PROCEDURE:
The records
of preparation and standardization details of volumetric solutions shall
be maintained as per (Logbook Format). The volumetric solution bottles shall
be labeled as per SOP for Labeling Policy. The control no. shall be given to
all volumetric solutions as VSXX-YYY, where VS stand for the volumetric
solution, XX is code no. of volumetric solution and YYY is serial no. of
volumetric solution Preparations and standardization of the various volumetric
solutions are given below: Standardize the Volumetric Solutions in
Triplicate set against the Primary Standard, chemical, equimolar/ Equi- normal
solution as applicable. The average of all three results will be treated as the
actual strength of the solution. The individual value will be taken up
to the 4th
decimal place and the mean of all three values will be taken up to the 3rd decimal place.
{tocify} $title={Table of Contents}
AMMONIUM THIOCYANATE (0.1M)
(Code
No. VS01)
PREPARATION
Weigh accurately 7.612gm of ammonium thiocyanate in a
1000 ml volumetric flask and add sufficient water to dissolve properly
and dilute to 1000 ml with water. Standardize the solution in the following
manner.
STANDARDIZATION
(TRIPLICATE)
Pipette 30 ml of 0.1 M silver nitrate standard
solution in a glass stoppered flask and dilute with water to 50 ml, add 2 ml of
nitric acid and 2 ml of ferric ammonium sulphate solution and titrate
with 0.1M ammonium thiocyanate solution to the first appearance
of a red-brown colour.
Calculation
Volume
taken of 0.1Msilver nitrate (ml) x Molarity of 0.1Msilver nitrate
Molarity
= --------------------------------------------------
Volume
consumed (ml) of 0.1 M ammonium thiocyanate
ACCEPTANCE
CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD*
of the triplicate results of standardization / re-standardization should not
more
than 0.2 %
Reference
In-House
Frequency
Preparation
1 Months
Standardization
Initially after preparation
Re-standardization
After 15 days
Storage conditions
Store the solution in a well-stoppered glass
bottle at ambient
temperature
Precautions (if any)
None specific
BENZETHONIUM CHLORIDE (0.004 M)
(Code No. VS02)
PREPARATION
Weigh accurately 1.792gm of benzethonium chloride (dried to
constant weight at 105˚C) in a 1000 ml volumetric flask and add
sufficient water to dissolve properly and dilute to 1000 ml with water.
Standardize the solution in the following manner.
STANDARDIZATION
(TRIPLICATE)
Dissolve 0.35 gm of the dried substance (benzethonium
chloride) in 30 ml of anhydrous glacial acetic acid, add 6ml of mercuric
acetate solution and carry out the non-aqueous titration (appendix 3.45, IP),
using 0.05 ml of crystal violet solution as indicator. Perform a blank
determination and any necessary correction.
Each ml of 0.1M perchloric acid is equivalent to 0.04481gm
of C27H42ClNO2
Calculation
Molarity : (W)
x (P)
---------------------
(W1) x 100
Where W = Actual Weight of benzethonium chloride used for
preparing Volumetric Solution
W1= Molecular Weight of benzethonium
chloride
P = Potency of benzethonium chloride
The potency of benzethonium Chloride (P): Vol. of HClO4
x Molarity of HClO4
×100 × 44.81
----------------------------------------------------------------------
Weight of
benzethonium Chloride × 0.1
ACCEPTANCE
CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization /
re-standardization should not be more
than 0.2 %.
Reference
I
P/In-House (IP 2007, Vol. I, Page No. 548)
Frequency
Preparation
1 Month
Standardization
Initially
after preparation
Re-standardization
After
15 days
Storage conditions
Store
the solution in a well-stoppered glass bottle at ambient temperature
Precautions (if any)
None specific
CERRIC AMMONIUM SULPHATE (0.1M)
(Code No. VS03)
PREPARATION
Dissolve 65.0 gm of cerric ammonium sulphate with the aid of
gentle/heat, in a mixture of 30 ml. of sulphuric acid and 500 ml. of
water. Cool, filter the solution, if turbid, and dilute to 1000 ml with
water. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.2 gm. of arsenic trioxide,
previously dried at 105ºC for 1 hour, and transfer to a 500 ml. conical flask
washes the inner walls of the flask with 25 ml. of an 8.0% w/v solution of
sodium hydroxide, swirl to dissolve, add 100 ml. of water and mix. Add 30 ml.
of dilute sulphuric acid, 0.15 ml. of osmic acid solution, 0.1 ml of
ferroin sulphate solution and slowly titrate with 0.1M cerric ammonium sulphate
solution until the pink colour is changed to a very pale blue, adding the
titrant slowly towards the end-point.
Each 1ml of 0.1M ferric ammonium sulphate is equivalent to
0.004946 gm of As2O3.
Calculation
Wt.
of arsenic trioxide (mg) x Potency of arsenic trioxide ×
0.1
Molarity =
---------------------------------------------
Volume
consumed (ml) x 4.946 x 100
Osmic acid solution
1 % w/v solution of osmic acid in water.
ACCEPTANCE CRITERIA
1)
Accuracy of the solution should be within ± 10% of the theoretical
concentration.
