EPA: 8315A:  Carbonyl Compounds in Water by HPLC and UV/vis

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Method 8315A: Dinitrophenylhydrazine Derivatization and High Performance Liquid Chromatography
Current Revision
Revision 1, December 1996
Media
WATER
Instrumentation
High Performance Liquid Chromatography with Ultraviolet Detection
Method Subcategory
Inorganic
Method Source
  EPA
Citation
  U.S. Environmental Protection, 1996, Method 8315A: Dinitrophenylhydrazine Derivatization and High Performance Liquid Chromatography. Revision 1 December 1996, 34 p.
Brief Method Summary
Liquid and Solid Samples (Use Procedure 1) 2.1.1 For wastes comprised of solids, and aqueous wastes containing greater than one percent solid material, the aqueous phase should be separated from the solid phase and stored, according to Sec. 6.2, for possible later analysis. If necessary, the particle size of the solids in the waste is reduced. The solid phase is extracted with a volume of fluid equal to 20 times the sample's weight. The extraction fluid employed is a function of the alkalinity of the solid phase of the waste. A special extractor is used when volatiles are being extracted. Following extraction, the extract is filtered through a 0.6 - 0.8 um glass fiber filter. 2.1.2 If compatible (i.e., multiple phases will not form on combination), the initial aqueous phase of the waste is added to the aqueous extract, and these liquids are analyzed together. If incompatible, the liquids are analyzed separately and the results are mathematically combined to yield a volume-weighted average concentration. 2.1.3 A measured volume of aqueous sample (approx. 100 mL) or an appropriate amount of solids extract (approx. 25 g), is buffered to pH 3 and derivatized with 2,4-dinitrophenylhydrazine (DNPH), using either the appropriate solid-phase or a liquid-liquid extraction technique. If the solid-phase extraction (SPE) option is used, the derivatized compound is extracted using solid sorbent cartridges, then eluted with ethanol. If the liquid-liquid option is used, the derivatized compound is serially extracted three (3) times with methylene chloride. The methylene chloride extracts are concentrated using the appropriate procedure 3500 series method and exchanged with acetonitrile prior to HPLC analysis. HPLC conditions are described which permit the separation and measurement of various carbonyl compounds in the extract by absorbance detection at 360 nm. 2.1.4 If formaldehyde is the only analyte of interest, the aqueous sample and/or solid sample extract should be buffered to pH 5.0 to minimize the formation of artifact formaldehyde.
Scope and Application
This method provides procedures for the determination of free carbonyl compounds in various matrices by derivatization with 2,4-dinitrophenylhydrazine (DNPH). The method utilizes high performance liquid chromatography (HPLC) with ultraviolet/visible (UV/vis) detection to identify and quantitate the target analytes. This method includes two procedures encompassing all aspects of the analysis (extraction to determination of concentration). The method described in NEMI is for water samples.
Applicable Concentration Range
50-1000
Interferences
Acetaldehyde is generated during the derivatization step if ethanol is present in the sample. This background will impair the measurement of acetaldehyde levels below 0.5 ppm (500 ppb). Method interferences may be caused by contaminated solvents, reagents, glassware, and other sample processing hardware which can lead to discrete artifacts and/or elevated chromatogram baselines. All materials should routinely demonstrate freedom from interferences under analysis conditions by analyzing laboratory reagent blanks as described in Sec. 8.5.
Quality Control Requirements
Laboratory QC proceedures should be part of its formal quality assurance program.
Sample Handling
All samples should be iced or refrigerated at 4oC from the time of collection until extraction.
Maximum Holding Time
3 or 30 days, depending on matrix and sample collection method.
Relative Cost
Less than $50
Sample Preparation Methods