Limit test for Chlorides

Aim: To perform the limit test for chlorides in the given sample.
Apparatus Required
Nessler cylinders
Glass rod
Stand
Chemicals Required
Dilute Nitric acid (10%)
Silver nitrate (5%)
Sodium chloride
Principle
It is based upon the chemical reaction between silver nitrate and
soluble chlorides in presence of dilute nitric acid to give opalescence of silver
chloride. If the Opalescence produced is compared with the standard solution.
If the opalescence in the sample is less than the standard, it passes the test. If
it is more than the standard, it fails the test.
dil HNO3
Cl-+AgNO3 AgCl + No3
Procedure
Take two 50 ml Nessler Cylinders. Label one as “Test” and the other as
‘Standard’.
Test Standard
Dissolve the specified quantity of the Place 1ml of 0.05845% w/v solution of
substance in distilled water and transfer NaCl and transfer to Nessler cylinder.
Add 10 ml of dil. Add 10ml of dil. Add 10ml of dil.HNO3 . Dilute to 50ml
HNO3. Dilute to 50ml with water and with water and add 1 ml of silver nitrate
add 1 ml of silver nitrate solution. Stir solution. Stir immediately with a glass
immediately with glass rod and allow rod and allow to stand for 5 minutes.
to stand for 5 minutes.

Observation:

Report:
 Limit test for Sulphates

Aim: To perform the limit test for sulphates in the given sample.
Apparatus Required
Nessler cylinders
Glass rod
Stand
Chemicals Required
1. Dilute Hydrochloric acid
2.Barium sulphate reagent.
Mix 15ml of 0.5m BaCl2,55ml of water and 20ml of sulphate free alcohol and
add 5 ml of 0.0181% w/v potassium sulphate. Dilute to 10ml with water and mix.
0.5m BaCl2 Barium chloride in 1000 ml of water.
Principle
It is based upon the chemical reaction between Barium chloride and soluble
sulphate in presence of dilute Hydrochloric acid . The turbidity produced is
compared with the standard solution. Barium sulphate reagent contains barium chloride,
sulphate – free alcohol and small quantity of potassium sulphate. The inclusion of the
small quantity of potassium sulphate in the reagent increase the sensitivity of the test.
Alcohol prevents super saturation and more uniform turbidity develops. If the turbidity
produced in the test is more intense than the standard turbidity it fails the test .
otherwise, it passes the test.
dil Hcl
SO42-+ BaCl2 BaCl2 + 2Cl -
Procedure
Take two 50 ml Nessler Cylinders. Label one as “Test” and the other as
‘Standard’.
Test Standard
Dissolve the sample in distilled water Place 1ml of 0.1089% w/v solution of
and transfer to a Nessler cylinder. Add 2 potassium sulphate and 2 ml of dil. HCI
ml of dilute Hydrochloride acid. Dilute to in a Nessler’s cylinder. Dilute to 45ml
45 ml with water and add 5ml of Barium with water and add 5ml of Barium
sulphate reagent. Stir immediately with a sulphate reagent. Stir immediately with
a glass rod and allow to stand for 5 glass rod and allow to stand for 5
minutes. minutes.

Observation:

Report:
 Limit test for Iron

Aim: To perform the limit test for Iron in the given sample.

Apparatus Required
Nessler cylinders
Glass rod
Stand
Chemicals Required
1. Standard Iron Solution :0.1726 gm of ferric ammonium Sulphate and dissolve
in 10ml of 0.1 N H2SO4 and sufficient water to produce 1000 ml.
2. 0.1 N H2SO4 :4.904 gm in 1000ml of water.
3. 20% Iron free citric acid.
4. Thioglycollic acid
5. Ammonia solution.

Principle
The test depends upon the reaction between ferrous iron and
thioglycollic acid in the presence of ammonia When a pale pink to deep
reddish purple colour is produced. Ferric iron is reduced to ferrous iron by
the thioglycollic acid and the compound produced is ferrous thioglycollate .
Citric acid forms a soluble complex with iron and prevents its precipitation
by ammonia as ferrous hydroxide. Ferrous thioglycollate is colourless in neutral or
acid solutions. The colour develops only in the presence of alkali. It is stable in the
absence of air but fades when exposed to air due to oxidation to the ferric compound.
Therefore the colours should be compared immediately after the time allowed for full
development of colours is over.
 2Fe++ ++ 2CH2SH.COOH 2Fe++ + + S.CH2.COOH
Ferric Iron Thioglycollic acid Ferrous Iron
S.CH2.COO +2H+

CH2SH OCO
++ +
2Fe + 2CH2SH.COOH

Fe +2H+

COO HS- CH2

Ferrous thioglycollate
(Coordination compound )

Procedure
Take two 50ml Nessler cylinders. Label one as ‘Test’ and the others as
‘standard’.