2)
RSD* of the triplicate results of standardization/ re-standardization should
not be more than 0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 549)
Frequency :
Preparation
01
Month
Standardization
Initially after preparation
Re- standardization
After15 days
DISODIUM EDETATE (0.1M)
(Code No. VS04)
PREPARATION
Weigh accurately 37.2 g of disodium edetate in a 1000 ml
volumetric flask and add sufficient water to dissolve properly and
dilute to 1000 ml with water. Standardize the solution in the following manner.
STANDARDIZATION
(TRIPLICATE)
Weigh accurately 0.2 g of calcium carbonate, previously
dried at 110°C for 2 hours and cooled in a desiccator and transferred in a 250
ml conical flask and add 10 ml of water, and swirl to form a slurry. Cover the
flask with a watch glass and introduce 2 ml of dilute hydrochloric acid from a
pipette. Swirl the content of the flask to dissolve the calcium carbonate
properly. Wash down the sides of the flask, the outer surface of the pipette
and the watch glass with water to dilute 100 ml. Add 30 ml of disodium edetate
solution from a 50 ml burette 15 ml of 1 M sodium hydroxide solution and 300 mg
of hydroxy naphthol blue, and continue the titration with 0.1M disodium edetate
solution to a blue endpoint.
Every 1 ml of 0.1M disodium edetate is equivalent to
0.010009gm of CaCO3
Calculation
Wt.
of Calcium Carbonate (mg) x Potency of CaCO3
× 0.1
Molarity
= -------------------------------------------
Volume
consumed (ml) x 10.009 × 100
ACCEPTANCE
CRITERIA
1) Accuracy of the solution should be within ± 10 % of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than
0.2 %.
Reference
IP/In-House (IP 2007, Vol. I, Page No.
549)
Frequency
Preparation
1 Month
Standardization
Initially after preparation
Re- standardization
After15
days
Storage conditions
Store the solution in a well-stoppered glass
bottle at ambient
temperature.
Precautions (if any)
Non specific
DISODIUM EDETATE (0.05 M)
(Code No. VS05)
PREPARATION
Weigh accurately 18.6 gm of disodium edetate in a 1000 ml
volumetric flask and add sufficient water to dissolve properly and
dilute to 1000 ml with water. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately 0.2 g of calcium carbonate, previously
dried at 110°C for 2 hours and cooled in a desiccator and transfer in a 250 ml
conical flask and add 10 ml of water, and swirl to form a slurry. Cover the
flask with a watch glass and introduce 2 ml of dilute hydrochloric acid from a
pipette. Swirl the content of the flask to dissolve the calcium carbonate
properly. Wash down the sides of the flask, the outer surface of the pipette
and the watch glass with water to dilute 100 ml. Add 15 ml of disodium edetate
solution from a 50 ml burette and 15 ml of 1 M sodium hydroxide solution and
300 mg hydroxyl naphthol blue, and continue the titration with 0.05M disodium
edetate solution to a blue endpoint.
Each 1 ml of 0.05M disodium edetate is equivalent to
0.0050045gm of CaCO3
Calculation
Wt.
of Calcium Carbonate (mg) x Potency of CaCO3×
0.05
Molarity
= --------------------------------------
Volume
consumed (ml) x 5.0045 × 100
ACCEPTANCE
CRITERIA
1)
Accuracy of the solution should be within ± 10% of the theoretical
concentration.
2) RSD* of the triplicate results of standardization /
re-standardization should not more
than 0.2 %.
Reference
In-House
Frequency
Preparation
1 Month
Standardization
Initially after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution in a well-stoppered glass
bottle at ambient
temperature.
Precautions (if any)
None specific
FERROUS AMMONIUM SULPHATE (0.1 M)
(Code No. VS06)
PREPARATION
Dissolve 40.0 gm of ferrous ammonium sulphate in a
previously cooled mixture of 40 ml. of sulphuric acid and 200 ml. of water,
dilute with sufficient boiled and cooled water to produce1000 ml. Standardize
the solution in the following manner
STANDARDIZATION
(TRIPLICATE)
Measure accurately 25.0 ml. of solution into a flask, add 2
drops of 1,10-phenanthroline solution and titrate with 0.1M ferric ammonium
sulphate until the red colour changed to pale blue.
Calculation
M2 x V2
Molarity
= ----------------------
V1
Where M2 = molarity of 0.1M ferric ammonium sulphate
solution.
V2 = volume of 0.1 M ferric
ammonium sulphate consumed in
ml
V1 = volume of 0.1 M ferrous
ammonium sulphate taken in ml.
1,10-phenanthroline
Dissolve 1.5 gm. Of 1,10-phenanthroline in sufficient water
to produce 100 ml.
ACCEPTANCE
CRITERIA
1)
Accuracy of the solution should be within ± 10% of the theoretical
concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 549)
Frequency :
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the
solution in a light-resistant container at ambient temperature
Precautions (if any) None specific
HYDROCHLORIC ACID (1M)
(Code No. VS07)
PREPARATION
Dilute 85 ml. of hydrochloric acid with water to produce
1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 1.5 gm. of anhydrous sodium
carbonate, previously dried at about 270°C for 1 hour. Dissolve it in 100 ml.
of water and add 0.1ml. of methyl red solution. Add the acid slowly from a
burette, with constant stirring, until the solution becomes faintly pink.
