ASTM: D5315: Standard Test Method for Carbamates in Water

Summary
Analytes
Revision
Data and Sites

Official Method Name

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

Current Revision

Reapproved 1998. Current edition approved Oct. 15, 1992. Published December 1992.

Media

WATER

Instrumentation

High Performance Chromatography with Post Column Derivitization and Fluorescence Detection

Method Subcategory

Organic

Method Source

ASTM

Citation

Annual Book of ASTM Standards, Section 11, Water and Environmental Technology, Volume 11.02, Water (I)

Brief Method Summary

The water sample is filtered, and a 200 to 400-mL aliquot is injected into a reverse phase HPLC column. Separation of the analytes is achieved using gradient elution chromatography. After elution from the HPLC column, the analytes are hydrolyzed with sodium hydroxide (2.0 g/L NaOH) at 95^oC. The methylamine formed during hydrolysis is reacted with o-phthalaldehyde (OPA) and 2-mercaptoethanol to form a highly fluorescent derivative that is detected by a fluorescence detector .

Scope and Application

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.

Applicable Concentration Range

Varies with analyte. Generally from < 10 ug/L

Interferences

Test method interferences may be caused by contaminants in solvents, reagents, glassware, and other sample processing apparatuses that lead to discrete artifacts or elevated baselines in liquid chromatograms. Specific sources of contamination have not been identified. All reagents and apparatus must be routinely demonstrated to be free of interferences under the analysis conditions by running laboratory reagent blanks in accordance with 12.2. Glassware must be cleaned scrupulously. The use of high-purity reagents and solvents helps to minimize interference problems. Purification of solvents by distillation in all-glass systems may be required.
Interfering contamination may occur when a sample containing low concentrations of analytes is analyzed immediately after a sample containing relatively high concentrations of analytes. A preventive technique is between-sample rinsing of the sample syringe and filter holder with two portions of water. Analyze one or more laboratory method blanks after analysis of a sample containing high concentrations of analytes.
Matrix interference may be caused by contaminants present in the sample. The extent of matrix interference will vary considerably from source to source, depending upon the water sampled. Positive identifications must be confirmed.

Quality Control Requirements

Minimum quality control (QC) requirements are as follows: an initial demonstration of laboratory capability; monitoring of the internal standard peak area or height in each sample and blank when internal standard calibration procedures are being used; and an analysis of laboratory reagent blanks, laboratory-fortified samples, laboratory-fortified blanks, and quality control samples.

Sample Handling

Collect the samples in accordance with Specification D 1192, Practices D 3370, or Practices D 3694. Additionally, grab samples must be collected in glass containers. Follow conventional sampling practices; however, the bottle must not be prerinsed with sample before collection.
Oxamyl, 3-hydroxycarbofuran, aldicarb sulfoxide, and carbaryl can all degrade rapidly in neutral and basic waters held at room temperature. This short-term degradation is of concern during the periods of time that samples are being shipped and that processed samples are held at room temperature in autosampler trays. Samples targeted for the analysis of these three analytes must be preserved at a pH of 3, as shown as follows. The pH adjustment also minimizes analyte biodegradation. Add 1.8 mL of monochloroacetic acid buffer solution (pH 3) to the 60-mL sample bottle. Add buffer to the sample bottle either at the sampling site or in the laboratory before shipping to the sampling site.
If residual chlorine is present, add 80 mg of sodium thiosulfate per litre of sample to the sample bottle prior to collecting the sample. After the sample is collected in a bottle containing buffer, seal the sample bottle and shake it vigorously for 1 min. Samples must be iced or refrigerated at 4^oC from the time of collection until storage; they must be stored at - 10^oC until analyzed.

