GENERAL TESTING PROCEDURES FOR RAW MATERIALS

COMPANY NAME
General Testing Procedure

Title
Supersedes
: DESCRIPTION OF MATERIAL
: Nil
Issue Date
10/04/2010
SOP No : GTP-10001
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 1
Objective:
To lay down a procedure for Description of raw materials & finish products.
Scope:
This procedure is applicable to all incoming Raw materials, In-process and Finished
products of Company Name.
Responsibility:
Q. C. Chemist / Q. C. Manager
Procedure:
Take about 10gm of the substance being examined in a dry Petri dish or disperse on a
white card. Note the Colour, Odour, shape and homogeneity of the sample.
Check for the presence of any foreign particles.
Raw Materials:
5-10 gm samples taken individually by each container & visually examined for:
Capsules:
Twenty arbitrarily selected capsules are visually examined for:
Tablets:
Appearance of capsules
Colour of body & cap
Printing matter on capsules
Appearance of filled medicine
Colour of filled medicine
Twenty arbitrarily selected tablets are visually examined for:
Oral Liquids:
Appearance of powder
Colour of powder
Odour of powder
Appearance of tablets
Colour of tablets
Shape of tablets
Coated/uncoated
Marking/Printing on tablets
Ten arbitrarily selected bottles are visually examined for:
Sealing of bottles.
Leakage in bottles
Labels on bottles
Appearance of Syrup / Suspension
Colour of Syrup / Suspension
Developed By :
Reviewed By :
Title
: SOLUBILITY
TESTING
Name:
Name:
SupersedesQA Officer
: Nil
Designation:
Issue Date
Designation:
Signature:
Signature:
SOP No : GTP-10002
Effective date
Quality10/04/2010
Head
10/04/2010
Authorized By :
Name:
Review date
Designation:
Signature:
Page number
AprilDirector
2012
Managing
1 of 1
COMPANY NAME
Objective:
To lay down a procedure for solubility tests for raw materials.
Scope:
Determination of Solubility in raw materials to ensure the supplied material passes

the prescribed tests.
Responsibility:
Procedure:
Solubility of raw materials are to be determine at a temperature between 15C and

25C with following manners:
Weigh the substance being examined as per the table given below and transfer
into a clean and dry test tube.
Take about 1 g of sample in test tube / volumetric flask (as applicable). Select the
solvent as per specification. Based on the solubility of the sample, add the required
volume of the particular solvent(s) as per table given below. Shake well to dissolve
ensuring that the test is carried out at a temperature between 20C to 30C.
Add prescribed volume of the solvent, shake well, sonicate if necessary. Observe
the solubility.
A smaller dilutions may be taken for costly products.
Check the solubility of the sample against the specification.
Title
Supersedes
Test
Quantity taken for test
Very soluble -
1 gm in less than 1ml
Freely soluble -
1 gm in 1-10ml
Soluble -
1 gm in 10ml-30ml
Sparingly soluble -
0.1gm in 3ml-10ml
Slightly soluble -
0.1gm in 10ml-100ml
Very Slightly soluble -
0.1gm in 100ml-1000ml
Practically insoluble -
0.1gm in more than 1000ml
: CLARITY OF SOLUTION
: Nil
Issue Date
SOP No : GTP-10003
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Developed By To
: lay down a procedure
Reviewed
By :of solution.
Authorized By :
Objective:
for clarity
Name:
Name:
Name:
Scope:
of clarity of
solution
in the raw materials
to ensureManaging
the supplied
Designation:
QA OfficerDetermination
Designation:
Quality
Head
Designation:
Director
Signature:
material passes
the prescribed tests.
Signature:
Signature:
COMPANY NAME
Responsibility:
Procedure:
Into separate matched, flat-bottomed test tubes, 15 to 25 mm in internal diameter

and of colorless, transparent, neutral glass, place sufficient of the solution being
prepared (e.g.1gm in 20ml water) and of the appropriate reference suspension,
freshly prepared as pharmacopoeia, such that the test tubes are filled to a depth of
40 mm. Five minutes after preparation of the reference suspension, compare the
clarity in diffused daylight, viewing horizontally against a white background with water
or reference suspension I.
A liquid is considered clear if its clarity is the same as that of water or of the solvent
used when examined under the conditions described above or if its opalescence is
not more pronounced than that of reference suspension I.
Title
Supersedes
: COLOUR OF SOLUTION
: Nil
Issue Date
SOP No : GTP-10004
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 3
Objective:
To lay down a procedure for color of solution.
Scope:
Determination of color of solution in the raw materials to ensure the supplied

material passes the prescribed tests.
Developed By Q.
: C. Chemist / Q.Reviewed
By :
Responsibility:
C. Manager
Name:
Name:
Authorized By :
Name:
Designation:
Designation:
Quality Head
Managing
Director
Procedure: QA OfficerUsing identical
tubes of colorless,
transparent, Designation:
neutral glass 12 mm
in external
Signature:
Signature:
Signature:
COMPANY NAME
Diameter compares 2.0 ml of the liquid being examined with 2.0 ml of water or of the
solvent or of the reference solution prescribed in the pharmacopoeia. Compare the
color in diffused daylight, viewing horizontally against a white background.
The examination of the color of solution in the range brown-yellow-red is carried out
by above method. A solution is considered colorless if it has the appearance of water
or the solvent or is not more intensely coloured than reference solution B9.
Apparatus :
Test tube
100 Volumetric flask
25 ml measuring cylinder
10 ml graduated pipette
Flat bottomed color matching test-tubes
Reagents :
Ferric chloride hexahydrate AR grade

Cobaltous chloride AR grade
Cupric sulphate AR grade
Concentrated hydrochloric acid AR grade
Potassium iodide AR grade
Starch solution
0.1M sodium thiosulphate
Hydrogen peroxide solution (10 volumes)
Sodium hydroxide solution
Dilute sulphuric acid
Acetic acid AR grade
Title
Supersedes
: Nil
Issue Date
SOP No : GTP-10004
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
2 of 3
Method :
A. Ferric chloride colorimetric solution (FCS) :
Dissolve about 5.5 g of ferric chloride hexahydrate in enough of a mixture of 25 ml of
hydrochloric acid and 97.5 ml of purified water to produce 100 ml. The solutions should be
stored protected from light.
Developed By :
Reviewed By :
Authorized By :
colorimetric solution (CCS) : Name:
Name:B. Cobaltous ChlorideName:
Dissolve
about 6.5 g ofDesignation:
cobaltous chloride
in enough of Designation:
a mixture of 2.5Managing
ml of hydrochloric
Designation:
QA Officer
Quality Head
Director
acid
and
97.5
ml
of
purified
water
to
produce
100
ml.
Signature:
Signature:
Signature:
COMPANY NAME
C. Cupric Sulphate Colorimetric Solution (CSS) :
Dissolve about 6.5 g of cupric sulphate in enough of a mixture of 2.5 ml of hydrochloric acid
and 97.5 ml of water to produce 100 ml.
Reference Solution :
Prepare by mixing the volumes of colorimetric solutions and hydrochloric acid (1% w/v) as
indicated in Table 1.
Note - Reference solutions must be prepared immediately before use from the colorimetric
solutions which may be stored.
Procedure :
Transfer to a flat-bottomed test-tube of neutral glass, 15 to 25 mm in diameter, a suitable
volume of the solution being examined such that the test-tubes is filled to a depth of 40 mm.
Into another matched test tube add the same volume of water or of the solvent used for
preparing the solution being examined or of the reference solution stated in the STP.
Examined the column of liquid in diffused light by viewing down the vertical axis of the tubes
against a white background.
Colourless Solution :
A solution is considered colorless if it has the same appearance as water or the solvent
used for preparing the solution or is not more intensely colored than reference solution BS8.
Title
Supersedes
: Nil
Issue Date
SOP No : GTP-10004
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
3 of 3
Table - 1
Colour of
reference
Solution
Yellow
Developed By :
Name: Greenish
yellow
Designation:
QA Officer
Signature:
Reference
solution
FCS
(ml)
CCS
(ml)
YS1
24.0
6.0
YS2
18.0
4.5
YS3
12.0
3.0
YS4
6.0
1.5
YS5
3.2
0.8
YS6
1.6
0.4
YS7
0.8 By : 0.2
Reviewed
GYS1
24.0
0.5
Name:
GYS2
14.5
Designation: Quality Head0.1
GYS3
8.5
0.05
Signature:
GYS4
5.0
0.05
CSS
(ml)
Hydrochloric
acid
(1% w/v HCI)
(ml)
0
70.0
0
77.5
0
85.0
0
92.5
0
96.0
0
98.0
0
99.0
Authorized
By :
0.5
75.0
Name:
0.1
85.5Managing Director
Designation:
0.05
Signature: 91.5
0.05
95.0
COMPANY NAME
GYS5
GYS6
GYS7
BYS1
BYS2
BYS3
BYS4
BYS5
BYS6
BYS7
BS1
BS2
BS3
BS4
BS5
BS6
BS7
BS8
RS1
RS2
RS3
RS4
RS5
RS6
RS7
Brownish
yellow
Brown
Red
5.8
2.9
2.9
24.0
18.0
12.0
6.0
3.0
1.5
1.0
22.5
15.0
11.2
7.5
3.7
1.5
0.8
0.4
10.0
7.5
5.0
3.8
2.5
1.3
0.5
0.05
0.05
0.05
10.0
7.5
5.0
2.5
1.5
0.8
0.4
22.5
15.0
11.2
7.5
3.7
1.5
0.8
0.4
20.0
15.0
10.0
7.6
5.0
2.6
1.0
0.05
0.05
0.05
4.0
3.0
2.0
1.0
0.5
0.2
0.1
18.0
12.0
9.0
6.0
3.0
1.2
0.6
0.2
0
0
0
0
0
0
0
194.0
197.0
397.0
62.0
71.5
81.0
90.5
95.0
97.5
98.5
37.0
58.0
68.5
79.0
89.5
96.0
98.0
99.0
70.0
77.5
85.0
88.5
92.5
96.0
98.5
Reference : IP-1996 (Appendix 6 , page A -78)
Title
Supersedes
: DETERMINATION OF MELTING POINT

: Nil
Issue Date
10/04/2010
SOP No : GTP-10005
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 1
Objective:
To lay down a procedure for determination of meting point.
Scope:
Determination of melting point of the raw materials to ensure the supplied material
passes the prescribed test.
Responsibility:
Procedure:
Dry a small quantity of the finely powdered substance at a pressure of 1.5 to 2.5 kPa over
anhydrous silica gel for 24 hours. Transfer a sufficient portion to a dry capillary tube (closed at one
end) to form a compact column 4 to 6 mm in height. Raise the temperature of the bath to about 10
below the presumed melting point and then adjust the rate of heating to about 1 per minute. When
Developed
By : is 5 below the
Reviewed
:
Authorized
the temperature
presumedBymelting
point, adjust the
height ofBy
the: calibrated
Name:
Name:
Name:
thermometer
so that the
immersion mark
is Head
level with theDesignation:
surface of the Managing
liquid andDirector
insert the
Designation:
QA Officer
Designation:
Quality
Signature:
Signature:
Signature:
COMPANY NAME
capillary tube so that its lower end is near the middle of the thermometer bulb. The temperature at
which the last solid particle passes into the liquid phase is the melting point of the substance.
Title
Supersedes
: DETERMINATION OF LOSS ON DRYING

: Nil
Issue Date
10/04/2010
SOP No : GTP-10006
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
Objective:
To lay down a procedure of loss on drying for raw materials & finish products.
Scope:
Loss on drying determines the loss of weight when material dried at prescribed temp.
Responsibility:
Procedure:
Weigh a glass stoppered, shallow weighing bottle that has been dried under the same conditions to
be employed in the determination. Transfer to the bottle the quantity of the sample about 1.0 g of
pallets, cover it and accurately weigh the bottle and the contents. Distribute the sample as evenly
as practicable by gentle sidewise shaking to a depth not exceeding 10mm. Place the loaded bottle
in the drying chamber (oven or desiccator) as directed in the monograph, remove the stopper and
leave it also in the chamber.
Dry the substance
weight or for the
prescribedBy
time
Developed
By : at prescribed temperature
Reviewed to
Byconstant
:
Authorized
: or at
Name: prescribed conditions. After
Name:
Name:
drying is completed, open the drying
chamber, close the bottle promptly
Designation: QA Officer
Designation:
Quality Head
Designation:
Managing Director
and allow it to cool to room

temperature (where applicable) in Signature:
a desiccator before weighing. Weigh
Signature:
Signature:
the bottle and the contents.
COMPANY NAME
Calculations:
Loss on drying (% w/w):
W1
W2
W3
=
=
=
Title
Supersedes
W2
W3
W2
100
W1
Weight of empty bottle

Weight of bottle + sample
Weight of the bottle + sample after drying
: DETERMINATION OF LOSS ON DRYING

: Nil
Issue Date
10/04/2010
SOP No : GTP-10006
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
Conditions of Loss on drying;

(a)
In a desiccators
: The drying is carried out over phosphorus pentaoxide at atmospheric

pressure and at room temperature.
(b)
In vacuum
: The drying is carried out over phosphorus pentoxide at a pressure of 1.5

to 2.5 kPa at room temperature.
(c)
In vacuum
: within a specified temperature range: The drying is carried out over

phosphorus pentoxide at a pressure of 1.5 to 2.5 kPa within the
temperature range specified in the monograph.
(d)
In an oven
: within a specified temperature range: The drying is carried out in an oven

within the temperature range specified in the monograph.
(e)
Under high vacuum: The drying is carried out over phosphorus pentoxide at a pressure not
exceeding 0.1 kPa at the temperature prescribed in the monograph.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: DETERMINATION OF BOILING POINT

: Nil
Issue Date
10/04/2010
SOP No : GTP-10007
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 1
Objective:
To lay down a procedure of determination of boiling point.
Scope:
Boiling Point of a liquid is the corrected temperature at which the vapour pressure
of the liquid reaches 101.3 kPa.
Responsibility:
Procedure:
Method Place in the flask 20 ml of the liquid being examined in the boiling point
apparatus, add a few pieces of porous material and heat rapidly to boiling. Record
the temperature at which liquid begins to run from the side arm into the condenser.
Correct the temperature reading for the effect of barometric pressure using the following expression:
t1 = t2 + K(101.3-b)
where t 1
the corrected temperature,
t2
the measured temperature,
the barometric pressure in kPa at the time of the

determination,
the correction factor, as given below:
K
Boiling point
K
Less than
Developed By :
Name:
More than
100
0.30
100-140
0.34
140-190
0.38
190-240
0.41
240
0.45
Reviewed By :
Name:
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: DETERMINATION OF REFRACTIVE INDEX

: Nil
Issue Date
10/04/2010
SOP No : GTP-10008
2.
3.
4.
5.
6.
7.
8.
9.
10.
10/04/2010
April 2012
Page number
1 of 1
Objective:
To lay down a procedure of determination of refractive index.
Scope:
Determination of Refractive index of a liquid to ensure the supplied material

Responsibility:
Procedure:
1.
Effective date
Review date
The refractive index (n) of a substance with reference to air is the ratio of the sine of the
angle of incidence to the sine of the angle of refraction of a beam of light passing from air
into the substance. Refractive indices, n D 20 are stated in terms of the wave-length of the
sodium D-line (589.3 nm) at a temperature of 19.5 to 20.5
Open the prism by unlocking the lever, place of few drops of the liquid under study on the
surface of the lower prism, which has a matt and ground surface.
Lift the lower prism and lock it with the upper prism by the same lever when the liquid will be
formed into a very thin layer between the two prisms.
Look through the telescope when a bright circular path of the light partly coloured will be seen.
Focus the eyepiece on the index line and adjust the reflecting mirror to get a maximum
illumination through the telescope.
Rotate the milled drum in front till a coloured band of light appears.
Rotate the milled drum till this sharp critical line of demarcation coincides with the junction of
the crossed index lines.
Look though the left eye piece and focus the lens till the refractive index scale and the index
line are in clear focus, take the reading of the scale, this gives the refractive index of the
sample,
Repeat the process to take a number of readings whose average gives the refractive index of
the liquid.
It the refractive index is to be determining at a fixed desired temperature, water from a
separate thermostatic bath is circulated within the prism box using the inlet and outlet tubes
and check the temp. with thermometer.
Before putting in any new liquid, the surface of the prism must be thoroughly cleaned with
water or other organic solvent like acetone to remove the solution previously used.
Developed By :
Name:
Name:
Reviewed By :
Supersedes
Signature:
Issue Date
Signature:
Authorized By :
Name:
Title
: DETERMINATION
OF Optical
Rotation
Optical Rotation
Designation:
QA Officer
Designation:
Quality
Head and Specific
Designation:
Managing Director
: Nil
10/04/2010
Review date
Signature:
April 2012
COMPANY NAME
SOP No : GTP-10009
Effective date
10/04/2010
Page number
1 of 2
Objective:
To lay down a procedure of determination of optical rotation & specific optical rotation.
Scope:
Determination of optical rotation & specific optical rotation to ensure the supplied material
Responsibility:
Procedure:
The optical rotation, a, unless otherwise specified, is measured at the wavelength of the sodium D-line
(589.3 nm) at a temperature of 20 in a layer 1 dm thick.
Dextrorotation is designated (+) and laevorotation is designated (-).
The specific optical rotation of a liquid is determined by measuring the angle of rotation at the wavelength
of the sodium D-line at a temperature of 20, unless otherwise specified, calculating the optical rotation with
reference to a layer 1 dm thick and dividing by the relative density at 20.
The specific optical rotation of a solid substance is determined, using the solution specified in the
monograph, by measuring the angle of rotation at the wavelength of the sodium D-line at a temperature of
20, unless otherwise specified, and calculating the result with reference to a layer 1 dm thick of a solution
containing 1 g of the substance per ml. The specific optical rotation of a solid is always expressed with
reference to a given solvent and concentration.
Title
Supersedes
: DETERMINATION OF Optical Rotation and Specific Optical Rotation

: Nil
Issue Date
10/04/2010
Review date
April 2012
10/04/2010
By :
By :
Authorized By
SOPDeveloped
No : GTP-10009
EffectiveReviewed
date
Page number
2 of:2
Name:
Name:
Designation:
QA Officer
Method:
Designation:
Signature:
Signature:
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
a.
Connect power plug to proper power supply through voltage stabilizer.
b.
Switch on main power supply & on the instrument by main ON / OFF Button, allow 15 minutes
for the Sodium lamp glow up.
c.
Weigh accurately a suitable quantity of the substance in to a volumetric flask. & Prepare the
solution in water, or other solvent, if specified in the monograph, reserving a portion of the
solvent for the blank determination.
d.
Transfer the prepared solution/or liquid sample to the Polarimeter tube of required length
(1dcm or 2dcm) within 30 minutes from the time of solution prepared & maintain the solution /
liquid sample at a temperature of 20oC.
e.
Polarimeter tube should be filled in such a way as to avoid air bubbles interfere with the
passage source of light.
f.
Determine the Zero point of the Polarimeter and then take at least five readings at 25oC with
the test solution. Take an equal number of readings in the same tube with the blank solution.
The blank reading is subtracted from the average observed reading of test solution.
g.
Calculate the specific optical rotation of a liquid substance, or of a solid in solution on dried
basis.
h.
Lens of Polarimeter tube should be thorkughly cleaned before taking the reading.
i.
Polarimeter tube should be clean properly with distilled water.
Lastly off the switch of voltage stabilizer and main power supply.
Calculate the specific optical rotation using the expression =

