Sodium Peroxide | ACS Reagent Chemicals - ACS Publications

Jun 1, 2016 - ... and titrate 100.0 mL with 0.1 N potassium permanganate volumetric ... Completely dissolve 20 g in 300 mL of cold water (10 °C), neut...
0 downloads 0 Views 163KB Size
Monograph pubs.acs.org/doi/book/10.1021/acsreagents

Sodium Peroxide 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 via UNIV OF SASKATCHEWAN on August 20, 2019 at 19:31:25 (UTC). See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

A u t h o r i t a t i v e V e r s i o n : This version is current as of 01 Jun 2016.

ABSTRACT This monograph for Sodium Peroxide provides, in addition to common physical constants, a general description including typical appearance, applications, 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, Chloride, Phosphate, Sulfate, Heavy Metals, Iron. Special caution is advised for the handling or testing of this substance.

+

Na2O2

O-Na+

Na-O

Formula Wt 77.98

CAS No. 1313-60-6

SUPPLEMENTS & UPDATES Published

Authoritative

28 Feb 2017

01 Jun 2016

Expired

Type

Summary

Other Versions

Original

First on-line publication, based on 11th ed.

C a u t i o n : This reagent should be stored in airtight containers in a cool place. Avoid contact with organic materials; fire or explosion may result.

Note: When dissolving sodium peroxide, the material should be added slowly and in small portions to well-cooled water; when neutralizing, the acid must be added cautiously in small portions, and the solution kept cool.

GENERAL DESCRIPTION Typical appearance . . . . . . . . . . . . . . . . . . . slightly yellow solid

© 2017 American Chemical Society

A

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

DOI:10.1021/acsreagents.4362.20160601 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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

Applications . . . . . . . . . . . . . . . . . . . . . . . . oxidizing agent Aqueous solubility . . . . . . . . . . . . . . . . . . . . soluble in cold water; decomposes in warm water

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥93.0% Na2O2

Chloride (Cl) . . . . . Phosphate (PO4) . . . Sulfate (SO4) . . . . . Heavy metals (as Pb) Iron (Fe) . . . . . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

Maximum Allowable 0.002% 5 ppm 0.001% 0.002% 0.005%

TESTS Assay (By titration of reducing power against permanganate). Weigh accurately about 0.7 g, and add slowly to 400 mL of dilute sulfuric acid (1:99) that has been cooled to 10 °C. Dilute to volume in a 500 mL volumetric flask with dilute sulfuric acid (1:99), and titrate 100.0 mL with 0.1 N potassium permanganate volumetric solution. One milliliter of 0.1 N potassium permanganate corresponds to 0.003899 g of Na2O2.

% Na 2O2 =

(mL × N KMnO4 ) × 3.899 Sample wt (g)/ 5

Chloride Add 1.0 g in small portions to 35 mL of water, cool, and slowly add 4 mL of nitric acid. Filter if necessary through a chloridefree filter, and dilute the filtrate with water to 40 mL. To 20 mL of the filtrate, add 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.

Phosphate [Part 2: Colorimetry and Turbidimetry; Phosphate; Procedure for Phosphate, Method 1 (Direct Molybdenum Blue)]. Dissolve 4.0 g in 50 mL of water, cautiously add 10 mL of nitric acid, and evaporate to dryness on a hot plate (~100 °C). Dissolve the residue in 25 mL of approximately 0.5 N sulfuric acid, and continue as described.

Sulfate Completely dissolve 20 g in 300 mL of cold water (10 °C), neutralize with hydrochloric acid, and note the volume used. Add an excess of 2 mL of the acid, and evaporate to a volume of about 200 mL. Filter if necessary, heat the filtrate to boiling, add 10 mL of 12% barium chloride reagent solution, digest in a covered beaker on a hot plate (~100 °C) for 2 h, and allow to stand for at least 8 h. If a precipitate is formed, filter, wash thoroughly, and ignite. Correct for the weight obtained in a complete blank test. For the blank, add about 10 mg of sodium carbonate and 1 mL of bromine water to the volume of hydrochloric acid used to neutralize the sodium peroxide, and evaporate to dryness. Dissolve in 2 mL of hydrochloric acid, add 200 mL of water, boil, and filter if necessary. Add 10 mL of 12% barium chloride reagent solution, and carry along with the sample.

© 2017 American Chemical Society

B

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

DOI:10.1021/acsreagents.4362.20160601 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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

Heavy Metals [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Add 2.0 g cautiously to 15 mL of dilute hydrochloric acid (1:2) cooled to 10 °C. Evaporate the solution to dryness on a hot plate (~100 °C), add 15 mL of dilute hydrochloric acid, and repeat the evaporation to dryness. Dissolve the residue in 20 mL of water, and dilute with water to 25 mL. For the control, add 0.02 mg of lead ion (Pb) to 15 mL of dilute hydrochloric acid, cool the acid to 10 °C, and cautiously add 1.0 g of the sample, continuing with the evaporations exactly as for the 2.0 g of sample.

Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Add 10 g, cautiously, to 75 mL of a cooled solution of dilute hydrochloric acid (1:2). Evaporate on a hot plate (~100 °C) to dryness, add 10 mL of hydrochloric acid, and again evaporate to dryness. Dissolve the residue in 80 mL of dilute hydrochloric acid (1:40), dilute with water to 100 mL, and use 2.0 mL of the solution.

© 2017 American Chemical Society

C

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

DOI:10.1021/acsreagents.4362.20160601 ACS Reagent Chemicals, Part 4