Ammonium Metavanadate - ACS Reagent Chemicals - ACS Publications

This monograph for Ammonium Metavanadate 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

Ammonium Metavanadate 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

Downloaded by CORNELL UNIV on May 16, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4027

ABSTRACT This monograph for Ammonium Metavanadate provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), and aqueous solubility. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Solubility in Ammonium Hydroxide, Carbonate, Chloride, and Sulfate.

NH4VO3

Formula Wt 116.98

CAS No. 7803-55-6

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

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white to pale yellow solid combustion analysis of carbon, hydrogen, and nitrogen melting point, 200 °C 0.44 g in 100 mL at 18 °C

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% NH4VO3 Maximum Allowable Solubility in ammonium hydroxide. . . . . . . . . . Passes test Carbonate (CO3) . . . . . . . . . . . . . . . . . . . . . Passes test Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.2% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.05%

© 2017 American Chemical Society

A

ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.

DOI:10.1021/acsreagents.4027 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

pubs.acs.org/doi/book/10.1021/acsreagents

TESTS Assay (By oxidation–reduction titration of vanadium). Weigh accurately about 0.4 g, dissolve in 50 mL of warm water, and add 1 mL of sulfuric acid and 30 mL of sulfurous acid. Boil gently until the sulfur dioxide is expelled, then boil for 15 min longer. Cool, dilute with water to 100 mL, and titrate with 0.1 N potassium permanganate. One milliliter of 0.1 N potassium permanganate corresponds to 0.01170 g of NH4VO3.

Downloaded by CORNELL UNIV on May 16, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4027

Solubility in Ammonium Hydroxide Dissolve 5.0 g in a mixture of ammonium hydroxide and 250 mL of hot water, and add ammonium hydroxide until the reagent dissolves. Heat the solution to boiling. The solution should be clear.

Carbonate To 0.5 g, add 1 mL of water and 2 mL of 10% hydrochloric acid reagent solution. No effervescence should be produced. (Limit about 0.3%.)

Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Dissolve 0.5 g in 50 mL of hot water, add 2 mL of nitric acid, and let stand for 1 h. Filter through a chloride-free filter, wash with a few milliliters of water, and dilute with water to 100 mL; use 1.0 mL.

Sulfate [Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 1]. Dissolve 0.5 g in 40 mL of hot water, add 2 mL of 10% hydrochloric acid reagent solution and 1.5 g of hydroxylamine hydrochloride, and heat at 60 °C for 5 min. Filter through a suitable filter paper, cool, and dilute with water to 100 mL. To 20 mL, add 1 mL of dilute hydrochloric acid (1:19), and continue as directed.

© 2017 American Chemical Society

B

ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.

DOI:10.1021/acsreagents.4027 ACS Reagent Chemicals, Part 4