ASTM: D5475: Nitrogen and Phosphorus-Containing Pesticides
- Summary
- Analytes
- Revision
- Data and Sites
Official Method Name
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Standard Test Method for Nitrogen- and Phosphorus-Containing Pesticides in Water by Gas Chromatography with a Nitrogen-Phosphorus Detector | ||||
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Current Revision
| Reapproved 1997. Current edition approved Dec. 15, 1993. Published March 1994. | ||||
Media
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WATER | ||||
Instrumentation
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Gas Chromatography with Nitrogen - Phosphorus Detection | ||||
Method Subcategory
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Organic | ||||
Method Source
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ASTM
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Citation
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Annual Book of ASTM Standards, Section 11, Water and Environmental Technology, Volume 11.02, Water (I)
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Brief Method Summary
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A measured volume of sample of approximately 1 L is extracted with methylene chloride by shaking in a separatory funnel or mechanical tumbling in a bottle. The methylene chloride extract is isolated, water is removed, and concentrated to a volume of 5 mL during a solvent exchange to methyl tert-butyl ether (MTBE). Chromatographic conditions are described that permit the separation and measurement of the analytes in the extract by capillary column GC with a nitrogen-phosphorus detector (NPD). | ||||
Scope and Application
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This is a gas chromatographic (GC) test method applicable to the determination of certain nitrogen- and phosphorus-containing pesticides in ground water and finished drinking water. The analytes listed in Table 1 have been validated using this test method. This test method has been validated on reagent water and finished drinking water by 10 volunteer laboratories. | ||||
Applicable Concentration Range
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Varies with the analytes listed ug/L | ||||
Interferences
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Test method interferences may be caused by contaminants in solvents, reagents, glassware, and other sample processing apparatus that lead to discrete artifacts or elevated baselines in gas chromatograms. All reagents and apparatus must be routinely demonstrated to be free from interferences under the conditions of the analysis by running laboratory reagent blanks as described in Section 12.2. | ||||
Quality Control Requirements
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Recommended quality control (QC) requirements are initial demonstration of laboratory capability, determination of surrogate compound recoveries in each sample and blank, monitoring internal standard peak area or height in each sample and blank (when internal standard calibration procedures are being employed), analysis of laboratory reagent blanks, laboratory fortified samples, laboratory fortified blanks, and QC samples. | ||||
Sample Handling
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Collect the samples in accordance with Practices D 3370, D 3694, and Specification D 1192. Instructions Specific to This Test Method - Grab samples must be collected in glass containers. Conventional sampling Practices D 3370 should be followed; however, the bottle must not be prerinsed with sample before collection. 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 preservative(s), seal the bottle and shake vigorously for 1 min. Ice or refrigerate the samples at 4oC away from light from the time of collection until extraction. Preservation study results indicated that most test method analytes present in samples were stable for 14 days when stored under these conditions. The analytes disulfoton sulfoxide, diazinon, pronamide, and terbufos exhibited significant aqueous instability, and samples to be analyzed for these compounds must be extracted immediately. The analytes carboxin, EPTC, fluridone, metolachlor, napropamide, tebuthiuron, and terbacil exhibited recoveries of less than 60 % after 14 days. Analyte stability may be affected by the matrix; therefore, the analyst should verify that the preservation technique is applicable to the samples under study. |
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Maximum Holding Time
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14 days | ||||
Relative Cost
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$201 to $400 | ||||
Sample Preparation Methods
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This method has 48 analytes associated with it.
Analyte | Detection Level |
Bias | Precision | Pct False Positive |
Pct False Negative |
Spiking Level |
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Alachlor(15972-60-8)
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0.380 ug/L | 93% Rec (ML) | 16.90 % RSD (ML) | 5.00 ug/L | ||
Ametryn(834-12-8)
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2.000 ug/L | 94% Rec (ML) | 15.10 % RSD (ML) | 2.00 ug/L | ||
Atrazine(1912-24-9)
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0.130 ug/L | 93% Rec (ML) | 14.50 % RSD (ML) | 2.00 ug/L | ||
Bromacil(314-40-9)
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2.500 ug/L | 96% Rec (ML) | 16.70 % RSD (ML) | 10.00 ug/L | ||
Butachlor(23184-66-9)
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0.380 ug/L | 94% Rec (ML) | 15.50 % RSD (ML) | 10.00 ug/L | ||
Butylate(2008-41-5)
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0.150 ug/L | 76% Rec (ML) | 23.40 % RSD (ML) | 5.00 ug/L | ||
Carbamate pesticides(E-12895)
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N/A | N/A | N/A | |||
Carboxin(5234-68-4)
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0.600 ug/L | 80% Rec (ML) | 21.40 % RSD (ML) | 10.00 ug/L | ||
Chlorpropham(101-21-3)
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0.500 ug/L | 98% Rec (ML) | 18.20 % RSD (ML) | 10.00 ug/L | ||
