Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Hydroxylamine Sulfate (Hydroxylammonium Sulfate) 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 Hydroxylamine Sulfate 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, Residue after Ignition, Chloride, Heavy Metals, Copper, and Iron.
(HONH3)2SO4
Formula Wt 164.13
CAS No. 10039-54-0
GENERAL DESCRIPTION Typical appearance . . . . . . . . . . . . . . . . . . . white solid Applications . . . . . . . . . . . . . . . . . . . . . . . . to purify aldehydes and ketones; reagent for mercury and silver detection in water; reducing agent Change in state (approximate) . . . . . . . . . . . . melting point, 170 °C Aqueous solubility . . . . . . . . . . . . . . . . . . . . freely soluble
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% (HONH3)2SO4 Maximum Allowable Residue after ignition. . . . . . . . . . . . . . . . . . 0.05% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001% Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 5 ppm Copper (Cu) . . . . . . . . . . . . . . . . . . . . . . . . 5 ppm Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 5 ppm
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4170 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay (By titration of the reductive capacity). Weigh accurately about 0.16 g, and dissolve in 25 mL of water. Add a solution of 5 g of ferric ammonium sulfate in a mixture of 15 mL of 10% sulfuric acid and 20 mL of water. Boil gently for 5 min. Cool, dilute with 100 mL of water, and add 1 mL of phosphoric acid. Titrate with 0.1 N potassium permanganate volumetric solution to a permanent pink color. One milliliter of 0.1 N potassium permanganate corresponds to 0.004104 g of (HONH3)2SO4.
Residue after Ignition [Part 2: Gravimetric Methods; Residue after Ignition]. Ignite 2.0 g. Retain the residue for the test for iron.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 1.0 g.
Heavy Metals [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Dissolve 5.0 g in about 20 mL of water, and dilute with water to 25.0 mL. Use 20.0 mL to prepare the sample solution, and use the remaining 5.0 mL to prepare the control solution.
Copper (By flame AAS, [Part 2: Trace and Ultratrace Elemental Analysis; Atomic Absorption Spectroscopy; Analysis; Procedure for Flame AAS]).
For the Determination of Copper
S a m p l e S t o c k S o l u t i o n . Dissolve 20.0 g of sample in water, and transfer to a 100 mL volumetric flask. Add 5 mL of nitric acid, and dilute to the mark with water (1 mL = 0.2 g).
For the Determination of Copper
Element
Wavelength (nm)
Sample Wt (g)
Standard Added (mg)
Flame Type*
Background Correction
Cu
324.8
4.0
0.02; 0.04
A/A
Yes
*A/A is air/acetylene.
Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. To the residue after ignition, add 3 mL of dilute hydrochloric acid (1:1), cover the dish, and digest on a hot plate (~100 °C) for 20 min. Remove
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4170 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
the cover, evaporate to dryness, dissolve the residue in 2 mL of hydrochloric acid, and dilute with water to 50 mL. Use the solution without further acidification.
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4170 ACS Reagent Chemicals, Part 4
