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Stp Pharma

The document outlines the method of analysis for Pharma Sugar Grade (IP), detailing its physical properties, solubility, identification tests, and limits for various impurities such as heavy metals and sulfites. It includes specific procedures for testing acidity, optical rotation, barium, calcium, and other components, along with calculations for determining acceptable limits. The document emphasizes the importance of maintaining specific conditions during testing to ensure accurate results.

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kuldeep kaushik
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26 views

Stp Pharma

The document outlines the method of analysis for Pharma Sugar Grade (IP), detailing its physical properties, solubility, identification tests, and limits for various impurities such as heavy metals and sulfites. It includes specific procedures for testing acidity, optical rotation, barium, calcium, and other components, along with calculations for determining acceptable limits. The document emphasizes the importance of maintaining specific conditions during testing to ensure accurate results.

Uploaded by

kuldeep kaushik
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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METHOD OF ANALYSIS

PHARMA SUGAR GRADE (IP)


Description:
Dry, Colourless crystals or almost white crystalline powder; odorless; taste sweet.

Solubility:
Very soluble in water ( 1 g in less than 1 ml)
Freely soluble in ethanol (70%); (1 gin 1 to 10 ml)
Sparingly soluble in ethanol ( 1 g in 30 to 100 ml)

Identification:
Dissolve 150.0 g in sufficient carbon dioxide-free water prepared from distilled water to produce
300ml ( solution A). Dilute 1 ml of solution A to 100 ml with water. To 5 ml of the solution add
2 ml of freshly prepared 2M sodium hydroxide and 0.15ml of freshly prepared copper sulphate
solution: the solution is clear and blue and remains so on boiling. To the hot solution add 4 ml of
2M hydrochloric acid, heat to boiling and add 4 ml of 2M sodium hydroxide; an orange
precipitate is produced immediately.

Acidity or Alkalinity:
To 10 ml of solution A, add 0.3 ml of phenolphthalein solution. The solution is colorless.
Titrate with 0.01 M Sodium hydroxide until the colour of the solution changes to pink.
Calculation: Acidity or Alkalinity: Burette reading x exact molarity of sodium hydroxide x 150
Wt. of sample in g x 0.01
Limit : Not more than 0.6 ml of 0.01M sodium hydroxide is required to change the color of the
solution to pink.

Specific Optical rotation = Observed angle x 100 Length of tube in dm X sample weight in g
Limit : Between +65.9° and +67.0° determined in a 10% w/v solution.

Barium : Test Solution: To 10 ml of solution A, add 1 ml of 1 M sulphuric acid. Standard


Solution: A mixture of 1 ml of distilled water and 10 ml of solution A. Examine immediately and
after 1 hour. Observation: Any opalescence produced with test solution is not more intense than
that of standard solution.

Calcium: To 1 ml of solution A add 8 ml of water and 1 ml of ammonium oxalate solution: The


solution remains clear for at least 1 minute.
Heavy Metals :
Lead standard solution ( 20 ppm Pb) : Dilute 1 volume of lead standard ( 100 ppm Pb) to 5
volume with water.
Standard Preparation : Into a 50 ml Nessler cylinder pipette 1.0 ml of standard lead solution (
20 ppm Pb), and dilute with water to 25 ml. Adjust with dilute acetic acid or dilute ammonia
solution to a pH between 3.0 and 4.0 , dilute with water to 35 ml , and mix.
Test Preparation : Into a 50-ml Nessler cylinder place 25 ml of the solution prepared by adding
8 ml of solution A, 0.1 ml of dilute hydrochloric acid and sufficient water to produce 25 ml.
Adjust with dilute acid or dilute ammonia solution to a pH between 3.0 and 4.0, dilute with water
to 35 ml , and mix.
Procedure : To each of the cylinder containing the standard solution and test solution
respectively add 10 ml of freshly prepared hydrogen sulphide solution, and mix, dilute to 50 ml
with water, allow to stand for 5 minutes and view downwards over a white surface.
Observation : The color produced with the test preparation should be less intense than color
produced with standard preparation.
Limit : Not more than 10 ppm

Sulphite : To 4 ml of solution A add sufficient water to produce 20 ml, add 0.05 ml of 0.1M
iodine and 0.05 ml of starch solution: a blue colour develops.

Dextrins : To 2 ml of solution A add 8 ml of water, 0.05 ml of 2M hydrochloric acid and 0.05


ml of 0.05M iodine; the solution remains yellow or becomes faint bluish green.

Colouring Matter:
1) To 100 ml of solution A in ground glass-stoppered tube, add 1 ml of dilute hypophosphorous
acid and allow to stand for 1 hour. No unpleasant odour is detectable.
2) Test solution: Use solution A
Standard Solution: weigh and transfer accurately about 10 mg of quinine sulphate into 250ml
volumetric flask, dissolve in 0.005 M sulphuric acid, and dilute to 250 ml with 0.005 M
sulphuric acid. Dilute 1 ml of this solution to 100 ml with 0.005 sulphuric acid.
Observation: When examined under ultra-violet light ( 365 nm), any fluorescence produced
with test solution is not more intense than that of standard solution.
Sulphated ash:
Heat a silica or platinum crucible to redness at 800 +/- 25 deg. C for 10 minutes, allow to cool in
a desiccator and weigh ( W1). Transfer to the crucible accurately about 5 g of the sample and
weigh the crucible and contents accurately ( W2) , dissolve in 5 ml water, Heat gently until the
substance is thoroughly charred, cool , then moisten the residue with 2 ml sulphuric acid, heat
gently until white fumes are no longer evolved and ignite at 800 +/- 25 deg. C until the carbon is
consumed. Cool in a dessicator, weigh ( W3) and calculate the percentage of residue. Repeat the
operation until two successive weighing do not differ by than 0.5 mg. The final weight will be (
W3).
Calculation :
Sulphated Ash = W3-W1 /W2-W1 x 100
Limit : Not more than 0.1%

Glucose and Invert Sugar:


Dissolve 50g in water and dilute to 100.00ml with the same solvent. To 5.0ml of this solution in
a test tube about 150mm long and 16mm in diameter add 05 ml of water, 1.0ml of 1M Sodium
hydroxide and 1.0ml of a 0.1 percent solution of methylene blue. Mix and place in a water-
bath. After exactly 02 minutes, take the test tube out of the bath and examine the solution
immediately.
The blue colour does not diappear completely. Ignore any blue colour at the air/solution
interface.

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