DOE Test Method OP130R

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View Actual DOE Method OP130R (PDF File)


Source:
DOE

Method Name:
TCLP for Semivolatiles and Pesticides. Official Name: Analysis of TCLP Semivolatiles and Pesticides in Radioactive Mixed Waste Sludges

Description:
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:
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.

Citation:
DOE Methods

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.

QC Requirements:
Lab control, reagent blanks, MS with each batch.

Media:
OTHER

Subcategory:
Organic

Concentration:
None given.

Precision:
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:
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 Number:
1997



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