Magnesium Hydroxide, Exams of Chemistry

(3) Magnesium Glycerophosphate responds to the. Qualitative Tests for magnesium. Purity (1) Clarity and color of solution—Dissolve. 2.5 of Magnesium ...

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KP X 765
the dried basis.
Description Magnesium Glycerophosphate appears
as white powder.
Magnesium Glycerophosphate is practically insoluble
in ethanol (95).
Magnesium Glycerophosphate dissolves in dilute solu-
tions of acids.
Magnesium Glycerophosphate is hygroscopic.
Identification (1) Mix 1 g of Magnesium Glycero-
phosphate with 1 g of potassium hydrogen sulfate in a
test tube fitted with a glass tube. Heat strongly and
direct the white vapor towards a piece of filter paper
impregnated with a freshly prepared 1 w/v % sodium
pentacyanonitrosylferrate (III) dihydrate solution: the
filter paper develops a blue color in contact with
piperidine.
(2) Ignite 0.1 g of Magnesium Glycerophosphate in
a crucible, add 5 mL of nitric acid to the residue, heat
in a water-bath for 1 min and filter. The filtrate re-
sponds to the Qualitative Tests (2) for phosphate.
(3) Magnesium Glycerophosphate responds to the
Qualitative Tests for magnesium.
Purity (1) Clarity and color of solution
Dissolve
2.5 of Magnesium Glycerophosphate in 50 mL of water:
this solution is not more opalescent than the reference
suspension
Reference suspensionTo 30 mL of standard sus-
pension, add 70 mL of water. Prepare when use and
shake well before use.
Standard suspensionPrepare as directed in the
reagent under the Test Methods for Plastic Containers.
(2) Acid
Dissolve 1.0 g of Magnesium Glycero-
phosphate in 100 mL of water and titrate with 0.1
mol/L sodium hydroxide VS (indicator: 2 drops of
phenolphthalein TS): less than 1.5 mL of 0.1 mol/L
sodium hydroxide VS consumed.
(3) Chloride
Proceed with 0.20 g Magnesium
Glycerophosphate and perform the test. Prepare the
control solution with 0.84 mL of 0.01 mol/L hydro-
chloric acid VS (not more than 0.015 %).
(4) Sulfate
Proceed with 0.20 g of Magnesium
Glycerophosphate and perform the test. Prepare the
control solution with 0.42 mL of 0.005 mol/L sulfuric
acid VS (not more than 0.1 %).
(5) Phosphate
Dissolve 2.5 g of Magnesium
Glycerophosphate in 50 mL of water. Pipet 4.0 mL of
this solution and add water to make 100 mL. Pipet 1.0
mL of this solution, add water to make 100 mL and use
this solution as the test solution. To 100 mL of the test
solution, add 4 mL of sulfomolybdic TS and 0.1 mL of
tin (II) chloride TS and allow the mixture to stand for
10 minutes: the color from this solution is not more
intense than that from a solution containing 2 mL of
standard phosphate solution and 98 mL of water (not
more than 0.5 %).
(6) Heavy metals
Dissolve 1.0 g of Magnesium
Glycerophosphate in 20 mL of water, add 15 mL of
hydrochloric acid and 25 mL of 4-methyl-2-pentanone,
and mix by shaking for 1 minute. After standing, take
the aqueous layer and evaporate to dryness. Dissolve
the residue in 2 mL of dilute acetic acid, add 50 mL of
water and perform the test using this solution as the test
solution. Prepare the control solution with 2.0 mL of
standard lead solution (not more than 20 ppm).
(7) Iron
Place 67 mg of Magnesium Glycero-
phosphate to a Nessler tube, add water to make 10 mL,
add 2 mL of 20 w/v % citric acid solution and 0.1 mL
of mercaptoacetic acid to mix, make the solution alka-
line by the addition of 10 mol/L ammonia water, add
water to make 20 mL and allow this solution to stand
for 5 minutes: the color from this solution is not more
intense than that from diluted standard iron solution (1
in 10) (not more than 150 ppm).
(8) Glycerol and alcohol-soluble substances
To
1.0 g of Magnesium Glycerophosphate, add 25 ml of
ethanol (95), mix by shaking for 2 min, filter and wash
the residue with 5 ml of ethanol (95). Combine the
filtrate and the washings, evaporate to dryness in a wa-
ter-bath, dry the residue at 70 °C for 1 h and weigh (not
more than 1.5 %).
Loss on Drying Not more than 12.0 % (1 g, 150 °C,
4 hours).
Assay Weigh accurately 0.2 g of Magnesium
Glycerophosphate, add 40 mL of water to dissolve, add
10 mL of ammonia-ammonium chloride buffer solution,
pH 10 and titrate with 0.1 mol/L disodium
ethylenediaminetetraacetate VS (indicator: 50 mg of
eriochrome black T-sodium chloride TS) until the color
of the solution changes from purple to blue.
Each mL of 0.1 mol/L
disodium ethylenediaminetetraacetate VS
= 2.431 mg of Mg
Containers and Storage Containers—Tight con-
tainers.
Magnesium Hydroxide
Mg(OH)2: 58.32
Magnesium dihydroxide [1309-42-8]
Magnesium Hydroxide, when dried, contains not less
than 95.0 % and not more than 100.5 % of magnesium
hydroxide [Mg(OH)2].
Description Magnesium Hydroxide is a white bulky
powder.
Magnesium Hydroxide is practically insoluble in water
or ethanol (95).
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KP X 765