Heat the solution to boiling, cool and continue the titration. Heat again to
boiling and titrate further as necessary until the faint pink colour is no
longer affected by continued boiling.
Every 1 ml of 1M hydrochloric acid is equivalent to
0.05299gm of Na2CO3
Calculation
Wt.
of sodium carbonate (mg) x Potency of Na2Co3
× 1
Molarity = ---------------------------------
Volume
consumed (ml) x 52.99 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical
concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than 0.2%.
Reference
I.P./In-
House (IP 2007, Vol. I, Page No. 550)
Frequency :
Preparation
01Month
Standardization
Initially after
preparation
Re- standardization
After 15 days
Storage conditions
Store the solution in a stoppered glass bottle at ambient
temperature
Precautions (if any)
1) Handle with care under the fuming cupboard.
2) Wear hand
gloves & nose mask during preparation
3) Never
add water to the acid.
HYDROCHLORIC ACID (0.5 M)
(Code No. VS08)
PREPARATION
Dilute 42.5 ml. of hydrochloric acid with water to produce
1000 ml. Standardize the solution in the following manner.
STANDARDIZATION (TRIPLICATE)
Weigh accurately 0.750 gm. of anhydrous sodium carbonate,
previously dried at about 270°C for 1 hour. Dissolve it in 100 ml. of water and
add 0.1ml. of methyl red solution. Add the acid slowly from a burette, with
constant stirring, until the solution becomes faintly pink. Heat the solution
to boiling, cool and continue the titration. Heat again to boiling and titrate
further as necessary until the faint pink colour is no longer affected by
continued boiling.
Each 1 ml of 0.5M hydrochloric acid is equivalent to
0.026495gm of Na2CO3
Calculation
Wt.
sodium carbonate (mg) x Potency of Na2Co3×
0.5
Molarity = ------------------------------------
Volume
consumed (ml) x 26.495 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency:
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution
in a stoppered glass bottle at ambient temperature.
Precautions (if any)
1) Handle with care under
the fuming cupboard.
2) Wear hand gloves & nose mask during preparation
3) Never add water to the acid.
HYDROCHLORIC ACID (0.1M)
(Code No. VS09)
PREPARATION
Dilute 8.5 ml. of hydrochloric acid with water to produce
1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh
accurately 0.150 gm of anhydrous sodium carbonate previously dried at about
270°C for 1 hour. Dissolve it in 100 ml. of water and add 0.1ml.of methyl red
solution. Add the acid slowly from a burette, with constant stirring, until the
solution becomes faintly pink. Heat the solution to boiling, cool and continue
the titration, heat again to boiling and titrate further as necessary until the
faint pink colour is no longer affected by continued boiling.
Each 1 ml of 0.1M hydrochloric acid is equivalent to
0.005299gm of Na2CO3
Calculation
Wt.
of sodium carbonate (mg) x Potency of Na2Co3
× 0.1
Molarity = -----------------------------------------
Volume
consumed (ml) x 5.299 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ±
10% of the theoretical
concentration.
2) RSD* of the triplicate results of
standardization/re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency :
Preparation
01 Months
Standardization
Initially after preparation
Re- standardization
After15 days
Storage conditions
Store the solution in a stoppered glass bottle at
ambient
temperature
Precautions (if any)
1) Handle with care under a fuming cupboard.
2) Wear hand gloves & nose mask during preparation
3) Never add water to the acid.
HYDROCHLORIC ACID (0.02M)
(Code No. VS10)
PREPARATION
Dilute 1.7 ml. of hydrochloric acid with water to produce
1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately 0.030 gm. of anhydrous sodium carbonate
previous heated at about 270°C for 1 hour. Dissolve it in 100 ml. of
water and add 0.1ml.of methyl red solution. Add the acid slowly from a burette,
with constant stirring, until the solution becomes faintly pink. Heat the
solution to boiling, cool and continue the titration. Heat again to boiling and
titrate further as necessary until the faint pink colour is no longer affected
by continued boiling.
Every 1 ml of 0.02M hydrochloric acid is equivalent to
0.0010598gm of Na2CO3
Calculation
Wt.
of sodium carbonate (mg) x Purity of Na2Co3×
0.02
Molarity = --------------------------------
Volume
consumed (ml) x 1.0598 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ±
10% of the theoretical
concentration.
2) RSD* of the triplicate results of
standardization/re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency :
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution in a stoppered glass bottle at ambient
temperature
Precautions (if any)
1) Handle with care
under the fuming cupboard.
2)
Wear hand gloves & nose mask during preparation
3) Never add
water to the acid.
