FL Sop

PROCEDURES
PREPAIRED BY:- ZAFAR IQBAL

Estimation of carbon in steel alloys
PROCEDRUE
5.1 PRE-OPERATIONAL 5.1.1 Furnace temperature from 1200 to 1300
0
C.
5.1.2 Sample combustion boats should be pre-heated.
5.1.3 Steel samples should be already degreased.
5.1.4 Gas purifying system between the gas cylinder and the furnace should be perfect.
5.1.5 Rubber connections of all the system should be OK and all the system should be leak
proof.
5.1.6 Furnace combustion tube should be in good condition.
5.1.7 Acidified (Red colour) water in the bottle and in the burette should be at the same level
5.2 PROCEDURE
Take 1.0 gm. sample in the pre heated combustion boat, and insert this boat in the furnace combustion
tube. Close the combustion tube with rubber cork attached with delivery tube to burette. After two
minutes( when the sample has been fused.) slowly pass on oxygen gas, and collect CO
2
gas + O
2
gas from
the combustion tube in the burette of the apparatus, which will be revealed by the drop of coloured
(Acidified) water level from the burette to the bottle. Then let the collected gas of the burette to pass
through the CO
2
absorbing system.( KOH 45% solution). Then bring back the gas to the burette from the
CO
2
absorbing system by the control of three-(3) ways stopcock. Then determine the decrease in the
volume of the gas on the burette. Note the reading from the calibrated-jacketed burette and multiply by
the factor.Run standard sample and determine the reading for correction factor.

Burette reading
Weight of the sample taken
FACTOR: (A) Note the room temp. in C
0
. (B) Note the Barometric pressure C) Determine the
Factor with help of reading A & B on the provided chart with the strohlein apparatus as Annex B.

6. SAFETY MEASURES
Wear Lab Coat and use cotton gloves during analysis
C% = X Factor
PROCEDURES
Estimation Manganese In Steel Containing
High Chromium, Vanadium & Cobalt
5. PROCEDRUE5.1 Reagents
i- H
2
S0
4
1:3
ii- HNO
3
1:2 sp.gr.
iii- Sodium Arsenite. Dissolve 4.5 gm of sodium Arsenite in one liter of water containing 5
gm of sodium Bi Carbonate.
5.2 Procedure
Dissolve 0.1 gm of the sample in 30 ml of 1:3 H
2
SO
4
.Add 5 mls of HNO
3
of
sp.gr.1.2.When the solution is complete or nearby complete. Boil
until brown fumes disappear then cool. Make a paste of Zinc oxide
with water. Add this paste till the supernatant liquid is milky. Dilute
with 25 ml water
Filter and wash three times. To the filtrate add 20 mls of HNO3 of sp.gr. 1.2 heat and add 10 ml of
AgNO3 1% and 10 ml of(NH4)2 S208 10%. When the colour is fully developed transfer to a cold water
bath and add 20 mls of cold water. When thoroughly cold, add 5 ml of 1% NaCl solution and run
standard Arsenite solution until pink colour is discharged. Similarly carry out standard sample for
comparison.

Mn % in Std.sample x Sodium Arsenite mls. used for sample.
Sodium Arsenite mls used for Std.sample.
6. SAFETY MEASURES

6.1 Wear Lab Coat and use Safety Goggles during analysis.
6.2 The analysis should be done in fuming Chamber.
6.3 Dispose off the sample after neutralization

Mn % =
PROCEDURES

Estimation Of Manganese In High Manganese Steel & Ferro Manganese
5. PROCEDRUE
5.1 REAGENTS
5.1.1 Dilute HNO
3
1.2 Sp. gr.
5.1.2 KMnO
4
Solution = N/10 Normality
5.1.3 Std. Oxalic Acid solution = N /10 Normality ( 6.3 gm /litr)
5.1.4 Dilute H
2
SO
4
1.20 sp. gr.
5.2 PROCEDURE
Weigh 0.25gm of the sample in 400-500 C.C. tall beaker. Add 30CC. dil. HNO
3
and
place on the hot plate. When completely dissolved add 60 mls of Conc. HNO
3
&
cool to room temp. Then continuously add 6-7 gm of potassium Chlorate. Stir.
Heat again on a hot plate for 15-20 minutesRemove from the hot plate and dilute
with hot water to about 100 mls. Then Filter through asbestos pad. wash with hot
water till free from Ferric salts and Nitric Acid. Transfer the asbestos pad with
precipitate into a 500 mls flask.
(a) For Manganese Steel:- Add 50CC of N/10 Oxalic Acid.and 20CC OF H
2

SO
4
(b)For Ferro manganese add 150 c.c. N/10 oxalic acid and 40 c.c. H
2
SO
4
Heat 70
0
C, Stir till brown particals disappear. Titrate against N/10KMNO
4
solution until
pink colour exists for 40 seconds.

CALCUALTION
(A -B) x 0.11
Wt. of sample.
A= Volume of N/ 10 Oxalic acid a

Mn%=
PROCEDURES

Estimation Of Nickel From Steel (Di Methylglyoxime Precipitation)

5. PROCEDRUE:
Dissolve 1.0 gm of sample in 40 CCS of Hydrochloric Acid, Oxidize the iron with
2CCS of HNO
3
, boiling for half a minute, dilute and filter if necessary. Further
dilute the filtrate to about 300 CCS. add 2 gms of tartaric Acid or Citric Acid. Heat
the solution to about 50
0
C, and add the 1% soln. of Di methylglyoxime reagent 25
mls. Make the mixture faintly but distinctively ammonical, ascertain that the
precipitation is complete by the addition of more reagents and digest the mixture
at the same temperature for 5 minutes.
Filter and wash the precipitate with water containing a little Ammonium
Nitrate. Transfer to a crucible and ignite with carefully at 750
0
C and weigh
as oxide.

Ni% = Wt. of the ppt. x 78. 58

PROCEDURES

Estimation Of Copper in Steel

5. PROCEDRUE

5.1 REAGENTS

Sodium Thiosulphaate (N /20) Standardize against Electrolytic copper foil.

5.2 PROCEDURE

10 gms of the sample is to be dissolved in 75 CCS (1:4) H
2
SO
4
.Dilute to 300
CCS.Boil and add cautiously 6 gms. of Sodium Thiosulphate and boil for 10
minutes (Cu & Mo ppt ). Filter and wash well with hot water or H
2
S water.
Ignite at low temperature (600
0
C). Transfer oxides to a beaker. Dissolve in 5
CCS of HNO
3
, dilute and add 5 gms. of Ammonium Chloride, boil neutralise
with Ammonia solution and filter wash with hot water. Make it filtrate
acidic with Acetic Acid and add 2.0 gms of Potassium Iodide. Shake it well
and titrate with standard sodium thiosulphate solution.

mls of N /20 Na
2
S
2
O
3
used
Wt. of sample.

