EPA Method 8270: Determination of Semi-volatile Organic

Compounds in Water using Solid Phase Extraction and

GC/MS

UCT Part Numbers:

EC82701M15 - 1000 mg 8270 sorbent/15 mL cartridge (≤ 500 mL sample)
EU52112M6 - 2000 mg activated carbon/6 mL cartridge (≤ 500 mL
sample)
EC82702M15 - 2000 mg 8270 sorbent/15 mL cartridge (> 500 mL sample)
EU52113M6 - 3000 mg activated carbon/6 mL cartridge (> 500 mL sample)
AD0000AS - Cartridge adaptor
VMFSTFR12 - Large volume sample transfer tubes
VMF016GL - 16 position glass block manifold
VMF02125 - 12 position large volume collection rack
RFV1F15P - 15 mL reservoirs with 1 frit, 10 micron porosity
ECSS25K - Sodium sulfate, anhydrous, ACS grade, granular, 60 mesh
GCLGN4MM-5 - GC liner, 4 mm splitless gooseneck

EPA method 8270 allows the use of liquid-liquid extraction (LLE) and solid phase
extraction (SPE) to extract semi-volatile organic compounds (SVOCs) in aqueous
samples and TCLP leachates. LLE requires multiple extractions at two different pH
values, consumes large amounts of organic solvents, and causes emulsion when real
world dirty samples are extracted.

This application note outlines a reliable, efficient, and cost-effective SPE method
utilizing two stacked SPE cartridges, UCT’s EC8270 and activated carbon cartridges for
the extraction of SVOCs in water and TCLP samples. Prior to extraction, samples are
dechlorinated and adjusted to pH < 2, then passed through the SPE system, the 8270
SPE cartridge retains the majority of the target analytes including acids, bases, and
neutrals with mid to high hydrophobicity, while the carbon cartridge connected
downstream will capture a few very polar compounds*, such as 1,4-dioxane, n-
nitrosodimethylamine, n-nitrosomethylethylamine, methyl methanesulfonate, ethyl
methanesulfonate, and1-Nitrosopyrrolidine. High sample throughout can be achieved by
extracting multiple samples simultaneously using a multi-port SPE manifold.
*: Carbon cartridge is NOT needed if none of the very polar analytes is being analyzed, such as
for the TCLP SVOCs list.
SPE Procedure:

1. Sample Pretreatment
a) Dechlorinate sample with 80 mg/L of sodium thiosulfate if free chlorine presents.
b) Adjust sample pH to < 2 using 6N HCl.
c) Spike with surrogates, and target analytes for fortified samples.

Tip 1: The spiking solutions should be prepared in water miscible solvents, such as
methanol, acetonitrile, or acetone.

2. SPE System Setup

a) Connect the carbon cartridge (EU52112M6 or EU52113M6 depending on
sample volume) to the end of the 8270 cartridge (EC82701M15 or EC82702M15
depending on sample volume) using a cartridge adaptor (AD0000AS).
b) Insert a loose plug of deactivated glass wool into the 8270 cartridge to prevent
sorbent clogging caused by samples with high particulate content.
c) Attach the connected SPE cartridges to the SPE manifold (VMF016GL).

Tip 2: The carbon cartridge is not needed if very polar analytes, such as 1,4-dioxane, n-
nitrosodimethylamine, n-nitrosomethylethylamine, methyl methanesulfonate, ethyl
methanesulfonate, and 1-Nitrosopyrrolidine are not being analyzed.

3. Cartridge Conditioning
a) Wash the SPE cartridges with 15 mL of dichloromethane (DCM), soak 1 min,
and apply full vacuum for 1 min.
b) Condition the SPE cartridges with 10 mL of methanol. Draw most of the way
through the column leaving a thin layer (about 0.5 cm) of solvent above the frit.
Do not allow cartridges to go dry from this step until instructed to do so in the
cartridge drying step.
c) Equilibrate the cartridges with 10 mL of reagent water and 10 mL of 0.05N HCl.
4. Sample Loading
a) Attach the large volume sample delivery tube (VMFSTFR12) to the top of the
8270 cartridge, and insert the stainless steel end of the tube into the sample
bottle.
b) Adjust vacuum for a fast dropwise sample flow (about 10-15 mL/min), and draw
the entire sample through.

5. Washing and Drying

a) Rinse the sample bottle with 10 mL of reagent water, and apply the rinsate to
the SPE cartridges.
b) Disassemble the transfer tube and the connected SPE cartridges. Dry the 8270
cartridge under full vacuum for 10 min, and the carbon cartridge for 15 min.

Tip 3: Remove as much water as possible, wet sorbents result in low analyte recovery.

6. Analyte Elution
a) Insert the collection rack (VMF02125) with 40-60 mL glass vials into the manifold.
b) Elute the SPE 8270 and carbon cartridges separately. Apply elution solvent to
the SPE cartridges, draw 1/3 through, soak 1-2 min, and then draw the
remaining solvent through the cartridge in a slow dropwise fashion. Leave full
vacuum on for 1 min after each elution.