Test Reading + blank reading x Volume of solution
Wt of substance in gm x Length of tube in decimeter
Calculate the optical rotation of liquids using the expression =
Test Reading + blank reading
Length of tube in decimeter
Title
Supersedes
: DETERMINATION OF WATER
: Nil
Issue Date
SOP No : GTP-10010
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 2
Objective
To lay down a procedure of determination of water.
Scope
Determination of water content in the pharmaceuticals to ensure the water content

present in prescribed limits.
Responsibility:
C. Manager
Developed By Q.
: C. Chemist / Q.Reviewed
By :
Name:
Procedure: QA Officer
Designation:
Signature:
Name:
Designation:
Signature:
Connect power plug to proper power supply.
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Turn the power switch ON and allow 5 minutes for the instrument to warm up.
Fill enough quantity of KARL FISCHER Reagent in the reservoir by lifting the adapter.
Remove the glass plug and add some methanol to the moisture beaker to such an extent that the platinum
wires of electrode in the beaker and fully immersed. Replace the flask plug.
Switch the titrator ON. Red LED of the MAINS will glow.
Adjust the suitable speed of the magnetic stirrer.
Fill automatic burette with K.F. Reagent up to zero mark.
Press the START button and release START. LED will glow.
As end point is reached, press STOP button to stop buzzer.
Quickly add a weighed amount of Sodium Tartrate Di hydrate (approx. 200 mg) or Water (approx. 20mg) in
to beaker & continue titration up to end point as done above.
Read volume of K.F. Reagent & calculate FACTOR for Karl Fischer Reagent.
Take weighted amount of sample in to beaker, Start titration with K.F. Reagent up to end point as done
above, read the volume & calculate moisture in the sample.
Clean reaction beaker, electrodes, and burette with acetone & dry the beaker for the next day.
Water should not be used for cleaning the burette or any other part.
Title
Supersedes
: DETERMINATION OF WATER
: Nil
Issue Date
SOP No : GTP-10010
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
2 of 2
Calculate the Water Content by the following equation :

Wt of water taken in mg
Factor
=
Volume of KF used for water neutralization in ml
( Factor between 3 and 5 )
Developed By :
Name:
% of water =
Name:
Signature:
Signature:
By : for substance neutralization

Authorized
By :
Factor xReviewed
Vol. of KF used
in ml x100
Name:
Designation:
Quality taken
Head for titration.
Designation:
Wt of substance
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: DETERMINATION OF SULPHATED ASH

: Nil
Issue Date
10/04/2010
SOP No : GTP-10011
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
Objective
To lay down a procedure of determination of Sulphated ash.
SCOPE
The procedure is applicable to all Active and Inactive raw materials
APPARATUS
Muffle furnace
Balance
Silica or Platinum or porcelain or quartz crucibles.
Graduated pipette-1 ml
Hot plate
Dessicator.
Nickel tongs
REAGENTS
Developed By :
Name:
Sulphuric acid
Reviewed By :
Name:
: AR grade
Signature:
PROCEDURE
Signature:
Use
Method I unless otherwise directed.Signature:
Designation:
Quality Head
Authorized By :
Name:
Designation:
Managing Director
COMPANY NAME
Method I (No. Ph. Eur. method)
Heat a platinum dish to redness for 10 minutes; allow cooling in a desiccator and weighing. Unless
otherwise specified in the monograph, place 1 g of the substance being examined in the dish, moisten with
sulphuric acid, ignite gently, again moisten with sulphuric acid and ignite at about 800C. Cool, weigh
again, ignite for 15 minutes and repeat this procedure until two successive weighing do not differ by more
than 0.5 mg.
Calculation:
W3 (or) Wn - W1
--------------------------W2 - W1
% w/w of Sulphated ash =

Where,
W1
=
W2
=
W3
=
Wn
=
Title
Supersedes
x 100
Weight of the empty crucible in grams.

Weight of the crucible with sample in grams
Weight of the crucible with ash in grams
Weight of the crucible with as in grams, ignition for 15 minutes (constant weight)
: DETERMINATION OF SULPHATED ASH

: Nil
Issue Date
10/04/2010
SOP No : GTP-10011
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
Method II (2.4.14) (Ph. Eur. method)

Ignite a platinum, porcelain or quartz crucible at 600C50C for 30 minutes, allow to cool in a desiccator
over silica gel and weigh. Place the prescribed amount of the substance being examined in the crucible
and weigh. Moisten the substance to be examined with a small amount of sulphuric acid (usually 1 ml) and
heat gently at as low a temperature as practicable until the sample is thoroughly charred.
After cooling, moisten the residue with a small amount of sulphuric acid, heat gently until white fumes are
no longer evolved and ignite at 600C 50C until the residue is completely incinerated. Ensure that
flames are not produced at any time during the procedure. Allow the crucible to cool in a desiccator over
silica gel, weigh it again and calculate the weight of the residue. If the weight of the residue so obtained
exceeds the prescribed limit, continue the ignition, as previously, to constant mass, unless otherwise
prescribed.
Calculation:
M3 (or) n - M1
------------------------ x 100
M2 - M1
% m/m of Sulphated ash =

Where,
M1
M2
M3
Mn
= Weight of the empty crucible in grams.

= Weight of the crucible with sample in grams
=Weight of the crucible with ash in grams
=Weight of the crucible with as in grams , ignition for 15 minutes (constant weight)
Developed By :
NOTE:
Name:
Name:
Reviewed By :
Designation:
Authorized By :
Name:
Quality Head
Designation:
Managing Director
The above document has been Signature:

prepared on the basis of appendix IXSignature:
A, Ph. Eur method/ method 2.4.14 of
Signature:
BP/ Ph. Eur.
COMPANY NAME
Calculate the % of Sulphate Ash by the following formula:
Wt of crucible after Ignition Wt of empty crucible x 100
% =
Wt of substance taken in crucible
Title
Supersedes
: DETERMINATION OF LOSS ON IGNITION

: Nil
Issue Date
10/04/2010
SOP No : GTP-10012
Objective
SCOPE:
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
To lay down a procedure of determination of Loss on Ignition.

This procedure is applicable to all active and inactive raw materials.
APPARATUS
Muffle furnace
Desiccator
Nickel tongs
Mortar and pestle
Crucibles
Balance
REAGENTS
Nil
PROCEDURE
Perform the test on finely powdered material, and break up lumps, if necessary, with the aid of a mortar
and pestle before weighing the specimen.
Weigh the specimen to be tested in g without further treatment, unless a preliminary drying at a lower
temperature, or other special pretreatment, is specified in the individual monograph. Unless other
equipment is designated in the individual monograph, conduct the ignition in a suitable muffle furnace or
oven that is capable of maintaining a temperature within 25C of that required for the test, and use a
suitable crucible, complete with cover, previously ignited for 1 hour at the temperature specified for the test,
Developed By :
Reviewed By :
cooled in a desiccator, and accurately weighed.
Name:
Name:
Name:
Designation:
Designation:
Signature:
Signature:
Quality Head
Authorized By :
Signature:
Managing Director
COMPANY NAME
Unless otherwise directed in the individual monograph, transfer to the tared crucible an accurately weighed
quantity, in g, of the substance to be tested, about equal to that calculated by the formula:
10 / L
in which L is the limit (or mean value of the limits) for Loss on ignition, in percentage.
Ignite the loaded uncovered crucible, and cover at the temperature ( 25C) and for the period of time
designated in the individual monograph. Ignite for successive 1-hour periods where ignition to constant
weight is indicated. Upon completion of each ignition, cover the crucible, and allow it to cool in a desiccator
to room temperature before weighing.
Title
Supersedes
: DETERMINATION OF LOSS ON IGNITION

: Nil
Issue Date
10/04/2010
SOP No : GTP-10012
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
Calculation:
W2 - W3 (or ) n
---------------------------- x 100
W2 - W1
% w/w of Loss on Ignition =

Where,
W1= Weight of the empty crucible in grams.
W2= Weight of the crucible with sample in grams ,before ignition

W3= Weight of the crucible with sample in grams ,after ignition (as time specified)
Wn= Weight of the crucible with sample in grams , after additional 1 hour (constant weight)
NOTE:
The term Constant weight means that two consecutive weightings do not differ by more than 0.5 milligram,
the second weighing being made after an additional period of ignition under the specified conditions.
(1 hour is usually suitable).
The above document has been prepared on the basis of <733> of USP.
END OF THE DOCUMENT

Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: LIMIT TEST OF CHLORIDES

: Nil
Issue Date
SOP No : GTP-10013
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Objective
To lay down a procedure of determination of chlorides in the raw materials.
Scope
Determination of chlorides in the pharmaceuticals to ensure the chlorides present

within prescribed limits.
Responsibility:
Procedure:
Test Solution: To a solution of the specified quantity of the substance being dissolved in 15 ml of water or to
15 ml of the prescribed solution add 1 ml of 2M nitric acid, pour the mixture as a single addition into 1 ml of
silver nitrate solution (1.7%) and allow to stand for 5 minutes protected from light. Standard solution:
Chloride Standard Solution (5 ppm Cl)- Dilute 1 volume of a 0.0824% w/v solution of sodium chloride to
100 volumes with water.
To a 10 ml of chloride standard solution (5 ppm Cl) and 5 ml of water solution add 1 ml of 2M nitric acid,
pour the mixture as a single addition into 1 ml of silver nitrate solution (1.7%) and allow to stand for 5
minutes protected from light.
Observation:
When test solution viewed transversely against a black background any opalescence produced is not more
intense than standard solution. Sample passes the limit test for chlorides.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: LIMIT TEST OF SULPHATES

: Nil
Issue Date
SOP No : GTP-10014
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Objective:
To lay down a procedure of determination of sulphate in the raw materials.
Scope:
Determination of sulphate in the pharmaceuticals to ensure the sulphate present

within prescribed limits.
Responsibility:
Procedure:
Test Solution:
Add 1 ml of a 25% w/v solution of barium chloride to 1.5 ml of sulphate standard

Solution (10 ppm SO4) R1, shake and allow to stand for 1 minute. Add 15 ml of the
prescribed solution or a solution of the specified quantity of the substance being
dissolved in 15 ml of water and 0.5 ml of 5M acetic acid and. allow standing for 5
minutes.
Standard solution: Sulphate Standard Solution (10 ppm SO4) Dilute 1 volume of a 0.181% w/v
Solution of potassium sulphate in distilled water to 100 volumes with the same
solvent.
Add 1 ml of a 25% w/v solution of barium chloride to 1.5 ml of sulphate standard
solution (10 ppm SO4) R1, shake and allow standing for 1 minute. To a 15 ml of
Sulphate Standard Solution (10 ppm SO4) and 0.5 ml of 5M acetic acid and. allow to
stand for 5 minutes.
Observation:
Any opalescence produced by test solution is not more intense than that of a standard solution- Sample
passes the limit test for sulphate.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: LIMIT TEST OF IRON

: Nil
Issue Date
SOP No : GTP-10015
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Objective:
To lay down a procedure of determination of iron in the raw materials.
Scope:
Determination of iron in the pharmaceuticals to ensure the iron present within

prescribed limits.
Responsibility:
APPARATUS
Nessler cylinder
20% w/v solution of Citric Acid.
Mercapto acetic Acid
10 M Ammonia
Standard Iron Solution
Water.
REAGENTS
Procedure:
Test Solution:
Dissolve the specified quantity of the substance being examined in sufficient water
to produce 10 ml or use 10 ml of the solution prescribed in the monograph and
transfer to a Nessler cylinder. Add 2 ml of a 20% w/v solution of citric acid and 0.1 ml
of mercaptoacetic acid, mix, make alkaline with 10M ammonia, dilute to 20 ml with
water and allow to stand for 5 minutes.
Standard solution: Iron Standard Solution (1 ppm Fe) Dilute 1 volume of iron standard solution (20
ppm Fe) to 20 volumes with water.
To 10ml of iron standard solution (1 ppm Fe) in a Nessler cylinder Add 2 ml of a 20%
w/v solution of citric acid and 0.1 ml of mercapto acetic acid, mix, make alkaline with
10M ammonia, dilute to 20 ml with water and allow to stand for 5 minutes.
Observation:
Any pink colour produced in test solution is not more intense than that of a standard solution- Sample
passes the limit test for Iron.
Developed By :
Name:
Name:
Designation:
Signature:
Title
Reviewed By :
Authorized By :
Name:
Quality Head
: LIMIT TEST Signature:

OF HEAVY METALS
Designation:
Signature:
Managing Director
COMPANY NAME
Supersedes
: Nil
SOP No : GTP-10016
Issue Date
10/04/2010
Review date
April 2012
Effective date
10/04/2010
Page number
1 of 4
Objective
The limit for heavy metals is indicated in the individual monographs in terms of
ppm, i.e., the parts of lead, Pb, per million parts (by weight) of the substance being
examined.
SCOPE
The procedure is applicable to all Active and inactive raw materials.
Responsibility
APPARATUS
REAGENTS
Volumetric Flasks (Class A)

Pipettes (Class A)
Nessler cylinders or 50 ml colour comparison tubes.
Short-range pH indicator paper
Kjeldahl flasks
Muffle furnace
Nickel tongs
White tiles
Silica crucibles
Glass rods
Membrane filter holder
Membrane filters
Prefilter
Ammonium acetate
: AR grade
Hydrochloric acid
: AR grade
Ammonia
: AR grade
Acetic acid
: AR grade
Thioacetamide
: AR grade
Glycerin
: AR grade
Lead nitrate
: AR grade
Sodium sulphide
: AR grade
Sulfuric acid
: AR grade
Sodium hydroxide
: RA grade
Nitric acid
: AR grade
Hydrogen Peroxide
: AR grade
Hydrochloric acid
: AR grade
Ferrous sulphide
: AR grade
Acetone
: AR grade
Magnesium sulfate
: AR grade
Phenolphthalein
: AR grade
Magnesium oxide
: AR grade.
Strong hydrogen peroxide solution (100 vol)
Concentrated ammonia R1 (about 18M)
Developed By :
Reviewed By :
Title
: DETERMINATION
Name:
Name:OF HEAVY METALS
: Nil
Designation:
Issue Date
Designation:
Signature:
Signature:
SOP No : GTP-10016
Effective date
Quality10/04/2010
Head
10/04/2010
Authorized By :
Name:
Review date
Designation:
Signature:
Page number
AprilDirector
2012
Managing
2 of 4
COMPANY NAME
Procedure:
Preparation Of H2S gas :
Na2S
Dilute H2SO4
Na2SO4 +
Sodium Sulphide Mol Wt. 78.05
H2S
Sodium Sulphate
Hydrogen Sulphite
Method A
Standard solution: Into a 50-ml Nessler cylinder pipette 1.0 ml of lead standard 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 about 35 ml and mix.
Test solution: Into a 50-ml Nessler cylinder place 25 ml of the solution prepared for the test as directed in
the individual monograph or dissolve the specified quantity of the substance being examined in sufficient
water to produce 25 ml. Adjust with dilute acetic acid or dilute ammonia solution to a pH between 3.0 and
4.0, dilute with water to about 35 ml and mix.
Procedure: To each of the cylinders containing the standard solution and test solution respectively add 10
ml of freshly prepared hydrogen sulphide solution, mix, dilute to 50 ml with water, allow to stand for 5
minutes and view downwards over a white surface; the colour produced with the test solution is not more
intense than that produced with the standard solution.
Title
Supersedes
: DETERMINATION OF HEAVY METALS

: Nil
Issue Date
10/04/2010
SOP No : GTP-10016
Developed
By :
Method
B
Name:
Effective date
10/04/2010
Review date
April 2012
Page number
3 of 4
Reviewed By :
Name:
Authorized By :
Name:
Designation:
QA Officer
Head
Standard solution:
Proceed asDesignation:
directed underQuality
Method
A.
Designation:
Signature:
Signature:
Signature:
Managing Director
COMPANY NAME
Test solution: Weigh in a suitable crucible the quantity of the substance specified in the individual
monograph, add sufficient sulphuric acid to wet the sample, ignite carefully at a low temperature until
thoroughly charred. Add to the charred mass 2 ml of nitric acid and 5 drops of sulphuric acid and heat
cautiously until white fumes are no longer evolved. Ignite, preferably in a muffle furnace, at 500 to 600 ,
until the carbon is completely burnt off. Cool, add 4 ml of hydrochloric acid, cover, digest on a water-bath
for 15 minutes, uncover and slowly evaporate to dryness on a water-bath. Moisten the residue with 1 drop
of hydrochloric acid, add 10 ml of hot water and digest for 2 minutes.
Add ammonia solution drop wise until the solution is just alkaline to litmus paper, dilute to 25 ml with water
and adjust with dilute acetic acid to a pH between 3.0 and 4.0. Filter, if necessary, rinse the crucible and
the filter with 10 ml of water, combine the filtrate and washings in a 50-ml Nessler cylinder, dilute with water
to about 35 ml and mix.
Procedure: Proceed as directed under Method A.
Title
Supersedes
: DETERMINATION OF HEAVY METALS

: Nil
Issue Date
10/04/2010
SOP No : GTP-10016
Effective date
10/04/2010
Review date
April 2012
Page number
4 of 4
Method C
Standard solution: Into a 50-ml Nessler cylinder pipette 1.0 ml of lead standard solution (20 ppm Pb), add
5 ml of dilute sodium hydroxide solution, dilute with water to 50 ml and mix.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Test solution: Into a 50-ml Nessler cylinder place 25 ml of the solution prepared for the test as directed in
the individual monograph, or dissolve the specified quantity of the substance being examined in a mixture
of 20 ml of water and 5 ml of dilute sodium hydroxide solution. Dilute with water to 50 ml and mix.
Procedure:
To each of the cylinders containing the standard solution and the test solution respectively add 5 drops of
sodium sulphide solution, mix, allow standing for 5 minutes and viewing downwards over a white surface;
the colour produced with the test solution is not more intense than that produced with the standard solution.
Method D
Standard solution: Into a small Nessler cylinder pipette 10.0 ml of either lead standard solution (1 ppm
Pb) or lead standard solution (2ppm Pb).
Test solution: Prepare as directed in the individual monograph and pipette 12 ml into a small Nessler
cylinder.
Procedure: To the cylinder containing the standard solution add 2.0 ml of the test solution and mix. To
each of the cylinders add 2 ml of acetate buffer pH 3.5, mix, add 1.2 ml of thioacetamide reagent, allow to
stand for 2 minutes and view downwards over a white surface; the colour produced with the test solution is
not more intense than that produced with the standard solution.
Title
Supersedes
: NON AQUEOUS TITRATION

