DIOCTAHEDRAL SMECTITE SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Dioctahedral Smectite 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  Magnesium assay:
5.1.1        Apparatus:
5.1.1.1  Glassware (1 100.0ml of beaker, 1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette, 1 500.0ml of conical flask).
5.1.1.2  Analytical weighing balance.
5.1.1.3  Water bath.
5.1.1.4  Magnetic stirrer.
5.1.1.5  Titration apparatus.
5.1.2        Material and reagents:
5.1.2.1  Purified water (q.s).
5.1.2.2  Dilute hydrochloric acid.
5.1.2.3  10.0ml of ammonium chloride buffer solution pH=10.
5.1.2.4  50.0mg of mordant black 11 triturate (as indicator).
5.1.2.5  0.1M sodium edetate.
5.1.3        Sample:
5.1.3.1  0.1g.
5.1.4        Method of analysis:
5.1.4.1  Sample titration:
5.1.4.1.1        Take a conical flask and add 0.1g of sample in it.
5.1.4.1.2        Mix it with 20.0ml of purified water and 2.0ml of dilute hydrochloric acid by using magnetic stirrer.
5.1.4.1.3        Dilute this prescribed solution to 300.0ml with purified water.
5.1.4.1.4        Add 10.0ml of ammonium chloride buffer solution pH 10 and about 50.0mg of mordant black 11 triturate (as indicator) mix it thoroughly.
5.1.4.1.5        Heat it to about 40oC on water bath.
5.1.4.1.6        Set titration apparatus.
5.1.4.1.7        Titrate with 0.1M sodium edetate at the same temperature until the colour changes from violet to full blue.
5.1.4.1.8        Note down the volume used as shown in Annexure-1.
5.1.4.1.9        And take average.
5.1.4.2  Blank titration:
5.1.4.2.1        Take a conical flask and add in it with 20.0ml of water and 2.0ml of dilute hydrochloric acid mix it by using magnetic stirrer.
5.1.4.2.2        Dilute it to 300.0ml with purified water.
5.1.4.2.3        Add 10.0ml of ammonium chloride buffer solution pH 10 and about 50.0mg of mordant black 11 triturate (as indicator) mix it thoroughly.
5.1.4.2.4        Heat it to about 40oC on water bath.
5.1.4.2.5        Set titration apparatus.
5.1.4.2.6        Titrate with 0.1M sodium edetate at the same temperature until the colour changes from violet to full blue.
5.1.4.2.7        Note down the volume used as shown in Annexure-1.
5.1.4.2.8        And take average.
5.1.4.3  Calculate percentage purity.
5.1.4.4  Calculations:
5.1.4.4.1        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.
5.1.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                             Weight of sample
5.1.4.4.3        Put values and calculate %age purity.
5.1.5        Factor:
5.1.5.1  1ml of 0.1M sodium edetate is equivalent to 2.431mg of magnesium Mg.
5.1.6        Limit:
5.1.6.1  95.0% to 100.5%.
5.2  Aluminium assay:
5.2.1        Apparatus:
5.2.1.1  Glassware (1 100.0ml of beaker, 1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Water bath.
5.2.1.4  Magnetic stirrer.
5.2.1.5  Titration apparatus.
5.2.2        Material and reagents:
5.2.2.1  10.0ml of hydrochloric acid R1.
5.2.2.2  Purified water (q.s).
5.2.2.3  10.0ml of dilute ammonia R1.
5.2.2.4  Smallest quantity of dilute hydrochloric acid.
5.2.2.5  0.1M sodium edetate.
5.2.2.6  155g/L solution of ammonium acetate R.
5.2.2.7  Dilute acetic acid.
5.2.2.8  50.0ml of ethanol.
5.2.2.9  3.0ml of a freshly prepared 0.25g/L solution of dithizone.
5.2.3        Sample:
5.2.3.1  0.8g
5.2.4        Method of analysis:
5.2.4.1  Take a 100.0ml of beaker and add 0.8g of sample in it.
5.2.4.2  Add 10.0ml of hydrochloric acid R1 in it, dissolve by using glass rod and heat on water-bath.
5.2.4.3  Cool it and dilute it to 50.0ml with purified water.
5.2.4.4  Take 10.0ml of the above solution in another 50.0ml beaker.
5.2.4.5  Add dilute ammonia R1 until a ppt begins to appear.
5.2.4.6  Add the smallest quantity of dilute hydrochloric acid to dissolve the ppt.
5.2.4.7  And finally dilute it to 20.0ml with purified water.
5.2.4.8  Take a conical flask of 500.0ml and add 20.0ml of the above prepared solution.
5.2.4.9  Add 25.0ml of 0.1M sodium edetate and 10.0ml of a mixture of equal volumes of a 155g/L solution of ammonium acetate R and dilute acetic acid.
5.2.4.10          Boil it for 2mins and then cool it.
5.2.4.11          Add 50.0ml of ethanol and 3.0ml of a freshly prepared 0.25g/L solution of dithizone in ethanol.
5.2.4.12          Set titration apparatus.
5.2.4.13          Titrate the excess of 0.1M sodium edetate with 0.1M zinc sulfate until the colour changes from greenish-blue to reddish-violet.
5.2.4.14          The above procedure is for sample titration and similarly performs the blank titration without using sample.
5.2.4.15          Note down the volume used as shown in Annexure-2.
5.2.4.16          And take average.
5.2.4.17          Calculate percentage purity.
5.2.4.18          Calculations:
5.2.4.18.1    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.
5.2.4.18.2    For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                              Weight of sample
5.2.4.18.3    Put values and calculate %age purity.
5.2.5        Factor:
5.2.5.1  1ml of 0.1M sodium edetate is equivalent to 2.698mg of aluminium Al.
5.2.6        Limit:
5.2.6.1  47.0% to 60.0%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  Manufacturer specifications.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Complexometric Titration: 2015, pp. 281-282.
8.0  ANNEXURES:
Annexure 1: Assay observations and calculations (Complexometric titration for magnesium).
Annexure 2: Assay observations and calculations (Complexometric titration for aluminium).

Annexure: 1
Assay observations and calculations (Complexometric titration for magnesium)
Complexometric titration
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: ____________________________________________________________

Annexure: 2
Assay observations and calculations (Complexometric titration for aluminium)
Complexometric titration
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
q.s
Quantity sufficient
g
Grams
ml
Milliliter
e.g.
For example
M
Molar
g/L
Grams per liter
mg
Milligram
oC
Degree centigrade
vi
Initial volume
vf
Final volume
B.P
British pharmacopoeia
Vol
Volume
QCA
Quality control active ingredient
F
Format


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