EPA Method 1673

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EPA Method 1673:
PEG-600 by Derivatization and HPLC. Official Name: Poly(ethylene glycol)-600 by Derivatization and High-Pressure Liquid Chromatography

Summary:
One liter of aqueous sample is placed into a liquid-liquid extractor and a known quantity of surrogate is added. Extraction with dichloromethane is carried out over an 18-hour period. The dichloromethane extracts are dried over anhydrous sodium sulfate, evaporated to a small volume and dried again. Remaining dichloromethane is removed and the water-free extract is derivatized using 3,5-dinitrobenzoyl chloride and pyridine in tetrahydrofuran. The tetrahydrofuran solution is diluted with diethyl ether, extracted to remove side products, evaporated, and solvent exchanged with acetonitrile/water and chromatographed on a reverse-phase C18 column with a solvent gradient of 40 percent acetonitrile/water to 100 percent acetonitrile. Detection is performed at 254 nm. The PEG-600 derivative is identified by its retention time relative to that of the derivatized surrogate and quantified by external standard techniques.

Scope:
This method is applicable to determining PEG-600 in aqueous samples specific to the pharmaceutical manufacturing industry.

Citation:
Analytical Methods for the Determination of Pollutants in Pharmaceutical Manufacturing Industry Wastewater, EPA 821-B-94-001 (Contains 1600-series methods)

Interferences:
(1) Method interferences caused by contaminants in solvents, reagents, glassware, and other sample processing hardware that lead to discrete artifacts and/or elevated baselines in chromatograms. (2) Matrix interferences caused by contaminants coextracted from the sample.

QC Requirements:
calibration verification (CV), initial precision and recovery (IPR), reagent blank (RB), ongoing precision and recovery (OPR)

Maximum Holding Time:
5 days (prior to extraction)

Media:
WATER

Subcategory:
Organic

Precision:
-

Detection:
The ML reported is the minimum level at which the entire analytical system shall give a recognizable signal and an acceptable calibration point.

Revision Number:
Jan-95