Method 8315A Solids

Determination of Carbonyl Compounds by High Performance Liquid Chromatography (HPLC)


This method is for the determination of free carbonyl compounds (aldehydes and ketones) in solid  matrices by derivatization with 2,4-dinitrophenylhydrazine (DNPH).  Samples are analyzed using high performance liquid chromatography (HPLC) with ultraviolet/visible (UV/vis) detection.  This method replaces SW-846 Method 8315.

Approximately 25g of sample is leached with 500 mL of fluid.  Smaller sample sizes may be leached but the method says to use a ratio where the amount of fluid is 20 times the weight of the sample. A 100 mL portion of the resulting leachate is buffered to a pH of 3.0.  If the analysis is for formaldehyde only, the sample is buffered to a pH of 5.0.  The sample is then deriviatized with DNPH and analyzed.

Formaldehyde is a common contaminant of the DNPH reagent, therefore, the DNPH reagent should be checked on a regular basis for contamination.  The method allows <25 mg/L of the target analytes.  The DNPH reagents should be stored at 4°C, in the dark, with minimum headspace and the solutions may be stable for up to 6 weeks.

All samples should be shipped and stored at 4°C.  The method notes to keep the holding time of leachates from solids to a minimum but doesn't specify a 3 day holding time from collection until the derivatization/extraction of the sample as with aqueous samples.  All derivatized sample extracts should be analyzed within 3 days of the sample preparation.


(EPA SW-846)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   Leachates holding time must be kept at a minimum and analyzed within 3 days of derivatization.
Preservatives:   Cool to 4°C
Required Preps:   None specified in method.
Collection Method:   Grab sampling
Analytical Methodology:   HPLC with UV/Vis detection
Documentation:   8315A

Analyte List*

Analyte Formula CAS Number Detection Limit
Cyclohexanone
C6H10O
108-94-1
20
 µg/kg
Valeraldehyde (Pentanal)
C5H10O
110-62-3
20
 µg/kg
Glutaraldehyde
C5H8O2
111-30-8
20
 µg/kg
Heptylaldehyde (heptanal)
C7H14O
111-71-7
20
 µg/kg
Decaldehyde (decanal)
C10H20O
112-31-2
20
 µg/kg
Propionaldehyde (Propanal)
C3H6O
123-38-6
20
 µg/kg
Butyraldehyde (Butanal)
C4H8O
123-72-8
20
 µg/kg
Crotonaldehyde
C4H6O
123-73-9
20
 µg/kg
Octanal
C8H16O
124-13-0
20
 µg/kg
Nonanal
C9H18O
124-19-6
20
 µg/kg
Formaldehyde
CH2O
50-00-0
20
 µg/kg
m-Tolualdehyde
C8H8O
620-23-5
20
 µg/kg
Hexaldehyde (hexanal)
C6H12O
66-25-1
20
 µg/kg
Acetaldehyde
C2H4O
75-07-0
50
 µg/kg

* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.