LFSMD LFSM LFSMD

LFSM

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 that525.3

- 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 m atrix. 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 (Se ct. 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 MODIFICA TION QC REQUIREMENTS

- The analyst is permitted to

modify GC columns, GC conditions, GC injection techniques, extract evaporation

techniques, MS conditions and QI s. 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 mad e, t he 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 perf orm 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 a n analyte

fortified surface water with moderate to high T OC (e.g., 2 mg/L or greater)

and a n analy t e fortifie d 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 ana lyzing 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 instrumen t 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 modifi cations necessar y 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 entir e peak to evaluate

the perform ance 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 BRE A KDOWN 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 perfo rmed 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 anal ytes, 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 mode525.3

- 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 inject ion 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 - In ject a 1

- μL aliquot into a hot, splitless injection

port held at 275 o C with a pressure pulse of 30 psi and a split delay

of 1 min. The temperature program is as follows: initial ov en temperature of 70 oC, hold for 1.5 min, ramp at 10 oC/min to 200

oC, ramp at seven o C/ min to a final temperature of 32 0 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 da ta

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 proper525.3

- 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 oper ation by sequencing multiple analysis batches ;

however, the entire analysis batch is invalid if one or more analyte

peaks have drift ed outside of designated time windows in the CCC

at the beginning or end of the analysis batch

.

10.2.3.3. SIM MS Acquistion Parameter s - P rior 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 QI s 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 interference s 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 f ive spectra durin g 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

se quencing multiple analysis batches ; however, the entire analysis

batch is invalid if one or more analyte peaks ha ve drift ed 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 meth od 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 the525.3

- 38 

### retention times of all method analytes in CCCs, LFB s and LFMs.

This requirement does not preclude continuous operation by

sequencing multiple analysis batch es; however, the entire a nalysis

batch is invalid if one or more analyte peaks ha ve drift ed 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, p repare 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 fo r 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 saturat e the detector at the higher concentrations. It is likely

that the calibration range for all analytes will not be the same. The use of

custo m calibration standards with varying analyte concentration s based on

their relative instrument response is a possible alternative.

10.2.5. CALIBRATION

- Calibrate the GC/MS system using the internal standard

tech nique in either full scan

, SIM or alternati ng 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 QI s for all method analytes are listed in

Table 1. Table 1 6 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. Howev er, 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 calibrat ion

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 of525.3

- 39 

### sugge sted peak selection, and Table 1 6 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

con centration 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 poi nts 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 meet ing 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

alterna te 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 a nalysis

batch must be at or be low 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 st andard (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 criteri on.

• Separat e 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 ha s 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 these525.3

- 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

calcu lated amount for each anal yte 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 h as been restored, with the following

exception. If the CCC at the end of an a nalysis 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

dete ction 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, repla cing filament assemblies, or replacing the

GC column, etc., will likely r equire 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. M ark

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 SUR525.3

- 41 

### PDS s (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 Fort ifi cation 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

- Th is 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 mo de 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

u sed.

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 tho se 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 oxidiz e 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. CARTR IDGE CLEANUP

- Ins tall the SPE cartridge ( Oasis HLB or J.T.

Baker H 2 

### O Phobic DVB as described in Sect. 6.11.1) into the vacuum

manifold . Wash the cartridge with 5 mL of EtOAc by adding the solvent to

the cartridge ; draw about half through the sorbent, soak for about one min,

then draw the remaining solvent through the cartridge

.

11.3.2. CARTRIDGE CONDITIONING

- Polymeric SPE sorbents are water

wettable (unlike C -18 SPE sorbents). Many manufacturers of polymeric

SPE media suggest that their products do not need to be kept wet during

conditioning and sample processing. However, little data have been shown525.3

- 42 

### to demonstrate performance under those conditions for the wide variety of

environmental contaminants using th ese media. Therefore, in the interest of

providing a single procedure for the sorbents and analytes in this method,

the authors chose to use procedure s similar to th ose 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

ex traction, 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 s ample 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 d ry b y 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 elu ent (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 , an d 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. 1 1.8 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 sample525.3

- 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 th e 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 cartrid ge 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 cartridge s 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. S oak for one min . Then d raw most of the MeOH

through, leaving a thin layer of MeOH on the surface of the

cartridge. Do NOT let the cartridge go dry f rom 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, leav ing a thin layer on the

surface of the cartridge. Do NOT l et 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 f ast drop- wise fashion

. A flow525.3

- 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

bottle s . Dry the cartridge s under full vacuum for 10 min.

11.4.4. CARTRIDGE ELUTION

- Remove cartridge adaptor s and insert 40- mL

glass vial s into the manifold to collect the eluent. Replace the cartridge

adaptors , cartridge s 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. 1 1.8 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 simple st, 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

- In sert a J.T. Baker Speedisk disk ( DVB H 2 

### O

Phobic, 55 mm ) onto a J.T. Baker Speedisk manifold apparatus. Wash the525.3

- 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

MeO H 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 wa ter 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 glas s 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 an d 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 ox idize 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 mo st

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 pass525.3

- 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 b ase) 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 set tle 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 filtr ation 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 EtO Ac: DCM . Draw the solvent through the disk and into th e

collect ion vial. Proceed to Sects. 1 1.8 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 auto matic sample

preparation device. Th e 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 so rbent 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 elutio n “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 

### St ep # 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 L RW 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

* Step s 6 and 7 of this proce dure w ere added subsequent to the collection of the data

shown in Tables 1 3 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. 1 1.8 and 11.9 to dry and concentrate the extract.

11.8. DRYING THE EXTRACT

- Transfer the combined elu ent 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 th e 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. 1 1.8 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 mo re volatile compounds will exhibit

diminished recovery. Transfer the extract to a 1 -mL volumetric flask and add the

internal standard s (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 to525.3

- 49 

### determine volume, reweigh the empty sample bottle. Su btract the empty bottle

weight f rom 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 concent ration

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 Figure s 1a-1d.

11.11.2. Establish a valid i nitial 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 IDENTIFICATIO N - 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

stan dard and surrogate analyte to identify them in QC and Field Sample

chromat ograms. 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 calcu late 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. T he mass spectrum

used for identification of each compound may have been acquired in t he full525.3

- 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 com ponent (i.e., broadened peak with shoulder(s) or valley

between two or more maxima), appropriate analyte spec tra 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 identif y 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 sp ectrum produced by merphos is identical to th at of tribufos.

Therefore, when tribufos is identified as a sample component in this

method, it is possible that the original contaminant may have been merphos.

12.1.6. For specific instructions on identification and quantitation of the multi

component analytes chlordane and toxaphene, and for instructions on

screen in g 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 m ust 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

sh ould 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 calibr ation 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 Dri nking 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.) If525.3

- 52 

### tran s-chlordane is not the major chlordane component observed, Option 1

must be used.

12.3.2. Aroclor screen ing

- 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 analyzi ng a duplicate sample by Method 508A 23



### .

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 a ny 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 contr act 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 w ere 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 m edia (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. D ata 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 Se ct. 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. O ne 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. PR ECISION 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 s ix sorbents described

in Sects. 6.9-6.13. Precision and accuracy data were also collected at a

single fortified concentration using two challenging w ater matrices. W ater

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. P erformance is similar for most analytes on most

sorbents, especially considering that the data were obtained by different525.3

- 54 

### analyst s using different instrumentation. A notable exception is dimet hipin.

T he data generated for dimethipin using the J.T. Baker H 2 

### O 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 H 2 

### O 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 H 2 

### OPhobic 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 re agent 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 2 2 ).

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 SCA N GC/MS

- The values in Table 1 5 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 variation s between the data sets should

be expected

.

13.3.2. SIM GC/MS - The values f or 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 H 2 

### O Phobic DVB Speedisks.525.3

- 55 

### These sorbents w ere 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. R andomly 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

Fig s. 3a-3c . These data we re used to establish the 14 day aqueous holding time for

most method analytes (Sect. 8.4).

Note s:

• 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 t wo compounds listed below using the sample collection,

preservati on 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 Fig s. 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 PROBLEM S/ 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 have525.3

- 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 T able 1. Although the use of matrix

- matched standards will

improve quantitative accuracy for th ese 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 a nalyzed

.

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

- Th is 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 th is compound

during method development was influential in establishing l ower 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 HCB 29,30 

### , there was no direct evidence during method

development that this was the cause of low recovery. The performance of

this compound during method develo pment 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 13 

### C-pentachlorophenol has been used as525.3

- 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 fo r 13 

### C-pentachlorophenol must be m/z 276 (Table 1 ). Alt hough

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 a ll 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

th e SIM mode for a subset of analytes (those listed in Table 18) was demonstrated b y three independent laboratories ( two commercial laborator ies 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. Annm arie 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, C A.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 fr om the A merican 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 identi fication 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 R eporting 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 Open525.3

- 59 

### Tubular Column Gas Chromatography with Splitless or Hot On-Column Injection and Fl ame

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., M as tovska, K., Lehotay, S.J., Evaluation of analyte protectants to

improve gas chromatographic analysis of pesticides, J. Chromatog. A , 2003, 1015 ,163-184.

