ASTM D5175-91(2017)e1
(Test Method)Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography
Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography
SIGNIFICANCE AND USE
5.1 The extensive and widespread use of organochlorine pesticides and PCBs has resulted in their presence in all parts of the environment. These compounds are persistent and may have adverse effects on the environment. Thus, there is a need to identify and quantitate these compounds in water samples.
SCOPE
1.1 This test method (1-3)2 is applicable to the determination of the following analytes in finished drinking water, drinking water during intermediate stages of treatment, and the raw source water:
Analyte
Chemical Abstract Service
Registry Number A
Alachlor
5972-60-8
Aldrin
309-00-2
Chlordane
57-74-9
Dieldrin
60-57-1
Endrin
72-20-8
Heptachlor
76-44-8
Heptachlor Epoxide
1024-57-3
Hexachlorobenzene
118-74-1
Lindane
58-89-9
Methoxychlor
72-43-5
Toxaphene
8001-35-2
Aroclor B 1016
12674-11-2
Aroclor B 1221
11104-28-2
Aroclor B 1232
11141-16-5
Aroclor B 1242
53469-21-9
Aroclor B 1248
12672-29-6
Aroclor B 1254
11097-69-1
Aroclor B 1260
11096-82-5
(A) Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH 43210-0334.(B) Aroclor is a registered trademark of Monsanto Co.
1.2 Detection limits for most test method analytes are less than 1 μg/L. Actual detection limits are highly dependent on the characteristics of the sample matrix and the gas chromatography system. Table 1 contains the applicable concentration range for the precision and bias statements. Only Aroclor 1016 and 1254 were included in the interlaboratory test used to derive the precision and bias statements. Data for other PCB products are likely to be similar. (A) Bias = C − X.(B) X = Mean recovery.(C) C = True concentration value.(D) St = Overall standard deviation.(E) So = Single analyst standard deviation.
1.3 Chlordane, toxaphene, and Aroclor products (polychlorinated biphenyls) are multicomponent materials. Precision and bias statements reflect recovery of these materials dosed into water samples. The precision and bias statements may not apply to environmentally altered materials or to samples containing complex mixtures of polychlorinated biphenyls (PCBs) and organochlorine pesticides.
1.4 For compounds other than those listed in 1.1 or for other sample sources, the analyst must demonstrate the applicability of this test method by collecting precision and bias data on spiked samples (groundwater, tap water) (4) and provide qualitative confirmation of results by gas chromatography/mass spectrometry (GC/MS) (5) or by GC analysis using dissimilar columns.
1.5 This test method is restricted to use by or under the supervision of analysts experienced in the use of GC and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results using the procedure described in Section 13.
1.6 Analytes that are not separated chromatographically, (analytes that have very similar retention times) cannot be individually identified and measured in the same calibration mixture or water sample unless an alternative technique for identification and quantitation exists (see 13.4).
1.7 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications and concentrations should be confirmed by at least one additional technique.
1.8 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered standard.
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices a...
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
´1
Designation: D5175 − 91 (Reapproved 2017)
Standard Test Method for
Organohalide Pesticides and Polychlorinated Biphenyls in
Water by Microextraction and Gas Chromatography
This standard is issued under the fixed designation D5175; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Warning notes were editorially updated throughout in December 2017.
1. Scope 1.3 Chlordane, toxaphene, and Aroclor products (polychlo-
rinatedbiphenyls)aremulticomponentmaterials.Precisionand
1.1 This test method (1-3) is applicable to the determina-
bias statements reflect recovery of these materials dosed into
tion of the following analytes in finished drinking water,
water samples. The precision and bias statements may not
drinking water during intermediate stages of treatment, and the
apply to environmentally altered materials or to samples
raw source water:
containing complex mixtures of polychlorinated biphenyls
Chemical Abstract Service
Analyte
A (PCBs) and organochlorine pesticides.
Registry Number
Alachlor 5972-60-8
1.4 Forcompoundsotherthanthoselistedin1.1orforother
Aldrin 309-00-2
Chlordane 57-74-9
sample sources, the analyst must demonstrate the applicability
Dieldrin 60-57-1
of this test method by collecting precision and bias data on
Endrin 72-20-8
spiked samples (groundwater, tap water) (4) and provide
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
qualitative confirmation of results by gas chromatography/
Hexachlorobenzene 118-74-1
mass spectrometry (GC/MS) (5) or by GC analysis using
Lindane 58-89-9
dissimilar columns.
Methoxychlor 72-43-5
Toxaphene 8001-35-2
B
1.5 This test method is restricted to use by or under the
Aroclor 1016 12674-11-2
B
Aroclor 1221 11104-28-2
supervision of analysts experienced in the use of GC and in the
B
Aroclor 1232 11141-16-5
B interpretation of gas chromatograms. Each analyst must dem-
Aroclor 1242 53469-21-9
B
Aroclor 1248 12672-29-6 onstrate the ability to generate acceptable results using the
B
Aroclor 1254 11097-69-1
procedure described in Section 13.
B
Aroclor 1260 11096-82-5
1.6 Analytes that are not separated chromatographically,
A
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH
(analytes that have very similar retention times) cannot be
43210-0334.
