Monograph pubs.acs.org/doi/book/10.1021/acsreagents
1-Pentanol (n-Amyl Alcohol)
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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 1-Pentanol 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, Water, Color (APHA), Residue after Evaporation, Acids, Esters, and Carbonyl Compounds.
CH3(CH2)3CH2OH
Formula Wt 88.15
CAS No. 71-41-0
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . .
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liquid, with mild characteristic odor solvent boiling point, 138 °C 2.7 g in 100 mL at 22 °C 0.81
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥98.0% CH3(CH2)3CH2OH Maximum Allowable Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.5% Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 30 Residue after evaporation . . . . . . . . . . . . . . . 0.003% Acids and esters . . . . . . . . . . . . . . . . . . . . . 0.075 meq/g Carbonyl compounds (as HCHO) . . . . . . . . . . . 0.1%
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4256 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay Analyze the sample by gas chromatography using the parameters cited in [Part 2: Chromatography; Recommended Procedures; Gas Chromatography]. The following specific conditions are also required. Column . . . . . . . . . . . . . . . . . . . . . . . . . . Type I, methyl silicone Measure the area under all peaks, and calculate the 1-pentanol content in area percent. Correct for water content.
Water
Downloaded by CORNELL UNIV on May 9, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4256
[Part 2: Titrimetric Methods; Water by the Karl Fischer Method; Volumetric Procedure; Volumetric Procedure for Samples Using Karl Fischer Reagent, Method 1]. Use 25 mL (20 g) of the sample.
Color (APHA) [Part 2: Measurement of Physical Properties; Color (APHA); Procedure for Color (APHA)].
Residue after Evaporation [Part 2: Gravimetric Methods; Residue after Evaporation]. Use 40.0 g (50 mL) of sample, evaporate to dryness on a hot plate (~100 °C), and complete drying at 105 °C.
Acids and Esters Dilute 8.1 g (10 mL) with 20 mL of ethyl alcohol, add 10 mL of 0.1 N sodium hydroxide, and reflux gently for 10 min. Cool, add 0.15 mL of phenolphthalein indicator solution, and titrate the excess sodium hydroxide with 0.1 N hydrochloric acid. Run a reagent blank. The net volume of 0.1 N sodium hydroxide consumed by the sample should not exceed 6.1 mL.
Carbonyl Compounds Test solution preparation: Add 203 µL formaldehyde solution, 150 µL acetaldehyde, 194 µL propionaldehyde, 199 µL acetone, 237 µL butyraldehyde, and 240 µL 2-butanone to 90.0 mL of the sample; add more sample to make 100.0 mL. (Molar equivalents to 1000 µg/g formaldehyde added). 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 inlet temperature and pressure to 120 °C and 164 kPa. Inject 1 µL of sample with a 5:1 split ratio. Oven temperature profile: isothermal at 40 °C for 20 min, 5 °C/min to 90 °C, hold 1 min, 40 °C/min to 220 °C, hold 5.75 min. The area of each of the carbonyl peaks in the sample should be no greater than half that of the corresponding peak in the test solution.
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4256 ACS Reagent Chemicals, Part 4
