Correction to “Process Safety Considerations for the Use of 1 M

2 days ago - Correction to “Process Safety Considerations for the Use of 1 M Borane Tetrahydrofuran Complex under General Purpose Plant Conditionsâ€...
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Addition/Correction Cite This: Org. Process Res. Dev. XXXX, XXX, XXX−XXX

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Correction to “Process Safety Considerations for the Use of 1 M Borane Tetrahydrofuran Complex under General Purpose Plant Conditions” Alexandre M. Monteiro* and Roy C. Flanagan*

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Org. Process Res. Dev. 2017, 21 (2), 241−246. DOI: 10.1021/acs.oprd.6b00407 The Hiden Analytical mass spectrometer was running MASsoft 7 Professional (Version 7.23.0.81) and was programmed to scan for mass to charge ratios (m/z) corresponding to expected BTHF decomposition species (see Table 3) using Table 3. Mass Spectrometer Scan Parameters

a

species

m/z

relative sensitivity

hydrogen diborane argon tetrahydrofuran tetraborane tributoxyborane pentaborane(9) pentaborane(11) hexaborane

2 26 40 42 48 57 59 61 71

0.78a 1.00b 1.20b 2.57a 1.00c 1.00c 1.00c 1.00c 1.00c

Experimentally determined. Unknown, defaulted to 1.00.

c

b

Reported by Hiden Analytical.

the multiple ion detection mode (MID). The relative sensitivity (RS) value for hydrogen (Sigma-Aldrich, St. Louis, MO) was experimentally obtained by flowing a known concentration of gas in nitrogen past the mass spectrometer’s inlet tee. The RS value was then adjusted until the average concentration reported by mass spectroscopy data matched the known gas concentration. Tetrahydrofuran’s RS was obtained by evaporating a small sample of liquid placed on top of a balance under a known nitrogen flow rate. The mass loss rate was used to calculate the concentration of solvent vapor in nitrogen, which was then used to calculate the RS value following the same procedure detailed for hydrogen. Due to tributoxyborane’s extremely low vapor pressure at room temperature and the difficulty of obtaining/handling higher boranes, the RS values for these species were defaulted to 1.00. Since these species are likely to make up only a minute amount of total gas flow, their impact on the total mass balance of decomposing products is expected to be minimal.

© XXXX American Chemical Society

A

DOI: 10.1021/acs.oprd.8b00419 Org. Process Res. Dev. XXXX, XXX, XXX−XXX