Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Explosives (by Gas Chromatography)
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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.
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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
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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 . . . . . . .
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. 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
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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
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5003 ACS Reagent Chemicals, Part 5
