Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Straight-Chain Hydrocarbons Part 5, Assay and Identification of Standard-Grade Reference Materials: Specifications and Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents
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ABSTRACT This ACS Reagent Chemicals Standard-Grade Reference Materials monograph for Straight-Chain Hydrocarbons, in addition to common physical constants, details the following specifications and corresponding tests for verifying that a substance meets ACS Standard-Grade specifications including: Identity by Gas Chromatography−Mass Spectrometry, Identity by Relative Retention Index, and Assay by Gas Chromatography.
SPECIFICATIONS Identity by Gas chromatography−mass spectrometry. . . . . Passes test Relative retention index . . . . . . . . . . . . . . . Passes test
Assay by Gas chromatography (using two methods) . . . . ≥98.0%
TESTS Identity by Gas Chromatography−Mass Spectrometry Analyze the sample by gas chromatography–mass spectrometry using method GCMS−SCHC1 described below. Method GCMS−SCHC1 Ionization Mode . . . . . . . . . . . . . . . . . . . . Electron ionization/70 eV Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Diphenyl–95% dimethylpolysiloxane, 30 m × 0.25 mm i.d., 0.25 µm film thickness Temperature Program. . . . . . . . . . . . . . . . . 35 °C for 5 min, then 30 °C/min to 320 °C, then hold 5 min Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 1 mL/min Injector . . . . . . . . . . . . . . . . . . . . . . . . . Split/splitless (100:1 split) Injector Temperature . . . . . . . . . . . . . . . . . 250 °C Scan Range . . . . . . . . . . . . . . . . . . . . . . . 32–600 amu Sample Size . . . . . . . . . . . . . . . . . . . . . . . 1 µL of a 1000 µg/mL solution
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5013 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
The identifying ions for the compound listed in Table 5-12 must be present. The spectrum is compared to the NIST standardized library of compounds, if available. Ions in the test spectrum must match those found in the NIST spectrum.
Downloaded by CORNELL UNIV on June 15, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5013
Table 5-12. Straight-Chain Hydrocarbons Compound Data
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/z) MS (m/z) MS (m/z) Relative MS-1 MS-2 MS-3 Retention
Decane
124-18-5
C10H22
142.29
43
142
57
1.000
Docosane
629-97-0
C22H46
310.61
43
57
71
1.578
Dodecane
112-40-3
C12H26
170.34
43
170
57
1.132
Dotriacontane
544-85-4
C32H66
450.88
43
57
71
1.989
Eicosane
112-95-8
C20H42
282.56
57
282
71
1.503
Heneicosane
629-94-7
C21H44
296.58
43
57
71
1.541
Hentriacontane
630-04-6
C31H64
436.85
43
57
71
1.927
Heptacosane
593-49-7
C27H56
380.75
43
57
71
1.752
Heptadecane
629-78-7
C17H36
240.48
57
240
71
1.382
Heptane
142-82-5
C7H16
100.21
43
100
71
0.528
Heptatriacontane
NA
C37H76
521.02
43
57
71
2.514
Hexacosane
630-01-3
C26H54
366.72
43
57
71
1.718
Hexadecane
544-76-3
C16H34
226.45
57
226
71
1.337
Hexane
110-54-3
C6H14
86.18
57
86
43
0.268
Hexatriacontane
630-06-8
C36H74
506.99
43
57
71
2.362
Nonacosane
630-03-5
C29H60
408.80
43
57
71
1.828
Nonadecane
629-92-5
C19H40
268.53
57
268
71
1.465
Nonane
111-84-2
C9H20
128.26
43
128
57
0.913
Octacosane
630-02-4
C28H58
394.77
43
57
71
1.788
Octadecane
593-45-3
C18H38
254.50
57
254
43
1.424
Octane
111-65-9
C8H18
114.23
43
114
85
0.791
Octatriacontane
7194-85-6
C38H78
535.04
43
57
71
2.666
Pentacosane
629-99-2
C25H52
352.69
43
57
71
1.684
Pentadecane
629-62-9
C15H32
212.42
57
212
71
1.291
Pentatriacontane
630-07-9
C35H72
492.96
43
57
71
2.243
Tetracontane
4181-95-7
C40H82
563.10
43
57
71
3.097
Tetracosane
646-31-1
C24H50
338.66
43
57
71
1.649
Tetradecane
629-59-4
C14H30
198.39
43
198
57
1.241
Tetratriacontane
14167-59-0
C34H70
478.93
43
57
71
9.88
Triacontane
638-68-6
C30H62
422.83
43
57
71
1.874
Tricosane
638-67-5
C23H48
324.64
43
57
71
1.614
Tridecane
629-50-5
C13H28
184.37
43
184
57
1.189
Tritriacontane
630-05-7
C33H68
464.91
43
57
71
2.060
Undecane
1120-21-4
C11H24
156.31
43
156
57
1.070
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5013 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Identity by Relative Retention Index
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Prepare a solution by adding equal amounts of the sample and n-decane in a suitable solvent for a final concentration of 500 µg/mL. Analyze the sample by gas chromatography using method GC–SCHC1 described below. Method GC−SCHC1 Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Diphenyl–95% dimethylpolysiloxane, 30 m × 0.53 mm i.d., 1.5 µm film thickness Detector . . . . . . . . . . . . . . . . . . . . . . . . . Flame ionization Detector Temperature . . . . . . . . . . . . . . . . 300 °C Injector . . . . . . . . . . . . . . . . . . . . . . . . . Splitless Injector Temperature . . . . . . . . . . . . . . . . . 250 °C Sample Size . . . . . . . . . . . . . . . . . . . . . . . 1 µL Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 5 mL/min Temperature Program. . . . . . . . . . . . . . . . . 35 °C for 5 min, then 30 °C/min to 320 °C, then hold 10 min Calculate the relative retention time of the sample versus n-decane by dividing the retention time of the sample by the retention time of n-decane. Assayed values must be within 1% of the stated values in Table 5-10.
Assay by Gas Chromatography Analyze the sample by gas below. Method GC–SCHC2 Column . . . . . . . . . . . . . Detector . . . . . . . . . . . . Detector Temperature . . . Injector . . . . . . . . . . . . Injector Temperature . . . . Sample Size . . . . . . . . . . Carrier Gas . . . . . . . . . . Temperature Program. . . .
chromatography using method GC–SCHC1 described above and method GC–SCHC2 described
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. 100% Dimethylpolysiloxane, 25 m × 0.25 mm i.d., 0.25 µm film thickness . Flame ionization . 300 °C . Split/splitless (100:1 split) . 250 °C . 1 µL of a 1000 µg/mL solution . Helium at 5 mL/min . 35 °C for 5 min, then 30 °C/min to 320 °C, then hold 10 min
Measure the area under all peaks (excluding the solvent peak), and calculate the analyte content in area percent.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5013 ACS Reagent Chemicals, Part 5
