ASTM: D5175: Organohalide Pesticides and PCBs in Water

Summary
Analytes
Revision
Data and Sites

Official Method Name

Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography

Current Revision

Reapproved 1996. Current edition approved Sept. 15, 1991. Published February 1992.

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture 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

This is a microextraction method in which 35 mL of sample are extracted with 2 mL of hexane. Two mL of the extract are injected into a gas chromatograph equipped with a linearized electron capture detector for separation and analysis. Aqueous calibration standards are extracted and analyzed in an identical manner to compensate for possible extraction losses. The extraction and analysis time is 30 to 50 min per sample depending upon the analytes and the analytical conditions chosen.
This test method is based largely on EPA Method 505.

Scope and Application

This test method is applicable to the determination of certain PCBs and organohalides in finished drinking water, drinking water during intermediate stages of treatment, and the raw source water.

Applicable Concentration Range

< 1 to 50 ug/L with the exception of toxaphene (5.6 to 70 ug/L)

Interferences

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 12.2.
Phthalate esters, frequently found in plastics, paints, and other common laboratory items, produce a positive response on an electron capture detector.
Interfering contamination may occur when a sample containing low concentrations of analytes is analyzed immediately following a sample containing relatively high concentrations of analytes.
Matrix interferences may be caused by contaminants that are coextracted from the sample. Also, note that all the analytes listed in the scope are not resolved from each other on any one column; one analyte of interest may be an interferent for another analyte of interest.
Caution must be taken in the determination of endrin since it has been reported that the splitless injector may cause endrin degradation. The analyst should be alerted to this possible interference resulting in an erratic response for endrin.
Variable amounts of pesticides and PCBs from aqueous solutions adhere to glass surfaces.
Aldrin and methoxychlor are rapidly oxidized by chlorine. Dechlorination with sodium thiosulfate at time of collection will retard further oxidation of these compounds.
An interfering, erratic peak has been observed within the retention window of heptachlor during many analyses of reagent, tap, and groundwater. It appears to be related to dibutyl phthalate; however, the specific source has not yet been determined. The observed magnitude and character of this peak randomly vary in numerical value from successive injections made from the same vial. This type of outlying observation normally is recognized.

Quality Control Requirements

Minimum quality control requirements are initial demonstration of laboratory capability, analysis of laboratory reagent blanks (LRB), laboratory fortified blanks (LFB), laboratory fortified sample matrix (LFM), and, if available, quality control samples (QCS). For a general discussion of good laboratory practices, see Guide D 3856 and Practice D 4210.

Sample Handling

Collect all samples in 40-mL vials into which 3 mg of sodium thiosulfate crystals have been added to the empty bottles just prior to shipping to the sampling site. Alternately, 75 mL of freshly prepared sodium thiosulfate solution (0.04 g/mL) may be added to empty 40-mL vials just prior to sample collection. In collecting field samples, add sodium thiosulfate solution at the sampling site.
When sampling from a water tap, open the tap and allow the system to flush until the water temperature has stabilized (usually about 10 min). Adjust the flow to about 500 mL/min and collect samples from the flowing stream.
When sampling from a well, fill a wide-mouth bottle or beaker with sample and carefully fill 40-mL sample vials.
Sample Preservation - The samples must be chilled to 4^oC at the time of collection and maintained at that temperature until the analyst is prepared for the extraction process. Field samples that will not be received at the laboratory on the day of collection must be packaged for shipment with sufficient ice to ensure they will be maintained at 4^oC until arrival at the laboratory.

Maximum Holding Time

14 days.

