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) NaClO4 • H2O (monohydrate)
Formula Wt 122.44 Formula Wt 140.46
CAS No. 7601-89-0 CAS No. 7791-07-3
Note: This specification includes the anhydrous form and the monohydrate.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
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colorless or white solid electrolyte; oxidimetric standard melting point, 130 °C 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%
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4360 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Calcium (Ca) . . . . . . . . . Potassium (K) . . . . . . . . . Heavy metals (by ICP–OES) Iron (Fe) . . . . . . . . . . . .
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0.02% 0.05% 5 ppm 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).
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4360 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 (mg)
Flame Type*
Background 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.
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4360 ACS Reagent Chemicals, Part 4