NOTE:
In a alloy Steel carbides are neglected and may be filtered off
Cu%=
X 0.318
PROCEDURES

ESTIMATION OF MOLYBDENUM IN STEEL(VANADIUM ABSENT
5. PROCEDRUE
5.1 REAGENTS
5.1.1 Acid mixture :- 150 mls H2 SO4 (Sp.gr. 1.84)
+150 mls of Phosphoric Acid + 700 mls of H2O.
5.1.2 Sulphuric Acid 25%
5.1.3 Perchloric Acid 10% Solution.
5.1.4 Sodium Sulpho Cyanide. 10% solution
5.1.5 Stannous chloride 10% solution (freshly prepared).
5.2 PROCEDURE

Take 1.0 gms of the sample in 250 mls conical flask. Add 15 to 20 mls of Acid mixture and
dissolve, when completely dissolved, oxidize the sample with few drops of HNO
3
. Evaporate
upto 5 mls at moderate temperature
Put the sample solution in 250 mls Volumetric flask and dilute it upto the mark. Shake well for
proper mixing. Treat the standard sample of Molybdum as sample, and make the volume to 250
mls. Now take three volumetric flask cap. 250 mls, which are already thoroughly washed. Take
25 mls of sample solution and standard sample solution in the two volumetric flask and in the
third take 25mls of distilled water as reference Blank. Add the following reagents in all the
three flasks.
(i) H
2
SO
4
25% = 10mls.
(ii) Perchloric Acid 10% =10mls.
(iii) Sodium Sulpho Cyanide 10% = 10mls.
(iv) Stannous Chloride = 10mls.

After 10-15 Minutes measure the Aborbance % of all these three specimens on Spectronic at
wavelength 465nm. (Spectonic 20 warm up time = 1/2 Hours)
Molybdnum % of Std. x Aborbance % of Sample.
Aborbance % of standard sample
Mo % of the sample =
PROCEDURES

Estimation Of Phosphorous In Carbon Steel

5. PROCEDRUE
REAGENTS

5.1.1 Potassium Permanganate solution (25 g / L)
5.1.2 Ammonium Molybdate Solution : Transfer to an 800 ml, beaker 65gm of ammonium
heptamolybdate (NH
4
)
6
Mo
7
O
24
, 4H
2
O), 225 g. of NH
4
NO
3,
15 ml Of NH
4
OH, and 600 ml of
water. Stir and heat gently, when the crystals have dissolved, filter (without washing),
and dilute to 1 liter with water.
5.1.3 Standard sodium Hydroxide solution (0.15 N)
(1 ml = 0.0002 g. Phosphorous approximately.
Dissolve 50 gm of NaOH in 50 ml water and transfer to a large test tube, taking care not
to wet the top. Stopper tightly and let stand in vertical position until supernatant liquid
is clear. Carefully withdraw about 7.5 ml of the clear liquid with a pipette and run it
into one litre of freshly boil and cooled water. Mix well and store away from contact
with air
5.2 PROCEDURE
Transfer 2 g of sample to a 500-ml Erlenmeyer flask. Dissolve the sample in 65 ml of HNO
3
(1:3)
and oxidize organic matter by adding 10 ml of KMnO
4
(25 g per lit) and boiling for 2 to 3 min. If
no precipitate forms, add more KMnO
4
and boil again.
Dissolve the precipitate by adding H
2
SO
3
drop by drop, and boil for a few minutes to expel
oxides of nitrogen. Adjust the volume to 60 ml and the temperature to 45
o
C, and add 50 ml of
ammonium Molybata solution. Stopper the flask, shake for 10 min, and allow the precipitate to
settle for20 min. at room temperature. Filter through a 9-cm. Close-texture paper.

Wash the flask, precipitate, and paper twice with 5-ml portions of HNO
3
(2:98) and then five
times with 5-ml, portions of KNO
3
(10 g / L). Finally, wash the paper about ten times (until free
of acid), directing the jet of KNO
3
solution around the edge of the paper and then spirally down.

PROCEDURES

Return the paper and precipitate to the flask, add 25 ml of water and a 2 to 5-ml excess of NaOH
(1ml = 0.0002 g), both free of CO
2
and shake or stir until the precipitate is dissolved. Dilute to
about 150 ml with water free of CO
2
, add 3 drops of phenolphthalein indicator, and titrate with
the standard HNO
3
to the disappearance of the pink color.
Blank: Make a blank determination, following the same procedure and using the same amounts
of all reagents.
Calculation
Calculate the percentage of phosphorus as follows:
Phosphorus % = [(A-BC)-(D-EC)]F / G x 100
Where:
A = milliliters of NaOH solution required by the sample
B = milliliters of HNO
3
required by the sample.
C = milliliters of NaOH solution equivalent to 1 ml of the HNO
3.

D = milliliters of NaOH solution required by the blank
E = milliliter of HNO
3
required by the blank.
F = Phosphorus equivalent of the NaOH solution, in g / ml
G = Grams of sample used.

PROCEDURES

Estimation Of Vanadium In Steel
5. PROCEDRUE
5.1 METHOD-I
5.1.1 (For steels containing over 0.2% Vanadium)
The method is most conveniently operated on the titrated solution remaining after a chromium
determination by either the vignal or persulphate process. Best results are obtained on steels
containing over 0.2% Vanadium. Below this value errors due to blank values, coupled with the
high Vanadium factors of the O.1KMnO
4
solution because more significant and it is normally
better in such cases to determine the vanadium by a modified method (Method .2There is very
little interference from other elements. Cobalt may be present upto 15% with out seriously
prejudicing the detection of the end point
Chromium in excess of 4% increase the uncertainty of end point for the determination of "V"
and in accurate work, corrections for increasing "Cr" contents must be made. high speed and
most other types of Cr, V, steels come within the scope of this method. Rust less and other high
chromium steels containing vanadium require special treatment. very low Vanadium contents
such as are found in Cast Iron, etc, also require special methods, calorimetric finish being used.
5.1.2 Notes on Solutions Required
Potassium Ferricyanide. Take a tiny crystals of K Fe3 (CN6)Potassium Ferricyanide, only a little
large than pin head, rinse quickly with water and discard the rinsing. Dissolve the remaining washed
crystals with sufficient water to give a very pale yellowsolution. (Potassium Ferrocyanide is not
satisfactory)
5.1.3 PROCEDURE
To the solution remaining after the determination of Chromium add 0.1 N Ferrous Ammonium sulphate
solution from the burette until the vanadium is completely reduced to the quadrivalent condition, as
indicated by the appearance of blue colour, when a trace of the solution is withdrawn on the end of a
glass rod and" spotted " externally with a very weak solution of Potassium Ferricyanide (The blue
colour indicates the presence of excess Ferrous Iron.) Then add a further 2 mls. of Ferrous Ammonium
Sulphate solution.