IODINE (0.05 M)
(Code No. VS11)
PREPARATION
Dissolve 14 gm of iodine in a solution of 36 gm of potassium
iodide in 100 ml of water, add 3 drops of hydrochloric acid and dilute with
water to 1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately 0.150 gm of arsenic trioxide previously
dried at 1050C
for 1 hour and cooled in desiccators, dissolve in 20 ml of 1 M sodium hydroxide
by warming (if necessary ) dilute with 40 ml of water, add 0.1 ml of methyl
orange solution and add dropwise dilute hydrochloric acid until the yellow
colour is changed to pink. Add 2 gm of sodium carbonate dilute with 50 ml of
water and add 3 ml of starch solution. Titrate with 0.05M iodine solution until
a permanent blue colour is produced.
Each 1ml of 0.05M iodine is equivalent to 0.004946gm of As2O3.
Calculation
Wt.
of Arsenic trioxide (mg) x Potency of Arsenic trioxide × 0.05
Molarity =
---------------------------------------
Volume
Consumed (ml) x 4.946 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 550)
Frequency :
Preparation
01 Months
Standardization
Initially after
preparation
Re- standardization
After15
days
Storage conditions
Store the
solution in well stoppered light-resistant
amber
coloured glass bottle.
Precautions (if any) 1) Handle with care.
2) Use hand gloves and a nose mask
during preparation
MERCURIC NITRATE (0.02M)
(Code No. VS12)
PREPARATION
Dissolve 6.85 gm of mercuric nitrate in 20 ml of 1M nitric
acid and add sufficient water to produce 1000 ml. Standardize the solution in
the following manner.
STANDARDISATION (TRIPLICATE)
Dissolve 15 mg of sodium chloride in 50ml of water and
titrate with the 0.02M mercuric nitrate solution determining the end-point
potentiometrically using a platinum or mercury mercurous sulphate reference
electrode.
Each 1 ml of 0.02M mercuric nitrate is equivalent to
0.002338gm of NaCl.
Calculation
Wt.
of sodium chloride (mg) x Potency of sodium chloride× 0.02
Molarity = ---------------------------------
Volume
Consumed (ml) x 2.338 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 550)
Frequency
Preparation
01 Months
Standardization
Initially after
preparation
Re- standardization
After
15 days
Storage conditions
ore the solution in a well stoppered
light-resistant amber coloured glass bottle.
Precautions (if any) None Specific
PERCHLORIC ACID (0.1M)
(Code No. VS13)
PREPARATION
Mix 8.5 ml. of perchloric acid with 500 ml. of anhydrous
glacial acetic acid and 25 ml. of acetic anhydride, cool and add anhydrous
glacial acetic acid to produce 1000 ml. Allow the prepared solution to
stand for 1 day for the excess acetic anhydride to be combined and carry out
the determination of water. If the water content exceeds 0.05%, add more acetic
anhydride. If the solution contains no titrable water, add sufficient
water to obtain a content of water between 0.02% and 0.05%. Allow the
solution to stand for one day and again titrate the water content. The
solution so obtained should contain between 0.02% and 0.05% of water.
Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.350 gm. of potassium hydrogen
phthalate (KHP) previously dried at 120°C for 2 hours and dissolve it in 50 ml.
of anhydrous glacial acetic acid add 0.1ml crystal violet solution as an
indicator and titrate with the 0.1M perchloric acid solution until the
violet colour changes to emerald-green. Perform a blank determination and make
any necessary corrections.
Each 1ml of 0.1M perchloric acid is equivalent to 0.02042gm
of C8H5KO4
Calculation
Wt.
of potassium hydrogen phthalate (mg) x Potency of
KHP×0.1
Molarity = ------------------------------------
Volume
consumed (ml) x 20.42 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 550)
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15
days
Storage conditions
Store the solution in a light-resistant airtight container at
ambient temperature
Precautions (if any)
1) Handle with care under a
fuming cupboard.
2) Handle with care, wear hand
gloves and nose mask
PERCHLORIC ACID (0.05M)
(Code No. VS14)
PREPARATION
Mix 4.25 ml. of perchloric acid with 500 ml. of
anhydrous glacial acetic acid and 12.5ml.of acetic anhydride, cool and add
anhydrous glacial acetic acid to produce 1000 ml. Allow the prepared solution
to stand for 1 day for the excess acetic anhydride to be combined and carry out
the determination of water. If the water content exceeds 0.05 %, add more
acetic anhydride. If the solution contains no titrable water, add sufficient
water to obtain the content of water between 0.02% and 0.05%. Allow the
solution to stand one day and again titrate the water content. The
solution so obtained should contain between 0.02% and 0.05% water content.
Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.1750 gm. of potassium hydrogen
phthalate (KHP), previously powdered lightly and heated at about 120°C for 2
hours and dissolve it in 50 ml. of anhydrous glacial acetic acid. Add 0.1ml.of
crystal violet solution as an indicator and titrate with 0.05M perchloric acid
solution until the violet colour changes to emerald-green. Perform a
blank determination and make any necessary corrections.
Each 1ml of 0.05M perchloric acid is equivalent to 0.01021gm
of C8H5KO4
Calculation
Wt.
of potassium hydrogen phthalate (mg) x Potency of KHP×0.05
Molarity =
----------------------------------
Volume
consumed (ml) x 10.21 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially after 24 hours of preparation
Re- standardization
After15
days
Storage conditions
Store the solution in a light-resistant airtight container at
ambient temperature
Precautions (if any)
1) Handle with care under
a fuming cupboard.