B
individually identified and measured in the same calibration
Aroclor is a registered trademark of Monsanto Co.
mixture or water sample unless an alternative technique for
1.2 Detection limits for most test method analytes are less
identification and quantitation exists (see 13.4).
than 1 µg/L. Actual detection limits are highly dependent on
1.7 When this test method is used to analyze unfamiliar
the characteristics of the sample matrix and the gas chroma-
samples for any or all of the analytes listed in 1.1, analyte
tography system. Table 1 contains the applicable concentration
identifications and concentrations should be confirmed by at
range for the precision and bias statements. OnlyAroclor 1016
least one additional technique.
and 1254 were included in the interlaboratory test used to
derive the precision and bias statements. Data for other PCB
1.8 The values stated in SI units are to be regarded as
products are likely to be similar.
standard. The values given in parentheses are mathematical
conversions to inch-pound units that are provided for informa-
tion only and are not considered standard.
This test method is under the jurisdiction of ASTM Committee D19 on Water
1.9 This standard does not purport to address all of the
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
safety concerns, if any, associated with its use. It is the
Organic Substances in Water.
Current edition approved Dec. 15, 2017. Published January 2018. Originally
responsibility of the user of this standard to establish appro-
approved in 1991. Last previous edition approved in 2011 as D5175 – 91 (2011).
priate safety, health, and environmental practices and deter-
DOI: 10.1520/D5175-91R17E01.
mine the applicability of regulatory limitations prior to use.
The boldface numbers in parentheses refer to a list of references at the end of
this standard. For specific hazard statements, see Section 9.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5175 − 91 (2017)
A
TABLE 1 Test Method Precision and Bias as Functions of Concentration
BCDE
Water Type
Compound Applicable Concentration Range, µg/L
Reagent water Ground water
Alachlor 0.50 to 37.50 S = 0.077X + 0.09 S = 0.075X + 0.05
o o
S = 0.107X + 0.15 S = 0.086X + 0.29
t t
X = 1.004C − 0.08 X = 1.059C + 0.03
Aldrin 0.04 to 1.42 S = 0.030X + 0.02 S =0.115X + 0.00
o o
S = 0.251X + 0.00 S = 0.189X + 0.01
t t
X = 1.066C + 0.00 X = 0.945C − 0.00
Chlordane 0.51 to 50.90 S = 0.083X + 0.06 S = 0.062X + 0.09
o o
S = 0.125X + 0.19 S = 0.147X + 0.24
t t
X = 1.037C + 0.06 X = 0.941C + 0.09
Dieldrin 0.10 to 7.53 S = 0.091X + 0.01 S = 0.089X + 0.04
o o
S = 0.199X + 0.02 S = 0.221X + 0.04
t t
X = 1.027C + 0.00 X = 0.961C + 0.01
Endrin 0.10 to 7.50 S =0.116X + 0.01 S = 0.045X + 0.15
o o
S = 0.134X + 0.02 S = 0.196X + 0.07
t t
X = 0.958C + 0.01 X = 0.958C + 0.05
Heptachlor 0.04 to 1.41 S = 0.104X + 0.01 S = 0.058X + 0.02
o o
S = 0.206X + 0.02 S = 0.153X + 0.02
t t
X = 1.002C + 0.02 X = 0.964C + 0.02
Heptachlor Epoxide 0.04 to 1.42 S = 0.031X + 0.02 S = 0.032X + 0.00
o o
S = 0.127X + 0.02 S = 0.103X + 0.02
t t
X = 0.952C + 0.00 X = 0.932C + 0.01
Hexachlorobenzene 0.01 to 0.37 S = 0.104X + 0.00 S = 0.148X + 0.00
o o
S = 0.231X + 0.00 S = 0.301X + 0.00
t t
X = 1.028C − 0.00 X = 0.901C − 0.00
Lindane 0.04 to 1.39 S = 0.056X + 0.01 S = 0.095X + 0.00
o o
S = 0.141X + 0.00 S = 0.134X − 0.00
t t
X = 1.009C − 0.00 X = 0.909C + 0.00
Methoxychlor 0.20 to 15.00 S =0.115X + 0.12 S = 0.179X + 0.02
o o
S = 0.122X + 0.21 S = 0.210X + 0.08
t t
X = 0.950C + 0.15 X = 1.014C + 0.07
Toxaphene 5.63 to 70.40 S = 0.132X − 0.32 S = 0.067X + 0.28
o o
S = 0.273X − 0.72 S = 0.181X + 1.52
t t
X = 1.087C + 0.24 X = 0.903C + 0.50
PCB-1016 0.50 to 49.80 S = 0.106X + 0.31 S = 0.141X + 0.13
o o
S = 0.144X + 0.46 S = 0.218X + 0.06
t t
X = 0.856C + 0.31 X = 0.958C + 0.07
PCB-1254 0.50 to 50.40 S = 0.122X + 0.12 S = 0.126X + 0.17
o o
S = 0.282X + 0.05 S = 0.396X + 0.02
t t
X = 0.872C − 0.01 X = 0.938C − 0.02
A
Bias =C−X.
B
X = Mean recovery.
C
C = True concentration value.
