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ASTM D5315-04

(Test Method)

Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization

Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization

SIGNIFICANCE AND USE
N-methylcarbamates and n-methylcarbomoyloximes are used in agriculture as insecticides and herbicides. They are sometimes found in both surface and ground waters and can be toxic to animals and plants at moderate to high concentrations. The manufacturing precursors and degradation products may be equally as hazardous to the environment.
SCOPE
1.1 This is a high-performance liquid chromatographic (HPLC) test method applicable to the determination of certain n-methylcarbamoyloximes and n-methylcarbamates in ground water and finished drinking water  (). This test method is applicable to any carbamate analyte that can be hydrolyzed to a primary amine. The following compounds have been validated using this test method:AnalyteChemical Abstract Services Registry Number  Aldicarb 116-06-3 Aldicarb sulfone 1646-88-4 Aldicarb sulfoxide 1646-87-3 Baygon 114-26-1 Carbaryl 63-25-2 Carbofuran 1563-66-2 3-Hydroxycarbofuran 16655-82-6 Methiocarb 2032-65-7 Methomyl 16752-77-5 Oxamyl 23135-22-0 Numbering system of Chemical Abstracts, Inc.
1.2 This test method has been validated in a collaborative round-robin study () and estimated detection limits (EDLs) have been determined for the analytes listed in (). Observed detection limits may vary between ground waters, depending on the nature of interferences in the sample matrix and the specific instrumentation used.
1.3 This test method is restricted to use by, or under the supervision of, analysts experienced in both the use of liquid chromatography and the interpretation of liquid chromatograms. Each analyst should demonstrate an ability to generate acceptable results with this test method using the procedure described in .
1.4 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in , analyte identifications should be confirmed by at least one additional qualitative technique.

General Information

Status
Historical
Publication Date
31-May-2004
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D5315-92(1998) - Standard Test Method for N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization
Effective Date
01-Jun-2004
Replaced By
ASTM D5315-04(2011) - Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization
Effective Date
01-May-2011
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
01-Jun-2004

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ASTM D5315-04 - Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column DerivatizationASTM D5315-04 - Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization
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ASTM D5315-04 - Standard Test Method for Determination of N-Methyl-Carbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-Column Derivatization
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Standards Content (Sample)

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
Designation: D5315 – 04
Standard Test Method for
Determination of N-Methyl-Carbamoyloximes and
N-Methylcarbamates in Water by Direct Aqueous Injection
1
HPLC with Post-Column Derivatization
This standard is issued under the fixed designation D5315; 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 (´) indicates an editorial change since the last revision or reapproval.
TABLE 1 Relative Retention Times for the Primary and
1. Scope
Confirmation Columns and EDLs for the 10 Carbamate
1.1 This is a high-performance liquid chromatographic
Pesticides
(HPLC) test method applicable to the determination of certain
Retention Time (minutes)
n-methylcarbamoyloximes and n-methylcarbamates in ground Analyte
A B C
Primary Confirmation EDL
2
water and finished drinking water (1) . This test method is
Aldicarb 27.0 21.4 1.0
applicable to any carbamate analyte that can be hydrolyzed to
Aldicarb sulfone 15.2 12.2 2.0
a primary amine. The following compounds have been vali-
Aldicarb sulfoxide 15.0 17.5 2.0
Baygon (Propoxur) 29.6 23.4 1.0
dated using this test method:
Carbaryl 30.8 25.4 2.0
Chemical Abstract Services
Carbofuran 29.3 24.4 1.5
A
Analyte Registry Number
3-Hydroxycarbofuran 23.3 19.0 2.0
Aldicarb 116-06-3
Methiocarb 34.9 28.6 4.0
Aldicarb sulfone 1646-88-4
Methomyl 18.4 14.8 0.50
Aldicarb sulfoxide 1646-87-3
Oxamyl 17.4 14.6 2.0
Baygon 114-26-1
A
Primary column—250 by 4.6 mm inside diameter Altex Ultrasphere ODS, 5
Carbaryl 63-25-2
µm.
Carbofuran 1563-66-2
B
Confirmation column—250 by 4.6 mm inside diameter Supelco LC-1, 5 µm.
3-Hydroxycarbofuran 16655-82-6
C
Estimated method detection limit in micrograms per litre.
Methiocarb 2032-65-7
Methomyl 16752-77-5
Oxamyl 23135-22-0
1.4 When this test method is used to analyze unfamiliar
________________
samples for any or all of the analytes listed in 1.1, analyte
A
Numbering system of Chemical Abstracts, Inc.
identifications should be confirmed by at least one additional
1.2 This test method has been validated in a collaborative
qualitative technique.
round-robin study (2) and estimated detection limits (EDLs)
1.5 The values stated in SI units are to be regarded as the
have been determined for the analytes listed in 1.1 (Table 1).
standard.
Observed detection limits may vary between ground waters,
1.6 This standard does not purport to address all of the
depending on the nature of interferences in the sample matrix
safety concerns, if any, associated with its use. It is the
and the specific instrumentation used.
responsibility of the user of this standard to establish appro-
1.3 This test method is restricted to use by, or under the
priate safety and health practices and determine the applica-
supervision of, analysts experienced in both the use of liquid
bility of regulatory limitations prior to use. Additional guid-
chromatography and the interpretation of liquid chromato-
ance on laboratory safety is available and suitable references
grams. Each analyst should demonstrate an ability to generate
for the information are provided (3-5).
acceptable results with this test method using the procedure
described in 12.3.
2. Referenced Documents
3
2.1 ASTM Standards:
1 D1129 Terminology Relating to Water
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved June 1, 2004. Published June 2004. Originally
3
approved in 1992. Last previous edition approved in 1998 as D5315–92 (1998). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D5315-04. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to the references at the end of this Standards volume information, refer to the standard’s Document Summary page on
test method. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D5315 – 04
D1192 GuideforEquipmentforSamplingWaterandSteam analytes are added in the laboratory. The LFB is analyzed
4
in Closed Conduits exactly as a sample is; its purpose is to determine whether the
D1193 Specification for Reagent Water methodology is in control and whether the laboratory is
D2777 Practice for Determination of Precision and Bias of capableofmakingaccurateandprecisemethodsattherequired
Applicable Test Methods of Committee D19 on Water
test method detection limit.
D3370 Practices for Sampling Water from Closed Conduits
3.2.7 laboratory-fortified sample matrix (LFM)—an aliquot
D3694 Practices fo
...

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