Explosives - ACS Reagent Chemicals (ACS Publications)

Feb 28, 2017 - This ACS Reagent Chemicals Standard-Grade Reference Materials monograph for Explosives, in addition to common physical constants, detai...
0 downloads 10 Views 67KB Size
Monograph pubs.acs.org/doi/book/10.1021/acsreagents

Explosives (by Gas Chromatography)

Downloaded by CORNELL UNIV on June 1, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5003

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

ABSTRACT This ACS Reagent Chemicals Standard-Grade Reference Materials monograph for Explosives, 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 Boiling Point, Identity by Melting Point, Assay by Gas Chromatography, and Assay by Thin-Layer Chromatography.

SPECIFICATIONS Identity by Gas chromatography−mass spectrometry. . . . . Passes test Melting point (solids) . . . . . . . . . . . . . . . . . Passes test

Assay by Gas chromatography . . . . . . . . . . . . . . . . . ≥98% Thin-layer chromatography . . . . . . . . . . . . . Passes test

TESTS Identity by Gas Chromatography−Mass Spectrometry Analyze the sample by gas chromatography−mass spectrometry using GCMS−EXP1 described below. Method GCMS–EXP1 Ionization Mode . . . . . . . . . . . . . . . . . . . . Electron ionization/70 eV Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Phenyl–95% dimethylpolysiloxane, 30 m × 0.25 mm i.d., 0.25 µm film thickness Temperature Program. . . . . . . . . . . . . . . . . 75 °C for 1 min, then 10 °C/min to 275 °C, hold 5 min Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 1 mL/min Injector . . . . . . . . . . . . . . . . . . . . . . . . . Split/splitless (20:1 split) Injector Temperature . . . . . . . . . . . . . . . . . 250 °C

© 2017 American Chemical Society

A

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

DOI:10.1021/acsreagents.5003 ACS Reagent Chemicals, Part 5

ACS Reagent Chemicals

Monograph

pubs.acs.org/doi/book/10.1021/acsreagents

Scan Range . . . . . . . . . . . . . . . . . . . . . . . 40–650 amu Sample Size . . . . . . . . . . . . . . . . . . . . . . . 1.0 µL of a 1 mg/mL solution The identifying ions listed in Table 5-2A 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 reference spectrum.

Downloaded by CORNELL UNIV on June 1, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5003

Table 5-2A. Explosives by Gas Chromatography Compound Data

Name

CAS No.

Chemical Formula

Formula Weight

MS (m/ MS (m/ MS (m/ MP(°C) z) z) z) MS-1 MS-2 MS-3

2-Amino-4,6-dinitrotoluene

35572-78-2

C7H7N3O4

197.15

197

180

78

182-187

4-Amino-2,6-dinitrotoluene

19406-51-0

C7H7N3O4

197.15

197

180

163

183-188

2,4-Diamino-6-nitrotoluene

6629-29-4

C7H9N3O2

167.17

167

150

121

131-136

2,6-Diamino-4-nitrotoluene

59229-75-3

C7H9N3O2

167.17

167

121

94

216-221

2,3-Dimethyl-2,3-dinitrobutane

3964-18-9

C6H12N2O4

176.17

100

69

57

211-216

1,2-Dinitrobenzene

528-29-0

C6H4N2O4

168.11

168

76

63

115-120

1,3-Dinitrobenzene

99-65-0

C6H4N2O4

168.11

168

122

75

3,5-Dinitroaniline

618-87-1

C6H5N3O4

183.12

183

137

91

162-167

2,4-Dinitrotoluene

121-14-2

C7H6N2O4

182.14

165

119

89

66-71

2,6-Dinitrotoluene

606-20-2

C7H6N2O4

182.14

165

89

63

62-67

3,4-Dinitrotoluene

610-39-9

C7H6N2O4

182.14

182

89

63

53-58

BP(°C)

294-299

Nitrobenzene

98-95-3

C6H5NO2

123.11

123

77

51

208-213

2-Nitrotoluene

88-72-2

C7H7NO2

137.14

137

120

65

119-124

3-Nitrotoluene

99-08-1

C7H7NO2

137.14

137

91

65

235-240

4-Nitrotoluene

99-99-0

C7H7NO2

137.14

137

91

65

52-57

Picramic acid

831-52-7

C6H5N3O5

199.12

199

153

106

166-171

Triacetone triperoxide

17088-37-8

C9H18O6

222.24

59

75

222

94-96

1,3,5-Trinitro-benzene

99-35-4

C6H3N3O6

213.11

75

213

120

121-122

2,4,6-Trinitro-toluene

118-96-7

C7H5N3O6

227.13

210

89

63

80-81

Note: MP = melting point; BP = boiling point.

Identity by Boiling Point Analyze the sample using the general procedure described in [Part 2: Measurement of Physical Properties; Boiling Point Range]. Assigned values must be within the ranges listed in Table 5-2A.

Identity by Melting Point Analyze the sample using the general procedure described in [Part 2: Measurement of Physical Properties; Melting Point]. Assigned values must be within the ranges listed in Table 5-2A.

Assay by Gas Chromatography Analyze the sample by gas chromatography using method GCFID-EXP1 described below. Method GCFID−EXP1 Column . . . . . . . . . . . . . . . . . . . . . . . . . . 5% Phenyl–95% dimethylpolysiloxane, 30 m × 0.53 mm i.d., 1.0 µm film thickness

© 2017 American Chemical Society

B

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

DOI:10.1021/acsreagents.5003 ACS Reagent Chemicals, Part 5

ACS Reagent Chemicals

Monograph

pubs.acs.org/doi/book/10.1021/acsreagents

Temperature Program. Carrier Gas . . . . . . . Injector . . . . . . . . . Injector Temperature . Detector Temperature Sample Size . . . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. . . . . .

. 75 °C for 1 min, then 10 °C/min to 275 °C, hold 5 min . Helium at 5 mL/min . Split/splitless (20:1) . 250 °C . 280 °C . 1.0 µL of a 1 mg/mL solution

Measure the area under each peak (excluding the solvent peak) and calculate the analyte content in area percent.

Assay by Thin-Layer Chromatography

Downloaded by CORNELL UNIV on June 1, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5003

Analyze the sample by thin-layer chromatography using the general procedure described in [Part 2: Chromatography; Recommended Procedures; Thin-Layer Chromatography]. Compound must exhibit a single spot.

© 2017 American Chemical Society

C

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

DOI:10.1021/acsreagents.5003 ACS Reagent Chemicals, Part 5