ADV01-05_1-298

• 14 •

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RESTEK Advantage

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Analysis of Complex

Semivolatiles Samples

Quantify 126 Semivolatile Compounds,

Using an Rtx

-5Sil MS Capillary GC Column

✔

Full complement of 126 EPA 8270 semivolatile/Appendix IX compounds in 3 mixes

✔

New 8270/Appendix IX Kit includes all 3 mixes

✔

New 32 component Appendix IX Mix

By Gary Stidsen, Innovations Team Manager and Katia May, Ph.D., R&D Chemist

Appendix IX is a list of organic and inorganic

Hazardous Constituents monitored in groundwater

during compliance monitoring and corrective actions

at RCRA-regulated hazardous waste treatment, stor-

age, and disposal facilities. The organics usually are

evaluated by following US EPA Method 8260

(volatiles), Method 8270 (semivolatiles), or Method

8080 (organochlorine pesticides).

Restek chemists determined the most commonly

analyzed Appendix IX compounds, carefully reviewed

the latest version of EPA Method 8270, and designed

a new reference mix of 32 compounds—Appendix

IX Mix #2 —to meet current needs of environmental

laboratories.

We formulated the new mix with the goal of prepar-

ing a product that is stable as well as useful.

Appendix IX constituents include many classes of

chemicals: polynuclear aromatic hydrocarbons

(PAHs), phenols, chlorinated aromatic hydrocar-

bons, aldehydes, anilines, benzidines, insecticides.

Unstable combinations of these compounds will pro-

duce chemical interactions—and flawed calibration

data. Methylene chloride is a common solvent for

semivolatile organics, but some grades of methylene

chloride contain low concentrations of methanol as a

stabilizer. Aldehydes (e.g., benzaldehyde) and chlori-

nated triazines (e.g., atrazine) can react with

methanol; chlorinated triazines also react with water.

Consequently, we use affirmed methanol-free, water-

free methylene chloride in formulating our mixes.

We package the new mix in deactivated amber glass

ampuls, to prevent reactions catalyzed by light.

Appendix IX Mix #2 is a highly useful complement to

our 8270 MegaMix

™

(76 compounds, cat.# 31686)

Ordering Information

Rtx

-5Sil MS column

30m,

0.25 mm ID,

0.25µm

cat.# 12723

and Appendix IX Mix #1 (18 compounds, cat.#

31625). The 126 semivolatiles in these three mixes

are separated on an Rtx

-5Sil MS column (cat.#

12723) (Figure 1, page 15). Because the PAHs elute

at temperatures over 300ºC, the analysis requires a

column that will not bleed at high temperatures.

Further, an inert column is important for the active

compounds (e.g., pentachlorophenol, dinitrophe-

nols). Rtx

-5Sil MS columns are widely used for ana-

lyzing various classes of semivolatiles, because they

exhibit versatility, inertness, and low bleed at high

temperature. The optimal combination of internal

diameter and film thickness of a 30m, 0.25 mm ID,

0.25µm Rtx

-5Sil MS column make this the best

choice for analyzing complex mixtures of semi-

volatiles. The Rtx

-5Sil MS column, in combination

with our 8270 MegaMix

™

mix, Appendix IX Mix #1,

and new Appendix IX Mix #2, and our internal stan-

dards and surrogates for EPA Method 8270 and

Appendix IX, make Restek the only place you need to

look when you want columns and reference materi-

als for semivolatiles analysis.

Appendix IX Mix #2

(32 components)

*Concentration is 500µg/mL.

1,2-diphenylhydrazine (8270-listed analyte) decomposes to

azobenzene (mix component).