Test
Dissolve a specified quantity of the
substance in 20 ml of water and transfer
to Nessler cylinder. Add 2 ml of a 20%
w/v solution of iron –free citric acid and
0.1ml of thioglycollic acid and mix.
Make alkaline with iron-free ammonia
solution. Dilute to 50ml with water and
and allow to stand for 5 minutes.
Standard
Dilute 2 ml of standard Iron solution with
20ml of water in a Nessler cylinder.
Add 2 ml of a 20% w/v solution of iron –
free citric acid and 0.1 ml of thioglycollic
acid and mix. Make alkaline with iron-
free ammonia solution. Dilute to 50ml
with water and allow to stand for 5
minutes.

Observation:

Report:
 Limit test for Heavy metals

Aim: To perform the limit test for Heavy metals in the given sample.
Apparatus Required
Nessler cylinders
Glass rod
Stand
Chemicals Required
(i) Dilute CH3.COOH(10% v/v)
(ii) Dilute Ammonia (10% v/v)
(iii) Hydrogen sulphide solution (Saturated of H2S).
(iv) Standard lead solution
10ml of the lead nitrate stock solution diluted to 100 ml with water.(20 ppm of
lead). Lead nitrate stock solution
Dissolve 0.1598 gm of lead nitrate in 100 ml of water , add 1 ml of con.
HNO3 and dilute to 1000 ml with water.
Principle
It is based on the reaction between the solution Heavy metals and a
saturated solution of Hydrogen sulphides. In acidic media, it produces reddish /
black colour with Hydrogen sulphide which is compared with standard lead
nitrate solution.
Pb+ H2S Pbs + H2
Procedure
Take two 50 ml Nessler Cylinders. Label one as “Test” and the other as ‘Standard’.
Test Standard
Place 25ml of the solution and adjust 2 ml of standard lead solution is taken
the pH 3-4 by using dilute acetic in a Nessler cylinders and dilute 25 ml
acid or dilute ammonia. Dilute to 35ml with water. Adjust the pH 3-4 by
with water and mix. Add 10ml of freshly using dilute acetic acid or dilute
prepared H2S solution. Dilute to 50ml ammonia. Dilute to 35ml with water and
with water. Mix well and allow to stand mix. Add 10ml of freshly H2S.
for five minutes. solution. Dilute to 50ml with water. Mix
and allow standing for five minutes.

Observation:

Report:
 Assay of Ammonium chloride

Aim – To perform the assay of Ammonium chloride by acid base titration

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Chemicals required – ammonium chloride, distill water, formaldehyde solution,
phenolphthalein indicator, sodium hydroxide solution
Theory – Acid base titration or neutralization titration involves neutralization of acid with
base or base with acid and the end point is determined by means of indicator.
Acidimetry titration – it is a direct or residual volumetric analysis of a base with a standard
acid. Direct titration is performed by introducing a standard acid solution gradually from a
burette into a solution of base being assayed till the end point is obtained e.g. assay of sodium
bicarbonate. Residual titration is used when the rate of reaction between a basic compound
with an acid is slow. In this, the solution of the base is treated with an excess of accurately
measured standard acid and excess acid is subsequently titrated with standard base e.g. assay
of zinc oxide.
Alkalimetry titration – it is an estimation of acid/acidic drugs by titration with standard alkali.
It also includes direct titration and residual/back titration methods as in acidimetry. Assay of
ammonium chloride comes under direct titration method of Alkalimetry titration.
Ammonium chloride is an example of diuretic and systemic acidifier. The assay of
ammonium chloride is based on the principle of formal titration. The formal titration is done
in the presence of formaldehyde. When ammonium chloride is treated with formaldehyde
(HCHO), HCl is liberated. The liberated hydrochloric acid is btitrated with a standard
solution of sodium hydroxide using phenolphthalein indicator.
Procedure –
1. 1 gm of ammonium chloride was accurately weighed and dissolved in 20 ml water.
2. 5 ml formaldehyde solution was added.
3. After two minutes, titration was started slowly with 0.1 N Sodium hydroxide (given
below) solution by using phenolphthalein indicator till pink color was obtained.
Preparation of 100 ml 0.1 N NaOH
Normality Volume Amount Dissolved in
1N 1000 ml 40 gm 1000 ml
0.5 N 1000 ml 20 gm 1000 ml
0.1 N 1000 ml 4 gm 1000 ml
0.1 N 500 ml 2 gm 500 ml
0.4 gm =
0.1 N 100 ml 400 mg 100 ml