: Nil
Issue Date
SOP No : GTP-10017
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 2
Protect the solution and titrate from atmospheric carbon dioxide and moisture throughout the
determination. Use the titrate, solvent and indicator specified in the individual monograph. The titrate is
standardized using the same method, solvent and indicator as specified for the substance.
Method A
Developed By :
Reviewed By :
Authorized By :
Dissolve the prescribed quantity of the substance being examined in a suitable volume of anhydrous glacial
Name:
Name:
Name:
acetic acid, warming
and coolingDesignation:
if necessary, or
prepare
a solution as
directed in the monograph
and
Designation:
QA Officer
Quality
Head
Designation:
Managing Director
Signature:
Signature:
determine the equivalence pointSignature:
potentiometrically using 0.1M Perchloric
acid as titrate, unless otherwise
COMPANY NAME
specified in the monograph. Potentionetric titration may be carried out using a glass electrode and a
standard reference electrode, e.g. calomel reference electrode containing saturated solution of potassium
chloride in water. Potentionetric titrations may also be carried out by using a glass electrode and a
saturated solution of potassium chloride in water has been replaced by a saturated solution of potassium
chloride in methanol. It must be ensured that no leakage of salt- bridge solution occurs. Alternatively, a
combined electrode may be used. The junction between the calomel electrode and the titration liquid
should have a reasonably low electrical resistance and there should be minimum of transfer of liquid from
one side to the other. The connections between the potentiometer and the electrode system must be made
according to the manufacturers instructions to avoid problems of instability.
When the temperature (t2) of the titrate at the time of the assay is different from the temperature (t1) of the
titrate when it was standardized, multiply the volume of the titrate required by [1 + 0.0011 (t1 -t2) and
calculate the result of the assay from the corrected volume.
Title
Supersedes
: NON AQUEOUS TITRATION

: Nil
Issue Date
SOP No : GTP-10017
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
2 of 2
Method B
Dissolve the prescribed quantity of the substance being examined in a suitable volume of anhydrous glacial
acetic acid previously neutralised using the indicator specified in the individual monograph, warming and
cooling if necessary, or prepare a solution as directed in the monograph. When the substance is a
hydrochloride or hydrobromide, add 15 ml of mercuric acetate solution unless otherwise directed in the
monograph Titrate with 0.1M Perchloric acid unless otherwise specified in the monograph to the full colour
change of indicator corresponding to the maximum absolute value of dE/dV (where E is the electromotive
force and V is the volume of the titrate) in a potentionetric titration of the substance being examined. The
Developed
Bytitration
:
By : the mercuric acetateAuthorized
By :
indicator
used for the
is also usedReviewed
for neutralizing
solution.
Name:
Name:
Name:
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
When the temperature of the titrant at the time of the assay is different from the temperature of the titrate
when it was standardized, the same correction factor as described under Method A is applied.
Title
Supersedes
: POTENTIOMETRIC TITRATION
: Nil
Issue Date
10/04/2010
SOP No : GTP-10018
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
A convenient and useful method of determining the equivalence point of a titration, i.e the point at which the
stoichiometric analytical reaction is complete, results from the use of electrochemical measurements. If an
indicator electrode, sensitive to the concentration of the chemical undergoing titrimetric reaction, and a
reference electrode, whose potential is not sensitive to any dissolved chemical in solution, are immersed in
the solution being examined to form a galvanic cell, the potential difference between the electrodes may be
sensed by a simple potentiometer or electromicdevice and used to
TABLE 1
Titration
Indicating
Electrode
Reference
Electrode
Applicability
Acid-base
Glass
Calomel or
silver-silver
chloride
Titration of acids and bases
Developed By :
Name:Precipitimetric
Silver
Name:
Reviewed By :
Designation:
Signature:
Signature:
Calomel
(with Head
Quality
potassium
nitrate salt
Authorized By :
Titration
with or of silver involving
Name:
halides
or
thiocyanateManaging Director
Designation:
Signature:
COMPANY NAME
bridge)
Chelometric
Mercurymercury(II)
Calomel
Titration of metals with disodium

edetate
Oxidationreduction
Platinum
Calomel or
silver-silver
chloride
Titration with bromine, dichromate

nitrite, etc.
follow the course of the reaction. If a graph of the variation of potential difference is plotted as a function of
the quantity of the titrant added, a sigmoid curve results with a rapidly changing portion in the vicinity of the
equivalence point. The mid - point of this linear vertical portion or the inflection point may taken as the end point of the titration.
in a titirimetric assay the end - point determination is an estimate of the reaction equivalence point. The
validity of this estimate depends upon, among other factors, the nature of the solution being titrated and the
concentration of the titrate. A blank correction is employed in titirimetric assays to enhance the reliability of
the end - point determination. With Potentionetric titrations the blank correction is usually negligible.
Title
Supersedes
: POTENTIOMETRIC TITRATION
: Nil
Issue Date
10/04/2010
SOP No : GTP-10018
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
Apparatus
The apparatus used comprises a voltmeter allowing readings to the nearest millivolt. the choice of the
electrode system is governed by the nature of the titration. Table 1 summary several acceptable electrode
systems.
Automatic titrations are commonly employed these days. Two types of instruments are available. In the first
one addition of titrate is carried out automatically and the electrode potential differences during the course
of titration are recorded as the expected sigmoid curve. In the second type, titrate addition is performed
automatically until or preset potential or pH, representing the end - point, is reached when the addition of
the titrate ceases.
Method
Plot a graph of the variations of potential difference versus the volume the titrate added, continuing the
addition of the titrate beyond the presumed equivalence point. The end - point corresponds to a sharp
variation of potential difference. Perform a blank titration by repeating the procedure in the same manner
omitting the substance being examined. The actual volume of titrate equivalent to the substance being
Developed By :
Reviewed By :
Authorized By :
examined is the difference between
he volume consumed in the blankName:
titration and that consumed in the
Name:
Name:
Designation:
Designation:
titration with QA
theOfficer
substance being
examined.
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: LIMIT TEST OF ARSENIC

: Nil
Issue Date
SOP No : GTP-10019
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 5
The test arsenic is intended to determine the tolerance of arsenic in a sample. The limit of arsenic
is expressed in the parts per million of arsenic trioxide.
Apparatus:
Consists of an arsenic generator (A) fitted with a scrubber unit (C) and an absorber tube (E) with standardtaper or ground glass ball and- socket joints (B and D) between the units. However any other suitable
apparatus, embodying the principle of the assembly described and illustrated, may be used.
ABSORBER TUBE
BALL-AND-SOCKET JOINTS
SCRUBER UNIT (c)
ARSENIC GENERATOR
Developed By :
Name:
A
B
C
Reviewed By :
Name:
: Generator flask (capsity: about 125 ml)

Designation: Quality Head
: Standard taper joint (24 /40 )
: ScrubberSignature:
unit
Authorized By :
Name:
Designation:
Signature:
Signature:
Managing Director
COMPANY NAME
D
E
F
Title
Supersedes
: Ground glass ball joint

: Absorber tube (capacity : about 15 ml )
: Clamp
( Unit : mm )

: Nil
Issue Date
SOP No : GTP-10019
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
2 of 5
Volumetric Solutions, Test Solutions and Reagents:

Arsenic S.S.:
Dissolve 0.100 g of arsenic trioxide, previously dried at 105 0 for 4 hrs, and
accurately weighed, in 5 ml of sodium hydroxide solution ( 1 5 ) in a 100 ml volumetric flask. Neutralize

the solution with 2 N sulfuric acid, add 10 ml more of 2 N sulfuric acid, then add recently boiled and cooled
water to volume, and mix. Transfer 10.0 ml of this solution to a 1000 ml volumetric flask, add 10 ml of 2 N
sulfuric acid, then add recently boiled and cooled water to volume , and mix. Each ml of standard
preparation contains the equivalent of 1 g of arsenic trioxide (AS2O3). Keep this solution in all glass
container, and use within 3 days.
Dilute Hydrochloric Acid (10 % ): Add water to 23.6 ml of hydrochloric acid to make 100 ml.
Hydrochloric Acid . Nitric Acid . Magnesium Nitrate . Sulfuric Acid . Sulfurous Acid . Strong
Hydrogen peroxide water . Perchloric Acid . Saturated Ammonium Oxalate Solution . 7 N Sulfuric
Acid
Potassium Iodide T.S.:
Dissolve 16.5 g of potassium iodide in water to make 100 ml. store in light resistant containers. Prepare
freshly before use.
Stannous Chloride , Acid ,m Stronger, T.S.:
Dissolve 40 g of stannous chloride in 100 ml of hydrochloric acid. Store in glass containers and within 3
months.
Lead Acetate T.S (0.5 N):
Dissolve 9.5 g of clear, transparent crystals of lead acetate in recently boiled water to make 100 ml. store in
well- stoppered bottles.
Silver Di ethyl di thio carbamate T.S:
Dissolve 1 g of silver diethyldithiocarbamate in 200 ml of recently distilled pyridine. Store in light resistant
containers, and use within 30 days.
Zinc (free
from arsenic
Developed
By : ):
Reviewed By :
Authorized By :
Use
No.
20
(ASTM)
granules (20
mesh) or granules of an equivalent Name:
particle size.
Name:
Name:
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
SOP No : GTP-10019
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
3 of 5
CAUTION:
Apparatus, reagents and test solutions used in the test should contain little or no arsenic , and , if
necessary, perform a blank determination.
Procedure:
Preparation of the sample solution:
Method 1:
Take the quantity of the indicated in the individual monograph into a generator flask (A), add 5 ml of water
and 5 ml of dilute hydrochloric acid, warm to dissolve, if necessary.
Method 2:
Take the quantity of the sample indicated in the individual monograph into a small beaker, add 5 ml of
water, and add 1 ml of sulfuric acid. Add 10 ml of sulfurous acid and evaporate the mixture on a water bath
until it is free from sulfurous acid and is reduced to about 2 ml in volume.
Method 3:
Take the quantity of the sample indicated in the individual monograph into a platinum, quartz or porcelain
crucible. Add 10 ml of a solution of magnesium nitrate in ethanol (1-50 ), ignite ethanol and heat gradually
to incinerate. If a carbonized material still remains in this method, moisten with small quantity of nitric acid,
and ignite again to incinerate. After cooling, add 3 ml of hydrochloric acid, heat on a water bath to dissolve
the residue, and designate it as the test solution.
Method 4:
Take the quantity of the sample indicated in the individual monograph into a generator flask (A), add 5 ml of
nitric acid and 2 ml of sulfuric acid. Put a small funnel on the flask then heat carefully until white fumes are
evolved. After cooling , add 2 ml of nitric acid two times and heat, then add 2 ml of strong hydrogen
peroxide water a few times, heat until the solution develops a white to pale yellow color. After cooling add
2ml of saturated ammonium oxalate solution and heat again until white fumes are evolved. After cooling,
add water to make 5 ml of the test solution.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
SOP No : GTP-10019
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
4 of 5
Method 5:
Take the quantity of the sample indicated in the individual monograph into a generator flask (A), add 5 ml of
nitric acid and 2 ml of sulfuric acid. Put a small funnel on the flask then heat carefully until white fumes are
evolved. After cooling add 2 ml of nitric acid two times and heat, then add 2 ml of nitric acid and 1 ml of
Perchloric acid a few times, heat until the solution develops a white to pale yellow color. After cooling, add
2 ml of standard ammonium oxalate solution and heat again until white fumes are evolved.
Method 6:
Take the quantity of the sample indicated in the individual monograph into a small beaker, add 8 ml of 3 N
hydrochloric acid, warm to dissolve, add 2 ml of 30 % hydrogen peroxide water, heat on the hotplate for 10
min. then add 1 ml of 30 % hydrogen peroxide water , heat until a bubble breaks. After cooling, dilute with
water to make 5 ml , and designate it as the test solution.
Test of the sample solution:
If the test preparation was not prepared in the generator flask (A), transfer to the flask a volume of the
solution prepared as directed in the individual monograph, and add water to make 35 ml to the sample
solution, add 20 ml of dilute sulfuric acid ( 1- 5 ) , 2 ml of potassium iodide T.S., and 0.5 ml of stronger acid
stannous chloride T.S ., and mix. Allow to stand for 30 min at room temp. pack the scrubber tube (C) with
two pledges of cotton that have been soaked in saturated lead acetate solution, from exceeded solution by
expression, and dried in vacuum at room temp. ,leaving a 2 mm space between the two pledges. Lubricate
the joints (B and D ) with a suitable stopcock grease (designed for use with organic solvents), and connect
the scrubber unit to the absorber tube (E). transfer 3.0 ml of silver di-ethyl-di-thio-carbamate T.S. to the
absorber tube. Alternatively, a larger accurately measured volume of the silver di-ethyl-di-thio-carbamate
T.S .may be employed, provided that the same volume is used for the control test and that the apparatus
will accommodate the layer volume. Add 3.0 g of granular zinc (No. 20 mesh) to the mixture in the flask,
immediately connect the assembled scrubber unit , place the generator flask (A) in a water bath maintained
at a temperature of 253.0 , and allow the evolution of hydrogen and the color development to proceed for
45 min, swirling the flask gently at 10 min intervals. ( If necessary , to obtain a more uniform rate of gas
evolution, 1 ml of isopropyl alcohol may be added to the generator ) . disconnect the absorber tube from
the generator and scrubber units, and transfer the silver di-ethyl-di-thio-carbamate T.S. to Nessler tubes.
: TEST OF ARSENIC
Reviewed By :
TitleDeveloped: By
LIMIT
Name:
Name:
Supersedes
: Nil
Issue Date
10/04/2010
Designation:
Authorized By :
Name:
Review date
April 2012
Signature:
SOP No : GTP-10019
Signature:
Effective date
Signature:
Page number
Quality10/04/2010
Head
Designation:
Managing Director
5 of 5
COMPANY NAME
The color of the silver di-ethyl-di-thio-carbamate T.S .corresponds to the volume of arsenic S.S. prepared
as the control. The test of the sample solution and the preparation of the control should be carried out
simultaneously.
Transfer test solution to the generator flask (A) , if necessary, wash the container with a small quantity of
water, and add water to make 35 ml. proceed as directed for procedure under the same method as
standard preparation. Compare the red color produced in the silver di-ethyl-di-thio-carbamate T.S. by the
sample solution with that of the control which is obtained by similarly treating the solution lining 2.0 ml of
arsenic S.S.
In a monograph, for example an indication, arsenic (As2O3):
Not more than 1ppm [ 2.0 g , (10, REF 2.0 ml of As 2O3 STD ], EXPRESSES THAT THE COLOR
PRODUCED BY 2.0 g of the sample is not more intense than that produced by 2.0 ml of arsenic S.S.
prepared as standard preparation, that is, arsenic trioxide is not more than 1 ppm of the sample tested.
Title
Supersedes
: Identification Reactions of Ions and functional Groups

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
1 of 11
Objective
functional groups
terms
Developed :By The
: identification ofReviewed
By : in the individual monographs
Authorizedin By
: of the
substance
being
examined.
Name:
Name:
Name:
SCOPE
Signature:
Designation:
Quality Head
Designation:
Managing Director
The procedure
is applicable to all Active & Inactive
raw materials and Finished
Signature:
Signature:
Products
COMPANY NAME
APPARATUS
As required by Individual Test
REAGENTS
As required by Individual Test
PROCEDURE
Acetates:
A)
Heat the substance being examined with an equal quantity of Oxalic Acid. Acidic vapors with the
characteristic odour of Acetic Acid are evolved.
B)
To about 30 mg of the substance being examined dissolved in 3 ml of Water or to 3 ml of the

prescribed solution add successively 0.25 ml of Lanthanum Nitrate Solution, 0.1 ml of 0.05 M Iodine
and 0.05 ml of 2 M Ammonia and heat the mixture carefully to boiling. After a few minutes a blue
precipitate or a dark blue colour is produced.
Acetyl Groups:
In a test tube (about 180 mm 18 mm) place about 15 mg of the substance being examined or the
prescribed quantity and 0.15 ml of Orthophosphoric Acid.
Close the tube with a stopper through which passes a small test tube (about 100 mm 10 mm) containing
water to act as a condenser. Hang a drop of Lanthanum Nitrate Solution on the outside of the smaller tube.
Except for substances hydrolysable only with difficulty, place the apparatus in a water bath for 5 minutes
and remove the smaller tube. Mix the drop with 0.05 ml of 0.01 M Iodine on a tile and add, at the edge,
0.05 ml of 2 M Ammonia. After 1 or 2 minutes a blue colour is produced at the junction of the two drops
which intensifies and persists for a short time.
For substances hydrolysable only with difficulty, proceed as described above but heat the mixture slowly to
boiling point over an open flame instead of using a water bath.
Alkaloids:
Dissolve a few mg or the prescribed quantity of the substance being examined in 5 ml of Water, acidify with
2M Hydrochloric Acid and add 1 ml of Potassium Iodobismuthate solution. An orange or orange-red
precipitate is produced immediately.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
2 of 11
Aluminum Salts:
Thioacetamide Reagent:
Add 1 ml of a mixture of 15 ml of 1M Sodium Hydroxide, 5 ml of Water and 20 ml of Glycerol (85%) to 0.2
ml of Thioacetamide solution, heat in a water bath for 20 seconds, cool and use immediately.
Developed By :
Name:
Procedure:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
To about 15 mg of the substance being examined dissolved in 2 ml of water or to 2 ml of the prescribed
solution add about 0.5 ml of 2M Hydrochloric Acid and about 0.5 ml of Thioacetamide Reagent; no
precipitate is produced. Add 2M Sodium Hydroxide drop wise; a gelatinous white precipitate is produced
which dissolves on further addition of 2M Sodium Hydroxide. Gradually add Ammonium Chloride Solution;
the gelatinous white precipitate reappears.
Amines, Primary Aromatic
Acidify the prescribed solution with 2M Hydrochloric Acid or dissolve 0.1 g in 2 ml of 2M Hydrochloric Acid
and add 0.2 ml of Sodium Nitrite solution. After 1 to 2 minutes add the solution to 1 ml of 2-naphthol
solution. An intense orange or red colour and, usually, a precipitate of the same colour are produced.
Ammonium Salts:
To the prescribed solution add 0.2 g of magnesium oxide. Pass a current of air through the mixture and
direct the gas that escapes just beneath the surface of a mixture of 1 ml of 0.1M Hydrochloric Acid and
0.05 ml of Methyl Red Solution; the colour of the solution changes to yellow. Add 1 ml of a freshly prepared
10% w/v solution of Sodium Cobaltinitrite; a yellow precipitate is produced.
Ammonium salts and salts of volatile bases:
To about 20 mg of the substance being examined dissolved in 2 ml of Water or to 2 ml of the prescribed
solution add 2 ml of 2M Sodium Hydroxide and heat. A vapour is evolved which can be identified by its
odour and which is Alkaline (Produce Blue colour when treated with Red Litmus Paper).
Antimony Compounds:
Dissolve with gentle heating about 10 mg of the substance being examined in a solution of 0.5 g of
potassium sodium (+)-Tartrate in 10 ml of Water and allow cooling. To 2 ml of this solution or to 2 ml of the
prescribed solution add Sodium Sulphide Solution drop wise. An orange-red precipitate is produced which
dissolves on addition of 2M Sodium Hydroxide.
Arsenic Compounds:
Heat 5 ml of the prescribed solution on a water bath with 5 ml of Hypo phosphorous Reagent. A brown
precipitate is produced.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
3 of 11
Barbiturates, non-nitrogen substituted:

Dissolve about 5 mg of the substance being examined in 3 ml of Methanol, add 0.1 ml of a solution
containing 10% w/v of Cobalt (II) Nitrate and 10% w/v of Calcium Chloride, mix and add, with shaking, 0.1
ml of 2M Sodium Hydroxide. A violet blue colour and precipitate are produced.
Benzoates:
A)
To 1 ml of aBy
10%
of the substance
being examinedAuthorized
or to 1 ml of By
the :prescribed
Developed
: w/v Neutral Solution
Reviewed
By :
Name: solution add 0.5 ml of Iron
Name:
(III) Chloride Solution. A dull yellowName:
precipitate is produced which is
soluble in Ether.
Signature:
Designation:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
B)
Moisten 0.2 g of the substance being examined, treated as prescribed if necessary, with 0.2 to 0.3
ml of sulphuric acid and gently warm the bottom of the tube. A white sublimate is deposited on the
inner wall of the tube.
C)
To 0.5 g of the substance being examined dissolved in 10 ml of Water or to 10 ml of the prescribed

solution add 0.5 ml of Hydrochloric Acid. The melting point of the precipitate, after recrystallisation
from Water and drying at a pressure of 2 kPa is 120 to 124
Bicarbonates:
A)
Introduce into a test tube 0.1 g of the substance being examined suspended in 2 ml of Water or use
2 ml of the prescribed solution. Add 3 ml of 2M Acetic Acid, close the tube immediately using a
stopper fitted with a glass tube bent at two right angles. The solution or suspension effervesces.
Heat gently and collect the gas in 5 ml of a 4.73% w/v solution of Barium Hydroxide. A white
precipitate is produced which dissolves on addition of an excess of 7M Hydrochloric Acid.
B)
Treat a solution of the substance being examined with a solution of Magnesium Sulphate; no
precipitate is produced (distinction from carbonates). Boil, a white precipitate is produced.
C)
A solution liberates Carbon Dioxide when boiled.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
4 of 11
Bismuth and Bismuth Compounds:

A.
To 0.5 g of the substance being examined add 10 ml of 2 M Hydrochloric Acid or use 10 ml of the
prescribed solution. Boil for 1 minute, cool, filter if necessary and to 1 ml of the resulting solution
add 20 ml of Water. A white or slightly yellow precipitate is produced which turns brown on addition
of 0.05 to 0.1 ml of Sodium Sulphide Solution.
B.
To about 45 mg of the substance being examined add 10 ml of 2 M Nitric Acid or use 10 ml of the
prescribed solution.
Developed By :
Reviewed By :
Authorized By :
Name:
Name:
Name:
Boil for 1 minute, allow to cool, filter if necessary and to 5 ml of the resulting solution add 2 ml of a 10% w/v
Designation:
Quality Head
Designation:
Managing Director
solution of Thiourea, a yellowish orange colour or an orange precipitate is produced. Add 4 ml of a 2.5%
Signature:
Signature:
Signature:
w/v solution of Sodium Fluoride; the solution is not decolorized within 30 minutes.
COMPANY NAME
Bromides:
A)
Dissolve a quantity of the substance being examined containing about 3 mg of Bromide Ion in 2 ml
of Water or use 2 ml of the prescribed solution. Acidify with 2M nitric acid, add 0.4 ml of Silver
Nitrate Solution, shake and allow to stand; a curdy, pale yellow precipitate is produced. Centrifuge
and wash the precipitate with three 1-ml quantities of Water. Carry out this operation rapidly in
subdued light disregarding the fact that the supernatant solution may not become perfectly clear.
Suspend the precipitate obtained in 2 ml of water and add 1.5 ml of 10M Ammonia; the precipitate
dissolves with difficulty.
B)
Introduce into a small test tube a quantity of the substance being examined containing about 5 mg
of bromide ion or the prescribed quantity, add 0.25 ml of Water, about 75 mg of Lead (IV) oxide and
0.25 ml of 5M Acetic Acid and shake gently.
Dry the inside of the upper part of the test tube with filter paper and allow to stand for 5 minutes. Moisten a
strip of suitable filter paper of appropriate size by dipping the tip in a drop of decolorized Fuchsine Solution
and introduce the moistened part immediately into the tube. Starting from the tip, a violet colour is
produced within 10 seconds, which is clearly distinguishable from the red colour of Fuchsine, which may be
visible on a small area at the top of the moistened part of the paper strip.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
5 of 11
Calcium and Calcium Salts:

A)
To 0.2 ml of a neutral solution containing about 0.2 mg of Calcium Ion per ml or to 0.2 ml of the
prescribed solution add 0.5 ml of a 0.2% w/v solution of Glyoxal bis (2-hydroxyanil) in Ethanol
(96%), 0.2 ml of 2M Sodium Hydroxide and 0.2 ml of Sodium Carbonate solution. Extract with 1 to 2
ml of Chloroform and add 1 to 2 ml of Water. The Chloroform layer is red.
B)
Dissolve about 20 mg of the substance being examined or the prescribed quantity in 5 ml of 5M

Acetic Acid and add 0.5 ml of Potassium Hexacyanoferrate (II) Solution; the solution remains clear.
Add about 50 mg of Ammonium Chloride; a white, crystalline precipitate is produced.
C)
To 5 ml of 0.4% w/v solution of the substance being examined add 0.2 ml of a 2% w/v solution of
Ammonium Oxalate. A white precipitate is produced which is only sparingly soluble in 6M Acetic
Acid but is soluble in hydrochloric acid.
Note: Only for BP material performs Test A, B & C, for Ph. Eur. Material perform Test A & B only.
Carbonates:
A)
Introduce into a test tube 0.1 g of the substance being examined suspended in 2 ml of Water or use
2 ml of the prescribed solution. Add 3 ml of 2M Acetic Acid, close the tube immediately using a
stopper fitted with a glass tube bent at two right angles. The solution or suspension effervesces
Developed
By :
Reviewed
: and collect the gas
Authorized
By :Barium
evolving a colourless
and odourless
gas. HeatBy
gently
in 5 ml of 0.1M
Name: Hydroxide. A white precipitate
Name:
Name:
is produced which dissolves on addition of an excess of 7M
Designation:
QA Officer
Designation:
Managing Director
Hydrochloric
Acid.
Signature:
Signature:
Signature:
COMPANY NAME
B)
Treat a solution of the substance being examined with a solution of Magnesium Sulphate. A white
precipitate is produced (distinction from bicarbonates).
Note: Only for BP material perform Test A, & B, for Ph. Eur. Material perform Test A only.
Carbonates and Bicarbonates:
Introduce into a test tube 0.1 g of the substance being examined suspended in 2 ml of water or use 2 ml of
the prescribed solution. Add 3 ml of 2M Acetic Acid, close the tube immediately using a stopper fitted with a
glass tube bent at two right angles. The solution or suspension effervesces evolving a colourless and
odourless gas. Heat gently and collect the gas in 5 ml of 0.1M Barium Hydroxide. A white precipitate is
produced which dissolves on addition of an excess of 7M Hydrochloric Acid.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
6 of 11
Chlorides:
A)
Dissolve a quantity of the substance being examined containing about 2 mg of Chloride Ion in 2 ml
of Water or use 2 ml of the prescribed solution. Acidify with 2M Nitric Acid, add 0.4 ml of Silver
Nitrate Solution, shake and allow standing; a curdy, white precipitate is produced. Centrifuge and
wash the precipitate with three 1-ml quantities of Water. Carry out this operation rapidly in subdued
light, disregarding the fact that the supernatant solution may not become perfectly clear. Suspend
the precipitate in 2 ml of water and add 1.5 ml of 10M Ammonia; the precipitate dissolves easily with
the possible exception of a few large particles, which dissolve slowly.
B)
Introduce into a test tube a quantity of the substance being examined containing about 15 mg of
chloride ion or the prescribed quantity, add 0.2 g of Potassium Dichromate and 1 ml of Sulphuric
Acid and place a filter paper strip moistened with 0.1 ml of Diphenylcarbazide solution over the
opening of the test tube. The paper turns violet-red. The moistened paper must not come into
contact with the Potassium Dichromate Solution.
Citrates:
A)
B)
To a quantity of the substance being examined corresponding to about 50 mg of Citric Acid

dissolved in 5 ml of Water or to 5 ml of the prescribed solution add 0.5 ml of Sulphuric Acid and 1 ml
of Potassium Permanganate Solution and warm until the colour of the Permanganate is discharged.
Add 0.5 ml of a 10% w/v solution of Sodium Nitroprusside in 1M Sulphuric Acid and 4 g of
Sulphamic Acid and add 13.5M Ammonia drop wise until all the Sulphamic Acid has dissolved. On
addition of an excess of 13.5M Ammonia a violet colour is produced which changes to violet-blue.
To a neutral solution of the substance being examined add a solution of Calcium Chloride; no
precipitate is produced. Boil the solution; a white precipitate is produced which is soluble in 6M
Developed
Reviewed By :
Authorized By :
Acetic Acid.By :
Name:
Name:
Name:
Designation:
QABP
Officer
Designation:
Quality
Head
Director
Note: Only for
material performs
Test A, & B,
for Ph.
Eur. MaterialDesignation:
performs Test A Managing
only.
Signature:
Signature:
Signature:
COMPANY NAME
Esters:
To about 30 mg of the substance being examined or to the prescribed quantity add 0.5 ml of a 7% w/v
solution of Hydroxylamine Hydrochloride in Methanol and 0.5 ml of a 10% w/v solution of Potassium
Hydroxide in Ethanol (96%). Heat to boiling, cool, acidify with 2M Hydrochloric Acid and add 0.2 ml of a 1%
w/v solution of Iron (III) Chloride Hexahydrate. A bluish red or red colour is produced.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
7 of 11
Iodides:
A)
Dissolve a quantity of the substance being examined containing about 4 mg of iodide ion in 2 ml of
water or use 2 ml of the prescribed solution. Acidify with 2M Nitric Acid, add 0.4 ml of silver nitrate
solution R1, shake and allow to stand; a curdy, pale yellow precipitate is produced. Centrifuge and
wash with three 1-ml quantities of water. Carry out these operations rapidly in subdued light
disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the
precipitate in 2 ml of water and add 1.5 ml of 10M Ammonia; the precipitate does not dissolve.
B)
To 0.2 ml of a solution of the substance being examined containing about 5 mg of Iodide Ion per ml
or to 0.2 ml of the prescribed solution add 0.5 ml of 1M Sulphuric Acid, 0.1 ml of Potassium
Dichromate Solution, 2 ml of water and 2 ml of Chloroform. Shake for a few seconds and allow to
stand. The Chloroform layer is violet or violet-red.
Iron and iron salts:

A)
To a quantity of the substance being examined containing about 10 mg of Iron (II) dissolved in 1 ml
of Water or to 1 ml of the prescribed solution add 1 ml of potassium Hexacyanoferrate (III) Solution.
A blue precipitate is produced which is insoluble in 2M Hydrochloric Acid (Iron (II) Salts).
B)
To 3 ml of a solution containing about 0.1 mg of Iron (III) or to 3 ml of the prescribed solution add 1
ml of 2M Hydrochloric Acid and 1 ml of Potassium Thiocyanate Solution; the solution is red. To 1 ml
of the solution add 5 ml of Isoamyl Alcohol or Ether, shake and allow to stand; the organic layer is
pink. To a further 1 ml of the solution add 2 ml of Mercury (II) Chloride Solution; the red colour is
discharged (Iron (III) Salts).
C)
To 1 ml of a solution containing not less than 1 mg of Iron (III) or to 1 ml of the prescribed solution
add 1 ml of Potassium Hexacyanoferrate (II) Solution. A blue precipitate is produced which is
insoluble in 5 ml of 2M Hydrochloric Acid (Iron (III) Salts).
Lactates:
To 5 ml of a solution of the substance being examined corresponding to about 5 mg of Lactic Acid or to 5
By
:
Reviewed
By and
: 0.5 ml of 1M Sulphuric
Authorized
: on a
ml of Developed
the prescribed
solution
add 1 ml of Bromine
Water
Acid andBy
heat
Name:
Name:
Name:
water bath until the colour is discharged, stirring occasionally with a glass rod.
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Add 4 g of Ammonium Sulphate, mix and add drop wise, without mixing, 0.2 ml of a 10% w/v solution of
Sodium Nitroprusside in 1M Sulphuric Acid. Still without mixing add 1 ml of 13.5M Ammonia and allow to
stand for 30 minutes. A dark green ring is produced at the interface of the two liquids.
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
April 2012
Page number
8 of 11
Lead and Lead Compounds:

A)
To 0.1 g of the substance being examined dissolved in 1 ml of 5M Acetic Acid or to 1 ml of the

prescribed solution add 2 ml of Potassium Chromate Solution. A yellow precipitate is produced
which is soluble in 2 ml of 10M Sodium Hydroxide.
B)
To 50 mg of the substance being examined dissolved in 1 ml of 5M Acetic Acid or to 1 ml of the

prescribed solution add 10 ml of Water and 0.2 ml of Potassium Iodide Solution; a yellow precipitate
is produced. Heat to boiling for 1 to 2 minutes and allow to cool; the precipitate reappears as
glistening, yellow plates.
Lignin:
A)
Lignin cell walls are coloured bright red by soaking them in a 1% w/v solution of Phloroglucinol in
Ethanol (90%) and adding 0.1 to 0.2 ml of Hydrochloric Acid.
B)
Lignified tissues are coloured yellow by Aniline Hydrochloride Solution.
Magnesium and Magnesium Salts:

A)

prescribed solution add 1 ml of 6M Ammonia; a white precipitate is produced which is dissolved by
adding 1 ml of Ammonium Chloride Solution. Add 1 ml of Disodium Hydrogen Phosphate Solution; a
white crystalline precipitate is produced.
B)
To 0.5 ml of a neutral or slightly acidic solution of the substance being examined add 0.2 ml of a
0.1% w/v solution of titan yellow and 0.5 ml of 0.1M Sodium Hydroxide. A bright red turbidity is
produced which gradually settles to give a bright red precipitate.
Note: Only for BP material performs Test A, & B, for Ph. Eur. Material performs Test A only.
Mercury and Mercury Compounds:
A)
Place about 0.1 ml of a solution of the substance being examined on well-scraped copper foil; a
dark grey stain is produced which becomes shiny on rubbing. Heat the dried copper foil in a test
tube; the spot disappears.
By : solution add 2MReviewed

By : until strongly alkaline,
Authorized
: colour
B) Developed
To the prescribed
Sodium Hydroxide
(ProduceBy
pink
Name: when treated with colourName:
Name:
less Phenolphthalein Paper). A dense, yellow precipitate is produced
Designation:
QA Officer
Designation:
(Mercury
(II) Compounds).
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
9 of 11
Nitrates:
To a mixture of 0.1 ml of Nitrobenzene and 0.2 ml of Sulphuric Acid add a quantity of the powdered
substance containing about 1 mg of Nitrate Ion or the prescribed quantity and allow to stand for 5 minutes.
Cool in ice, add slowly with stirring 5 ml of Water, then 5 ml of 10M Sodium Hydroxide and 5 ml of Acetone
shake and allow to stand. The upper layer is deep violet.
Odour:
Spread 0.5 to 2.0 g of the substance being examined in a thin layer on a watch glass 6 to 8
cm in diameter. After 15 minutes determine the odour or verify the absence of odour.
Phosphates (Orthophosphates):
Molybdovanadic Reagent:
Suspend 4 g of finely powdered Ammonium Molybdate and 0.1 g of finely powdered Ammonium Molybdate
in 70 ml of Water and grind until dissolved. Add 20 ml of Nitric Acid and dilute to 100 ml with Water.
A)
To 5 ml of the prescribed solution, neutralised if necessary, add 5 ml of silver nitrate solution R1. A
yellow precipitate is produced the colour of which is not changed on boiling and which is soluble in
10M ammonia.
B)
Mix 1 ml of the prescribed solution with 2 ml of Molybdovanadic Reagent. A yellow colour develops.
Potassium and potassium salts

A)

solution add 1 ml of Sodium Carbonate Solution and heat; no precipitate is produced. Add while hot
0.05 ml of Sodium Sulphide solution; no precipitate is produced. Cool in ice and add 2 ml of a 15%
w/v solution of (+)-Tartaric Acid and allow to stand; a white, crystalline precipitate is produced.
B)

prescribed solution add 1 ml of 2M Acetic Acid and 1 ml of a freshly prepared 10% w/v solution of
Sodium Cobalt nitrite. A yellow or orange-yellow precipitate is produced immediately.
Salicylates:
A)
To 1 ml of a 10% w/v neutral solution of the substance being examined or to 1 ml of the prescribed
solution add 0.5 ml of Iron (III) Chloride Solution. A violet colour is produced which is not discharged
on the addition of 0.1 ml of 5M Acetic Acid.
B)
Developed
By : point of the precipitate,
Authorized
By :
solution addBy
0.5: ml of hydrochloricReviewed
acid. The melting
after recrystallisation
Name: from hot Water and drying
Name:
Name:
at a pressure of 2 kPa is 156 to 161
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10020
Effective date
10/04/2010
Page number
April 2012
10 of 11
Silicates:
In a lead or platinum crucible mix to a thin slurry using a copper wire the prescribed quantity of the
substance being examined with 10 mg of Sodium Fluoride and 0.2 ml of Sulphuric Acid. Cover the crucible
with a thin, transparent plate of plastic from which a drop of Water is suspended and warm gently. A white
ring is rapidly produced around the drop of Water.
Silver and silver compounds:
To 10 mg of the substance being examined dissolved in 10 ml of Water or to 10 ml of the prescribed
solution add 0.3 ml of 7M Hydrochloric Acid; a curdy, white precipitate is produced which is soluble in 3 ml
of 6M Ammonia.
Sodium and Sodium Salts:
Methoxyphenylacetic Acid Reagent:
Dissolve 2.7 g of Methoxyphenylacetic acid in 6 ml of Tetramethylammonium Hydroxide Solution and add
20 ml of Absolute Ethanol.
A)

solution add 2 ml of a 15% w/v solution of Potassium Carbonate and heat to boiling; no precipitate
is produced. Add 4 ml of freshly prepared Potassium Antimonate (VS) solution and heat to boiling.
Allow cooling in ice and if necessary scratching the inside of the tube with a glass rod; a dense,
white precipitate is produced.
B)
To 0.5 ml of a solution containing about 2 mg of sodium ion or to 0.5 ml of the prescribed solution
add 1.5 ml of Methoxyphenylacetic Acid Reagent and cool in ice for 30 minutes; a voluminous,
white, crystalline precipitate is produced. Warm in Water at 20 and stir for 5 minutes; the
precipitate does not dissolve. Add 1 ml of 6M Ammonia; the precipitate dissolves completely. Add 1
ml of a 16% w/v solution of Ammonium Carbonate; no precipitate is produced.
Sulphates:
A)