13. Poole, C.F., Matrix induced response enhancement in pesticide residue analysis by gas

chromatography, J. Chromatogr. A , 2007, 1158 , 241-250.

14. Thurman, E.M., Mills , M.S., Solid Phase Extraction Principles and Practice , John Wiley and

Sons, Inc. , 1998, p. 66.

15. Prudent Practices in the Laboratory : Handling and Disposal of Chemicals , National

Academies Press (1995), available at http://www.nap.edu (accessed October 5, 2011 ).

16. OSHA Safety and Health Standards, General Industry , (29CFR1910), Occupational Safety

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

17. Safety in Academic Chemistry Laboratories , American Chemical Society Publication,

Committee on Chemical Safety, 7th Edition. Available online at http://portal.acs.org/portal/

PublicWebSite/abo ut/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 Publicat ions Internet

Site (NPEIS) database.

19. USEPA Office of Ground Water and Drinking Water, Technical Support Center, Alternate

Test Procedure Coordinator, 26 W. Martin Luther King Dr., Cincinnati, OH, 45268.525.3

- 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

G as 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 Envi ronmental Assessment, Australian Pesticides and Veterinary Medicines

Authority, 2008. Available at http://www.apvma.gov.au (accessed October 5, 2011).

26. Dichlorovos, Extension Toxicology Network, 1993, Available at http://pmep.cce.cornell.edu

(accessed October 5, 2011).

27. Szelewski, M., Environmental Semivolatiles Using an Agilent Multimode Inlet for

Maximum Sensitivity - Application Note. Agilent Technologies, Inc. 2850 Centerville Rd.,

Wilmington, DE 19809-1610.

28. Toxicological Profile for Hexachlorocyclopentadiene (HCCPD), U.S. Department of Health

and Human Services, Public Health Service, Agency for Toxic Substances and Disease

Regis try (1999). Available at http://www.atsdr.cd c.gov/ToxProfiles/tp112.pdf (accessed

October 5, 2011).

29. Yamada, M., Naito, N., Takada, M., Nakai, S., Hosomi, M., Photodegradation of

Hexachlorobenzene and T heoretical P rediction of its D eg ra dation P athways Using Q uantum

C hemical C alculation

, Chemosph ere , 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 Chlorinated525.3

- 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. Det ermination

of Chlorinated Acids in Drinking Water by Liquid- Liquid Microextraction, Derivatization,

and Fast Gas Chromatography with Electron Capture Detection. 2000. Available on- line at

http://www.nemi.gov (accessed October 5, 2011).

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

USEPA, Office of Pesticide Programs, Environmental Service Center, Ft. Meade, MD.

Available on

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

(access Nove mber 10, 2011).525.3

- 62 

### 17. TABLES, FIGURES AND VALIDATION DATA

T able 1

. Retention Times (R T s), Suggested Quantitation Ions (Q I s), Suggested

Confirmation Ions, a nd 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

- d 10 (IS 1) 162 164 a

41 16.35 13 C- pentachlorophenol (IS 4) 276

-- b,c,d

47 16.73 phenanthrene

- d 10 (IS 2) 188 160* a

116 24.29 chrysene

- d 12 (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 a525.3

- 63 

### T able 1

. Retention Times (R T s), Suggested Quantitation Ions (Q I s), Suggested

Confirmation Ions, a nd 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,e525.3

- 64 

### T able 1

. Retention Times (R T s), Suggested Quantitation Ions (Q I s), Suggested

Confirmation Ions, a nd 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 e thyl 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 2 64 (b) 2 164 66, 111 a,h

80 19.72 h eptachlor 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 t rans -c hlordane 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 c is

- chlordane 2 375 373, 377 a

88 20.59 endosulfan I 2 241 195, 207 a525.3

- 65 

### T able 1

. Retention Times (R T s), Suggested Quantitation Ions (Q I s), Suggested

Confirmation Ions, a nd 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 t rans

- 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 t ribufos ( +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 a525.3

- 66 

### T able 1

. Retention Times (R T s), Suggested Quantitation Ions (Q I s), Suggested

Confirmation Ions, a nd 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 c is

- permethrin 3 183 163* a,d,e

123 26.82 t rans

- permethrin 3 183 163* a,d,e

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

125 27.54 b enzo [ k ] fluoranthene 3 252 126* a

126 28.22 b enzo [ a ] pyrene

- d 12 (SUR) 3 264 132* a

127 28.28 b enzo [ 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 d ibenzo [ a,h ] anthracene 3 278 139* a

131 31.20 b enzo [ g,h,i ] perylene 3 276 138* a

* C onfirmation ions may be at or below 30% relative abundance depending on instrument tune

.

-- C ompounds 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 i nduced 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 potenti al for matrix

i nduced 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 designa ted 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. U sers 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 resp o nse for each compound when analyzed at the same

concentration. The mass spectrum observed matched the NIST MS library for tribuf os.525.3

- 67 

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



### Mass ( m/z ) Relative Abundance Criteria Purpose of Checkpoint b



### 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 no t 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 methods 22 

### 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, co nstitute 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 Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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 10 6 3.6 10 7 5.6 10 2 3.0

aldrin 96.2 2.0 87.1 6.2 86.4 2.0

ametryn 10 5 4.6 10 2 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

b enzo [ 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

b enzo [ 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

b enzo [ k ] fluoranthene 103 5.6 10 2 4.5 92.8 3.3

BHT ND e ND e 92.8 1.3

bromacil 119 2.1 103 12 99.5 1.4

butachlor 106 4.8 10 6 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

c hlordane , cis 99.1 2.9 10 5 3.7 99.8 0.86

c hlordane , trans 91.7 1.4 99.3 3.6 105 3.8

chlorfenvinphos 10 1 6.8 10 5 3.9 108 2.6

chlorobenzilate 10 9 1.1 10 9 4.5 96.8 2.0

chloroneb 91.8 5.5 97.5 5.0 94.9 2.4

chlorothalonil 102 2.7 10 1 2.9 106 2.6

chlorpropham 119 11 10 5 5.6 92.7 2.0

chlorpyrifos 11 2 13 99.8 6.3 94.4 2.3

chrysene 95.6 8.3 107 2.3 89.8 0.39

cyanazine 10 7 9.4 11 1 6.3 95.5 1.0525.3

- 69 

### Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent

Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges ; Full

Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

cycloate 90.4 2.7 99.6 5.0 90.7 1.8

d acthal (DCPA) 91.5 7.3 103 4.4 101 1.5

DDD, 4,4 ′- 10 1 6.0 103 5.7 92.5 0.7 0

DDE, 4,4 ′- 98.1 1.2 100 5.9 95.0 2.4

DDT, 4,4 ′- 10 6 5.0 10 4 6.1 95.7 0.8 0

DEET 102 4.1 101 2.9 94.2 0.8 1

di(2

- ethylhexyl)adipate 10 6 5.2 104 3.2 94.9 3.9

di(2

- ethylhexyl)phthalate 14 4 27 112 4.6 91.3 1.8

d ibenzo [ 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 10 1 3.6 95.5 1.1

DIMP 104 5.3 96.2 1.6 90.6 2.1

d initrotoluene , 2,4

- 109 6.7 96.8 4.4 91.1 0.59

d initrotoluene , 2,6

- ND f 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 0.7 0

endosulfan sulfate 98.7 6.2 10 6 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 10 9 21 10 3 8.6 92.1 2.1

e thyl parathion 101 16 89.8 3.8 95.8 1.6525.3

- 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 Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

etridiazole 97.7 4.6 96.0 4.7 93.7 0.4 1

fenarimol 10 8 14 112 7.5 95.6 1.2

fluorene 92.6 3.2 97.1 2.2 88.5 1.8

fluridone 11 6 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 10 3 4.4 106 4.5 98.9 1.4