A further external spot test should now give a very distinct blue colour immediately with
potassium Ferricyanide. Add 5 mls of H3 PO4 (Sp. gr. 1.75) if Chromium has been determined
by the Viginal method.( This is unnecessary if the persulphate method has been used, since

PROCEDURES

H3PO4 is already present in this case), and add 5mls. of freshly prepared Ammonium per
sulphate solution
Shake well and allow to stand for two minutes (or until an external spot test no longer shows
the reaction for ferrous Iron). This oxidises all the Ferrous sulphate but leaves the Vanadyl
sulphate un oxidized. Titrate the Vanadium with Std. O.IN KMnO
4
solution until end point is
obtained which persist on shaking for at least 60 seconds after the last addition. Note the
KMnO
4
reading only. The Ferrous sulphate addition is disregarded since it is merely used for
reducing the Vanadium to quadrivalent condition and takes no part in the final titration.
5.1.4 BLANK CORRECTION This is in general, a function of the coloured elements
present in solution. It could best be assessed by determining the amount of per manganate
necessary to give an end point, similar to that observed in the test but on a solution of a steel
free from vanadium but other wise similar to the steel under test. In practice, Chromium
appears to be the chief cause of blank and it is generally sufficient to deduct a blank calculated
as follows, provided that the first pink tinge is taken as end point.
5.1.5 BLANK
( 0.05 + ( 0.025 x % Cr present) Mls e.g. with 4% Cr
present blank = -O5 + (4 x .025) = 0.15 mls
Alternatively the blank may be assessed by adding about 0.2 mls excess permanganate to the
solution after titration, boiling for 10 minutes, cooling to room temp. and again titrating with
permanganate to the same tinge at which the first end point was assumed
This final titration represent the blank, calculation: deduct the blank
titration from the KMNO
4
titration. The difference represents the
0.1 KMNO
4
equivalent of the oxidation. Since 1 ml of 0.1 N KMNO
4
= .0051 gm.
Vanadium, the Vanadium contents is given by
% Vanadium (ml of 0.1NKMNO4-mls of Blank) x.0051 x 100
Wt. of the sample taken.

PROCEDURES

5.2 METHOD-2

Volumetric method with Ferrous sulphate titration(Based on
method by W. B.Shaw Metallurgical, Feb.1951
5.2.1 DISCUSSION
The method is best applied for the determination of Vanadium only, and not as an addition to a
chromium determination, Although it may be applied after a vignal or persulphate
determination of chromium by modification of the conditions. It is applicable to all steels with
out modification except those containing W in W Steel, the W must be removed. It is more
useful than method I in that an accurate figure may be obtained on low vanadium steel
by virtue of the fact that the end point is clearly defined and that solution weaker and
decinormal are used, thus giving a more favourable factor.

5.2.2 SOLUTION REQUIRED

5.2.2.1 Sulphuric-Phosphoric Acid mixture
If no solution is available, a suitable mixture for 2 gm. sample can be prepared
by adding 15 mls of H
2
SO
4
(Sp.g. 1.840 and 11 mls H
3
PO
4
(Sp.gr 1.75) to 50 mls
of cold water and mix it well.

5.2.2.2 Dilute Sulphuric Acid (1:1) Add 500 mls H
2
SO
4
Sp.gr. 1.84 very carefully to 500
mls of water mix it well, cool and dilute to one litre, and mix again.

5.2.2.3 Dilute Phosphoric Acid ( 1:1) Add 500 mls of H
3
PO
4
(Sp.gr. 1.75) to 500 mls.
water, mix it well, cool, dilute to one litre and mix it again

5.2.2.4 1% KMNO
4
solution This is strong solution.

PROCEDURES

5.2.3 PROCEDURE

Weigh 2.0 gm. sample into 750 mls flask add 75 mls of (H
2
SO
4
-H
3
PO
4
) mixture. Heat to dissolve
then oxidize with HNO
3
(Sp.gr. 1.42) (If not free from carbide at this point evaporate the
solution to fumes and boil again in a litre water). Cool down to room temp. and then dilute to
200 mls. Add 1% KMnO
4
solution drop by drop, until the solution remain, pink but avoiding the
large excess. Allow to stand for two minutes,If fading occurs, add two drops ;further and let
stand for further two minutes. Then add 20 drops ( counted). of 0.5% NaNO
2
and swirl. Allow to
stand for 20 seconds. Then add 5 mls of 10% sulphuric acid and swirl again. Add 10 drops of 0.2%
Barium diphenyl amine sulphonate solution, Allow to stand untill violet colour appears and run in
from a burette sufficient 0.0392 N Ferrous ammonium sulphate solution to remove the violet
colour and add 2 mls in excess. Back titrate the excess of Ferrous ammonium sulphate solution
with .0392N K
2
Cr
2
0
7
solution to a full violet end point.

5.2.4 STANDARDIZATION OF FERROUS AMMONIUM SULPHATE
SOLUTION

Run 20 mls of the Ferrous solution into a flask containing a mixture of 10 mls of dil.H
2
SO
4
(1:1,
10 mls of dil H
3
P0
4
(1:1) and 20 mls of H
2
O. Add 2 drops of 0.2% Barium diphenylamine-
Sulphonate and then titrate to a full violet colour with .0392N K
2
Cr
2
O
7
solution.

Factor of Fe SO
4
= Mls. exactly.0392N Potassium Dichromate
(NH
4
) SO
4
mls.Approx. .0392N Ferro ammonium
sulphate
5.2.5 CALCUALTION

The volume of Fe
2
S0
4
solution used is corrected by the multiplication by the factor.This Volume,
less the volume of K
2
Cr
2
O
7
std. used, gives the volume of .0392 N Fe
2
SO
4
solution used to
reduce the "V" from the V
2
0
5
state to V
2
0
4
state. Each ml, used is equivalent to .002 gm "V" or.
1% "V" on a 2gm. sample.
5.2.6 SPECIMEN CALCULTION

Vanadium in Steel = mls of .0392 N Fe SO
4
x .002 x 100 = % Vanadium
Wt. of the sample.

PROCEDURES

Chemical Analysis Of Ferro Vanadium
. 5. PROCEDRUE
5.1 VOLUMETRIC METHOD :Transfer 0.5095 gm of the sample to an 800 ml.
flask, add 70 ml. of dilute sulphuric acid 1:6 and digest until vigorous action
subsides. Add dropwise 3 ml, of nitric acid (sp.gr. 1.42) and digest until
complete decomposition is obtained (note 3). Dilute to 250 ml. with
hot water, heat to boiling and add potassium permanganate solution(1.2 per
cent) until a pink colour persists, followed by 3 drop in excess. After boiling for 15
minutes, clear the solution by drop wise addition of saturated FeSO
4
or
sulphurous acid and again boil until sulphur dioxide is completely expelled. Add
50 ml. of dilute sulphuric acid (1:6) dilute to 350 ml. and cool
Prepare the solution for titration by adding N/10 potassium permanganate
dropwise until a permanent pink colour is obtained and persists for 1
minute. Remove the pink colour of potassium permanganate by cautious
addition of sodium nitrite solution (5 per cent), the excess of which must be
less than 5 drops. Add 2 gm. of urea and allow standing for 5 minutes.

Add 5 ml. of hydrofluoric acid and 10 drops oxidised diphenylamine sodium
sulphonate indicator. Allow the purple colour to develop and titrate with N
/10 ferrous ammonium sulphate until the colour just changes to green.

Vanadium %age.= _________A__________ X .5095
Wt. of sample taken

Where A= ml. of N/10 ferrous ammonium sulphate.

PROCEDURES
NOTES
(i) The sample must be ground to pass a 60 mesh sieve.

(ii) The addition of 2 ml. of hydroflouric acid towards the end of
the initial reaction assists decomposition particularly of
samples of high silicon content. After oxidation, evaporate to
fumes, re dissolve in water and proceed with the potassium
permanganate treatment.