The reaction involved is-

HCl + NaOH → NaCl + H2O
Equivalent Factor – 1 ml of 0.1 N NaOH is equivalent to 0.005349 g of NH4Cl
Observation table –
 VOLUMJE
VOLUME OF OF 0.1 N
AMMONIUM SODIUM
CHLORIDE INITIAL FINAL HYDROXIDE
SOLUTION BURETTE BURETTE CONSUMED
S.NO. IN ML READING READING IN ML
33 17 (suppose)
1 25 50 (suppose)

Calculation –
Percentage purity of ammonium chloride =
Volume of 0.1 N sodium hydroxide x equivalent factor x 100 x normality of sodium
hydroxide (actual)
Weight of ammonium chloride in grams x normality of sodium hydroxide (expected)

Result – Assay of Ammonium chloride by acid base titration was carried out and the
percentage purity was found _____%.
 Assay of Copper sulphate
Aim – To perform the assay of Ammonium chloride by acid base titration
Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle: Iodometric determination of copper is based on the oxidation of iodides to iodine
by copper (II) ions, which get reduced to Cu+.
Comparison of standard potentials for both half reactions (Cu2+/Cu+ E0=0.17 V, I2/I-
E0=0.54 V) suggests that it is iodine that should be acting as oxidizer. However, that's not the
case, as copper (I) iodide CuI is very weakly soluble (Ksp = 10-12). That means concentration
of Cu+ in the solution is very low and the standard potential of the half reaction Cu2+/Cu+ in
the presence of iodides is much higher (around 0.88 V).
In effect reaction taking place in the solution is
2Cu2+ + 4I- → 2CuI(s) + I2
and produced equivalent amount of iodine can be titrated with thiosulfate solution.
For the best results reaction should take place in the slightly acidic solution (pH around 4-5),
correct pH is obtained by addition of ammonia and acetic acid, effectively creating acetic
buffer. Lab practice shows that the end point is sharper when we add some thiocyanate to the
solution. Copper (I) thiocyanate is slightly less soluble than iodide, which makes
concentration of Cu+ even lower, increasing the oxidation potential of the Cu2+/Cu+ system.
Solution should be free of other substances that can oxidize iodides to iodine (for example
Fe3+ or nitrates).
reaction
As it was already explained, first reaction taking place is:
2Cu2+ + 4I- → 2CuI(s) + I2
This is followed during titration by the reaction of the iodine with the thiosulfate:
2S2O32- + I2 → S4O62- + 2I-
sample size
For 0.1 M titrant and assuming 50 mL burette, aliquot taken for titration should contain about
0.22-0.28 g of copper (3.5-4.5 millimoles).
end point detection
To detect titration end point we will use a standard indicator for iodine titrations - starch. We
start with a solution containing relatively high concentration of iodine, so indicator has to be
added close to the end point. See iodometric titration end point detection for a more detailed
explanation.
procedure
Procedure below assumes that original solution is acidic or neutral.
 Pipette aliquot containing copper (II) into 250 mL conical flask with a glass stopper.
 Add concentrated ammonia till solution turns dark blue.
 Add concentrated acetic acid till solution loses dark blue color, and then about 3 mL.
 Add 2 g of solid potassium iodide, swirl well.
 Put stopper on the flask and put solution in a dark place for 5 minutes.
 Titrate swirling the flask, until a pale yellow.
 Add 5 ml of the starch solution.
 Add 1 g of potassium thiocyanate.
 Titrate swirling the flask, until blue color disappears.