the dried basis.

Description Magnesium Glycerophosphate appears as white powder. Magnesium Glycerophosphate is practically insoluble in ethanol (95). Magnesium Glycerophosphate dissolves in dilute solu- tions of acids. Magnesium Glycerophosphate is hygroscopic.

Identification (1) Mix 1 g of Magnesium Glycero- phosphate with 1 g of potassium hydrogen sulfate in a test tube fitted with a glass tube. Heat strongly and direct the white vapor towards a piece of filter paper impregnated with a freshly prepared 1 w/v % sodium pentacyanonitrosylferrate (III) dihydrate solution: the filter paper develops a blue color in contact with piperidine. (2) Ignite 0.1 g of Magnesium Glycerophosphate in a crucible, add 5 mL of nitric acid to the residue, heat in a water-bath for 1 min and filter. The filtrate re- sponds to the Qualitative Tests (2) for phosphate. (3) Magnesium Glycerophosphate responds to the Qualitative Tests for magnesium.

Purity (1) Clarity and color of solution ⎯Dissolve

2.5 of Magnesium Glycerophosphate in 50 mL of water: this solution is not more opalescent than the reference suspension

Reference suspension ⎯To 30 mL of standard sus- pension, add 70 mL of water. Prepare when use and shake well before use.

Standard suspension ⎯Prepare as directed in the reagent under the Test Methods for Plastic Containers.

(2) Acid ⎯Dissolve 1.0 g of Magnesium Glycero-

phosphate in 100 mL of water and titrate with 0. mol/L sodium hydroxide VS (indicator: 2 drops of phenolphthalein TS): less than 1.5 mL of 0.1 mol/L sodium hydroxide VS consumed.

(3) Chloride ⎯Proceed with 0.20 g Magnesium

Glycerophosphate and perform the test. Prepare the control solution with 0.84 mL of 0.01 mol/L hydro- chloric acid VS (not more than 0.015 %).

(4) Sulfate ⎯Proceed with 0.20 g of Magnesium

Glycerophosphate and perform the test. Prepare the control solution with 0.42 mL of 0.005 mol/L sulfuric acid VS (not more than 0.1 %).

(5) Phosphate ⎯Dissolve 2.5 g of Magnesium

Glycerophosphate in 50 mL of water. Pipet 4.0 mL of this solution and add water to make 100 mL. Pipet 1. mL of this solution, add water to make 100 mL and use this solution as the test solution. To 100 mL of the test solution, add 4 mL of sulfomolybdic TS and 0.1 mL of tin (II) chloride TS and allow the mixture to stand for 10 minutes: the color from this solution is not more intense than that from a solution containing 2 mL of standard phosphate solution and 98 mL of water (not

more than 0.5 %).