2) Handle with care, wear hand gloves and
nose mask
POTASSIUM PERMANGANATE (0.02M)
(Code No. VS15)
PREPARATION
Dissolve 3.2 gm of potassium permanganate in 1000 ml water,
heat on the water bath, allow standing for 2 days and filter through glass
wool. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
To 25 ml of this solution in a glass stoppered flask add 2
gm of potassium iodide, followed by 10 ml of 1M sulphuric acid. Titrate the
liberated iodine with 0.1 M sodium thiosulphate using 3 ml of starch solution,
added towards the end of the titration, as the indicator. Perform the blank
determination and any necessary correction.
Each 1ml of 0.1M sodium thiosulphate is equivalent to
0.00316 gm of KMnO4.
Calculation
M2 x V2
Molarity
= ----------------------
V1
Where M2 = molarity of 0.1M sodium thiosulphate
solution.
V2 = volume of 0.1 M sodium
thiosulphate consumed in
ml
V1 = volume of 0.1 M potassium
permanganate taken in ml.
ACCEPTANCE
CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization /
re-standardization should not be more
than 0.2 %.
Reference
I
P/In-House (IP 2007, Vol. I, Page No. 551)
Frequency
Preparation
01 Months
Standardization
Initially after preparation
Re-standardization
After 15 days
Storage conditions
Store the solution
in a well-stoppered glass bottle at ambient
temperature
Precautions (if any)
None specific
POTASSIUM IODATE (0.05M)
(Code No. VS16)
PREPARATION
Weigh accurately 10.70 gm of potassium iodate previously
dried at 110°C to constant weight in sufficient water to produce 1000 ml.
Standardise the solution in the following method.
STANDARDISATION (TRIPLICATE)
Weigh accurately 0.35 gm of potassium iodide, dissolve in
about 10 ml of water, add 35 ml of hydrochloric acid and 5 ml of chloroform.
Titrate with 0.05 M potassium iodate until the purple colour of iodine
disappears from the chloroform. Add the last portion of the iodate solution
dropwise and agitate vigorously and continuously. Allow standing for 5 minutes.
If any colour develops in the chloroform layer continue the titration until the
chloroform is decolourised.
Each 1ml of 0.05 M potassium iodate is equivalent to
0.0166gm of potassium iodide.
Calculation
Wt.
of potassium iodide (mg) x Potency of potassium iodide× 0.05
Molarity =
---------------------------
Volume
consumed (ml) x 16.6 × 100
ACCEPTANCE
CRITERIA
1)
Accuracy of the solution should be within ± 10% of the theoretical
concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 551)
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in
light-resistant container at ambient
temperature
Precautions (if any)
None specific
POTASSIUM HYDROXIDE (0.1M)
(Code No. VS17)
PREPARATION
Dissolve 6 gm of potassium hydroxide in sufficient
carbon dioxide-free water to produce 1000 ml. Standardize the solution
in the following manner.
STANDARDISATION (TRIPLICATE)
Titrate 20.0 ml of the solution with 0.1 M hydrochloric acid
using 0.5 ml of phenolphthalein solution as an indicator.
Each ml of 0.1 M hydrochloric acid is equivalent to 0.005611 g of KOH.
Calculation
Vol.
taken in ml. (0.1 M KOH) X Molarity of HCl (0.1M)
Molarity
= -----------------------------
Volume
consumed of 0.1M HCl (ml)
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than 0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 551)
Frequency
Preparation
01 Months
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in a
light-resistant container at ambient temperature
Precautions (if any) None
specific
POTASSIUM HYDROXIDE ETHANOLIC (0.5M)
(Code No.VS18)
PREPARATION
Dissolve 30 g of potassium hydroxide in 40 ml of
water and then add sufficient ethanol (60 %) to produce 1000 ml.
STANDARDISATION (TRIPLICATE)
Titrate 20.0 ml of the solution with 0.5 M hydrochloric acid
using 0.1 ml of phenolphthalein solution as indicator until the
permanent pale-pink colour is produced.
Each ml of 0.5 M hydrochloric acid is equivalent to
0.02806 g of KOH.
Calculation
Vol.
taken in ml. (0.5 M HCl) X Molarity of HCl (0.5M)
Molarity
= -----------------------------------
Volume
consumed of 0.5M Eth. KOH (ml)
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/ re-standardization
should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 551)
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution in the light-resistant container at ambient
temperature
Precautions (if any) None
specific
SILVER NITRATE (0.1M)
(Code No. VS19)
PREPARATION
Dissolve 17.0 gm of Silver Nitrate in sufficient water to
produce 1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.1 gm. of sodium chloride,
(previously dried at 110°C for 2 hours) and dissolve in 5 ml. of
water. Add 5 ml. of acetic acid, 50 ml. of methanol and 0.15 ml of eosin
solution. Stir, preferably with a magnetic stirrer, and titrate with 0.1M
silver nitrate
solution.
