Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Zirconyl Chloride Octahydrate (Zirconium Oxide Chloride, Octahydrate)
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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 Zirconyl Chloride Octahydrate provides, in addition to common physical constants, a general description including typical appearance and applications. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Sulfate, Heavy Metals, Iron, and Titanium.
ZrOCl2 • 8H2O
Formula Wt 322.24
CAS No. 13520-92-8
GENERAL DESCRIPTION Typical appearance . . . . . . . . . . . . . . . . . . . white solid Applications . . . . . . . . . . . . . . . . . . . . . . . . reagent for fluoride determination in water analyses; reagent for reduction of nitro compounds to primary amines
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% ZrOCl2 · H2O Maximum Allowable Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 0.001% Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.001% Titanium (Ti) . . . . . . . . . . . . . . . . . . . . . . . 0.005%
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4431 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay
Downloaded by CORNELL UNIV on June 15, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4431
(By indirect complexometric titration of zirconium). Accurately weigh 1.0 g of sample, and transfer to a 250 mL Erlenmeyer flask. Add 5 mL of hydrochloric acid and then 50.0 mL of 0.1 M EDTA volumetric solution. Heat to boiling, cool, and add ammonium acetate buffer solution to a pH of 4.5 (using a pH meter). Add 75 mL of alcohol and 2 mL of dithizone indicator solution, and titrate with 0.1 M zinc chloride volumetric solution to a pink end point. One milliliter of 0.1 M EDTA corresponds to 0.03222 g of ZrOCl2 · 8H2O.
Sulfate [Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 1]. Dissolve 1 g in 30 mL of hot water, and pour slowly, with stirring, into a mixture of 3 mL of ammonium hydroxide and 40 mL of water. Boil for 10 min, and filter through a sintered glass crucible. Wash the filtrate with small portions of water. Boil one half of the filtrate down to about 10 mL, and neutralize with hydrochloric acid.
Heavy Metals [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Dissolve 2 g in 30 mL of water, and add 2 g of sodium acetate, trihydrate. Adjust the pH of the solution to between 3 and 4 with acetic acid, and dilute to 40 mL. Any brown color should not exceed that produced by a 0.02-mg lead ion (Pb) standard solution treated exactly as the sample.
Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Use 1.0 g.
Titanium Dissolve 1.0 g in 5 mL of water, and add 0.2 mL of 25% hydrochloric acid and 1 mL of 3% hydrogen peroxide reagent solution. Compare the immediate resulting color with that of an equally treated control solution containing 0.05 mg of titanium.
© 2017 American Chemical Society
B
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4431 ACS Reagent Chemicals, Part 4
