DOE: OP130R: TCLP for Semivolatiles and Pesticides

Summary
Analytes
Revision
Data and Sites

Official Method Name

Analysis of TCLP Semivolatiles and Pesticides in Radioactive Mixed Waste Sludges

Current Revision

1997

Media

OTHER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

DOE

Citation

DOE Methods

Brief Method Summary

A sample is extracted three times with methylene chloride. The solvent extracts are pooled and concentrated. The concentrations of SVOCs in the concentrate are determined using a capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).

Scope and Application

This method determines Toxicity Characteristic Leach Procedure (TCLP) semivolatile organic compounds (SVOCs) and pesticides in radioactive mixed waste (RMW) sludges. No acidic SVOCs are determined.

Applicable Concentration Range

None given.

Interferences

(1) Contamination of samples, solvent, and carrier gases with target analytes (especially compounds common to environmental laboratories, like methylene chloride).
(2) Contamination of samples with sulfur (primarily present in base-neutral fractions).
(3) Septum bleed (compounds from the injection septum are analyzed with the sample).
(4) Column bleed (compounds from column coating break down, decreasing column efficiency).
(5) Ghost peaks (compounds adsorb strongly to the column and carry over to later runs).
(6) Coelution of species.
(7) Coextracted contaminants.
(8) Phthalate esters interfere with detection of pesticides via electron capture detector.

Quality Control Requirements

Lab control, reagent blanks, MS with each batch.

Sample Handling

Follow all applicable radiochemical laboratory procedures and health physics monitoring practices, to ensure that the DOE ALARA principle is performed. Sample collection, preservation, and handling should be addressed in the planning process.

Maximum Holding Time

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 16 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1,4-Dichlorobenzene(106-46-7) 1,4-Dichlorobenzene Benzene, 1,4-dichloro- Chlorinated benzenes, mono- and di- Di-chloricide PDB Paramoth p-Dichlorobenzene para-dichlorobenzene	1.970 ug/g	89% Rec (SL)	N/A	10.00 ug/g
2,4-Dinitrotoluene(121-14-2) 1-Methyl-2,4-dinitrobenzene 2,4-DNT 2,4-Dinitrotoluene 2,4-Dinitrotoluol Benzene, 1-methyl-2,4-dinitro Benzene,2-methyl-2,4-dinitro- Dinitrobenzene,1-methyl-2,4- Dinitrotoluene, 2,4 Methyl-2,4-dinitrobenzene,1- Toluene, 2,4-dinitro-	0.010 ug/g	108% Rec (SL)	N/A	0.04 ug/g
Chlordane(57-74-9) Chlordane Chlordane, .alpha.,.beta., and .gamma. isomers Chlorindan Compound K (FDA) Corodane Octachloro-4,7-methanotetrahydroindane Toxichlor Velsicol 1068	0.120 ug/g	93% Rec (SL)	N/A	0.60 ug/g
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	0.020 ug/g	109% Rec (SL)	N/A	0.04 ug/g
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	0.030 ug/g	105% Rec (SL)	N/A	0.04 ug/g
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.030 ug/g	85% Rec (SL)	N/A	0.04 ug/g
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.020 ug/g	101% Rec (SL)	N/A	0.04 ug/g
Hexachlorobutadiene(87-68-3) 1,3-Butadiene, 1,1,2,3,4,4-hexachloro- Butadiene,hexachloro-1,3- Hexachloro-1,3-butadiene Hexachlorobutadiene Perchlorobutadiene	0.030 ug/g	85% Rec (SL)	N/A	0.04 ug/g
Hexachloroethane(67-72-1) 1,1,1,2,2,2-Hexachloroethane Carbon hexachloride Ethane hexachloride Ethane, hexachloro- Hexachlorethane Hexachloroethane Perchloroethane Phenohep	0.030 ug/g	83% Rec (SL)	N/A	0.04 ug/g
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	0.030 ug/g	79% Rec (SL)	N/A	0.04 ug/g
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	0.010 ug/g	109% Rec (SL)	N/A	0.04 ug/g
Nitrobenzene(98-95-3) Benzene, nitro- EPA Pesticide Chemical Code 056501 Essence of mirbane Essence of myrbane Mirbane oil Mononitrobenzene Nitrobenzene Nitrobenzol Oil of mirbane Oil of myrbane RCRA waste number U169	0.020 ug/g	40% Rec (SL)	N/A	0.04 ug/g
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
Toxaphene(8001-35-2) Alltox Camphechlor Camphechlor, Camphene, octachloro- Camphochlor Estonox Geniphene Phenacide Phenatox Polychlorocamphene Toxaphene Toxaphene ( Technical chlorinated camphene (67-69% ...	1.620 ug/g	85% Rec (SL)	N/A	10.00 ug/g
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A

Precision Descriptor Notes:	Precision and accuracy were determined by making 3-5 replicate analyses of sand spiked with the analytes of interest. Additional precision and accuracy data from the analysis of different matrices are available in Section 10 of the method.
Detection Level Note:	DLs were calculated according to : Hubaux, A. and G. Vos. 1970. "Decision and Detection Limits for Linear Calibration Curves." Anal. Chem., 42:849-855. DL for chlordane was calculated using first eluting peak.

Revision	PDF/Link
1997

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DOE: OP130R: TCLP for Semivolatiles and Pesticides

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