Maximum Holding Time

28 days at pH 3 and - 10^oC.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 11 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
3-Hydroxycarbofuran(16655-82-6) 3,7-Benzofurandiol, 2,3-dihydro-2,2-dimethyl-, 3-Hydroxycarbofuran	2.000 ug/L	104% Rec (ML)	6.50 % RSD (ML)	20.00 ug/L
Aldicarb(116-06-3) 2-Methyl-2-(methylthio)propanal, O-((methylamino)carbonyl)oxime Aldicarb Carbanolate Temik UC-21149	1.000 ug/L	105% Rec (ML)	5.80 % RSD (ML)	10.00 ug/L
Aldicarb sulfone(1646-88-4) Aldicarb sulfone Aldicarb sulfone, wh Aldoxycarb Aldoxycarb (ANSI) Standak Sulfocarb Temik sulfone	2.000 ug/L	104% Rec (ML)	6.70 % RSD (ML)	20.00 ug/L
Aldicarb sulfoxide(1646-87-3) 2-Methyl-2-(methylsulfinyl)propanal O-((methylamino)carbonyl)oxime Aldicarb sulfoxide Temik sulfoxide	2.000 ug/L	104% Rec (ML)	6.80 % RSD (ML)	20.00 ug/L
Carbamate pesticides(E-12895) Carbamate pesticides Carbamate pesticides, N-methyl- N-methyl carbamate pesticides	N/A	N/A	N/A
Carbaryl(63-25-2) 1-Naphthyl methylcarbamate 1-Naphthyl-N-methylcarbamate Carbamic acid, methyl-, 1-naphthyl ester Carbaril Carbaryl Carbaryl (ANSI) Carbaryl [1-naphthalenol, methylcarbamate] Sevimol Sevin	2.000 ug/L	99% Rec (ML)	6.80 % RSD (ML)	20.00 ug/L
Carbofuran(1563-66-2) 2,3-Dihydro-2,2-dimethyl-7-benzofuranyl methylcarbamate Carbofuran Carbofuran (ANSI) Dihydro-2,2-dimethyl-7-benzofuranyl methylcarbamate,2,3- Euradan Furadan	1.500 ug/L	105% Rec (ML)	3.40 % RSD (ML)	20.00 ug/L
Methiocarb(2032-65-7) 3,5-Dimethyl-4-(methylthio)phenol methylcarbamate 4-(Methylthio)-3,5-xylyl methylcarbamate Carbamic acid, methyl-, 4-(methylthio)-3,5-xyl Carbamic acid, methyl-, 4-(methylthio)-3,5-xylyl ester Mercaptodimethur Mesurol Methiocarb Phenol, 3,5-dimethyl-4-(methylthio)-, methylca Phenol, 3,5-dimethyl-4-(methylthio)-, methylcarbamate	4.000 ug/L	106% Rec (ML)	7.90 % RSD (ML)	50.00 ug/L
Methomyl(16752-77-5) Acetamidic acid, thio-N-[(methyl-carbamoyl)oxy Acetamidic acid, thio-N-[(methyl-carbamoyl)oxy]-, ... Dupont 1179 Insecticide 1179 Lannate Methomyl S-methyl-n-((methylcarbamoyl)oxy)thioacetimidate	0.500 ug/L	102% Rec (ML)	7.40 % RSD (ML)	5.00 ug/L
Oxamyl(23135-22-0) 2-o-Methylcarbamoyl monoxime DPX 1410 Oxamyl Thioxamyl Vydate Vydate L	2.000 ug/L	103% Rec (ML)	7.20 % RSD (ML)	20.00 ug/L
Propoxur(114-26-1) 2-Isopropoxyphenyl-n-methylcarbamate Aprocarb Baygon Blattenex Isocarb N-methyl-2-isopropoxyphenylcarbamate Phenol, 2-(1-methylethoxy)-, methylcarbamate Propoxur Propoxur [phenol, 2-(1-methylethoxy)-, methylcarbamate] Sendran, Suncide Unden o-Isopropoxyphenyl methylcarbamate	1.000 ug/L	105% Rec (ML)	7.80 % RSD (ML)	10.00 ug/L

Precision Descriptor Notes:	Eight laboratories participated in the study. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. Reagent and finished drinking water were spiked with the 12 analytes, each at six concentration levels, prepared as three Youden pairs. Analyses of the spiked reagent water evaluated the proficiency of this test method on a sample free from interferences. Analyses of the spiked finished drinking water allowed an analysis of variance test. Only Aldicarb sulfoxide was affected by sample matrix.
Detection Level Note:	None.

Precision Descriptor Notes:

Eight laboratories participated in the study. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. Reagent and finished drinking water were spiked with the 12 analytes, each at six concentration levels, prepared as three Youden pairs. Analyses of the spiked reagent water evaluated the proficiency of this test method on a sample free from interferences. Analyses of the spiked finished drinking water allowed an analysis of variance test. Only Aldicarb sulfoxide was affected by sample matrix.

Detection Level Note:

None.

Revision	PDF/Link
Reapproved 1998. Current edition approved Oct. 15, 1992. Published December 1992.

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ASTM: D5315: Standard Test Method for Carbamates in Water

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