EPA-NERL: 506:  Phthalate and Adipate Esters in Water by GCPID

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Determination of Phthalate and Adipate Esters in Drinking Water by Liquid-Liquid Extraction or Liquid Solid Extraction and Gas Chromatography with Photoionization Detection
Current Revision
Revision 1.1, 1995
Media
WATER
Instrumentation
Gas Chromatography with Photoionization Detection
Method Subcategory
Organic
Method Source
  EPA-NERL
Citation
  Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)
Brief Method Summary
Samples are extracted using liquid/liquid extraction (LLE) or liquid/solid extraction (LSE). For LLE, a 1-L sample is extracted with methylene chloride followed by hexane using a glass separatory funnel, and the final extract is dried and reduced to a to a volume of 1-mL. For LSE a measured volume of sample is extracted with a LSE cartridge or disk, and eluted using acetonitrile and methylene chloride (or pure methylene chloride), and the eluent/extract is reduced to a volume of 1-mL. The concentrations of esters in the extracts are measured using a gas chromatography (GC) system equipped with a photoionization detector (PID).
Scope and Application
This method determines certain phthalate and adipate esters in drinking water.
Applicable Concentration Range
Ranges differ for each analyte depending on matrix and instrumentation.
Interferences

(A) Phthalate ester interference: Avoid the use of plastics and use pure reagents to avoid contamination by these ubiquitous compounds.

(B) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.

(C) Reagent contamination: Use high purity reagents.

(D) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by cleaning the extract.

(E) Variable solvents: Use the same solvent for each analysis.

Quality Control Requirements
Initial demonstration of laboratory capability, followed by analysis of laboratory reagent blanks (LRB), laboratory fortified blanks (LFB), laboratory fortified sample matrix (LFM), and quality control samples (QCS). A MDL for each analyte must also be determined. Additional quality control practices are recommended.
Sample Handling
Grab samples must be collected in amber glass containers. Conventional sampling practices should be followed; however, the bottle must not be pre-rinsed with sample prior to collection. Add 80 mg of sodium thiosulfate for dechlorination to the sample bottle at the sampling site or in the laboratory prior to shipping to the sampling site. After sample is collected, seal the bottle and swirl until the sodium thiosulfate is dissolved. Samples must be iced or refrigerated at 4oC free from light from the time of collection until extraction.
Maximum Holding Time
Samples must be extracted within 14 days. Extracts can be held for an additional 14 days prior to analysis.
Relative Cost
$201 to $400
Sample Preparation Methods