D
S = Overall standard deviation.
t
E
S = Single analyst standard deviation.
o
1.10 This international standard was developed in accor- 2. Referenced Documents
dance with internationally recognized principles on standard-
2.1 ASTM Standards:
ization established in the Decision on Principles for the
D1129 Terminology Relating to Water
Development of International Standards, Guides and Recom-
D1193 Specification for Reagent Water
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
´1
D5175 − 91 (2017)
D3534 Test Method for Polychlorinated Biphenyls (PCBs) 3.2.5 laboratory fortified blank (LFB), n—an aliquot of
in Water (Withdrawn 2003) reagent water to which known quantities of the analytes are
D3856 Guide for Management Systems in Laboratories added in the laboratory. The LFB is analyzed exactly like a
Engaged in Analysis of Water sample, and its purpose is to determine whether the method-
D4128 Guide for Identification and Quantitation of Organic ology is in control, and whether the laboratory is capable of
Compounds in Water by Combined Gas Chromatography making accurate and precise measurements.
and Electron Impact Mass Spectrometry
3.2.6 laboratory fortified sample matrix (LFM), n—an ali-
D4210 Practice for Intralaboratory Quality Control Proce-
quot of an environmental sample to which known quantities of
dures and a Discussion on Reporting Low-Level Data
the analytes are added in the laboratory. The LFM is analyzed
(Withdrawn 2002)
asasample,anditspurposeistodeterminewhetherthesample
E355 Practice for Gas ChromatographyTerms and Relation-
matrix contributes bias to the analytical results. The back-
ships
ground concentrations of the analytes in the sample matrix
2.2 EPA Standards:
must be determined in a separate aliquot and the measured
Method 505 Analysis of Organohalide Pesticides and Aro-
values in the LFM corrected for background concentrations.
clors in Water by Microextraction and Gas Chromatogra-
3.2.7 laboratory reagent blank (LRB), n—an aliquot of
phy
reagent water that is treated as a sample including exposure to
Method 680 Determination of Pesticides and PCBs in Water
all glassware, equipment, solvents, and reagents used with
and Soil/Sediment by Gas Chromatography/Mass Spec-
other samples. The LRB is used to determine if method
trometry
analytes or other interferences are present in the laboratory
environment, the reagents, or the apparatus.
3. Terminology
3.2.8 standard solution, secondary dilution, n—asolutionof
3.1 Definitions:
several analytes prepared in the laboratory from stock standard
3.1.1 For definitions of terms used in this standard, refer to
solutions and diluted as needed to prepare calibration solutions
Terminology D1129 and Practice E355.
and other needed analyte solutions.
3.2 Definitions of Terms Specific to This Standard:
3.2.9 standard solution, stock, n—a concentrated solution
3.2.1 field duplicates (FD 1 and FD 2), n—two separate
containing a single certified standard that is an analyte or a
samples collected at the same time and placed under identical
concentrated solution of a single analyte prepared in the
circumstances and treated exactly the same throughout field
laboratory with an assayed reference compound. Stock stan-
and laboratory procedures. Analyses of FD 1 and FD 2 give a
dardsolutionsareusedtopreparesecondarydilutionstandards.
measure of the precision associated with sample collection,
preservationandstorage,aswellaswithlaboratoryprocedures.
3.2.10 quality control sample (QCS), n—a sample contain-
ing analytes or a solution of analytes in a water-miscible
3.2.2 field reagent blank (FRB), n—reagent water placed in
solventusedtofortifyreagentwaterorenvironmentalsamples.
a sample container in the laboratory and treated as a sample in
The QCS must be independent of solutions used to prepare
all respects, including exposure to sampling site conditions,
standards and should be obtained from a source external to the
storage, preservation, and all analytical procedures. The re-
laboratory. The QCS is used to check laboratory performance
agent water must be transferred to an empty, clean sample
with externally prepared test materials.
container in the field. The purpose of the FRB is to determine
if analytes or other interferences are present in the field
4. Summary of Test Method
environment.
3.2.3 instrument performance check solution (IPC), n—a
4.1 This is a microextraction method in which 35 mL of
solution of analytes used to evaluate the performance of the
sample are extracted with 2 mL of hexane. Two µL of the
instrument system with respect to test method criteria.
extract are injected into a gas chromatograph equipped with a
linearizedelectroncapturedetectorforseparationandanalysis.
3.2.4 laboratory duplicates (LD 1 and LD 2), n—two
Aqueous calibration standards are extracted and analyzed in an
sample aliquots taken in the analytical laboratory and analyzed
identical manner to compensate for possible extraction losses.
separately with identical procedures.Analyses of LD 1 and LD
2 give a measure of the precision associated with laboratory
4.2 The extraction and analysis time is 30 to 50 min per
procedures but not with sample collection, preservation, or
sample depending upon the analytes and the analytical condi-
storage procedures.
tions chosen.
4.3 This test method is based largely on EPA Method 505.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 5. Significance and Use
Standards volume information, refer to the standard’s Document Summary page on
5.1 The extensive and widespread use of organochlorine
the ASTM website.
The last approved version of this historical standard is referenced on
pesticides and PCBs has resulted in their presence in all parts
www.astm.org.
of the environment. These compounds are persistent and may
AvailablefromUnitedStatesEnvironmentalProtectionAgency(EPA),William
have adverse effects on the environment. Thus, there is a need
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov. to identify and quantitate these compounds in water samples.