(iii) Occasional Ferro-Vanadium alloys yield a slight insoluble
residue, which, after filtration and ignition, must be fused with
2 gm. of sodium carbonate and 0.1 gm of potassium

PROCEDURES

Estimation Of Ferro Silicon

5. PROCEDRUE
5.1 SODIUM PEROXIDE FUSION.
Transfer 0.4672 gm. of finely grounded sample to a nickel crucible containing 8
gms. of sodium peroxide and 4 gms. of sodium carbonate.Mix intimately, the
sample and fusion mixture, cover the crucible and warm gently on the hot plate for
5 minutes Fuse the mixture over a low flame while imparting a gentle swirling
motion to the crucible. After holding molten for 3 minutes, increase the
temperature to bright red for 1 minute and allow to cool.

Place the crucible in a suitable platinum or nickel dish and rinse the crucible
lid with a jet of hot water. Continuously add hot water to the covered
platinum or nickel dish until the crucible is just submerged.

Warm gently until the melt is extracted, remove and rinse the crucible.
After cautiously acidifying the alkaline extract by addition of 40 ml. of
hydrochloric acid (sp.gr. 1.16) transfer the solution to a porcelain dish, 8
inch. diameter, and if hydrated manganese dioxides remains un-dissolved,
clear the solution by addition of 5 ml. of saturated sulphurous acid.

Evaporate to dryness on a water bath and bake for 1 hour in an oven
thermostatically regulated to a temperature of 105
0
to 110
0
C. Maximum.
Cool moisten with 20 ml. of hydrochloric acid (1:1) and after 1 minute add
150 ml of hot water, stirring until the salts are completely in solution. Filter
on a pulp pad and collect the filtrate in a 600 ml squat beaker. Rinse the
porcelain basin with warm dilute hydrochloric acid ( 5:95) detaching the
silica by means of a bobby.

Wash the paper six to eight times with warm dilute hydrochloric acid (5:95),

PROCEDURES

twice with warm dilute sulphuric acid (5:95) and finally ten times with hot
water Transfer the paper and residue to a platinum crucible and dry in the
air oven.

To the filtrate add 10 gms. of ammonium chloride, heat nearly to boiling
and make alkaline with a slight excess of dilute ammonium hydroxide (1:1)
Digest for 1 minute and filter the precipitate of hydroxides plus silica on a
whatman No.541 paper, 15 cms., washing twice with hot water. Wash the
ppt. from the paper into the original 600 ml. beaker, dissolve in 50 ml of dil.
sulphuric acid (1:1) and evaporate to fumes of sulphur trioxide. After
cooling slightly, add 150 ml. of warm water and heat to redissolve the
soluble salts. Filter on paper pad, wash with hot dilute hydrochloric acid
(5:95) and cold water and add the pad to the main ppt. in the platinum
crucible.
Heat at a low temperature until the paper is completely ignited and finally
at 1100
0
C. to constant weight. Cool the crucible in a newly charged
desiccator and weigh as quickly as possible. Moisten the residue with 2 ml.
of sulphuric acid (1:1) and 10 ml of hydrofluoric acid, evaporate to low bulk
treat with a further 5 ml. of hydrochloric acid and evaporate to dryness.
Ignite at 1100
0
C. Coup and weigh as B.

Carry out a blank determination under similar conditions and correct the
silicon content of the sample for the blank value.
Silicon per cent __________A-B___________ X 46.72
Wt. of sample taken.
Where A - B Wt. of silica SiO
2
.

PROCEDURES

5.2 NOTES

5.2.1 The sample should be ground to pass 60 mesh and finely
floured in an agate mortar. Use 0.9344 gm. sample for silicon
manganese alloys.
5.2.2 A suitable size of crucible is 2 in. diameter by 1
3
/4 in. high. Iron
crucibles of the Armco type are equally satisfactory.
5.2.3 This preliminary heating is necessary to expel moisture and so
avoid spattering in the subsequent fusion.
5.2.4 The fusion is conducted cautiously at a dull red heat, with a
gentle swirling motion while the contents of the crucible
slowly melt down without spattering. The gentle rotation is
maintained for the full fusion period to strip up the material
from the bottom or sides of the crucible.

5.2.5 After removing from the burner, continue the general rotation
so that the melt solidifies as a thin layer on the sides of the
crucible.
5.2.6 The crucible should be finally rinsed and bobbied with hot
dilute hydrochloric acid (1: 9) adding the washings to the main
acidified extracts.
5.2.7 With a platinum dish, the alkaline extract should be cooled and
treated with 20 ml. of saturated sulphurous acid, before the
addition of hydrochloric acid, to prevent attack on the dish.
PROCEDURES

when a platinum dish is used, it is not necessary to transfer the
acidified solution to a porcelain dish for the subsequent
evaporation.
5.2.8 During evaporation, stir frequently with a flat glass rod,
particularly when nearing dryness, and when dry crush the
separated salts to a powder before baking.
5.2.9 Removal of sodium salts is facilitated by washing with hot
water.
5.2.10 The weighing must be carried out as quickly as possible on
account of the hygroscopic nature of the silica residue. A
correct weight is best obtained by first weighing approximately
and there after re-ignition, weighing again, using the first
weight as a guide to attain a balance quickly.

PROCEDURES

Estimation Of Ferro-Tungsten And Tungsten Powder

5. PROCEDRUE

5.1 ACID EXTRACTION.

Transfer 1 gm. of the powdered sample to a weighed 60 ml. covered platinum dish, add 10 ml.
of hydrofluoric acid, followed by dilute nitric acid (Sp. gr. 1.20), a little at a time, keeping the
dish covered as much as possible, until a further addition of nitric acid produces no vigorous
attack on the sample. Digest until decomposition is complete, rinse and remove the cover, and
then add 20 ml. of dilute sulphuric acid (1:1). Evaporate slowly on a sand bath to dense fumes of
sulphur trioxide and fume for 10 minutes. Cool, carefully add 10 ml. of water and 20 ml. of
hydrochloric acid (Sp.gr. 1.160) warm, and transfer to a 600 ml. squat beaker.

Wash the platinum dish with water, dilute to 250 ml. and gently boil for 10 minutes. Dilute to
500 ml. with hot water and allow to settle for a few hours preferably overnight).

Filter on a paper pad, washing with hot, dilute hydrochloric acid (5:95)
followed by ammonium nitrate solution (2 per cent). Remove any tungsten
oxide adhering to the beaker and platinum dish with filter paper moistened
with dilute ammonia (1:1) and clear this paper in the platinum dish before
adding to the principal precipitate of tungsten oxide. Transfer the pad and
main precipitate to the dish dry and ignite to a constant wt. A ( note.2) at a
temperature which must not exceed 800
0
C.

Mix the ignited tungsten oxide ;with 5 gm of sodium carbonate, cover with
a further 3 gm gradually increase the temp. and fuse at 900
0
C. for 5
minutes. Extract in 100 ml. of hot water, Boil for a few minutes and filter on
a paper pad, washing with hot water until free from sodium salts. Ignite in
the original platinum dish, cool, and weigh (B) (note 3).
PROCEDURES

Tungsten percent. = ____________A -B_________ X 79. 30
Wt. of Sample taken

Where A-B = Wt. of tungsten oxide (WO
3
)

5.2 NOTES

5.2.1 A total addition of 10 ml. of dilute nitric acid
(Sp.gr. 1.20) is usually sufficient.
5.2.2 The weight of residue is an approximate measure
of the tungsten content of the sample.
5.2.3 Weight B must be corrected for the weight of
residue obtained from 8 gms of sodium carbonate
in a blank determination.

