SOPs For Chemicals

SOPs FOR Chemicals:
I A) SULPHURIC ACID
(COMMERCIAL GRADE):
a) DETERMINATION OF TOTAL ACIDITY % BY MASS:

REAGENTS
1) 1N Sodium hydroxide:
Prepare by dissolving 1 N NaOH ampule and dilute to 500 ml in the volumetric
flask.
2) Methyl red indicator:
Dissolve 1 g of Methyl Red in 95 % (V/V) ethanol and dilute to 100ml with same
ethanol.
PROCEDURE:
Weigh about 2 g of the sample and transfer to 1000 ml conical flask containing
approximately 300 ml of distilled water. Add 2 drops of methyl red indicator and
titrate to the end point with 1 N sodium hydroxide solution until colour changes
from pink to yellow.
Total acidity % by mass (as H2SO4) = V x N x 4.904
M
V = Volume in ml of the standard sodium hydroxide solution used for the titration.
N = Normality of the sodium hydroxide solution
M = Mass of the sample taken for the test.
I B) SULPHURIC ACID
FOR GERBER TEST:
Concentrated sulphuric acid (L.R grade) should be colourless to faint amber colour.
Specific gravity 1.84 at 20 0C.
1) PREPARATION OF GERBER SULPHURIC ACID:
Take required volume of water in a pyrex flask kept in cold water. Carefully add the
sulphuric acid [LR grade] to the water in pyrex flask [NEVER ADD WATER TO ACID]
in small quantities at a time. Keep the container sufficiently cold. Mix gently. The
diluted acid specific gravity should be in the range of 1.815 to 1.820 at 20 0C.
[Generally 80 ml water for 920 ml of concentrated sulphuric acid is needed],
2) Determination of Fat in Sulphuric acid [BLANK TEST]:
1.
to
2.
3.
4.
5.
6.
Take 20 ml of test sample of sulphuric acid using an automatic tilt measure in

the butyrometer.
Transfer 1ml amyl alcohol to the above butyrometer.
Fix the lock stopper and mix the content by shaking the butyrometer.
Place the butyrometer in the centrifuge and balance the machine.
Centrifuge for 5 min at 1000 to 1200 rpm. Read the Fat column.
Column should be clear.
ii) NITRIC ACID
(LR GRADE):
A) DETERMINATION OF STRENGTH:
REAGENTS:
1) 1 N Sodium Hydroxide solution:
Prepare by adding one 1 N NaOH ampule and dilute to 500 ml in volumetric flask
2) 1N Standard Sulphuric acid solution:
28 ml of conc. sulphuric acid [LR grade] is diluted to 1000 ml in volumetric flask.
3) Methyl orange indicator:
Dissolve 0.05 g of methyl orange powder in 100 ml distilled water.
PROCEDURE:
Weigh about 2 g of the sample into a conical flask containing 100 ml of distilled
water and add 50 ml of 1N sodium hydroxide solution. Add 4 drops of methyl
orange indicator to the solution in the conical flask and titrate the excess of
sodium hydroxide with 1 N sulphuric acid solution until colour changes from
orange to red. Carryout a blank test simultaneously.
Total acidity % by mass = [V1-V2] 6.3 x N
M
V1 = Volume in ml of the standard sulphuric acid required in blank titration
V2 = Volume in ml of the standard H2SO4
N = Normality of standard H2SO4
M = Mass in grams of the test portion.
III) SODIUM CARBONATE
(WASHING SODA):
REAGENTS:
1) 0.25 N H2SO4: Dissolve 7 ml of H2SO4 in distilled water and dilute to 1 litre in
volumetric flask
2) Methyl Orange: Dissolve 0.05 g of methyl orange in 100 ml of distilled water.
Procedure:
Weigh about 1 g of sample (dried at 100 1 0C) into a 500 ml conical flask
containing 100 ml of distilled water. Add 4 drops of Methyl Orange indicator and
titrate to the end point with 0.25 N H2SO4 until color changes from light yellow to
light pink.
Strength = 5.3 x N x V
W
Where V = Volume of H2SO4 used for titration
N = Normality of H2SO4
W = Weight of test portion
IV) CAUSTIC SODA
(COMMERCIAL GRADE):
REAGENTS:
1) Barium chloride: L.R grade
2) 0.4 N Oxalic acid: 2.5214 g crystallized oxalic acid (di-hydrate) dissolved in
water and make up the volume to 1000 ml in volumetric flask
3) Phenolphthalein Indicator: Dissolve 5 g of reagent in 500 ml of ethanol
(neutralized) and add 500 ml of distilled water.
PROCEDURE:
Weigh about 0.4 g of sample into 250 ml of conical flask and also weigh 1 g of
BacCl2 into the same flask and dissolve with 100 ml of distilled water. Add 3 to 4
drops of phenolphthalein indicator and titrate to the end point with 0.4N Oxalic
acid until the colour changes from Pink to colorless.
Total Alkalinity
4xVxN
W
Where V = Volume of oxalic acid used for titration