Report:
 ESTIMATION OF CALCIUM GLUCONATE BY COMPLEXOMETRY

Aim – To perform the assay of calcium gluconate by complexometric titration

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:

Calcium Gluconate is calcium D-gluconate monohydrate. Calcium Gluconate contains not

less than 98.5 per cent and not more than 102.0 per cent of C12H22CaO14,H2O.

Description. A white, crystalline powder or granules.

Preparation and Standardization of 0.05 M Disodium EDTA

 0.05M Disodium EDTA: Weigh accurately about 18.6g of Disodium EDTA, dissolve
it in sufficient quantity of distilled water in 1000 ml volumetric flask and make the
volume upto the mark with the help of distilled water.
 0.05M Calcium Chloride: Weigh accurately about 3.675g of Calcium Chloride,
dissolve it in sufficient quantity of distilled water in 500 ml volumetric flask and make
the volume upto the mark with the help of distilled water.
 Ammonium Chloride: Weigh accurately about 1.68g of ammonium chloride, add it in
14ml of strong ammonium in 250 ml volumetric flask, shake it properly and make the
volume upto the mark with the help of distilled water.
 Standardization of 0.05 M Disodium EDTA: Pipette out 25ml of 0.05M calcium
chloride solution in conical flask. Add 5ml of ammonium chloride solution to it. Add
pinch of modern black indicator and titrate it against prepared disodium EDTA
solution till color changes from wine red to pale blue.

Assay procedure: Weigh accurately about 0.5 g and dissolve in 50 ml of warm water;
cool, add 5.0 ml of 0.05 M magnesium sulphate and 10 ml of strong ammonia solution and
titrate with 0.05 M disodium EDTA using mordant black II mixture as indicator. From the
volume of 0.05 M disodium EDTA required subtract the volume of the magnesium
sulphate solution added.

IP factor: 1ml of the remainder of 0.05M disodium EDTA is equivalent to 0.02242 g of

C12H22CaO14, H2O. C12 H22 CaO14, H2O Ca++ + (C12 H22 O14)-2

Report:
 ESTIMATION OF HYDROGEN PEROXIDE BY PERMANGANOMETRY

Aim – To perform the assay of Hydrogen Peroxide by Permanganometric titration

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:
Hydrogen peroxide is usually treated as a strong oxidizer, but in the presence of even stronger
oxidizer it can become a reducing agent:

H2O2 → O2 + 2H+ + 2e-

Permanganate in low pH is strong enough to quantitatively oxidize hydrogen peroxide to

oxygen. This reaction is used for the determination of hydrogen peroxide concentration.

Reaction taking place during titration is

2MnO4- + 5H2O2 + 6H+ → 2Mn2+ + 5O2 + 8H2O

For 0.02 M titrant and assuming 50 mL burette, aliquot taken for titration should contain
about 0.060-0.077 g of hydrogen peroxide (1.7-2.3 millimoles).

End point detection

As usual in the case of permanganate titrations, pink color of excess permanganate is strong
enough so that there is no need for any other end point indicators.

To perform titration we will need titrant - 0.02 M potassium permanganate solution,

concentrated sulfuric acid (diluted 1:4) and some amount of distilled water to dilute hydrogen
peroxide sample.

procedure
 Pipette aliquot of hydrogen peroxide solution into 500mL Erlenmeyer flask.

 Dilute with distilled water to about 200 mL.

 Add 20 mL of sulfuric acid (1:4) solution.
 Titrate with permanganate solution until a faint pink color persists for 30 seconds.

Report:
 ASSAY OF SODIUM BENZOATE BY NON-AQUEOUS TITRATION

Aim – To perform the assay of sodium benzoate by Non-aqueous titration

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:
Molecular formula : C7H5NaO2 Mol. Wt. 144.1
Sodium Benzoate contains not less than 99.0 per cent and not more than 100.5 per cent of
C7H5NaO2 calculated on the dried basis.
Description: A white, crystalline or granular powder or flakes; odourless or with a faint
odour; hygroscopic.
Preparation of 0.1N solution of HClO4 and its standardization: Dissolve 8.5 ml of
72% HClO4 in about 900 ml glacial acetic acid with constant stirring, add about 30 ml
acetic anhydride and make up the volume (1000 ml) with glacial acetic acid and keep the
mixture for 24 hour. Acetic anhydride absorbed all the water from HClO4 and glacial
acetic acid and renders the solution virtually anhydrous. HClO4 must be well diluted with
glacial acetic acid before adding acetic anhydride because reaction between HClO4 and
acetic anhydride is explosive.