HCH , δ 10 4 8.3 104 6.0 98.0 2.1

HCH , γ (lindane) 96.7 3.6 10 4 5.6 98.7 4.0

heptachlor 83.5 5.0 108 9.7 92.1 1.2

h eptachlor 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

i ndeno [ 1,2,3

- c,d ] pyrene 10 1 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 10 8 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 10 4 2.6 96.3 6.7 98.9 2.6

mevinphos 10 3 8.5 95.5 5.8 90.3 2.5

MGK 2 64 (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 10 2 13 10 2 3.0 92.7 1.6

n onachlor , trans 91.4 11 104 5.4 10 2 0.55

norflurazon 103 9.2 101 8.7 92.3 1.3

oxyfluorfen 10 6 2.6 107 2.9 91.6 0.2 3525.3

- 71 

### Table 3. Precision and Accuracy Data Obtained for Method Analytes Fortified in Reagent

Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges ; Full

Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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

p ermethrin , cis 101 5.4 109 5.2 88.5 3.2

p ermethrin , 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 0.9 2

prometon 93.5 13 110 7.5 92.4 2.1

prometryn 10 9 8.7 10 4 6.7 101 3.6

pronamide 10 2 2.4 10 4 6.8 100 1.9

propachlor 102 7.6 10 3 4.4 92.9 1.2

propazine 99.6 5.1 10 7 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 10 7 4.7 107 6.7 10 7 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 10 4 7.1 98.7 3.4

terbutryn 11 1 4.6 107 5.8 100 1.4

tetrachlorvinphos 109 6.3 104 7.8 94.8 2.4

triadimefon 99.6 7.5 1 10 6.8 98.0 2.7

tribufos+merphos 11 1 2.8 105 4.2 99.1 1.3

trifluralin 94.4 1.1 10 4 5.2 90.7 0.7 2

vernolate 95.3 1.6 96.5 5.1 92.3 0.8 2

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 1.5525.3

- 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 Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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 0.7 3

2,3,3 ′ ,4 ′ ,6

- pentachlorobiphenyl (110) 98.2 6.7 98.1 4.3 94.6 0.6 0

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 10 3 4.5 97.6 0.7 4

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

b enzo [ a ] pyrene

- d 12 101 4.7 86.5 3.5 91.2 3.0

triphenyl phosphate 10 2 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 0.05 0 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 labor atory reagent blank values.

f. ND = Not determined

. Analyte could not be determined because of the low concentration.525.3

- 73 

### T able 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

acenaphthylene 2.0 90.5 1.7 99.3 2.5

acetochlor 2.0 102 3.8 12 8 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 10 6 3.6

b enzo [ a ] anthracene 2.0 99.1 4.0 10 4 3.7

benzo [ a ] pyrene 2.0 91.1 4.2 99.9 1.2

b enzo [ 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

b enzo [ k ] fluoranthene 2.0 97.2 2.7 96.7 4.6

BHT 2.0 ND e ND d

bromacil 2.0 89.4 2.3 108 2.9

butachlor 2.0 102 4.0 11 7 4.8

butylate 2.0 10 1 1.9 114 2.6

butylbenzylphthalate 2.0 1 10 4.7 99.8 4.0

c hlordane , cis

- 2.0 96.9 3.9 11 2 2.4

c hlordane , trans 2.0 92.0 4.0 106 3.3

chlorfenvinphos 2.0 10 4 3.3 102 3.6

chlorobenzilate 2.0 10 5 4.1 11 6 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 10 4 3.1

cyanazine 2.0 10 3 2.7 10 2 1.8

cycloate 2.0 92.9 2.2 10 5 2.0525.3

- 74 

### T able 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

d acthal (DCPA) 2.0 98.7 2.8 10 8 2.7

DDD, 4,4 ′- 2.0 95.2 2.8 105 2.9

DDE, 4,4 ′- 2.0 93.7 3.5 10 4 2.7

DDT, 4,4 ′- 2.0 102 4.5 11 7 2.2

DEET 2.0 10 3 1.7 103 2.4

di(2

- ethylhexyl)adipate 2.0 10 1 2.9 106 3.8

di(2

- ethylhexyl)phthalate 2.0 101 3.7 99.8 6.3

d ibenzo [ a,h ] anthracene 2.0 85.6 5.8 102 2.4

dibutyl phthalate 2.0 11 4 4.5 109 8.5

dichlorvos 2.0 94.3 1.6 118 2.2

dieldrin 2.0 96.0 3.0 10 1 3.8

diethylphthalate 2.0 90.5 1.2 10 2 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

d initrotoluene , 2,4

- 2.0 100 0.4 0 11 5 2.9

d initrotoluene , 2,6

- 2.0 103 2.6 12 4 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 10 6 2.8 10 8 4.0

endosulfan sulfate 2.0 94.3 9.1 10 2 2.9

endrin 2.0 107 5.2 118 2.0

EPTC 2.0 96.1 1.2 1 10 2.6

ethion 2.0 104 3.7 105 2.4

ethoprop 2.0 97.9 2.4 12 2 2.3

e thyl parathion 2.0 87.1 4.0 93.8 10

etridiazole 2.0 98.8 2.0 12 1 4.1

fenarimol 2.0 101 3.0 11 2 4.1525.3

- 75 

### T able 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

h eptachlor 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

i ndeno [ 1,2,3

- c,d ] pyrene 2.0 96.0 4.8 111 1.1

isophorone 2.0 92.4 1.2 10 6 3.2

methoxychlor 2.0 102 1.8 120 4.4

methyl parathion 2.0 10 2 3.3 10 8 4.2

metolachlor 2.0 10 2 1.6 11 4 2.7

metribuzin 2.0 89.4 5.9 92.1 6.2

mevinphos 2.0 94.9 3.2 11 6 2.9

MGK 2 64 (a) 1.6 98.1 3 .0 1 10 2.7

MGK 264(b) 0.4 97.8 4 .0 1 10 3.6

molinate 2.0 91.3 3.5 10 7 4.7

napropamide 2.0 103 1.3 112 3.3

nitrofen 2.0 96.8 3.5 10 2 3.4

nonachlor , trans 2.0 96.7 4.2 10 7 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 10 9 1.9

pentachlorophenol 8 .0 81.9 13 96.3 7.3

p ermethrin

, trans 1.1 95.8 3.0 107 2.9525.3

- 76 

### T able 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 10 8 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 10 1 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 11 2 1.1 107 1.2

tebuthiuron 2.0 10 5 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 1 10 4.4

triadimefon 2.0 10 4 3.1 109 3.7

tribufos+merphos 2.0 10 5 2.4 110 1.9

trifluralin 2.0 10 1 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 2.8525.3

- 77 

### T able 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

2,2 ′ ,3,5 ′- tetrachlorobiphenyl (44) 2.0 93.6 3.4 10 5 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 10 2 2.0

2,3 ′ ,4,4 ′ ,5

- pentachlorobiphenyl (118) 2.0 91.2 3.7 10 2 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 10 6 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 10 7 2.5

Surrogate Analytes

1,3

- dimethyl -2- nitrobenzene (SUR) 5 .0 92.3 1.7 97.9 2.8

b enzo [ a ] pyrene

- d 12 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 g round w ater source with high mineral content. Tap water h ardness was 290 mg/L as calcium

carbonate.

c. Tap water from a s urface w ater 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 H 2 

### O Phobic DVB

SPE Columns ( Cartridges ); Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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 10 1 3.3 97.9 2.5

atrazine 100 6.7 99.3 1.0 100 3.4

b enzo [ 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

b enzo [ 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

b enzo [ 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

c hlordane , cis 97.2 5.2 97.9 2.6 103 2.2

c hlordane , trans 93.7 5.3 10 6 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 3.7525.3

- 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 H 2 

### O Phobic DVB

SPE Columns ( Cartridges ); Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

cycloate 86.1 3.4 93.8 1.7 94.6 1.9

d acthal (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 ND e 106 9.1 92.5 3.0

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

dibutylphthalate 94.7 32 10 5 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

d initrotoluene , 2,4

- ND 97.9 4.1 92.1 1.3

d initrotoluene , 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 10 1 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

e thyl parathion 79.2 14 99.9 2.4 96.1 3.0525.3

- 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 H 2 

### O Phobic DVB

SPE Columns ( Cartridges ); Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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 10 1 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

h eptachlor 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

i ndeno [ 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 10 2 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 2 64 (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

n onachlor , 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 2.2525.3

- 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 H 2 

### O Phobic DVB

SPE Columns ( Cartridges ); Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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

p ermethrin , cis 91.6 4.4 99.3 3.2 91.2 2.8

p ermethrin , 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 0.78525.3

- 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 H 2 

### O Phobic DVB

SPE Columns ( Cartridges ); Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n= 8 Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] pyrene

- d 12 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 Forti fied into

Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE C olumns (C artridges ); N=4 for Each Matrix;

Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

acenaphthylene 2.0 84.8 1.5 91.5 2.0

acetochlor 2.0 10 6 2.2 103 2.7

alachlor 2.0 10 8 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

b enzo [ a ] anthracene 2.0 101 2.6 96.4 2.3

benzo [ a ] pyrene 2.0 105 4.8 97.5 6.0

b enzo [ b ] fluoranthene 2.0 10 1 3.1 100 2.1

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

b enzo [ k ] fluoranthene 2.0 10 6 3.5 102 1.7

BHT 2.0 96.4 1.6 109 2.0

bromacil 2.0 10 4 2.2 123 16

butachlor 2.0 10 3 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 10 6 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 10 4 6.4 99.9 4.4

chrysene 2.0 10 5 3.2 101 2.8

cyanazine 2.0 108 1.2 98.0 3.0525.3

- 84 

### Table 6

. Precision and Accuracy Data Obtained for Method Analytes Forti fied into

Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE C olumns (C artridges ); N=4 for Each Matrix;

Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 10 9 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 10 6 1.7 126 29

d ibenzo [ a,h ] anthracene 2.0 116 3.8 102 7.2

dibutyl phthalate 2.0 12 2 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 10 1 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 10 6 3.3 106 4.1

ethoprop 2.0 97.2 0.57 93.2 4.3

e thyl parathion 2.0 87.4 4.1 88.0 4.8

etridiazole 2.0 100 3.4 103 2.4525.3

- 85 

### Table 6

. Precision and Accuracy Data Obtained for Method Analytes Forti fied into

Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE C olumns (C artridges ); N=4 for Each Matrix;

Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 10 5 2.4 105 5.2

HCH, α 2.0 97.9 0.9 2 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 11 1 3.3 105 1.4

h eptachlor 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 1 10 6.7 100 2.8

i ndeno [ 1,2,3

- c,d ] pyrene 2.0 11 5 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 10 1 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 2 64 (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 10 5 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 10 9 3.0 110 4.1

pebulate 2.0 94.5 4.0 92.4 2.7525.3

- 86 

### Table 6

. Precision and Accuracy Data Obtained for Method Analytes Forti fied into

Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE C olumns (C artridges ); N=4 for Each Matrix;

Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 10 5 2.5 99.8 1.6

propachlor 2.0 100 1.8 97.6 1.4

propazine 2.0 10 2 2.2 93.3 3.1

pyrene 2.0 105 5.6 102 4.0

simazine 2.0 75.4 0.8 2 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 10 1 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 10 8 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 2.3525.3

- 87 

### Table 6

. Precision and Accuracy Data Obtained for Method Analytes Forti fied into

Finished Drinking Water from Ground and Surface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE C olumns (C artridges ); N=4 for Each Matrix;

Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] pyrene

- d 12 5.0 94.0 4.2 90.5 2.6

triphenyl phosphate 5.0 10 4 4.0 107 1.9

a. Data obtained on the instrumentation described in Sect. 13.1.1.1.

b. Tap water from a g round w ater source with high mineral content. Tap water h ardness was 342 mg/L as calcium

carbonate.

c. Tap water from a s urface w ater 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 H 2 

### O Phobic DVB

SPE ; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n=8 Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] anthracene 85.6 0.4 3 94.0 4.9 90.1 0.88

benzo [ a ] pyrene 94.5 11 81.3 5.9 94.6 3.5

b enzo [ 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

b enzo [ k ] fluoranthene 10 3 7.4 90.1 4.7 94.1 2.8

BHT 50.4 11 107 2.6 85.4 1.8

bromacil 10 2 8.2 99.6 28 106 1.8

butachlor 103 2.1 95.5 2.7 10 5 2.0

butylate 91.5 2.6 87.6 3.6 95.8 1.4

butylbenzylphthalate 91.3 5.8 121 5.7 10 8 1.5

c hlordane , cis 106 5.2 94.9 4.9 10 5 4.3

c hlordane , trans 10 1 5.3 89.6 5.2 104 4.4

chlorfenvinphos 10 6 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 10 3 2.5

chlorpropham 77.3 12 88.7 11 10 2 1.4

chlorpyrifos 101 13 98.7 4.2 110 3.0

chrysene 96.5 7.9 95.4 5.2 94.2 0.7 3

cyanazine 10 1 6.4 91.8 6.7 106 2.5525.3

- 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 H 2 

### O Phobic DVB

SPE ; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n=8 Fortified Conc.

5.0 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

cycloate 94.0 3.4 89.1 2.4 98.8 1.7

d acthal (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 10 6 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 0.6 4

di(2

- ethylhexyl)adipate 96.1 7.8 10 5 8.3 97.6 0.9 1

di(2

- ethylhexyl)phthalate ND e 104 9.3 94.4 3.7

d ibenzo [ a,h ] anthracene 10 1 14 90.9 10 10 6 3.1

dibutylphthalate 99.1 32 110 3.5 10 7 2.9

dichlorvos 109 5.0 100 9.5 102 2.3

dieldrin 10 6 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

d initrotoluene , 2,4

- 77.5 3.3 87.4 16 99.8 3.5

d initrotoluene , 2,6

- ND f 97.3 14 92.2 1.1

diphenamid 10 5 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 10 3 2.0

endrin 110 8.6 1 20 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 10 1 1.1

ethoprop 108 4.2 95.9 7.7 103 2.8

e thyl parathion 90.6 14 90.0 9.6 104 2.3525.3

- 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 H 2 

### O Phobic DVB

SPE ; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n=8 Fortified Conc.

5.0 μg/L d

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 10 3 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 10 1 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 11 2 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

h eptachlor epoxide 98.9 3.2 98.0 5.2 10 4 2.6

hexachlorobenzene 79.4 5.9 76.4 5.6 95.7 0.5 2

hexazinone 10 7 9.7 89.1 4.2 10 3 1.3

i ndeno [ 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 0.5 2

methoxychlor 97.4 6.5 98.7 9.8 96.3 0.8 0

methyl parathion 10 3 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 1 10 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 10 7 1.6

nitrofen 10 3 9.1 97.4 8.3 99.4 3.5

n onachlor , trans 90.1 3.7 86.0 4.5 10 3 1.5

norflurazon 102 10 96.1 14 1 10 0.76

oxyfluorfen 98.3 8.3 93.2 4.6 101 1.2525.3

- 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 H 2 

### O Phobic DVB

SPE ; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n=8 Fortified Conc.

5.0 μg/L d

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

p ermethrin , cis 89.5 4.4 96.3 7.0 93.8 1.5

p ermethrin , 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 10 5 4.3 10 8 1.9

profenofos 11 6 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 10 3 1.0

propazine 95.0 4.1 88.5 3.9 10 2 2.6

pyrene 99.2 2.7 98.0 2.3 103 0.9 1

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 0.9 1

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 10 5 2.9

tetrachlorvinphos 10 8 5.6 97.5 4.0 1 10 3.8

triadimefon 1 10 11 94.4 4.9 103 3.4

tribufos+merphos 12 6 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 10 2 1.4

PCB congeners (by IUPAC#)

2- chlorobiphenyl (1) 90.2 4.6 78.9 4.7 91.0 2.2525.3

- 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 H 2 

### O Phobic DVB

SPE ; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b

n=4 Fortified Conc.

2.0 μg/L c

n=8 Fortified Conc.

5.0 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

4- chlorobiphenyl (3) 87.9 6.5 80.5 5.8 92.7 0.8 2

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 10 3 2.1

2,2 ′ ,3,5 ′- tetrachlorobiphenyl (44) 97.5 4.2 89.5 3.9 10 8 2.4

2,2 ′ ,5,5 ′- tetrachlorobiphenyl (52) 89.0 3.6 95.0 3.1 10 3 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 10 5 1.6

2,2 ′ ,3,4,4 ′ ,5 ′- hexachlorobiphenyl (138) 93.7 0.8 90.9 3.3 10 5 3.4

2,2 ′ ,3,4 ′ ,5 ′ ,6

- hexachlorobiphenyl (149) 96.4 4.2 92.4 2.0 10 3 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

b enzo [ a ] pyrene

- d 12 10 1 3.7 82.1 3.1 91.9 2.2

triphenyl phosphate 103 2.2 1 10 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, pentachloropheno l

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 relativ e 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 Su rface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE ; N=4 for Each Matrix; Full Scan GC/MS

Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 11 4 4.3 83.0 6.4

atrazine 2.0 119 5.9 93.0 4.8

b enzo [ a ] anthracene 2.0 93.6 2.6 95.2 2.1

benzo [ a ] pyrene 2.0 80.2 4.5 85.6 11

b enzo [ 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

b enzo [ 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 11 4 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 11 8 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 10 2 4.8 82.8 5.0

chlorpropham 2.0 100 5.5 99.3 1.1

chlorpyrifos 2.0 12 3 2.5 88.4 3.3

chrysene 2.0 95.0 6.3 93.9 2.9

cyanazine 2.0 12 1 4.4 84.4 6.2525.3

- 94 

### Table 8

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Water from Ground and Su rface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE ; N=4 for Each Matrix; Full Scan GC/MS

Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

cycloate 2.0 105 3.2 91.9 1.9

dacthal (DCPA) 2.0 11 6 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 11 2 3.5 87.5 6.0