Every 1 ml of 0.1M silver nitrate is equivalent to
0.005844gm of NaCl.
Calculation
Wt.
of sodium chloride (mg) x Potency of NaCl × 0.1
Molarity = --------------------------------------
Volume
consumed (ml) x 5.844 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 551)
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After
15 days
Storage conditions
Store the solution in
tightly stoppered amber coloured
glass bottles at ambient
temperature.
Precautions (if any) 1)
Avoid direct contact during weighing and its spillage.
2) Use hand gloves.
SILVER NITRATE (0.1M) POTENTIOMETRIC
(Code No. VS20)
PREPARATION
Dissolve 17.0 gm of silver nitrate in sufficient water to
produce 1000 ml. Standardize the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.1 gm. of sodium chloride in a 100
ml beaker and dissolve in it 50 ml. of water. Carry out the titration
potentiometrically.
Every 1 ml of 0.1M silver nitrate is equivalent to
0.005844gm of NaCl.
Calculation
Wt.
of sodium chloride (mg) x Potency of NaCl × 0.1
Molarity = --------------------------------
Volume
consumed (ml) x 5.844 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15
days
Storage conditions
Store the solution in tightly stoppered amber coloured
glass bottles at ambient temperature.
Precautions (if any)
1) Avoid direct contact during weighing and its spillage.
2) Use hand gloves.
SODIUM HYDROXIDE (1M)
(Code No. VS21)
PREPARATION
Dissolve 42.0 gm of Sodium hydroxide in sufficient carbon
dioxide-free to produce 1000 ml. Standardize the solution in the following
manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately 5.0 gm. of potassium hydrogen phthalate (KHP),
previously powdered and dried at 120°C for 2 hours and dissolved in 75 ml. of
carbon dioxide-free water. Add 0.1 ml. of phenolphthalein solution and titrate
with 1M sodium hydroxide solution until a permanent pink colour is produced.
Each 1ml of 1M sodium hydroxide is equivalent to 0.2042 gm
of C8H5KO4
Calculation
Wt.
of potassium hydrogen phthalate (mg) x Potency of KHP× 1
Molarity =
-----------------------------------------
Volume
consumed (ml) x 204.2 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
IP/In-House (IP- 2007, Vol. I. Page No. 552)
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution in a well-stoppered
light-resistant HDPE bottle,
which prevent access to atmospheric Carbon Dioxide at ambient temperature.
Precautions (if any)
1) Handle with care.
2) Use hand gloves and a nose mask
during preparation.
SODIUM HYDROXIDE (0.1M)
(Code No. VS22)
PREPARATION
Dissolve 4.2 gm of sodium hydroxide in sufficient carbon
dioxide-free water to produce 1000 ml. Standardize the solution in the
following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.5 gm. of potassium hydrogen
phthalate (KHP), previously powdered and dried at 120°C for 2 hours and
dissolve in 75 ml of carbon dioxide-free water. Add 0.1 ml. of phenolphthalein
solution and titrate with the 0.1M sodium hydroxide solution until a permanent
pink colour is produced.
Each 1ml of 0.1M sodium hydroxide is equivalent to 0.02042
gm of C8H5KO4
Calculation
Wt.
of potassium hydrogen phthalate (mg) x Potency of KHP × 0.1
Molarity =
--------------------------------------
Volume
consumed (ml) x 20.42 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions
Store the solution in well-stoppered
light-resistant HDPE bottle
which prevent access to atmospheric
carbon dioxide at ambient
temperature
Precautions (if any) 1)
Handle with care.
2) Use hand gloves and a nose mask
during preparation.
SODIUM HYDROXIDE (0.05M)
(Code No. VS23)
PREPARATION
Dissolve 2.1gm of sodium hydroxide in sufficient carbon
dioxide-free water to produce 1000 ml. Standardize the solution in the
following
manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.25 gm. of potassium hydrogen
phthalate (KHP), previously powdered and dried at 120°C for 2 hours and
dissolve in 75 ml. of carbon dioxide-free water. Add 0.1 ml. of phenolphthalein
solution and titrate with 0.05M sodium hydroxide solution until a permanent
pink colour is produced.
Each 1ml of 0.05M sodium hydroxide is equivalent to
0.01021gm of C8H5KO4
Calculation
Wt.
of potassium hydrogen phthalate (mg) x Potency of KHP×0.05
Molarity = ------------------------------------
Volume
consumed (ml) x 10.21 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After15 days
Storage conditions Store
the solution in well-stoppered light-resistant HDPE
the
bottle which prevents access to atmospheric carbon dioxide at
ambient
temperature.
Precautions (if any) 1) Handle with care.
2) Use hand gloves and a nose mask
during preparation.
