USGS-NWQL: O-3106-93: Triazines in Water by Gas Chromatography

Summary
Analytes
Revision
Data and Sites

Official Method Name

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography with Nitr.-Phos. Detectors

Current Revision

1994

Media

WATER

Instrumentation

Gas Chromatography with Nitrogen - Phosphorus Detection

Method Subcategory

Organic

Method Source

USGS-NWQL

Citation

Markovchick, D.J., Lewis, J.A., Brenton, R.W., Iverson, J.L.,and Wharry, H.L., 1994, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of triazine and other nitrogen-containing compounds by gas chromatography with nitrogen phosphorous detectors: U.S. Geological Survey Open-File Report 94-037.

Brief Method Summary

The pH of a measured volume (about 1 L) of sample is adjusted to range from 7.0 to 9.0. Then 50 g of NaCl is added and dissolved. The sample is extracted with methylene chloride. The methylene chloride extract is isolated, dried, and concentrated to a volume of 1 mL during a solvent exchange to methyl-t-butyl ether (MTBE). Chromatographic conditions are described that permit the separation and determination of the compounds in the extract by capillary column GC with a nitrogen phosphorus detector (NPD).

Scope and Application

This method is suitable for the determination of triazine herbicides and other selected nitrogen-containing compounds in water and mixtures of water-suspended sediment.

Applicable Concentration Range

0.1 - 5.0 (undiluted)

Interferences

Method interferences might 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 need to be routinely demonstrated to be free from interferences under the conditions of the analysis by running laboratory reagent blanks. The use of ultrapure solvents and reagents will help to minimize interference problems. System contamination might interfere when a sample containing small concentrations of compounds is analyzed immediately following a sample containing large concentrations of compounds. After a sample is injected, the syringe is rinsed 10 times with solvent to reduce the chance of cross-contamination. Matrix interferences might be caused by contaminants that are coextracted from the sample. The extent of matrix interferences will vary from source to source, depending on the water sampled. This potential problem is addressed using a dual column confirmation procedure. If there are further questions about compound identification, the sample is submitted for confirmation using gas chromatography/mass spectrometry (GC/MS). It is important that samples and calibration standards be contained in the same solvent. If this is not the case, chromatographic comparability of standards to sample might be affected.

Quality Control Requirements

Quality-control samples area analyzed at a minimum of one in every ten samples. These QC samples include at least one of each of the following: blanks, quality control samples, third party check solutions, replicates, and spikes. Correlation coefficients for calibration curves must be at least 0.99. QC samples must fall within 1.5 standard deviations of the mean value. If all of the data-acceptance criteria in the SOPs are met, then the analytical data are acceptable.

Sample Handling

This schedule consumes the entire sample. Description: 1 L Glass bottle, amber bottle baked at 450^oC by laboratory. Chill sample and maintain at 4^oC, ship immediately.

