Monograph

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

Sodium Perchlorate
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 Sodium Perchlorate 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, pH of a 5% Solution at 25.0 °C, Insoluble Matter, Chloride, Sulfate, Calcium, Potassium,
Heavy Metals, and Iron.

NaClO4 (anhydrous) Formula Wt 122.44 CAS No. 7601-89-0

NaClO4 • H2O (monohy- Formula Wt 140.46 CAS No. 7791-07-3
drate)

Note: This specification includes the anhydrous form and the monohydrate.

GENERAL DESCRIPTION
Typical appearance . . . . . . . . . . . . . . . . . . . colorless or white solid
Applications . . . . . . . . . . . . . . . . . . . . . . . . electrolyte; oxidimetric standard
Change in state (approximate) . . . . . . . . . . . . melting point, 130 °C
Aqueous solubility . . . . . . . . . . . . . . . . . . . . 209 g in 100 mL

SPECIFICATIONS
Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98.0–102.0% NaClO4 (anhydrous) 85.0–90.0% NaClO4 · H2O (monohydrate)
pH of a 5% solution at 25.0 °C . . . . . . . . . . . . 6.0–8.0
Maximum Allowable
Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.005%
Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.003%
Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.002%

DOI:10.1021/acsreagents.4360
© 2017 American Chemical Society A ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

Calcium (Ca) . . . . . . . . . . . . . . . . . . . . . . . 0.02%

Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.05%
Heavy metals (by ICP–OES) . . . . . . . . . . . . . . 5 ppm
Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 5 ppm

TESTS
Assay
(By argentimetric titration of chloride content after perchlorate reduction to chloride). Weigh accurately about 0.28 g of
sample into a preconditioned platinum crucible or dish. Add 3 g of sodium carbonate, and heat, gently at first, then to
fusion until a clear melt is obtained. Leach with minimal 10% nitric acid, and boil gently to expel carbon dioxide. Cool to
room temperature, add 10 mL of aqueous 30% ammonium acetate solution, and titrate with 0.1 N silver nitrate volumetric
solution, using dichlorofluorescein indicator solution to the pink end point. One milliliter of 0.1 N silver nitrate corresponds
to 0.01225 g of NaClO4 or 0.01405 g of NaClO4 · H2O.

pH of a 5% Solution at 25.0 °C
[Part 2: Direct Electrometric Methods; pH Potentiometry; pH Range; Procedure for pH of a 5% Solution at 25.0 °C].

Insoluble Matter
[Part 2: Gravimetric Methods; Insoluble Matter]. Use 5.0 g dissolved in 50 mL of water.

Chloride
[Part 2: Colorimetry and Turbidimetry; Chloride]. Dissolve 0.33 g in 20 mL of water.

Sulfate
[Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 1]. Dissolve 2.5 g in 5 mL of water.

Calcium and Potassium

(By flame AAS, [Part 2: Trace and Ultratrace Elemental Analysis; Atomic Absorption Spectroscopy; Analysis; Procedure for
Flame AAS]).

For the Determination of Calcium and Potassium

S a m p l e S t o c k S o l u t i o n . Dissolve 1.0 g of sample with water in a 100 mL volumetric flask, add 10 mL of hydrochloric
acid, and dilute to the mark with water (1 mL = 0.01 g).

DOI:10.1021/acsreagents.4360
© 2017 American Chemical Society B ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals Monograph

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

For the Determination of Calcium and Potassium

Element Wavelength (nm) Sample Wt (g) Standard Added Flame Type* Background
(mg) Correction
Ca 422.7 0.10 0.02; 0.04 N/A No
K 766.5 0.10 0.05; 0.10 A/A No
*A/A is air/acetylene; N/A is nitrous oxide/acetylene.

Heavy Metals
([Part 2: Trace and Ultratrace Elemental Analysis; Inductively Coupled Plasma−Optical Emission Spectroscopy (ICP–OES);
Calculation of Heavy Metals (by ICP–OES) Results], by ICP–OES). Use 1.0 g sample.

Iron
[Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Use 2.0 g.

DOI:10.1021/acsreagents.4360
© 2017 American Chemical Society C ACS Reagent Chemicals, Part 4