JP XVI Official Monographs / Light Anhydrous Silicic Acid 1385

solution of Siccanin in ethanol (99.5) (1 in 10,000) as di- Mobile phase: A mixture of methanol and phosphate
rected under Ultraviolet-visible Spectrophotometry <2.24>, buffer solution, pH 5.9 (19:6).
and compare the spectrum with the Reference Spectrum or Flow rate: Adjust the flow rate so that the retention time
the spectrum of a solution of Siccanin RS obtained in the of siccanin is about 17 minutes.
same manner as the sample solution: both spectra exhibit System suitability—
similar intensities of absorption at the same wavelengths. System performance: When the procedure is run with 10
(2) Determine the infrared absorption spectrum of Sicca- mL of the standard solution under the above operating con-
nin as directed in the potassium bromide disk method under ditions, siccanin and the internal standard are eluted in this
the Infrared Spectrophotometry <2.25>, and compare the order with the resolution between these peaks being not less
spectrum with the Reference Spectrum or the spectrum of than 3.
Siccanin RS: both spectra exhibit similar intensities of ab- System repeatability: When the test is repeated 6 times
sorption at the same wave numbers. with 10 mL of the standard solution under the above operat-
ing conditions, the relative standard deviation of the ratios
Optical rotation <2.49> [a]20
D : －165 – －1759(0.1 g, ethanol
of the peak area of siccanin to that of the internal standard is
(99.5), 10 mL, 100 mm).
not more than 1.0z.
Melting point <2.60> 138 – 1429C
Containers and storage Containers—Tight containers.
Purity (1) Heavy metals <1.07>—Proceed with 1.0 g of
Siccanin according to Method 4, and perform the test. Pre-
pare the control solution with 2.0 mL of Standard Lead So- Light Anhydrous Silicic Acid
lution (not more than 20 ppm).
(2) Related substances—Dissolve 0.20 g of Siccanin in 10 軽質無水ケイ酸
mL of acetone, and use this solution as the sample solution.
Pipet 1 mL of the sample solution, add acetone to make ex-
Light Anhydrous Silicic Acid, calculated on the in-
actly 200 mL, and use this solution as the standard solution.
cinerated basis, contains not less than 98.0z of silicon
Perform the test with these solutions as directed under Thin-
dioxide (SiO2: 60.08).
layer Chromatography <2.03>. Spot 5 mL each of the sample
solution and standard solution on a plate of silica gel for Description Light Anhydrous Silicic Acid occurs as a white
thin-layer chromatography. Develop the plate with a mixture to bluish white, light, fine power. It is odorless and tasteless,
of cyclohexane and acetone (5:1) to a distance of about 10 and smooth to the touch.
cm, and air-dry the plate. Spray evenly 4-chlorobenzenedia- It is practically insoluble in water, in ethanol (95), and in
zonium TS on the plate: the number of the spots other than diethyl ether.
the principal spot obtained from the sample solution is not It dissolves in hydrofluoric acid, in hot potassium hydrox-
more than three, and they are not more intense than the spot ide TS and in hot sodium hydroxide TS, and does not dis-
from the standard solution. solve in dilute hydrochloric acid.
Loss on drying <2.41> Not more than 0.5z (1 g, reduced Identification (1) Dissolve 0.1 g of Light Anhydrous
pressure not exceeding 0.67 kPa, 809C, 3 hours). Silicic Acid in 20 mL of sodium hydroxide TS by boiling,
and add 12 mL of ammonium chloride TS: a white,
Residue on ignition <2.44> Not more than 0.1z (1 g).
gelatinous precipitate is produced. The precipitate does not
Assay Weigh accurately an amount of Siccanin and Sicca- dissolve in dilute hydrochloric acid.
nin RS, equivalent to about 50 mg (potency), dissolve each in (2) To the precipitate obtained in (1) add 10 mL of a so-
the internal standard solution to make exactly 50 mL, and lution of methylene blue trihydrate (1 in 10,000), and wash
use these solutions as the sample solution and standard solu- with water: the precipitate has a blue color.
tion. Perform the test with 10 mL each of the sample solution (3) Prepare a bead by fusing ammonium sodium
and standard solution as directed under Liquid Chromatog- hydrogenphosphate tetrahydrate on a platinum loop. Bring
raphy <2.01> according to the following conditions, and cal- the hot, transparent bead into contact with Light Anhydrous
culate the ratios, QT and QS, of the peak area of siccanin to Silicic Acid, and fuse again: an insoluble matter is percepti-
that of the internal standard. ble in the bead. The resulting bead, upon cooling, becomes
opaque and acquires a reticulated appearance.
