ASTM D5175-91(2024)

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  
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.  
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 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 th...

General Information

• Status: Published
• Publication Date: 31-Mar-2024
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D5175-91(2017)e1 - Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography
• Effective Date: 01-Apr-2024
• Referred By: ASTM D4128-18 - Standard Guide for Identification and Quantitation of Organic Compounds in Water by Combined Gas Chromatography and Electron Impact Mass Spectrometry
• Effective Date: 01-Apr-2024
• Referred By: ASTM D5241-92(2024) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
• Effective Date: 01-Apr-2024
• Referred By: ASTM D3694-96(2024) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-Apr-2024

Standards Content (Sample)

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.
Designation: D5175 − 91 (Reapproved 2024)
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.
1. Scope bias statements reflect recovery of these materials dosed into
water samples. The precision and bias statements may not
1.1 This test method (1-3) is applicable to the determina-
apply to environmentally altered materials or to samples
tion of the following analytes in finished drinking water,
containing complex mixtures of polychlorinated biphenyls
drinking water during intermediate stages of treatment, and the
(PCBs) and organochlorine pesticides.
raw source water:
Chemical Abstract Service
1.4 For compounds other than those listed in 1.1 or for other
Analyte
A
Registry Number
sample sources, the analyst must demonstrate the applicability
Alachlor 5972-60-8
of this test method by collecting precision and bias data on
Aldrin 309-00-2
Chlordane 57-74-9
spiked samples (groundwater, tap water) (4) and provide
Dieldrin 60-57-1
qualitative confirmation of results by gas chromatography/
Endrin 72-20-8
Heptachlor 76-44-8 mass spectrometry (GC/MS) (5) or by GC analysis using
Heptachlor Epoxide 1024-57-3
dissimilar columns.
Hexachlorobenzene 118-74-1
Lindane 58-89-9
1.5 This test method is restricted to use by or under the
Methoxychlor 72-43-5
supervision of analysts experienced in the use of GC and in the
Toxaphene 8001-35-2
B
Aroclor 1016 12674-11-2
interpretation of gas chromatograms. Each analyst must dem-
B
Aroclor 1221 11104-28-2
onstrate the ability to generate acceptable results using the
B
Aroclor 1232 11141-16-5
B
procedure described in Section 13.
Aroclor 1242 53469-21-9
B
Aroclor 1248 12672-29-6
B
Aroclor 1254 11097-69-1 1.6 Analytes that are not separated chromatographically,
B
Aroclor 1260 11096-82-5
(analytes that have very similar retention times) cannot be
individually identified and measured in the same calibration
A
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH
mixture or water sample unless an alternative technique for
43210-0334.
B
Aroclor is a registered trademark of Monsanto Co.
identification and quantitation exists (see 13.4).
1.2 Detection limits for most test method analytes are less
1.7 When this test method is used to analyze unfamiliar
than 1 μg/L. Actual detection limits are highly dependent on
samples for any or all of the analytes listed in 1.1, analyte
the characteristics of the sample matrix and the gas chroma-
identifications and concentrations should be confirmed by at
tography system. Table 1 contains the applicable concentration
least one additional technique.
range for the precision and bias statements. Only Aroclor 1016
1.8 The values stated in SI units are to be regarded as
and 1254 were included in the interlaboratory test used to
derive the precision and bias statements. Data for other PCB standard. The values given in parentheses are mathematical
conversions to inch-pound units that are provided for informa-
products are likely to be similar.
tion only and are not considered standard.
1.3 Chlordane, toxaphene, and Aroclor products (polychlo-
rinated biphenyls) are multicomponent materials. Precision and
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 appro-
This test method is under the jurisdiction of ASTM Committee D19 on Water
priate safety, health, and environmental practices and deter-
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
mine the applicability of regulatory limitations prior to use.
Organic Substances in Water.
For specific hazard statements, see Section 9.
Current edition approved April 1, 2024. Published April 2024. Originally
ɛ1
approved in 1991. Last previous edition approved in 2017 as D5175 – 91 (2017) .
1.10 This international standard was developed in accor-
DOI: 10.1520/D5175-91R24.
2 dance with internationally recognized principles on standard-
The boldface numbers in parentheses refer to a list of references at the end of
this standard. ization established in the Decision on Principles for the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5175 − 91 (2024)
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
Development of International Standards, Guides and Recom- D1193 Specification for Reagent Water
mendations issued by the World Trade Organization Technical D3534 Test Method for Polychlorinated Biphenyls (PCBs)
Barriers to Trade (TBT) Committee. in Water (Withdrawn 2003)
D3856 Guide for Management Systems in Laboratories
2. Referenced Documents
Engaged in Analysis of Water (Withdrawn 2024)
2.1 ASTM Standards: D4128 Guide for Identification and Quantitation of Organic
Compounds in Water by Combined Gas Chromatography
D1129 Terminology Relating to Water
and Electron Impact Mass Spectrometry
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
D5175 − 91 (2024)
D4210 Practice for Intralaboratory Quality Control Proce- must be determined in a separate aliquot and the measured
dures and a Discussion on Reporting Low-Level Data values in the LFM corrected for background concentrations.
(Withdrawn 2002)
3.2.7 laboratory reagent blank (LRB), n—an aliquot of
E355 Practice for Gas Chromatography Terms and Relation-
