SODIUM CHLORIDE METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Sodium chloride from the Pharmacopoeial specifications.
2.0 SCOPE:
This
SOP shall be applicable in Q.C laboratory.
3.0 RESPONSIBILITY:
3.1
Q.C Analyst.
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.
5.1.1.2
Crystalline
powder.
5.1.1.3
Colourless
crystals.
5.1.1.4
White or almost
white pearls.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (2 test
tubes, 1 spatula).
5.1.2.1.2
Anhydrous ethanol.
5.1.2.1.3
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 2 test tubes
and add small quantity of sample for testing solubility according to B.P
specifications.
5.1.2.3.2
Add purified water
in test tube 1 and observe.
5.1.2.3.3
Add anhydrous
ethanol in test tube 2 and observe.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1containing with purified water is freely soluble.
5.1.2.4.2
The sample in test
tube 2 containing with anhydrous ethanol is practically insoluble.
5.2 Identification
tests:
5.2.1
Chlorides
test:
5.2.1.1
Material and equipment:
5.2.1.1.1
Glassware (test
tube, spatula, beaker, glass rod).
5.2.1.1.2
Centrifugation
machine.
5.2.1.1.3
Dilute nitric
acid.
5.2.1.1.4
Purified water.
5.2.1.1.5
0.4ml of Silver
nitrate R1.
5.2.1.1.6
Ammonia.
5.2.1.2
Sample:
5.2.1.2.1
Quantity of
substance to be examined equivalent to about 2.0mg of chloride.
5.2.1.3
Method:
5.2.1.3.1
Take a test tube
add in it 2.0ml of water with the help of pipette.
5.2.1.3.2
Dissolve in 2.0ml
of water a quantity of the substance to be equivalent to about 2.0mg of
chloride.
5.2.1.3.3
Acidify with
dilute nitric acid.
5.2.1.3.4
And add 0.4ml of
silver nitrate R1.
5.2.1.3.5
Shake and allow it
to stand.
5.2.1.3.6
A curdled, white
ppt is formed.
5.2.1.3.7
Centrifuge it in
centrifugation machine, according to SOP No. BM/QCEO/SOP010-00.
5.2.1.3.8
The obtained ppt
is wash with 3 quantities, each of 1ml, of water.
5.2.1.3.9
Carry out this operation
rapidly is subdued light, degrading the fact that the supernatant solution may
not become perfectly clear.
5.2.1.3.10 Suspend
the precipitate in 2.0ml of water and add 1.5ml of ammonia
5.2.1.4
Observations:
5.2.1.4.1
The precipitate
dissolves easily with the possible exception of a few large particles which
dissolves slowly.
5.2.2
Chlorides
test:
5.2.2.1
Material and equipment:
5.2.2.1.1
Glassware (test
tube, spatula, glass rod).
5.2.2.1.2
0.2g of potassium
dichromate R.
5.2.2.1.3
1.0ml of sulfuric
acid R.
5.2.2.1.4
Filter paper.
5.2.2.1.5
0.1ml of
diphenylcarbazide solution.
5.2.2.2
Sample:
5.2.2.2.1
Quantity of
substance to be examined equivalent to about 15.0mg of chloride.
5.2.2.3
Method:
5.2.2.3.1
Take a test tube
add in it a quantity of the substance to be equivalent to about 2.0mg of
chloride.
5.2.2.3.2
Add 0.2g of
potassium dichromate R and 1.0ml of sulfuric acid R.
5.2.2.3.3
Place a filter
paper strip impregnated with 0.1ml of diphenylcarbazide solution R over the
opening of the test tube.
5.2.2.3.4
Observe the
changes.
5.2.2.3.5
The impregnated
paper must not come into contact with the potassium dichromate.
5.2.2.4
Observations:
5.2.2.4.1
The paper turns violet-red.