Maximum Holding Time

7 days from arrival at the lab

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 25 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Alachlor(15972-60-8) 2-Chloro-N-(2,6-diethylphenyl)-N-(methoxymethy Acetanilide,2-chloro-2',6'-diethyl-n-(methoxymethyl)- Alachlor Alanex Lasso Metachlor Methachlor	0.200 ug/L	83% Rec (SL)	13.00 % RSD (SL)	1.00 ug/L
Ametryn(834-12-8) 2-Ethylamino-4-isopropylamino-6-methylthio-s-t 2-Ethylamino-4-isopropylamino-6-methylthio-s-triazine 2-Ethylamino-4-isopropylamino-6-methylthio-s-trizaine Ametryn Ametryn (ANSI) Ametryn (N-Ethyl-N'-(1-methylethyl)-6-(methylthio)-1 ... Ametryne Cemerin Evik Gesapax	0.100 ug/L	92% Rec (SL)	2.30 % RSD (SL)	0.89 ug/L
Atrazine(1912-24-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N-ethyl-N'-(1- ... 2-Chloro-4-(ethylamino)-6-(isopropylamino)-S-triazine 2-Chloro-4-(ethylamino)-6-(isopropylamino)-s-t 2-Chloro-4-ethylamino-6-isopropylamine-sym-triazine AAtrex Atratol 8P Atrazine Atrazine (ANSI) Bicep	0.100 ug/L	90% Rec (SL)	2.30 % RSD (SL)	1.00 ug/L
Bromacil(314-40-9) 5-Bromo-3-sec-butyl-6-methyluracil Borea Bromacil Bromacil (ANSI) Bromax Hyvar Uragon Urox "B" Urox 'B'	0.200 ug/L	50% Rec (SL)	7.00 % RSD (SL)	1.00 ug/L
Butachlor(23184-66-9) 2-Chloro-2',6'-diethyl-N-(butoxymethyl)acetanilide Acetamide, N-(butoxymethyl)-2-chloro-N-(2,6-di Acetanilide,2-chloro-2',6'-diethyl-n-(butoxymethyl)- Butachlor Butachlor (ANSI) Butanox Hiltachlor Machete N-(Butoxymethyl)-2-chloro-N-(2,6-diethylphenyl)acetamide N-(butoxymethyl)-2-chloro-2',6'-diethyl acetan N-(butoxymethyl)-2-chloro-2',6'-diethyl acetanilide	0.100 ug/L	93% Rec (SL)	13.00 % RSD (SL)	1.00 ug/L
Butylate(2008-41-5) Anelda Butylate Carbamic acid, diisobutylthio-, S-ethyl ester Carbamothioic acid, bis(2-methylpropyl)-, S-et Carbamothioic acid, bis(2-methylpropyl)-, S-ethyl ester Diisocarb S-Ethyl diisobutylthiocarbamate S-Ethyldiisobutyl thiocarbamate Sutan bis(2-Methylpropyl)carbamothioate-S-ethyl n,n-Diisobutylthiocarbamate-Ethyl	0.100 ug/L	64% Rec (SL)	5.00 % RSD (SL)	1.20 ug/L
Carboxin(5234-68-4) 2,3-Dihydro-6-methyl-1,4-oxathiin-5-carboxanil 2,3-Dihydro-6-methyl-1,4-oxathiin-5-carboxanilide 5,6-Dihydro-2-methyl-1,4-oxathiin-3-carboxanalide Carbathiin Carboxin Carboxin (5,6-Dihydro-2-methyl-N-phenyl-1,4-oxathiin ... Fenoxan Vitavax	0.200 ug/L	82% Rec (SL)	2.90 % RSD (SL)	1.10 ug/L
Cyanazine(21725-46-2) 2-((4-Chloro-6-(ethylamino)-1,3,5-triazin-2-yl)amino)-2-methylpropanenitrile 2-((4-Chloro-6-(ethylamino)-s-triazin-2-yl)amino)-2-methylpropionitrile Bladex Cyanazine Fortrol Payze	0.200 ug/L	94% Rec (SL)	13.00 % RSD (SL)	1.00 ug/L
Cycloate(1134-23-2) Carbamothioic acid, cyclohexylethyl-, S-ethyl Carbamothioic acid, cyclohexylethyl-, S-ethyl ester Cycloate Cyclohexanecarbamic acid,n-ethylthio-, s-ethyl ester Etsan Etsan, Eurex Eurex Hexylthiocarbam N-ethylthiocyclohexanecarbamic acid, s-ethyl ester Ro-Neet S-Ethyl N-cyclohexyl-N-ethylthiocarbamate S-Ethyl cyclohexylethylthiocarbamate S-Ethyl-N-cyclohexyl-N-ethylthiocarbamate Sabet	0.100 ug/L	70% Rec (SL)	3.60 % RSD (SL)	6.30 ug/L
Desethylatrazine(6190-65-4) 1,3,5-Triazine-2,4-diamine, 6-chloro-N-(1-methylethyl)- (9CI) 2-Amino-4-chloro-6-(isopropylamino)-s-triazine 2-Chloro-4-amino-6-isopropylamino-1,3,5-triazine 2-Chloro-4-amino-6-isopropylamino-s-triazine 2-Chloro-4-isopropylamino-6-amino-s-triazine Atrazine-desethyl Chloroaminoisopropylaminotriazine DEA Deethylatratone Desethylatrazine s-Triazine, 2-amino-4-chloro-6-(isopropylamino)- (6CI,7CI,8CI)	0.200 ug/L	73% Rec (SL)	2.30 % RSD (SL)	1.40 ug/L
Desisopropylatrazine(1007-28-9) 2-Amino-4-chloro-6-(ethylamino)-s-triazine 2-Chloro-4-amino-6-(ethylamino)-s-triazine 2-Chloro-4-ethylamino-6-amino-1,3,5-triazine 2-Chloro-4-ethylamino-6-amino-s-triazine 4-Amino-2-chloro-6-(ethylamino)-s-triazine 4-Amino-2-chloro-6-ethylamino-1,3,5-triazine Atrazine-desisopropyl DIA Deethylsimazine Deisopropylatrazine Desisopropylatrazine F703 G 28279 NSC 13909 s-Triazine, 2-amino-4-chloro-6-(ethylamino)- (6CI,7CI,8CI)	0.200 ug/L	40% Rec (SL)	1.30 % RSD (SL)	0.91 ug/L