10 mL 1:1 acetone:n-hexane
(bottle rinse added to 8270 cartridge using transfer tube)
8270 Cartridge 10 mL DCM
3 - 4 mL ammonium hydroxide (28-30%), drain to waste
3 x 7 mL DCM
Carbon Cartridge 5 x 3 mL DCM

Tip 4: Bottle rinse is critical for good recovery of PAHs, which tend to adsorb on the glass wall.
 7. Eluate Drying

a) Dry the eluates using a 15-mL reservoir (or a glass funnel stopped with glass
wool) holding about 15-20 g of anhydrous Na2SO4, pre-rinse the Na2SO4 with 10
mL of DCM.
b) Insert the collection rack with 40-60 mL glass vials into the manifold to collect
the dried eluates.
c) Pass the eluates through the Na2SO4 bed.
d) Rinse the eluate vials with 2 x 5 mL of DCM, transfer the rinses to the Na2SO4
bed.

Tip 5: If Na2SO4 appears greenish, rinse with more solvent until it turns white.

8. Concentration

a) Concentrate the eluates to 0.7-0.9 mL under a gentle stream of N2 at 40 ºC.

b) Add internal standards, transfer the extract to a 2-mL auto-sampler vial, and
adjust the final volume to 1 mL.
c) The samples are ready for GC/MS analysis.

GC/MS Method
GC/MS Agilent 6890N GC coupled to a 5975C MSD

Injection 1 μL splitless injection at 250 ºC, split vent of 30 mL/min at 1 min

GC Liner 4 mm splitless gooseneck (GCLGN4MM-5), packed with deactivated glass wool

GC Column Restek Rxi®-5sil MS 30m x 0.25mm, 0.25µm with 10m integrated guard column

Carrier Gas Ultra high purity helium at a constant flow of 1.5 mL/min

Oven Temp. Initial temperature at 40 ºC, hold for 3 min; ramp at 15 ºC/min to 240 ºC;
Program ramp at 6 ºC/min to 310 ºC; and hold for 2 min

MSD Temp. Transfer line 280 ºC; Source 250 ºC; Quadrupole 150 ºC
Full Scan 35 - 500 amu
Range

SPE Setup

Recovery and RSD in Laboratory Fortified Blanks

(500 mL sample fortified with 40 μg/L of 139 analytes and 6 surrogates)

