CALCIUM CARBONATE SOP


CALCIUM CARBONATE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Calcium carbonate from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  White or almost white powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (1 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Purified water.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take a test tube and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add purified water in it and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube containing with water is practically insoluble.
5.2  Solution S:
5.2.1        Material and equipment:
5.2.1.1  Glassware (1 100.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.2.1.2  Dilute acetic acid.
5.2.1.3  Water-bath.
5.2.1.4  Analytical weighing balance.
5.2.1.5  Magnetic stirrer.
5.2.2        Sample:
5.2.2.1  5.0g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 100.0ml and add sample 5.0g in it.
5.2.3.2  Add in it 80.0ml of dilute acetic acid.
5.2.3.3  Dissolve it by using magnetic stirrer operate.
5.2.3.4  When the effervescence ceases, boil for 2min on water-bath.
5.2.3.5  Allow it to cool.
5.2.3.6  Dilute it to 100.0ml with dilute acetic acid.
5.2.3.7  Filter it by using filtration apparatus, if necessary, through the sintered-glass filter.
5.3  Identification tests:
5.3.1        Carbonates test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (test tubes, beakers, spatula, stirrer & stoppers of test tube).
5.3.1.1.2        Magnetic stirrer.
5.3.1.1.3        3.0ml of 2M acetic acid.
5.3.1.1.4        5.0ml of 0.1M barium hydroxide.
5.3.1.1.5        Excess of 7M hydrochloric acid.
5.3.1.1.6        Magnesium sulfate.
5.3.1.1.7        Purified water (q.s).
Test no.
Sample
Method
Observation
1.
0.1g
Take a test tube and add 0.1g of sample in it. Dissolve in 2.0ml of purified water.
Add 3.0ml of 2M acetic acid in another test tube.
Close the test tube immediately using a stopper fitted with a glass tube bent at two right angles.
The solution or suspension produces effervesce evolving a colourless and odorless gas.
Heat it gently on burner & collect gas in 5.0ml of 0.1M barium hydroxide, which is in another test tube taken.
Observe change in colour and appearance of solution after addition of an excess of 7M hydrochloric acid.
A white ppt is produced which dissolves on addition of an excess of 7M hydrochloric acid.
2.
Solution S
Take a test tube and add solution S in it.
Add in it solution of magnesium sulfate.
Observe changes.
A white ppt is produced (distinction from bicarbonates).

5.3.2        Calcium test:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (according to requirement).
5.3.2.1.2        0.5ml of a 2.0g/L solution of glyoxal-hydroxyanil in ethanol (96%).
5.3.2.1.3        0.2ml of dilute sodium hydroxide solution.
5.3.2.1.4        0.2ml of sodium carbonate solution.
5.3.2.1.5        Chloroform (1-2ml).
5.3.2.1.6        Purified water.
5.3.2.2  Sample:
5.3.2.2.1        0.2ml of solution S.
5.3.2.3  Method of analysis:
5.3.2.3.1        Take a test tube and add 0.2ml of solution S.
5.3.2.3.2        Add 0.5ml of a 2.0g/L solution of glyoxal-hydroxyanil in ethanol (96%), 0.2ml of dilute sodium hydroxide solution, 0.2ml of sodium carbonate solution.
5.3.2.3.3        Shake it well with 1-2ml of chloroform.
5.3.2.3.4        And add 1-2ml of purified water.
5.3.2.3.5        Observe the colour change.
5.3.2.4  Observations:
5.3.2.4.1        The chloroform layer is colored red.
5.4  Loss on drying:
5.4.1        Material and equipment:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Oven.
5.4.2        Sample:
5.4.2.1  1.0g.
5.4.3        Method:
5.4.3.1  Weigh 1.0g of the test sample.
5.4.3.2  Set the oven apparatus. Operate it according to the SOP.
5.4.3.3  Place the sample into the tray and dry it.
5.4.3.4  Set the temperature of oven at 200±10oC for at least 45 minutes.
5.4.3.5  And wait till the sample loses its moisture.
5.4.3.6  After 45 minutes weigh the sample again by using analytical weighing balance i.e. the final weight. Operate analytical weighing balance according.
5.4.3.7  Note down readings on given Annexure-1
5.4.4        Observation:
5.4.4.1  Maximum 2.0%.
5.5  Assay:
5.5.1        Apparatus:
5.5.1.1  Glassware (1 100.0ml of beaker, 1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.5.1.2  Analytical weighing balance.
5.5.1.3  Water bath.
5.5.1.4  Magnetic stirrer.
5.5.1.5  Titration apparatus.
5.5.2        Material and reagents:
5.5.2.1  0.1M sodium edetate.
5.5.2.2  3.0ml of dilute hydrochloric acid.
5.5.2.3  6.0ml of strong sodium hydroxide.
5.5.2.4  200mg of calconecarboxylic acid triturate (as indicator).
5.5.2.5  Purified water (q.s).
5.5.3        Sample:
5.5.3.1  0.150g
5.5.4        Method of analysis:
5.5.4.1  Take a 100.0ml of beaker and add 0.150g of sample in it.
5.5.4.2  Add mixture of 3.0ml of dilute hydrochloric acid and 20.0ml of purified water in it, dissolve by using glass rod and heat on water-bath until boil for 2min.
5.5.4.3  Allow it to cool and dilute it to 50.0ml with purified water.
5.5.4.4  Take a conical flask of 500.0ml and add above prepared solution.
5.5.4.5  And dilute it to 300.0ml with purified water.
5.5.4.6  Add 6.0ml of strong sodium hydroxide and about 200mg of calconecarboxylic acid triturate (as indicator).
5.5.4.7  Set titration apparatus.
5.5.4.8  Titrate with 0.1M sodium edetate until the colour changes from violet to full blue.
5.5.4.9  The above procedure is for sample titration and similarly performs the blank titration without using sample.
5.5.4.10 Note down the volume used as shown in Annexure-2.
5.5.4.11 Take 3 readings at least and take average for both sample titration and blank titration.
5.5.4.12 Calculate percentage purity.
5.5.4.13          Calculations:
5.5.4.13.1    After taking average volume of both blank titration and sample titration. Calculate the volume used by the examined substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.5.4.13.2    For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                         Weight of sample
5.5.4.13.3    Put values and calculate %age purity.
5.5.5        Factor:
5.5.5.1  1ml of 0.1M sodium edetate is equivalent to 10.01mg of CaCO3.
5.5.6        Limit:
5.5.6.1  98.5% to 100.5% (dried substance).
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Calcium carbonate: 2015, pp. 364-365.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
7.3  The British Pharmacopoeia. Vol V., Official Monograph /Complexometric Titration: 2015, pp. 281-282.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Observations and calculations of assay of calcium carbonate.

Annexure: 1
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:






Remarks: _______________________________________________________________







Annexure: 2
Observations and calculations of assay of calcium carbonate.
Indicator: ___________________
Weight of sample: ____________                                                Factor: _____________
Titrant: _____________________
Sample titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Blank titration
Sr.#
Initial volume (vi)
(ml)
Final volume (vf)
(ml)
vf-vi
(ml)
1.



2.



3.



Average volume: _________________
Calculations:
Volume used by substance = Blank titration - Sample titration.

%age purity = volume used by substance x factor x 100
                                                                     Weight of sample

Result: ____________________________________________________________________


9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Sr.#
Serial number
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
Min
Minutes
ppt
Precipitates
oC
Degree centigrade
mg
Milligram
M
Molar
Vol
Volume
vi
Initial volume
vf
Final volume
QCA
Quality control active ingredient
F
Format
g/L
Gran per liter
R
Reagent


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