ASTM D5790-95(2001)
(Test Method)Standard Test Method for Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry
Standard Test Method for Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry
SCOPE
1.1 This test method covers the identification and simultaneous measurement of purgeable volatile organic compounds. It has been validated for treated drinking water, wastewater, and ground water. This test method is not limited to these particular aqueous matrices; however, the applicability of this test method to other aqueous matrices must be demonstrated.
1.2 This test method is applicable to a wide range of organic compounds that have sufficiently high volatility and low water solubility to be efficiently removed from water samples using purge and trap procedures. Table 1 lists the compounds that have been validated for this test method. This test method is not limited to the compounds listed in Table 1; however, the applicability of the test method to other compounds must be demonstrated.
1.3 Analyte concentrations up to approximately 200 μg/L may be determined without dilution of the sample. Analytes that are inefficiently purged from water will not be detected when present at low concentrations, but they can be measured with acceptable accuracy and precision when present in sufficient amounts.
1.4 Analytes that are not separated chromatographically, but that have different mass spectra and noninterfering quantitation ions, can be identified and measured in the same calibration mixture or water sample. Analytes that have very similar mass spectra cannot be individually identified and measured in the same calibration mixture or water sample unless they have different retention times. Coeluting compounds with very similar mass spectra, such as structural isomers, must be reported as an isomeric group or pair. Two of the three isomeric xylenes are examples of structural isomers that may not be resolved on the capillary column, and if not, must be reported as an isomeric pair.
1.5 It is the responsibility of the user to ensure the validity of this test method for untested matrices.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.7 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 and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation: D 5790 – 95 (Reapproved 2001)
Standard Test Method for
Measurement of Purgeable Organic Compounds in Water by
Capillary Column Gas Chromatography/Mass Spectrometry
This standard is issued under the fixed designation D 5790; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the identification and simulta-
responsibility of the user of this standard to establish appro-
neous measurement of purgeable volatile organic compounds.
priate safety and health practices and determine the applica-
It has been validated for treated drinking water, wastewater,
bility of regulatory limitations prior to use.
and ground water. This test method is not limited to these
particular aqueous matrices; however, the applicability of this
2. Referenced Documents
test method to other aqueous matrices must be demonstrated.
2.1 ASTM Standards:
1.2 Thistestmethodisapplicabletoawiderangeoforganic
D1129 Terminology Relating to Water
compounds that have sufficiently high volatility and low water
D2777 Practice for Determination of Precision and Bias of
solubility to be efficiently removed from water samples using
Applicable Methods of Committee D-19 on Water
purge and trap procedures. Table 1 lists the compounds that
D3871 Test Method for Purgeable Organic Compounds in
havebeenvalidatedforthistestmethod.Thistestmethodisnot
Water Using Headspace Sampling
limited to the compounds listed in Table 1; however, the
D3973 Test Method for Low-Molecular Weight Haloge-
applicability of the test method to other compounds must be
nated Hydrocarbons in Water
demonstrated.
D4210 Practice for Intralaboratory Quality Control Proce-
1.3 Analyte concentrations up to approximately 200 µg/L
dures and a Discussion on Reporting Low-Level Data
may be determined without dilution of the sample. Analytes
E355 Practice for Gas Chromatography Terms and Rela-
that are inefficiently purged from water will not be detected
tionships
when present at low concentrations, but they can be measured
2.2 Other Document:
with acceptable accuracy and precision when present in suffi-
Code of Federal Regulations, 40 CFR Part 261
cient amounts.
1.4 Analytesthatarenotseparatedchromatographically,but
3. Terminology
thathavedifferentmassspectraandnoninterferingquantitation
3.1 Definitions:
ions, can be identified and measured in the same calibration
3.1.1 For definitions of terms used in this test method, refer
mixture or water sample.Analytes that have very similar mass
to Definitions D1129 and Practice E355.
spectra cannot be individually identified and measured in the
3.2 Definitions of Terms Specific to This Standard:
same calibration mixture or water sample unless they have
3.2.1 calibration standard—a solution prepared from the
different retention times. Coeluting compounds with very
primarydilutionstandardsolutionandstockstandardsolutions
similar mass spectra, such as structural isomers, must be
oftheinternalstandardsandsurrogateanalytes.Thecalibration
reportedasanisomericgrouporpair.Twoofthethreeisomeric
standards are used to calibrate the instrument response with
xylenes are examples of structural isomers that may not be
respect to analyte concentration.
resolved on the capillary column, and if not, must be reported
3.2.2 field duplicates —two separate samples collected at
as an isomeric pair.
the same time and place under identical circumstances and
1.5 It is the responsibility of the user to ensure the validity
treated exactly the same throughout field and laboratory
of this test method for untested matrices.
procedures. Analysis of field duplicates gives an indication of
1.6 The values stated in SI units are to be regarded as the
the precision associated with sample collection, preservation,
standard. The values given in parentheses are for information
and storage, as well as with laboratory procedures.
only.