Ave RSD%
Compound
Recovery% (n=4)
1,2,4,5-Tetrachlorobenzene 99.5 4.1
1,2,4-Trichlorobenzene 88.5 5.7
1,2-Dichlorobenzene 90.3 3.9
1,3,5-Trinitrobenzne 124.4 2.8
1,3-Dichlorobenzene 85.8 2.8
1,4-Dichlorobenzene 89.1 1.1
1,4-Naphthalenedione 95.3 4.3
1-Chloronaphthalene 112.2 2.7
1-Methyl fluorene 86.9 0.9
1-Methyl phenanthrene 89.8 1.3
1-Methylnaphthalene 102.1 2.7
1-Naphthalenamine 112.3 4.7
1-Nitrosopiperidine 88.9 5.8
1-Nitrosopyrrolidine 91.8 7.2
2,3,4,6-Tetrachlorophenol 103.2 0.9
2,3-Dichloroaniline 91.4 0.6
2,4,5-Trichlorophenol 123.5 4.7
2,4,6-Trichlorophenol 106.5 3.6
2,4-Dichlorophenol 97.3 6.5
2,4-Dimethylphenol 99.0 6.4
2,4-Dinitrophenol 122.4 2.0
2,4-Dinitrotulene 112.0 1.7
2,6-Dichlorophenol 113.3 0.7
2,6-Dinitrotoluene 106.3 2.3
2-Acetylaminofluorene 109.0 6.5
2-Chloronaphthalene 96.9 2.8
2-Chlorophenol 99.4 2.9
2-Isopropyl naphthalene 73.1 0.1
2-Methylnaphthalene 101.2 4.9
2-Methylphenol 97.6 6.7
2-Naphthalenamine 130.5 2.7
2-Nitroaniline 107.5 3.6
2-Nitrophenol 98.2 5.9
2-Picoline 74.4 5.0
3&4-Methylphenol 104.2 6.6
3,3'-Dichlorobenzidine 72.3 11.4
3,6-Dimethyl phenanthrene 90.6 0.9
3-Methylcholanthrene 106.5 1.4
3-Nitroaniline 100.4 4.9
3-Nitrophenol 99.5 8.2
4,4'-DDD 94.4 0.8
4,4'-DDE 91.8 0.4
4,4'-DDT 94.0 0.3
4,6-Dinitro-2-methylphenol 116.8 4.5
4-Aminobiphenyl 103.8 13.5
4-Chloro-3-methylphenol 111.7 6.3
4-Chloroaniline 105.0 3.9
4-Chlorophenylphenylether 99.5 3.0
4-Nitroaniline 114.9 4.6
4-Nitrophenol 97.2 3.0
5-Nitro-o-toluidine 94.7 4.0
7,12-Dimethyl benz[a]anthracene 99.9 6.1
Acenaphthene 100.1 1.3
Acenaphthylene 102.6 0.6
Acetophenone 101.8 7.4
Aldrin 89.5 0.8
alpha lindane 90.1 0.2
Aniline 90.0 3.2
Anthracene 109.7 1.1
Azobenzene 105.5 5.2
Benz[a]anthracene 103.3 6.2
Benzidine 66.8 14.0
Benzo[a]pyrene 99.3 2.1
Benzo[b]fluoranthene 99.4 7.0
Benzo[ghi]perylene 104.2 1.1
Benzo[k]fluoranthene 108.1 5.4
Benzoic acid 115.0 4.7
Benzyl alcohol 72.9 12.9
Benzyl butyl phthalate 111.8 6.0
beta lindane 95.2 1.1
Bis(2-ethylhexyl) phthalate 113.2 2.0
Bis[2-chloroethoxy]methane 91.0 7.8
Bis[2-chloroethyl]ether 88.5 3.0
Bis[2-chloroisopropyl]ether 87.3 4.5
Bromophenoxybenzene 99.6 4.8
Carbazole 109.6 3.3
Chlorobenzilate 116.3 9.4
Chrysene 103.3 1.2
delta lindane 95.2 0.8
Diallate (cis & trans) 104.7 4.5
Dibenz[ah]anthracene 108.8 2.5
Dibenzofuran 102.0 0.6
Dibutyl phthalate 114.6 6.2
Dieldrin 94.5 0.7
Diethyl phthalate 110.4 1.2
Dimethoate 96.6 0.7
Dimethyl phthalate 110.3 1.3
Di-n-octyl phthalate 116.6 5.9
Dinoseb 121.9 1.7
Diphenylamine 109.9 4.8
Disulfoton 87.0 0.6
Endosulfan I 93.8 0.7
Endosulfan II 96.5 0.5
Endosulfan sulfate 96.2 0.7
Endrin 97.4 1.0
Endrin aldehyde 93.4 0.5
Ethyl methanesulfonate 92.5 3.7
Famphur 109.3 1.2
Fluoranthene 105.8 6.1
Fluorene 103.7 2.6
gamma lindane 93.1 1.3
Heptachlor 88.1 1.0
Heptachlor epoxide 93.4 0.9
Hexachlorobenzene 101.3 6.1
Hexachlorobutadiene 85.0 1.0
Hexachloroethane 92.6 6.0
Hexachloropropene 72.1 1.1
Hexachorocyclopentadiene 85.9 3.1
Indeno[123-cd]pyrene 103.2 2.5
Isodrin 105.1 7.2
Isophorone 91.0 6.8
Isosafrole (cis & trans) 102.9 6.1
Methyl methanesulfonate 70.8 3.5
Methyl parathion 96.6 0.4
Naphthalene 97.2 2.3
Nitrobenzene 94.0 7.2
N-nitro-di-n-propylamine 99.3 6.3
N-nitroso di-n-butylamine 99.9 4.7
N-nitrosodiethylamine 89.4 3.7
N-nitrosodimethylamine 68.8 3.0
N-nitrosomethylethylamine 87.4 2.5
o,o,o-Triethylphosphorothioate 90.8 0.4
o-Toluidine 91.4 9.7
Parathion 95.8 0.7
p-Dimethylaminoazobenzene 91.5 10.5
Pentachlorobenzene 90.9 1.0
Pentachloroethane 86.0 3.8
Pentachloronitrobenzene 104.3 4.2
Pentachlorophenol 109.3 3.3
Phenacetin 116.4 3.9
Phenanthrene 108.0 0.4
Phenol 56.2 4.2
Phorate 86.7 0.1
Pronamide 111.2 5.2
Pyrene 109.1 8.5
Pyridine 46.1 8.0
Safrole 90.7 4.3
 Sulfotep 92.5 0.8
Thionazin 95.1 0.7
Surrogates
2-Fluorophenol (S) 87.2 0.6
Phenol d6 (S) 59.1 0.4
Nitrobenzene d5 (S) 94.3 1.0
2-Fluorobiphenyl (S) 81.5 0.5
2,4,6-Tribromophenol (S) 95.4 0.2
p-Terphenyl d14 (S) 97.5 1.0

Chromatogram of an LFB Fortified at 40 μg/L

A b u n d a n c e

T IC : L F B 4 0 .D \ d a ta .m s

6 0 0 0 0 0 0

5 5 0 0 0 0 0

5 0 0 0 0 0 0

4 5 0 0 0 0 0

4 0 0 0 0 0 0

3 5 0 0 0 0 0

3 0 0 0 0 0 0

2 5 0 0 0 0 0

2 0 0 0 0 0 0

1 5 0 0 0 0 0

1 0 0 0 0 0 0

5 0 0 0 0 0

4 .0 0 6 .0 0 8 .0 0 1 0 .0 0 1 2 .0 0 1 4 .0 0 1 6 .0 0 1 8 .0 0 2 0 .0 0 2 2 .0 0 2 4 .0 0 2 6 .0 0 2 8 .0 0
T im e - - >

5108-04-01

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