• 7 •
2003
Volume 3
800-356-1688
By KatiaMay, Ph.D., R&DChemist, andGary Stidsen, Innovations TeamManager
4,6-dinitro-2-methylphenol
2,4-dinitrophenol
2-nitroaniline
3-nitroaniline
4-nitroaniline
4-nitrophenol
2,4,5-trichlorophenol
FortificationMix
(7 components)
2,000µg/mL each inmethylene chloride, 1mL/ampul
Each
5-pk.
10-pk.
31813
31813-510
—
w/data pack
31813-500
31813-520
31913
acenaphthylene-d8
anthracene-d10
benzo(a)pyrene-d12
4-chloroaniline-d4
bis-(2-chloroethyl)ether-d8
2-chlorophenol-d4
2,4-dichlorophenol-d3
dimethylphthalate-d6
4,6-dinitro-methylphenol-d2
fluorene-d10
4-methylphenol-d8
nitrobenzene-d5
2-nitrophenol-d4
4-nitrophenol-d4
phenol-d5
pyrene-d10
OLC03.2SVOADeuteratedMonitoring
Compounds (DMC)
(16components)
2,000µg/mL each inmethylene chloride, 1mL/ampul
Each
5-pk.
31810
31810-510
Figure 1
- Excellent resolution and rapid analysis of OLC 03.2 semivolatile compounds, using
anRtx
®
-5Sil MS column and newRestek referencemixes.
1. benzaldehyde
2. phenol
3. bis(2-chloroethyl)ether
4. 2-chlorophenol
5. 1,4-dichlorobenzene-d4 (IS)*
6. 2-methylphenol
7. bis(2-chloroisopropyl)ether
8a. 4-methylphenol
8b. 3-methylphenol
9. acetophenone
10. N-nitroso-di-
n
-propylamine
11. hexachloroethane
12. nitrobenzene
13. isophorone
14. 2-nitrophenol
15. 2,4-dimethylphenol
16. bis(2-chloroethoxy)methane
17. 2,4-dichlorophenol
18. naphthalene-d8 (IS)*
19. naphthalene
20. 4-chloroaniline
21. hexachlorobutadiene
22 caprolactam
23. 4-chloro-3-methylphenol
24. 2-methylnaphthalene
25. hexachlorocyclopentadiene
26. 1,2,4,5-tetrachlorobenzene
27. 2,4,6-trichlorophenol
28. 2,4,5-trichlorophenol**
29. biphenyl
30. 2-chloronaphthalene
31. 2-nitroaniline**
32. dimethylphthalate
33. 2,6-dinitrotoluene
34. acenaphthylene
35. 3-nitroaniline**
36. acenaphthene-d10 (IS)
37. acenaphthene
38. 2,4-dinitrophenol**
39. 4-nitrophenol**
40. dibenzofuran
41. 2,4-dinitrotoluene
42. diethyl phthalate
43. fluorene
44. 4-chlorophenyl phenyl ether
45. 4-nitroaniline**
46. 4,6-dinitro-2-methylphenol**
47. diphenylamine
48. 4-bromophenyl phenyl ether
49. hexachlorobenzene
50. atrazine
51. pentachlorophenol
52. phenanthrene-d10 (IS)*
53. phenanthrene
54. anthracene
55. di-
n
-butylphthalate
56. fluoranthene
57. pyrene
58. butyl benzyl phthalate
59. benzo(a)anthracene
60. 3,3'-dichlorobenzidine**
61. chrysene-d12 (IS)*
62. chrysene
63. bis(2-ethylhexyl)phthalate
64. di-
n
-octyl phthalate
65. benzo(b)fluoranthene
66. benzo(k)fluoranthene
67. benzo(a)pyrene
68. perylene-d12 (IS)*
69. indeno(1,2,3-cd)pyrene
70. dibenzo(a,h)anthracene
71. benzo(ghi)perylene
GC_EV00683
Rtx
®
-5Sil MS 30m, 0.25mm ID, 0.25µm (cat.# 12723)
Sample:
1µLof a combination of cat.# 31812 (10µg/mL),
cat.# 31813 (50µg/mL), cat.# 31026 (50µg/mL), cat.# 31206 (20µg/mL),
cat.# 31211 (10µg/mL). 10ppm each component on-column, except as noted.