Annual Book of ASTM Standards, Vol 11.01.
1 3
This test method is under the jurisdiction ofASTM Committee D19 on Water Annual Book of ASTM Standards, Vol 11.02.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor Annual Book of ASTM Standards, Vol 14.01.
Organic Substances in Water. Available from the Superintendent of Documents, U.S. Government Printing
Current edition approved Sept. 10, 1995. Published November 1995. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5790 – 95 (2001)
3.2.3 field reagent blank—reagent water placed in a sample from a source external to the laboratory and is used to check
container,takentothefieldalongwiththesamples,andtreated laboratoryperformancewithexternallypreparedtestmaterials.
as a sample in all respects, including exposure to sampling site 3.2.13 stock standard solution—a concentrated solution
conditions,storage,preservation,andallanalyticalprocedures. containing a single certified standard that is a test method
The purpose of the field reagent blank is to determine if test analyte prepared in the laboratory with an assayed reference
method analytes or other interferences are present in the field compound. Stock standard solutions are used to prepare
environment. primarydilutionstandards.Commerciallyavailablestockstan-
dard solutions may be used.
3.2.4 internal standard—a pure analyte added to a solution
3.2.14 surrogate analyte—a pure analyte that is extremely
in a known amount, that is used to measure the relative
unlikely to be found in any sample, that is added to a sample
responses of other test method analytes and surrogates that are
aliquot in a known amount, and is measured with the same
components of the same solution. The internal standard must
procedures used to measure other components.The purpose of
be an analyte that is not a sample component.
asurrogateanalyteistomonitortestmethodperformancewith
3.2.5 laboratory duplicates—two sample aliquots taken in
each sample.
theanalyticallaboratoryandanalyzedseparatelywithidentical
procedures. Analysis of laboratory duplicates gives an indica-
4. Summary of Test Method
tionoftheprecisionassociatedwithlaboratoryprocedures,but
notwithsamplecollection,preservation,orstorageprocedures.
4.1 Volatile organic compounds with low water-solubility
3.2.6 laboratory-fortified blank—an aliquot of reagent are purged from the sample matrix by bubbling an inert gas
watertowhichknownquantitiesofthetestmethodanalytesare through the aqueous sample. Purged sample components are
added in the laboratory. The laboratory-fortified blank is trapped in a tube containing suitable sorbent materials. When
analyzed exactly like a sample, and its purpose is to determine purgingiscomplete,thesorbenttubeisheatedandbackflushed
whether the methodology is in control and whether the with inert gas to desorb the trapped sample components into a
laboratory is capable of making accurate and precise measure- capillary gas chromatography (GC) column interfaced to a
ments at the required detection limit. mass spectrometer (MS). The GC column is temperature
programmed to separate the test method analytes which are
3.2.7 laboratory-fortified sample matrix—an aliquot of an
then detected with the MS. Compounds eluting from the GC
environmental sample to which known quantities of the test
column are identified by comparing their measured mass
method analytes are added in the laboratory. The laboratory-
spectra and retention times to reference spectra and retention
fortified sample matrix is analyzed exactly like a sample, and
times in a database. Reference spectra and retention times for
itspurposeistodeterminewhetherornotthesamplematrixor
analytes are obtained by the measurement of calibration
the addition of preservatives or dechlorinating agents to the
standards under the same conditions used for the samples.The
sample contributes bias to the analytical results. The back-
concentration of each identified component is measured by
ground concentrations of the analytes in the sample matrix
relating the MS response of the quantitation ion produced by
must be determined in a separate aliquot, and the measured
that compound to the MS response of the quantitation ion
values in the laboratory-fortified sample matrix must be
produced by a compound that is used as an internal standard.
corrected for background concentrations.
Surrogate analytes, whose concentrations are known in every
3.2.8 laboratory performance check solution—a solution of
sample, are measured with the same internal standard calibra-
one or more compounds (analytes, surrogates, internal stan-
tion procedure.
dard, or other test compounds) used to evaluate the perfor-
manceoftheinstrumentsystemwithrespecttoadefinedsetof
5. Significance and Use
test method criteria.
3.2.9 laboratory reagent blank —an aliquot of reagent 5.1 Purgeable organic compounds have been identified as
water that is treated exactly as a sample including exposure to contaminants in treated drinking water, wastewater, ground
allglassware,equipment,solvents,reagents,internalstandards, water, andToxicity Characteristic Leaching Procedure (TCLP)
andsurrogatesthatareusedwithothersamples.Thelaboratory leachate. These contaminants may be harmful to the environ-
reagent blank is used to determine if test method analytes or ment and to people. Purge and trap sampling is a generally
other interferences are present in the laboratory environment, applicable procedure for concentrating these components prior
the reagents, or the apparatus. to gas chromatographic analysis.