´1
D5175 − 91 (2017)
6. Interferences 6.7 Variable amounts of pesticides and PCBs from aqueous
solutions adhere to glass surfaces. It is recommended that
6.1 Interferences may be caused by contaminants in
sample transfers and glass surface contacts be minimized.
solvents, reagents, glassware, and other sample processing
6.8 Aldrin and methoxychlor are rapidly oxidized by chlo-
apparatus that lead to discrete artifacts or elevated baselines in
rine. Dechlorination with sodium thiosulfate at time of collec-
gas chromatograms. All reagents and apparatus must be rou-
tion will retard further oxidation of these compounds.
tinely demonstrated to be free from interferences under the
conditions of the analysis by running laboratory reagent blanks
6.9 Aninterfering,erraticpeakhasbeenobservedwithinthe
as described in 12.2.
retention window of heptachlor during many analyses of
6.1.1 Glassware must be scrupulously cleaned (2). Clean all reagent, tap, and groundwater. It appears to be related to
glassware as soon as possible after use by thoroughly rinsing
dibutylphthalate;however,thespecificsourcehasnotyetbeen
with the last solvent used in it. Follow by washing with hot tap determined.Theobservedmagnitudeandcharacterofthispeak
water and detergent and thoroughly rinsing with tap and randomly vary in numerical value from successive injections
reagent water. Drain dry and heat in an oven or muffle furnace made from the same vial. This type of outlying observation
normallyisrecognized.Ifencountered,additionalanalyseswill
at 400°C for 1 h. Do not heat volumetric ware. Thermally
stable materials might not be eliminated by this treatment. be necessary.
Thorough rin
...
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: D5175 − 91 (Reapproved 2017)
Standard Test Method for
Organohalide Pesticides and Polychlorinated Biphenyls in
Water by Microextraction and Gas Chromatography
This standard is issued under the fixed designation D5175; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Warning notes were editorially updated throughout in December 2017.
1. Scope 1.3 Chlordane, toxaphene, and Aroclor products (polychlo-
2 rinated biphenyls) are multicomponent materials. Precision and
1.1 This test method (1-3) is applicable to the determina-
bias statements reflect recovery of these materials dosed into
tion of the following analytes in finished drinking water,
water samples. The precision and bias statements may not
drinking water during intermediate stages of treatment, and the
apply to environmentally altered materials or to samples
raw source water:
containing complex mixtures of polychlorinated biphenyls
Chemical Abstract Service
Analyte
A (PCBs) and organochlorine pesticides.
Registry Number
Alachlor 5972-60-8
1.4 For compounds other than those listed in 1.1 or for other
Aldrin 309-00-2
Chlordane 57-74-9
sample sources, the analyst must demonstrate the applicability
Dieldrin 60-57-1
of this test method by collecting precision and bias data on
Endrin 72-20-8
spiked samples (groundwater, tap water) (4) and provide
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
qualitative confirmation of results by gas chromatography/
Hexachlorobenzene 118-74-1
mass spectrometry (GC/MS) (5) or by GC analysis using
Lindane 58-89-9
dissimilar columns.
Methoxychlor 72-43-5
Toxaphene 8001-35-2
B
1.5 This test method is restricted to use by or under the
Aroclor 1016 12674-11-2
B
Aroclor 1221 11104-28-2
supervision of analysts experienced in the use of GC and in the
B
Aroclor 1232 11141-16-5
B interpretation of gas chromatograms. Each analyst must dem-
Aroclor 1242 53469-21-9
B
Aroclor 1248 12672-29-6 onstrate the ability to generate acceptable results using the
B
Aroclor 1254 11097-69-1
procedure described in Section 13.
B
Aroclor 1260 11096-82-5
1.6 Analytes that are not separated chromatographically,
A
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH
(analytes that have very similar retention times) cannot be
43210-0334.
B individually identified and measured in the same calibration
Aroclor is a registered trademark of Monsanto Co.
mixture or water sample unless an alternative technique for
1.2 Detection limits for most test method analytes are less
identification and quantitation exists (see 13.4).
than 1 µg/L. Actual detection limits are highly dependent on
1.7 When this test method is used to analyze unfamiliar
the characteristics of the sample matrix and the gas chroma-
samples for any or all of the analytes listed in 1.1, analyte
tography system. Table 1 contains the applicable concentration
identifications and concentrations should be confirmed by at
range for the precision and bias statements. Only Aroclor 1016
least one additional technique.
and 1254 were included in the interlaboratory test used to
derive the precision and bias statements. Data for other PCB
1.8 The values stated in SI units are to be regarded as
products are likely to be similar.
standard. The values given in parentheses are mathematical
conversions to inch-pound units that are provided for informa-
tion only and are not considered standard.
This test method is under the jurisdiction of ASTM Committee D19 on Water
1.9 This standard does not purport to address all of the
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
safety concerns, if any, associated with its use. It is the
Organic Substances in Water.
Current edition approved Dec. 15, 2017. Published January 2018. Originally
responsibility of the user of this standard to establish appro-
approved in 1991. Last previous edition approved in 2011 as D5175 – 91 (2011).
priate safety, health, and environmental practices and deter-
DOI: 10.1520/D5175-91R17E01.
2 mine the applicability of regulatory limitations prior to use.
