Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Periodic Acid (para-Periodic Acid)
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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 Periodic Acid 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, Insoluble Matter, Residue after Ignition, Other Halogens, Sulfate, Heavy Metals, and Iron.
H5IO6
Formula Wt 227.96
CAS No. 10450-60-9
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
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hygroscopic, colorless solid; may become pale yellow on exposure to air Oxidizer; determination of manganese melting point, 122 °C; decomposes at 130–140 °C very soluble
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99.0–101.0% H5IO6 Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.01% Residue after ignition. . . . . . . . . . . . . . . . . . 0.01% Other halogens (as Cl) . . . . . . . . . . . . . . . . . 0.01% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.01% Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 0.005% Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.003%
© 2017 American Chemical Society
A
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4260 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay (By titration of oxidizing power). Weigh accurately about 0.12 g, transfer to an iodine flask, and dissolve in about 50 mL of water. Add 1 mL of sulfuric acid and 3 g of potassium iodide, swirl, and let stand in the dark for 10 min. Titrate the liberated iodine with 0.1 N sodium thiosulfate volumetric solution, adding starch indicator solution near the end of the titration. One milliliter of 0.1 N thiosulfate corresponds to 0.002849 g of H5IO6.
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Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Use 10.0 g dissolved in 100 mL of water.
Residue after Ignition [Part 2: Gravimetric Methods; Residue after Ignition]. Use a 10.0 g sample.
Other Halogens Dissolve 1.0 g in 20 mL of water with 1 mL of phosphoric acid. Add 1 mL of hydrogen peroxide, and boil until the iodine is expelled. Wash down the sides with water, add 1 mL of hydrogen peroxide, and boil. If iodine color forms, repeat the treatment until no more iodine is evolved. Boil an additional 10 min and dilute to 100 mL. Dilute 10 mL to 23 mL, and add 1 mL of nitric acid and 1 mL of silver nitrate reagent solution. The turbidity should not exceed that produced by 0.01 mg of chloride ion in an equal volume containing the quantities of all reagents used in the test.
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For the Determination of Sulfate, Heavy Metals, and Iron
S a m p l e S o l u t i o n A . Dissolve 10.0 g in 20 mL of water. Add 1 mL of 1% sodium carbonate reagent solution and 20 mL of hydrochloric acid, and evaporate to dryness on a hot plate (~100 °C). Repeat the evaporation twice, using 10 mL of hydrochloric acid. Dissolve the residue in 20 mL of water and dilute to 100 mL (1 mL = 0.10 g). B l a n k S o l u t i o n B . Use the quantity of hydrochloric acid added to sample solution A and 10 mg of sodium carbonate. Evaporate to dryness, dissolve in 20 mL of water, and dilute to 100 mL.
Sulfate† [Part 2: Colorimetry and Turbidimetry; Sulfate; Procedure for Sulfate, Method 1]. Use 5 mL of sample solution A (0.5 g sample).
Heavy Metals† [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Dilute 4 mL of sample solution A (0.4 g sample) to 25 mL. Use 4 mL of blank solution B to prepare the standard.
© 2017 American Chemical Society
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ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4260 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Iron
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Downloaded by CORNELL UNIV on May 16, 2017 | http://pubs.acs.org Publication Date (Web): February 28, 2017 | doi: 10.1021/acsreagents.4260
[Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 2 (Hydroxylamine and 1,10-Phenanthroline)]. Use 3.3 mL of sample solution A (0.33 g sample). For the standard, use 3.3 mL of blank solution B.
© 2017 American Chemical Society
C
ACS Reagent Chemicals ACS Reagent Chemicals; American Chemical Society: Washington, DC, 2017.
DOI:10.1021/acsreagents.4260 ACS Reagent Chemicals, Part 4