Inj.:
splitless (hold 0.4min.), DrilledUniliner
®
(cat.# 20756)
Inj. Temp.:
275°C
Carrier Gas:
helium, constant flow
FlowRate:
1mL/min.
Oven Temp.:
35°C (hold 1min.) to 260°C@ 20°C/min. to 330°C@ 6°C/min. (hold 1min.)
Det:
MS
Transfer Line Temp.:
280°C
ScanRange:
35–550amu
Ionization:
EI
Mode:
scan
*20ppm **50ppm
Bold type indicates components of
OLC 03.2 SVMegaMix
™
(cat.# 31812)
OLC 03.2 SVMegaMix
™
(57 components)
Components listed in Figure 1 (bold)
1,000µg/mL each inmethylene chloride:benzene (75:25)
(3-methylphenol & 4-methylphenol at 500µg/mL), 1mL/ampul
Each
5-pk.
10-pk.
31812
31812-510
—
w/data pack
31812-500
31812-520
31912
For other referencemixes, refer to our catalog or web site.
ID df (µm)
temp. limits
30-Meter
0.25mm 0.25 -60 to 330/350°C 12723
Rtx
®
-5SilMS Column (fused silica)
New Semivolatiles ReferenceMix
for OLC 03.2 Statement ofWork
✔
All referencematerials needed for analysis of semivolatiles.
✔
NewMegaMix
™
includes 57 target compounds; co-eluters 3- and
4-methylphenol at one-half concentration of other semivolatiles.
✔
Fortificationmix includes seven semivolatiles that must be calibrated
at higher, variable concentrations.
✔
Deuteratedmonitoring compoundsmix for quality control.
RevisionOLC03.2 adds six compounds to the target list of CLP semivolatile analytes: acetophenone, atrazine, ben-
zaldehyde, 1,1'-biphenyl, caprolactam, and1,2,4,5-tetrachlorobenzene. Balancing economy, convenience and long
shelf life, Restek chemists have combined64 target compounds in twomixes: a new semivolatilesMegaMix
™
ref-
erencemix and a fortificationmix. OLC03.2 SVMegaMix
™
contains 57 analytes, at 1000µg/mL each, inmethanol-
freemethylene chloride.We include co-eluting isomers 3- and4-methylphenol at one-half the concentrationof the
other compounds, allowing these analytes tobe calibrated at lower detection limits (Figure 1). N-Nitrosodiphenyl-
amine decomposes todiphenylamine at theGC inlet. In formulating the newMegaMix
™
we include the compound
that is analyzed, diphenylamine, rather than the parent compound, N-nitrosodiphenylamine.
We designed the new FortificationMix to simplify the analysis— it includes the seven compounds thatmust be
calibrated at higher and variable concentrations, at 2000µg/mL each. To avoiddecomposition and reaction issues,
we offer 3,3'-dichlorobenzidine (cat.#31835) and
4-chloroaniline (cat.#31211) as individual solutions.
Because benzaldehyde reactswith alcohols, we use
methanol-freemethylene chloride toprepare theOLC
3.2 calibration and single componentmixes, to
improve the shelf-life of thesemixes. In addition, we
recommendworking dilutions be preparedwith
methanol-freemethylene chloride, to ensure stability.
Benzaldehyde also reacts rapidlywith4-chloroaniline
or 3,3'-dichlorobenzidine; the analyst should consider
generating a separate calibration curve for 4-
chloroaniline and3,3'-dichlorobenzidine, independ-
ent of the primary calibration curve.
OLC 03.2 specifies addition of deuteratedmonitoring
compounds to every semivolatiles sample, standard,
and blank. Our newOLC 03.2 SVOADeuterated
Monitoring Compounds (DMC)mixmeets the
requirement. Together with our Semivolatile Internal
StandardMix (cat.# 31206 or 31006), AcidMatrix
SpikeMix (cat.# 31005, 31075, or 31085),
Base/Neutral SpikeMix (cat.# 31492) and SV Tuning
Compound (cat.# 31001), the new formulations
make a full complement of referencematerials for
the semivolatiles listed inOLC 03.2 SOW.
Carefully formulated referencemixes and capillary
columns designed specifically for challenging environ-
mental analysesmakeRestek the perfect source for all
of your CLPmethods needs.