5.2.3
Sodium
test:
5.2.3.1
Material and equipment:
5.2.3.1.1
Glassware (test
tube, spatula, beaker, glass rod).
5.2.3.1.2
2.0ml of 150g/L
solution of potassium carbonate.
5.2.3.1.3
4.0ml of potassium
pyroantimonate solution.
5.2.3.1.4
Iced water.
5.2.3.1.5
Purified water.
5.2.3.2
Sample:
5.2.3.2.1
0.1g.
5.2.3.3
Method:
5.2.3.3.1
Take a test tube
and add 0.1g of the substance to be examined in 2.0ml of purified water.
Dissolve it thoroughly.
5.2.3.3.2
Add 2.0ml of
150g/L solution of potassium carbonate and heat it to boiling on burner.
5.2.3.3.3
Observe the
changes.
5.2.3.3.4
No ppt is formed.
5.2.3.3.5
Add 4.0ml of
potassium pyroantimonate solution again heat it to boiling on burner.
5.2.3.3.6
And then take a
beaker of filled with iced water, put test tube in it and allow it to cool.
5.2.3.3.7
If necessary rub
the inside of the test tube with a glass rod.
5.2.3.3.8
Observe the
changes.
5.2.3.4
Observations:
5.2.3.4.1
A dense white ppt
is formed.
5.2.4
Sodium
test:
5.2.4.1
Material and equipment:
5.2.4.1.1
Glassware (test
tube, spatula, beaker, glass rod).
5.2.4.1.2
1.5ml of
methoxyphenylacetic reagent R.
5.2.4.1.3
Ice-water.
5.2.4.1.4
1.0ml of dilute
ammonia R1.
5.2.4.1.5
1.0ml of ammonium
carbonate solution R.
5.2.4.2
Sample:
5.2.4.2.1
2.0mg.
5.2.4.3
Method:
5.2.4.3.1
Take a test tube
with 0.5ml of purified water and add 2.0mg of sodium (Na+), dissolve
it.
5.2.4.3.2
Add 1.5ml of
methoxyphenylacetic reagent R and cool in ice-water for 30min.
5.2.4.3.3
Observe the
changes.
5.2.4.3.4
A voluminous,
white, crystalline ppt is formed.
5.2.4.3.5
Place it in
water-bath at 20oC and stir for 5 min.
5.2.4.3.6
The ppt does not
disappear.
5.2.4.3.7
Add 1.0ml of
dilute ammonia R1.
5.2.4.3.8
The ppt dissolves
completely.
5.2.4.3.9
Add 1.0ml of
ammonium carbonate solution R.
5.2.4.3.10 Observe
the changes.
5.2.4.4
Observations:
5.2.4.4.1
No ppt is formed.
5.3 Loss
on drying:
5.3.1
Material and equipment:
5.3.1.1
Glassware
(according to requirement).
5.3.1.2
Analytical
weighing balance.
5.3.1.3
Oven.
5.3.2
Sample:
5.3.2.1
1.0g.
5.3.3
Method:
5.3.3.1
Weigh 1.0g of the
test sample.
5.3.3.2
Set the oven
apparatus. Operate it according to the SOP.
5.3.3.3
Place the sample
into the tray and dry it.
5.3.3.4
Set the
temperature of oven at 105oC for at least 2 hours.
5.3.3.5
And wait till the
sample loses its moisture.
5.3.3.6
After 2 hours
weigh the sample again by using analytical weighing balance i.e. the final
weight.
5.3.3.7
Note down readings
on given Annexure-1.
5.3.4
Observation:
5.3.4.1
Maximum 0.5%.
5.4 Assay:
5.4.1
Apparatus:
5.4.1.1
Glassware
(according to requirement).
5.4.1.2
Potentiometer.
5.4.1.3
Magnetic stirrer.
5.4.2
Material
and reagents:
5.4.2.1
0.1M silver
nitrate.
5.4.2.2
Purified water.
5.4.3
Sample:
5.4.3.1
50.0mg.