(6) Heavy metals ⎯Dissolve 1.0 g of Magnesium

Glycerophosphate in 20 mL of water, add 15 mL of hydrochloric acid and 25 mL of 4-methyl-2-pentanone, and mix by shaking for 1 minute. After standing, take the aqueous layer and evaporate to dryness. Dissolve the residue in 2 mL of dilute acetic acid, add 50 mL of water and perform the test using this solution as the test solution. Prepare the control solution with 2.0 mL of standard lead solution (not more than 20 ppm).

(7) Iron ⎯Place 67 mg of Magnesium Glycero-

phosphate to a Nessler tube, add water to make 10 mL, add 2 mL of 20 w/v % citric acid solution and 0.1 mL of mercaptoacetic acid to mix, make the solution alka- line by the addition of 10 mol/L ammonia water, add water to make 20 mL and allow this solution to stand for 5 minutes: the color from this solution is not more intense than that from diluted standard iron solution ( in 10) (not more than 150 ppm).

(8) Glycerol and alcohol-soluble substances ⎯To

1.0 g of Magnesium Glycerophosphate, add 25 ml of ethanol (95), mix by shaking for 2 min, filter and wash the residue with 5 ml of ethanol (95). Combine the filtrate and the washings, evaporate to dryness in a wa- ter-bath, dry the residue at 70 °C for 1 h and weigh (not more than 1.5 %).

Loss on Drying Not more than 12.0 % (1 g, 150 °C, 4 hours).

Assay Weigh accurately 0.2 g of Magnesium Glycerophosphate, add 40 mL of water to dissolve, add 10 mL of ammonia-ammonium chloride buffer solution, pH 10 and titrate with 0.1 mol/L disodium ethylenediaminetetraacetate VS (indicator: 50 mg of eriochrome black T-sodium chloride TS) until the color of the solution changes from purple to blue.

Each mL of 0.1 mol/L disodium ethylenediaminetetraacetate VS = 2.431 mg of Mg

Containers and Storage Containers— Tight con- tainers.

Magnesium Hydroxide

Mg(OH) 2 : 58.

Magnesium dihydroxide [ 1309-42-8 ]

Magnesium Hydroxide, when dried, contains not less than 95.0 % and not more than 100.5 % of magnesium hydroxide [Mg(OH) (^) 2].

Description Magnesium Hydroxide is a white bulky powder. Magnesium Hydroxide is practically insoluble in water or ethanol (95).

766 Monographs, Part I

Magnesium Hydroxide is soluble in dilute hydrochloric acid.

Identification A 3 mol/L solution of Magnesium Hydroxide in hydrochloric acid TS (1 in 20) responds to the Qualitative Tests (1) for magnesium.

Purity (1) Soluble salts— Boil 2.0 g of Magnesium Hydroxide with 100 mL of water for 5 minutes in a covered beaker, filter while hot, cool, and dilute the filtrate with water to 100 mL. Titrate 50 mL of the di- luted filtrate with 0.1 mol/L sulfuric acid, using methyl red TS as the indicator: not more than 2.0 mL of acid is consumed. Evaporate 25 mL of the diluted filtrate to dryness, and dry at 105 °C for 3 hours: not more than 10 mg of residue remains. (2) Carbonate— Boil a mixture of 0.10 g of Mag- nesium Hydroxide with 5 mL of water, cool, and add 5 mL of 6 mol/L acetic acid: not more than a slight ef- fervescence is observed. (3) Calcium— Transfer 0.25 g of Magnesium Hy- droxide, previously dried, to a beaker, add 30 mL of dilute hydrochloric acid (1 in 10), and stir until dis- solved, heating if necessary. Transfer this solution to a 200 mL volumetric flask containing 4 mL of lantha- num TS, dilute with water to volume, mix, and use this solution as the test solution. Separately, Weigh accu- rately 249.7 mg of calcium chloride, previously dried at 300 °C for 3 hours and cooled in a silica gel desicca- tor for 2 hours, dissolve in small quantities of hydro- chloric acid, dilute with water to exactly 100 mL. Pipet each 5.0, 10.0, 15.0 mL of this solution, put each in 1000 mL volumetric flasks, add each 20 mL of Lan- thanum TS and 40 mL of diluted hydrochloric acid ( in 10), dilute with water to volume and use these solu- tions as the standard solutions. 1 mL of each standard solution contains 5.0, 10.0, 15.0 μg of calcium, respec- tively. Transfer 4 mL of Lanthanum TS and 10 mL of diluted hydrochloric acid (1 in 10) in a 200 mL volu- metric flask and dilute with water to volume and use this solution as the balnk solution. Perform the test with the blank, the test, and the standard solutions as directed under the Atomic Absorption Spectrophotome- try according to the following conditions and calculate the calcium content of the test solution from the cali- bration curve obtained from the absorbance of the standard solution (not more than 1.5 %).