Diphenamid(957-51-7) 2,2-Diphenyl-N,N-dimethylacetamide Acetamide,n,n-dimethyl-2,2-diphenyl Benzeneacetamide, N,N-dimethyl-.alpha.-phenyl- Diherbid Dimid, Dymid Diphenamid Diphenamid (ANSI) Dymid Enide N,N-Dimethyl-2,2-diphenylacetamide N,N-Dimethyldiphenylacetamide Rideon	0.100 ug/L	91% Rec (SL)	2.50 % RSD (SL)	0.98 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Hexazinone(51235-04-2) 1,3,5-Triazine-2,4(1H,3H)-dione, 3-cyclohexyl- 1,3,5-Triazine-2,4(1H,3H)-dione, 3-cyclohexyl-6-(di ... 3-Cyclohexyl-6-(dimethylamino)-1-methyl-1,3,5- ... 3-Cyclohexyl-6-(dimethylamino)-1-methyl-s-tria 3-Cyclohexyl-6-(dimethylamino)-1-methyl-s-triazine-2 ... Cyclohexyl-6-(dimethylamino)-1-methyl-1,3,5-triazine ... Cyclohexyl-6-(dimethylamino)-1-methyl-s-triazine-2,4 ... Hexazinone Velpar	0.200 ug/L	53% Rec (SL)	6.90 % RSD (SL)	1.00 ug/L
Metolachlor(51218-45-2) 2-Chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-4- ... 2-Chloro-N-(6-ethyl-o-tolyl)-N-(2-methoxy-1- ... 2-chloro-6'-ethyl-N-(2-methoxy-1-methylethyl)-o- ... Acetamide, 2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2- ... Codal Cycle Dual Metelilachlor Metolachlor Metolachlor (ANSI)	0.200 ug/L	86% Rec (SL)	9.30 % RSD (SL)	1.20 ug/L
Metribuzin(21087-64-9) 4-Amino-6-(1,1-dimethylethyl)-3-(methylthio)-1 Bay 94337 Lexone Metribuzin Sencoral Sencorer	0.100 ug/L	90% Rec (SL)	12.00 % RSD (SL)	1.10 ug/L
Prometon(1610-18-0) 2,4-bis(Isopropylamino)-6-methoxy-S-triazine 2,4-bis(Isopropylamino)-6-methoxy-sym-triazine 2,6-Diisopropylamino-4-methoxytriazine Gesafram 50 Methoxypropazine Pramitol Prometon Prometon (ANSI) Prometon(pramitol) Prometone	0.200 ug/L	84% Rec (SL)	9.10 % RSD (SL)	1.00 ug/L
Prometryn(7287-19-6) 1,3,5-Triazine-2,4-diamine, N,N'-bis(1-methyle 1,3,5-Triazine-2,4-diamine, N,N'-bis(1-methylethyl)- ... 2,4-bis(Isopropylamino)-6-(methylthio)-S-triazine 2,4-bis(Isopropylamino)-6-methylthio-sym-triazine Caparol Gesagard Gesagard, Gesagaro Primatol Q Prometrin, Prometryn (ANSI), Prometryne Prometryn Prometryn (N,N'-Bis(1-methylethyl)-6-methylthio-1,3, ... Selectin Uvon	0.100 ug/L	91% Rec (SL)	3.10 % RSD (SL)	1.10 ug/L
Propachlor(1918-16-7) 2-Chloro-N-isopropylacetanilide 2-Chloro-n-isopropyl-n-phenylacetamide Acetamide, 2-chloro-N-(1-methylethyl)-N-phenyl Acetamide, 2-chloro-N-(1-methylethyl)-N-phenyl- Bexton Propachlor Propachlore Ramrod	0.100 ug/L	82% Rec (SL)	2.60 % RSD (SL)	0.84 ug/L
Propazine(139-40-2) 1,3,5-Triazine-2,4-diamine, 6-chloro-N,N'-bis( 2-Chloro-4,6-bis(isopropylamino)-S-triazine Chloro-4,6-bis(isopropylamino)-sym-triazine,2- Gesamil Milocep Milogard Primatol P Propasin Propazine Propazine (ANSI)	0.100 ug/L	95% Rec (SL)	14.00 % RSD (SL)	1.00 ug/L
Simazine(122-34-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N,N'-diethyl- 2,4-bis(Ethylamino)-6-chloro-s-triazine 2-Chloro-4,6-bis(ethylamino)-1,3,5-triazine 2-Chloro-4,6-bis(ethylamino)-S-triazine 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diami 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diamine Aquazine Princep Radocon S-Triazine,2-chloro-4,6-bis(ethylamino)- Simadex, Simanex, Simazine (ANSI) Simazine	0.100 ug/L	92% Rec (SL)	1.60 % RSD (SL)	1.00 ug/L
Simetryn(1014-70-6) 1,3,5-Triazine-2,4-diamine, N,N'-diethyl-6-(me 1,3,5-Triazine-2,4-diamine, N,N'-diethyl-6-(methylthio)- 2,4-Bis(ethylamino)-6-(methylthio)-s-triazine 2,4-bis(Ethylamino)-6-methylmercapto-s-triazine Simetryn	0.100 ug/L	89% Rec (SL)	1.60 % RSD (SL)	1.20 ug/L
Terbacil(5902-51-2) 2,4(1H,3H)-Pyrimidinedione, 5-chloro-3-(1,1-di 2,4(1H,3H)-Pyrimidinedione, 5-chloro-3-(1,1-dimethyl ... 3-tert-Butyl-5-chloro-6-methyluracil 3-tert-Butyl-s-chloro-6-methyluracil 5-Chloro-3-(1,1-dimethylethyl)-6-methyl- 2 ... Geonter Sinbar Terbacil Turbacil	0.200 ug/L	75% Rec (SL)	8.10 % RSD (SL)	1.20 ug/L
Trifluralin(1582-09-8) Commence Dinitro-n,n-dipropyl-4-(trimethylfluoro)benzenamine,2,6- Treflan Trifluoralin, Trifluraline Trifluralin Triflurex p-Toluidine, alpha, alpha, alpha-trifluoro-2,6	0.100 ug/L	76% Rec (SL)	14.00 % RSD (SL)	1.00 ug/L
Vernolate(1929-77-7) Carbamothioic acid, dipropyl-, S-propyl ester PPTC Propyl-n,n-dipropylthiocarbamate S-Propyl dipropylthiocarbamate S-Propyldipropylthiocarbamate Vernam Vernolate	0.100 ug/L	66% Rec (SL)	14.00 % RSD (SL)	1.20 ug/L

