Monograph pubs.acs.org/doi/book/10.1021/acsreagents
Aluminum Nitrate Nonahydrate 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 Aluminum Nitrate Nonahydrate 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, Chloride, Sulfate, Calcium, Magnesium, Potassium, Sodium, Heavy Metals, and Iron.
Al(NO3)3 · 9H2O
Formula Wt 375.13
CAS No. 7784-27-2
GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
. . . .
colorless, deliquescent solid metal standard solution; extraction of uranium melting point, 73 °C 64 g in 100 mL at 25 °C
SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98.0–102.0% Al(NO3)3 · 9H2O Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.005% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001% Sulfate (SO4) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Calcium (Ca) . . . . . . . . . . . . . . . . . . . . . . . 0.005% Magnesium (Mg) . . . . . . . . . . . . . . . . . . . . . 0.001% Potassium (K) . . . . . . . . . . . . . . . . . . . . . . . 0.002% Sodium (Na) . . . . . . . . . . . . . . . . . . . . . . . . 0.005% Heavy metals (by ICP–OES) . . . . . . . . . . . . . . 0.001% Iron (Fe) . . . . . . . . . . . . . . . . . . . . . . . . . . 0.002%
© 2017 American Chemical Society
A
DOI:10.1021/acsreagents.4010 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
TESTS Assay (By indirect complexometric titration of AlIII). Weigh accurately 5 g, and transfer to a 250 mL volumetric flask. Dissolve in about 75 mL of water, add 5 mL of hydrochloric acid, dilute to volume with water, and mix. Place a 25.0 mL aliquot of this solution in a 250 mL beaker, add 50 mL of water, and mix. While stirring, add 40.0 mL of 0.1 M EDTA volumetric solution and 20 mL of ammonium acetate–acetic acid buffer solution. Heat the solution to near boiling for 5 min, and cool. (The pH should be 4.0–5.0 and should be maintained in that range by adding more buffer during the titration if necessary.) Add 50 mL of alcohol and 2 mL of dithizone indicator solution, and titrate the excess EDTA with 0.1 M zinc chloride volumetric solution until the color changes from a green-violet to a rose-pink. One milliliter of 0.1 M EDTA corresponds to 0.03751 g of Al(NO3)3 · 9H2O.
Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Dissolve 20 g in 150 mL of water and filter immediately without digesting.
Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 1.0 g.
Sulfate Dissolve 4.0 g in 10 mL of hydrochloric acid, and evaporate to dryness on a hot plate (~100 °C). Take up the residue in 10 mL of hydrochloric acid, and again evaporate to dryness. Dissolve the residue in 100 mL of water, add a slight excess of ammonium hydroxide, and boil the solution until the odor of ammonia is entirely gone. Dilute with water to 200 mL, filter, and evaporate 50 mL of the filtrate to 10 mL. To the evaporated filtrate, add 1 mL of dilute hydrochloric acid (1:19) and 1 mL of 12% barium chloride reagent solution. Any turbidity should not exceed that produced by 0.05 mg of sulfate ion (SO4) in an equal volume of solution containing 1 mL of dilute hydrochloric acid (1:19) and 1 mL of 12% barium chloride reagent solution. Compare 10 min after adding the barium chloride to the sample and standard solutions.
Calcium, Magnesium, 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, Magnesium, Potassium, and Sodium
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 80 mL of water, add 2 mL of nitric acid (1:1), transfer to a 100 mL volumetric flask, dilute to the mark with water, and mix (1 mL = 0.20 g).
© 2017 American Chemical Society
B
DOI:10.1021/acsreagents.4010 ACS Reagent Chemicals, Part 4
ACS Reagent Chemicals
Monograph
pubs.acs.org/doi/book/10.1021/acsreagents
For the Determination of Calcium, Magnesium, 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
Mg
285.2
2.0
0.01; 0.02
A/A
Yes
K
766.5
2.0
0.02; 0.04
A/A
No
Na
589.0
0.40
0.01; 0.02
A/A
No
*A/A is air/acetylene; N/A is nitrous oxide/acetylene.
Heavy Metals ([Part 2: Trace and Ultratrace Elemental Analysis; Inductively Coupled Plasma−Optical Emission Spectroscopy (ICP–OES); Calculation of Heavy Metals (by ICP–OES) Results], heavy metals by ICP–OES). Sample size 1.0 g.
Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Dissolve 1.0 g in 50 mL of water, and use 25 mL of this solution.
© 2017 American Chemical Society
C
DOI:10.1021/acsreagents.4010 ACS Reagent Chemicals, Part 4