Gas: Dissolved acetylene – Air. Lamp: A calcium hollow cathode lamp. Wavelength: 422.7 nm.

(4) Heavy metals —Dissolve 1.0 g of Magnesium Hydroxide in 15 mL of 3 mol/L hydrochloric acid TS, and evaporate the solution on a steam bath to dryness. Dissolve the residue in 20 mL of water, and filter. To the filtrate, add 2 mL of 1 mol/L acetic acid, which should be neutral to litmus, dilute with water to 50 mL and use this solution as test solution. Separately, pre- pare the control solution with 15 mL of 3 mol/L hydro-

chloric acid in the same manner as the test solution and 2.0 mL of standard lead solution (not more than 20 ppm) directed for the preparation of the control solu- tion. (5) Lead —Dissolve 1.0 g of Magnesium Hydrox- ide in 20 mL of 3 mol/L hydrochloric acid TS and use this solution as the test solution. Transfer the test solu- tion into a separatory funnel, wash with 10 mL of wa- ter, and combine the washings into the separatory fun- nel. Add 6 mL of a solution of diammonium hydrogen citrate and 2 mL of hydroxylamine hydrochloride TS and 2 drops of phenolred, and alkalinize with strong ammonia water. Allow to cool if necessary, add 2 mL of potassium cyanide solution, extract with each 5 mL of dithizone solution for extraction until the extract become green, and combine the extracts in a separatory funnel. To the combined extracts add 20 mL of diluted nitric acid (1 in 100), shake for 30 second to mix, and discard the chloroform layer. To the nitric acid layer add 5.0 mL of standard dithizone solution and 4 mL of ammonia–cyanide TS, shake for 30 second, and com- pare the color of the solution with that of the control solution obtained from the same procedure with 1. mL of diluted standard lead solution (1 in 10): the color obtained from the test solution is not darker than that from the control solution (not more than 1.5 ppm).

Ammonia–cyanide TS —Dissolve 2 g of potassium cyanide in 15 mL of ammonia solution (28) and dilute with water to 100 mL.

(6) Arsenic ⎯To 0.5 g of Magnesium Hydroxide add 10 mL of dilute hydrochloric acid, and warm to dissolve. After cooling, use this solution as the test solution and perform the test (not more than 4 ppm).

Loss on Drying Not more than 2.0 % (1 g, 105 °C, 2 hours).

Loss on Ignition 30.0 ~ 33.0 % (1 g, 800 °C).

Microbial Limit Escherichia coli is not observed.

Assay Weigh accurately about 75 mg of Magnesium Hydroxide, previously dried, and transfer to a conical flask. Add 2 mL of 3 mol/L hydrochloride TS and swirl to dissolve. Add 100 mL of water and adjust the reaction of the solution to a pH of 7 with 1 mol/L sodi- um hydroxide TS, add 5 mL of ammonia·ammonium chloride buffer solution, pH 10.7, and titrate with 0. mol/L disodium ethylenediaminetetraacetate VS until the color of the solution changes to blue (indicator : 0.15 mL of eriochrome black T TS)

Each mL of 0.05 mol/L disodium ethylenediaminetetraacetate VS = 2.916 mg Mg(OH) (^2)

Containers and Storage Containers— Tight con- tainers.