ADV01-05_1-298

• 7 •

www.restekcorp.com

2003

Volume 3

800-356-1688

By Katia May, Ph.D., R&D Chemist, and Gary Stidsen, Innovations Team Manager

4,6-dinitro-2-methylphenol

2,4-dinitrophenol

2-nitroaniline

3-nitroaniline

4-nitroaniline

4-nitrophenol

2,4,5-trichlorophenol

Fortification Mix

(7 components)

2,000µg/mL each in methylene 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

OLC 03.2 SVOA Deuterated Monitoring

Compounds (DMC)

(16 components)

2,000µg/mL each in methylene chloride, 1mL/ampul

Each

5-pk.

31810

31810-510

Figure 1

- Excellent resolution and rapid analysis of OLC 03.2 semivolatile compounds, using

an Rtx

-5Sil MS column and new Restek reference mixes.

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-

-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-

-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-

-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 0.4 min.), Drilled Uniliner

(cat.# 20756)

Inj. Temp.:

275°C

Carrier Gas:

helium, constant flow

Flow Rate:

1mL/min.

Oven Temp.:

35°C (hold 1 min.) to 260°C @ 20°C/min. to 330°C @ 6°C/min. (hold 1 min.)

Det:

Transfer Line Temp.:

280°C

Scan Range:

35–550amu

Ionization:

Mode:

scan

*20ppm **50ppm

Bold type indicates components of

OLC 03.2 SV MegaMix

™

(cat.# 31812)

OLC 03.2 SV MegaMix

™

(57 components)

Components listed in Figure 1 (bold)

1,000µg/mL each in methylene 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 reference mixes, 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

-5Sil MS Column (fused silica)

New Semivolatiles Reference Mix

for OLC 03.2 Statement of Work

✔

All reference materials needed for analysis of semivolatiles.

✔

New MegaMix

™

includes 57 target compounds; co-eluters 3- and

4-methylphenol at one-half concentration of other semivolatiles.

✔

Fortification mix includes seven semivolatiles that must be calibrated

at higher, variable concentrations.

✔

Deuterated monitoring compounds mix for quality control.

Revision OLC 03.2 adds six compounds to the target list of CLP semivolatile analytes: acetophenone, atrazine, ben-

zaldehyde, 1,1'-biphenyl, caprolactam, and 1,2,4,5-tetrachlorobenzene. Balancing economy, convenience and long

shelf life, Restek chemists have combined 64 target compounds in two mixes: a new semivolatiles MegaMix

™

ref-

erence mix and a fortification mix. OLC 03.2 SV MegaMix

™

contains 57 analytes, at 1000µg/mL each, in methanol-

free methylene chloride. We include co-eluting isomers 3- and 4-methylphenol at one-half the concentration of the

other compounds, allowing these analytes to be calibrated at lower detection limits (Figure 1). N-Nitrosodiphenyl-

amine decomposes to diphenylamine at the GC inlet. In formulating the new MegaMix

™

we include the compound

that is analyzed, diphenylamine, rather than the parent compound, N-nitrosodiphenylamine.

We designed the new Fortification Mix to simplify the analysis — it includes the seven compounds that must be

calibrated at higher and variable concentrations, at 2000µg/mL each. To avoid decomposition and reaction issues,

we offer 3,3'-dichlorobenzidine (cat.# 31835) and

4-chloroaniline (cat.# 31211) as individual solutions.

Because benzaldehyde reacts with alcohols, we use

methanol-free methylene chloride to prepare the OLC

3.2 calibration and single component mixes, to

improve the shelf-life of these mixes. In addition, we

recommend working dilutions be prepared with

methanol-free methylene chloride, to ensure stability.

Benzaldehyde also reacts rapidly with 4-chloroaniline

or 3,3'-dichlorobenzidine; the analyst should consider

generating a separate calibration curve for 4-

chloroaniline and 3,3'-dichlorobenzidine, independ-

ent of the primary calibration curve.

OLC 03.2 specifies addition of deuterated monitoring

compounds to every semivolatiles sample, standard,

and blank. Our new OLC 03.2 SVOA Deuterated

Monitoring Compounds (DMC) mix meets the

requirement. Together with our Semivolatile Internal

Standard Mix (cat.# 31206 or 31006), Acid Matrix

Spike Mix (cat.# 31005, 31075, or 31085),

Base/Neutral Spike Mix (cat.# 31492) and SV Tuning

Compound (cat.# 31001), the new formulations

make a full complement of reference materials for

the semivolatiles listed in OLC 03.2 SOW.

Carefully formulated reference mixes and capillary

columns designed specifically for challenging environ-

mental analyses make Restek the perfect source for all

of your CLP methods needs.