Standardisation of HClO4: To 500 mg of potassium acid phthalate add 25 ml of glacial

acetic acid and add few drops of 5% w/v crystal violet in glacial acetic acid as indicator.
This solution is titrated with 0.1 HClO4. The colour changes from blue to blue green.

1 ml of 0.1N HClO4 = 0.020414 gms of potassium acid Phthalate.

Assay Procedure: Weigh accurately about 0.25 g of Sodium Benzoate, dissolve in 20 ml
of anhydrous glacial acetic acid, warming to 50º if necessary, cool. Titrate with 0.1 M
perchloric acid, using 0.05 ml of 1- naphtholbenzein solution as indicator. Carry out a
blank titration.
Equivalent factor or I.P factor : 1 ml of 0.1 M perchloric acid is equivalent to 0.01441 g of
C7H5NaO2.

Report
 ASSAY OF SODIUM CHLORIDE BY PRECIPITATION TITRATION

Aim – To perform the assay of sodium chloride by precipitation titration

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:

Sodium Chloride NaCl Mol. Wt.: 58.4

Sodium Chloride contains not less than 99.0 per cent and not more than 100.5 per cent of
NaCl, calculated on the dried basis.

Description. White or colourless crystals or a white crystalline powder.

A ssay Procedure: Weigh accurately about 0.1 g and dissolve in 50 ml of water in a

glass-stoppered flask. Add
50.0 ml of 0.1 M silver nitrate, 5 ml of 2 M nitric acid and 2 ml of dibutyl phthalate, shake
well and titrate with
0.1 M ammonium thiocyanate using 2 ml of ferric ammonium sulphate solution as
indicator, until the colour becomes reddish yellow. (Volhards method)
IP factor: 1 ml of 0.1 M silver nitrate is equivalent to 0.005844 g of NaCl.
OR

A ssay Procedure: Weigh accurately about 0.25 g of sodium chloride and dissolve it in 50
ml of distilled water
in conical flask. Titrate the above solution with prestandardised 0.1 N silver nitrate
solution using potassium chromate (5% w/v) as an indicator till color changes from
yellow to red brown.

NaCl + AgNO3 AgCl + NaNO3 Sodium Chloride

K2CrO4 + 2AgNO3 2KNO3 + Ag2CrO4

Potassium Chromate Silver Nitrate Potassium Nitrate Silver

Chromate

Report:
 ASSAY OF POTASSIUM IODATE
Aim – To perform the assay of Potassium Iodate by Redox titration.
Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:

Iodometry is one of the most important redox titration methods. Iodine reacts directly, fast
and quantitively with many organic and inorganic substances. Thanks to its relatively low,
pH independent redox potential, and reversibility of the iodine/iodide reaction, iodometry can
be used both to determine amount of reducing agents (by direct titration with iodine) and of
oxidizing agents (by titration of iodine with thiosulfate). In all cases the same simple and
reliable method of end point detection, based on blue starch complex, can be used.

Reversible iodine/iodide reaction mentioned above is

2I- ↔ I2 + 2e-

and obviously whether it should be treated as oxidation with iodine or reduction with iodides
depends on the other redox system involved.

Second important reaction used in the iodometry is reduction of iodine with thiosulfate:

2S2O32- + I2 → S4O62- + 2I-

In the case of both reactions it is better to avoid low pH. Thiosulfate is unstable in the
presence of acids, and iodides in low pH can be oxidized by air oxygen to iodine. Both
processes can be source of titration errors.

Iodine is very weakly soluble in the water, and can be easily lost from the solution due to its
volatility. However, in the presence of excess iodides iodine creates I3- ions. This lowers free
iodine concentration and such solutions are stable enough to be used in lab practice. Still, we
should remember that their shelf life is relatively short (they should be kept tightly closed in
dark brown bottles, and standardized every few weeks). Iodine solutions are prepared
dissolving elemental iodine directly in the iodides solution. Elemental iodine can be prepared
very pure through sublimation, but because of its high volatility it is difficult to weight. Thus
use of iodine as a standard substance, although possible, is not easy nor recommended. Iodine
solutions can be easily normalized against arsenic (III) oxide (As2O3) or sodium thiosulfate
solution.