5.4.4
Method
of analysis:
5.4.4.1 Take
a 50.0ml of beaker and add 50.0mg of sample in it.
5.4.4.2 Dissolve
it in sufficient quantity of purified water by using magnetic stirrer i.e. SOP.
5.4.4.3 Dilute
it to 50.0ml with purified water.
5.4.4.4 Fill
the right hand side burette with titrant 0.1M silver nitrate.
5.4.4.5 Carry
out a Potentiometric titration.
5.4.4.6 Operate
potentiometer according to SOP.
5.4.4.7 To
neutralize analyte add titrant fixed volume (1ml, 0.5ml or 0.1ml) from burette
every time note the reading of change in potential difference (millivolts) for
each addition in given annexure-2.
5.4.4.8 Plot
a graph, volume used v/s millivolts.
5.4.4.9 Find
out the END POINT.
5.4.4.10 Peak
of graph indicates END POINT i.e. the point at which maximum millivolts. Note
down volume used at that point.
5.4.4.11 Perform
blank titration without using sample. Similarly, as sample titration performed.
Record observations in annexure-2.
5.4.4.12 Calculate
volume used by substance by using formula:
Volume used by
substance = Blank titration - Sample titration.
5.4.4.13 Calculate
percentage purity of the sample by using formula:
%age purity = volume
used by substance x factor x 100
Weight
of sample
5.4.5
Factor:
5.4.5.1 1ml
of 0.1M silver nitrate is equivalent to 5.844mg of sodium chloride NaCl.
5.4.6
Limit:
5.4.6.1
99.0% 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 II., Official
Monograph / Potassium chloride: 2015, pp. 621-622.
7.2
The British
Pharmacopoeia. Vol V.,
Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0 ANNEXURES:
Annexure 1: Observations
of Percentage Loss of drying by using oven.
Annexure 2: Assay
observations and calculations (Potentiometric titration).
Annexure: 1
Observations
of percentage loss of drying by using Oven
|
Percentage
loss of drying by using Oven
Weight
of Sample = _____________
Time
period = _____________
Pressure=
_________________
Average % Loss of Moisture: _____________
Remarks: _______________________________________________________________
|
||||||||||||||||||||||||
Annexure:
2
Assay
observations and calculations (Potentiometric titration)
|
Potentiometric titration
Reference
electrode: ___________________
Indicator
electrode: ____________________
Speed
of magnetic stirrer: _______________
Titrant
used: __________________________
Indicator:
____________________________
Blank
titration:
Plot a graph, volume used v/s millivolts and find out peak
of graph i.e. END POINT of blank titration.
Sample
titration:
Plot a graph, volume used v/s millivolts and find out peak
of graph i.e. END POINT of sample titration:
Volume used by Blank titration: __________________
Volume used by Sample titration: _________________
Volume used by substance = Blank titration - Sample
titration.
mV used by Blank titration: __________________
mV used by Sample titration: _________________
mV used by substance = Blank
titration - Sample titration.
Volume
used by substance: _______________________
Voltmeter
(mV) used by substance: _________________
RESULT: ____________________________________________________________
|
9.0 ABBREVIATIONS:
|
Abbreviation
|
Expanded Form
|
|
SOP
|
Standard
operating procedure
|
|
&
|
And
|
|
No.
|
Number
|
|
Ltd.
|
Limited
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|
|
Q.C
|
Quality
control
|
|
Vol
|
Volume
|
|
%
|
Percentage
|
|
g
|
Grams
|
|
ml
|
Milliliter
|
|
M
|
Molar
|
|
g/L
|
Grams
per liter
|
|
mg
|
Milligram
|
|
B.P
|
British
pharmacopoeia
|
|
oC
|
Degree
centigrade
|
|
R
|
Reagent
|
|
v/s
|
Verses
|
|
mV
|
Millivolts
|
|
H
|
Hours
|