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Monograph pubs.acs.org/doi/book/10.1021/acsreagents ... Note: Great care should be taken in the test during the addition of the sample and the titrati...
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Monograph pubs.acs.org/doi/book/10.1021/acsreagents

4-Methyl-2-pentanone (Methyl Isobutyl Ketone) 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 4-Methyl-2-pentanone 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, Color (APHA), Residue after Evaporation, Titrable Acid, and Water.

(CH3)2CHCH2COCH3

Formula Wt 100.16

CAS No. 108-10-1

GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . .

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clear, colorless liquid solvent; extraction solvent boiling point, 118 °C moderately soluble 0.8

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥98.5% (CH3)2CHCH2COCH3 Maximum Allowable Color (APHA) . . . . . . . . . . . . . . . . . . . . . . . 15 Residue after evaporation . . . . . . . . . . . . . . . 0.005% Titrable acid . . . . . . . . . . . . . . . . . . . . . . . 0.002 meq/g Water (H2O) . . . . . . . . . . . . . . . . . . . . . . . . 0.1%

© 2017 American Chemical Society

A

DOI:10.1021/acsreagents.4226 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 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 area under all peaks, and calculate the 4-methyl-2-pentanone 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 100 g (125 mL) to dryness in a tared, preconditioned dish on a hot plate (~100 °C), and dry the residue at 125 °C for 30 min.

Titrable Acid To 25 mL of ethyl alcohol in a glass-stoppered flask, add 0.50 mL of phenolphthalein indicator solution. Add 0.01 N sodium hydroxide solution until a slight pink color persists after shaking for 30 s. Add 25 mL of the sample, mix, and titrate with 0.01 N sodium hydroxide until the pink color is restored. Not more than 4.0 mL of the sodium hydroxide solution should be required. Note: Great care should be taken in the test during the addition of the sample and the titration to avoid contamination from carbon dioxide.

Water [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 and a methanol-free system to prevent ketal formation with liberation of water.

© 2017 American Chemical Society

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DOI:10.1021/acsreagents.4226 ACS Reagent Chemicals, Part 4