SODIUM THIOSULPHATE (0.1M)
(Code No. VS24)
PREPARATION
Dissolve 25
gm of sodium thiosulphate and 200 mg. of sodium carbonate in carbon
dioxide-free water to produce 1000 ml. Standardize the solution in the
following manner
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.2 gm. of potassium bromate and
dissolve sufficient water to produce 250 ml. To 50 ml. of this solution
add 2 gm. of Potassium Iodide and 3 ml. of 2M Hydrochloric acid and titrate
with 0.1M sodium thiosulphate solution using starch solution added towards the
end of the titration, as indicator until the blue colour is discharged to
end-point
Every 1 ml of 0.1M sodium thiosulphate is equivalent to
0.002784gm of KBrO3
Calculation
Wt.
of potassium bromate(mg) × 50 x Potency of potassium bromate× 0.1
Molarity
= ------------------------------------
Volume
consumed (ml) x 2.784 x 250 × 100
Starch solution
Triturate 1 gm. of soluble starch with 5 ml. of
water and add, stirring continuously, to produce 100 ml. of
boiling water containing 10 mg of mercuric Iodide, This solution complies with
the following test which should be carried out each time the reagent is used.
Sensitivity to Iodine
Mix 1 ml. with 20 ml. of water, add about 50mg. of potassium
iodide and 0.05 ml. of 0.005M Iodine a blue colour is produced.
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/ re-standardization
should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 552)
Frequency
Preparation
01 Month
Standardization
Initially after
preparation
Re- standardization
After
15 days
Storage conditions Store the solution
in a light-resistant container at ambient
temperature
Precautions (if any)
None specific
SODIUM THIOSULPHATE (0.001M)
(Code No.
VS25)
PREPARATION
Take 10 ml 0.1M of sodium thiosulphate in a 1000 ml
volumetric flask and produce 1000 ml with carbon dioxide-free water.
Standardize the solution in the following manner
STANDARDISATION (TRIPLICATE)
Weigh accurately about 0.05 gm. of potassium bromate and
dissolve sufficient water to produce 500 ml. To 10 ml. of this solution
add 2 gm of Potassium Iodide and 3 ml. of 2M hydrochloric acid and titrate with
0.001M sodium thiosulphate solution using starch solution added towards the end
of the titration, as indicator until the blue colour is discharged to a blue
coloured end-point
Each 1 ml of 0.001M sodium thiosulphate is equivalent to
0.00002784gm of KBrO3.
Calculation
Wt.
of potassium bromate(mg) x 10 x Potency of potassium bromate ×0.001
Molarity =
-----------------------------------
Volume
consumed (ml) x 0.02784 x 500 × 100
Starch solution
Triturate 1 gm. of soluble starch with 5 ml. of
water and add, stirring continuously, to produce 100 ml. of
boiling water containing 10 mg of mercuric Iodide, this solution complies with
the following test which should be carried out each time the reagent is used.
Sensitivity to Iodine
Mix 1 ml. with 20 ml. of water, add about 50mg. of potassium
iodide and 0.05 ml. of 0.005M iodine, the blue colour is produced.
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than 0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in a
light-resistant container at ambient
temperature
Precautions (if any) None
specific
SODIUM NITRITE (0.1M)
(Code No.VS26)
PREPARATION
Dissolve 7.5 gm of sodium nitrite insufficient water to
produce 1000 ml of water. Standardize the solution in the following manner
STANDARDISATION (TRIPLICATE)
Dissolve 0.3 gm of sulphanilic acid in 50 ml of 2M
hydrochloric acid, add 3 gm of potassium bromide, cool in ice and titrate with
the 0.1M sodium nitrite solution determining the end-point potentiometrically.
Each 1ml of 0.1M sodium nitrite is equivalent to 0.01732gm
of C6H
7NO3S.
Calculation
Wt.
of sulphanilic acid (mg) x Potency of sulphanilic acid × 0.1
Molarity = -------------------------------------
Volume
consumed (ml) x 17.32 ×100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than 0.
2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 552)
Frequency
Preparation
01 Month
Standardization
Initially after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in a well-stoppered
light-resistant HDPE bottle
which prevent access to atmospheric
carbon dioxide at ambient
temperature.
Precautions (if any)
None specific
SODIUM LAURYL SULPHATE (0.004M)
(Code No. VS27)
PREPARATION
Dissolve 0.2884gm of sodium decyl sulphate, calculated in
reference to the substance at 105˚C for 2 hrs, in sufficient water to produce
1000ml. Standardise the solution in the following manner.
STANDARDISATION (TRIPLICATE)
To 50 ml of the solution add 15ml of chloroform, 10 ml of
sulphuric acid and 1ml of dimethyl yellow–orate blue solution. Titrate with
0.004M benzethonium chloride, shaking vigorously and allowing the layer to
separate after each addition until the chloroform layer acquires a permanent clear
green colour.
Each 1ml of 0.004M benzethonium chloride is equivalent to
0.001154gm of C12H25NaO4S.
Calculation
M2 x V2
Molarity
= ----------------------
V1
Where M2 = molarity of 0.004M benzethonium
chloride solution.
V2 = volume of
0.004Mbenzethonium chloride consumed in
ml
V1 = volume of 0.004M
sodium lauryl sulphate taken in ml.
ACCEPTANCE
CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization /
re-standardization should not be more than 0.2 %.