The boldface numbers in parentheses refer to a list of references at the end of
this standard. For specific hazard statements, see Section 9.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5175 − 91 (2017)
A
TABLE 1 Test Method Precision and Bias as Functions of Concentration
B C D E
Water Type
Compound Applicable Concentration Range, µg/L
Reagent water Ground water
Alachlor 0.50 to 37.50 S = 0.077X + 0.09 S = 0.075X + 0.05
o o
S = 0.107X + 0.15 S = 0.086X + 0.29
t t
X = 1.004C − 0.08 X = 1.059C + 0.03
Aldrin 0.04 to 1.42 S = 0.030X + 0.02 S = 0.115X + 0.00
o o
S = 0.251X + 0.00 S = 0.189X + 0.01
t t
X = 1.066C + 0.00 X = 0.945C − 0.00
Chlordane 0.51 to 50.90 S = 0.083X + 0.06 S = 0.062X + 0.09
o o
S = 0.125X + 0.19 S = 0.147X + 0.24
t t
X = 1.037C + 0.06 X = 0.941C + 0.09
Dieldrin 0.10 to 7.53 S = 0.091X + 0.01 S = 0.089X + 0.04
o o
S = 0.199X + 0.02 S = 0.221X + 0.04
t t
X = 1.027C + 0.00 X = 0.961C + 0.01
Endrin 0.10 to 7.50 S = 0.116X + 0.01 S = 0.045X + 0.15
o o
S = 0.134X + 0.02 S = 0.196X + 0.07
t t
X = 0.958C + 0.01 X = 0.958C + 0.05
Heptachlor 0.04 to 1.41 S = 0.104X + 0.01 S = 0.058X + 0.02
o o
S = 0.206X + 0.02 S = 0.153X + 0.02
t t
X = 1.002C + 0.02 X = 0.964C + 0.02
Heptachlor Epoxide 0.04 to 1.42 S = 0.031X + 0.02 S = 0.032X + 0.00
o o
S = 0.127X + 0.02 S = 0.103X + 0.02
t t
X = 0.952C + 0.00 X = 0.932C + 0.01
Hexachlorobenzene 0.01 to 0.37 S = 0.104X + 0.00 S = 0.148X + 0.00
o o
S = 0.231X + 0.00 S = 0.301X + 0.00
t t
X = 1.028C − 0.00 X = 0.901C − 0.00
Lindane 0.04 to 1.39 S = 0.056X + 0.01 S = 0.095X + 0.00
o o
S = 0.141X + 0.00 S = 0.134X − 0.00
t t
X = 1.009C − 0.00 X = 0.909C + 0.00
Methoxychlor 0.20 to 15.00 S = 0.115X + 0.12 S = 0.179X + 0.02
o o
S = 0.122X + 0.21 S = 0.210X + 0.08
t t
X = 0.950C + 0.15 X = 1.014C + 0.07
Toxaphene 5.63 to 70.40 S = 0.132X − 0.32 S = 0.067X + 0.28
o o
S = 0.273X − 0.72 S = 0.181X + 1.52
t t
X = 1.087C + 0.24 X = 0.903C + 0.50
PCB-1016 0.50 to 49.80 S = 0.106X + 0.31 S = 0.141X + 0.13
o o
S = 0.144X + 0.46 S = 0.218X + 0.06
t t
X = 0.856C + 0.31 X = 0.958C + 0.07
PCB-1254 0.50 to 50.40 S = 0.122X + 0.12 S = 0.126X + 0.17
o o
S = 0.282X + 0.05 S = 0.396X + 0.02
t t
X = 0.872C − 0.01 X = 0.938C − 0.02
A
Bias = C − X.
B
X = Mean recovery.
C
C = True concentration value.
D
S = Overall standard deviation.
t
E
S = Single analyst standard deviation.
o
1.10 This international standard was developed in accor- 2. Referenced Documents
dance with internationally recognized principles on standard-
2.1 ASTM Standards:
ization established in the Decision on Principles for the
D1129 Terminology Relating to Water
Development of International Standards, Guides and Recom-
D1193 Specification for Reagent Water
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
´1
D5175 − 91 (2017)
D3534 Test Method for Polychlorinated Biphenyls (PCBs) 3.2.5 laboratory fortified blank (LFB), n—an aliquot of
in Water (Withdrawn 2003) reagent water to which known quantities of the analytes are
D3856 Guide for Management Systems in Laboratories added in the laboratory. The LFB is analyzed exactly like a
Engaged in Analysis of Water sample, and its purpose is to determine whether the method-
D4128 Guide for Identification and Quantitation of Organic ology is in control, and whether the laboratory is capable of
Compounds in Water by Combined Gas Chromatography making accurate and precise measurements.
and Electron Impact Mass Spectrometry
3.2.6 laboratory fortified sample matrix (LFM), n—an ali-
D4210 Practice for Intralaboratory Quality Control Proce-
quot of an environmental sample to which known quantities of
dures and a Discussion on Reporting Low-Level Data
the analytes are added in the laboratory. The LFM is analyzed
(Withdrawn 2002)
as a sample, and its purpose is to determine whether the sample
E355 Practice for Gas Chromatography Terms and Relation-
matrix contributes bias to the analytical results. The back-
ships
ground concentrations of the analytes in the sample matrix
2.2 EPA Standards:
must be determined in a separate aliquot and the measured
Method 505 Analysis of Organohalide Pesticides and Aro-
values in the LFM corrected for background concentrations.
clors in Water by Microextraction and Gas Chromatogra-
3.2.7 laboratory reagent blank (LRB), n—an aliquot of
phy
reagent water that is treated as a sample including exposure to
Method 680 Determination of Pesticides and PCBs in Water
all glassware, equipment, solvents, and reagents used with
and Soil/Sediment by Gas Chromatography/Mass Spec-
other samples. The LRB is used to determine if method
trometry
analytes or other interferences are present in the laboratory
environment, the reagents, or the apparatus.
3. Terminology
3.2.8 standard solution, secondary dilution, n—a solution of
3.1 Definitions:
several analytes prepared in the laboratory from stock standard
3.1.1 For definitions of terms used in this standard, refer to
solutions and diluted as needed to prepare calibration solutions
Terminology D1129 and Practice E355.
and other needed analyte solutions.
