Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Halogenated 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 Halogenated 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 and Assay by Gas Chromatography.
SPECIFICATIONS Identity by Gas chromatography−mass spectrometry. . . . . 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–HHC1 described below. Method GCMS−HHC1 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 10 min, then 4 °C/min to 200 °C, hold 10 min Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 0.8 mL/min Injector . . . . . . . . . . . . . . . . . . . . . . . . . Split/splitless (100:1 split) Injector Temperature . . . . . . . . . . . . . . . . . 200 °C Scan Range . . . . . . . . . . . . . . . . . . . . . . . 35–400 amu Sample Size . . . . . . . . . . . . . . . . . . . . . . . 1 µL of a 100 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.5004 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
The spectrum must comply with either identifying ions for the compound listed in Table 5-3 or the spectrum listed for the compound in the NIST standardized library of compounds.
Downloaded by CORNELL UNIV on June 15, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5004
Table 5-3. Halogenated Hydrocarbons Compound Data
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/z) MS-1
MS (m/z) MS-2
MS (m/z) MS-3
Allyl chloride
107-05-1
C3H5Cl
76.53
41
76
78
1-Bromo-2-chloroethane
107-04-0
C2H4BrCl
143.41
63
142
65
2-Bromo-1-chloropropane
3017-95-6
C3H6BrCl
157.44
77
156
79
Bromochloromethane
74-97-5
CH2BrCl
129.38
49
128
130
Bromodichloromethane
75-27-4
CHBrCl2
163.82
83
127
85
Bromoethane
74-96-4
C2H5Br
108.97
108
110
79
Bromoform
75-25-2
CHBr3
252.73
173
250
171
Carbon tetrachloride
56-23-5
CCl4
153.81
117
119
82
3-Chloro-2-methylpropene
563-47-3
C4H7Cl
90.55
55
90
75
1-Chlorobutane
109-69-3
C4H9Cl
92.57
56
63
41
Chlorodibromomethane
124-48-1
CHBr2Cl
208.28
127
206
129
Chloroform
67-66-3
CHCl3
119.37
83
117
85
1-Chlorohexane
544-10-5
C6H13Cl
120.62
91
93
69
1,2-Dibromo-3-chloropropane
96-12-8
C3H5ClBr2
236.33
157
155
75
1,2-Dibromoethane
106-93-4
C2H4Br2
187.86
107
186
109
Dibromofluoromethane
1868-53-7
CHBr2F
191.83
111
190
113
Dibromomethane
74-95-3
CH2Br2
173.84
174
172
93
cis-1,4-Dichloro-2-butene
1476-11-5
C4H6Cl2
125.00
53
88
75
trans-1,4-Dichloro-2-butene
110-57-6
C4H6Cl2
125.00
75
124
53
1,3-Dichlorobutane
1190-22-3
C4H8Cl2
127.01
55
90
63
1,4-Dichlorobutane
110-56-5
C4H8Cl2
127.01
55
90
62
1,1-Dichloroethane
75-34-3
C2H4Cl2
98.95
63
98
83
1,2-Dichloroethane
107-06-2
C2H4Cl2
98.95
62
98
64
1,1-Dichloroethene
75-35-4
C2H2Cl2
96.94
61
96
63
cis-1,2-Dichloroethene
156-59-2
C2H2Cl2
96.94
61
96
63
trans-1,2-Dichloroethene
156-60-5
C2H2Cl2
96.94
61
96
98
1,2-Dichloropropane
78-87-5
C3H6Cl2
112.98
63
112
76
1,3-Dichloropropane
142-28-9
C3H6Cl2
112.98
76
112
78
2,2-Dichloropropane
594-20-7
C3H6Cl2
112.98
77
97
41
1,1-Dichloropropene
563-58-6
C3H4Cl2
110.97
75
109
77
Diiodomethane
75-11-6
CH2I2
267.84
268
141
127
Hexachlorobutadiene
87-68-3
C4Cl6
260.74
225
258
190
Hexachlorocyclopentadiene
77-47-4
C5Cl6
272.76
237
270
235
Hexachloroethane
67-72-1
C2Cl6
236.72
117
201
119
Hexachloropropene
1888-71-7
C3Cl6
248.73
213
246
141
Iodomethane
74-88-4
CH3I
141.94
142
127
141
Methylene chloride
75-09-2
CH2Cl2
84.93
49
84
86
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5004 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Downloaded by CORNELL UNIV on June 15, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5004
Table 5-3. Halogenated Hydrocarbons Compound Data (continued)
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/z) MS-1
MS (m/z) MS-2
MS (m/z) MS-3
Pentachloroethane
76-01-7
C2HCl5
202.28
117
167
119
Tetrachloroethene
127-18-4
C2Cl4
165.82
166
164
131
1,1,1,2-Tetrachloroethane
630-20-6
C2H2Cl4
167.84
131
117
95
1,1,2,2-Tetrachloroethane
79-34-5
C2H2Cl4
167.84
83
166
95
1,1,1-Trichloroethane
71-55-6
C2H3Cl3
133.40
97
99
61
1,1,2-Trichloroethane
79-00-5
C2H3Cl3
133.40
97
132
83
Trichloroethene
79-01-6
C2HCl3
131.38
95
130
132
1,2,3-Trichloropropane
96-18-4
C3H5Cl3
147.42
75
110
61
Assay by Gas Chromatography Analyze the sample by gas chromatography using method GC–HHC1 described below. Method GC–HHC1 Column . . . . . . . . . . . . . . . . . . . . . . . . . . 3% Diphenyl–3% cyanopropyl–94% dimethylpolysiloxane, 30 m × 0.53 mm i.d., 3.0 µm film thickness Detector . . . . . . . . . . . . . . . . . . . . . . . . . Thermal conductivity Detector Temperature . . . . . . . . . . . . . . . . 300 °C Injector . . . . . . . . . . . . . . . . . . . . . . . . . Split/splitless (10:1 split) Injector Temperature . . . . . . . . . . . . . . . . . 200 °C Sample Size . . . . . . . . . . . . . . . . . . . . . . . 2 µL of a 1000 µg/mL solution Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 3.0 mL/min Temperature Program. . . . . . . . . . . . . . . . . 35 °C for 10 min, then 4 °C/min to 200 °C, hold 9 min Measure the area under all peaks (excluding the solvent peak), and calculate the analyte content in area percent for each analysis.
© 2017 American Chemical Society
C
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5004 ACS Reagent Chemicals, Part 5