Amount [ mg (potency)] of C22H30O3
＝ MS × QT/QS × 1000 Purity (1) Chloride <1.03>—Dissolve 0.5 g of Light An-
hydrous Silicic Acid in 20 mL of sodium hydroxide TS by
MS: Amount [mg (potency)] of Siccanin RS
boiling, cool, filter if necessary, and wash with 10 mL of
Internal standard solution—A solution of 1,4-diphenylben- water. Combine the filtrate and washings, add 18 mL of di-
zene in methanol (1 in 30,000). lute nitric acid, shake, and add water to make 50 mL. Per-
Operating conditions— form the test using this solution as the test solution. To 0.15
Detector: An ultraviolet absorption photometer (wave- mL of 0.01 mol/L hydrochloric acid VS add 20 mL of sodi-
length: 280 nm). um hydroxide TS, 18 mL of dilute nitric acid and water to
Column: A stainless steel column 4.6 mm in inside diame- make 50 mL, and use this solution as the control solution
ter and 15 cm in length, packed with octadecylsilanized silica (not more than 0.011z).
gel for liquid chromatography (5 mm in particle diameter). (2) Heavy metals <1.07>—Dissolve 0.5 g of Light Anhy-
Column temperature: A constant temperature of about drous Silicic Acid in 20 mL of sodium hydroxide TS by boil-
409 C. ing, cool, add 15 mL of acetic acid (31), shake, filter if nec-
1386 Silver Nitrate / Official Monographs JP XVI
essary, wash with 10 mL of water, combine the filtrate and ric acid, and heat. Allow to cool to room temperature, add
washings, and add water to make 50 mL. Perform the test 20 to 25 mL of hot water, filter rapidly, and wash the residue
using this solution as the test solution. Add acetic acid (31) with warm water until the last washing becomes negative to
to 20 mL of sodium hydroxide TS and 1 drop of phenol- the Qualitative Tests <1.09> (2) for chloride. Transfer the
phthalein TS until the color of this solution disappears, add residue together with the filter paper to a platinum crucible,
2.0 mL of Standard Lead Solution, 2 mL of dilute acetic ignite to ash, and continue the ignition for 30 minutes. Cool,
acid and water to make 50 mL, and use this solution as the weigh the crucible, and designate the mass as a (g). Moisten
control solution (not more than 40 ppm). the residue in the crucible with water, add 6 mL of hydro-
(3) Iron <1.10>—To 40 mg of Light Anhydrous Silicic fluoric acid and 3 drops of sulfuric acid, and evaporate to
Acid add 10 mL of dilute hydrochloric acid, and heat for 10 dryness. Heat strongly for 5 minutes, cool, weigh the cruci-
minutes in a water bath while shaking. After cooling, add ble, and designate the mass as b (g).
0.5 g of L-tartaric acid to dissolve by shaking. Prepare the
Content (g) of silicon dioxide (SiO2) ＝ a － b
test solution with this solution according to Method 2, and
perform the test according to Method B. Prepare the control Containers and storage Containers—Tight containers.
solution with 2.0 mL of Standard Iron Solution (not more
than 500 ppm).
(4) Aluminum—Dissolve 0.5 g of Light Anhydrous Silver Nitrate
Silicic Acid in 40 mL of sodium hydroxide TS by boiling,
cool, add sodium hydroxide TS to make 50 mL, and filter. 硝酸銀
Measure 10 mL of the filtrate, add 17 mL of acetic acid (31),
shake, add 2 mL of aluminon TS and water to make 50 mL,
AgNO3: 169.87
and allow to stand for 30 minutes: the color of this solution
is not deeper than that of the following control solution.