Precision Descriptor Notes:	Recoveries are adequate for alachlor, ametryn, atrazine, butachlor, carboxin, cyanazine, cycloate, desethylatrazine, diphenamid, metolachlor, metribuzin, prometon, prometryn, propachlor, propazine, simazine, simetryn, terbacil, and trifluralin. The recoveries of bromacil and hexazinone were marginal in the reagent-water matrix, but adequate for both the surface-water and ground-water matrices. Vernolate and butylate recoveries were marginal from all three matrices. Recoveries generally were in the 60-percent range for both compounds. Vernolate recoveries ranged from 59 to 73 percent. The recovery of desisopropylatrazine ranged from 39 to 42 percent in all three water matrices. Requests for bromacil, butylate, desisopropylatrazine, hexazinone, and vernolate need to be made with the understanding that recoveries for these compounds are less than ideal.
Detection Level Note:	Method detection limits (MDLs) were determined for this method using the procedures of the U.S. Environmental Protection Agency (1997).

Precision Descriptor Notes:

Recoveries are adequate for alachlor, ametryn, atrazine, butachlor, carboxin, cyanazine, cycloate, desethylatrazine, diphenamid, metolachlor, metribuzin, prometon, prometryn, propachlor, propazine, simazine, simetryn, terbacil, and trifluralin. The recoveries of bromacil and hexazinone were marginal in the reagent-water matrix, but adequate for both the surface-water and ground-water matrices. Vernolate and butylate recoveries were marginal from all three matrices. Recoveries generally were in the 60-percent range for both compounds. Vernolate recoveries ranged from 59 to 73 percent. The recovery of desisopropylatrazine ranged from 39 to 42 percent in all three water matrices. Requests for bromacil, butylate, desisopropylatrazine, hexazinone, and vernolate need to be made with the understanding that recoveries for these compounds are less than ideal.

Detection Level Note:

Method detection limits (MDLs) were determined for this method using the procedures of the U.S. Environmental Protection Agency (1997).

Revision	PDF/Link
1994

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USGS-NWQL: O-3106-93: Triazines in Water by Gas Chromatography

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