3.2 Definitions of Terms Specific to This Standard:
3.2.9 standard solution, stock, n—a concentrated solution
3.2.1 field duplicates (FD 1 and FD 2), n—two separate
containing a single certified standard that is an analyte or a
samples collected at the same time and placed under identical
concentrated solution of a single analyte prepared in the
circumstances and treated exactly the same throughout field
laboratory with an assayed reference compound. Stock stan-
and laboratory procedures. Analyses of FD 1 and FD 2 give a
dard solutions are used to prepare secondary dilution standards.
measure of the precision associated with sample collection,
preservation and storage, as well as with laboratory procedures.
3.2.10 quality control sample (QCS), n—a sample contain-
ing analytes or a solution of analytes in a water-miscible
3.2.2 field reagent blank (FRB), n—reagent water placed in
solvent used to fortify reagent water or environmental samples.
a sample container in the laboratory and treated as a sample in
The QCS must be independent of solutions used to prepare
all respects, including exposure to sampling site conditions,
standards and should be obtained from a source external to the
storage, preservation, and all analytical procedures. The re-
laboratory. The QCS is used to check laboratory performance
agent water must be transferred to an empty, clean sample
with externally prepared test materials.
container in the field. The purpose of the FRB is to determine
if analytes or other interferences are present in the field
4. Summary of Test Method
environment.
3.2.3 instrument performance check solution (IPC), n—a
4.1 This is a microextraction method in which 35 mL of
solution of analytes used to evaluate the performance of the
sample are extracted with 2 mL of hexane. Two µL of the
instrument system with respect to test method criteria.
extract are injected into a gas chromatograph equipped with a
linearized electron capture detector for separation and analysis.
3.2.4 laboratory duplicates (LD 1 and LD 2), n—two
Aqueous calibration standards are extracted and analyzed in an
sample aliquots taken in the analytical laboratory and analyzed
identical manner to compensate for possible extraction losses.
separately with identical procedures. Analyses of LD 1 and LD
2 give a measure of the precision associated with laboratory
4.2 The extraction and analysis time is 30 to 50 min per
procedures but not with sample collection, preservation, or
sample depending upon the analytes and the analytical condi-
storage procedures.
tions chosen.
4.3 This test method is based largely on EPA Method 505.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 5. Significance and Use
Standards volume information, refer to the standard’s Document Summary page on
5.1 The extensive and widespread use of organochlorine
the ASTM website.
The last approved version of this historical standard is referenced on
pesticides and PCBs has resulted in their presence in all parts
www.astm.org.
of the environment. These compounds are persistent and may
Available from United States Environmental Protection Agency (EPA), William
have adverse effects on the environment. Thus, there is a need
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov. to identify and quantitate these compounds in water samples.
´1
D5175 − 91 (2017)
6. Interferences 6.7 Variable amounts of pesticides and PCBs from aqueous
solutions adhere to glass surfaces. It is recommended that
6.1 Interferences may be caused by contaminants in
sample transfers and glass surface contacts be minimized.
solvents, reagents, glassware, and other sample processing
6.8 Aldrin and methoxychlor are rapidly oxidized by chlo-
apparatus that lead to discrete artifacts or elevated baselines in
rine. Dechlorination with sodium thiosulfate at time of collec-
gas chromatograms. All reagents and apparatus must be rou-
tion will retard further oxidation of these compounds.
tinely demonstrated to be free from interferences under the
conditions of the analysis by running laboratory reagent blanks
6.9 An interfering, erratic peak has been observed within the
as described in 12.2. retention window of heptachlor during many analyses of
6.1.1 Glassware must be scrupulously cleaned (2). Clean all
reagent, tap, and groundwater. It appears to be related to
glassware as soon as possible after use by thoroughly rinsing dibutyl phthalate; however, the specific source has not yet been
with the last solvent used in it. Follow by washing with hot tap
determined. The observed magnitude and character of this peak
water and detergent and thoroughly rinsing with tap and randomly vary in numerical value from successive injections
reagent water. Drain dry and heat in an oven or muffle furnace made from the same vial. This type of outlying observation
at 400°C for 1 h. Do not heat volumetric ware. Thermally normally is recognized. If encountered, additional analyses will
be necessary.
stable materials might not be eliminated by this treatment.
Thorough rinsing wit
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5175 − 91 (Reapproved 2011) D5175 − 91 (Reapproved 2017)
Standard Test Method for
Organohalide Pesticides and Polychlorinated Biphenyls in
Water by Microextraction and Gas Chromatography
This standard is issued under the fixed designation D5175; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Warning notes were editorially updated throughout in December 2017.
1. Scope
1.1 This test method (11-3, 2, 3) is applicable to the determination of the following analytes in finished drinking water, drinking
water during intermediate stages of treatment, and the raw source water:
Chemical Abstract Service
Analyte
A
Registry Number
Chemical Abstract Service
A
Analyte Registry Number
Alachlor 5972-60-8
Aldrin 309-00-2
Chlordane 57-74-9
Dieldrin 60-57-1
Endrin 72-20-8
Heptachlor 76-44-8
Heptachlor Epoxide 1024-57-3
Hexachlorobenzene 118-74-1
Lindane 58-89-9
Methoxychlor 72-43-5
Toxaphene 8001-35-2
B
Aroclor 1016 12674-11-2
B
Aroclor 1221 11104-28-2
B
Aroclor 1232 11141-16-5
B
Aroclor 1242 53469-21-9
B
Aroclor 1248 12672-29-6
B
Aroclor 1254 11097-69-1
B
Aroclor 1260 11096-82-5
A
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH 43210-0334.
B
Aroclor is a registered trademark of Monsanto Co.
