• 6 •
RESTEKAdvantage
800-356-1688
By KatiaMay, Ph.D., R&DChemist andChris English, Environmental Innovations Chemist
Figure 1
– Ten-minute analysis of 50+OLC 03.2 volatile compounds, using anRtx
®
-VMS column and newRestek referencemixes.
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 5mLROwater
OLC 03.2 VOAMegaMix
™
, cat.# 30492
502.2 CalibrationMix #1 (gases), cat.# 30042
VOACalibrationMix #1 (ketones), cat.# 30006
L/CVOA Internal StandardMix, cat.# 30091
Concentrator:
Tekmar 3100 Purge and Trap
Trap:
Vocarb 3000
Purge:
11min. @ 40mL/min. @ ambient temperature
Dry purge:
1min. @ 40mL/min. (MCS bypassed)
Desorb preheat:
245°C
Desorb:
250°C for 1min. @ 40mL/min.
Bake:
260°C for 8min.
Interface:
30:1 split using
1
/
16
" Silcosteel
®
tee (cat.# 20513)
& 0.3m of 0.25mm ID fused silica tubing for split line
Carrier gas:
24psi helium, constant pressure
Flow rate:
1.3mL/min. @ 45°C
Dead time:
0.77 min. @ 45°C
Oven temp.:
45°C (hold 4min.) to 225°C@ 32°C/min. (hold 2min.)
Det:
Agilent 5971AGC/MSw/ K&M electronmultiplier
Transfer line temp.:
280°C
Scan range:
35–260 amu
Tune:
PFTBA/BFB
Ionization:
EI
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.
m
-xylene
43.
p
-xylene
44.
o
-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 03.2VOAMegaMix
™
(42 components)
Components listed in Figure 1 (bold)
2,000µg/mL each in P&Tmethanol (m-& p-xylene at
1,000µg/mL), 1mL/ampul
Each
5-pk.
10-pk.
30492
30492-510
—
w/data pack
30492-500
30492-520
30592
Bold type–components of OLC 03.2 VOAMegaMix
™
(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
OLC03.2VOADeuterated
MonitoringCompounds (DMC)
(14components)
100µg/mL each in P&Tmethanol, 1mL/ampul
Ketones:
2-butanone-d5
2-hexanone-d5
200µg/mL each in P&Tmethanol, 0.5mL/ampul
Each
5-pk.
30493
30493-510
Rtx
®
-VMSColumn (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, themethod requires adding 14 deuterated
monitoring compounds (DMC) to a volatiles sam-
ple as a sample-by-sample accuracy indicator.
Volatiles andDMC are purged from a sample,
trapped, and desorbed into the GC/MS for analysis.
Our newOLC 03.2 VOAMegaMix
™
referencemix
contains themaximum number of volatile analytes
consistent with stable formulation. Co-eluting
m-
and
p-
xylene are included at one-half the concentration
of the other 40 compounds, allowing these analytes
NewVolatiles ReferenceMix
for OLC 03.2 Statement ofWork
✔
All materials needed for analysis of volatiles.
✔
NewMegaMix
™
includes 42 target compounds in a singlemixture.
✔
Co-eluters
m-
and
p-
xylene at one-half concentration of other volatiles.
✔
Deuteratedmonitoring compoundmixes for quality control.
✔
Rtx
®
-VMS column separates OLC 03.2 volatiles in less than 10minutes.
to be calibrated at lower detection limits and thus
eliminating the time and expense of a second cali-
bration. NewOLC 03.2 VOADeuteratedMonitoring
CompoundsMix contains all 14DMC specified in
OLC 03.2. In combinationwith the two newmixes,
our gas and ketonemixes (cat.# 30042 and cat.#
30006) and L/C VOA Internal StandardMix (cat.#
30091)make a complete set of referencematerials
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 bleedwhen analyzing
higher-boiling analytes. A 20m, 0.18mm ID, 1.0µm
Rtx
®
-VMS column separates the OLC 03.2 volatiles
in less than 10minutes (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.
