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Figure 1

The Rtx

®

-200 column provides unique

separation of the VOCs listed in

US EPA Method 8260.

• 4 •

www.restekcorp.com

Xylenes are aromatic hydrocarbons that naturally

occur in petroleum and coal tar; they also can be

commercially derived from these substrates. The US

Environmental Protection Agency (EPA) does not

require separation of the three xylene isomers(

m-

,

p-

,

o-

xylene), but rather requests their calculation

as totals or sums.

1

Some states, such as New York,

have action limits based on

m

- and

p

-xylene sepa-

rately. However, the isomers of

m

- and

p

-xylene are

difficult to resolve using gas chromatography (GC)

and most capillary columns.

Separating

m-

and

p-

Xylene Isomers

Using an Rtx

®

-200 GC Column

by Christopher English, Environmental Innovations Chemist

The common way to perform a GC separation of

m

- and

p

-xylene is by using a polyethylene glycol

(PEG) stationary phase, such as the Restek

Stabilwax

®

column. Chromatographically, baseline

separation is possible with this column; however,

the highly polar phase does not separate many of

the other volatile organic compounds (VOCs).

The more ideal column choice for this separation is

the Rtx

®

-200 column. The Crossbond

®

trifluoro-

propylmethyl polysiloxane (TFP) stationary phase

features exceptionally low bleed at operating tem-

peratures up to 360°C.

The Rtx

®

-200 column provides unique separation

of VOCs listed in US EPA Methods 524 and 8260

(Figure 1), and is the best column to separate

xylene isomers for specific state requirements

(Figure 2). The only limitation of this column is the

resolution of the gases.

Trifluoropropyl stationary phases, like that of the

Rtx

®

-200 column, have a unique selectivity because

of the electrophilic nature of the fluorine-contain-

ing polymer. This creates interactions with electron-

rich molecules like ketones and halogenated com-

pounds. The unique selectivity results in different

elution orders and resolves compounds that phenyl,

cyano, and methyl phases cannot. The Rtx

®

-200

column can be used to confirm tentatively identified

compounds and resolve multiple coelutions, mak-

ing it ideal for requirements such as those dictated

by New York State.

1. Toxicologicological Profile for Total Xylenes. Prepared by

Clements Associates, Inc., under Contract No. 205-88-0608.

Prepared for Agency of Toxic Substances and Disease Registry,

US Public Health Services, Atlanta, GA. December 1990.

Reference not available from Restek.

57

58

59

60

61

62

63,64

67

68

57. 1,3-dichloropropane

58. ethyl methacrylate

59. bromoform

60. 1,1,1,2-tetrachloroethane

61. ethylbenzene

62. 4-methyl-2-penanone

63. chlorobenzene

64. chlorobenzene-D5

65.

m

-xylene

66. 2-picoline (250ppb)

67.

p

-xylene

68.

n

-butyl acetate

69.

o-

xylene

Conditions for Figures 1 & 2

60m, 0.25 mm ID, 1.0µm Rtx

®

-200 (cat.# 15056)

10ppb each component in 5mL of RO water;

Concentrator:

Tekmar LSC-3100 Purge and Trap;

Trap:

Vocarb

®

3000 (type K);

Purge:

11 min. @

40mL/min. @ ambient temperature;

Dry purge:

1 min. @ 40mL/min.;

Desorb preheat:

245°C;

Desorb:

250°C for 2 min., flow 10mL/min.;

Bake:

260°C for 8 min.;

Interface:

transfer line

0.53mm ID Silcosteel

®

MXT

®

tubing;

Oven program:

40°C (hold 10 min.) to 100°C @ 6°C/min. (hold 1

min.) to 210°C @ 30°C/min. (hold 7 min.);

Carrier

gas:

helium @ ~1.3mL/min. constant flow (adjust

dichlorodifluoromethane to a retention time of 4.1

min. @ 40°C);

Detector:

Agilent 5973 MS, scan

range 35 to 300 AMU

65,66

m-

xylene

p-

xylene

Ions 91 and 106

(peaks 65, 67, 69, Figure 1)

Ion 91

Ion 106

o-

xylene

Figure 2

An extracted ion chromatogram shows the Rtx

®

-200 column separates

m/p

-xylene isomers.

Innovations at Work

Separate m/p-xylene isomers!

Rtx

®

-200 Columns

(Crossbond

®

trifluoropropylmethyl polysiloxane) Stable to 360°C

For the complete Rtx

®

-200 column offering, refer to Restek’s

Annual Chromatography Products Guide

(lit. cat.# 59960).

Rtx

®

-200 (Fused Silica Tubing)

ID df (µm)

temp. limits

15-Meter

30-Meter

60-Meter

105-Meter

0.25mm 1.00 -20 to 290/310°C 15050

15053

15056

15059

MXT

®

-200 (MXT

®

Tubing)

ID df (µm)

temp. limits

15-Meter

30-Meter

0.25mm 1.00

-20 to 310°C

75050

75053

for

more

info

Request Applications Note #59190.

69

22

20

min.

GC_EV00381

GC_EV00380

Unique separation of VOCs

satisfy state requirements

Low bleed at high operating

temperatures (stable to 360°C)

An extensive selection of

analytical reference materials

for US EPA

Method 8260B is available from Restek. Please see page 16 of this

newsletter or visit our web site at

www.restekcorp.com

for ordering

information.

22.00

21.80

22.40

22.20

22.80

22.60

23.00

min.