Method 531.1

Measurment of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post Column Derivatization


This method is for the determinations of certain N-methylcarbamoyloximes and N-methylcarbamates in ground water and finished drinking water.  The water sample is filtered and a 400 µL aliquot is injected into a reverse phase HPLC column.  The analytes are separated using gradient elution chromatography.  After elution from the HPLC column, the analytes are hydrolyzed with 0.05 N sodium hydroxide (NaOH) at 95°C.  The methyl amine formed during hydrolysis is reacted with o-phthalaldehyde (OPA) and 2-mercaptoethanol to form a highly fluorescent derivative which is detected by a fluorescence detector.


(EPA: Office of Water)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   28 days from collection to analysis to analysis if samples are properly preserved.
Preservatives:   Samples must be preserved at pH ≤ 3. Add 1.8 mL of monochloroacetic acid buffer per 60mL prior to collection. Add 80 mg of sodium thiosulfate/L prior to collection if residual chlorine is present. Samples must be iced or refrigerated at 4°C from the time of collection to analysis.
Required Preps:   60mL Amber glass bottle with Teflon-lined cap.
Collection Method:   Grab sampling
Analytical Methodology:   HPLC with fluorescence detection
Documentation:   531.1

Analyte List*

Analyte Formula CAS Number Detection Limit
Propoxur (Baygon)
C11H15NO3
114-26-1
0.5
 µg/L
Aldicarb (Temic)
C7H14N2O2S
116-06-3
0.5
 µg/L
Carbofuran
C12H15NO3
1563-66-2
0.5
 µg/L
Aldicarb Sulfoxide
C7H14N2O3S
1646-87-3
0.5
 µg/L
Aldicarb sulfone
C7H14N2O4S
1646-88-4
0.5
 µg/L
3-Hydroxycarbofuran
C12H15NO4
16655-82-6
0.5
 µg/L
Methomyl (Lannate)
C6H12N2O3S
16752-77-5
0.5
 µg/L
Methiocarb (Mesurol)
C11H15NO2S
2032-65-7
0.5
 µg/L
Oxamyl (Vydate)
C7H13N3O3S
23135-22-0
0.5
 µg/L
Carbaryl (Sevin)
C12H11NO2
63-25-2
0.5
 µg/L

* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.