Bismuth Nitrate Pentahydrate - American Chemical Society

Add about 50 mg of ascorbic acid and 50 mg of xylenol orange indicator mixture. Titrate with standard 0.1 M EDTA volumetric solution to canary yellow...
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Monograph pubs.acs.org/doi/book/10.1021/acsreagents

Bismuth Nitrate Pentahydrate (Bismuth(III) Nitrate Pentahydrate) 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 Bismuth Nitrate Pentahydrate 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 Matter, Arsenic, Chloride, Sulfate, Calcium, Copper, Iron, Lead, Potassium, Sodium, and Silver.

Bi(NO3)3 · 5H2O

Formula Wt 485.07

CAS No. 10035-06-0

GENERAL DESCRIPTION Typical appearance . . . . . . . . . . . . . . . . . . . colorlesssolid Applications . . . . . . . . . . . . . . . . . . . . . . . . trace metal analysis Aqueous solubility . . . . . . . . . . . . . . . . . . . . decomposes

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥98.0% Bi(NO3)3 · 5H2O Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.005% Arsenic (As) . . . . . . . . . . . . . . . . . . . . . . . . 0.001% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Calcium (Ca) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Copper (Cu) . . . . . . . . . . . . . . . . . . . . . . . . 0.002% Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.001% Lead (Pb) . . . . . . . . . . . . . . . . . . . . . . . . . 0.002% Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.01%

© 2017 American Chemical Society

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DOI:10.1021/acsreagents.4058 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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

Sodium (Na) . . . . . . . . . . . . . . . . . . . . . . . . 0.02% Silver (Ag) . . . . . . . . . . . . . . . . . . . . . . . . . 0.001%

TESTS Assay (By complexometric titration for bismuth). Weigh accurately about 1.8 g, and transfer to a 400 mL beaker. Dissolve in 5 mL of nitric acid, and add about 250 mL of water. Add about 50 mg of ascorbic acid and 50 mg of xylenol orange indicator mixture. Titrate with standard 0.1 M EDTA volumetric solution to canary yellow. (The solution color changes from purple to salmon pink just before the canary yellow end point). One milliliter of 0.1 M EDTA corresponds to 0.04851 g of Bi(NO3)3 · 5H2O.

Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Use 20 g dissolved in 100 mL of dilute nitric acid (1:4).

Arsenic [Part 2: Colorimetry and Turbidimetry; Arsenic]. Mix 0.5 g with 5 mL of water, and cautiously add 2 mL of sulfuric acid. Heat the mixture until white fumes of sulfur trioxide are evolved copiously. Cool, cautiously add 10 mL of water, and evaporate to strong fumes of sulfur trioxide. Cool, cautiously add another 10 mL of water, and again evaporate to strong fumes of sulfur trioxide. Cool, and cautiously wash the solution into a generator flask with sufficient water to make the volume 35 mL. The solution should show not more than 0.005 mg of arsenic.

Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 1.0 g.

Sulfate Dissolve 3.0 g in 5 mL of warm hydrochloric acid, dilute with water to 100 mL, and nearly neutralize with 10% ammonium hydroxide. Filter, and wash the residue and the filter with hot water to 150 mL. Transfer 100.0 mL to an evaporating dish, evaporate to about 15 mL, add 0.5 g of sodium carbonate, evaporate to dryness, and ignite gently. Cool, add 15 mL of hot water, neutralize with 10% hydrochloric acid, filter, and wash with water to 20 mL. Add to the combined filtrate and washings 1 mL of 1 N hydrochloric acid and 2 mL of 12% barium chloride reagent solution, and allow to stand for 10 min. Any turbidity should not exceed that of a standard prepared as follows. To 0.5 g of sodium carbonate, add 0.1 mg of sulfate ion (SO4) and 2 mL of hydrochloric acid, and evaporate to dryness on a hot plate (~100 °C). Dissolve the residue in 20 mL of water, and add 1 mL of 1 N hydrochloric acid and 2 mL of 12% barium chloride reagent solution.

Calcium, Copper, Iron, Lead, Potassium, and Sodium (By flame AAS, [Part 2: Trace and Ultratrace Elemental Analysis; Atomic Absorption Spectroscopy; Analysis; Procedure for Flame AAS]).

© 2017 American Chemical Society

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DOI:10.1021/acsreagents.4058 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

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

For the Determination of Calcium, Copper, Iron, Lead, Potassium, and Sodium

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 20 mL of nitric acid and 20 mL of water. Transfer to a 100 mL volumetric flask, and dilute to the mark with water (1 mL = 0.1 g).

For the Determination of Calcium, Copper, Iron, Lead, Potassium, and Sodium

Element

Wavelength (nm)

Sample Wt (g)

Standard Added (mg)

Flame Type*

Background Correction

Ca

422.7

2.0

0.05; 0.10

N/A

No

Cu

324.7

2.0

0.02; 0.04

A/A

Yes

Fe

248.3

2.0

0.02; 0.04

A/A

Yes

Pb

217.0

2.0

0.04; 0.08

A/A

Yes

K

766.5

0.10

0.01; 0.02

A/A

No

Na

589.0

0.10

0.01; 0.02

A/A

No

*A/A is air/acetylene; N/A is nitrous oxide/acetylene.

Silver Dissolve 1.0 g in a mixture of 5 mL of nitric acid and 15 mL of water, and add 0.05 mL of hydrochloric acid. Any turbidity should not exceed that of a standard containing 0.01 mg of silver.

© 2017 American Chemical Society

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DOI:10.1021/acsreagents.4058 ACS Reagent Chemicals, Part 4