DEET 2.0 106 1.9 95.4 1.2

di(2

- ethylhexyl)adipate 2.0 11 2 6.4 102 1.9

di(2

- ethylhexyl)phthalate 2.0 113 7.4 108 5.2

d ibenzo [ a,h ] anthracene 2.0 90.4 3.8 90.0 5.3

dibutyl phthalate 2.0 13 2 4.2 102 5.1

dichlorvos 2.0 116 4.2 112 2.7

dieldrin 2.0 12 6 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 11 1 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 12 1 5.1 95.5 5.3

disulfoton 2.0 91.9 4.8 84.9 1.8

endosulfan I 2.0 12 1 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

e thyl parathion 2.0 95.4 5.7 99.8 1.1525.3

- 95 

### Table 8

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Water from Ground and Su rface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE ; N=4 for Each Matrix; Full Scan GC/MS

Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 11 6 5.1 84.5 7.2

h eptachlor epoxide 2.0 12 1 3.4 93.0 2.8

hexachlorobenzene 2.0 94.8 4.0 78.1 2.8

hexazinone 2.0 10 4 4.1 79.3 5.6

i ndeno [ 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 10 9 3.2 102 3.8

methyl parathion 2.0 10 7 4.7 100 5.0

metolachlor 2.0 1 20 3.0 94.9 4.2

metribuzin 2.0 10 1 5.0 80.6 2.7

mevinphos 2.0 94.3 2.6 94.2 2.6

MGK 246(a) 1.6 11 6 5.6 94.7 5.5

MGK 264(b) 0.4 11 4 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 12 1 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 11 4 1.9 101 5.6525.3

- 96 

### Table 8

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Water from Ground and Su rface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE ; N=4 for Each Matrix; Full Scan GC/MS

Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

pebulate 2.0 98.0 4.6 84.4 1.7

pentachlorophenol 8.0 11 8 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 12 6 5.2 97.6 3.9

profenofos 2.0 120 4.8 97.7 8.0

prometon 2.0 11 7 4.6 82.6 3.5

prometryn 2.0 11 8 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 11 3 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 11 6 4.0 88.3 6.5

tebuconazole 10.0 10 5 2.6 97.8 4.2

tebuthiuron 2.0 101 4.3 81.9 3.7

terbacil 2.0 1 20 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 12 1 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 11 7 4.6 96.1 5.1

PCB congeners (by IUPAC#)

2- chlorobiphenyl (1) 2.0 94.2 2.8 81.3 2.0525.3

- 97 

### Table 8

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Water from Ground and Su rface Water Sources, and Extracted Using

J.T. Baker Speedisk H 2 

### O Phobic DVB SPE ; N=4 for Each Matrix; Full Scan GC/MS

Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 12 1 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 11 3 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 11 6 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

b enzo [ a ] pyrene

- d 12 5.0 79.8 3.4 86.0 2.8

triphenyl phosphate 5.0 11 5 3.7 115 2.3

a. Data obtained on the instrumentation described in Sect. 13.1.1.1.

b. Tap water from a g round w ater source with high mineral content. Tap water hardness was 342 mg/L as calcium

carbonate.

c. Tap water from a s urface w ater 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 D isks; N=4 for Each

Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.20 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ 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

b enzo [ 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

b enzo [ 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

c hlordane , cis 96.3 5.0 90.7 2.9 88.8 7.9

c hlordane , 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 7.1525.3

- 99 

### Table 9

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

Water at Three Concentrations and Extracted Using Empore SDB

- XC D isks; N=4 for Each

Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.20 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

d acthal (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

d ibenzo [ 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

d initrotoluene , 2,4

- 116 5.4 90.5 2.2 90.4 6.7

d initrotoluene , 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

e thyl 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 7.3525.3

- 100 

### Table 9

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

Water at Three Concentrations and Extracted Using Empore SDB

- XC D isks; N=4 for Each

Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.20 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

h eptachlor 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

i ndeno [ 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 2 64 (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

n onachlor , 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

p ermethrin , cis 112 6.3 92.2 3.4 99.7 7.5525.3

- 101 

### Table 9

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

Water at Three Concentrations and Extracted Using Empore SDB

- XC D isks; N=4 for Each

Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.20 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

p ermethrin , 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 6.7525.3

- 102 

### Table 9

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

Water at Three Concentrations and Extracted Using Empore SDB

- XC D isks; N=4 for Each

Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.20 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] pyrene

- d 12 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 0.1 2 μg/L, and t

- permethrin is 0.2 9 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 1 0

. 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 D isks; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] anthracene 2.0 105 2.4 99.8 8.4

benzo [ a ] pyrene 2.0 95.1 3.4 91.5 9.8

b enzo [ 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

b enzo [ 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 7.1525.3

- 104 

### Table 1 0

. 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 D isks; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

d ibenzo [ 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 9.4525.3

- 105 

### Table 1 0

. 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 D isks; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

h eptachlor 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

i ndeno [ 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 2 64 (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 8.8525.3

- 106 

### Table 1 0

. 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 D isks; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 7.3525.3

- 107 

### Table 1 0

. 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 D isks; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] pyrene

- d 12 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 g round w ater source with high mineral content. Tap water h ardness 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 1 1

. Precision and Accuracy Data Obtained for Method Analy tes Fortified in Reagent

Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4

for Each Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] anthracene 112 5.1 99.1 3.8 112 3.6

benzo [ a ] pyrene 109 5.5 103 1.7 111 1.2

b enzo [ 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

b enzo [ k ] fluoranthene 105 1.9 103 2.4 113 3.1

BHT ND e 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

c hlordane , cis 98.0 5.3 102 2.5 101 1.3

c hlordane , 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 1.2525.3

- 109 

### Table 1 1

. Precision and Accuracy Data Obtained for Method Analy tes Fortified in Reagent

Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4

for Each Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

d acthal (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

d ibenzo [ 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

d initrotoluene , 2,4

- 126 1.8 105 2.6 113 2.5

d initrotoluene , 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

e thyl 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 3.4525.3

- 110 

### Table 1 1

. Precision and Accuracy Data Obtained for Method Analy tes Fortified in Reagent

Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4

for Each Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

h eptachlor 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

i ndeno [ 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

n onachlor , 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

p ermethrin , cis 110 3.6 107 1.3 107 2.2525.3

- 111 

### Table 1 1

. Precision and Accuracy Data Obtained for Method Analy tes Fortified in Reagent

Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4

for Each Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

p ermethrin , 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 0.48525.3

- 112 

### Table 1 1

. Precision and Accuracy Data Obtained for Method Analy tes Fortified in Reagent

Water at Three Concentrations and Extracted Using UCT 525 Universal Cartridges; N=4

for Each Concentration; Full Scan GC/MS Analyses a

Analytes Fortified Conc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] pyrene

- d 12 112 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 0.1 3 μg/L, t

- permethrin is 0.3 8 μg/L , MGK 264 (a) is 0.08 5 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 a re 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 1 2

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] anthracene 2.0 104 1.5 102 2.4

benzo [ a ] pyrene 2.0 106 3.2 100 2.7

b enzo [ b ] fluoranthene 2.0 104 3.3 100 3.9

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

b enzo [ 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 1.6525.3

- 114 

### Table 1 2

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

d ibenzo [ 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 3.3525.3

- 115 

### Table 1 2

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

h eptachlor 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

i ndeno [ 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 2 64 (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 4.3525.3

- 116 

### Table 1 2

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 4.9525.3

- 117 

### Table 1 2

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

UCT 525 Universal Cartridges; N=4 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] pyrene

- d 12 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 3 00 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 1 3

. 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 Analyses a

Analytes Fortified C onc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ 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

b enzo [ 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

b enzo [ 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

c hlordane , cis 92.1 6.5 89.2 4.9 89.7 2.5

c hlordane , 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 0.32525.3

- 119 

### Table 1 3

. 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 Analyses a

Analytes Fortified C onc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

d acthal (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 ND e 77.0 2.7 72.7 2.8

d ibenzo [ 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

d initrotoluene , 2,4

- 88.6 5.8 92.1 1.4 97.0 1.3

d initrotoluene , 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

e thyl 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 3.4525.3

- 120 

### Table 1 3

. 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 Analyses a

Analytes Fortified C onc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

h eptachlor 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

i ndeno [ 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

n onachlor , 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

p ermethrin , cis 87.7 2.0 79.8 1.3 80.9 3.5525.3

- 121 

### Table 1 3

. 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 Analyses a

Analytes Fortified C onc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

Mean %

Recovery RSD Mean %

Recovery RSD Mean %

Recovery RSD

p ermethrin , 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 0.41525.3

- 122 

### Table 1 3

. 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 Analyses a

Analytes Fortified C onc.

0.25 μg/L b Fortified Conc.

2.0 μg/L c Fortified Conc.

