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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

C

ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.

DOI:10.1021/acsreagents.5012 ACS Reagent Chemicals, Part 5