3.2.10 primary dilution standard solution—a solution of
6. Interferences
severalanalytespreparedinthelaboratoryfromstockstandard
solutionsanddilutedasneededtopreparecalibrationsolutions
6.1 During analysis, major contaminant sources are volatile
and other needed analyte solutions.
materials in the laboratory and impurities in the inert purging
3.2.11 purgeable organic—any organic material that is
gas and in the sorbent trap. Avoid the use of plastic tubing or
removed from aqueous solution under the purging conditions
thread sealants other than PTFE, and avoid the use of flow
described in this test method.
controllers with rubber components in the purging device.
3.2.12 quality control sample—a sample matrix containing These materials out-gas organic compounds that will be
test method analytes or a solution of method analytes in a concentrated in the trap during the purge operation. Analyses
water-miscible solvent that is used to fortify reagent water or of laboratory reagent blanks provide information about the
environmental samples.The quality control sample is obtained presenceofcontaminants.Whenpotentialinterferingpeaksare
D 5790 – 95 (2001)
noted in laboratory reagent blanks, the analyst should change portionsofreagentwater.Afteranalysisofasamplecontaining
the purge gas source and regenerate the molecular sieve purge high concentrations of volatile organic compounds, one or
gas filter. Reagents should also be checked for the presence of
morelaboratoryreagentblanksshouldbeanalyzedtocheckfor
contaminants. Subtracting blank values from sample results is
cross contamination. After analyzing a highly contaminated
not permitted.
sample, it may be necessary to use methanol to clean the
6.2 Interfering contamination may occur when a sample
sample chamber, followed by heating in an oven at 105°C.
containinglowconcentrationsofvolatileorganiccompoundsis
6.3 Samples can be contaminated by diffusion of volatile
analyzed immediately after a sample containing higher con-
organics through the septum seal into the sample during
centrations of volatile organic compounds. Experience gained
shipment and storage. The analytical and sample storage area
from the test method validation has shown that there is a
should be isolated from all atmospheric sources of volatile
carryover of approximately 2% of the concentration of each
organic compounds, otherwise random background levels may
analyte from one sample to the next. The effect was observed
result. Since methylene chloride will permeate through PTFE
when samples containing 1 µg/L of analyte were analyzed
tubing, all gas chromatography carrier gas lines and purge gas
immediately after samples containing 20 µg/L of analyte. For
plumbing should be constructed of stainless steel or copper
that reason, when low concentrations of analytes are measured
tubing. Personnel who have been working directly with sol-
in a sample, it is very important to examine the results of the
vents such as those used in liquid/liquid extraction procedures
preceding samples and interpret the low-concentration results
accordingly.Onepreventivetechniqueisbetween-samplerins- should not be allowed into the analytical area until they have
ing of the purging apparatus and sample syringes with two washed and changed their clothing.
TABLE 1 Compounds Validated for This Test Method
Secondary Quantitation Approximate Elution
Compound CAS Registry Number Primary Quantitation Ion
Ion Order
Benzene 71-43-2 78 77 20
Bromobenzene 108-86-1 156 77, 158 44
Bromochloromethane 74-97-5 128 49, 130 16
Bromodichloromethane 75-27-4 83 85, 127 25
Bromoform 75-25-2 173 175, 252 41
Bromomethane 74-83-9 94 96 4
n-butylbenzene 104-51-8 91 134 57
sec-butylbenzene 135-98-8 105 134 53
tert-butylbenzene 98-06-6 119 91 52
Carbon disulfide 75-15-0 76 78 8
Carbon tetrachloride 56-23-5 117 119 19
Chlorobenzene 108-90-7 112 77, 114 35
Chloroethane 75-00-3 64 66 5
Chloroform 67-66-3 83 85 15
Chloromethane 74-87-3 50 52 2
2-chlorotoluene 95-49-8 91 126 47
4-chlorotoluene 106-43-4 91 126 50
Dibromochloromethane 124-48-1 129 127 33
1,2-dibromo-3-chloropropane 96-12-8 75 155, 157 60
1,2-dibromoethane 106-93-4 107 109, 188 34
Dibromomethane 74-95-3 93 95, 174 26
1,2-dichlorobenzene 95-50-1 146 111, 148 58
1,3-dichlorobenzene 541-73-1 146 111, 148 54
1,4-dichlorobenzene 106-46-7 146 111, 148 56
trans-1,4-dichloro-2-butene 110-57-6 75 53, 89 48
Dichlorodifluoromethane 75-71-8 85 87 1
1,1-dichloroethane 75-34-3 63 65, 83 11
1,2-dichloroethane 107-06-2 62 98 21
1,1-dichloroethene 75-35-4 96 61, 63 7
cis-1,2-dichloroethene 156-59-4 96 61, 98 13
trans-1,2-dichloroethene 156-60-5 96 61, 98 10
1,2-dichloropropane 78-87-5 63 112 24
1,3-dichloropropane 142-28-9 76 78 32
2,2-dichloropropane 590-20-7 77 97 12
1,1-dichloropropene 563-58-6 75 110, 77 18
cis-1,3-dichloro
...
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