Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Monocyclic 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 Monocyclic 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 Boiling Point, Identity by Melting Point, Identity by Relative Retention Index, and Assay by Gas Chromatography.
SPECIFICATIONS Identity by Gas chromatography−mass spectrometry. . . Boiling point (liquids) . . . . . . . . . . . . . . . Melting point (solids) . . . . . . . . . . . . . . . Relative retention index (for m-, o-, and pxylene only) . . . . . . . . . . . . . . . . . . . . .
. . Passes test . . Passes test . . Passes test . . 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−MCA1 described below. Method GCMS−MCA1 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 5 min, then 5 °C/min to 300 °C, hold 10 min
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5006 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Carrier Gas . . . . . . . Injector . . . . . . . . . Injector Temperature . Scan Range . . . . . . . Sample Size . . . . . . .
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. Helium 1.0 mL/min . Split/splitless (100:1 split) . 240 °C . 35–550 amu . 2 µL of a 1000 µg/mL solution
The identifying ions for the compound listed in Table 5-5 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 5-5. Monocyclic Aromatic Hydrocarbons Compound Data
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/ MS (m/ MS (m/ MP (°C) z) MS-1 z) MS-2 z) MS-3
BP (°C)
Benzal chloride
98-87-3
C7H6Cl2
161.03
125
160
202-207
Benzene
71-43-2
C6H6
78.11
78
52
Benzyl chloride
100-44-7
C7H7Cl
126.55
91
126
65
176–181
Bromobenzene
108-86-1
C6H5Br
157.00
77
156
51
153–158
n-Butylbenzene
104-51-8
C10H14
134.22
91
134
65
180–185
sec-Butylbenzene
135-98-8
C10H14
134.22
105
134
91
170–175
tert-Butylbenzene
98-06-6
C10H14
134.22
119
91
134
166–171
Chlorobenzene
108-90-7
C6H5Cl
112.56
112
77
51
129–134
2-Chlorotoluene
95-49-8
C7H7Cl
126.55
91
126
63
156–161
4-Chlorotoluene
106-43-4
C7H7Cl
126.55
91
126
63
159–164
1,2-Dichlorobenzene
95-50-1
C6H4Cl2
147.00
146
111
75
178–183
1,3-Dichlorobenzene
541-73-1
C6H4Cl2
147.00
146
111
75
1,4-Dichlorobenzene
106-46-7
C6H4Cl2
147.00
146
111
75
Ethylbenzene
100-41-4
C8H10
106.17
91
106
51
Hexachlorobenzene
118-74-1
C6Cl6
284.77
284
142
249
Isopropylbenzene
98-82-8
C9H12
120.20
105
120
77
150–155
4-Isopropyltoluene
99-87-6
C10H14
134.22
119
134
91
174–179
Pentachlorobenzene
608-93-5
C6HCl5
250.33
250
215
108
n-Propylbenzene
103-65-1
C9H12
120.20
91
120
38
156–161
Styrene
100-42-5
C8H8
104.15
104
91
78
142–147
1,2,3,4-Tetrachlorobenzene
634-66-2
C6H2Cl4
215.88
216
179
109
251–256
1,2,3,5-Tetrachlorobenzene
634-90-2
C6H2Cl4
215.88
216
179
108
52–57
1,2,4,5-Tetrachlorobenzene
95-94-3
C6H2Cl4
215.88
216
179
108
137–142
Toluene
108-88-3
C7H8
92.14
91
65
51
1,2,3-Trichlorobenzene
87-61-6
C6H3Cl3
181.44
180
145
109
1,2,4-Trichlorobenzene
120-82-1
C6H3Cl3
181.44
180
145
109
89
77-82
170–175 50–55 134–139 227–232
83–88
108–113 51–56 211–216
1,3,5-Trichlorobenzene
108-70-3
C6H3Cl3
181.44
180
145
109
a,a,a-Trichlorotoluene
98-07-7
C7H5Cl3
195.44
159
194
123
218–223
1,2,3-Trimethylbenzene
526-73-8
C9H12
120.20
105
120
77
173–178
1,2,4-Trimethylbenzene
95-63-6
C9H12
120.20
105
120
77
166–171
61–66
1,3,5-Trimethylbenzene
108-67-8
C9H12
120.20
105
120
77
162–167
m-Xylene
108-38-3
C8H10
106.17
91
106
51
136–141
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5006 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Table 5-5. Monocyclic Aromatic Hydrocarbons Compound Data (continued)
Name
CAS No.
Chemical Formula
Formula Weight
MS (m/ MS (m/ MS (m/ MP (°C) z) MS-1 z) MS-2 z) MS-3
BP (°C)
o-Xylene
95-47-6
C8H10
106.17
91
106
51
141–146
p-Xylene
106-42-3
C8H10
106.17
91
106
51
135–140
Note: MP = melting point; BP = boiling point.
Identity by Boiling Point Analyze the liquid sample using the procedure cited in [Part 2: Measurement of Physical Properties; Boiling Point Range]. Boiling point values must be within the ranges listed in Table 5-5.
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Identity by Melting Point Analyze the solid sample using the procedure cited in [Part 2: Measurement of Physical Properties; Melting Point]. Melting point values must be within the ranges listed in Table 5-5.
Identity by Relative Retention Index Prepare a solution by adding equal amounts of the sample and toluene in a suitable solvent for a final concentration of 500 µg/mL. Analyze the sample by gas chromatography using method GC–MCA1 described below. Calculate the relative retention time of the sample versus toluene by dividing the retention time of the sample by the retention time of toluene. Assayed values must be within 1% of 1.63 for m-xylene, 1.90 for o-xylene, and 1.59 for p-xylene.
Assay by Gas Chromatography Analyze the sample by gas chromatography using method GC–MCA1 and method GC–MCA2 described below. Method GC−MCA1 Column . . . . . . . . . . Detector . . . . . . . . . Detector Temperature Injector . . . . . . . . . Injector Temperature . Sample Size . . . . . . . Carrier Gas . . . . . . . Temperature Program.
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. Polyethylene glycol, 30 m × 0.53 mm i.d., 1.0 µm film thickness . Flame ionization . 200 °C . Splitless . 200 °C . 2 µL of a 1000 µg/mL solution . Helium at 5 mL/min . 35 °C for 10 min, then 2.5 °C/min to 200 °C
Method GC–MCA2 Column . . . . . . . . . . . . . . . . . . . . . . . . . . 6% Cyanopropylphenyl–94% dimethylpolysiloxane, 75 m × 0.53 mm i.d., 3.0 µm film thickness Detector . . . . . . . . . . . . . . . . . . . . . . . . . Flame ionization Detector Temperature . . . . . . . . . . . . . . . . 200 °C Injector . . . . . . . . . . . . . . . . . . . . . . . . . Splitless Injector Temperature . . . . . . . . . . . . . . . . . 200 °C Sample Size . . . . . . . . . . . . . . . . . . . . . . . 2 µL of a 1000 µg/mL solution Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 10 mL/min Temperature Program. . . . . . . . . . . . . . . . . 70 °C, then 5 °C/min to 210 °C, hold 10 min
© 2017 American Chemical Society
C
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5006 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.5006
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
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5006 ACS Reagent Chemicals, Part 5