PROCEDURES

Chemical analysis Of Ferro Molybdenum
5. PROCEDRUE5.1 LEAD MOLYBDATE PRECIPITATION
Transfer 0.5 gm. of sample to a 250 ml. tall form beaker, add 10 ml of dil. nitric acid (sp. gr. 1.20)
and digest below boiling point. After action has ceased, add 4 ml. of hydrochloric acid (sp.gr.
1.16) boil gently for 5 minutes allow to cool and dilute with 20 ml. of water.
Transfer the solution to a tap funnel, washing with hot water.Run the
molybdenum solution dropwise into 200 ml. of nearly boiling sodium
hydroxide solution(10 per cent) contained in a 600 ml. conical flask. The
sodium hydroxide solution must be stirred vigorously during the addition of
molybdenum solution.
After cooling to room temperature, dilute to 500 ml. in a graduated
flask.
Transfer to a dry tall-form,600 ml. beaker, mix, allow to settle for 5 minutes
and filter through a double whatman No. 54 paper, 15 cm.(After
discarding the first runnings, collect 200 ml. of the filtrate in a graduated
flask, and transfer to a 600 ml. tall form beaker, acidifying with 30 ml. of
hydrochloric acid (Sp. gr. 1.16). Boil, add 80 ml. of lead acetate solution (4
per cent.) and while still boiling make dropwise additions of dilute
ammonium hydroxide (1:1) Until a faint turbidity persists. Clear the solution
with 8 or 10 drops of hydrochloric acid (Sp.gr. 1.16) and add 50 ml. of
boiling ammonium formate solution (30 per cent). Continue boiling for 5
minutes, allow to settle and filter on a Whatman No. 40 paper, 15
cm.washing with hot ammonium acetate solution (2 per cent). Ignite the
paper and residue cautionsly in a porcelain crucible at a temperature not
exceeding 650
0
C.
After cooling dissolve the residue by heating gently with 40 ml. of dilute hydrochloric acid
(1:1)contained in a 200 ml.beaker.Filter through a Whatman No.40 paper, 11 cm. into a 600 ml.
beaker, washing with hot dilute hydrochloric acid 5:95). Dilute to 300 ml. with boiling water, add
two drops of methyl red indicator (0.1 per cent). and make just alkaline with ammonium hydroxide
(1:1). Reacidify with hydrochloric acid ( 1:1) adding 10 ml. of acid in access, and boil to clear the
solution. Repercipitate the lead molybdate by dropwise addition of ammonium hydroxide and
hydrochloric acid, followed by ammonium formate solution as described in the previous paragraph.

PROCEDURES

Filter on a Whatman No. 40 paper, 15 cm. washing with hot ammonium acetate solution (2 per
cent). Transfer the paper and residue to a porcelain crucible, dry ignite cautiously at a
temperture not exceeding 650
0
C..Cool and weigh as lead molybdate.

Molybdenum per cent. = A x 26.13
B
Where A = Wt. of lead molybdate.
B = Wt. of sample represented by the fraction
taken after the sodium hydroxide separation.

5.2 NOTES

5.2.1 The entire sample must be ground to pass a 60-mesh sieve separated into
coarse and fine portions on a 200-mesh sieve, and each portion weighed. The
sample for analysis must comprise proportionate weights of each fraction.
5.2.2 Complete the washing of the 250-ml. beaker by rinsing with
hot sodium hydroxide solution, and add this to the main
sodium hydroxide solutions.

PROCEDURES

Chemical analysis Of Ferro Manganese

5. PROCEDRUE

5.1 ESTIMATION OF MANGANESE (BISMUTHATE METHOD)

Transfer 0.275 gm of sample to a 300 ml. R..B. flask, add 40 ml of dilute
nitric acid (Sp. gr. 1.2) and digest until complete solution is obtained . Boil
to expel nitrous oxides, cool slightly and add sodium bismuthate in small
portions ( i.e. 0.25 gm) until on subsequent boiling, a brown precipitate is
obtained. Clear by the addition of a few drops of saturated sulphurous acid
and boil for 2 minutes. Dilute to 100 ml. with 2% nitric acid and cool to
15
0
C.
(With ferro- manganese sample i.e. manganese content 70 to 80%, )
dilute the solution to 500 ml. in a graduated flask, mix well and withdraw a
100 ml fraction into a 400 ml flask. Add 15 ml of nitric acid ( sp.gr. 1.2) boil
for 2 or 3 minutes and cool to 15
0
C.)
Add 2 gms of sodium bismuthate, shake vigorously and allow standing for 2
minutes. Filter through a prepared asbestos pad washing with cold dilute
nitric acid (2: 98) until the washings are colourless,
Titrate with N /10 ferrous ammonium sulphate until the pink colour
disappear, add 2 to 3 ml. in excess and back titrate with N /10 potassium
permanganate until a faint pink colour is obtained.

PROCEDURES

Manganese percent.= _______A -B_________X 0.11
Wt. of sample.
Where A= ml. of N /10 Ferrous Ammonium Sulphate.
B= ml. of N /10 Potassium permanganate.
NOTES
i. With manganese content less than 10% use 0.55 gm sample.
ii. Ferro-manganese samples should be finely agated. A-60- mesh
sample is usually sufficient for Spiegel alloys
iii. The asbestos pad should be washed thoroughly before use with
dilute nitric acid (1: 9) containing a little potassium permanganate,
and finally, with dilute nitric acid(2:98) until the washings are
colourless.

5.2 ESTIMATION OF SILICON (SULPHURIC ACID METHOD)

Transfer 0.9344 gm of sample ground to pass a 60-Mesh sieve, to a
400 ml. squat beaker and dissolve by gently digesting with 50 ml. of
dilute sulphuric acid (1:4). Add 20 ml. of dilute sulphuric acid (1:1)
and evaporate to fumes of sulphur trioxide. Cool add 10 ml. of dilute
sulphuric acid (1:4) and 150 ml of cold water. Warm until soluble
salts are in solution and oxidise with dropwise additions of nitric acid
(sp.gr. .1.42).Cool, add 40 ml of dilute hydrochloric acid (1:1) Dilute
to 150 ml. with hot water and heat to boiling.
Filter on an ashless filter pad, washing the filter free of iron salts with hot
hydrochloric acid (1:9) and cold water alternately. Detach the silica adhering to

PROCEDURES

the sides of the beaker by means of a bobby. Transfers the residue and pad
to a platinum crucible, dry ignite at 1100
0
C, cool and weigh (A). Treat the residue
with 1 ml of sulphuric acid ( 1: 4) and 2 ml.of hydrofluoric acid. Evaporate to
dryness, ignite cool, and weigh (B).
Silicon percent. = _______A -B_______x 46.72
Wt. of sample taken
Where A -B = Weight of Silica (SiO
2
)

PROCEDURES

Chemical analysis Of Ferro Chromium
5. PROCEDRUE
5.1 ESTIMATION OF CHROMIUM
Transfer 0.4334 gm. of sample to a nickel or iron crucible (2 in.dia3/4 in.
high) containing 8 gm. of sodium peroxide and 4 gm. of sodium carbonate Mix
Throughly the sample and fusion mixture and carry out the fusion as for silicon in
Ferro-Silicon.

