Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Sodium Hydrogen Sulfate, Fused 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 Hydrogen Sulfate, Fused 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: Acidity, Insoluble Matter, Chloride, Phosphate, Heavy Metals, Iron, Calcium, Magnesium, and Potassium.
CAS No. 7681-38-1
Note: This product is usually a mixture of sodium pyrosulfate, Na2S2O7, and sodium hydrogen sulfate, NaHSO4.
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
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opaque or white solid fusion matrix melting point, 315 °C 50 g in 100 mL at 0 °C
SPECIFICATIONS Acidity (as H2SO4) . . . . . . . . . . . . . . . . . . . . 39.0–42.0% Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.01% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001% Phosphate (PO4) . . . . . . . . . . . . . . . . . . . . . 0.001% Heavy metals (as Pb) . . . . . . . . . . . . . . . . . . 5 ppm Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.002% Calcium (Ca) . . . . . . . . . . . . . . . . . . . . . . . 0.002%
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4349 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Magnesium (Mg) . . . . . . . . . . . . . . . . . . . . . 0.001% Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.005%
TESTS Acidity Weigh accurately about 4.0 g, dissolve in 50 mL of water, and titrate with 1 N sodium hydroxide volumetric solution, using 0.15 mL of methyl orange indicator solution. One milliliter of 1 N sodium hydroxide corresponds to 0.04904 g of H2SO4.
Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Dissolve 20.0 g in 200 mL of water.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 1.0 g.
Phosphate Dissolve 2.0 g in 15 mL of dilute ammonium hydroxide (1:2), and evaporate to dryness. Dissolve the residue in 25 mL of 0.5 N hydrochloric acid, add 1 mL of ammonium molybdate–nitric acid reagent solution and 1 mL of 4-(methylamino)phenol sulfate reagent solution, and allow to stand for 2 h at room temperature. Any blue color should not exceed that produced by 0.02 mg of phosphate ion (PO4) in an equal volume of solution containing the quantities of reagents used in the test, including the residue from evaporation of 5 mL of ammonium hydroxide.
Heavy Metals [Part 2: Colorimetry and Turbidimetry; Heavy Metals (as Lead); Procedure for Heavy Metals, Method 1]. Dissolve 6.0 g in about 25 mL of water, and dilute with water to 30 mL. Use 25 mL to prepare the sample solution, and use the remaining 5.0 mL to prepare the control solution.
Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Dissolve 5.0 g in 80 mL of dilute hydrochloric acid (1:3), and boil gently for 10 min. Cool, dilute with water to 100 mL, and use 10 mL.
Calcium, Magnesium, 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, Magnesium, and Potassium
S a m p l e S t o c k S o l u t i o n . Dissolve 10.0 g of sample in a 100 mL volumetric flask, and dilute to the mark with water (1 mL = 0.10 g).
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4349 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
For the Determination of Calcium, Magnesium, and Potassium
Element
Wavelength (nm)
Sample Wt (g)
Standard Added (mg)
Flame Type*
Background Correction
Ca
422.7
1.0
0.02; 0.04
N/A
No
Mg
285.2
1.0
0.01; 0.02
A/A
Yes
K
766.5
0.40
0.01; 0.02
A/A
No
*A/A is air/acetylene; N/A is nitrous oxide/acetylene.
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4349 ACS Reagent Chemicals, Part 4
