Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Polybrominated Diphenyl Ethers 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
Downloaded by NEW YORK UNIV on May 18, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5010
ABSTRACT This ACS Reagent Chemicals Standard-Grade Reference Materials monograph for Polybrominated Diphenyl Ethers, 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, and Assay by Gas Chromatography.
SPECIFICATIONS Identity by Gas chromatography–mass spectrometry . . . . . Passes test Melting point . . . . . . . . . . . . . . . . . . . . . . Passes test
Assay by Gas chromatography . . . . . . . . . . . . . . . . . ≥98.0%
TESTS Identity by Gas Chromatography−Mass Spectrometry Analyze the sample by gas chromatography–mass spectrometry using method GCMS–PBDE1 described below. Method GCMS–PBDE1 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. . . . . . . . . . . . . . . . . 140 °C for 1 min, then 10 °C/min to 340 °C, then hold 10 min Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . Helium at 1 mL/min Injector . . . . . . . . . . . . . . . . . . . . . . . . . Splitless Injector Temperature . . . . . . . . . . . . . . . . . 280 °C Scan Range . . . . . . . . . . . . . . . . . . . . . . . 50–1000 amu Sample Size . . . . . . . . . . . . . . . . . . . . . . . 2 µL of a 50 µg/mL solution in isooctane (for PBDE #209, use 1000 ppm).
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5010 ACS Reagent Chemicals, Part 5
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Identity by Melting Point Analyze the sample using the procedure in [Part 2: Measurement of Physical Properties; Melting Point]. Melting point values must be within the ranges listed in Table 5-9.
Downloaded by NEW YORK UNIV on May 18, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.5010
Table 5-9. Polybrominated Diphenyl Ether Compound Data
PB
Compound Name
CAS No.
Chemical Formula
Formula Weight
Ions
MP (°C)
28
2,4,4′-Tribromodiphenyl ether
41318-75-6
C12H7Br3O
406.90
406/246/ 139
55–56
47
2,2′,4,4′-Tetrabromodiphenyl ether
5436-43-1
C12H6Br4O
485.79
326/486/ 163
82–84
66
2,3′,4,4′-Tetrabromodiphenyl ether
189084-61-5
C12H6Br4O
485.79
326/486/ 163
6–7
71
2,3′,4′,6-Tetrabromodiphenyl ether
189084-62-6
C12H6Br4O
485.79
326/486/ 163
133–134
85
2,2′,3,4,4′-Pentabromodiphenyl ether
182346-21-0
C12H5Br5O
564.69
404/564/ 202
134–135
99
2,2′,4,4′,5-Pentabromodiphenyl ether
60348-60-9
C12H5Br5O
564.69
406/564/ 202
92–93
100
2,2′,4,4’,6-Pentabromodiphenyl ether
189084-64-8
C12H5Br5O
564.69
404/564/ 296
88–89
153
2,2′,4,4′,5,5′-Hexabromodiphenyl ether
68631-49-2
C12H4Br6O
643.58
484/644/ 242
153–154
154
2,2′,4,4′,5,6′-Hexabromodiphenyl ether
207122-15-4
C12H4Br6O
643.58
484/242/ 644
134–135
183
2,2′,3,4,4′,5′,6-Heptabromodiphenyl ether 207122-16-5
C12H3Br7O
722.48
562/718/ 280
158–160
Note: MP = melting point.
Assay by Gas Chromatography Analyze the sample by gas chromatography using method GCMS−PBDE1 described above. Measure the area under all peaks except the solvent. Calculate the area percent for the major peak.
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.5010 ACS Reagent Chemicals, Part 5
