Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Tetrahydrofuran Part 4, Monographs for Reagent Chemicals: General Descriptions, Specifications, and Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents
Downloaded by CORNELL UNIV on June 14, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4396
ABSTRACT This monograph for Tetrahydrofuran provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), aqueous solubility, density, and pKa. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Color (APHA), Peroxide, Residue after Evaporation, Water. Special caution is advised for the handling or testing of this substance.
C4H8O
Formula Wt 72.11
CAS No. 109-99-9
Note: Generally, a stabilizer is present to retard peroxide formation.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . . pKa . . . . . . . . . . . . . . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
. . . . . .
clear, colorless liquid solvent boiling point, 67 °C miscible 0.89 –2.2
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% C4H8O Maximum Allowable Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 20
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4396 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Peroxide (as H2O2). . . . . . . . . . . . . . . . . . . . 0.015% Residue after evaporation . . . . . . . . . . . . . . . 0.03% Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.05%
TESTS Assay Analyze the sample by gas chromatography using the general parameters cited in [Part 2: Chromatography; Recommended Procedures; Gas Chromatography]. The following specific conditions are also required. Column . . . . . . . . . . . . . . . . . . . . . . . . . . Type I, methyl silicone
Downloaded by CORNELL UNIV on June 14, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4396
Measure the area under all peaks, and calculate the tetrahydrofuran content in area percent. Correct for water content.
Color (APHA) [Part 2: Measurement of Physical Properties; Color (APHA); Procedure for Color (APHA)].
Peroxide To 44.0 g (50 mL) in a conical flask, add 10 mL of 10% potassium iodide solution and 2 mL of 10% sulfuric acid reagent solution. Titrate the liberated iodine with 0.1 N sodium thiosulfate volumetric solution. Not more than 3.9 mL should be required. C a u t i o n : If peroxide is present, do not perform the test for residue after evaporation.
Residue after Evaporation [Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 20.0 g (22.5 mL) to dryness in a tared, preconditioned dish on a hot plate (~100 °C), and dry the residue at 105 °C for 30 min.
Water [Part 2: Titrimetric Methods; Water by the Karl Fischer Method; Coulometric Procedure; Coulometric Procedure for Samples Using Karl Fischer Reagent, Method 2]. Use 100 µL (88 mg).
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4396 ACS Reagent Chemicals, Part 4
