Ceric Ammonium Nitrate - ACS Reagent Chemicals (ACS Publications)

Jun 1, 2016 - The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade ...
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Monograph

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

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Ceric Ammonium Nitrate

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Portions of this monograph have been updated. Please visit http://pubs.acs.org/doi/full/10.1021/acsreagents.4086 for a summary of changes.

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ABSTRACT

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This monograph for Ceric Ammonium Nitrate 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, Insoluble in Dilute Sulfuric Acid, Chloride, Phosphate, and Iron.

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Formula Wt 548.20

CAS No.16774-21-3

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(NH4)2Ce(NO3)6

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SUPPLEMENTS & UPDATES Authoritative

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Summary

28 Feb 2017

01 Jun 2016

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

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GENERAL DESCRIPTION

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Typical appearance . . . . . . . . . . . . . . . . . . . orange-red or orange-yellow solid Applications . . . . . . . . . . . . . . . . . . . . . . . . oxidimetric standard Aqueous solubility . . . . . . . . . . . . . . . . . . . . 141 g in 100 mL

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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

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(Ammonium Hexanitratocerate(IV))

© 2017 American Chemical Society

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

DOI: 10.1021/acsreagents.4086.20160601 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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SPECIFICATIONS

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Maximum Allowable 0.05% 0.01% 0.02% 0.005%

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Insoluble in dilute sulfuric acid. Chloride (Cl) . . . . . . . . . . . . Phosphate (PO4) . . . . . . . . . . Iron (Fe) . . . . . . . . . . . . . . .

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Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥98.5% (NH4)2Ce(NO3)6

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TESTS

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Assay

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(By titration of oxidative capacity of CeIV). Weigh accurately 2.4–2.5 g, and dissolve in 50 mL of water. From a pipette, add 50 mL of 0.1 N ferrous ammonium sulfate volumetric solution, and swirl until the precipitate that forms is redissolved. Add 10 mL of phosphoric acid and 0.10 mL of diphenylaminesulfonic acid, sodium salt, indicator solution (described below). Titrate at once with 0.1 N potassium dichromate volumetric solution to a change from faint green to violet. Record this titration volume as A mL. Pipette 25 mL of 0.1 N ferrous ammonium sulfate volumetric solution into 50 mL of water, and treat it in the same way (with phosphoric acid and indicator but without sample). Titrate to a change from green to grayblue, and record this titration volume as B mL. One milliliter of 0.1 N ferrous ammonium sulfate corresponds to 0.05482 g of (NH4)2Ce(NO3)6.

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[(2B − A mL) × N K 2Cr2O7 ] × 54.82 Sample wt (g)

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% (NH4)2 Ce(NO3)6 =

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For the Assay

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D i p h e n y l a m i n e s u l f o n i c A c i d , S o d i u m S a l t , I n d i c a t o r S o l u t i o n . Dissolve 0.10 g of the salt in 100 mL of water.

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Insoluble in Dilute Sulfuric Acid

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Chloride

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To 5.0 g, add 10 mL of sulfuric acid, stir, and then cautiously add 90 mL of water to dissolve. Heat to boiling, and digest in a preconditioned covered beaker on a hot plate (~100 °C) for 1 h. Filter through a tared filtering crucible, wash thoroughly, and dry at 105 °C.

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[Part 2: Colorimetry and Turbidimetry; Chloride]. Use 0.10 g dissolved in 10 mL of water. The comparison is best made by the general method for chloride in colored solutions.

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Phosphate

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[Part 2: Colorimetry and Turbidimetry; Phosphate; Procedure for Phosphate, Method 2 (Extracted Molybdenum Blue)]. Dissolve 0.25 g in 30 mL of dilute sulfuric acid (1:9), add hydrogen peroxide until the solution just turns colorless, then boil to destroy excess peroxide. Cool, and dilute with water to 50 mL. Dilute 10 mL with water to 60 mL, and adjust the pH between 2 and 3 (using pH paper) with ammonium hydroxide.

© 2017 American Chemical Society

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

DOI: 10.1021/acsreagents.4086.20160601 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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Note: This neutralization must be made with care to avoid formation of a permanent precipitate that would void the test. If this happens, discard the solution and start with another 10 mL.

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Add 0.5 g of ammonium molybdate, and adjust the pH to 1.8 (using a pH meter) with dilute hydrochloric acid (1:9). Heat the solution to boiling and cool to room temperature. Dilute with water to 90 mL, add 10 mL of hydrochloric acid, and continue as described. Carry along a standard containing 0.01 mg of phosphate ion (PO4) in 10 mL of dilute sulfuric acid (3:47) treated exactly as the 10 mL of sample.

Iron

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[Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 2 (Hydroxylamine and 1,10-Phenanthroline)]. Dissolve 1.0 g in 30 mL of dilute sulfuric acid (1:9), and add, dropwise, 3% hydrogen peroxide solution until the yellow color disappears. For the standard, add 0.05 mg of iron ion (Fe) to 30 mL of dilute sulfuric acid (1:9) and the same volume of 3% hydrogen peroxide solution used for the sample. To each solution, add ammonium hydroxide until the pH is between 1 and 3, cool to room temperature, and adjust the pH to 3.5 (using a pH meter). Dilute each solution with water to 50 mL, and use 10 mL of each.

© 2017 American Chemical Society

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

DOI: 10.1021/acsreagents.4086.20160601 ACS Reagent Chemicals, Part 4