ADV01-05_1-298

Innovators of High Resolution

Chromatography Products

the

in this issue

Rt-Msieve

™

5A & MXT

-5A

PLOT Columns

…pg. 5

HPLC Analysis of

Narcotic/Acetaminophen Mixtures

…pg. 6–7

More Reliable Results from

Semivolatiles Analysis

…pg. 8–9

New Analytical Reference Materials

…pg. 9

Scotty

Transportables

…pg. 10

Order ChemService Pesticides from

Restek

…pg. 11

Polar Analytes by HPLC/

Replacement Instrument Parts

…pg. 12–13

Super-Clean

™

Gas-Trapping

System for LC/MS

…pg. 14

New Reference Books

…pg. 14

Cool Tools

…pg. 15

Behind the Scenes

…pg. 16

800-356-1688

814-353-1300

www.restekcorp.com

2002

vol. 3

by Frank Dorman, Ph.D., Innovations Team, Director of Technical Development

Optimized Analysis of

Brominated Flame Retardants

Using an Rtx

-500 GC Capillary Column

Advantage

Rtx

-500 GC

Capillary Column

…pg. 1–2

Vespel

Ring Inlet Seal

…pg. 3

Leak Detective

™

Electronic Leak Detector

…pg. 3

Bringing Packed Column

Technology Back to Life

…pg. 4

✔

Elutes decabromodiphenyl ether in 30 minutes.

✔

Low bleed for sensitive ECD and MS analyses.

✔

Separates other higher molecular weight compounds.

new

Brominated flame retardants are an emerging envi-

ronmental concern that present a unique challenge

to analysts. One of the most heavily used types of

brominated flame retardants are the polybrominat-

ed diphenyl ethers (PBDEs). These compounds

have the structure shown in Figure 1, with 1 to 10

bromines substituted on the two rings. This makes

these compounds fairly heavy (up to approximately

1000amu), thus placing difficult requirements on

the gas chromatographic (GC) analytical system.

While the analysis may be performed using either

electron capture detection (ECD) or mass spectro-

metric detection (MS), the compounds require a

high oven temperature to elute in a reasonable

amount of time. This requires an analytical GC col-

umn featuring high-temperature fused silica or

metal tubing and a high-temperature stationary

phase that has both low bleed and the selectivity

necessary to separate the PBDE congeners.

Restek chemists, working in conjunction with Karen

MacPherson and Eric Reiner at the Ontario Ministry

of the Environment, have developed a new fused sil-

ica capillary GC column and analytical procedure

for separating PBDE congeners in a reasonable

time. The new Rtx

-500 column incorporates a

carborane-stabilized polydimethylsiloxane polymer

in special high-temperature fused silica tubing. The

column can be heated to 380°C, and exhibits very

low bleed at this extreme temperature. The column

combines the stability required for separating high-

er molecular weight compounds with the sensitivity

required for ECD or MS analysis.

PBDE congeners up to decabromodiphenyl ether

(PBDE 209) are separated in less than 45 minutes

Figure 1

PBDEs can have high molecular weight, due

to bromine substitution around the two rings.

using the new Rtx

-500 column in a GC-high resolu-

tion MS analysis (Figure 2). In a GC-ECD analysis of

the same PBDE congeners, decabromodiphenyl

ether is eluted in 30 minutes. This same system has

been used for baseline separation of toxic PCB con-

geners and is currently under investigation for analy-

ses of the brominated and chlorinated dioxins and

furans. If you must analyze PBDEs or other high

molecular weight compounds, we highly recommend

the Rtx

-500 column for fast separations and reli-

able quantitation.

(contd. on page 2)