Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Butyl Alcohol (1-Butanol) 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
ABSTRACT This monograph for Butyl Alcohol provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), aqueous solubility, and density. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Butyl Ether, Color (APHA), Residue after Evaporation, Titrable Acid, and Carbonyl Compounds.
CH3(CH2)2CH2OH
Formula Wt 74.12
CAS No. 71-36-3
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . .
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clear, colorless liquid solvent boiling point, 118 °C 7.4 g in 100 mL 0.81
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.4% CH3(CH2)2CH2OH Maximum Allowable Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 10 Residue after evaporation . . . . . . . . . . . . . . . 0.005% Titrable acid . . . . . . . . . . . . . . . . . . . . . . . 0.0008 meq/g Carbonyl compounds (as butyraldehyde) . . . . . . 0.01% Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.1% Butyl ether (C8H18O) . . . . . . . . . . . . . . . . . . 0.2%
© 2017 American Chemical Society
A
DOI:10.1021/acsreagents.4068 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay and Butyl Ether 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 Measure the areas under all peaks, and calculate the butyl alcohol and butyl ether content in area percent. Correct for water content.
Color (APHA) [Part 2: Measurement of Physical Properties; Color (APHA); Procedure for Color (APHA)].
Residue after Evaporation [Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 20 g (25 mL) to dryness in a tared, preconditioned platinum dish on a hot plate (~100 °C), and dry the residue at 105 °C for 30 min.
Titrable Acid To 60 g (74 mL) in a glass-stoppered flask, add 0.10 mL of phenolphthalein indicator solution, and titrate with 0.01 N methanolic potassium hydroxide to a pink end point that persists for at least 15 s. Not more than 5.0 mL of 0.01 N methanolic potassium hydroxide should be consumed.
Carbonyl Compounds Prepare a test solution by adding 9.9 µL butyraldehyde to 100 ml of the n-butanol sample. Analyze the sample and the test solution by GC–MS according to the procedure in [Part 2: Chromatography; Gas Chromatography–Mass Spectrometry]. For the column in [Part 2: Chromatography; Gas Chromatography–Mass Spectrometry], set the inlet temperature and pressure to 120 °C and 154 kPa. Inject 5 µL of sample with a 5:1 split ratio. Oven temperature profile: isothermal at 80 °C for 10 min, 5 °C/min to 120 °C, and hold 2 min. The area of the butyraldehyde peak in the sample should not be greater than half the corresponding peak area in the test solution.
© 2017 American Chemical Society
B
DOI:10.1021/acsreagents.4068 ACS Reagent Chemicals, Part 4
