EPA Method 7580


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EPA Method 7580:
White Phosphorus in water, soil, and sediment by GC/NPD . Official Name: White Phosphorus (P4) by Solvent Extraction and Gas Chromatography

Summary:
Method 7580 may be used to determine the concentration of white phosphorus in soil, sediment, and water samples using solvent extraction and gas chromatography (GC). Water samples are extracted by one of two procedures, depending on the sensitivity required. For the more sensitive procedure, a 500-mL water sample is extracted with 50 mL of diethyl ether. The extract is concentrated by back extraction with reagent water, yielding a final extract volume of approximately 1.0 mL. A 1.0 uL aliquot of this extract is injected into a GC equipped with a nitrogen-phosphorus detector (NPD). This procedure provides sensitivity on the order of 0.01 ug/L. Wet soil or sediment samples are analyzed by extracting a 40 g wet-weight aliquot of the sample with a mixture of 10.0 mL degassed reagent water and 10.0 mL isooctane. The extraction is performed in a glass jar on a platform shaker for 18 hours. A 1.0 uL aliquot of the extract is analyzed by GC-NPD, providing sensitivity on the order of 1 ug/kg.

Scope:
Trace analysis of white phosphorous (P4) in water, soil,and sediment samples.

Citation:
SW-846 Online: Test Methods for Evaluating Solid Waste, Physical/Chemical Methods

Interferences:
To date, no chromatographic interferences with this determination have been reported, in part due to the selectivity of the nitrogen-phosphorus detector. This procedure offers several advantages compared to other procedures described in the literature which determine P4 by converting it to phosphate, in that background concentrations of phosphate are quite common in many water and sediment samples.

QC Requirements:
Initial demonstration of laboratory capability and an ongoing analysis of spiked samples to evaluate and document data quality. 10 extracts, the injection of the tenth extract, the mid-point calibration standard must be injected to verify the calibration.

Maximum Holding Time:
5 days suggested

Media:
WATER

Subcategory:
Inorganic

Precision:
Performance data and detection levels shown are for water samples. To date, only single laboratory performance data have been generated. Those data indicate that there may be problems with the recovery of P4 from soils containing high concentrations of metals. Therefore, laboratories employing this method are encouraged to develop in-house performance data including MDLs and accuracy and precision data for routinely encountered matrices. These data should be developed in accordance with the procedures outlined in Method 8000.

Detection:
This method includes two different extraction procedures for water samples. The first procedure provides sensitivity on the order of 0.01 µg/L, and may be used to assess compliance with Federal water quality criteria. The second procedure provides sensitivity on the order of 0.1 µg/L. The method includes one procedure for the extraction of soil/sediment samples which provides sensitivity on the order of 1 µg/kg.

Revision Number:
Dec-96

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