Method 5021A/8260B

Headspace Analysis for Volatile Organic Compounds by GC/MS


Method 5021 is a general purpose method for the preparation of volatile organic compounds (VOCs) purged into the headspace of soil/sediment and solid waste matrices and analyzed by GC/MS following Method 8260B procedures.  The method is applicable to a wide range of VOCs having high volatility.  A high volatility is required to effectively removethe VOCs from soil and solid matrices.

Typically, a 2 gram sample size is spiked with surrogate standards and allowed to equilibrate within the matrix at room temperature.  It is important to spike the standards into the sample prior to extracting the VOCs into the headspace.  The surrogate standards will give a measure of the efficiency of volatilizing the compounds.  The method does allow for the use of a matrix modifying solution to help preserve the samples but use of this solution is not required.  One hour prior to analysis the sample should be moved to the heated zone of the headspace analyzer.  The method does require collection and analysis of a field blank.

Samples that are high in oil content or organic sludge wastes will inhibit the partitioning of the VOCs into the headspace giving low surrogate recoveries.  Additionally, absorption potential of the soil, biological activity of the soil, and the soil composition may also affect the partitioning ability.

Once the VOCs are partitioned into the headspace, an aliquot of the headspace is analyzed using GC/MS.  Note that samples are also commonly analyzed by GC/FID (8015B).  Other GC techniques may be used as well.


(EPA SW-846)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   14 days from sample collection to analysis
Preservatives:   Store samples at 4°C until analysis.
Required Preps:   None specified in method.
Collection Method:   Grab sampling
Analytical Methodology:   GC/MS following EPA Method 8260B
Documentation:   5021A
8260B

Analyte List*

Analyte Formula CAS Number Detection Limit
Ethylbenzene
C8H10
100-41-4
3.4
 ug/kg
Styrene
C8H8
100-42-5
3.4
 ug/kg
n-Propylbenzene
C9H12
103-65-1
3.4
 ug/kg
n-Butylbenzene
C10H14
104-51-8
3.4
 ug/kg
p-Xylene
C8H10
106-42-3
3.4
 ug/kg
4-Chlorotoluene
C7H7Cl
106-43-4
3.4
 ug/kg
1,4-Dichlorobenzene
C6H4Cl2
106-46-7
3.4
 ug/kg
1,2-Dibromoethane
C2H4Br2
106-93-4
3.4
 ug/kg
1,2-Dichloroethane
C2H4Cl2
107-06-2
3.4
 ug/kg
m-Xylene
C8H10
108-38-3
3.4
 ug/kg
1,3,5-Trimethylbenzene
C9H12
108-67-8
3.4
 ug/kg
Bromobenzene
C6H5Br
108-86-1
3.4
 ug/kg
Toluene
C7H8
108-88-3
3.4
 ug/kg
Chlorobenzene
C6H5Cl
108-90-7
3.4
 ug/kg
1,2,4-Trichlorobenzene
C6H3Cl3
120-82-1
3.4
 ug/kg
Chlorodibromomethane
CHBr2Cl
124-48-1
3.4
 ug/kg
Tetrachloroethene
C2Cl4
127-18-4
3.4
 ug/kg
sec-Butylbenzene
C10H14
135-98-8
3.4
 ug/kg
1,3-Dichloropropane
C3H6Cl2
142-28-9
3.4
 ug/kg
cis-1,2-Dichloroethene
C2H2Cl2
156-59-2
3.4
 ug/kg
trans-1,2-Dichloroethene
C2H2Cl2
156-60-5
3.4
 ug/kg
1,3-Dichlorobenzene
C6H4Cl2
541-73-1
3.4
 ug/kg
Carbon tetrachloride
CCl4
56-23-5
3.4
 ug/kg
1,1-Dichloropropene
C3H4Cl2
563-58-6
3.4
 ug/kg
2,2-Dichloropropane
C3H6Cl2
594-20-7
3.4
 ug/kg
1,1,1,2-Tetrachloroethane
C2H2Cl4
630-20-6
3.4
 ug/kg
Chloroform
CHCl3
67-66-3
3.4
 ug/kg
Benzene
C6H6
71-43-2
3.4
 ug/kg
1,1,1-Trichloroethane
C2H3Cl3
71-55-6
3.4
 ug/kg
Bromomethane
CH3Br
74-83-9
3.4
 ug/kg
Chloromethane (Methyl chloride)
CH3Cl
74-87-3
3.4
 ug/kg
Dibromomethane
CH2Br2
74-95-3
3.4
 ug/kg
Bromochloromethane
CH2BrCl
74-97-5
3.4
 ug/kg
Chloroethane
C2H5Cl
75-00-3
3.4
 ug/kg
Vinyl chloride
C2H3Cl
75-01-4
3.4
 ug/kg
Methylene chloride
CH2Cl2
75-09-2
3.4
 ug/kg
Bromoform
CHBr3
75-25-2
3.4
 ug/kg
Bromodichloromethane
CHBrCl2
75-27-4
3.4
 ug/kg
1,1-Dichloroethane
C2H4Cl2
75-34-3
3.4
 ug/kg
1,1-Dichloroethene
C2H2Cl2
75-35-4
3.4
 ug/kg
Trichlorofluoromethane
CCl3F
75-69-4
3.4
 ug/kg
Dichlorodifluoromethane
CCl2F2
75-71-8
3.4
 ug/kg
1,2-Dichloropropane
C3H6Cl2
78-87-5
3.4
 ug/kg
1,1,2-Trichloroethane
C2H3Cl3
79-00-5
3.4
 ug/kg
Trichloroethene
C2HCl3
79-01-6
3.4
 ug/kg
1,1,2,2-Tetrachloroethane
C2H2Cl4
79-34-5
3.4
 ug/kg
1,2,3-Trichlorobenzene
C6H3Cl3
87-61-6
3.4
 ug/kg
Hexachlorobutadiene
C4Cl6
87-68-3
3.4
 ug/kg
Naphthalene
C10H8
91-20-3
3.4
 ug/kg
o-Xylene
C8H10
95-47-6
3.4
 ug/kg
2-Chlorotoluene
C7H7Cl
95-49-8
3.4
 ug/kg
1,2-Dichlorobenzene
C6H4Cl2
95-50-1
3.4
 ug/kg
1,2,4-Trimethylbenzene
C9H12
95-63-6
3.4
 ug/kg
1,2-Dibromo-3-Chloropropane
C3H5Br2Cl
96-12-8
3.4
 ug/kg
1,2,3-Trichloropropane
C3H5Cl3
96-18-4
3.4
 ug/kg
tert-Butylbenzene
C10H14
98-06-6
3.4
 ug/kg
Cumene (Isopropylbenzene)
C9H12
98-82-8
3.4
 ug/kg
Cymene (4-Isopropyltoluene)
C10H14
99-87-6
3.4
 ug/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.