Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Acetic Anhydride 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
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ABSTRACT This monograph for Acetic Anhydride 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, Residue after Evaporation, Chloride, Phosphate, Sulfate, Heavy Metals, Iron, and Substances Reducing Permanganate.
(CH3CO)2O
Formula Wt 102.09
CAS No. 108-24-7
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . Density . . . . . . . . . . . . . . . .
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liquid with a pungent odor preparation of anhydrous acetic acid in nonaqueous titrimetry boiling point, 139 °C gradually dissolves with formation of acetic acid 1.08
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥97.0% (CH3CO)2O Maximum Allowable Residue after evaporation . . . . . . . . . . . . . . . 0.003% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 5 ppm Phosphate (PO4) . . . . . . . . . . . . . . . . . . . . . 0.001% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 5 ppm Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 2 ppm
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4004 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 5 ppm Substances reducing permanganate . . . . . . . . . Passes test
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 NEW YORK UNIV on May 18, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4004
Measure the area under all peaks and calculate the area percent for acetic anhydride.
Residue after Evaporation [Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 50 g (46 mL) in a tared, preconditioned dish on a hot plate (~100 °C), and dry the residue at 105 °C for 30 min.
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For the Determination of Chloride, Phosphate, Sulfate, Heavy Metals, Iron, and Substances Reducing Permanganate
S a m p l e S o l u t i o n A . Dilute 40 g (37 mL) of the sample with water to 200 mL (1 mL = 0.2 g).
Chloride† [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 10 mL of sample solution A (2 g sample).
Phosphate† [Part 2: Colorimetry and Turbidimetry; Phosphate; Procedure for Phosphate, Method 1 (Direct Molybdenum Blue)]. Evaporate 10 mL of sample solution A (2 g sample) to dryness on a hot plate (~100 °C), and dissolve the residue in 25 mL of 0.5 N sulfuric acid.
Sulfate† [Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 3]. Use 50 mL of sample solution A (10 g sample).
Heavy Metals† [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. To 50 mL of sample solution A (10 g sample), add about 1.0 mL of 1% sodium carbonate reagent solution, evaporate to dryness on a hot plate (~100 °C), dissolve the residue in about 20 mL of water, and dilute with water to 25 mL.
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4004 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Iron
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[Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. To 10 mL of sample solution A (2 g sample), add 10 mg of sodium carbonate, and evaporate to dryness. Dissolve the residue in 2 mL of hydrochloric acid, dilute with water to 50 mL, and use the solution without further acidification.
Substances Reducing Permanganate†
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To 10 mL of sample solution A (2 g sample), add 0.4 mL of 0.1 N potassium permanganate, and allow to stand for 5 min. The pink color should not be entirely discharged.
© 2017 American Chemical Society
C
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4004 ACS Reagent Chemicals, Part 4