It is also possible to prepare iodine solutions mixing potassium iodide with potassium iodate
in the presence of strong acid:

5I- + IO3- + 6H+ → 3I2 + 3H2O

Potassium iodate is a primary substance, so solution prepared this way can have exactly
known concentration. However, this approach is not cost effective and in lab practice it is
much better to use iodate as a primary substance to standardize thiosulfate, and then
standardize iodine solution against thiosulfate.
Procedure
Weigh accurately about 100 mg of the sample, previously dried at 105o for 3 h, and dissolve
in 50 ml of water contained in a 250 ml glass-stoppered conical flask. Add 3 g of potassium
iodide, followed by 3 ml of dilute hydrochloric acid (3 in 10), and stopper the flask. Allow
the mixture to stand for 5 min., add 100 ml of cold water, and titrate the liberated iodine with
0.1 N sodium thiosulfate, adding starch TS as the end-point is approached. Perform a blank
determination. Each ml of 0.1 N sodium thiosulfate is equivalent to 3.567 mg of KIO3.

Report:
 ASSAY OF BARIUM SULPHATE BY GRAVIMETRY:

Aim – To perform the assay of Barium Sulphate by Gravimetry.

Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:
Barium Sulphate: BaSO4 Mol. Wt. 233.4

Barium Sulphate contains not less than 97.5 per cent and not more than 100.5 per cent of
BaSO4.

Description. A fine, heavy, white powder, free from gritty particles; odourless.

Assay procedure: Weigh accurately about 0.6 g in a platinum crucible, add 5 g of sodium
carbonate and 5 g of potassium carbonate and mix. Heat to 1000° and maintain at this
temperature for 15 minutes. Allow to cool and suspend the residue in 150 ml of water.
Wash the crucible with 2 ml of acetic acid and add to the suspension. Cool in ice and filter
by decantation, transferring as little of the solid matter as possible to the filter. Wash the
residue with successive quantities of a 2 per cent w/v solution of sodium carbonate until the
washings are free from sulphate and discard the washings. Add 5 ml of dilute hydrochloric
acid to the filter and wash through into the vessel containing the bulk of the solid matter
with water. Add 5 ml of hydrochloric acid and dilute to 100 ml with water. Add 10 ml of a
40 per cent w/v solution of ammonium acetate, 25 ml of a 10 per cent w/v solution of
potassium dichromate and 10 g of urea. Cover, digest in an oven at 80° to 85° for 16 hours
and filter while still hot through a sintered-glass filter (porosity No. 4), washing the
precipitate initially with a 0.5 per cent w/v solution of potassium dichromate and finally
with 2 ml of water. Dry to constant weight at 105°.

1 g of the residue is equivalent to 0.9213 g of BaSO4.

Report:
 Assay of Antimony Potassium Tartrate
Aim – To perform the assay of Antimony potassium Tratrate
Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:
The assay of Antimony Potassium Tartrate employs a direct iodimetric titration using 0.1N
Iodine VS. An oxidation reduction reaction takes place between the analyte and the titrant
resulting in the reduction of iodine to iodide and oxidation of the trivalent Antimony to
pentavalent Antimony. The indicator used is starch TS in which the appearance of a
persistent blue color indicates the endpoint of the titration. The titration must be carried out in
a mildly alkaline (pH 8) medium rendered by the addition of sodium borate.