1.2 Detection limits for most test method analytes are less than 1 μg/L. Actual detection limits are highly dependent on the
characteristics of the sample matrix and the gas chromatography system. Table 1 contains the applicable concentration range for
the precision and bias statements. Only Aroclor 1016 and 1254 were included in the interlaboratory test used to derive the precision
and bias statements. Data for other PCB products are likely to be similar.
1.3 Chlordane, toxaphene, and Aroclor products (polychlorinated biphenyls) are multicomponent materials. Precision and bias
statements reflect recovery of these materials dosed into water samples. The precision and bias statements may not apply to
environmentally altered materials or to samples containing complex mixtures of polychlorinated biphenyls (PCBs) and
organochlorine pesticides.
1.4 For compounds other than those listed in 1.1 or for other sample sources, the analyst must demonstrate the applicability of
this test method by collecting precision and bias data on spiked samples (groundwater, tap water) (4) and provide qualitative
confirmation of results by gas chromatography/mass spectrometry (GC/MS) (5) or by GC analysis using dissimilar columns.
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved May 1, 2011Dec. 15, 2017. Published June 2011January 2018. Originally approved in 1991. Last previous edition approved in 20032011 as
D5175 – 91 (2003).(2011). DOI: 10.1520/D5175-91R11.10.1520/D5175-91R17E01.
The boldface numbers in parentheses refer to a list of references at the end of this test method.standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D5175 − 91 (2017)
A
TABLE 1 Test Method Precision and Bias Bias as Functions of Concentration
B C D E
Water Type
Applicable Concentration Range,μ
Compound
g/LRange, μg/L
Reagent water Ground water
Alachlor 0.50 to 37.50 S = 0.077X + 0.09 S = 0.075X + 0.05
o o
S = 0.107X + 0.15 S = 0.086X + 0.29
t t
X = 1.004C − 0.08 X = 1.059C + 0.03
Aldrin 0.04 to 1.42 S = 0.030X + 0.02 S = 0.115X + 0.00
o o
S = 0.251X + 0.00 S = 0.189X + 0.01
t t
X = 1.066C + 0.00 X = 0.945C − 0.00
Chlordane 0.51 to 50.90 S = 0.083X + 0.06 S = 0.062X + 0.09
o o
S = 0.125X + 0.19 S = 0.147X + 0.24
t t
X = 1.037C + 0.06 X = 0.941C + 0.09
Dieldrin 0.10 to 7.53 S = 0.091X + 0.01 S = 0.089X + 0.04
o o
S = 0.199X + 0.02 S = 0.221X + 0.04
t t
X = 1.027C + 0.00 X = 0.961C + 0.01
Endrin 0.10 to 7.50 S = 0.116X + 0.01 S = 0.045X + 0.15
o o
S = 0.134X + 0.02 S = 0.196X + 0.07
t t
X = 0.958C + 0.01 X = 0.958C + 0.05
Heptachlor 0.04 to 1.41 S = 0.104X + 0.01 S = 0.058X + 0.02
o o
S = 0.206X + 0.02 S = 0.153X + 0.02
t t
X = 1.002C + 0.02 X = 0.964C + 0.02
Heptachlor Epoxide 0.04 to 1.42 S = 0.031X + 0.02 S = 0.032X + 0.00
o o
S = 0.127X + 0.02 S = 0.103X + 0.02
t t
X = 0.952C + 0.00 X = 0.932C + 0.01
Hexachlorobenzene 0.01 to 0.37 S = 0.104X + 0.00 S = 0.148X + 0.00
o o
S = 0.231X + 0.00 S = 0.301X + 0.00
t t
X = 1.028C − 0.00 X = 0.901C − 0.00
Lindane 0.04 to 1.39 S = 0.056X + 0.01 S = 0.095X + 0.00
o o
S = 0.141X + 0.00 S = 0.134X − 0.00
t t
X = 1.009C − 0.00 X = 0.909C + 0.00
Methoxychlor 0.20 to 15.00 S = 0.115X + 0.12 S = 0.179X + 0.02
o o
S = 0.122X + 0.21 S = 0.210X + 0.08
t t
X = 0.950C + 0.15 X = 1.014C + 0.07
Toxaphene 5.63 to 70.40 S = 0.132X − 0.32 S = 0.067X + 0.28
o o
S = 0.273X − 0.72 S = 0.181X + 1.52
t t
X = 1.087C + 0.24 X = 0.903C + 0.50
PCB-1016 0.50 to 49.80 S = 0.106X + 0.31 S = 0.141X + 0.13
o o
S = 0.144X + 0.46 S = 0.218X + 0.06
t t
X = 0.856C + 0.31 X = 0.958C + 0.07
PCB-1254 0.50 to 50.40 S = 0.122X + 0.12 S = 0.126X + 0.17
o o
S = 0.282X + 0.05 S = 0.396X + 0.02
t t
X = 0.872C − 0.01 X = 0.938C − 0.02
A
Bias = C − XC − X. .
B
X = Mean recovery.
C
C = True concentration value.
D
S = Overall standard deviation.
t
E
S = Single analyst standard deviation.
o
1.5 This test method is restricted to use by or under the supervision of analysts experienced in the use of GC and in the
interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results using the procedure
described in Section 1313.
1.6 Analytes that are not separated chromatographically, (analytes that have very similar retention times) cannot be individually
identified and measured in the same calibration mixture or water sample unless an alternative technique for identification and
quantitation exists (see section 13.4).
1.7 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications
and concentrations should be confirmed by at least one additional technique.