Cool, transfer the crucible and fused mass to a 800 ml. squat beaker and add hot water until the
crucible is just submerged. Warm gently till the melt is extracted, remove the crucible and lid,
washing with hot water. Boil the solutionBriskly for 10 minutes. Cool the solution slightly and
cautiously acidify with dilute sulphuric acid (1:4) using 50 ml. in excess. Heat to boiling to obtain
complete solution
If pink coloration or brown precipitate is not evident, add potassium
permanganate solution (1.2 per cent.) drop wise to yield a definite pink colour.
Boil for 5 minutes, cool slightly, treat with 5 ml. of manganese sulphate solution
(4 percent.) and boil for a further 5 minutes. cool slightly and filter through an
ignited asbestos pad into a tall, litre beaker, washing with hot water.
After cooling the filtrate, titrate with N/5 ferrous ammonium sulphate and
N/10 potassium permanganate, using an excess of 3 to 5 ml. The addition of 10
drop of disulphine blue or ortho-phenanthroline solution as indicator. The
addition of 10 drops of disulphine blue aqueous solution (0.5 per cent.) produces
an enhanced reddish tint in the titrated solution in the presence of 1 drop excess
of N/10 KMno4.The end point must, however, be approached carefully since
the indicator has a very slight time log of a second or two for full development of
its colour.
The use of 2 drops of 0.025 M ortho-phenanthroline indicator solution gives a
sharp end point in the titration from pink to a clear green colour persisting for 1
minute. Prepare the indicator by dissolving 0.695 gm. of ferrous sulphate crystals
in l00 ml of water. Add l.485 gm of ortho-phenanthroline monobydrate and stir
until dissolved to a dark red solution.

PROCEDURES

Chromium percent. = 2A-B x o.l734
Wt. of sample

where A= ml. of N/5 ferrous ammonium sulphate.
B=ml. of N/10 potassium permanganate.
5.1.2 Notes
5.1.2.1 With low carbon ferrochromium alloys, lightly pound the
sample drilling to pass a 30 mesh sieve. With high carbon
ferrochromium alloys. grind the alloy to pass a 60 mesh sieve.
5.1.2.2 Boiling is necessary to destroy excess peroxide.
5.1.2.3 The use of a burette of 100 ml. capacity for the N/5 ferrous
ammonium sulphate facilitates titration.

PROCEDURES

ESTIMATION OF SILICON
Sodium peroxide fusion for Acid insoluble samples.
Transfer 0.9344 gm. of the 60 mesh sample to an Armeo iron crucible (1
1
/2" dia,
1.3/8 " high) Containing 4 gms of sodium peroxide and 1 gm of sodium
carbonate.Mix intimately the sample and fusin mixture and carry out the fusion
and extraction as for silicon in Ferro-Silicon. Continuously acidify the alkaline
extract with 35 ml of hydrochloric acid (S.G. 1.16) digest until soluble salts are in
solution and transfer to a 800 ml Squat beaker.
Add 50 ml of sulphuric acid (S.G. 1.84) evaporate to fumes and complete
the determination as for silcon in Ferro- Manganese.
"

Chemical analysis Of Zinc And Iron Phosphating Solution

5. PROCEDRUE
5.1 PREPARATION AND WORKING OF PHOSPHATING BATH
5.1.1 The phosphating solution is diluted 33 times with water in the
tank to make working bath.
5.1.2 The strength and free acidity of the bath is regulated between
the limits as shown below:-
Strength (pointage) = 29-32
Free Acidity =10-14%

PROCEDURES

5.2 METHOD OF ANALYSIS OF PHOSPHATING BATH

5.2.1 STRENGTH (POINTAGE)
Take 10ml of the cooled bath solution. Dilute with 50ml of distilled water and
titrate with N/10 NaOH Solution using Phenolphthalein as indicator.
Strength (Pointage) = ml of N/10 NaOH used
5.2.2 FREE ACIDITY
Take 10 mls of cooled bath solution, dilute with 50 mls of distilled water and
titrate with N/10 NaOH solution using Methyl orange as indicator.
Free Acidity = mls of NaOH used x 100
strength

5.3 PERMITTED LIMITS FOR IRON PHO SOLUTION

Strength ( pointage) = 28-32.
Free Acidity = 10-14%

PROCEDURES

Estimation Of Cobalt In Tugston Alloy

5. PROCEDRUE
5.1 REAGENTS
5.1.1 Hydrochloric Acid. (1:1) H C L + H
2
O
5.1.2 Hydrogen Per Oxide. 30 % H
2
O
2
5.1.3 Tartaric Acid (aq.sol.) 30 % C
4
H
6
O
6

5.1.4 Sodium Acetate 50 % CH
3
COONa
5.1.5 Sodium Nitrite 5 % Na NO
2

5.1.6 Sulphuric Acid 1: 1 H
2
SO
4
+ H
2
O
(Sp.gr=1.84)
5.1.7 Nitroso-R-Salt 0.5 % C
10
H
6
N Na O
8
S
2

5.1.8 Sodium Hydroxide 10 % Na OH
5.1.9 Cobalt standard solution 10 ugm/ml
5.1.10 Congo-red test paper
5.1.11 Tungsten matrix solution.
[ 1 g W(99.99 %) + 15 ml H
2
O
2
(2.2) + 20 ml H Cl (2.1) ]
[ + 80 ml C
4
H
6
O
6
(2.3), heat to dissolve, add water to make 1000
ml. ]
5.1.12 Spectrophotometer type 72 or 721.

PROCEDURES

5.2 PRINCIPLE

The sample is dissolved into Hydrochloric Acid with Hydrogen Per Oxide.
Tartaric Acid is added to cover Tungsten. In buffer medium of sodium acetate,
Trivalent Cobalt reacts chemically with Nitroso-R-salt and the reaction is
resulted in red complex compound. Then colorimetric measurement can be
done. By Tartaric Acid covering Tungsten, Copper, Nickel and Iron allowable
value of interfering elements becomes wider to eliminate the influence on
measurement of Cobalt.

5.3 METHOD

Weigh 0.10g sample and put it into a 150-ml conical flask. Pour 2ml
Hydrochloric Acid (2.1) and 10 ml Hydrogen peroxide (2.2) into the conical flask
then heat up.

When reaction is intense remove the conical flask from electric heater, the
sample is automatically dissolved. After the reaction is completed, pour 10 ml
Tartaric Acid solution (2.3) , then heat up until bubbles are formed. Remove the
conical flask from electric heater and cool the solution to room temperature.