N-nitrosodiphenylamine (8270-listed analyte) decomposes to

diphenylamine (mix component).

acenaphthene

acenaphthylene

aniline

anthracene

azobenzene

benzo(a)anthracene

benzo(a)pyrene

benzo(b)fluoroanthene

benzo(ghi)perylene

benzo(k)fluoroanthene

benzyl alcohol

benzyl butyl phthalate

bis 2-ethylhexyl adipate

bis(2-chloroethoxy)methane

bis(2-chloroethyl)ether

bis(2-chloroisopropyl)ether

bis(2-ethylhexyl)phthalate

4-bromophenyl phenyl ether

carbazole

4-chloroaniline

4-chloro-3-methylphenol

2-chloronaphthalene

2-chlorophenol

4-chlorophenyl phenyl ether

chrysene

dibenz(a,h)anthracene

dibenzofuran

1,2-dichlorobenzene

1,3-dichlorobenzene

1,4-dichlorobenzene

2,4-dichlorophenol

diethyl phthalate

dimethyl phthalate

2,4-dimethylphenol

1,2-dinitrobenzene

1,3-dinitrobenzene

1,4-dinitrobenzene

4,6-dinitro-2-methylphenol

2,4-dinitrophenol

2,4-dinitrotoluene

2,6-dinitrotoluene

di-

-butyl phthalate

di-

-octyl phthalate

diphenylamine

fluorene

fluoroanthene

hexachlorobenzene

hexachlorobutadiene

hexachlorocyclopentadiene

hexachloroethane

indeno(1,2,3-cd)pyrene

isophorone

1-methylnaphthalene

2-methylnaphthalene

2-methylphenol

3-methylphenol*

4-methylphenol*

naphthalene

2-nitroaniline

3-nitroaniline

4-nitroaniline

nitrobenzene

2-nitrophenol

4-nitrophenol

N-nitrosodimethylamine

N-nitroso-di-

-propylamine

pentachlorophenol

phenanthrene

phenol

pyrene

pyridine

2,3,4,6-tetrachlorophenol

2,3,5,6-tetrachlorophenol

1,2,4-trichlorobenzene

2,4,5-trichlorophenol

2,4,6-trichlorophenol

8270 MegaMix

™

(76 components)

1,000µg/mL each (except where noted) in methylene

chloride:benzene (75:25), 1mL/ampul

Each

5-pk.

10-pk.

31686

31686-510

—

w/data pack

31686-500

31686-520

31786

acetophenone

Aramite (2 isomers)

atrazine

benzaldehyde

biphenyl

caprolactam (epsilon)

chlorobenzilate

1-chloronaphthalene

diallate

dibenz(a,h)acridine

2,6-dichlorophenol

7,12-dimethylbenz(a)anthracene

1,4-dioxane

diphenyl ether

ethyl methacrylate

ethyl methanesulfonate

hexachloropropene

isodrin

isosafrole (

cis & trans

)

kepone

methyl methanesulfonate

3-methylcholanthrene

1,4-naphthoquinone

4-nitroquinoline-N-oxide

pentachlorobenzene

pentachloroethane

pentachloronitrobenzene

phenacetin

pronamide

safrole

1,2,4,5-tetrachlorobenzene

1,3,5-trinitrobenzene

1,000µg/mL each in methylene chloride, 1mL ampul

Each

5-pk.

10-pk.

31806

31806-510

—

w/data pack

31806-500

31806-520

31906

2-acetylaminofluorene

4-aminobiphenyl

-dimethylaminoazobenzene

3,3'-dimethylbenzidine

,-dimethylphenethylamine (free base)

methapyrilene (free base)

1-naphthylamine

2-naphthylamine

5-nitro-

-toluidine

N-nitrosodibutylamine

N-nitrosodiethylamine

N-nitrosomethylethylamine

N-nitrosomorpholine

N-nitrosopiperidine

N-nitrosopyrrolidine

1,4-phenylenediamine

2-picoline

-toluidine

Appendix IX Mix #1

(18 components)

2,000µg/mL each in methylene chloride, 1mL/ampul

Each

5-pk.

10-pk.

31625

31625-510

—

w/data pack

31625-500

31625-520

31725

31686: 8270 MegaMix

™

31030: Benzidine Mix, EPA 605

31625: Appendix IX Mix #1

31806: Appendix IX Mix #2

8270/Appendix IX Kit

Contains 1mL each of these mixtures.

Kit

Kit w/Data Pack

31815

31815-500