N = Normality of oxalic acid
W = Weight of the sample
V) IODOPHORE:
A) DETERMINATION OF IODINE STRENGTH:
REAGENTS:
1) 0.1N Sodium Thiosulphate solution:Dissolve 24.80g of Sodium Thiosulphate crystals in distilled water and dilute to
1000 ml.
2) 1% starch indicator:
Dissolve 1 g of starch powder in 20 ml of cold distilled water and add 80 ml of

boiled distilled water.
PROCEDURE:
Weigh about 10g of sample into 250ml conical flask add 100g of distilled water.
Titrate with standard sodium thiosulphate till colour of solution turns straw
yellow. Add 1 ml of freshly prepared starch indicator and continue the titration
with standard sodium thiosulphate solution till the solution colour disappears.
% of available iodine: 12.69 x V x N
W
V = Volume of Na2S203 used for titration
N= Normality of Na2S203
W = Weight of test portion
B) DETERMINATION OF pH: Take well-mixed sample into a 100ml plastic beaker.
Check the pH of 1% solution with pH meter and note the reading after stabilization
of the reading.
VI) COMMON SALT:

A) DETERMINATION OF MOISTURE CONTENT:
Grind the sample in the mixer. Weigh accurately about 20g each in to two petriplates (previously dried and weighed). Dry in an oven at 140 0C for 4 hrs. Cool in a
desiccator and weigh.
Moisture, % by weight = (W1-W2) x 100

W1
Where W1= Initial weight in g of the material
W2=Final weight in g of the material
B) INSOLUBLE MATTER:
Accurately weigh about 50g of the sample, dissolve in 200ml of water in a
beaker and heat to boiling and cool. Filter the solution through a pre-weighed
filter paper [ordinary]. Wash the filter paper residue till it is free from soluble
salts. Dry the filter paper along with the insoluble residue in hot air oven up to
constant weight.
% of insoluble matter = W1 x 100
W2
Where W1 = weight in g of the residue
W2 = weight in g of the dried sample taken for the test
VII) SOAP OIL: A) DETERMINATION OF TOTAL SOLIDS:

Mix the sample properly in a beaker. Weigh accurately about 5 6g of sample in
two petri-plates (previously dried and weighed). Dry on a boiling water bath for 30
min and then in oven at 1020C for 4 hrs. Cool in a desiccator and weigh.
Moisture, % by weight = (W1-W2) x 100
W1
Where W1= initial weight in g of the material.
W2=final weight in g of the material
% Total Solids = (100 Moisture)
B) DETERMINATION OF pH: Take well-mixed sample into a 100ml plastic beaker.
Check the pH with pH meter and note the reading after stabilization of the reading.
V111) CAUSTIC (LYE) STRENGTH:

Pipette 10 ml of sample into a 100ml Beaker. Add 5drops phenolphthalein
indicator. Titrate with 0.25N sulphuric acid. Note down the burette reading when
the colorless end point is attained.
Alkalinity:
4 x V xN
Sample weight
1X) NITRIC ACID SOLUTION STRENGTH:

Pipette 10ml sample into a 100ml beaker. Add 5drops methyl orange indicator.
Titrate with 1N sodium hydroxide until color changes from orange to yellow.
Note down the burette reading.
Strength:
6.3 x Burette reading x N
Sample volume
x) SOFT WATER ANALYSIS (HARDNESS OF WATER): o Take 100ml of sample water in a sterilized conical flask.
o Add 1ml of ammonium buffer and a pinch of Erichrome Black -T indicator.
o Mix well. Titrate against 0.02 N EDTA solution till the colour changes from
pinkish red to blue.
o Hardness [ppm] = Reading x 10

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SOPs FOR Chemicals:

a) DETERMINATION OF TOTAL ACIDITY % BY MASS:

FOR GERBER TEST:

Take 20 ml of test sample of sulphuric acid using an automatic tilt measure in

ii) NITRIC ACID

III) SODIUM CARBONATE

IV) CAUSTIC SODA

Where V = Volume of oxalic acid used for titration

Dissolve 1 g of starch powder in 20 ml of cold distilled water and add 80 ml of

VI) COMMON SALT:

Moisture, % by weight = (W1-W2) x 100

VII) SOAP OIL: A) DETERMINATION OF TOTAL SOLIDS:

V111) CAUSTIC (LYE) STRENGTH:

1X) NITRIC ACID SOLUTION STRENGTH:

6.3 x Burette reading x N

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