Pour the above solution into a 100ml measuring flask. Rinse the conical flask
with water and pour into the measuring flask. Dilute the solution with water
until surface reaches graduation mark, mix up uniformly, test solution is ready
for further processing.
PROCEDURES

Put 10ml above-mentioned solution into a 50ml conical flask. Then pour
sodium Hydroxide solution (2.8) into the flask until Congo-red test paper
become purple. Pour 10-ml sodium acetate solution (2.4) then shake evenly.
Pour 5ml Sulphuric Acid solution (2.6), no need to heat. Transfer to a 50ml
measuring flask. Dilute with water until surface reach graduation mark and
shake evenly.
Measure the absorbance on spectrophotometer using a 3cm calorimetric cell at
525-nm wavelength light.
All operations are carried out on solution of Tungsten matrix, first add Sulphuric Acid
solution (2.6) then Nitroso-R-Salt solution (2.7) as comparison solution to measure
absorbance.
5.4 STANDARD CURVE

Prepare a series of 50ml measuring flasks. Put 10ml Tungsten matrix solution
(2.11) into each flask. Then pour 0,1,2,3,4 & 5 ml Cobalt standard solution (2.9)
respectively into different flask. Do the same operation (3.2) but referring
solution is Tungsten matrix solution with zero ml Cobalt which should be treated
through all above mentioned operations except that Sulphuric Acid solution
(2.6) is added before Nitroso-R-salt solution (2.7). Then measure the absorbance
and draw their standard curves on coordinate paper.

NOTES

(a) If content of Cobalt is more than 0.5 %, less Tungsten matrix solution (2.11)
should be used.

PROCEDURES

(b) Addition of sodium Nitrite speeds up oxidation of bivalent Cobalt and finish
color development at once. No need to heat. The color of complex
compound will not be changed within 10 hours.

(c) Addition of color reagent first and Sulfuric acid second is used to improve
acid degree, to disturb complex compound of interfering Ions and color
reagent, but not to disturb complex compound of Cobalt. The reason for
adding Sulfuric Acid before Nitroso-R-Salt is that complex compound of
Cobalt can not be produced in this condition.
(d) Stability and reactivity of absorbance measured from improving acid degree
by adding sulfuric acid is better than that by adding Nitric acid.

(e) When measuring Cobalt, absorption of trivalent Iron (Fe) makes absorbance
fall down. In order to complete color development shake evenly for 5
minutes after adding Sulfuric acid then measure the absorbance.

Estimation Of Manganese In Tugston Alloy

5. PROCEDRUE

5.1 REAGENTS

5.1.1 Sulfuric acid. (Sp.gr.= 1.84) H
2
SO
4

5.1.2 Phosphoric Acid (Sp.ge= 1.70) H
3
PO
4

5.1.3 Nitric acid (Sp.gr= 1.42) H N O
3

5.1.4 Sodium Nitrite (aq.sol.) 4 % Na NO
2

PROCEDURES

5.1.5 Potassium periodate sol. 5 %
[ Put 50 g potassium periodate in 100ml water, add 160 mls Nitric
Acid(2.30) Heat for solving. After complete dissolution. Cool to room
temperature then dilute with water to one liter.
5.1.6 Manganese standard solution : 0.05 mg/ml

5.2 PRINCIPLE

Bivalent manganese in Tungsten alloy is oxidized by Potassium periodate as
Oxidant in septa valence manganese. Then calorimetric measurement can
be done
Weigh 0.10g sample and put it into a 150ml quartz conical flask, then pour
6ml Phosphoric acid (2.2) and 5 ml Sulphuric acid(2:1) into the conical
flakes. Heat on high temperature position of electric heater to dissolve the
sample ( when thick smoke appears, the sample will be dissolved rapidly).
After complete dissolution, remove the flask form electric heater and cool
it with cooling water. Add 15-ml water and heat on the electric heater again
until slightly boiling. Remove the flask from electric heater. Add 10 ml
Potassium periodate sol. (2.5) and shake evenly. Then heat up for oxidation
and keep 4-5 min after boiling. Remove from electric heater and cool it to
room temperature. Pour the above solution into a 50-ml measuring flask.
Dilute with water to graduation mark and mix up.

Pour test solution in two (2) cm colorimetric cells. Add two drops sodium
Nitrite sol (2.4) in only on of the colorimetric cell for colour fading, it will be
used as reference solution.
PROCEDURES

Measure the absorbance on Spectrophotometer using 530 nm wave
length.

5.4 STANDARD CURVE

Pour Manganese test solution (3.1) 1,2,3,4 & 5 ml into a series of 150 mls
conical flasks separately. The Add 6 ml Phosphoric Acid (2.2), 5 ml sulphuric
Acid (2.1) and 15ml water. Add 10 ml Potassium Periodate sol (2.5) and
operate according to the operation mentioned above (3.1).

Measure the absorbance and draw their standard curve on coordinate
paper.

NOTE

a) When contents of manganese is less than 0.05 % , weigh 0.2000 g
sample and use more Phosphoric Acid. When content of Manganese is
more than 0.125 % use 1 cm colorimetric cell or weigh less sample.
Excessive Phosphoric acid complex a great deal of otherwise Tungstic Acid
settlings will appear which is unfavourable to measurement. In high thick
Phosphoric Acid medium, it is uneasy for
b) Ammonium Persulphate to oxidize bivalent Manganese, so
Potassium Periodate (2.5) should be used.

c)To offset influence of other metal ions faded solution (3.2) is used as
reference solution.

PROCEDURES

Estimation Of Aluminum In Steel
5. PROCEDRUE
5.1 REAGETNS
5.1.1 Hydrochloric Acid
5.1.2 Nitric Acid
5.1.3 Hydro Fluoric Acid
5.1.4 Sulphuric Acid
5.1.5 Ammonium Hydroxide
5.1.6 Sodium Hydroxide 10%
5.1.7 Ammonium Nitrate 5%
5.1.8 Ammonium Chloride

5.2 PROCEDURE

Dissolve 0.5 to 5.0 gram sample in Aqua-regia (3:1 HCL + HNO
3
). Add
20 ml of 10%NaoH to precipitate Iron as Fe(OH)
3
. Filter the solution
through 541 filter paper and wash with 5% NH
4
No
3
solution until
chlorides are removed (Apply sliver Nitrate test to check the
chloride.)Boil the filtrate and neutralize with HCL. Add 5 gm of NH
4
CL
and 15 ml of NH
4
OH
4
to precipitates AL(OH)
3
.
weighed platinum crucible in Muffle furnace at 1000
O
C for 30
minutes. Cool in a desiccator and then treat the precipitates with 5
ml HF acid then add few drops of H
2
SO
4
. Heat the crucible at 700-800

PROCEDURES

O
C for 10 minutes. Cool in desiccator weight the crucible and note
the weight of precipitates. Dissolve the precipitates in 20 ml of HCL
and shift in 500 ml conical flask then reduce with 10 gm Zn drilling.
Cool and titrate with N/10 KMnO
4

Al% = Wt of ppt (ml of N/10 KMnO
4
X 0.008)
Wt of sample

X 52.94
PROCEDURES

Work Instruction For Preparation Of Standard Solutions And Indicators
.
3. Apparatus/ Material:
Analytical balance, Calibrated Masses and Double Distilled Water.
4. Procedure:

4.1 Cylinder and burette are tested at 05 equally spaced locations over its full
graduation range where as pipette and measuring flask are tested only at one mark.