1.8 The values stated in SI units are to be regarded as the standard. The inch-pound units values given in parentheses are for
information only.mathematical conversions to inch-pound units that are provided for information only and are not considered
standard.
´1
D5175 − 91 (2017)
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.
1.10 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D3534 Test Method for Polychlorinated Biphenyls (PCBs) in Water (Withdrawn 2003)
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D4128 Guide for Identification and Quantitation of Organic Compounds in Water by Combined Gas Chromatography and
Electron Impact Mass Spectrometry
D4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data (Withdrawn
2002)
E355 Practice for Gas Chromatography Terms and Relationships
2.2 EPA Standards:
Method 505, Method 505 Analysis of Organohalide Pesticides and Aroclors in Water by Microextraction and Gas Chromatog-
raphy
Method 680,Method 680 Determination of Pesticides and PCBs in Water and Soil/Sediment by Gas Chromatography/Mass
Spectrometry
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this test method, refer to Terminology D1129 and Practice E355.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129 and Practice E355.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 field duplicates (FD 1 and FD 2), n—two separate samples collected at the same time and placed under identical
circumstances and treated exactly the same throughout field and laboratory procedures. Analyses of FD 1 and FD 2 give a measure
of the precision associated with sample collection, preservation and storage, as well as with laboratory procedures.
3.2.2 field reagent blank (FRB), n—reagent water placed in a sample container in the laboratory and treated as a sample in all
respects, including exposure to sampling site conditions, storage, preservation, and all analytical procedures. The reagent water
must be transferred to an empty, clean sample container in the field. The purpose of the FRB is to determine if analytes or other
interferences are present in the field environment.
3.2.3 instrument performance check solution (IPC), n—a solution of analytes used to evaluate the performance of the instrument
system with respect to test method criteria.
3.2.4 laboratory duplicates (LD 1 and LD 2), n—two sample aliquots taken in the analytical laboratory and analyzed separately
with identical procedures. Analyses of LD 1 and LD 2 give a measure of the precision associated with laboratory procedures but
not with sample collection, preservation, or storage procedures.
3.2.5 laboratory fortified blank (LFB), n—an aliquot of reagent water to which known quantities of the analytes are added in
the laboratory. The LFB is 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.
3.2.6 laboratory fortified sample matrix (LFM), n—an aliquot of an environmental sample to which known quantities of the
analytes are added in the laboratory. The LFM is analyzed as a sample, and its purpose is to determine whether the sample matrix
contributes bias to the analytical results. The background concentrations of the analytes in the sample matrix must be determined
in a separate aliquot and the measured values in the LFM corrected for background concentrations.
3.2.7 laboratory reagent blank (LRB), n—an aliquot of reagent water that is treated as a sample including exposure to all
glassware, equipment, solvents, and reagents used with other samples. The LRB is used to determine if method analytes or other
interferences are present in the laboratory environment, the reagents, or the apparatus.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available from US EPA, Environmental Monitoring Systems Laboratory, Cincinnati, OH 45268.United States Environmental Protection Agency (EPA), William Jefferson
Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://www.epa.gov.
´1
D5175 − 91 (2017)
3.2.8 standard solution, secondary dilution, n—a solution of several analytes prepared in the laboratory from stock standard
solutions and diluted as needed to prepare calibration solutions and other needed analyte solutions.
3.2.9 standard solution, stock, n—a concentrated solution containing a single certified standard that is an analyte or a
concentrated solution of a single analyte prepared in the laboratory with an assayed reference compound. Stock standard solutions
are used to prepare secondary dilution standards.
3.2.10 quality control sample (QCS), n—a sample containing analytes or a solution of analytes in a water-miscible solvent used
to fortify reagent water or environmental samples. The QCS must be independent of solutions used to prepare standards and should
be obtained from a source external to the laboratory. The QCS is used to check laboratory performance with externally prepared
test materials.
4. Summary of Test Method
4.1 This is a microextraction method in which 35 mL of sample are extracted with 2 mL of hexane. Two μL of the extract are
injected into a gas chromatograph equipped with a linearized electron capture detector for separation and analysis. Aqueous
calibration standards are extracted and analyzed in an identical manner to compensate for possible extraction losses.
4.2 The extraction and analysis time is 30 to 50 min per sample depending upon the analytes and the analytical conditions
chosen.
4.3 This test method is based largely on EPA Method 505.
5. Significance and Use
5.1 The extensive and widespread use of organochlorine pesticides and PCBs has resulted in their presence in all parts of the
environment. These compounds are persistent and may have adverse effects on the environment. Thus, there is a need to identify
and quantitate these compounds in water samples.
6. Interferences
6.1 Interferences may be caused by contaminants in solvents, reagents, glassware, and other sample processing apparatus that
lead to discrete artifacts or elevated baselines in gas chromatograms. All reagents and apparatus must be routinely demonstrated
to be free from interferences under the conditions of the analysis by running laboratory reagent blanks as described in 12.2.
6.1.1 Glassware must be scrupulously cleaned (2). Clean all glassware as soon as possible after use by thoroughly rinsing with
the last solvent used in it. Follow by washing with hot tap water and detergent and thoroughly rinsing with tap and reagent water.
Drain dry and heat in an oven or muffle furnace at 400°C for 1 h. Do not heat volumetric ware. Thermally stable materials might
not be eliminated by this treatment. Thorough rinsing with acetone may be substituted for the heating. After drying and cooling,
seal and store glassware in a clean environment to prevent any accumulation of dust or other contaminants. Store inverted or
c
...
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