5.0 μg/L d

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

b enzo [ a ] pyrene

- d 12 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. 05 0 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 1 4

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Synthetic Hard Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ 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

b enzo [ 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

b enzo [ 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 2.0525.3

- 124 

### Table 1 4

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Synthetic Hard Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

d ibenzo [ 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 1.8525.3

- 125 

### Table 1 4

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Synthetic Hard Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

h eptachlor 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

i ndeno [ 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 2 64 (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 2.1525.3

- 1 26 

### Table 1 4

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Synthetic Hard Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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 3.4525.3

- 127 

### Table 1 4

. Precision and Accuracy Data Obtained for Method Analytes Fortified into

Finished Drinking Waters from Ground and Surface Water Sources, and Extracted Using

Horizon Atlantic DVB Disks; N=5 for Each Matrix; Full Scan GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Synthetic Hard Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d 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

b enzo [ a ] pyrene

- d 12 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, R eference 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 1 5

. 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 SPE a ,b Laboratory 2

Empore PSDVB SPE c

DL Fortified

conc. of

DL

replicate s LCMRL DL Fortified

conc. of

DL

replicates LCMRL

acenaphthylene 0.015 0.050 NC d 0.0029 0.0 25 0.0 28

acetochlor 0.037 0.050 0.19 0.0 11 0.025 0.0 54

alachlor 0.035 0.10 0.25 0.00 84 0.025 0.0 97

aldrin 0.056 0.10 0.30 0.0 10 0.025 0.420

ametryn 0.038 0.050 0.17 0.0 17 0.025 0.12

anthracene 0.018 0.050 0.12 0.0078 0.025 0.0 59

atraton 0.016 0.10 0.12 0.00 55 0.025 0.12

atrazine 0.030 0.050 0.29 0.0 10 0.025 0.0 86

b enzo [ a ] anthracene 0.021 0.050 0.12 0.00 62 0.025 0.0 43

benzo [ a ] pyrene 0.043 0.050 0.18 0.0 35 0.025 0.11

b enzo [ b ] fluoranthene 0.031 0.050 0.14 0.0 13 0.0 50 0.11

benzo [ g,h,i ] perylene 0.021 0.10 0.31 0.0 11 0.025 0.0 47

b enzo [ k ] fluoranthene 0.048 0.050 0.18 0.0 26 0.025 0.190

BHT 0.092 0.10 0.32 0.00 64 0.025 0.50

bromacil ND e 0.31 0.0 37 0.0 50 0.10

butachlor 0.028 0.050 0.39 0.00 43 0.025 0.0 89

butylate 0.024 0.050 0.16 0.00 53 0.025 0.0 89

butylbenzylphthalate 0.068 0.10 0.40 0.0 16 0.025 0.20

c hlordane , cis 0.10 0.10 0.33 0.00 94 0.0 25 0.0 68

c hlordane , trans 0.027 0.050 0.28 0.0 10 0.025 0.0 43

chlorfenvinphos 0.095 0.10 0.52 0.00 62 0.025 0.0 98

chlorobenzilate 0.034 0.050 0.30 0.00 42 0.025 0.0 91

chloroneb 0.068 0.10 0.16 0.19 0.025 0.90

chlorothalonil 0.036 0.10 0.17 0.00 74 0.025 0.11

chlorpropham 0.026 0.050 0.21 0.0 13 0.025 0.14

chlorpyrifos 0.091 0.10 0.45 0.0 26 0.025 0.0 76

chrysene 0.017 0.050 0.15 0.0 10 0.0 50 0.0 35

cyanazine 0.032 0.050 0.33 0. 19 0.0 50 0.15525.3

- 129 

### Table 1 5

. 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 SPE a ,b Laboratory 2

Empore PSDVB SPE c

DL Fortified

conc. of

DL

replicate s LCMRL DL Fortified

conc. of

DL

replicates LCMRL

cycloate 0.039 0.050 0.27 0.0 18 0.025 0.14

d acthal (DCPA) 0.018 0.050 0.44 0.0055 0.025 0.0 40

DDD, 4,4 ′- 0.019 0.050 0.35 0.00 31 0.025 0.0 92

DDE, 4,4 ′- 0.033 0.050 0.32 0.00 23 0.025 0.0 88

DDT, 4,4 ′- 0.036 0.050 0.25 0.0 22 0.025 0.12

DEET 0.019 0.050 0.14 0.00 42 0.025 0.0 66

di(2

- ethylhexyl)adipate 0.079 0.10 0.38 0.0 13 0.025 0.0 83

di(2

- ethylhexyl)phthalate ND 0.050 0.29 0.0 20 0.025 0.40

d ibenzo [ a,h ] anthracene 0.014 0.050 0.30 0.0 14 0.025 0.14

dibutyl phthalate ND 0.050 0.88 0.13 0.025 1 .4

dichlorvos 0.021 0.050 0.46 0.00 51 0.025 0.0 81

dieldrin 0.064 0.10 0.28 0.0 17 0.025 0.0 84

diethylphthalate 0.037 0.050 0.074 0.0 18 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 0.0 46

DIMP 0.039 0.050 0.19 0.0036 0.025 >5.0

d initrotoluene , 2,4

- 0.026 0.050 0.23 0.0076 0.025 0. 19

d initrotoluene , 2,6

- 0.056 0.10 0.31 0.0 53 0.0 75 0.20

diphenamid 0.033 0.050 0.29 0.0 10 0.025 0.0 89

disulfoton 0.12 0.10 0.12 0.0066 0.025 0. 11

endosulfan I 0.039 0.050 0.62 0.0 15 0.0 50 0.11

endosulfan II 0.14 0.10 0.38 0.0 24 0.050 NC

endosulfan sulfate 0.068 0.10 0.39 0.0 25 0.050 0.12

endrin 0.045 0.050 0.40 0.0 33 0.050 0.12

EPTC 0.037 0.050 0.13 0.0048 0.025 0.0 68

ethion 0.010 0.050 0.29 0.0 13 0.025 0.13

ethoprop 0.13 0.10 0.39 0.0048 0.025 0.12

e thyl parathion 0.15 0.10 0.46 0.0 13 0.0 50 0.19525.3

- 130 

### Table 1 5

. 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 SPE a ,b Laboratory 2

Empore PSDVB SPE c

DL Fortified

conc. of

DL

replicate s LCMRL DL Fortified

conc. of

DL

replicates LCMRL

etridiazole 0.024 0.050 0.24 0.0 12 0.0 25 0.17

fenarimol 0.10 0.10 0.28 0.0 41 0.0 50 0.20

fluorene 0.016 0.050 0.08 0.0058 0.0 25 0.0 51

fluridone 0.11 0.10 0.33 0.0 45 0.0 50 0.27

HCCPD 0.012 0.050 0.24 0.0066 0.0 25 0.084

HCH , α 0.036 0.050 0.31 0.0037 0.0 25 0.0 62

HCH , β 0.10 0.10 0.24 0.0 21 0.0 50 0. 11

HCH , δ 0.019 0.050 0.31 0.0 15 0.025 0.0 99

HCH , γ (lindane) 0.036 0.050 0.24 0.0 14 0.025 0.0 78

heptachlor 0.034 0.050 0.27 0.00 32 0.025 0.0 29

h eptachlor epoxide 0.039 0.10 0.11 0.00 53 0.025 0.0 63

hexachlorobenzene 0.016 0.050 0.40 0.00 94 0.025 0.0 87

hexazinone 0.025 0.050 0.26 0.0 12 0.025 0.14

i ndeno [ 1,2,3

- c,d ] pyrene 0.11 0.10 0.40 0.0 39 0.025 0.20

isophorone 0.014 0.050 0.11 0.00 43 0.025 0.0 63

methoxychlor 0.024 0.050 0.23 0.00 64 0.025 0.0 61

methyl parathion 0.036 0.050 0.28 0.0088 0.0 50 0.16

metolachlor 0.019 0.050 0.11 0.00 42 0.025 0.14

metribuzin 0.036 0.050 0.076 0.00 70 0.025 0.11

mevinphos 0.035 0.10 0.21 0.00 40 0.025 0.0 93

MGK 2 64 (a) 0.072 0.080 0.32 0.0026 0.025 0.0 31

MGK 264(b) 0.023 0.020 0.09 0.0096 0.025 0.0 83

molinate 0.062 0.10 0.29 0.0036 0.025 0.0 74

napropamide 0.077 0.10 0.44 0.0 25 0.0 50 0.11

nitrofen 0.093 0.10 0.39 0.0 42 0.0 50 0.13

n onachlor , trans 0.035 0.050 0.35 0.00 62 0.0 25 0.0 49

norflurazon 0.057 0.10 0.26 0.0 62 0.0 50 0.14

oxyfluorfen 0.037 0.050 0.34 0.0 15 0.0 50 0.28525.3

- 131 

### Table 1 5

. 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 SPE a ,b Laboratory 2

Empore PSDVB SPE c

DL Fortified

conc. of

DL

replicate s LCMRL DL Fortified

conc. of

DL

replicates LCMRL

pebulate 0.020 0.050 0.20 0.00 53 0.025 0.0 40

pentachlorophenol 0.060 0.20 0.56 0.0 69 0.025 0.16

p ermethrin , cis 0.015 0.028 0.13 0.0026 0.025 0.0 36

p ermethrin , trans 0.031 0.072 0.10 0.0 12 0.025 0. 0 87

phenanthrene 0.025 0.10 0.097 0.0069 0.025 0.51

phorate 0.032 0.050 0.20 0.0 52 0.0 50 0. 15

phosphamidon 0.040 0.10 0.23 0.0029 0.0 25 0. 11

profenofos 0.11 0.10 0.31 0.0 55 0.0 50 0. 11

prometon 0.065 0.10 0.22 0.0 10 0.025 0.12

prometryn 0.021 0.050 0.24 0.0 12 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 0.0 68