prescribed solution add 1 ml of 2M Hydrochloric Acid and 1 ml of Barium Chloride Solution. A
white precipitate is produced.
B)
Add 0.1 ml of 0.05M Iodine to the suspension obtained in reaction A; the suspension remains yellow
(distinction from Sulphites and Dithionite) but is decolorized by adding, drop wise, Tin (II) Chloride
Solution (distinction from Iodated). Boil the mixture; no coloured precipitate is produced (distinction
from Selenate and Tungstate).
Developed By :
Reviewed By :
Authorized By :
Name:
Name:
Name:
Title
Designation:
: Nil
Signature:
Designation:
Issue Date
Signature:
Quality10/04/2010
Head
Designation:
Review date
Signature:
Managing
AprilDirector
2012
COMPANY NAME
SOP No : GTP-10020
Effective date
10/04/2010
Page number
11 of 11
Tartrates:
A)

prescribed solution add 0.05 ml of a 1% w/v solution of Iron (II) Sulphate and 0.05 ml of Hydrogen
Peroxide Solution (10 vol); a transient yellow colour is produced. After the colour has disappeared
add 2M Sodium Hydroxide dropwise; an intense blue colour is produced.
B)
To 0.1 ml of a solution containing the equivalent of about 15 mg of Tartaric Acid per ml or to 0.1 ml
of the prescribed solution add 0.1 ml of a 10% w/v solution of Potassium Bromide, 0.1 ml of a 2%
w/v solution of Resorcinol and 3 ml of Sulphuric Acid and heat on a water bath for 5 to 10 minutes.
A dark blue colour is produced which changes to red when the solution is allowed to cool and
poured into Water.
Xanthines:
Mix a few mg of the substance being examined or the prescribed quantity with 0.1 ml of Hydrogen Peroxide
Solution (100 vol) and 0.3 ml of 2M Hydrochloric Acid, heat to dryness on a water bath until a yellowish red
residue is produced and add 0.1 ml of 2M Ammonia. The colour of the residue changes to violet-red.
Zinc and Zinc salts:
To 0.1 g of the substance being examined dissolved in 5 ml of Water or to 5 ml of the prescribed solution
add 0.2 ml of 10M Sodium Hydroxide; a white precipitate is produced. Add a further 2 ml of 10M Sodium
Hydroxide; the precipitate dissolves. Add 10 ml of Ammonium Chloride solution; the solution remains clear.
Add 0.1 ml of sodium Sulphide Solution; a flocculent, white precipitate is produced.
Note: The above document is prepared on the basis of Appendix VI / method 2.3.1 of BP / Ph. Eur.
Title
Supersedes
:IDENTIFICATION BY UV
: Nil
Issue Date
By :
SOPDeveloped
No : GTP-10021
Name:
10/04/2010
10/04/2010
By :
EffectiveReviewed
date
Name:
Review date
Authorized By
Page number
1 of:1
Name:
Designation:
Designation:
Head
Designation:
Objective QA: OfficerTo lay down
a procedureQuality
of Identification
test by
UV.
Signature:
Signature:
April 2012
Signature:
Managing Director
COMPANY NAME
SCOPE
This procedure is applicable to all Active Material, Inactive Material of In-process and
Finished Products.
APPARATUS
UV-Visible spectrophotometer
Quartz Cuvettes or Quartz Cells (1.0 cm)
REAGENTS
Freshly distilled Water

Solvents as specified
Chemicals as specified
: AR Grade
: AR Grade
PROCEDURE
Set the spectrophotometer in the photometric mode. Select the specified wavelength. Prepare the test
solution as per the requirement by dissolving accurately weighed amount of sample in the specified volume
of solvent or diluents. Transfer the solvent or diluents, in which samples prepared, in both the reference
and sample cuvette.
Place the cuvette in cuvette holders of the instrument. Auto zero the displayed reading of absorbance to
nullify the interference of the solvent. Remove only the sample cuvette from its holder, and rinse it with
about 2 to 3 ml of test solution, twice.
Fill the cuvette with the test solution and place it in the sample cuvette holder. Record the absorbance from
the display. Where specific absorbance is required calculate using the formula given below.
Specific Absorbance =
10 x Absorbance in 1-cm cell x Dilution

---------------------------------------------------Weight in milligram
The Test solution must be clear. (Absorbance of hazy or partially dissolved substance cannot be
measured.)
Note: The above document is prepared on the basis USP, Ph.Eur & BP.
Title
Supersedes
: THIN LAYER CHROMATOGRAPHY

: Nil
Issue Date
10/04/2010
SOP No : GTP-10022
Objective
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 4
To lay down a procedure of Identification test Or Related Substance by TLC.
SCOPE
: By This
procedure is applicable
all Active
Material, Inactive
Material of By
In-process
and
Developed
:
ReviewedtoBy
:
Authorized
:
Finished Products.
Name:
Name:
Name:
APPARATUS
Signature:
Designation:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Thin Layer Chromatographic Plates

Fluorescence detection device
Microsyringes
Micropipettes
Calibrated disposable capillaries
Chromatographic tank
REAGENTS
Reagents as described in the monograph
PROCEDURE
Thin-layer chromatography is a separation technique in which a stationary phase consisting of an
appropriate material is spread in a uniform thin layer on a support (plate) of glass, metal or plastic.
Solutions of analytes are deposited on the plate prior to development. The separation is based on
adsorption, partition, ion exchange or on combinations of these mechanisms and is carried out by migration
(development) of solutes (solutions of analytes) in a solvent or a suitable mixture of solvents (mobile
phase) through the thin-layer (stationary phase).
APPARATUS
Plates:
The chromatography is carried out using pre-coated plates.
Preconditioning of the plates:

It may be necessary to wash the plates prior to separation. This can be done by migration of an appropriate
solvent. The plates may also be impregnated by procedures such as development, immersion or spraying.
At the time of use, the plates may be activated, if necessary, by heating in an oven at 100-105 C for
1 hour.
A chromatographic tank with a flat bottom or twin trough, of inert, transparent material, of a size suitable for
the plates used and provided with a tightly fitting lid. For horizontal development the tank is provided with a
trough for the mobile phase and it additionally contains a device for directing the mobile phase to the
stationary phase.
Micropipettes, micro syringes, calibrated disposable capillaries or other application devices suitable for the
proper application of the solutions.
Fluorescence detection device to measure direct fluorescence or the inhibition of fluorescence.
Visualization reagents to detect the separated spots by spraying, exposure to vapour or immersion.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10022
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 4
METHOD
Vertical development:
Line the walls of the chromatographic tank with filter paper. Pour into the chromatographic tank a sufficient
quantity of the mobile phase for the size of the tank to give after impregnation of the filter paper a layer of
appropriate depth related to the dimension of the plate to be used. For saturation of the chromatographic
: allow to stand atReviewed
:
Authorized
By :
tank, Developed
replace the lidBy
and
20-25 C forBy
1 hour.
Unless otherwise
indicated, the
chromatographic separation is performed
Name:
Name: in a saturated tank.
Name:
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Apply the prescribed volume of the solutions in sufficiently small portions to obtain bands or circular spots
at an appropriate distance from the lower edge and from the sides of the plate. Apply the solutions on a line
parallel to the lower edge of the plate with an interval of at least 10 mm between the spots.
When the solvent has evaporated from the applied solutions, place the plate in the chromatographic tank,
ensuring that the plate is as vertical as possible and that the spots or bands are above the surface of the
mobile phase. Close the chromatographic tank, maintain it at 20-25 C and protect from sunlight. Remove
the plate when the mobile phase has moved over the prescribed distance. Dry the plate and visualise the
chromatograms as prescribed.
For two-dimensional chromatography, dry the plates after the first development and carry out a second
development in a direction perpendicular to that of the first development.
Horizontal development:
Apply the prescribed volume of the solutions in sufficiently small portions to obtain circular spots 1 mm to
2 mm in diameter, or bands 5 mm to 10 mm by 1 mm to 2 mm, at an appropriate distance from the lower
edge and from the sides of the plate.
Apply the solutions on a line parallel to the lower edge of the plate with an interval of at least 5 mm
between the spots. When the solvent has evaporated from the applied solutions, introduce a sufficient
quantity of the mobile phase into the trough of the chamber using a syringe or pipette, place the plate
Horizontally in the chamber and connect the mobile phase direction device according to the manufacturers
instructions.
If prescribed, develop the plate starting simultaneously at both ends. Close the chamber and maintain it at
20-25 C. Remove the plate when the mobile phase has moved over the distance prescribed in the
monograph. Dry the plate and visualize the chromatograms as prescribed.
For two-dimensional chromatography, dry the plates after the first development and carry out a second
development in a direction perpendicular to that of the first development.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10022
Effective date
10/04/2010
Review date
April 2012
Page number
3 of 4
VISUAL ESTIMATION:
Identification:
The principal spot in the chromatogram obtained with the test solution is visually compared to the
corresponding spot in the chromatogram obtained with the reference solution by comparing the colour, the
size and the retention factor (Rf) of both spots.
The retention factor (Rf) is defined as the ratio of the distance from the point of application to the centre of
the spot and the distance travelled by the solvent front from the point of application.
Developed
:
Reviewed
By :
Verification
of theBy
separating
power for
identification:
Name:
Name:
Authorized By :
Name:
Designation:
Officer
Quality
Head
Designation:
Managing
Normally theQA
performance
givenDesignation:
by the suitability
test described
in Reagents
is sufficient.
Only inDirector
special
Signature:
Signature:
cases an additional performanceSignature:
criterion is prescribed in the monograph.
COMPANY NAME
Related substances test:
The secondary spot(s) in the chromatogram obtained with the test solution is (are) visually compared to
either the corresponding spot(s) in the chromatogram obtained with the reference solution containing the
impurity(ies) or the spot in the chromatogram obtained with the reference solution prepared from a dilution
of the test solution.
Verification of the separating power:
The requirements for the verification of the separating power are prescribed in the monographs concerned.
Verification of the detecting power:
The detecting power is satisfactory if a spot or band is clearly visible in the chromatogram obtained with the
most dilute reference solution.
Quantitative Measurement
The requirements for resolution and separation are prescribed in the monographs concerned.
Substances separated by thin-layer chromatography and responding to UV-Vis irradiation can be
determined directly on the plate, using appropriate instrumentation. While moving the plate or the
measuring device, examine the plate by measuring the reflectance or transmittance of the incident light.
Similarly, fluorescence may be measured using an appropriate optical system.
Substances containing radionuclides can be quantified in three ways: either directly by moving the plate
alongside a suitable counter or vice versa by cutting the plates into strips and measuring the radioactivity
on each individual strip using a suitable counter or by scraping off the stationary phase, dissolving it in a
suitable scintillation cocktail and measuring the radioactivity using a liquid scintillation counter.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10022
Effective date
10/04/2010
Review date
April 2012
Page number
4 of 4
Apparatus:
The apparatus for direct measurement on the plate consists of:
a device for exact positioning and reproducible dispensing of the amount of substances onto the plate,
a mechanical device to move the plate or the measuring device along the x-axis or the y-axis,
a recorder and a suitable integrator or a computer,
for substances responding to UV-Vis irradiation:
a photometer with a source of light, an optical device able to generate monochromatic light
and a photo
cell of adequate sensitivity are used for the measurement of reflectance or transmittance. In the case
where fluorescence is measured, a monochromatic filter is required in addition, to select a particular
spectral region of the emitted light,
for substances containing radionuclides:
a suitable counter for radioactivity. The linearity range of the counting device is to be verified.
Method.
Developed By :
Reviewed By :
Authorized By :
Name:
Name:
Name:
Prepare the solution of the substance to be examined (test solution) as prescribed in the monograph and, if
Designation:
QA Officer
Designation:
Quality
Head to be determined
Designation:
Managing
Director
necessary, prepare
the reference
solutions of the
substance
using the
same solvent
as in
Signature:
the test solution. Apply the sameSignature:
volume of each solution to the plateSignature:
and develop.
COMPANY NAME
Substances responding to UV-Vis irradiation:
Prepare and apply not fewer than three reference solutions of the substance to be examined, the
concentrations of which span the expected value in the test solution (about 80, 100 and 120 per cent).
Spray with the prescribed reagent, if necessary, and record the reflectance, the transmittance or
fluorescence in the chromatograms obtained with the test and reference solutions. Use the measured
results for the calculation of the amount of substance in the test solution.
Substances containing radionuclides:
Prepare and apply a test solution containing about 100 per cent of the expected value. Determine the
radioactivity as a function of the path length and report the radioactivity in each resulting peak as a
percentage of the total amount of radioactivity.
Dissolve the specified quantity of the substance being examined in sufficient water to produce 10 ml or
use 10 ml of the solution prescribed in the monograph and transfer to a Nessler cylinder. Add 2 ml of a 20%
w/v solution of citric acid and 0.1 ml of mercaptoacetic acid, mix, make alkaline with 10M ammonia, dilute
to 20 ml with water and allow to stand for 5 minutes. Any pink colour produced is not more intense than
that obtained by treating 10 ml of iron standard solution (1 ppm Fe) in the same manner.
Top of Form
Bottom of Form
Top of Form
Bottom of Form
Note: The above document is prepared on the basis of 2.2.27 & Appendix. IIIA of Ph.Eur & BP
Respectively
Title
Supersedes
: LIMIT TEST FOR CALCIUM

: Nil
Issue Date
SOP No : GTP-10023
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Objective
The limit for Calcium is indicated in the individual monographs in terms of

ppm, i.e., the parts of lead, Pb, per million parts (by weight) of the substance being
examined.
SCOPE
The procedure is applicable to all Active and Inactive raw materials
APPARATUS:
Nessler cylinder
Alcoholic Calcium Standard Solution

2 M Acetic Acid
Ammonium Oxalate
Distilled Water
REAGENTS:
PROCEDURE:
The solutions used for this test should be prepared with Distilled Water.
Developed By :
Reviewed By :
Authorized By :
To 0.2 ml of Alcoholic Calcium Standard
ml of Ammonium Oxalate Solution.
Name:
Name: Solution (100 ppm Ca) add 1Name:
Designation:
Signature:
Signature:
Quality Head
Designation:
Managing Director
After 1 minute add a mixture of 1 ml of 2M Acetic Acid and 15 ml of a solution containing the prescribed
Signature:
quantity of the substance being examined and shake. After 15 minutes any opalescence produced is not
COMPANY NAME
more intense than that of a standard prepared in the same manner using a mixture of 10 ml of Calcium
Standard Solution (10 ppm Ca) and 5 ml of Water in place of the solution of the substance being examined.
Note: The above document is prepared on the basis of Appendix VII / method 2.4.3 of BP / Ph. Eur.
Title
Supersedes
: DETREMINATION OF pH
: Nil
Issue Date
SOP No : GTP-10024
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 2
Objective
To lay down a procedure of determination of pH in the raw materials.
SCOPE
The procedure is applicable to all active raw materials, inactive raw materials,
in-process and finished products.
APPARATUS
pH meter
Analytical Balance
Beakers
Graduated pipette
Potassium chloride
REAGENTS
: AR grade
PROCEDURE
Operate the pH meter as per the SOP
Check whether pH meter is calibrated or not. If not calibrate it.
All measurements should be made at the same temperature of 23C to 25C unless otherwise specified in
the monograph.
Immerse the electrodes in the solution being examined and measure the pH at the same temperature as
for theDeveloped
buffer solutions.
By :
Reviewed By :
Authorized By :
Name:
Name:
Name:
All solutions QA
andOfficer
suspensions ofDesignation:
substances being
examined
reference buffer Managing
solutions must
be
Designation:
Quality
Head and theDesignation:
Director
prepared
using
carbon
dioxide-free
water.
Signature:
Signature:
Signature:
COMPANY NAME
When measuring pH values above 10.0, ensure that the glass electrode is suitable for use under alkaline
conditions and apply any correction that is necessary.
For monographs other than those from the European Pharmacopoeia and USP, record the pH of the
solution used to standardise the meter and electrodes at the end of a set of measurements. If the
difference between this reading and the original value is greater than 0.05, the set of measurements must
be repeated.
Weigh accurately the substance as given in individual test procedure and transfer it into a clean beaker,
add specified quantity of purified water / solvent, dissolve the substance completely or prepare the sample
solution / suspension as mentioned in the test procedure.
Title
Supersedes
: DETREMINATION OF pH
: Nil
Issue Date
SOP No : GTP-10024
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
2 of 2
Wash the electrode with purified water and blot it with tissue paper.
Determine the pH to the nearest 0.1 unit and record the reading in the worksheet.
NOTE:
In case of measurement of pH of water sample, add 0.3 ml of saturated potassium chloride solution for
every 100 ml of sample under test and measure the pH.
The above document has been prepared on the basis of Appendix V L/ method 2.2.3 and <791> of BP/ Ph.
Eur. and USP.
END OF THE DOCUMENT
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: DETREMINATION OF OXIDISING SUBSTANCES

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10025
Effective date
10/04/2010
April 2012
Page number
1 of 1
Objective
To lay down a procedure of determination of oxidizing substance in the raw

materials.
SCOPE
The procedure is applicable to all Active and inactive raw materials
APPARATUS:
Conical Flask
Centrifuge Tube
Potassium Iodide
0.002 M sodium Thiosulphate
Glacial Acetic Acid
Water
REAGENTS
PROCEDURE
Transfer 4.0 g to a glass-stopper, 125 ml conical flask and add 50.0 ml of Water. Insert the stopper and
swirl for 5 min. Transfer to a glass-stopper 50 ml centrifuge tube and centrifuge. Transfer 30.0 ml of the
clear supernatant liquid to a glass-stopper 125 ml conical flask. Add 1 ml of Glacial Acetic Acid and 0.5 g to
1.0 g of Potassium Iodide. Insert the stopper, swirl, and allow standing for 25 min to 30 min in the dark. Add
1 ml of Starch Solution and titrate with 0.002 M Sodium Thiosulphate until the starch-iodine colour
disappears. Carry out a blank determination. Not more than 1.4 ml of 0.002 M Sodium Thiosulphate is
required (0.002 per cent, calculated as H2O2).
1 ml of 0.002 M Sodium Thiosulphate is equivalent to 34 g of Oxidizing Substances, calculated as
hydrogen peroxide.
Note: The above document is prepared on the basis of Appendix X L / method 2.5.30 of BP / Ph. Eur.
Developed By :
Name:
Name:
Reviewed
:
END
OF THEBy
DOCUMENT
Designation:
Signature:
Signature:
Quality Head
Authorized By :
Name:
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: DETREMINATION OF ACID VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10026
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 1
Objective
To lay down a procedure of determination of Acid Value in the raw materials.
SCOPE
The procedure is applicable to all Active and inactive raw materials
APPARATUS :
REAGENTS
50 ml Burette (Class A)
250 ml Conical Flask
25 ml Measuring Cylinder
Ethanol (96%)
Ether
0.1 M Potassium Hydroxide
Phenolphthalein Solution
: AR grade
: AR grade
: AR grade
: AR grade
PROCEDURE:
Acid Value: The acid value is the number that expresses in milligrams the quantity of Potassium Hydroxide
required to neutralize the free acids present in 1 g of the substance.
Unless otherwise specified in the monograph weigh 10 g of the substance being examined and add 50 ml
of a mixture of equal volumes of Ethanol (96%) and Ether that has been neutralised with 0.1M Potassium
Hydroxide VS using 0.5 ml of Phenolphthalein Solution as indicator. When the substance has completely
dissolved, titrate with 0.1M Potassium Hydroxide VS, shaking constantly until a pink colour that persists for
at least 15 seconds is produced.
Calculate the Acid Value from the following expression,
5.610 x v x M
= ---------------------------0.1 x w
Where,
v = Volume, in ml, of Potassium Hydroxide solution required
w = Weight, in g, of substance taken.
M = Molarity of 0.1 M Potassium Hydroxide.
Note: The above document is prepared on the basis of Appendix X B / method 2.5.1 of BP / Ph. Eur.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: FRIABILITY
: Nil
Issue Date
SOP No : GTP-10027
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 2
Objective
To lay down a procedure of determination of friability in the tablets.
SCOPE
This procedure is applicable to all In-process and Finished Products of tablets.
APPARATUS
Friability test apparatus
PROCEDURE
For tablets weighing up to 0.65 g each, take a sample of twenty tablets; for tablets weighing more than 0.65
g each, take ten tablets.
Place the tablets on a sieve no. 100 and remove any loose dust with the aid of air pressure or a soft brush.
Accurately weigh the tablet sample and place the tablets in the drum.
Rotate the drum 100 times and remove the tablets.
Remove any loose dust from the tablets as before.
If no tablets are cracked, split or broken, weigh the tablets to the nearest milligram.
Generally the test is run once. If the results are doubtful or if the mass loss is greater than 1%, repeat the
test twice and determine the mean of the three tests.
A maximum loss of 1% of the mass of the tablets tested is considered to be acceptable for most products.
For tablets having a diameter of 13 mm or greater, problems of reproducibility may be encountered due to
frequent irregular tumbling.
In such cases, adjust the drum so that the tablets may fall freely and do not bind together when lying next
to each other, adjusting the drum so that the axis forms a 10 angle with the base is usually satisfactory.
The friability is expressed as the loss of mass and it is calculated as a percentage of the initial mass.
Indicate the number of tablets used.
Title
: FRIABILITY
Supersedes
Nil :
Issue Date
10/04/2010
Developed :By
Reviewed By
:
10/04/2010
Name:
Name:
SOP No : GTP-10027
Effective date Quality Head
Designation:
QA Officer
Designation:
Signature:
Signature:
ReviewAuthorized
date
April: 2012
By
Name:
Page number Managing

