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 4^oC 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

This method has 12 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
(E)-Crotonaldehyde(123-73-9) (E)-Crotonaldehyde 2-Butenal, (E)- 2-Crotonaldehyde Crotonaldehyde, (E) trans-Crotonaldehyde	5.900 ug/L	N/A	34.80 RSD (ML)	160.00 ug/L
Acetaldehyde(75-07-0) Acetaldehyde	110.200 ug/L	N/A	N/A
Butanal(123-72-8) Butanal Butyraldehyde	7.800 ug/L	N/A	22.70 RSD (ML)	160.00 ug/L
Cyclohexanone(108-94-1) Cyclohexanone	6.900 ug/L	N/A	39.20 RSD (ML)	160.00 ug/L
Decanal(112-31-2) Decanal	13.100 ug/L	N/A	40.00 RSD (ML)	160.00 ug/L
Formaldehyde(50-00-0) Formaldehyde	23.200 ug/L	N/A	30.50 RSD (ML)	160.00 ug/L
Heptanal(111-71-7) Heptanal	6.600 ug/L	N/A	N/A
Hexanal(66-25-1) Hexaldehyde Hexanal	12.400 ug/L	N/A	34.60 RSD (ML)	160.00 ug/L
Nonanal(124-19-6) Nonanal	7.400 ug/L	N/A	N/A
Octanal(124-13-0) Octanal	9.900 ug/L	N/A	40.10 RSD (ML)	160.00 ug/L
Pentanal(110-62-3) Pentanal Valeraldehyde	13.400 ug/L	N/A	N/A
Propanal(123-38-6) Propanal Propionaldehyde	8.400 ug/L	N/A	22.40 RSD (ML)	160.00 ug/L

Precision Descriptor Notes:	Procedure 1, was tested by 12 laboratories using organic-free reagent water and ground waters spiked at six concentrations over the range 30-2200 ug/L. Method accuracy and precision were found to be directly related to the concentration of the analyte and independent of the sample matrix. Mean recovery weighted linear regression equations, calculated as a function of spike concentration, as well as overall and single-analyst precision regression equations, calculated as functions of mean recovery, are presented in Table 5. These equations can be used to estimate mean recovery and precision at any concentration value within the range tested.
Detection Level Note:	The MDL for a specific sample may differ from the listed value, depending upon the interferences in the sample matrix and the volume of sample used in the procedure. With the exception of acetaldehyde, all reported MDLs are based upon analyses of 6 to 8 replicate blanks spiked at 25 ug/L. Values are also based on the liquid-liquid extraction (method also provides liquid-solid extraction performance criteria as well as air sample analysis data)

Precision Descriptor Notes:

Procedure 1, was tested by 12 laboratories using organic-free reagent water and ground waters spiked at six concentrations over the range 30-2200 ug/L. Method accuracy and precision were found to be directly related to the concentration of the analyte and independent of the sample matrix. Mean recovery weighted linear regression equations, calculated as a function of spike concentration, as well as overall and single-analyst precision regression equations, calculated as functions of mean recovery, are presented in Table 5. These equations can be used to estimate mean recovery and precision at any concentration value within the range tested.

Detection Level Note:

The MDL for a specific sample may differ from the listed value, depending upon the interferences in the sample matrix and the volume of sample used in the procedure. With the exception of acetaldehyde, all reported MDLs are based upon analyses of 6 to 8 replicate blanks spiked at 25 ug/L. Values are also based on the liquid-liquid extraction (method also provides liquid-solid extraction performance criteria as well as air sample analysis data)

Revision	PDF/Link
Revision 1, December 1996

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

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