4.2 Note the ambient conditions.

4.3 Wash/ clean the apparatus to be calibrated with distilled water and dry it
completely.

4.4 Switch On and allow the balance to warm up for the time period
recommended in the technical manual for the balance.

4.5 Place beaker on balance and tare it to zero.

4.6 Fill burette, cylinder, pipette or measuring flask with double distilled
water.

4.7 Pour distilled water into beaker from burette, cylinder, pipette or
measuring flask upto selected reading / mark and note the weight of water.
4.8 Using weight volume table, calculate volume of the water corrected to 23
o
C.This is the measured value of the volume of water.

4.9 Note this measured volume against the nominal (shown by the graduation
mark) value.

4.10 Repeat steps 3.7 to 3.10 five times for each graduation marks.

Calculate uncertainty, if required.

PROCEDURES

4.11 Note the calibration data in calibration data record sheet
(TP-03/ML-04/01 )

4.12 Prepare and issue calibration certificate to the concerned department and
retain office copy of the same for record.

4.13 Affix the status sticker showing date of calibration and next due date on
calibrated apparatus.

PROCEDURES

Work Instruction For Preparation Of Standard Solutions And Indicators

5. PROCEDRUE

5.1 POTASSIUM PERMANGANATE SOLUTION 0.05N

Disslove 1.6 gms of KMnO
4
in about 300 mls of distilled water. filter
on whatman No. 41 and make the solution up to 1000 ml and standardize
against dryed sodium oxalate (A.R).
5.2 FERROUS AMM. SULPHATE SOLUTION 0.05N
Fe SO
4
(NH
4
)
2
SO
4
6 H
2
O
Dissolve 20.0 gm ferrous ammonium sulphate (A.R) in cold water
containing 75 ml H
2
SO
4
(Conc) and make the volume upto 1000 ml with the
help of measuring flask. Standardise it against 0.05N
KMnO
4
solution.
5.3 SODIUM HYDROXIDE SOLUTION 0.15N. Dissolve 6.0 gms. NaOH
(A.R) (avoiding exposure to atmosphere during weighing) in distilled water and
make the volume upto 1000 ml. Standardise it against dried Potassium Hydrogen
Phthalate (A.R)using phenolphthalein as indicator.
5.4 POTASSIUM IODATE SOLUTION 0.03N
Dissolve 1.07 g KIO
3
A.R (Dried 180
o
C to constant weight) in 200 ml
water containing 1.0 g NaOH 10 g KI. When solution is complete
dilute to one liter with water. This is a primary standard use of
theoretical equivalent is satisfactory.

PROCEDURES

5.5 SODIUM THIO SULPHATE SOLUTION 0.05N
(Na
2
S
2
O
3
5 H
2
O)
Dissolve 12.5 gms of the A.R salt in water and make up to 1 litre
and standardise it against Electrolytic Copper foil using starch as
indicator
5.6 NITRIC ACID SOLUTION 0.15N Dilute 10.0 ml clear conc.HNO3 A.R
to 1.0 litres and with distilled water and standardise it against 0.15N.sodium
hydroxide using phenolphthalein as indicator.
5.7 SODIUM ARSENITE SOLUTION (1 ml = 0.0007 g Mn)
Dissolve 20 g of NaAsO
2
in water, dilute to 1 liter, and allow to age for
3 weeks. Dilute 233 ml of the aged solution to 1 liter, and filter if not
clear. Saturate the solution with CO
2
or Sodium bi carbonate.
5.8 BROMO CRESOL GREEN INDICATOR PH.3.6 TO 5.2
Warm 0.l gm with 2.9 ml of N/20 NaoH and 5 mls of absolute
industrial Methylated spirit until dissolved; dilute with industrial
methylated spirit 20% to produce 250mls.

5.9 BROMO CRESOL PURPLE INDICATOR PH 5.2 TO 6.8
warm 0.1 gm with 5ml of absolute industrial methylated spirit until
dissolved ; dilute with l00 mls of industrial methylated spirit 2%, add
3.7 ml of N/20 sodium hydroxide and sufficient spirit to produce 250
mls.

PROCEDURES

5.10 BROMO PHENOL BLUE INDICATOR PH 2.8 TO 4.6

Warm 0.l gm with 3.0 ml of N/20 sodium hydroxide and five mls of
absolute industrial methylated spirit until dissolved; dilute with spirit
20 % to dilute 250 mls.

5.11 BROMO THYMOL BLUE INDICATOR PH 6.0 TO 7.6
Warm 0.1 gm with 3.2 mls of N/20 NaOH and 5 ml of industrial
methylated spirit until dissolved; dilute with methylated spirit 20 %
to produce 250 mls.

5.12 METHYL ORANGE INDICATOR PH. 2.8 TO 4.6
Dissolve 0.04 gm in 100 mls of industrial methylated spirit 20%.

5.13 METHYL RED INDICATOR PH 4.2 TO 6.3
Warm 0.025 gm with 0.95 mls of N/20 sodium hydroxide and 5 ml
of absolute spirit untill dissolved dilute with inductrial methylated
spirit 50 % to prodice 250 mls.

5.14 PHENO PHTHALEIN INDICATOR PH. 8.3 TO 10.0
Dissolve 0.5 gm of in 100 mls of industrial methylated sprite 66.%

PROCEDURES

5.15 PHENOL RED INDICATOR P.H 6.8 TO 8.4

Warm 0.05 gm with 2.85 mls of N/20 NaoH and 5mls spirit until
dissolved, dilute with spirit 20 % to produce 250 mls.

5.16 STARCH INDICATOR

Mix 0.5 gm of soluble starch with 5 mls of cold water, add this
mixture with stirring to 95 mls of boiling water and heat on a boiling
water bath for 5 minutes.

5.17 THYMOL BLUE INDICATOR P.H 8.0 TO 9.6

Warm 0.1 gm with 4.3 mls of N/20 NaoH and 5 mls of absolute methylated
spirit 20% to produce 250 mls

PROCEDURES

Calibration of volumetric glassware

5. PROCEDURE:

5.1 Operates / Material i.e analytical balance, calibrated masses and doubled
distilled are required for calibration.

5.2 Cylinder and burette are tested at 05 equally spaced locations over its full
graduation range where as pipette and measuring flask are tested only at one
mark

5.3 Note the ambient conditions.

5.4 Wash/ clean the apparatus to be calibrated with distilled
water and dry it completely.

5.5 Switch On and allow the balance to warm up for the
time period recommended in the technical manual for the
balance.
5.6 Place beaker on balance and tare it to zero.

5.7 Fill burette, cylinder, pipette or measuring flask with double
distilled water.

5.8 Pour distilled water into beaker from burette, cylinder, pipette or
measuring flask upto selected reading / mark and note the
weight of water.

PROCEDURES

5.9 Using weight volume table, calculate volume of the water
corrected to 23
o
C.This is the measured value of the volume of
water.

5.10 Note this measured volume against the nominal (shown by the
graduation mark) value.

5.11 Repeat steps 5.7 to 5.10 five times for each graduation marks.

5.12 Prepare and issue calibration certificate (MR/4/013) to the
concerned department and retain office copy of the same for
record.

5.13 Affix the status sticker showing date of calibration and next due
date on calibrated apparatus.

FL Sop

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PREPAIRED BY:- ZAFAR IQBAL

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