STP of Purified Talc BP

Techno Drugs, Unit-2
B.K. Bari, Mirzapur, Gazipur

RAW MATERIAL TEST PROCEDURE
Ref. Doc. SOP No. TD2-QC-003-00
Name Purified Talc BP Code IE-013 Version 00 Spec. Ref. No. SIE-013
STP
TIE-013 Effective Date 23.02.2019 Next Review Date 22.02.2022 Page 1 of 9
No.
1. Appearance Spread approximately 3.0 g of sample over a white paper and

Ref. BP 2019 examine visually. Check the appearance for color, nature and any
visible foreign particles. Record its appearance, extraneous matter, if
any. The sample should be light, homogeneous, white or almost
white powder, greasy to the touch (non abrasive).
2. Solubility Practically insoluble in water, in ethanol (96 %) and in dilute
Ref. BP 2019 solutions of acids and alkali hydroxides:
Take about 10 mg of the sample in three different dry and clean 200
ml volumetric flasks. To each of these add 100 ml of purified water,
ethanol (96%) and dilute hydrochloric acid or dilute sodium hydroxide
respectively and shake. The dispersion should not be clear
(suspended particles will be observed).
3. Identification A. IR Spectrum:
Ref. BP 2019
Infrared absorption spectroscopy (ATR mode)
Fill the sample holder with test sample , then tight the screw slightly
and take IR spectrum. Similarly take IR spectrum of Working
standard or down load previous one working standard spectrum.
Compare both the spectrum.
IR spectrum of sample must corresponds to that of working standard.
4. Acidity or Bromothymol Blue Solution R1:

alkalinity:
Ref. BP 2019 Dissolve 50 mg of Bromothymol blue in a mixture of 4 ml of 0.02M
Sodium Hydroxide and 20 ml of ethanol (96%) and dilute to 100 ml
with purified water (pH range, 6.0 to 7.6).
Phenolphthalein Solution R1:A 1.0% w/v solution of

phenolphthalein in ethanol (96%).
Procedure:
Boil 2.5 g of sample with 50 ml of purified waterunder reflux. Filter in

vacuo. To 10 ml of the filtrate add 0.1 ml of bromothymol blue
Name Designation Signature & Date
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M A A Mahmud Sr. Executive, Quality Control
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Dr.Md.Moniruzzaman Manager, Quality Control
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Sk. Abu Naser Md. Shamim Manager, Quality Assurance
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Form No.: QC-003-01
STP
No.
solution R1; not more than 0.4 ml of 0.01 M hydrochloric acid is

required to change the colour of the indicator to green.To 10 ml of the
filtrate add 0.1 ml of phenolphthalein solution R1; add gradually 0.01
M Sodium Hydroxide to change the colour of the indicator to pink.
Limit: Not more than 0.3 ml of 0.01 M sodium hydroxide is required

to change the colour of the indicator to pink.
5. Water-soluble Limit: Not more than traces of matter other than starch granules are
substances: present. No starch grains of any other origin are present.
Ref. BP 2019
Procedure:
Examined under a microscope using a mixture of equal volumes of
glycerol R and water R, not more than traces of matter other than
starch granules are present. No starch grain of any other origin is
present.
6. Aluminium: AAS system:

Ref. BP 2019 Lamp :Aluminium hollow-cathode lamp.
Wavelength : 309.3 nm.
Atomisation device :Nitrous oxide-acetylene flame.
Blank solution: Use the mixture of 10.0 ml of hydrochloric acid and

10 ml of a 25.34 g/L solution of caesium chloride.
Aluminium Standard Solution (100 ppm Al):
Dissolve 8.947 g of aluminium chloride in 500 ml of purified water,

and dilute 1000 ml with purified water, mix. Immediately before use,
dilute 10 ml of this solution to 100 ml with purified water, mix.
Reference solutions:
Into 5 identical 100 ml volumetric flasks, each containing 10.0 ml of

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No.
hydrochloric acid and 10 ml of a 25.34 g/L solution of caesium

chloride, introduce respectively 5.0 ml, 7.5 ml, 10.0 ml, 15.0 ml and
20.0 ml of aluminium standard solution (100 ppm Al) and dilute to
100.0 ml with purified water, mix. These are 5 ppm, 7.5 ppm, 10 ppm,
15.0 ppm and 20 ppm respectively.
Test solution:
To 5.0 ml of solution S2, add 10 ml of a 25.34 g/L solution of caesium

chloride, 10.0 ml of hydrochloric acid and dilute to 100.0 ml with
purified water.
Procedure:
Take a blank reading then gradually take reading of reference

solutions and test solution.
From the concentration of Aluminium in test solution calculate the
content of aluminium in percentage.
Limit: Maximum 2.0%.
7. Calcium: AAS system:

Ref. BP 2019
Lamp : Calcium hollow-cathode lamp
Atomisation device : Nitrous oxide-acetylene flame.
Calcium Standard Solution (100 ppm Ca) R1:
Dissolve 0.2769 g of anhydrous calcium chloride (CaCl2) in 2M

Hydrochloric acid and dilute to 100 ml with the same solvent.
Immediately before use, dilute 1 ml of this solution to 10 ml with
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Form No.: QC-003-01
STP
No.
purified water, mix.
Lanthanum Chloride Solution:
To 58.65 g of lanthanumtrioxide add slowly 100 ml of Hydrochloric

acid and heat to boiling. Allow to cool and add sufficient water to
produce 1000 ml.
Blanksolution: Use the mixture of 10.0 ml of Hydrochloricacidand 10

ml of lanthanum chloride solution.

Hydrochloric acid and 10 ml of lanthanum chloride solution, introduce
respectively 1.0 ml, 2.0 ml,2.5 ml, 3.0 ml and 5.0 ml of calcium
standard solution (100 ppm Ca) R1 and dilute to 100.0 ml with
purified water. These are 1 ppm, 2 ppm , 2.5 ppm, 3 ppm and 5 ppm
respectively.
Test solution:
To 5.0 ml of solution S2 add 10.0 ml of hydrochloric acid, 10 ml of

lanthanum chloride solution and dilute to 100.0 ml with purified water.
Procedure:
From the concentration of calcium in test solution calculate the
content of calcium in percentage.
Limit: Maximum 0.9 %.

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No.
8. Iron: AAS system:

Ref. BP 2019
Lamp : Iron hollow-cathode lamp.
Atomisation device : Air-acetylene flame.
Correction : Deuterium lamp.
Blank solution:0.5 M Hydrochloric acid.
Iron Standard Solution (250 ppm Fe):
Dissolve 4.840 g of ferric chloride in 1.5 M hydrochloric acid and

dilute to 100 ml with the same solvent, mix. Immediately before use,
dilute 2.5 ml of this solution to 100 ml with purified water, mix.

0.5 M Hydrochloric acid, introduce respectively 2.0 ml, 2.5 ml, 3.0 ml
and 4.0 ml, 6.0 ml of iron standard solution (250 ppm Fe) and dilute
to 100.0 ml with purified water. These are 5 ppm, 6.25 ppm , 7.5 ppm,
10 ppm and 15 ppm respectively.
Test solution:
To 2.5 ml of solution S1, add 50.0 ml of 0.5 M Hydrochloric acid and

dilute to 100.0 ml with purified water, mix.
Procedure:

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9. Lead: AAS system:

Ref. BP 2019
Lamp : Lead hollow-cathode lamp.
Blank solution: 0.5 M Hydrochloric acid.
Lead Standard Solution (10 ppm Pb) R1:
Dissolve 0.160 g of lead nitrate in 100 ml of purified water and add 1

ml of lead-free nitric acid, dilute to 1000 ml with purified water, mix.
Immediately before use, dilute 10 ml of this solution to 100 ml with
purified water, mix.

0.5 M Hydrochloric acid , introduce respectively 5.0 ml, 7.5 ml, 10.0
ml,12.5 ml and 15.0 ml of lead standard solution (10 ppm Pb) R1 and
dilute to 100.0 ml with purified water. These are 0.5 ppm, 0.75 ppm, 1
ppm, 1.25 ppm and 1.5 ppm respectively.
Test solution:
Use solution S1.

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Procedure:
Limit: Maximum 10 ppm.
10. Magnesium: AAS system:

Ref. BP 2019
Lamp : Magnesium hollow-cathode lamp.
Magnesium Standard Solution (10 ppm Mg) R1:
Dissolve 8.365 g of magnesium chloride in 1000.0 ml of dilute

Hydrochloric acid, mix. Immediately before use, dilute 1 ml of this
solution to 100 ml with purified water, mix.
Lanthanum Chloride Solution:
To 58.65 g of lanthanumtrioxide add slowly 100 ml of Hydrochloric

acid and heat to boiling. Allow to cool and add sufficient water to
produce 1000 ml.
Blank solution: Use the mixture of 10.0 ml of Hydrochloric acid

and 10 ml of lanthanum chloride solution.

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Form No.: QC-003-01
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No.