Silver Nitrate, when dried, contains not less than
Control solution: Dissolve 0.176 g of aluminum potassium
99.8z of AgNO3.
sulfate dodecahydrate in water, and add water to make 1000
mL. To 15.5 mL of this solution add 10 mL of sodium hy- Description Silver Nitrate occurs as lustrous, colorless or
droxide TS, 17 mL of acetic acid (31), 2 mL of aluminon TS white crystals.
and water to make 50 mL. It is very soluble in water, soluble in ethanol (95), and
(5) Calcium—Dissolve 1.0 g of Light Anhydrous Silicic practically insoluble in diethyl ether.
Acid in 30 mL of sodium hydroxide TS by boiling, cool, add It gradually turns grayish black by light.
20 mL of water, 1 drop of phenolphthalein TS and dilute
Identification A solution of Silver Nitrate (1 in 50) re-
nitric acid until the color of this solution disappears, imme-
sponds to the Qualitative Tests <1.09> for silver salt and for
diately add 5 mL of dilute acetic acid, shake, add water to
nitrate.
make 100 mL, and obtain a clear liquid by centrifugation or
filtration. To 25 mL of this liquid add 1 mL of oxalic acid Purity (1) Clarity and color of solution, and acidity or
TS and ethanol (95) to make 50 mL, immediately shake, and alkalinity—Dissolve 1.0 g of Silver Nitrate in 10 mL of
allow to stand for 10 minutes: the turbidity of this solution is freshly boiled and cooled water: the solution is clear and
not deeper than that of the following control solution. colorless. It is neutral.
Control solution: Dissolve 0.250 g of calcium carbonate, (2) Bismuth, copper and lead—To 5 mL of a solution of
previously dried at 1809 C for 4 hours, in 3 mL of dilute hy- Silver Nitrate (1 in 10) add 3 mL of ammonia TS: the solu-
drochloric acid, and add water to make 100 mL. To 4 mL of tion is clear and colorless.
this solution add 5 mL of dilute acetic acid and water to
Loss on drying <2.41> Not more than 0.20z (2 g, silica gel,
make 100 mL. To 25 mL of this solution add 1 mL of oxalic
light resistant, 4 hours).
acid TS and ethanol (95) to make 50 mL, and shake.
(6) Arsenic <1.11>—Dissolve 0.40 g of Light Anhydrous Assay Weigh accurately about 0.7 g of Silver Nitrate, pre-
Silicic Acid in 10 mL of sodium hydroxide TS by boiling in a viously powdered and dried, dissolve in 50 mL of water, add
porcelain crucible, cool, add 5 mL of water and 5 mL of di- 2 mL of nitric acid, and titrate <2.50> with 0.1 mol/L ammo-
lute hydrochloric acid, shake, and perform the test with this nium thiocyanate VS (indicator: 2 mL of ammonium iron
solution as the test solution (not more than 5 ppm). (III) sulfate TS).
Loss on drying <2.41> Not more than 7.0z (1 g, 1059C, Each mL of 0.1 mol/L ammonium thiocyanate VS
4 hours). ＝ 16.99 mg of AgNO3
Loss on ignition <2.43> Not more than 12.0z (1 g, 850 – Containers and storage Containers—Tight containers.
9009C, constant mass). Storage—Light-resistant.
Volume test Weigh 5.0 g of Light Anhydrous Silicic Acid,
transfer gradually to a 200-mL measuring cylinder, and al-
low to stand: the volume is not less than 70 mL.
Assay Weigh accurately about 1 g of Light Anhydrous
Silicic Acid, add 20 mL of hydrochloric acid, and evaporate
to dryness on a sand bath. Moisten the residue with hydro-
chloric acid, evaporate to dryness, and heat between 1109C
and 1209C for 2 hours. Cool, add 5 mL of dilute hydrochlo-