Nitrobenzene - ACS Reagent Chemicals (ACS Publications)

Feb 28, 2017 - This monograph for Nitrobenzene provides, in addition to common physical constants, a general description including typical appearance,...
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Monograph pubs.acs.org/doi/book/10.1021/acsreagents

Nitrobenzene 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 Nitrobenzene 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, Water-Soluble Titrable Acid, and Chloride.

C6H5NO2

Formula Wt 123.11

CAS No. 98-95-3

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

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pale yellow liquid solvent; anticoagulant for titrations boiling point, 211 °C 0.19 g in 100 mL at 20 °C 1.21

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% C6H5NO2 Maximum Allowable Residue after evaporation . . . . . . . . . . . . . . . 0.005% Water-soluble titrable acid . . . . . . . . . . . . . . 0.0005 meq/g Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 5 ppm

© 2017 American Chemical Society

A

DOI:10.1021/acsreagents.4246 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 nitrobenzene content in area percent. Correct for water content.

Residue after Evaporation [Part 2: Gravimetric Methods; Residue after Evaporation]. Evaporate 20 g (16.7 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-Soluble Titrable Acid Shake 25 g (21 mL) with 60 mL of water for 1 min, and allow the layers to separate. Draw off and discard the nitrobenzene. Titrate 48 mL of the water extract with 0.01 N sodium hydroxide, using 0.15 mL of bromphenol blue indicator solution. Not more than 1.0 mL of 0.01 N sodium hydroxide should be required.

Chloride Dilute the remaining 12 mL of the water extract from the test for acidity with water to 25 mL, filter through a chloride-free filter, and dilute 10 mL of the filtrate with water to 20 mL. Add 1 mL of nitric acid and 1 mL of silver nitrate reagent solution. Any turbidity should not exceed that produced by 0.01 mg of chloride ion (Cl) in an equal volume of solution containing the quantities of reagents used in the test.

© 2017 American Chemical Society

B

DOI:10.1021/acsreagents.4246 ACS Reagent Chemicals, Part 4