reagent water that is treated as a sample including exposure to
ships
all glassware, equipment, solvents, and reagents used with
2.2 EPA Standards:
other samples. The LRB is used to determine if method
Method 505 Analysis of Organohalide Pesticides and Aro-
analytes or other interferences are present in the laboratory
clors in Water by Microextraction and Gas Chromatogra-
environment, the reagents, or the apparatus.
phy
3.2.8 standard solution, secondary dilution, n—a solution of
Method 680 Determination of Pesticides and PCBs in Water
several analytes prepared in the laboratory from stock standard
and Soil/Sediment by Gas Chromatography/Mass Spec-
solutions and diluted as needed to prepare calibration solutions
trometry
and other needed analyte solutions.
3. Terminology 3.2.9 standard solution, stock, n—a concentrated solution
containing a single certified standard that is an analyte or a
3.1 Definitions:
concentrated solution of a single analyte prepared in the
3.1.1 For definitions of terms used in this standard, refer to
laboratory with an assayed reference compound. Stock stan-
Terminology D1129 and Practice E355.
dard solutions are used to prepare secondary dilution standards.
3.2 Definitions of Terms Specific to This Standard:
3.2.10 quality control sample (QCS), n—a sample contain-
3.2.1 field duplicates (FD 1 and FD 2), n—two separate
ing analytes or a solution of analytes in a water-miscible
samples collected at the same time and placed under identical
solvent used to fortify reagent water or environmental samples.
circumstances and treated exactly the same throughout field
The QCS must be independent of solutions used to prepare
and laboratory procedures. Analyses of FD 1 and FD 2 give a
standards and should be obtained from a source external to the
measure of the precision associated with sample collection,
laboratory. The QCS is used to check laboratory performance
preservation and storage, as well as with laboratory procedures.
with externally prepared test materials.
3.2.2 field reagent blank (FRB), n—reagent water placed in
a sample container in the laboratory and treated as a sample in
4. Summary of Test Method
all respects, including exposure to sampling site conditions,
4.1 This is a microextraction method in which 35 mL of
storage, preservation, and all analytical procedures. The re-
sample are extracted with 2 mL of hexane. Two μL of the
agent water must be transferred to an empty, clean sample
extract are injected into a gas chromatograph equipped with a
container in the field. The purpose of the FRB is to determine
linearized electron capture detector for separation and analysis.
if analytes or other interferences are present in the field
Aqueous calibration standards are extracted and analyzed in an
environment.
identical manner to compensate for possible extraction losses.
3.2.3 instrument performance check solution (IPC), n—a
4.2 The extraction and analysis time is 30 min to 50 min per
solution of analytes used to evaluate the performance of the
sample depending upon the analytes and the analytical condi-
instrument system with respect to test method criteria.
tions chosen.
3.2.4 laboratory duplicates (LD 1 and LD 2), n—two
4.3 This test method is based largely on EPA Method 505.
sample aliquots taken in the analytical laboratory and analyzed
separately with identical procedures. Analyses of LD 1 and LD
5. Significance and Use
2 give a measure of the precision associated with laboratory
procedures but not with sample collection, preservation, or
5.1 The extensive and widespread use of organochlorine
storage procedures.
pesticides and PCBs has resulted in their presence in all parts
3.2.5 laboratory fortified blank (LFB), n—an aliquot of of the environment. These compounds are persistent and may
have adverse effects on the environment. Thus, there is a need
reagent water to which known quantities of the analytes are
added in the laboratory. The LFB is analyzed exactly like a to identify and quantitate these compounds in water samples.
sample, and its purpose is to determine whether the method-
ology is in control, and whether the laboratory is capable of 6. Interferences
making accurate and precise measurements.
6.1 Interferences may be caused by contaminants in
3.2.6 laboratory fortified sample matrix (LFM), n—an ali-
solvents, reagents, glassware, and other sample processing
quot of an environmental sample to which known quantities of apparatus that lead to discrete artifacts or elevated baselines in
the analytes are added in the laboratory. The LFM is analyzed
gas chromatograms. All reagents and apparatus must be rou-
as a sample, and its purpose is to determine whether the sample tinely demonstrated to be free from interferences under the
matrix contributes bias to the analytical results. The back-
conditions of the analysis by running laboratory reagent blanks
ground concentrations of the analytes in the sample matrix
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
Available from United States Environmental Protection Agency (EPA), William
with the last solvent used in it. Follow by washing with hot tap
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov. water and detergent and thoroughly rinsing with tap and
D5175 − 91 (2024)
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
stable materials might not be eliminated by this treatment. be necessary.
Thorough rinsing with acetone may be substituted for the
7. Apparatus
heating. After drying and cooling, seal and store glassware in
a clean environment to prevent any accumulation of dust or 7.1 Sample Containers, 40 mL screw cap vials each
other contaminants. Store inverted or capped with aluminum
equipped with a size 24 cap with a flat, disc-like PTFE facing
foil. backed with a polyethylene film/foam extrusion. Prior to use,
6.1.2 The use of high purity reagents and solvents helps to wash vials and septa with detergent and rinse with tap and
reagent waters. Allow the vials and septa to air dry at room
minimize interference problems. Purification of solvents b
...