ASTM D5175-91(2011)
(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
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, 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:
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5175 − 91 (Reapproved 2011)
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 1.3 Chlordane, toxaphene, and Aroclor products (polychlo-
2 rinatedbiphenyls)aremulticomponentmaterials.Precisionand
1.1 This test method (1, 2, 3) is applicable to the determi-
bias statements reflect recovery of these materials dosed into
nation 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
A (PCBs) and organochlorine pesticides.
Analyte 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
qualitative confirmation of results by gas chromatography/
Heptachlor Epoxide 1024-57-3
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
1.5 This test method is restricted to use by or under the
B
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
interpretation of gas chromatograms. Each analyst must dem-
B
Aroclor 1242 53469-21-9
B onstrate the ability to generate acceptable results using the
Aroclor 1248 12672-29-6
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
(analytes that have very similar retention times) cannot be
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH
43210-0334.
individually identified and measured in the same calibration
B
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 section 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 the
products are likely to be similar.
standard. The inch-pound units given in parentheses are for
information only.
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 May 1, 2011. Published June 2011. Originally
responsibility of the user of this standard to establish appro-
approved in 1991. Last previous edition approved in 2003 as D5175 – 91 (2003).
priate safety and health practices and determine the applica-
DOI: 10.1520/D5175-91R11.
2 bility of regulatory limitations prior to use. For specific hazard
The boldface numbers in parentheses refer to a list of references at the end of
this test method. statements, see Section 9.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5175 − 91 (2011)
A
TABLE 1 Test Method Precision and Bias as Functions of Concentration
BCDE
Water Type
Compound Applicable Concentration Range,µ g/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
2. Referenced Documents D3534 Test Method for Polychlorinated Biphenyls (PCBs)
3 in Water (Withdrawn 2003)
2.1 ASTM Standards:
D3856 Guide for Management Systems in Laboratories
D1129 Terminology Relating to Water
Engaged in Analysis of Water
D1193 Specification for Reagent Water
D4128 Guide for Identification and Quantitation of Organic
Compounds in Water by Combined Gas Chromatography
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
D5175 − 91 (2011)
and Electron Impact Mass Spectrometry must be determined in a separate aliquot and the measured
D4210 Practice for Intralaboratory Quality Control Proce- values in the LFM corrected for background concentrations.
dures and a Discussion on Reporting Low-Level Data
3.2.7 laboratory reagent blank (LRB), n—an aliquot of
(Withdrawn 2002)
reagent water that is treated as a sample including exposure to
E355 Practice for Gas ChromatographyTerms and Relation-
all glassware, equipment, solvents, and reagents used with
ships
other samples. The LRB is used to determine if method
2.2 EPA Standards:
analytes or other interferences are present in the laboratory
Method 505, Analysis of Organohalide Pesticides and
environment, the reagents, or the apparatus.
Aroclors in Water by Microextraction and Gas Chroma-
3.2.8 standard solution, secondary dilution, n—asolutionof
tography
several analytes prepared in the laboratory from stock standard
Method 680, Determination of Pesticides and PCBs in
solutions and diluted as needed to prepare calibration solutions
Water and Soil/Sediment by Gas Chromatography/Mass
and other needed analyte solutions.
Spectrometry
3.2.9 standard solution, stock, n—a concentrated solution
containing a single certified standard that is an analyte or a
3. Terminology
concentrated solution of a single analyte prepared in the
3.1 Definitions—For definitions of terms used in this test
laboratory with an assayed reference compound. Stock stan-
method, refer to Terminology D1129 and Practice E355.
dardsolutionsareusedtopreparesecondarydilutionstandards.
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
solventusedtofortifyreagentwaterorenvironmentalsamples.
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
preservationandstorage,aswellaswithlaboratoryprocedures.
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
linearizedelectroncapturedetectorforseparationandanalysis.
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 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
5.1 The extensive and widespread use of organochlorine
procedures but not with sample collection, preservation, or
pesticides and PCBs has resulted in their presence in all parts
storage procedures.
of the environment. These compounds are persistent and may
3.2.5 laboratory fortified blank (LFB), n—an aliquot of
have adverse effects on the environment. Thus, there is a need
reagent water to which known quantities of the analytes are
to identify and quantitate these compounds in water samples.
added in the laboratory. The LFB is analyzed exactly like a
sample, and its purpose is to determine whether the method-
6. Interferences
ology is in control, and whether the laboratory is capable of
making accurate and precise measurements. 6.1 Interferences may be caused by contaminants in
solvents, reagents, glassware, and other sample processing
3.2.6 laboratory fortified sample matrix (LFM), n—an ali-
apparatus that lead to discrete artifacts or elevated baselines in
quot of an environmental sample to which known quantities of
gas chromatograms. All reagents and apparatus must be rou-
the analytes are added in the laboratory. The LFM is analyzed
tinely demonstrated to be free from interferences under the
asasample,anditspurposeistodeterminewhetherthesample
conditions of the analysis by running laboratory reagent blanks
matrix contributes bias to the analytical results. The back-
as described in 12.2.
ground concentrations of the analytes in the sample matrix
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
Available from US EPA, Environmental Monitoring Systems Laboratory,
Cincinnati, OH 45268. water and detergent and thoroughly rinsing with tap and
D5175 − 91 (2011)
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 normallyisrecognized.Ifencountered,additionalanalyseswill
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 by
distillation in all-glass systems may be required. temperature. Place the vials in a 400°C over for 1 h. Remove
and allow to cool in an area known to be free of organics.
6.2 Phthalate esters, frequently found in plastics, paints, and
7.2 Vials, auto sampler with septa and caps. Vials should be
othercommonlaboratoryitems,produceapositiveresponseon
compatible with automatic sample injector and should have an
an electron capture detector. Therefore, samples and solvents
internal volume of not greater than 2 mL.
should come in contact only with those materials specified in
this test method.
7.3 Automatic Sample Injector,forgaschromatograph,must
not require more than 0.5 mL of solution per injection
6.3 Interfering contamination may occur when a sample
(including rinsin
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