Relative Cost

Unknown

Sample Preparation Methods

This method has 14 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Aldrin(309-00-2) Aldrex Aldrin Aldrin-R Aldrite Aldrosol HHDN Hexachlorohexahydro-endo-exo-dimethanonaphthalene Octalene Seedrin liquid	0.040 ug/L	93% Rec (ML)	25.10 % RSD (ML)	0.10 ug/L
Chlordane(57-74-9) Chlordane Chlordane, .alpha.,.beta., and .gamma. isomers Chlorindan Compound K (FDA) Corodane Octachloro-4,7-methanotetrahydroindane Toxichlor Velsicol 1068	0.510 ug/L	90% Rec (ML)	31.50 % RSD (ML)	1.00 ug/L
Dieldrin(60-57-1) 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6 1,2,3,4,10,10-Hexachloro-6,7-epoxy-1,4,4a,5, 6,7,8, ... 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6 2,7:3,6-Dimethanonaphth(2,3-b)oxirene, 3,4,5,6,9,9- ... Alvit Dieldrin Dieldrin (hexachloroepoxyoctahydro-endo,exo- ... Dieldrin/aldrin Dimethanonaphthalene, 1,2,3,4,10,10-hexachloro-6,7- ... Heod Octalox	0.100 ug/L	97% Rec (ML)	21.90 % RSD (ML)	1.00 ug/L
Endrin(72-20-8) 2,7:3,6-Dimethanonaphth[2,3-b]oxirene, 3,4,5,6,9,9- ... 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-oct 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-octahydro ... Compound 269 Endrin Hexachloroepoxyoctahydro-endo,endo-dimethanonaphthalene Hexadrin Mendrin Nendrin	0.100 ug/L	103% Rec (ML)	15.40 % RSD (ML)	1.00 ug/L
Heptachlor(76-44-8) 1,4,5,6,7,8,8-Heptachlorotetrahydro-4,7-methanoindene Drinox Heptachlor Heptachlor [1,4,5,6,7,8,8-heptachloro-3a,4,7,7a- ... Heptachlor/Heptachlor epoxide (SARA 110) Heptachlorodicyclopentadiene Heptagran Heptamul Velsicol-104	0.040 ug/L	98% Rec (ML)	40.60 % RSD (ML)	0.10 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.040 ug/L	101% Rec (ML)	32.70 % RSD (ML)	0.10 ug/L
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.010 ug/L	100% Rec (ML)	23.10 % RSD (ML)	0.10 ug/L
Lindane(58-89-9) Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha, 2- ... HCH-gamma Hexachlorocyclohexane (gamma) Lindane Lindane ( gamma isomer of benzene hexachloride ) (99 ... gamma-BHC gamma-Benzenehexachloride gamma-HCH gamma-Hcch gamma-Hexachlorocyclohexane	0.040 ug/L	100% Rec (ML)	14.10 % RSD (ML)	0.10 ug/L
Methoxychlor(72-43-5) 1,1'-(2,2,2-Trichloroethylidene)bis[4-methoxybenzene] 1,1,1-Trichloro-2,2-bis(4-methoxyphenyl)ethane Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-methoxy- Dimethoxy DDT Ethane, 1,1,1-trichloro-2,2-bis(p-methoxypheny Ethane, 1,1,1-trichloro-2,2-bis(p-methoxyphenyl)- Marlate Methoxcide Methoxychlor Metox p,p'-Methoxychlor p,p'DMDT	0.200 ug/L	90% Rec (ML)	33.20 % RSD (ML)	1.00 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
PCB-1016(12674-11-2) Aroclor 1016 PCB-1016	0.500 ug/L	111% Rec (ML)	19.00 % RSD (ML)	10.00 ug/L
PCB-1254(11097-69-1) Arochlor 1254 Aroclor 1254 PCB-1254	0.500 ug/L	113% Rec (ML)	28.70 % RSD (ML)	10.00 ug/L
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	5.630 ug/L	89% Rec (ML)	20.10 % RSD (ML)	10.00 ug/L

Precision Descriptor Notes:	This test method has been tested by ten laboratories using reagent water and ground water spiked at six concentration levels as three Youden pairs. Single operator precision, overall precision, and test method bias were found to be directly related to the concentration of the analyte and virtually independent of the sample matrix. Linear equations to describe the relationships are presented in Table 1.
Detection Level Note:	None.

Precision Descriptor Notes:

This test method has been tested by ten laboratories using reagent water and ground water spiked at six concentration levels as three Youden pairs. Single operator precision, overall precision, and test method bias were found to be directly related to the concentration of the analyte and virtually independent of the sample matrix. Linear equations to describe the relationships are presented in Table 1.

Detection Level Note:

None.

Revision	PDF/Link
Reapproved 1996. Current edition approved Sept. 15, 1991. Published February 1992.

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ASTM: D5175: Organohalide Pesticides and PCBs in Water

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