2 of Director
2
Designation:
Signature:
COMPANY NAME
Calculations:
Weight of tablets before rotation
W1
Weight of tablets after rotation
W2
Friability
(W1 W2)
---------------------------W1
x 100
Note: The above document has been prepared on the basis of <1216> and Appendix XVII G/ method
2.9.7 of USP and BP/ Ph. Eur.
END OF THE DOCUMENT
Title
Supersedes
: BULK DENSITY AND TAPPED DENSITY

: Nil
Issue Date
10/04/2010
SOP No : GTP-10028
Objective
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 5
To lay down a procedure of determination of bulk density of powder.
Developed
: procedure is applicable
Reviewed
:
Byin:process
SCOPE
: By The
to By
all Active
and inactive rawAuthorized
materials and
Name:
Name:
Name:
and finished products.
Designation:
Signature:
APPARATUS
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10028
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 5
PROCEDURE
The apparatus consists of the following:
(a)
A settling apparatus capable of producing in 1 min 250 15 taps from a height of 3 0.2 mm. The
support for the graduated cylinder, with its holder, has a mass of 450 5 g;
(b)
250 ml graduated
withBy
a mass
of 220 40 g. Authorized By :
Developed
By : cylinder (2 ml intervals)
Reviewed
:
Name:
Name:
Name:
Method:
Designation:
QA Officer
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Into the dry cylinder, introduce without compacting 100.0 g (m g) of the substance to be examined. If this is
not possible, select a test sample with an apparent volume between 50 ml and 250 ml and specify the
mass in the expression of results. Secure the cylinder in its holder. Read the unsettled Apparent Volume V0
to the nearest milliliter. Carry out 10, 500 and 1250 taps and read the corresponding volumes V10, V500
and V1250, to the nearest millilitre. If the difference between V500 and V1250 is greater than 2 ml, carry
out another 1250 taps.
Expression of the results:
Apparent Density / Bulk Density (Before settling)
= m / V0 (g / ml)
Tapped Density
= m / V1250 (or) m / V2500 (g / ml)
(After settling)
Where,
m
V0
V1250
=
=
=
Weight of the substance to be examined .

Bulk volume before settling
Apparent volume after settling (or) V2500
Bulk Density is determined by measuring the volume of a known mass of powder sample that has been
passed through a screen into graduated cylinder (Method I) or through a volume-measuring apparatus into
a cup (Method II).
Method I Measuring in a Graduated Cylinder
Procedure:
Unless otherwise specified, pass a quantity of material sufficient to complete the test
through 1.00 mm screen (No. 18) to break up agglomerates that may have formed during
stored into a dry 250 ml cylinder introduce, without compacting, approximately 100 g of test
sample, M, weighed with 0.1 % accuracy. If it is not possible to use 100 g, the amount
of the test sample and the volume of the cylinder may be modified and the test conditions
specified with the results. Select a sample mass having an untapped apparent volume of
150 to 250 ml. A 100 ml cylinder is used for apparent volumes between 50 ml and 100 ml.
Carefully level the powder without
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10028
M Vo -
Effective date
10/04/2010
Review date
April 2012
Page number
3 of 5
Weight of sample taken in g compacting, if necessary, and read the unsettled apparent volume,
to the nearest graduated unit.
Calculate the bulk density, in g per ml, by the formula:

M
---Vo
Where,
Vo - Apparent Volume
Developed
:
Reviewed
Bydetermination
:
Authorized By :
Generally
replicateBy
determinations
are desirable
for the
of this property.
Name:
Name:
Name:
Designation:
Officer
Method II QA
Measurement
in a Designation:
Volumeter
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Allow an excess of powder to flow through the apparatus into the sample receiving cup until it overflows,
using a minimum of 25 cm3 of powder with the square cup and 35 cm3 of powder with the cylindrical cup.
Carefully scrape excess powder from the top of the cup by smoothly moving the edge of the blade of a
spatula perpendicular to and in contact with the top surface of the cup, taking care to keep the spatula
perpendicular to prevent packing or removal of powder from the cup. Remove any material from the sides
of the cup, and determine the weight, M, of the powder to the nearest 0.1 %.
Calculate the bulk density, in g per ml, by the formula:
M
---Vo
Where,
M - Weight of sample taken in g
Vo - Volume of the cup in ml.
Generally replicate determinations are desirable for the determination of this property.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10028
Effective date
10/04/2010
Review date
April 2012
Page number
4 of 5
Tapped Density
Tapped Density is achieved by mechanically tapping a measuring cylinder containing a powder sample.
After observing the initial volume, the cylinder is mechanically tapped, and volume readings are taken until
little further volume change is observed. The mechanical tapping is achieved by raising the cylinder and
allowing it to drop under its own weight a specified distance by either of two methods as described below.
Devices that rotate the cylinder during tapping may be preferred to minimize any possible separation of the
mass during tapping down.
Method I
Procedure: Unless otherwise specified, pass a quantity of material sufficient to complete the test through
1.00 mm screen (No. 18) to break up agglomerates that may have formed during storage. Into a dry 250 ml
glass graduated cylinder (readable to 2 ml) weighing 220 44gm and mounted on a holder weighing 450
10 g introduce without compacting, approximately 100 g of test sample, M, Weighed with 0.1 % accuracy.
If it is not possible, use 100 g, the amount of the test sample may be reduced and the volume of the
cylinder may be modified by using a suitable 100ml graduated cylinder (readable to 1ml) weighing 130 16
g and mounted on a holder weighing 240 12 g. The modified test conditions are specified with the results.
Carefully
level powder
if necessary
apparent volume,
Developed
By :without compacting,
Reviewed
By and
: read the unsettledAuthorized
By : V0, to the
nearest graduated unit.
Name:
Name:
Name:
Designation:
Quality Head
Designation:
Managing Director
Mechanically tap the cylinder containing

the sample by raising the cylinder
and allowing it to drop under its
Signature:
Signature:
Signature:
own weight using a suitable mechanical tapped density tester that provides a fixed drop of 14 2 mm at a
COMPANY NAME
nominal rate of 300 drops / minute. Unless otherwise specified, tap the cylinder 500 times initially and
measure the tapped volume, Va to the nearest graduated unit. Repeat the tapping an additional 750 times
and measure the tapped volume, Vb, to the nearest graduated unit (Note: fewer taps may be appropriate, if
validated, for some powders).
If the difference between two volumes is less than 2 %, Vb, in the final tapped volume, Vf. Repeat in
increments of 1250 taps, as needed, until the difference between succeeding measurements is less than 2
%.
Calculate the tapped density, in grams per ml, by the formula
M
---Vf
Where,
M - Weight of sample taken in g
Vf - final tapped volume in ml.
Generally replicate determinations are desirable for the determination of this property.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10028
Effective date
10/04/2010
Review date
April 2012
Page number
5 of 5
Method II
Proceed as directed under Method I except that a suitable mechanical tapped density tester that provides a
fixed drop of 3 mm ( 10 %) at a nominal rate of 250 drops per minute is used.
.
Note: The above document is prepared on the basis of General Chapter <616> Bulk Density and Tapped
Density of USP Appendix XVII D / method 2.9.15 of BP / Ph. Eur.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
END OF THE DOCUMENT
Title
Supersedes
: Determination Uniformity Of Weight Of Tablets and Capsules

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10029
Effective date
10/04/2010
April 2012
Page number
1 of 2
Objective
To lay down a procedure of determination of Uniformity of weight.
SCOPE
The procedure is applicable to all In process and Finished products.
APPARATUS
Analytical Balance
PROCEDURE
Tablets
Method:
Weigh individually twenty units taken at random and determine the average weight (mass).
Not more than two of the individual weights (mass) deviate from the average weight (mass) by more
than the percentage deviation shown below and none deviated by more than twice that percentage.
Pharmaceutical
form
Tablets
(Uncoated and
Film coated )
Developed By :
Name:
Average weight
% deviation
Less than 80 mg
10
More than 80 and less than 250 mg
7.5
More than 250mg
Reviewed By :
Name:
Authorized By :
Name:
Designation:
Officer
Designation:
Head
Calculate theQA
percentage
deviation
for highest Quality
individual
weight tabletDesignation:
as follows:
Signature:
Signature:
Signature:
Managing Director
COMPANY NAME
Highest individual weight of tablet in mg
------------------------------------------------------ x
Average weight of tablets in mg
Title
Supersedes
100
100
: Determination Uniformity Of Weight Of Tablets and Capsules

: Nil
Issue Date
10/04/2010
Review date
SOP No : GTP-10029
Effective date
10/04/2010
April 2012
Page number
2 of 2
Calculate the percentage deviation for lowest individual weight tablet as follows:
Lowest individual weight of tablet in mg
------------------------------------------------------ x 100
Average weight of tablets in mg
100.
Capsules:
Weigh an intact capsule. Open the capsule without losing any part of seal and remove the contents as
completely as possible. Wash shells with ether or other suitable solvent and allow stand until the Odour of
solvent is not longer perceptible; Weigh the shell, the weight (mass) of the contents is the difference
Between the weight of the intact capsule and the empty shell. Repeat the procedure with another nineteen
capsules. Determine the average weight not more than two of the individual weight deviate from the
average weight by more than the percentage deviation shown below and none deviates by more than twice
that percentage.
Pharmaceutical
form
Capsules,
Granules,
Uncoated single
dose)
Average weight
% deviation
Less than 300 mg
10
More than 300 mg
7.5
Note: The above document is prepared on the basis of Appendix XIIG / method 2.9.5 of BP / Ph. Eur.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
END OF THE DOCUMENT
Title
Supersedes
: Determination Of THICKNESS OF TABLETS

: Nil
Issue Date
10/04/2010
SOP No : GTP-10030
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 1
Objective
To lay down a procedure of determination of thickness.
SCOPE
This procedure is applicable to all In-process and Finished Products.
APPARATUS
Vernier Calipers
PROCEDURE
Ensure the instrument /Vernier Calipers is clean and calibrated.
Switch on the instrument using green button.
Bring the jaws together so that their is no gap/they touch each other.
Then set for 0.00mm using yellow (Zero) button .
Keep the sample to be tested between the jaws and hold it tightly. Then note down the reading shown in
display.
Perform the test for 10 tablets to measure thickness for circular/Caplet shaped tablets and also to measure
the length and breadth of capsules.
Report the range of the measurement observed.
Switch off the equipment and clean it with dry cloth.
The acceptance limits are given Master Formula record.
END OF THE DOCUMENT
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: Determination Of HARDNESS
: Nil
Issue Date
SOP No : GTP-10031
Effective date
10/04/2010
Review date
April 2012
10/04/2010
Page number
1 of 1
Objective
To lay down a procedure of determination of Hardness of tablet.
SCOPE
APPARATUS
Hardness Tester
PROCEDURE
Ensure that Hardness tester is clean and calibrated.
Keep the tablet to be tested in vertical position in between the upper plunger and the jackscrew.
Turn the Knurled wheel so that the tablet is just held in between the plunger and the jackscrew.
Apply pressure with the help of handle liver by raising the handle lever up and down until the tablet breaks.
Note down the reading.
Perform the test for 10 tablets to measure the hardness.
Report the range observed.
END OF THE DOCUMENT
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes
: Determination Of CONDUCTIVITY
: Nil
Issue Date
10/04/2010
SOP No : GTP-10032
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 3
Objective
To lay down a procedure of determination of Conductivity.
SCOPE
This procedure is applicable to all Active Material and Inactive Material.
APPARATUS:
Conductivity Meter
Conductivity Cell
Potassium Chloride
Carbon Dioxide free Water prepared from Distilled Water.
REAGENTS:
PROCEDURE:
The conductivity of a solution () is, by definition, the reciprocal of resistivity (). Resistivity is defined as the
quotient of the electric field and the density of the current. The resistance R () of a conductor of crosssection S (cm2) and length L (cm) is given by the expression:
The unit of conductivity in the International System is the siemens per meter (Sm1). In practice, the
electrical conductivity of a solution is expressed in siemens per centimeter (Scm1) or in micro siemens
per centimetre (Scm1). The unit of resistivity in the International System is the ohm-meter (m).
The resistivity of a solution is generally expressed in ohm-centimeters (cm). Unless otherwise
prescribed, the reference temperature for the expression of conductivity or resistivity is 20 C.
Apparatus:
The apparatus used (conductivity meter or resistivity meter) measures the resistance of the column of
liquid between the electrodes of the immersed measuring device (conductivity cell). The apparatus is
supplied with alternating current to avoid the effects of electrode polarization. It is equipped with a
temperature compensation device or a precision thermometer.
The conductivity cell contains two parallel platinum electrodes coated with platinum black, each with a
surface area S, and separated from the other by a distance L. Both are generally protected by a glass tube
that allows good exchange between the solution and the electrodes.
:
Reviewed By :
TitleDeveloped: By
Determination
Of CONDUCTIVITY
Supersedes
: Nil
Issue Date
10/04/2010
Name:
Name:
Designation:
SOP No : GTP-10032
Signature:
Effective date
Signature:
Quality10/04/2010
Head
Authorized By :
Review date
April 2012
Name:
Designation:
Page number
Signature:
Managing Director
2 of 3
COMPANY NAME
The cell constant C of the conductivity cell is given in cm1 according to the equation:
a dimensionless numerical coefficient, which is characteristic of the cell design.
Reagents:
Prepare three standard solutions of Potassium Chloride containing 0.7455 g, 0.0746 g and 0.0149 g,
respectively, of Potassium Chloride per 1000.0 g of solution, using Carbon Dioxide-free Water, prepared
from Distilled Water whose conductivity does not exceed 2 Scm1.The conductivity and resistivity of
these three solutions at 20 C are given below:
Conductivity and resistivity of Potassium Chloride solutions:
Concentration in g
per 1000.0 g of
Solution
0.7455
0.0746
0.0149
Conductivity
Scm1
Resistivity
cm
1330
133.0
26.6
752
7519
37594
If the determination cannot be made at the temperature of 20 C, use the following equation to correct the
conductivity of the potassium chloride solutions indicated in the table. This equation is valid only for
temperatures in the range 20 5 C.
Where,
T
=
CT
=
C20 =
Measurement temperature prescribed in the monograph

Conductivity of the solution at T C
Conductivity of the solution at 20 C.
Operating Procedure
Determination of the cell constant:
Choose a conductivity cell that is appropriate for the conductivity of the solution to be examined. The higher
the expected conductivity, the higher the cell constant that must be chosen (low ) so that the
value measured is as large as possible for the apparatus used. Commonly used conductivity cells have cell
constants of the order of 0.1 cm1, 1 cm1 and 10 cm1. Use a standard solution of potassium chloride
that is appropriate for the measurement.
Title
Supersedes
: Determination Of CONDUCTIVITY
: Nil
Issue Date
10/04/2010
SOP No : GTP-10032
Effective date
10/04/2010
Review date
April 2012
Page number
3 of 3
Rinse the cell several times with carbon dioxide-free water prepared from distilled water and at least twice
Developed By :
Reviewed By :
Authorized By :
with the Potassium Chloride Solution used for the determination of the cell constant of the conductivity cell.
Name:
Name:
Name:
Measure the resistance of the conductivity cell using the Potassium Chloride Solution at 20 0.1 C or at
Designation:
Managing Director
the temperature prescribed in the
monograph. The constant C (in cm1)
of the conductivity
cell is given by
Signature:
Signature:
Signature:
the expression:
COMPANY NAME
C
RKCl =
kKCl =
RKCl -
kKCl
Measured resistance, expressed in mega-ohms

Conductivity of the standard solution of Potassium Chloride used, expressed in Scm1.
The measured constant C of the conductivity cell must be within 5 per cent of the given value.
Determination of the conductivity of the solution to be examined.
After calibrating the apparatus with one of the standard solutions, rinse the conductivity cell several times
with Carbon Dioxide-Free Water prepared from Distilled Water and at least twice with the aqueous solution
to be examined at 20 0.1 C or at the temperature prescribed in the monograph. Carry out successive
measurements as described in the monograph.
Note: The above document is prepared on the basis of Appendix V.O / method 2.2.38 of BP / Ph. Eur.
Title
Supersedes
: Determination Of HYDROXYL VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10033
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 3
Objective
To lay down a procedure of determination of Hydroxyl Value.
SCOPE
This procedure is applicable to all Active Material and Inactive Material.
APPARATUS:
Developed
By : Cylinder
Reviewed By :
Nessler
Name:
Name:
Name:
Designation:
REAGENTS:QA Officer
Designation:
Signature:
Designation:
Signature:
Quality Head
Authorized By :
Signature:
Managing Director
COMPANY NAME
Acetic Anhydride
Anhydrous Pyridine
Potassium Hydroxide
Aldehyde free Ethanol (96%)
Propionic Anhydride Reagent
Aniline
Cyclohexane
Glacial Acetic Acid
Perchloric Acid
Crystal Violet Solution
Water
Acetic Anhydride Solution :

