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12

2007.01

8-Minute Dual Column Analysis of Organochlorine Pesticides

Using Rtx®-CLPesticides / Rtx®-CLPesticides2 Columns

By Jason Thomas, Environmental Chemist

Rtx®-CLPesticides Column (fused silica)

ID df (µm)

temp. limits

length cat. #

price

0.18mm 0.18 -60 to 310/330°C 20-Meter 42102

$430

Rtx®-CLPesticides2 Column (fused silica)

ID df (µm)

temp. limits

length cat. #

price

0.18mm 0.14 -60 to 310/330°C 20-Meter 42302

$430

IP Deactivated Guard Column

length, ID

cat. #

price

5m, 0.53mm ID

10045

$60

Ferrules Fit Column ID

qty.

cat.#

price

0.25/0.28mm

kit

20276

$228

• Analysis and confirmation of 20 pesticides in 8 minutes.

• Baseline resolution of all compounds, for improved accuracy.

• Low-bleed columns, for reliable data.

Analyses for organochlorine pesticides are among the most common pesticide methodologies in use today. US EPA Method 8081,

for example, requires separation of 20 organochlorine pesticides, some of which are isomers or are otherwise structurally similar and,

therefore, are difficult to separate. Restek introduced two proprietary phases to address this issue, the Rtx®-CLPesticides phase and

the Rtx®-CLPesticides2 phase, which have proven very popular within the environmental community. The unique selectivities of this

column pair allow laboratories to significantly reduce analysis times for Method 8081.

There is a constant need for faster analyses, to help increase sample throughput and, thereby, increase productivity. Fast GC is a good

solution, but the reduced column internal diameters and thinner phase film coatings associated with fast GC have been deterrents, due

to concerns about the columns’ ability to cope with the harsh sample matrices often encountered in environmental samples, and short-

ened column lifetimes have not been acceptable.

Using a 0.53mm ID guard column at the inlet end

of a dual column configuration protects the ana-

lytical columns downstream. This configuration

allows 20m x 0.18mm ID thin film columns to be

used, with their associated high efficiency, to great-

ly reduce analysis time without the reduction of

column lifetime usually associated with introduc-

ing “dirty” samples into small bore columns.

Figure 1 shows separation of the 20 target pesticides

in EPA Method 8081 in 8 minutes using 20m x

0.18mm ID Rtx®-CLPesticides/Rtx®-CLPesticides2

columns with a 0.53 ID guard column. In addition

to rapid, baseline resolution, the pesticides are elut-

ed as sharp, symmetric peaks. This, in turn, helps

assure reliable quantification data for these analytes.

Clearly the Rtx®-CLPesticides/Rtx®-CLPesticides2

columns, in conjunction with a 0.53mm ID guard

column, are an excellent choice for analyzing EPA

Method 8081 pesticides, or equivalent target lists of

these pesticides.

Figure 1

20 organochlorine pesticides resolved and confirmed

in 8 minutes, using Rtx®-CLPesticides/Rtx®-CLPesticides2 columns.

3.0

4.0

5.0

6.0

7.0

8.0

GC_EV00892

GC_EV00893

3.0

4.0

5.0

6.0

7.0

8.0

SeCure™“Y”Connector Kits

Column:

Rtx

®

-CLPesticides, 20m, 0.18mm ID, 0.18µm (cat.# 42102) (top) and

Rtx

®

-CLPesticides2, 20m, 0.18mm ID, 0.14µm (cat.# 42302) with 5m x 0.53mm ID

intermediate-polarity deactivated guard tubing (cat.# 10045), connected using

SeCure

“Y” Connector Kit (cat.# 20276) with Universal “Y” Press-Tight

®

Connector

Sample:

Organochlorine Pesticide Mix AB #2 (cat.# 32292), 8-80µg/mL each component in hexane/

toluene, Pesticide Surrogate Mix (cat.# 32000), 200µg/mL each component in acetone

Inj.:

0.5µL splitless (hold 0.75 min.), 2mm single gooseneck inlet liner (cat.# 20795)

Inj. temp.:

250°C

Carrier gas:

helium, constant flow

Linear velocity: 20cm/sec. @ 140°C

Oven temp.:

140°C (hold 1 min.) to 250°C @ 35°C/min. (hold 1 min.) to 330°C @ 35°C/min. (hold 3 min.)

Det.:

ECD @ 350°C

1. 2,4,5,6-tetrachloro-

m

-xylene (surr.)

2.

α

-BHC

3.

γ

-BHC

4.

β

-BHC

5.

δ

-BHC

6. heptachlor

7. aldrin

8. heptachlor epoxide

9.

γ

-chlordane

10.

α

-chlordane

11. endosulfan I

12. 4,4’ DDE

13. dieldrin

14. endrin

15. 4,4’ DDD

16. endosulfan II

17. 4,4’ DDT

18. endrin aldehyde

19. endosulfan sulfate

20. methoxychlor

21. endrin ketone

22. decachlorobiphenyl

(surr.)

10

12

11

13

14

15 16 17

18

20

19

21

22

1

2

5 6

7

8 9

3

4

22

21

20

19 18

17 16

15

14

13 12

10

11

1

2

8 9

4

3 5 6 7

Dual column analysis in

less than 8 minutes!