propazine 0.023 0.050 0.20 0.00 65 0.025 0.0 55

pyrene 0.013 0.050 0.17 0.00 45 0.025 0.0 62

simazine 0.023 0.050 0.12 0.0059 0.025 0.0 83

simetryn 0.037 0.050 0.28 0.0 13 0.025 0.12

tebuconazole 0.24 0.50 2.1 0.0 53 0.0 50 0. 18

tebuthiuron 0.027 0.050 0.21 0.0 60 0.0 75 0.13

terbacil 0.082 0.10 0.41 0.0 39 0.0 75 0.13

terbutryn 0.029 0.050 0.18 0.00 51 0.0 25 0.0 93

tetrachlorvinphos 0.048 0.10 0.35 0.00 42 0.0 25 0. 14

triadimefon 0.053 0.050 0.35 0.0 48 0.0 50 0.11

tribufos+merphos 0.12 0.10 0.53 0.0 13 0.0 25 0. 18

trifluralin 0.027 0.050 0.28 0.0 19 0.0 25 0.12

vernolate 0.038 0.050 0.11 0.00 51 0.0 25 0.0 80

vinclozolin 0.029 0.050 0.34 0.016 0.0 50 0.12

PCB congeners (by IUPAC#)

2- chlorobiphenyl (1) 0.021 0.050 0.14 0.00 61 0.025 0.0 54525.3

- 132 

### Table 1 5

. 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 SPE a ,b Laboratory 2

Empore PSDVB SPE c

DL Fortified

conc. of

DL

replicate s LCMRL DL Fortified

conc. of

DL

replicates LCMRL

4- chlorobiphenyl (3) 0.019 0.050 0.24 0.0059 0.025 0.0 65

2,4 ′- dichlorobiphenyl (8) 0.024 0.050 0.18 0.0037 0.025 0.0 88

2,2 ′ ,5

- trichlorobiphenyl (18) 0.024 0.050 0.086 0.0 28 0.025 0.14

2,4,4 ′- trichlorobiphenyl (28) 0.036 0.050 0.069 0.00 73 0.025 0.0 36

2,2 ′ ,3,5 ′- tetrachlorobiphenyl (44) 0.029 0.050 0.23 0.0079 0.025 0.0 41

2,2 ′ ,5,5 ′- tetrachlorobiphenyl (52) 0.043 0.10 0.092 0.00 55 0.025 0.0 78

2,3 ′ ,4 ′ ,5

- tetrachloroobiphenyl (70) 0.043 0.050 0.30 0.00 44 0.025 0.0 46

2,3,3 ′ ,4 ′ ,6

- pentachlorobiphenyl (110) 0.026 0.050 0.36 0.00 30 0.025 0.0 84

2,3 ′ ,4,4 ′ ,5

- pentachlorobiphenyl (118) 0.046 0.050 0.36 0.00 50 0.025 0.0 95

2,2 ′ ,3,4,4 ′ ,5 ′- hexachlorobiphenyl (138) 0.19 0.10 0.41 0.00 71 0.025 0.0 58

2,2 ′ ,3,4 ′ ,5 ′ ,6

- hexachlorobiphenyl (149) 0.020 0.050 0.37 0.0039 0.025 0.0 56

2,2 ′ ,4,4 ′ ,5,5 ′- hexachlorobiphenyl (153) 0.029 0.050 0.38 0.00 33 0.025 0.0 92

2,2 ′ ,3,4,4 ′ ,5,5 ′- heptachlorobiphenyl (180) 0.058 0.10 0.31 0.0066 0.025 0.0 36

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 concentra tion.525.3

- 133 

### Table 1 6 . Example SIM P arameters for Selected Method Analytes

SIM

Segment Compound RT

(min) Q I

( 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

- d 10 (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

50 0.60 2,4'

- dichlorobiphenyl 15.61 222 152, 224

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

13 C- 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

- d 10 (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 h eptachlor epoxide 19.50 353 81, 355

50 0.47

2,3',4',5

- tetrachlorobiphenyl 19.62 220 292

# 11 t rans

- chlordane 20.02 375 373, 377

50 0.60 c is

- chlordane 20.35 375 373, 377

t rans

- nonachlor 20.42 409 407, 411525.3

- 134 

### Table 1 6 . Example SIM P arameters for Selected Method Analytes

SIM

Segment Compound RT

(min) Q I

( 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 e ndrin 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

- d 12 (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

- d 12 (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 1 7 . Precision and Accuracy D ata Obtained for Selected Method Analytes Fortified in

Reagent Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges;

SIM GC/MS Analyses a

Analytes Fortified Conc.

0.025 μg/L b

n=4 Fortified Conc.

0. 1 0 μg/L c

n= 4 Fortified Conc.

0.25 μg/L d

n=4

Mean %

Recovery RSD Mean %

Recovery Mean %

Recovery Mean %

Recovery RSD

acetochlor 10 3 1.8 109 1.9 105 2.2

alachlor 11 4 2.7 11 2 1.1 104 3.1

atrazine 117 5.7 11 8 3.6 111 1.8

benzo [ a ] pyrene 81.0 4.8 10 3 2.2 97.4 7.5

c hlordane , cis 110 4.1 10 2 2.9 100 3.0

c hlordane , trans 89.9 1.4 99.4 5.3 100 2.8

di(2

- ethylhexyl)adipate ND e 11 4 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 10 5 3.7 100 1.6

ethoprop 89.4 19 109 3.2 112 1.7

HCCPD 102 7.6 10 8 1.2 100 4.3

HCH , α 112 5.6 11 4 3.3 99.6 4.5

HCH , γ (lindane) 10 4 6.9 1 10 2.0 100 6.2

heptachlor 104 9.3 99.9 3.4 89.2 2.7

h eptachlor 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 11 3 8.4 116 2.8 104 1.6

metolachlor 114 1.0 115 4.3 10 7 1.7

molinate 104 5.7 10 9 2.3 109 1.4

n onachlor , trans 98.9 2.8 96.4 5.5 99.9 3.4

oxyfluorfen 114 12 115 5.2 12 4 6.3

pentachlorophenol 79.0 7.9 96.3 6.7 97.2 2.0

p ermethrin , cis 91.5 9.7 11 3 3.2 105 2.0

p ermethrin , trans 94.6 2.5 10 4 2.0 103 1.5

profenofos 102 8.4 92.0 2.3 11 2 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 10 5 3.9

vinclozolin 93.1 4.4 110 2.0 104 2.4525.3

- 136 

### Table 1 7 . Precision and Accuracy D ata Obtained for Selected Method Analytes Fortified in

Reagent Water at Three Concentrations and Extracted Using Oasis HLB SPE Cartridges;

SIM GC/MS Analyses a

Analytes Fortified Conc.

0.025 μg/L b

n=4 Fortified Conc.

0. 1 0 μg/L c

n= 4 Fortified Conc.