Dissolve 25 ml of Acetic Anhydride in Anhydrous Pyridine and dilute to 100 ml
with Anhydrous Pyridine.
0.5M Ethanolic Potassium Hydroxide:
Dissolve 3 g of Potassium Hydroxide in 5 ml of water and add sufficient
Aldehyde-free Ethanol (96%) to produce 100 ml. Allow the solution to stand
for 24 hours and decant the clear solution.
PROCEDURE:
The hydroxyl value of a substance is the number of mg of Potassium Hydroxide required to neutralize the
acid combined by acylation in 1 g of the substance.
Use Method A unless otherwise specified in the monograph.
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10033
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 3
Method A:
Unless otherwise specified in the monograph place the quantity of the substance being examined
prescribed in the Table 1 in a 150-ml acetylation flask fitted with an air condenser and add the
corresponding volume of Acetic Anhydride Solution. Heat for 1 hour in a water-bath, maintaining the level of
the water about 2.5 cm above the level of the liquid in the flask throughout. Remove the flask and
condenser, allow cooling and adding 5 ml of water through the top of the condenser; if this causes
cloudiness, and add sufficient pyridine to produce a clear liquid, recording the volume added. Shake the
flask, replace in the water-bath for 10 minutes, remove and allow cooling. Rinse the condenser and the
walls of the flask with 5 ml of ethanol (96%), previously neutralised to phenolphthalein solution. Titrate with
0.5M Developed
Ethanolic Potassium
using 0.2 mlBy
of phenolphthalein
solution
as indicator.
the
By : Hydroxide VS Reviewed
:
Authorized
ByRepeat
:
operation without the substanceName:
being examined.
Name:
Name:
Designation:
Quality Head
Calculate the hydroxyl value from

the expression,
Signature:
Signature:
Designation:
Signature:
Managing Director
COMPANY NAME
a + 28.05 v / w
Where,
v is the difference, in ml, between the titrations,
a is the acid value and
w is the weight, in g, of the substance taken.
Table 1
Presumed Hydroxyl
value
10 to 100
100 to 150
150 to 200
200 to 250
250 to 300
300 to 350
350 to 700
700 to 950
Title
Supersedes
Quantity of Substance
(g)
2.0
1.5
1.0
0.75
0.60 or 1.20
1.0
0.75
0.5

: Nil
Issue Date
10/04/2010
SOP No : GTP-10033
Effective date
10/04/2010
Volume of Acetic
Anhydride solution (ml)
5.0
5.0
5.0
5.0
5.0 or 10.0
10.0
15.0
15.0
Review date
April 2012
Page number
3 of 3
Method B:
To the specified quantity of the substance being examined in a perfectly dry 5-ml conical flask add 2 ml of
Propionic Anhydride Reagent, close the flask with a ground-glass or suitable plastic stopper and shake
gently to dissolve the substance. Allow to stand for 2 hours, unless otherwise prescribed, remove the
stopper and transfer the flask and its contents to a 500-ml wide-necked conical flask containing 25.0 ml of
a 0.9% w/v solution of Aniline in Cyclohexane and 30 ml of Glacial Acetic Acid, swirl, allow to stand for 5
minutes and titrate with 0.1M Perchloric Acid VS, using 0.05 ml of Crystal Violet Solution as indicator, until
the solution is emerald green. Repeat the operation without the substance being examined.
Calculation:
Calculate the hydroxyl value from the expression.
=
5.610 V M
-----------------------0.1 W By :
Developed
Name:
Where,
Designation:
QA Officer
Signature:
V
W
=
=
Reviewed By :
Name:
Designation:
Authorized By :
Name:
Quality Head
Designation:
difference,
in ml, between the titrations Signature:
Signature:
weight, in g, of substance taken.
Managing Director
COMPANY NAME
M
Molarity of 0.1 M Potassium Hydroxide.
Determine the water content (A %) of the substance, and calculate the corrected hydroxyl value from the
following expression,
Corrected Hydroxyl Value
Hydroxyl value
31.1 A
Note: The above document is prepared on the basis of Appendix X.D / method 2.5.3 of BP / Ph. Eur.
Title
Supersedes
: Determination Of Disintegration time

: Nil
Issue Date
10/04/2010
SOP No : GTP-10034
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
Objective
To lay down a procedure of determination of Disintegration time.
SCOPE
This procedure is applicable to all In-process and Finished Products of tablets and
capsules and empty hard gelatin capsules.
APPARATUS
REAGENTS
Disintegration test apparatus.
Not applicable
PROCEDURE
Fill the beaker with specified liquid such that at the highest point of the upward stroke the wire mesh
remains at least 2.5 cm below the surface of the liquid and descends to not less than 2.5 cm from the
bottom of the vessel on the downward stroke.
For Uncoated tablets, Plain coated tablets and Hard gelatin capsules:
Place 1 tablet or capsule in each of the six tubes of the basket.
If prescribed in the appropriate general monograph, add a disc to each tube.
Developed By :
Reviewed By :
Authorized By :
Name:
Name:
Name:
Operate the apparatus, using water maintained at 37C 2C as the immersion fluid unless otherwise
Designation:
QA individual
Officer
Designation:
specified in the
monograph.
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
At the end of the time limit specified in the monograph, lift the basket form the fluid, and observe the tablets
or capsules.
Tablets pass the test if all have disintegrated. Capsules pass the test if all have disintegrated except for
fragments of the capsule shells.
If 1 or 2 tablets or capsules fail to disintegrate completely, repeat the test on 12 additional numbers.
Not less than 16 of the total of 18 numbers tested disintegrate completely.
Title
Supersedes
: Determination Of Disintegration time

: Nil
Issue Date
10/04/2010
SOP No : GTP-10034
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
For Delayed-release (enteric coated) Tablets:

Place 1 tablet in each of the six tubes of the basket and, if the tablet has a soluble external coating,
immerse the basket in water at room temperature for 5 minutes.
Operate the apparatus, using simulated gastric fluid TS maintained at 37C 2C as the immersion fluid.
After 1 hour of operation in simulated gastric fluid TS, lift the basket form the fluid, and observe the tablets.
The tablets show no evidence of disintegration, cracking, or softening.
Operate the apparatus, using simulated intestinal fluid TS maintained at 37C 2C as the immersion fluid,
for the time specified in the monograph.
Lift the basket from the fluid, and observe the tablets.
The tablets pass the test if all have disintegrated completely.
If 1 or 2 tablets fail to disintegrate completely, repeat the test on 12 additional tablets.
Not less than 16 of the total of 18 tablets tested disintegrate completely.
For Empty hard gelatin capsules:
Place 1 capsule in each of the six tubes of the basket.
Operate the apparatus, using water maintained at 37C 2C as the immersion fluid.
At the end of 15 minutes lift the basket form the fluid, and observe the capsules.
Developed
Reviewed By :
The capsules
passBy
the:test if all have disintegrated.
Name:
Name:
Authorized By :
Name:
Designation:
QAto
Officer
Designation:
Quality
Head
Designation:
If capsules fail
disintegrate completely,
repeat
the test
on 12 additional
numbers.
Signature:
Signature:
Signature:
Managing Director
COMPANY NAME
Not less than 16 of the total of 18 numbers tested disintegrate completely.
Note: The above document has been prepared on the basis of <721> and Appendix XII A/ method 2.9.1 of
USP and BP/ Ph. Eur.
END OF THE DOCUMENT
Title
Supersedes
: Determination of IODINE VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10035
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 4
Objective
To lay down a procedure of determination of Iodine Value.
SCOPE
This procedure is applicable to all Active Material and Inactive Materials.
APPARATUS
250 ml Iodimetirc flask

Burette
M Sodium Thiosulphate
Glacial Acetic Acid
Chloroform
Potassium Iodide
Iodine Bromide Solution
Cyclohexane
Starch
Dichloromethane
Iodine Monochloride Solution
Water
REAGENTS
PROCEDURE
The iodine value II is the number that expresses in grams the quantity of halogen, calculated as Iodine that
can be fixed in the prescribed conditions by 100 g of the substance.
When the monograph does not specify the method to be used, method A is applied. Any change from
method A to method B is validated.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10035
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 4
METHOD A: (BP & Ph. Eur. Method)

Unless otherwise prescribed, use the following quantities of samples as per below table for the
determination.
Presumed Value (II)
Quantity of Sample (g)
Less than 20
1.0
20 60
0.5 0.25
60 100
0.25 0.15
More than 100
0.15 0.10
Introduce the prescribed quantity of the substance to be examined (m g) into a 250 ml flask fitted with a
ground-glass stopper and previously dried or rinsed with Glacial Acetic Acid, and dissolve it in 15 ml of
Chloroform unless otherwise prescribed. Add very slowly 25.0 ml of Iodine Bromide Solution. Close the
flask and keep it in the dark for 30 min unless otherwise prescribed, shaking frequently. Add 10 ml of a 100
g / l solution of Potassium Iodide and 100 ml of water. Titrate with 0.1 M Sodium Thiosulphate, shaking
vigorously until the yellow colour is almost discharged. Add 5 ml of Starch Solution and continue the
titration adding the 0.1 M Sodium Thiosulphate dropwise until the colour is discharged (n1 ml of 0.1 M
Sodium Thiosulphate). Carry out a blank test under the same conditions (n2 ml of 0.1 M Sodium
Thiosulphate).
Calculate the Iodine value by following expressions,
Iodine Value (II)
1.269 (n2 - n1)

------------------------m
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10035
Effective date
10/04/2010
Review date
April 2012
Page number
3 of 4
METHOD B: (BP & Ph. Eur. Method)

Unless otherwise prescribed, use the following quantities as per below Table for the determination.
<3
Mass (g)
(Corresponding to an
excess of 150 per cent
ICl)
10
10
Iodine
chloride
solution
(ml)
25
8.4613
10.5760
25
5.0770
6.3460
25
10
2.5384
3.1730
20
20
0.8461
1.5865
20
40
0.6346
0.7935
20
60
0.4321
0.5288
20
80
0.3173
0.3966
20
100
0.2538
0.3173
20
120
0.2115
0.2644
20
140
0.1813
0.2266
20
160
0.1587
0.1983
20
180
0.1410
0.1762
20
200
0.1269
0.1586
20
Presumed
value
(II)
Mass (g)
(Corresponding to an
excess of 100 per cent ICl)
The mass of the sample is such that there will be an excess of Iodine Chloride Solution of 50 % to 60 % of
the amount added, i.e. 100 % to 150 % of the amount absorbed.
Introduce the prescribed quantity of the substance to be examined (m g) into a 250 ml flask fitted with a
ground-glass stopper and previously rinsed with Glacial Acetic Acid or dried, and dissolve it in 15 ml of a
mixture of equal volumes of Cyclohexane and Glacial Acetic Acid, unless otherwise prescribed. If
necessary, melt the substance before dissolution (melting point greater than 50 C). Add very slowly the
volume of Iodine Chloride Solution stated in Table -2. Close the flask and keep it in the dark for 30 min,
By :
Reviewed
: of a 100 g / l solution
Authorized
ByIodide
:
unlessDeveloped
otherwise prescribed,
shaking frequently.
Add By
10 ml
of Potassium
and
Name:
Name:
Name:
100 ml of Water.
Designation:
QA Officer
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Title
Supersedes

: Nil
Issue Date
10/04/2010
SOP No : GTP-10035
Effective date
10/04/2010
Review date
April 2012
Page number
4 of 4
Titrate with 0.1 M Sodium Thiosulphate, shaking vigorously until the yellow colour is almost discharged.
Add 5 ml of Starch Solution and continue the titration adding the 0.1 M Sodium Thiosulphate dropwise until
the colour is discharged (n1 ml of 0.1 M Sodium Thiosulphate). Carry out a blank test under the same
conditions (n2 ml of 0.1 M Sodium Thiosulphate).
Calculate the Iodine value by following expressions,
1.269 (n2 - n1)
Iodine Value (II) = -----------------------m
IODINE MONOCHLORIDE METHOD: (BP Method)
When the use of iodine flasks is prescribed, use flasks with a nominal capacity of 250 ml and complying
with British Standard 2735:1956 (Specification for iodine flasks), unless otherwise specified.
Dissolve the specified quantity of the substance being examined in 10 ml of Dichloromethane in a dry
iodine flask. Add 20 ml of Iodine Monochloride solution, insert the stopper, previously moistened with Dilute
Potassium Iodide Solution, and allow to stand in the dark at 15 to 25 for 30 minutes. Place 15 ml of Dilute
Potassium Iodide Solution in the top cup, carefully remove the stopper, rinse the stopper and the sides of
the flask with 100 ml of Water, shake and titrate with 0.1M Sodium Thiosulphate VS using Starch Mucilage,
added towards the end of the titration, as indicator. At the same time carry out the operation in exactly the
same manner, but without the substance being examined.
Calculate the Iodine Value from the expression given below.
Iodine Value (II) =
1.269 x V
-----------------------M
Where,
V
W
=
=
The difference, in ml, between the titrations

The weight, in g, of the substance taken.
The approximate weight, in g, of the substance to be taken may be calculated by dividing 20 by the highest
expected Iodine Value. If more than half of the available halogen is absorbed, the test must be repeated,
using a smaller quantity of the substance.
Note: The above document is prepared on the basis of General Chapter X.E / 2.5.4 of BP & Ph.Eur
respectively.
END OF THE DOCUMENT
Title
: Determination of SAPONIFICATION VALUE
Supersedes
Nil :
Issue Date
10/04/2010
Developed :By
Reviewed By
:
10/04/2010
Name:
Name:
SOP No : QA
GTP-10036
Effective date Quality Head
Designation:
Officer
Designation:
Signature:
Objective
Signature:
ReviewAuthorized
date
April: 2012
By
Name:
Page number Managing

1 of Director
2
Designation:
Signature:
To lay down a procedure of determination of Saponification Value.
COMPANY NAME
SCOPE
APPARATUS
Burette
200-ml flask
250 ml borosilicate glass flask
Reflux condenser
Potassium Hydroxide
Ethanol (96%)
0.5M Hydrochloric Acid
Water
REAGENTS
PROCEDURE
The Saponification Value IS, is the number of mg of Potassium Hydroxide required to neutralise the free
acids and to saponify the esters in 1 g of the substance.
Use Method I unless otherwise specified in the monograph.
Method I (BP Method):
Dissolve 35 to 40 g of Potassium Hydroxide in 20 ml of Water and add sufficient Ethanol (96%) to produce
1000 ml. Allow to stand overnight and pour off the clear liquid.
Weigh 2 g of the substance into a 200-ml flask; add 25 ml of the Ethanolic solution of Potassium Hydroxide
and boil under a reflux condenser for 1 hour, rotating the contents frequently. While the solution is still hot,
titrate the excess of alkali with 0.5M Hydrochloric Acid VS using 1 ml of Phenolphthalein Solution as
indicator. Repeat the operation without the substance being examined.
Title
Supersedes
: Determination of SAPONIFICATION VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10036
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
Calculate
the Saponification
Value from
the following
Developed
By :
Reviewed
By : expression,
Authorized By :
28.05 x V
Name:
Name:
Name:
IS
=
Designation:
QA Officer
Signature:
Where,
-----------------Designation:
Quality Head
W
Signature:
Designation:
Signature:
Managing Director
COMPANY NAME
V
W
=
=
Difference, in ml, between the titrations

Weight, in g, of substance taken.
Method II (BP / Ph.Eur. Method)

Unless otherwise prescribed, use the quantities indicated in the following table for the determination.
Presumed Value IS
Qty. of Sample (g)
3 to 10
10 to 40
40 to 60
60 to 100
100 to 200
200 to 300
300 to 400
12 to 15
8 to 12
5 to 8
3 to 5
2.5 to 3
1 to 2
0.5 to 1
Introduce the prescribed quantity of the substance being examined (m g) into a 250-ml borosilicate glass
flask fitted with a reflux condenser. Add 25.0 ml of 0.5M Alcoholic Potassium Hydroxide and a few glass
beads. Attach the condenser and heat under a reflux condenser for 30 minutes, unless otherwise
prescribed. Add 1 ml of Phenolphthalein Solution and titrate immediately (while still hot) with 0.5M
Hydrochloric Acid VS (n1 ml of 0.5M Hydrochloric Acid). Carry out a blank test under the same conditions
(n2 ml of 0.5M Hydrochloric Acid).
IS
28.05 (n2 n1)

----------------------m
Note: The above document is prepared on the basis of General Chapter X.G / 2.5.6 of BP / Ph.Eur
respectively.
END OF THE DOCUMENT
Title
Supersedes
: Determination of ACID VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10037
Effective date
10/04/2010
Review date
April 2012
Page number
1 of 2
Objective
To lay down a procedure of determination of Acid Value.
SCOPE
APPARATUS
Burette
Developed By :
Reviewed By :
250 ml Conical flask
Name:
Name:
Name:
Designation:
Signature:
REAGENTS
Reflux condenser
Designation:
Signature:
Quality Head
Authorized By :
Signature:
Managing Director
COMPANY NAME
Alcohol
Ether
0.1N Sodium Hydroxide
Water
PROCEDURE
The acidity of fats and fixed oils may be expressed as the number of ml of 0.1N Alkali required to neutralize
the free acids in 10.0g of substance. Acidity is frequently expressed as the Acid value, which is the number
of mg of Potassium Hydroxide required to neutralize the free acids in 1.0 g of the substance.
Procedure :
Unless otherwise directed, dissolve about 10.0 g of the substance, accurately weighed, in 50 ml of a
mixture of equal volumes of Alcohol and Ether (which has been neutralized to Phenolphthalein with 0.1N
Sodium Hydroxide) contained in a flask. If the test specimen does not dissolve in the cold solvent, connect
the flask with a suitable condenser and warm slowly, with frequent shaking, until the specimen dissolves.
Add 1 ml of Phenolphthalein, and titrate with 0.1N Sodium Hydroxide VS until the solution remains faintly
pink after shaking for 30 seconds. Calculate either the Acid value or the volume of 0.1N Alkali required to
neutralize 10.0 g of specimen (free fatty acids), whichever is appropriate.
Title
Supersedes
: Determination of ACID VALUE

: Nil
Issue Date
10/04/2010
SOP No : GTP-10037
Effective date
10/04/2010
Review date
April 2012
Page number
2 of 2
If the volume of 0.1N Sodium Hydroxide VS required for the titration is less than 2 ml, a more dilute titrant
may be used, or the sample size may be adjusted accordingly. The results may be expressed in terms of
the volume of titrant used or in terms of the equivalent volume of 0.1N Sodium Hydroxide.
If the oil has been saturated with carbon dioxide for the purpose of preservation, gently reflux the alcoholether solution for 10 minutes before titration. The oil may be freed from Carbondioxide also by exposing it
in a shallow dish in a vaccum desicator for 24 hours before weighing the test specimens.
By :
Reviewed
:
Authorized
By :
Note:Developed
The above document
is prepared on
the basis By
of General
Chapter <401>
of USP.
Name:
Name:
Name:
Designation:
Signature:
Signature:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
END OF THE DOCUMENT
Title
:
Supersedes
Determination of Dynamic Viscosity , Kinetic Viscosity and Apparent Viscosity

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Objective
Effective date
10/04/2010
Page number
1 of 7
To lay down a procedure of determination of Viscosity.
SCOPE
APPARATUS
As per Individual Method
REAGENTS
NA
PROCEDURE
Dynamic Viscosity or Viscosity Coefficient ():
It is the tangential force per unit surface area, known as shearing stress, , and expressed in Pascals,
necessary to move, parallel to the sliding plane, a layer of liquid of 1 square meter at a rate (v) of 1 meter
per second relative to a parallel layer at a distance (x) of 1 meter.
The ratio dv/dx is a speed gradient giving the rate of shear D expressed in reciprocal seconds
Developed By :
Dynamic Viscosity () = /D
Name:
Name:
Reviewed By :
Designation:
Signature:
milli Pascal second (mPa s).
Signature:
(s1).
Authorized By :
Name:
Quality Head
Designation:
Managing Director
The unit of Dynamic Viscosity is the Pascal second (Pa s). The most commonly used submultiples is the
Signature:
COMPANY NAME
Kinematics Viscosity ():
It is expressed in square meters per second, is obtained by dividing the dynamic viscosity, , by the
density, , expressed in kilograms per cubic meter, of the liquid measured at the same temperature.
Kinematics Viscosity() = /.
The kinematic viscosity is usually expressed in square millimetres per second.
Method I (BP Method)
The apparatus consists of a glass U-tube viscometer as shown in figure made of clear borosilicate glass
and constructed in accordance with the dimensions shown in the figure and in Table 1. The monograph
states the size of viscometer to be used.
Title
:
Supersedes

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Effective date
Developed By :
Name:
Name:
Designation:
Signature:
Signature:
10/04/2010
Page number
Reviewed By :
2 of 7
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Procedure:
Fill the viscometer with the liquid being examined through tube L to slightly above the mark G, using a long
pipette to minimise wetting the tube above the mark. Place the tube vertically in a water bath and when it
has attained the specified temperature, adjust the volume of the liquid so that the bottom of the meniscus
settles at the mark G. Suck or blow the liquid to a point about 5 mm above the mark E. After releasing
pressure or suction, measure the time taken for the bottom of the meniscus to fall from the top edge of
mark E to the top edge of mark F.
Title
:
Supersedes

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Effective date
10/04/2010
Page number
3 of 7
Table 1
Calculate the Kinematic Viscosity () in square millimetres per second (mm2 s1) from the following
expression:
= Kt
Calculate the Dynamic Viscosity () in millipascal seconds (mPa s) from the following expression:
=By
Kt
Reviewed
:
Developed By :
Where,
Name:
Name:
Designation:
t
Signature:
=
=
Authorized By :
Name:
Quality Head
Designation:
Managing Director
Time in seconds
for the meniscus to fall from ESignature:
to F,
Signature:
Mass/volume (g cm3) obtained by multiplying the relative density of the fluid
COMPANY NAME
K
being examined by 0.9982.