Procedure
Dissolve about 500mg of Antimony Potassium Tartrate, accurately weighed, in 50mL of
water, add 5g of potassium sodium tartrate, 2g of sodium borate, and 3mL of starch TS, and
immediately titrate with 0.1N iodine VS to the production of a persistent blue color. Each mL
of 0.1N iodine is equivalent to 16.70mg of C8H4K2O12Sb2·3H2O.
I. Official Requirement
Antimony Potassium Tartrate contains not less than 99.0 percent and not more
than 103.0 percent of C8H4K2O12Sb2·3H2O.
II. Clean-up Procedure
1. The titrated solution may be disposed into the sink.
III. Reasons for Important Steps
1. The sample must be dried to remove its water of hydration.
2. Potassium sodium tartrate is added to prevent the precipitation of basic salts of
antimony by hydrolysis. (). Precipitated salt of antimony would no longer be
able to participate in the titration, thus the results of the assay will be
compromised.
3. Sodium Borate is added as a buffer to maintain the solution’s alkalinity. The
mildly alkaline condition for this assay is important because of several
reasons:
a. The indicator used in this assay, starch, tends to hydrolyze or decompose
in acidic medium, thus, the end point may be affected.
b. The pH of the solution affects the reduction potential of the trivalent
antimony.
KOOCCHOHCHOCHOHCOO(SbO) + I2 + H2O 
KOOCCHOHCHOHCOO(SbO2) + 2H+ + 2I+
As seen on the equation above, when the H+ concentration is high, the
equilibrium is shifted to the left. Thus, employing an alkaline solution will
prevent the left shift of the reaction by neutralizing the hydrogen ions.
c. The iodide ions produced in the reaction tends to be oxidized by dissolved
oxygen in the acid solution.
4I- + O2 + H+  2I2 +H2O
Since in an alkaline medium, the hydrogen ions are neutralized, there will be no
hydrogen ions to participate in the reaction above.
 d. The solution must only be mildly alkaline (pH 8) and not too alkaline
because iodine will disproportionate to hypoiodate and iodide.
4. 0.1N Iodine VS is the titrant due to its moderately strong oxidizing property.
5. Starch is the indicator used in this assay because when all the trivalent
antimony have been oxidized to pentavalent antimony, iodine will
consequently not be reduced to iodide and starch will be able adsorb iodine,
forming a persistently blue colored solution. B13 +

Report:
 DETERMINATION OF THE AMOUNT OF SODIUM CARBONATE AND SODIUM
HYDROXIDE IN A MIXTURE
Aim – To estimate and determine the amount of sodium carbonate and sodium hydroxide in
a given mixture.
Glasswares & apparatus required – digital balance, pipette, burette, burette stand, conical
flask
Principle:
Carbonate ion reacts with hydrogen ions in steps:

(38.1)

The pKa1 and pKa2 values of H2CO3 are quite distinct and so when a carbonate
solution is titrated against hydrochloric acid, there occur two distinct regions of
sharp pH change. The first corresponding to the formation of HCO (pH 8 to
10) and the second due to complete neutralization at pH 4-6. The first is
roughly in the pH range in which colour of phenolphthalein changes from red to
colourless and the second is that at which methyl orange changes from yellow
to orange red. This end point, however, is not very sharp in the titration of the
strong base NaOH. The sharp change of pH occurs over a range of pH that
includes the regions of colour change of both the indicators, so both of them
give the end point correctly.

When we have both sodium carbonate and sodium hydroxide present together
in a solution, a titration using phenolphthalein gives the titre (volume at the
equivalence point) corresponding to sodium hydroxide plus half the carbonate
and the titre obtained with methyl orange corresponds to the total alkali. The
individual sodium carbonate and hydroxide concentrations may be calculated
from the data.

The HCl solution used may be standardized by titration with a standard solution
of sodium tetraborate decahydrate (borax) or anhydrous sodium carbonate. The
reaction involved in the case of borax is

(38.2)
Borax is preferable as a primary standard because of its higher equivalent weight.
Procedure :
Prepare 100 mL of a standard solution of Na 2 B4 O 7 .10H2 O (approximately
N/20) by weighing accurately about one gram of borax, dissolving it in distilled
water and making up to 100 mL. Titrate 10 mL portion of this solution against
the supplied hydrochloric acid till concordant titres are obtained, using 2 drops
of methyl orange as indicator. Calculate the strength of the HCl solution.

Pipette out 10 mL solution of a mixture of sodium carbonate and sodium

 hydroxide into a conical flask, add two drops of methyl orange indicator and
titrate against HCl, till the colour changes from pale yellow to orange.
Note the titre value (V1 ). Titrate 10 mL portions of the solution using
phenolphthalein as indicator (1-2 drops). The color changes here at the end
point is from red to colourless and is quite sharp. Let the titre be V2 of HCl.
Therefore, 2(V1 - V2 ) corresponds to carbonate, and V1 – 2(V1– V 2 ) = 2V2–
V1 corresponds to sodium hydroxide. Calculate the amount of NaOH and
Na2CO3 present in a litre of the given solution in g/L.

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