Reference
In-House
Frequency
Preparation
1 Months
Standardization
Initially after preparation
Re-standardization After 15 days
Storage conditions
Store the solution
in a well-stoppered glass bottle at ambient
temperature
Precautions (if any)
None specific
SULPHURIC ACID (1M)
(Code No. VS28)
PREPARATION
Add slowly, with stirring, 60 ml. of sulphuric acid to
produce 1000 ml with water, allowing cooling to 25°C. Standardise the solution
in the following manner.
STANDARDISATION (TRIPLICATE)
Weigh accurately about 1.5 gm of anhydrous sodium carbonate
(previously heated at about 270°C for 1 hour). Dissolve it in 100 ml. of water
and add 0.1 ml. of methyl red solution. Add the acid slowly from a burette,
with constant stirring, until the solution becomes faintly pink. Heat the
solution to boiling, cool and continue the titration, Heat again to boiling and
titrate further as necessary until the faint pink colour is no longer affected
by continued boiling.
Each 1ml of 1M sulphuric acid is equivalent to 0.10598gm of
Na2CO3
Calculation
Wt.
of sodium carbonate (mg) x Potency of Na2Co3
×1
Molarity = -------------------------------------
Volume
consumed (ml) x 105.98 × 100
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ±
10% of the theoretical concentration.
2)
RSD* of the triplicate results of standardization/ re-standardization
should not be more than 0.2%.
Reference
I.P./In-House (IP
2007, Vol. I, Page No. 552)
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15 days
Storage conditions
Store the solution
in a well-stoppered glass bottle at
ambient temperature.
Precautions (if any) 1)
Handle with care in the fuming cupboard.
2) Use hand gloves and a nose
mask during preparation.
3) Never add water to acid.
ZINC SULPHATE (0.1M)
(Code No. VS29)
PREPARATION
Dissolve 29 gm of zinc sulphate in sufficient water to
produce 1000 ml. Standardise the solution in the following manner.
STANDARDISATION (TRIPLICATE)
Measure accurately 25 ml. of 0.1 M zinc sulphate into a 250
ml Conical flask and add 25 ml of ammonia ammonium chloride buffer TS. Titrate
with 0.1M disodium edetate using erichrome black T as an indicator.
Calculation
Molarity
of 0.1 M EDTA x Taken volume of 0.1 M EDTA (ml)
Molarity =
-----------------------------------
The
volume of 0.1 M zinc sulphate consumed (ml)
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than 0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in a
light-resistant container at ambient
temperature
Precautions (if any) None
specific
ZINC SULPHATE (0.05M)
(Code No. VS30)
PREPARATION
Dissolve 14 gm of zinc sulphate in sufficient water to
produce 1000 ml. Standardise the solution in the following manner
STANDARDISATION (TRIPLICATE)
Measure accurately 25 ml. of 0.05 M zinc sulphate into a
250ml conical flask and add 25 ml of ammonia ammonium chloride buffer TS.
Titrate with 0.05M disodium edetate using erichrome black T as an indicator.
Calculation
Molarity
of 0.05 M EDTA x Taken volume of 0.05 M EDTA (ml)
Molarity = --------------------------------
The
volume of 0.05 M zinc sulphate consumed (ml)
ACCEPTANCE CRITERIA
1) Accuracy of the solution should be within ± 10% of the
theoretical concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more than 0.2%.
Reference
In-House
Frequency
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After15
days
Storage conditions Store the solution
in light-resistant container at ambient
temperature
Precautions (if any) None
specific
FERRIC AMMONIUM SULPHATE (0.1 M)
(Code No. VS31)
PREPARATION
Dissolve 50 gm of ferric ammonium sulphate in a mixture of
300 ml of water and 6 ml of sulphuric acid, dilute with water to 1000 ml and
mix. Standardise the solution as follows.
STANDARDISATION (TRIPLICATE)
Accurately measure about 25 ml of the solution into a glass
stoppered flask, add 3 ml of hydrochloric acid, mix and add a solution of 2 gm
of potassium iodide in 10 ml of water. Insert the stopper, allow to stand for
10 minutes, then titrate the liberated iodine with 0.1 M sodium thiosulphate
VS, adding 3 ml of starch TS as the endpoint is approached.
Each ml of 0.1 M sodium thiosulphate is equivalent to
0.004822g of FeNH4 (SO4)
2 12 H
2O.
Calculation
M2 x V2
Molarity
= ----------------------
V1
Where M2 = molarity of 0.1M sodium thiosulphate
solution.
V2 = volume of 0.1 M sodium
thiosulphate consumed in
ml
V1 = volume of 0.1 M ferric ammonium sulphate taken in ml.
ACCEPTANCE
CRITERIA
1)
Accuracy of the solution should be within ± 10% of the theoretical
concentration.
2) RSD* of the triplicate results of standardization/
re-standardization should not be more
than
0.2%.
Reference
I.P./In-House (IP 2007, Vol. I, Page No. 549)
Frequency :
Preparation
01 Month
Standardization
Initially
after preparation
Re- standardization
After 15
days
Storage conditions Store the solution in a
light-resistant container at ambient
  temperature
Precautions (if any) None specific
*RSD formula: 100 ( N (xi - X )2 )1/2
∑ N -1
 X
i =1
where N = set of measurement
xi
= Individual measurement
x
=mean of the set