0.25 μg/L d

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) 10 9 12 110 7.1 10 2 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 10 5 1.7 101 1.3

2,2 ′ ,3,5 ′- tetrachlorobiphenyl (44) 94.5 4.2 10 8 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 10 3 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

b enzo [ a ] pyrene

- d 12 87.9 3.0 92.1 2.4 94.5 8.8

triphenyl phosphate 103 1.9 10 6 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 0.1 2 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 1.0 2 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

acetochlor 0.10 109 9.6 NA e

alachlor 0.10 1 10 5.9 112 3.6

atrazine 0.10 112 11 1 01 0.45

benzo [ a ] pyrene 0.10 86.3 2.7 104 7.6

c hlordane , cis 0.10 98.1 3.4 9 7.9 3.9

c hlordane , trans 0.10 10 1 4.3 102 3 .7

di(2

- ethylhexyl)adipate 0.10 116 7.4 1 14 4.8

di(2

- ethylhexyl)phthalate 0.10 ND f ND

dimethipin 0.10 96.0 7.4 1 03 18

endrin 0.10 11 2 4.4 107 3.3

ethoprop 0.10 111 9.6 102 3.6

HCCPD 0.10 12 2 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

h eptachlor epoxide 0.10 96.5 4.5 103 1.4

hexachlorobenzene 0.10 90.4 4.9 8 3.8 3.3

methoxychlor 0.10 116 4.1 128 1.3

metolachlor 0.10 112 6.3 NA

molinate 0.10 1 20 7.2 NA

n onachlor , 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

p ermethrin , cis 0.0 6 g 10 6 5.0 10 2 5.1

p ermethrin , trans 0.1 4 h 10 1 3.6 10 8 3.0

profenofos 0.10 10 7 3.5 110 6.8

simazine 0.10 101 10 1 05 3 .0

tebuconazole 0.50 115 5.6 99.9 4.5

tribufos 0.10 10 7 5.9 110 3.5525.3

- 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 Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery d RSD

vinclozolin 0.10 10 3 8.3 10 4 4.2

PCB congeners (by IUPAC#)

2- chlorobiphenyl (1) 0.10 87.8 9.6 9 5.8 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 9 2.3 3.0

2,2 ′ ,3,4,4 ′ ,5 ′- hexachlorobiphenyl (138) 0.10 101 4.6 9 6.9 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 9 4.5 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

b enzo [ a ] pyrene

- d 12 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 wa ter 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 c oncentration in ground water is as listed in the table. The c oncentration in surface water is 0.03 0 μg/L.

h. The c oncentration in ground water is as listed in the table. The c oncentration in surface water is 0.0 70 μg/L.525.3

- 139 

### Table 19 . Precision and Accuracy D ata Obtained for Selected Method Analytes Fortified in

Reagent Water at Three Concentration s and Extracted Using J.T. Baker H 2 

### O Phobic

Speedisk s ; SIM GC/MS Analyses a

Analytes Fortified Conc.

0.02 5 μg/L b

n=4 Fortified Conc.

0. 10 μg/L c

n= 4 Fortified Conc.

0.25 μg/L d

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 ND e 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 6.6525.3

- 140 

### Table 19 . Precision and Accuracy D ata Obtained for Selected Method Analytes Fortified in

Reagent Water at Three Concentration s and Extracted Using J.T. Baker H 2 

### O Phobic

Speedisk s ; SIM GC/MS Analyses a

Analytes Fortified Conc.

0.02 5 μg/L b

n=4 Fortified Conc.

0. 10 μg/L c

n= 4 Fortified Conc.

0.25 μg/L d

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

- d 12 100 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 0.03 6 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 0.05 8 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 0.3 6 μg/L.

e. ND = Not determined. Matrix spike recover y could not be determined due to the low fortificatio n con centration

relative to the background concentration. 96.2525.3

- 141 

### T able 2 0 a

. 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 H 2 

### O Ph obic Speedisk s ; N=4 for Each Matrix; SIM GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery c RSD

acetochlor NA d

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

c hlordane , cis 0.10 91.0 4.5 98.4 1.8

c hlordane , 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 ND e ND e

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

h eptachlor 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

n onachlor , trans NA

oxyfluorfen 0.10 100 6.2 141 1.3

pentachlorophenol 0. 40 90.2 5.5 89.0 1.8

p ermethrin , cis 0.058 87.1 4.5 108 4.3

p ermethrin , 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 3.2525.3

- 142 

### T able 2 0 a

. 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 H 2 

### O Ph obic Speedisk s ; N=4 for Each Matrix; SIM GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d 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

b enzo [ a ] pyrene

- d 12 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 wa ter 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 

### T able 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 H 2 

### O Phobic Speedisk s ; N=4 for Each Matrix; SIM GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d RSD Mean %

Recovery c RSD

acetochlor NA d

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

c hlordane , cis 0.50 92.5 1.1 94.6 2.8

c hlordane , 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 ND e ND e

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

h eptachlor 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

n onachlor , trans NA

oxyfluorfen 0. 50 93.0 0.83 107 2.7

pentachlorophenol 2.0 92.3 1.3 89.7 2.8

p ermethrin , cis 0.15 81.1 1.4 86.1 4.4

p ermethrin , 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 2.5525.3

- 144 

### T able 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 H 2 

### O Phobic Speedisk s ; N=4 for Each Matrix; SIM GC/MS Analyses a

Analytes Fortified

Conc. (μg/L) Ground Water b Surface Water c

Mean %

Recovery d 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 0.6 5 108 0.93

b enzo [ a ] pyrene

- d 12 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 wa ter 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

- HLB a 82.9 5.0 101 3.3 89.5 8.8

J.T

. Baker H 2 O Phobic

cartridge a 100 3.63 104 3.8 98.5 1.7

J.T

. Baker H 2 O Phobic

Speedisk b 114 1.0 103 3.4 98.5 2.8

Empore SDB

- XC a 107 5.3 111 2.1 101 0.15

UCT 525 Universal

Cartridge a NA c 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 Univers a l 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 μ g/L, n=4 Surface Water b

Fortified Conc.

10 μg/L

, n=4

Mean % R ecovery RSD Mean % Recovery RSD

Oasis

- HLB c 95.4 3.7 94.2 5.9

J.T

. Baker H 2 O Phobic

cartridge c 102 5.6 103 3.5

J.T

. Baker H 2 O Phobic

Speedisk d 120 2.4 124 1.9

Empore SDB

- XC c 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 Calcul ated 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 H 2 

### O Phobic Speedisk s,

All Samples Analyzed in SIM Mo de , All concentrations in μg/L

Analytes Oasis HLB a Baker Speedisk b

DL c 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

c hlordane , cis 0.0016 0.010 0.0073 0.0039

c hlordane , trans 0.0028 0.010 0.0097 0.0020

di(2

- ethylhexyl)adipate ND d 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

h eptachlor 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

n onachlor , trans 0.0029 0.010 0.0061 0.0066

oxyfluorfen 0.0038 0.010 0.035 0.031

pentachlorophenol 0.04 7 0. 100 0.068 0.0086

p ermethrin , cis 0.0041 0.006 0.012 0.0015

p ermethrin , trans 0.0080 0.014 0.020 0.0023

profenofos 0.0081 0.010 0.029 0.012

simazine 0.010 0.0 25 0.048 0.018

tebuconazole 0.0 42 0.12 0.20 0.037525.3

- 147 

### Table 23. DLs and LCMRLs Calcul ated 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 H 2 

### O Phobic Speedisk s,

All Samples Analyzed in SIM Mo de , All concentrations in μg/L

Analytes Oasis HLB a Baker Speedisk b

DL c Fortified conc. of

DL replicates LCMRL LCMRL

toxaphene 0.32 1.0 1.4 NF e

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 0.0 25 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 fortifi ed.525.3

- 148 

### Table 24. Initial Demonstration of Capability (IDC) and Quality Control (QC) Requirements (S ummary )

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 analyte s are ≤ 1/3 the

MRL , and that possible interferences from

extraction media do not prevent the ide ntification

and/or quantification of any analyte s, SURs or ISs

. Note: This includes the absence of interferences at

both the Q Is 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 ± 3 0% 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 LFB s at the

proposed MRL concentration. Calculate the mean

, standard deviation and HR PIR 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. ± 3 0% 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 informati on 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 Q uality Control (QC) R equirements (S ummary )

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 E xtract 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

S amples

. Demonstrate that the method analyte concentration

is ≤ 1 / 3 the MRL, and confirm that possible

interferences do not prevent quantification

. If the

background concentration exceed s 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 F ield S amples. Rotate the fortified concentrations

between low, medium, and high amounts. Res ults 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 In ternal 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 the ir 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 IS s do not meet th ese criteri a , target analyte

results are invalid. Consult Sect. 9.3.5 for further

information.

Sect

. 9.3.6 Surrogate (SUR)

Standards The SUR standard s 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

a ny 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 analyte s 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 Q uality Control (QC) R equirements (S ummary ) (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 . A n

LFSMD may be substituted for a FD when the

frequency of detects fo r analytes of interest are low.

Calculate RPDs. Method analyte RPDs for the LF S MD 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

effec t.

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

.

Sect s

. 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 c riteria are given in Table 2

.

S ect. 10.3 Continuing Calibration

Check (CCC) Verify initial calibration by analyzing a calibration

standard at the beginning of each a nalysis b atch prior to

analyzing samples, after every 10 Field S amples, 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 calibrat ion 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 Sect s. 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 number s 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 thos e 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 4 b. Results of Extract Holding Time Study (Sect. 13.5)525.3

- 161 

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