Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Polycyclic Aromatic 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 Polycyclic Aromatic 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 Melting Point, Assay by Gas Chromatography, Assay by Thin-Layer Chromatography, and Liquid Chromatography Suitability.
SPECIFICATIONS Identity by Gas chromatography−mass spectrometry. . . . . Passes test Melting point . . . . . . . . . . . . . . . . . . . . . . Passes test
Assay by Gas chromatography . . . . . . . . . . . . . . . . . ≥98.0% Thin-layer chromatography . . . . . . . . . . . . . Passes test
Specific Use Liquid chromatography suitability . . . . . . . . . Passes test
TESTS Identity by Gas Chromatography−Mass Spectrometry Analyze the sample by gas chromatography–mass spectrometry using method GCMS−PAH1 described below. Method GCMS−PAH1 Ionization Mode . . . . . . . . . . . . . . . . . . . . Electron ionization/70 eV Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Diphenyl–95% dimethylpolysiloxane, 30 m × 0.25 mm i.d., 0.25 µm film thickness
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5012 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Temperature Program. Carrier Gas . . . . . . . Injector . . . . . . . . . Injector Temperature . Scan Range . . . . . . . Sample Size . . . . . . .
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. 50 °C, then 10 °C/min to 310 °C, hold 10 min . Helium at 0.8 mL/min . Split/splitless (100:1 split) . 250 °C . 50–550 amu . 0.5 µL of a 1000 µg/mL solution
Identifying ions for the compound listed in Table 5-11 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.
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Table 5-11. Polycyclic Aromatic Hydrocarbons Compound Data
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/z) MS (m/z) MS (m/z) MP (°C) MS-1 MS-2 MS-3
Acenaphthene
83-32-9
C12H10
154.21
154
153
76
91–96
Acenaphthylene
208-96-8
C12H8
152.20
152
151
76
90–95
Anthracene
120-12-7
C14H10
178.23
178
176
89
214–219
Benz[a]anthracene
56-55-3
C18H12
228.29
228
226
114
158–163
Benzo[a]pyrene
50-32-8
C20H12
252.32
252
126
113
173–178
Benzo[b]fluoranthene
205-99-2
C20H12
252.32
252
126
113
166–171
Benzo[g,h,i]perylene
191-24-2
C22H12
276.34
276
277
138
277–282
Benzo[j]fluoranthene
205-82-3
C20H12
252.32
252
250
126
161–166
Benzo[k]fluoranthene
207-08-9
C20H12
252.32
252
126
133
215–220
Chrysene
218-01-9
C18H12
228.29
228
114
101
254–259
Dibenz[a,h]acridine
226-36-8
C21H13N
279.34
279
280
139
226–231
Dibenz[a,h]anthracene
53-70-3
C22H14
278.35
278
279
139
266–271
Dibenz[a,j]acridine
224-42-0
C21H13N
279.34
279
280
139
217–222
Dibenzo[a,e]pyrene
192-65-4
C24H14
302.37
302
303
151
242–247
Dibenzo[a,i]pyrene
189-55-9
C24H14
302.37
302
303
152
280–285
Fluoranthene
206-44-0
C16H10
202.26
202
101
88
108–113
Fluorene
86-73-7
C13H10
166.22
166
165
83
114–119
Indeno[1,2,3-c,d]pyrene
193-39-5
C22H12
276.34
276
274
138
158–163
3-Methylcholanthrene
56-49-5
C21H16
268.36
268
252
126
177–182
Naphthalene
91-20-3
C10H8
128.17
128
127
102
78–83
Phenanthrene
85-01-8
C14H10
178.23
178
176
152
97–102
Pyrene
129-00-0
C16H10
202.26
202
203
101
150–155
Note: MP = melting point.
Identity by Melting Point Analyze the sample by using the general procedure cited in [Part 2: Measurement of Physical Properties; Melting Point]. Assayed values must be within the ranges stated in Table 5-11.
Assay by Gas Chromatography Analyze the sample by gas chromatography using method GC–PAH1 described below.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5012 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Method GC–PAH1 Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Diphenyl–95% dimethylpolysiloxane, 30 m × 0.53 mm i.d., 1.5 µm film thickness Detector . . . . . . . . . . . . . . . . . . . . . . . . . Flame ionization Detector Temperature . . . . . . . . . . . . . . . . 325 °C Injector . . . . . . . . . . . . . . . . . . . . . . . . . Splitless Injector Temperature . . . . . . . . . . . . . . . . . 250 °C Sample Size . . . . . . . . . . . . . . . . . . . . . . . 1 µL of a 1000 µg/mL solution Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Hydrogen at 3.5 mL/min Temperature Program. . . . . . . . . . . . . . . . . 70 °C, then 10 °C/min to 310 °C, hold 10 min Measure the area under all peaks (excluding the solvent peak), and calculate the analyte content in area percent.
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Assay by Thin-Layer Chromatography Analyze the sample by thin-layer chromatography using the general procedure described in [Part 2: Chromatography; Recommended Procedures; Thin-Layer Chromatography]. The following specific conditions are also required. Stationary Phase . . . . . . . . . . . . . . . . . . . . Silica Mobile Phase . . . . . . . . . . . . . . . . . . . . . . 9:1 (v/v) Hexane:dichloromethane Detection Methods. . . . . . . . . . . . . . . . . . . UV at 254 nm and iodine Compound must exhibit a single spot.
Liquid Chromatography Suitability Analyze the sample by Method HPLC−PAH1 Column . . . . . . . . . . Mobile Phase . . . . . . Flow Rate . . . . . . . . Detector . . . . . . . . . Sensitivity . . . . . . . . Sample Size . . . . . . .
liquid chromatography using method HPLC-PAH1 described below. . . . . . .
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. Octadecyl, 250 mm × 4.6 mm i.d., 5 µm . 80:20 Acetonitrile:water . 2.0 mL/min . UV, 254 nm . 0.05 AUFS . 1 µL of a 100 µg/mL solution in acetonitrile
Measure the area under all peaks (excluding the solvent peak), and calculate the analyte and total impurities content in area percent. The sum of all impurity peaks should not exceed 5%, with no single peak greater than 3%.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5012 ACS Reagent Chemicals, Part 5