Constant (K) of the instrument is determined using the appropriate European
Pharmacopoeia reference liquid for viscometers.
Method II - Capillary Viscometer Method (BP & Ph.Eur Method)

The apparatus consists of a glass suspended-level viscometer as shown in Figure-2 made of clear
borosilicate glass and constructed in accordance with the dimensions shown in Table 2.
Title
:
Supersedes

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Effective date
10/04/2010
Page number
4 of 7
Procedure
Fill the viscometer through tube L with a sufficient quantity of the liquid being examined at 20 to fill bulb A
but ensuring that the level of liquid in bulb B is below the exit to ventilation tube M. After the tube has been
placed vertically in a water bath at 19.9 to 20.1 unless otherwise specified, allow it to stand for not less
than 30 minutes. Close tube M and apply suction to tube N until the liquid reaches a level about 8 mm
above mark E. Hold the liquid at this level by closing tube N and open tube M. When the liquid is clear of
the capillary end of tube N and the lower end of tube M, open tube N. Measure the time taken, to the
nearest 0.2 second, for the bottom of the meniscus to fall from the top edge of mark E to the top edge of
mark F.
The result is not valid unless two consecutive readings do not differ by more than 1%. The average of not
fewer than three readings gives the flow time of the liquid being examined.
Calculate the Kinematics Viscosity () in square millimeters per second (mm2 s1) from the following
expression:
Developed By :
Reviewed By : = Kt
Authorized By :
Name:
Name:
Name:
Designation:
Officer ViscosityDesignation:
Quality
Head (mPa s) from
Designation:
Director
Calculate theQA
Dynamic
() in milli Pascal
seconds
the followingManaging
expression:
Signature:
Signature:
= Kt
Signature:
COMPANY NAME
Where,
t
=
=
Time in seconds for the meniscus to fall from E to F,

Mass/volume (g cm3) obtained by multiplying the relative density of the fluid being
examined by 0.9982.
Constant (K) of the instrument is determined using the appropriate European
Pharmacopoeia reference liquid for viscometers.
Title
:
Supersedes

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Effective date
Page number
10/04/2010
5 of 7
Table - 2
Method III Rotating Viscometer Method - (BP & Ph.Eur Method)

Commonly used types of rotating viscometers are based on the measurement of shearing forces in a liquid
medium placed between two coaxial cylinders, one of which is driven by a motor and the other is made to
revolve by the rotation of the first. Under these conditions, the viscosity (or apparent viscosity) becomes a
measurement (M) of the angle of deflection of the cylinder made to revolve, which corresponds to a
moment of force expressed in newton metres. For laminar flow, the dynamic viscosity, , expressed in
Pascal seconds is given by the formula:
where,
= By The
in metres
revolve in the
Developed
: height of immersion
Reviewed
By :of the cylinder made to
Authorized
Byliquid
:
medium,
Name:
Name:
Name:
RA and RB
Signature:
Designation:
Quality Head
Designation:
Managing Director
The radii in
metres of the cylinders, RA being smaller
than RB , and
Signature:
Signature:
COMPANY NAME
Title
:
Supersedes
The angular velocity in radians per second.

: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10038
Effective date
10/04/2010
Page number
6 of 7
The constant k of the apparatus may be determined at various speeds of rotation using a Pharmacopoeia
viscometer calibration liquid. Commercially available apparatus is supplied with tables giving the constants
of the apparatus in relation to the surface area of the cylinders used and their speed of rotation. The
viscosity then corresponds to the formula:
= k(M/)
Procedure:
Measure the viscosity according to the instructions for the operation of the rotating viscometer. The
temperature for measuring the viscosity is indicated in the monograph. For pseudo plastic and other nonNewtonian systems, the monograph indicates the type of viscometer to be used and the angular velocity or
the shear rate at which the measurement is made. If it is impossible to obtain the indicated shear rate
exactly, use a shear rate slightly higher and a shear rate slightly lower and interpolate.
Method IV - Falling Ball Viscometer Method - (BP & Ph.Eur Method)
The determination of dynamic viscosity of Newtonian liquids using a suitable falling ball viscometer is
performed at 20 0.1C, unless otherwise prescribed in the monograph.
The time required for a test ball to fall in the liquid to be examined from one ring mark to the other is
determined. If no stricter limit is defined for the equipment used the result is valid only if 2 consecutive
measures do not differ by more than 1.5%.
The falling ball viscometer consists of a glass tube enclosed in a mantle, which allow precise control of
temperature; six balls made of glass, nickeliron or steel with different densities and diameters. The tube is
fixed in such a way that the axis is inclined by 10 1 with regard to the vertical. The tube has 2 ring marks
which define the distance the ball has to roll. Commercially available apparatus is supplied with tables
giving the constants, the density of the balls and the suitability of the different balls for the expected range
of viscosity.
Developed By :
Name:
Name:
Designation:
Title
Signature:
Supersedes
Reviewed By :
Authorized By :
Name:
Quality Head
Designation:
Managing Director

Signature:
Signature:
: Nil
Issue Date
10/04/2010
Review date
April 2012
COMPANY NAME
SOP No : GTP-10038
Effective date
10/04/2010
Page number
7 of 7
Procedure:
Fill the clean, dry tube of the viscometer, previously brought to 20 0.1C, with the liquid to be examined,
avoiding bubbles. Add the ball suitable for the range of viscosity of the liquid so as to obtain a falling time
not less than 30 seconds. Close the tube and maintain the solution at 20 0.1C for at least 15 minutes.
Let the ball run through the liquid between the 2 ring marks once without measurement. Let it run again
and measure with a stop-watch, to the nearest one-fifth of a second, the time required for the ball to roll
from the upper to the lower ring mark. Repeat the test run at least 3 times.
Calculate the dynamic viscosity in millipascal seconds using the formula:
Where
k
1
2
=
=
=
Constant, expressed in millimeter squared per second squared,

Density of the ball used, expressed in grams per cubic centimeter,
Density of the liquid to be examined, expressed in grams per cubic centimeter,
Obtained by multiplying its relative density, d2020 by 0.9982,
Falling time of the ball, in seconds.
Note: The above document is prepared on the basis of General Chapter V.H / 2.2.8, 2.2.9, 2.2.10 & 2.2.49
of BP & Ph.Eur.
Title
Supersedes
: Determination of Diameter Width and Length

: Nil
Issue Date
10/04/2010
Review date
April 2012
10/04/2010
Developed By :
Reviewed By :
Authorized By :
SOP No : GTP-10039
Effective date
Page number
1 of 1
Name:
Name:
Name:
Objective
Signature:
Designation:
Quality Head
Designation:
To lay down
a procedure of determination of length
width.
Signature:
Signature:
Managing Director
COMPANY NAME
SCOPE
APPARATUS
Vernier Calipers
REAGENTS
Not applicable.
PROCEDURE
Ensure the instrument / Vernier Calipers is clean and calibrated
Switch on the instrument using green button.
Bring the jaws together so that their is no gap/they touch each other.
Then set for 0.00mm using yellow (Zero) button .
Keep the sample to be tested between the jaws and hold it tightly. Then note down the reading shown in
display.
Perform the test for 10 tablets to measure thickness for Diameter, Width & length of tablets.
The diameter, Width & length readings shall be expressed in mm.
Report the range of the measurement observed
Switch off the equipment and clean it with dry cloth.
The acceptance limits are given Specification.
END OF THE DOCUMENT
Title
: DETERMINATION OF READILY CARBONIZABLE SUBSTANCES TEST
Supersedes
: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10040
Objective
Effective date
10/04/2010
Page number
1 of 2
To lay down a procedure of determination of Carbonizable Substance.
SCOPE:
procedure is applicable
all Active
Material and Inactive
Material.
Developed By This
:
ReviewedtoBy
:
Authorized
By :
Name:
Name:
Designation:
APPARATUS:
Signature:
Signature:
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
o
Comparison Container
Sulfuric Acid
Cobaltous Chloride
Ferric Chloride
Cupric Sulphate
Water
REAGENTS:
PROCEDURE
Unless otherwise directed, add the specified quantity of the substance, finely powdered if in solid form, in
small portions to the comparison container, which contains the specified volume of sulfuric acid TS. Stir the
mixture with a glass rod until solution is complete, allow the solution to stand for 15 minutes and compare
the color of the solution with that of the specified matching fluid (Refer table) in a comparison container,
viewing the fluids transversely against a background of white porcelain or white glass
Title
: DETERMINATION OF READILY CARBONIZABLE SUBSTANCES TEST
Supersedes
: Nil
Issue Date
10/04/2010
Review date
April 2012
SOP No : GTP-10040
Effective date
10/04/2010
Page number
2 of 2
MATCHING FLUID
Matching
Fluids
Parts of
Cobaltous
Chloride CS
A
0.1By :
Developed
B
0.3
Name:
C
0.1
D
0.3
Signature:
E
0.4
Parts of Ferric
Chloride CS
Parts of Cupric
Sulphate CS
0.4
Reviewed
By :
0.1
4.4By :
Authorized
0.3
3.5
Name:
0.1 Designation:
4.2
Managing Director
0.4
3.7
Signature:
0.3
3.1
Name: 0.9
0.6
0.6
Signature:
1.2
Parts of
Water
COMPANY NAME
F
G
H
I
J
K
L
M
N
O
P
Q
R
S
T
0.3
0.5
0.2
0.4
0.4
0.5
0.8
0.1
0.0
0.2
0.2
0.2
0.3
0.2
0.5
1.2
1.2
1.5
2.2
3.5
4.5
3.8
2.0
4.9
4.8
0.4
0.3
0.4
0.1
0.5
0.0
0.2
0.0
0.1
0.1
0.0
0.1
0.1
0.1
0.1
0.1
0.1
0.2
0.0
0.4
3.5
3.1
3.3
2.3
1.0
0.0
0.3
2.8
0.0
0.0
4.3
4.4
4.1
4.7
3.6
Note: The above document is prepared on the basis of General chapter <271> of USP.
END OF THE DOCUMENT
Annexure
The following people have read this General testing procedure and currently using these
Procedures in the laboratory.
Date
Name with Company

profile
Developed By :
Name:
Name:
Designation:
Signature:
Signature:
Signature
Reviewed By :
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
INDEX
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Sl.No
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
34.
35.
Subject
SOP. No.
DESCRIPTION OF MATERIAL
SOLUBILITY TESTING
CLARITY OF SOLUTION
COLOUR OF SOLUTION
DETERMINATION OF MELTING POINT
DETERMINATION OF LOSS ON DRYING
DETERMINATION OF BOILING POINT
DETERMINATION OF REFRACTIVE INDEX
DETERMINATION OF OPTICAL ROTATION AND SPECIFIC
OPTICAL ROTATION
DETERMINATION OF WATER
DETERMINATION OF SULPHATED ASH
DETERMINATION OF LOSS ON IGNITION
LIMIT TEST OF CHLORIDES
LIMIT TEST OF SULPHATES
LIMIT TEST OF IRON
LIMIT TEST OF HEAVY METALS
NON AQUEOUS TITRATION
POTENTIOMETRIC TITRATION
LIMIT TEST OF ARSENIC
IDENTIFICATION REACTION OF IONS AND FUNCTIONAL
GROUPS
IDENTIFICATION BY UV
THIN LAYER CHROMATOGRAPHY
LIMIT TEST FOR CALCIUM
DETERMINATION OF pH
DETERMINATION OF OXIDISING SUBSTANCE
DETERMINATION OF ACID VALUE
DETERMINATION OF FRIABILITY
BULK DENSITY AND TAPPED DENSITY
DETERMINATION OF UNIFORMITY OF WEIGHT OF TABLET AND
CAPSULE
DETERMINATION OF THICKNESS OF TABLET
DETERMINATION OF HARDNESS
DETERMINATION OF CONDUCTIVITY
DETERMINATION OF HYDROXYL VALUE
DETERMINATION OF DISINTEGRATION TIME
DETERMINATION OF IODINE VALUE
No. of Pages
1
1
1
3
1
2
1
1
2
GTP-10001
GTP-10002
GTP-10003
GTP-10004
GTP-10005
GTP-10006
GTP-10007
GTP-10008
GTP-10009
GTP-10010
GTP-10011
GTP-10012
GTP-10013
GTP-10014
GTP-10015
GTP-10016
GTP-10017
GTP-10018
GTP-10019
2
2
2
1
1
1
4
2
2
2
11
GTP-10020
GTP-10021
GTP-10022
GTP-10023
GTP-10024
GTP-10025
GTP-10026
GTP-10027
GTP-10028
1
4
1
1
1
1
2
5
2
GTP-10029
GTP-10030
GTP-10031
GTP-10032
GTP-10033
GTP-10034
GTP-10035
1
1
3
3
2
4
INDEX
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director
COMPANY NAME
Sl.No
36.
37.
38.
39.
40.
Subject
SOP. No.
DETERMINATION OF SAPONIFICATION VALUE

DETERMINATION OF ACID VALUE
DETERMINATION OF DYNAMIC VISCOSITY ,
KINETIC VISCOSITY AND APPARENT VISCOSITY
DETERMINATION OF DIAMETER , WIDTH AND
LENGTH
DETERMINATION OF READILY CARBONIZABLE
SUBSTANCE TEST
No. of Pages
2
2
7
GTP-10036
GTP-10037
GTP-10038
1
GTP-10039
2
GTP-10040
41.
42.
43.
44.
45.
46.
47.
48.
49.
50.
51.
52.
53.
54.
55.
56.
57.
58.
59.
60.
61.
62.
63.
64.
65.
66.
67.
68.
69.
70.
Developed By :
Name:
Name:
Reviewed By :
Designation:
Signature:
Signature:
Authorized By :
Name:
Quality Head
Designation:
Signature:
Managing Director

GENERAL TESTING PROCEDURES FOR RAW MATERIALS

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

GENERAL TESTING PROCEDURES FOR RAW MATERIALS

Uploaded by

Copyright:

Available Formats

COMPANY NAME

General Testing Procedure

Twenty arbitrarily selected capsules are visually examined for:

Twenty arbitrarily selected tablets are visually examined for:

Ten arbitrarily selected bottles are visually examined for:

To lay down a procedure for solubility tests for raw materials.

Determination of Solubility in raw materials to ensure the supplied material passes

Solubility of raw materials are to be determine at a temperature between 15C and

Quantity taken for test

1 gm in less than 1ml

Very Slightly soluble -

0.1gm in more than 1000ml

Into separate matched, flat-bottomed test tubes, 15 to 25 mm in internal diameter

To lay down a procedure for color of solution.

Determination of color of solution in the raw materials to ensure the supplied

Ferric chloride hexahydrate AR grade

Reference : IP-1996 (Appendix 6 , page A -78)

: DETERMINATION OF MELTING POINT

To lay down a procedure for determination of meting point.

: DETERMINATION OF LOSS ON DRYING

and allow it to cool to room

Weight of empty bottle

: DETERMINATION OF LOSS ON DRYING

Conditions of Loss on drying;

: The drying is carried out over phosphorus pentaoxide at atmospheric

: The drying is carried out over phosphorus pentoxide at a pressure of 1.5

: within a specified temperature range: The drying is carried out over

: within a specified temperature range: The drying is carried out in an oven

: DETERMINATION OF BOILING POINT

To lay down a procedure of determination of boiling point.

the corrected temperature,

the measured temperature,

the barometric pressure in kPa at the time of the

: DETERMINATION OF REFRACTIVE INDEX

To lay down a procedure of determination of refractive index.

Determination of Refractive index of a liquid to ensure the supplied material

: DETERMINATION OF Optical Rotation and Specific Optical Rotation

Connect power plug to proper power supply through voltage stabilizer.

Polarimeter tube should be clean properly with distilled water.

Calculate the specific optical rotation using the expression =

To lay down a procedure of determination of water.

Determination of water content in the pharmaceuticals to ensure the water content

Connect power plug to proper power supply.

Calculate the Water Content by the following equation :

( Factor between 3 and 5 )

By : for substance neutralization

: DETERMINATION OF SULPHATED ASH

To lay down a procedure of determination of Sulphated ash.

The procedure is applicable to all Active and Inactive raw materials

% w/w of Sulphated ash =

Weight of the empty crucible in grams.

: DETERMINATION OF SULPHATED ASH

Method II (2.4.14) (Ph. Eur. method)

% m/m of Sulphated ash =

= Weight of the empty crucible in grams.

The above document has been Signature:

: DETERMINATION OF LOSS ON IGNITION

To lay down a procedure of determination of Loss on Ignition.

: DETERMINATION OF LOSS ON IGNITION

% w/w of Loss on Ignition =

W2= Weight of the crucible with sample in grams ,before ignition

END OF THE DOCUMENT