Hydrochloric acid and 10 ml of lanthanum chloride solution, introduce
respectively 2.5 ml, 3.0 ml, 4.0 ml , 5.0 ml and 6.0 ml of magnesium
standard solution (10 ppm Mg) R1 and dilute to 100.0 ml with purified
water. These are 0.25 ppm, 0.3 ppm, 0.4 ppm, 0.5 ppm and 0.6 ppm
respectively.
Test solution:
Dilute 0.5 ml of solution S2 to 100.0 ml with purified water. To 4.0 ml

of the solution, add 10.0 ml of hydrochloric acid, 10 ml of lanthanum
chloride solution and dilute to 100.0 ml with purified water.
Procedure:
Limit:17.0 % to 19.5 %.
11. Loss on Equipment:

ignition:
Ref. BP 2019 a) Muffle furnace
b) Desiccator
c) Analytical Balance.
Procedure:
Ignite a silica crucible in a muffle furnace at 1050- 1100°C and cool in

a desiccator, weigh (W1).Weigh 1.00 g of sample (W2) and transfer it
into the silica crucible. Ignite in a muffle furnace to constant weight at
1050- 1100°C and cool in desiccator, weigh (W3).
Calculate the loss on ignition by the equation given below.

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Form No.: QC-003-01
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No.
Loss on ignition=
W 1  W 2  W 3  100 (% w/w)
W2
Where,
W1 = weight of ignited crucible in g

W2 = weight of crucible with sample in g
W3 = weight of crucible with sample after ignition in g
REVISION HISTORY
Version Effective Reason for Revision

No. Date
00 23.02.2019 New

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Techno Drugs, Unit-2

B.K. Bari, Mirzapur, Gazipur

1. Appearance Spread approximately 3.0 g of sample over a white paper and

4. Acidity or Bromothymol Blue Solution R1:

Phenolphthalein Solution R1:A 1.0% w/v solution of

Boil 2.5 g of sample with 50 ml of purified waterunder reflux. Filter in

THIS PRE-PRINTED BLUE BAND INDICATES MASTER DOCUMENT(S)

solution R1; not more than 0.4 ml of 0.01 M hydrochloric acid is

Limit: Not more than 0.3 ml of 0.01 M sodium hydroxide is required

6. Aluminium: AAS system:

Wavelength : 309.3 nm.

Atomisation device :Nitrous oxide-acetylene flame.

Blank solution: Use the mixture of 10.0 ml of hydrochloric acid and

Aluminium Standard Solution (100 ppm Al):

Dissolve 8.947 g of aluminium chloride in 500 ml of purified water,

Into 5 identical 100 ml volumetric flasks, each containing 10.0 ml of

THIS PRE-PRINTED BLUE BAND INDICATES MASTER DOCUMENT(S)

hydrochloric acid and 10 ml of a 25.34 g/L solution of caesium

To 5.0 ml of solution S2, add 10 ml of a 25.34 g/L solution of caesium

Take a blank reading then gradually take reading of reference

Limit: Maximum 2.0%.

7. Calcium: AAS system:

Calcium Standard Solution (100 ppm Ca) R1:

Dissolve 0.2769 g of anhydrous calcium chloride (CaCl2) in 2M

THIS PRE-PRINTED BLUE BAND INDICATES MASTER DOCUMENT(S)

purified water, mix.

Lanthanum Chloride Solution:

To 58.65 g of lanthanumtrioxide add slowly 100 ml of Hydrochloric

Blanksolution: Use the mixture of 10.0 ml of Hydrochloricacidand 10

Into 5 identical 100 ml volumetric flasks, each containing 10.0 ml of

To 5.0 ml of solution S2 add 10.0 ml of hydrochloric acid, 10 ml of

Limit: Maximum 0.9 %.

Name Designation Signature & Date

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8. Iron: AAS system:

Wavelength : 248.3 nm.

Atomisation device : Air-acetylene flame.

Correction : Deuterium lamp.

Blank solution:0.5 M Hydrochloric acid.

Iron Standard Solution (250 ppm Fe):

Dissolve 4.840 g of ferric chloride in 1.5 M hydrochloric acid and

Into 5 identical 100 ml volumetric flasks, each containing 50.0 ml of

To 2.5 ml of solution S1, add 50.0 ml of 0.5 M Hydrochloric acid and

Take a blank reading then gradually take reading of reference

THIS PRE-PRINTED BLUE BAND INDICATES MASTER DOCUMENT(S)

From the concentration of calcium in test solution calculate the

Limit: Maximum 0.25 %.

9. Lead: AAS system:

Wavelength : 217.0 nm.

Atomisation device : Air-acetylene flame.

Blank solution: 0.5 M Hydrochloric acid.

Lead Standard Solution (10 ppm Pb) R1:

Dissolve 0.160 g of lead nitrate in 100 ml of purified water and add 1

Into 5 identical 100 ml volumetric flasks, each containing 50.0 ml of

Use solution S1.

Name Designation Signature & Date

THIS PRE-PRINTED BLUE BAND INDICATES MASTER DOCUMENT(S)