Cycloate(1134-23-2)
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0.250 ug/L | 56% Rec (ML) | 19.50 % RSD (ML) | 5.00 ug/L | ||
Diazinon(333-41-5)
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0.250 ug/L | 89% Rec (ML) | 19.20 % RSD (ML) | 2.00 ug/L | ||
Dichlorvos(62-73-7)
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2.500 ug/L | 100% Rec (ML) | 15.60 % RSD (ML) | 5.00 ug/L | ||
Diphenamid(957-51-7)
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0.600 ug/L | 94% Rec (ML) | 15.90 % RSD (ML) | 5.00 ug/L | ||
Disulfoton(298-04-4)
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0.300 ug/L | 86% Rec (ML) | 19.00 % RSD (ML) | 2.00 ug/L | ||
Disulfoton sulfone(2497-06-5)
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3.800 ug/L | 104% Rec (ML) | 21.70 % RSD (ML) | 10.00 ug/L | ||
Ethion(563-12-2)
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0.250 ug/L | 86% Rec (ML) | 18.70 % RSD (ML) | 2.00 ug/L | ||
Ethoprophos(13194-48-4)
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0.190 ug/L | 92% Rec (ML) | 20.20 % RSD (ML) | 2.00 ug/L | ||
Fenamiphos(22224-92-6)
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1.000 ug/L | 90% Rec (ML) | 19.50 % RSD (ML) | 20.00 ug/L | ||
Fenarimol(60168-88-9)
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0.380 ug/L | 97% Rec (ML) | 22.40 % RSD (ML) | 5.00 ug/L | ||
Fluridone(59756-60-4)
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3.800 ug/L | 102% Rec (ML) | 24.20 % RSD (ML) | 10.00 ug/L | ||
Herbicides(E-12839)
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N/A | N/A | N/A | |||
Hexazinone(51235-04-2)
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0.760 ug/L | 99% Rec (ML) | 21.30 % RSD (ML) | 5.00 ug/L | ||
MGK 264(113-48-4)
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0.500 ug/L | 93% Rec (ML) | 18.00 % RSD (ML) | 10.00 ug/L | ||
Merphos(150-50-5)
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0.250 ug/L | 50% Rec (ML) | 36.40 % RSD (ML) | 10.00 ug/L | ||
Methylparaoxon(950-35-6)
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2.500 ug/L | 100% Rec (ML) | 17.20 % RSD (ML) | 10.00 ug/L | ||
Metolachlor(51218-45-2)
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0.750 ug/L | 93% Rec (ML) | 13.20 % RSD (ML) | 10.00 ug/L | ||
Metribuzin(21087-64-9)
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0.150 ug/L | 97% Rec (ML) | 19.80 % RSD (ML) | 2.00 ug/L | ||
Mevinphos(7786-34-7)
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5.000 ug/L | 97% Rec (ML) | 13.20 % RSD (ML) | 10.00 ug/L | ||
Molinate(2212-67-1)
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0.150 ug/L | 94% Rec (ML) | 18.20 % RSD (ML) | 2.00 ug/L | ||
Napropamide(15299-99-7)
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0.250 ug/L | 87% Rec (ML) | 15.70 % RSD (ML) | 5.00 ug/L | ||
Norflurazon(27314-13-2)
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0.500 ug/L | 96% Rec (ML) | 24.80 % RSD (ML) | 5.00 ug/L | ||
Organophosphate pesticides(E-12873)
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N/A | N/A | N/A | |||
Oxydisulfoton(2497-07-6)
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0.380 ug/L | 95% Rec (ML) | 19.50 % RSD (ML) | 10.00 ug/L | ||
Pebulate(1114-71-2)
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0.130 ug/L | 89% Rec (ML) | 21.80 % RSD (ML) | 2.00 ug/L | ||
Prometon(1610-18-0)
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0.300 ug/L | 96% Rec (ML) | 17.20 % RSD (ML) | 2.00 ug/L | ||
Pronamide(23950-58-5)
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0.760 ug/L | 97% Rec (ML) | 15.20 % RSD (ML) | 10.00 ug/L | ||
Propazine(139-40-2)
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0.130 ug/L | 93% Rec (ML) | 17.20 % RSD (ML) | 2.00 ug/L | ||
Simazine(122-34-9)
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0.075 ug/L | 95% Rec (ML) | 14.60 % RSD (ML) | 2.00 ug/L | ||
Simetryn(1014-70-6)
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0.250 ug/L | 96% Rec (ML) | 18.00 % RSD (ML) | 2.00 ug/L | ||
Tebuthiuron(34014-18-1)
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1.300 ug/L | 97% Rec (ML) | 18.40 % RSD (ML) | 10.00 ug/L | ||
Terbacil(5902-51-2)
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4.500 ug/L | 100% Rec (ML) | 18.80 % RSD (ML) | 50.00 ug/L | ||
Terbufos(13071-79-9)
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0.500 ug/L | 83% Rec (ML) | 18.10 % RSD (ML) | 10.00 ug/L | ||
Terbutryn(886-50-0)
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0.250 ug/L | 95% Rec (ML) | 12.80 % RSD (ML) | 2.00 ug/L | ||
Tetrachlorvinphos(22248-79-9)
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0.760 ug/L | 93% Rec (ML) | 20.90 % RSD (ML) | 20.00 ug/L | ||
Triadimefon(43121-43-3)
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0.650 ug/L | 98% Rec (ML) | 20.30 % RSD (ML) | 2.00 ug/L | ||
Tricyclazole(41814-78-2)
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1.000 ug/L | 91% Rec (ML) | 16.30 % RSD (ML) | 20.00 ug/L | ||
Vernolate(1929-77-7)
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0.130 ug/L | 81% Rec (ML) | 25.40 % RSD (ML) | 2.00 ug/L | ||
bis(2-Chloroethyl) ether(111-44-4)
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0.600 ug/L | 94% Rec (ML) | 17.30 % RSD (ML) | 5.00 ug/L |
Precision Descriptor Notes: | Ten laboratories participated in the study. Two samples, different in concentration of the 45 analytes, were analyzed as Youden pairs at each of 3 levels to provide data for estimating single-analyst precision. Analyses of the spiked reagent water evaluated the proficiency of the test method on a sample free of interferences. Analyses of the spiked finished drinking waters were intended to demonstrate the suitability of the test method on a regulated matrix and to compare the results with those of reagent water. |
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Detection Level Note: | None. |
Revision | PDF/Link |
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Reapproved 1997. Current edition approved Dec. 15, 1993. Published March 1994. |
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