ADV01-05_1-298

• 6 •

www.restekcorp.com

RESTEK Advantage

800-356-1688

By Katia May, Ph.D., R&D Chemist and Chris English, Environmental Innovations Chemist

Figure 1

– Ten-minute analysis of 50+ OLC 03.2 volatile compounds, using an Rtx

-VMS column and new Restek reference mixes.

1. dichlorodifluoromethane

2. chloromethane

3. vinyl chloride

4. bromomethane

5. chloroethane

6. trichlorofluoromethane

7. 1,1-dichloroethene

8. carbon disulfide

9. Freon

113

GC_EV00681

Rtx

-VMS 20m, 0.18mm ID, 1.0µm (cat.# 49915)

Sample:

Components at 10ppb (50 ppb ketones) in 5mL RO water

OLC 03.2 VOA MegaMix

™

, cat.# 30492

502.2 Calibration Mix #1 (gases), cat.# 30042

VOA Calibration Mix #1 (ketones), cat.# 30006

L/C VOA Internal Standard Mix, cat.# 30091

Concentrator:

Tekmar 3100 Purge and Trap

Trap:

Vocarb 3000

Purge:

11 min. @ 40mL/min. @ ambient temperature

Dry purge:

1 min. @ 40mL/min. (MCS bypassed)

Desorb preheat:

245°C

Desorb:

250°C for 1 min. @ 40mL/min.

Bake:

260°C for 8 min.

Interface:

30:1 split using

" Silcosteel

tee (cat.# 20513)

& 0.3m of 0.25mm ID fused silica tubing for split line

Carrier gas:

24psi helium, constant pressure

Flow rate:

1.3 mL/min. @ 45°C

Dead time:

0.77 min. @ 45°C

Oven temp.:

45°C (hold 4 min.) to 225°C @ 32°C/min. (hold 2 min.)

Det:

Agilent 5971A GC/MS w/ K&M electron multiplier

Transfer line temp.:

280°C

Scan range:

35–260 amu

Tune:

PFTBA/BFB

Ionization:

10. methylene chloride

11. acetone

12.

trans

-1,2-dichloroethene

13. methyl acetate

14. methyl

tert

-butyl ether

15. 1,1-dichloroethane

16.

cis

-1,2-dichloroethene

17. cyclohexane

18. bromochloromethane

19. chloroform

20. carbon tetrachloride

21. 1,1,1-trichloroethane

22. 2-butanone

23. benzene

24. 1,2-dichloroethane

25. methyl cyclohexane

26. trichloroethene

27. 1,4-difluorobenzene

28. 1,2-dichloropropane

29. bromodichloromethane

30.

cis

-1,3-dichloropropene

31. toluene

32. tetrachloroethene

33. 4-methyl-2-pentanone

34.

trans

-1,3-dichloropropene

35. 1,1,2-trichloroethane

36. dibromochloromethane

37. 1,2-dibromoethane

38. 2-hexanone

39. chlorobenzene-d5

40. chlorobenzene

41. ethylbenzene

42.

-xylene

43.

-xylene

44.

-xylene

45. styrene

46. bromoform

47. isopropylbenzene

48. 1,1,2,2-tetrachloroethane

49. 1,3-dichlorobenzene

50. 1,4-dichlorobenzene-d4

51. 1,4-dichlorobenzene

52. 1,2-dichlorobenzene

53. 1,2-dibromo-3-chloropropane

54. 1,2,4-trichlorobenzene

55. 1,2,3-trichlorobenzene

OLC 03.2 VOA MegaMix

™

(42 components)

Components listed in Figure 1 (bold)

2,000µg/mL each in P&T methanol (m-& p-xylene at

1,000µg/mL), 1 mL/ampul

Each

5-pk.

10-pk.

30492

30492-510

—

w/data pack

30492-500

30492-520

30592

Bold type–components of OLC 03.2 VOA MegaMix

™

(cat.# 30492)

Non-Ketones:

benzene-d6

bromoform-d

chloroethane-d5

chloroform-d

1,2-dichlorobenzene-d4

1,2-dichloroethane-d4

1,1-dichloroethene-d2

1,2-dichloropropane-d6

trans

-1,3-dichloropropene-d4

1,1,2,2-tetrachloroethane-d2

toluene-d8

vinyl chloride-d3

OLC 03.2 VOA Deuterated

Monitoring Compounds (DMC)

(14 components)

100µg/mL each in P&T methanol, 1mL/ampul

Ketones:

2-butanone-d5

2-hexanone-d5

200µg/mL each in P&T methanol, 0.5mL/ampul

Each

5-pk.

30493

30493-510

Rtx

-VMS Column (fused silica)

ID df (µm)

temp. limits

40-Meter

0.18mm 1.00 -40 to 240/260°C 49915

The latest revision to the US EPA Contract

Laboratory Program (CLP) methods, OLC 03.2,

adds nine compounds to the target list of volatile

organic analytes: cyclohexane, dichlorodifluo-

romethane, isopropylbenzene, methyl acetate,

methyl

tert-

butyl ether, methylcyclohexane, 1,2,3-

trichlorobenzene, trichlorofluoromethane, and

1,1,2-trichloro-1,2,2-trifluoroethane (Freon

113).

Further, the method requires adding 14 deuterated

monitoring compounds (DMC) to a volatiles sam-

ple as a sample-by-sample accuracy indicator.

Volatiles and DMC are purged from a sample,

trapped, and desorbed into the GC/MS for analysis.

Our new OLC 03.2 VOA MegaMix

™

reference mix

contains the maximum number of volatile analytes

consistent with stable formulation. Co-eluting

and

xylene are included at one-half the concentration

of the other 40 compounds, allowing these analytes

New Volatiles Reference Mix

for OLC 03.2 Statement of Work

✔

All materials needed for analysis of volatiles.

✔

New MegaMix

™

includes 42 target compounds in a single mixture.

✔

Co-eluters

and

xylene at one-half concentration of other volatiles.

✔

Deuterated monitoring compound mixes for quality control.

✔

Rtx

-VMS column separates OLC 03.2 volatiles in less than 10 minutes.

to be calibrated at lower detection limits and thus

eliminating the time and expense of a second cali-

bration. New OLC 03.2 VOA Deuterated Monitoring

Compounds Mix contains all 14 DMC specified in

OLC 03.2. In combination with the two new mixes,

our gas and ketone mixes (cat.# 30042 and cat.#

30006) and L/C VOA Internal Standard Mix (cat.#

30091) make a complete set of reference materials

for OLC 03.2 SOW volatiles.

We designed Rtx

-VMS capillary columns specifi-

cally for fast analyses of volatile organics. Excellent

thermal stability ensures low bleed when analyzing

higher-boiling analytes. A 20m, 0.18mm ID, 1.0µm

Rtx

-VMS column separates the OLC 03.2 volatiles

in less than 10 minutes (Figure 1). These opti-

mized conditions resolve carbon tetrachloride from

1,1,1-trichloroethane (peaks 20 and 21) and pre-

vent ions from these analytes from interfering with

quantification. The 45ºC initial temperature allows

rapid oven cycles without sacrificing resolution of

the gases.