Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Bismuth Chloride (Bismuth (III) Chloride) 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 Chloride 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, Nitrate, Sulfate, Arsenic, Calcium, Copper, Iron, Lead, Potassium, Sodium, and Silver.
BiCl3
Formula Wt 315.33
CAS No. 7787-60-2
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
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white solid catalyst for organic reagents melting point, 230 °C decomposes into BiOCl
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98.0–102.0% BiCl3 Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.01% Nitrate (NO3) . . . . . . . . . . . . . . . . . . . . . . . 0.01% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.01% Arsenic (As) . . . . . . . . . . . . . . . . . . . . . . . . 0.001% Calcium (Ca) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Copper (Cu) . . . . . . . . . . . . . . . . . . . . . . . . 0.001% Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.005% Lead (Pb) . . . . . . . . . . . . . . . . . . . . . . . . . 0.01% Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.01%
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4057 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
Sodium (Na) . . . . . . . . . . . . . . . . . . . . . . . . 0.02% Silver (Ag) . . . . . . . . . . . . . . . . . . . . . . . . . 0.002%
TESTS Assay (By indirect complexometric titration of bismuth). Weigh accurately about 1.2 g of sample, and transfer to a 250 mL beaker. Dissolve in 5 mL of hydrochloric acid. Add 50.0 mL of 0.1 M EDTA volumetric solution, and add ammonium acetate buffer solution to a pH of 4.5 as measured using a pH meter. Add 75 mL of alcohol and 2 mL of dithizone indicator solution, and titrate with standard 0.1 M zinc chloride volumetric solution to a pink end point. One milliliter of 0.1 M EDTA corresponds to 0.03153 g of BiCl3.
Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Use 20 g dissolved in 100 mL of dilute hydrochloric acid (1:4).
Nitrate [Part 2: Colorimetry and Turbidimetry; Nitrate; Procedure for Nitrate, Method 1 (Brucine Sulfate)].
For the Determination of Nitrate
S a m p l e S o l u t i o n A . Dissolve 0.20 g in 1 mL of 6 M hydrochloric acid and 2 mL of water by heating on a hot plate (~100 °C). Cautiously add 20 mL of nitrate-free sulfuric acid (2:1), and cool in an ice bath. Dilute to 50 mL with brucine sulfate reagent solution. C o n t r o l S o l u t i o n B . Dissolve 0.20 g in 1 mL of 6 M hydrochloric acid and 2 mL of the nitrate ion (NO3) standard solution by heating on a hot plate (~100 °C). Cautiously add 20 mL of nitrate-free sulfuric acid (2:1), and cool in an ice bath. Dilute to 50 mL with brucine sulfate reagent solution. B l a n k S o l u t i o n C . To 1 mL of 7 M hydrochloric acid, cautiously add 20 mL of nitrate-free sulfuric acid (2:1), and cool in an ice bath. Dilute to 50 mL with brucine sulfate reagent solution.
Continue with the procedure, starting with “Heat the three solutions…”.
Sulfate Dissolve 3.0 g in 5 mL of warm hydrochloric acid, dilute with warm water to 100 mL, and nearly neutralize with 10% ammonium hydroxide. Filter and wash the residue with hot water. Dilute the filtrate to 150 mL. Transfer 100 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. To the combined filtrate and washings, add 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 0.2 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, 1 mL of 1 N hydrochloric acid, and 2 mL of 12% barium chloride reagent solution.
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4057 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
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. For the standard, use 0.005 mg of arsenic.
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]).
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 hydrochloric acid and 20 mL of water. Transfer to a 100 mL volumetric flask, and dilute to the mark with water (1 mL = 0.10 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
0.10; 0.20
A/A
Yes
Pb
217.0
2.0
0.20; 0.40
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 Add 1.0 g to 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 0.02 mg of silver ion treated as the sample.
© 2017 American Chemical Society
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DOI:10.1021/acsreagents.4057 ACS Reagent Chemicals, Part 4
