T.Y.B.Sc.

Chemistry

Sem. –V

Course No:- CH-368

Subject: Inorganic Chemistry Practical.

Experiment :- 1 to 6
Inorganic Qualitative Analysis: (Six binary Mixtures containing common anions)
(Excluding phosphates and borates)

Experiment :-7 to 8
2. Ore Analysis: (Any Two)
Heamatite ore - Estimation of Iron volumetrically
Pyrolusite ore- Estimation of Manganese volumetrically
Dolamite ore - Estimation of Calcium volumetrically

Experiment :-9 to 10
3. Alloy Analysis : (Any Two)
i) Estimation of Zinc from Brass Alloy by EDTA method.
ii) Estimation of Tin gravimetrically as SnO2 from solder alloy.
iii) Estimation of Copper iodometrically from nichrome alloy.

Minerals :-Naturally occurring inorganic solid definite chemical composition ordered internal structure
Rocks- A rock is made up of two or more minerals. You need minerals to make rocks, but you don't need
rocks to make minerals. All rocks are made of minerals.
Ore:- Naturally occurring source of mineral from which metals are extracted economically. Processed
mineral (Usually heterogeneous)
Alloy:- A homogeneous mixture of a metal with other types of elements( Generally metals have zero
oxidation state)

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 INORGANIC QUALITATIVE ANALYSIS
The given plot of analytic procedure will help to identify Acid and Basic radicals in stepwise manner and the
chance of error can be minimized.
Physical observations:
A) State
B) Colour
Chemical observations:
A) Dry test basic radicals(preliminary tests)
B) Dry test acidic radicals(preliminary tests)
C) Wet test acidic radicals (Confirmatory tests)
D) Wet test basic radicals (Confirmatory tests)
Preliminary examination of a salt often furnishes important information, which simplifies further course of
analysis. Although these tests are not conclusive but sometimes they give quite important clues for the
presence of certain anions or cations. These tests can be performed within 10-15 minutes. These involve
noting the general appearance and physical properties, such as colour, smell, solubility etc. of the salt. These
are named as dry tests.
Precautions:-
(a) Firstly read Test and observation completelythen and then only perform test
(b)Before using any reagent or a chemical, read the label on the bottle carefully. Never use unlabeled
Reagent.
(c) Do not mix chemicals and reagents unnecessarily
(d) Be careful in smelling chemicals or vapours. Always fan( by hand) the vapours gently towards your nose
(e) Always pour acid into water for dilution. Never add water to acid.
(f) Be careful while heating the test tube. The test tube should never point towards yourself or towardsyour
neighbours while heating or adding a reagent.
(g) Always use the reagents in minimum quantity. Use of reagents in excess, not only leads to wastage of
Chemicals but also causes damage to the environment.

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Preliminary Test
Test Observation Inference
1. Nature Crystalline ( water soluble) SO4 , NO3 ,Cl , Br , I- of soluble salts or CO32- of
2- - - -

alkali salts present/may be present.

Amorphous ( water insoluble) CO3-2, BO3 -3, PO4-3of heavy metal salts present/may
be present.
2. Colour Pink Co2+, Mn2+ salts present.
Green/Bluish green Cu2+, Fe2+, Cr3+, Ni2+ salts present
Blue Hydrated Cu2+ salt present
Black CuO, CuS, PbS, NiS, CoS, MnO2 salt present
Yellow PbO, SnS, PbI2, CdS, As2S3, CrO42- salts present.

Orange or Red Dichromate and Sb2S3 salts present

Coloured Coloured radical present
White/Colourless Coloured salts are absent,Salts of
Na+,K+,NH4+and alkaline earth metals, Al, Zn, Ca,
Sr, Ba, Mg, salts may be present .

Test Observation Inference

 Dry tests for Basic radicals:-
1.Heating in dry a) Decrepitating (crackling sound is Salts like NaCl, KCl, KNO3, KI,
test tube:-Take a produced due to the breaking of the crystals Pb(NO3)2 etc. present/may be present.
pinch of mixture in and particles flying off) (no decrepitating )
dry test tube and heata) b) Substance fuses( just melt) or ( shrinks)/ Salts of Na+, K+, NH4+ or some salts
it strongly. Observe b) (no particular observation) of Ca2+, Ba2+, Sr2+, Mg2+ or hydrated
the changes taking salts etc.
place (test tube hold c) Sublimation (Condenses on cooler part
almost horizontal on of test tube.)
the burner flame.) i) Greyish or Black I-, As3+, Sb3+ salts etc.
ii) White NH4+, As3+ Sb3+ salts etc
iii) Yellow S2- salts etc
/(no particular observation)
d) Change in colour of residue
blue to white Cu2+
green to yellow Ni2+
yellow (when hot) to white (when cold) Zn2+, Sb3+
colourless to brown or black on heating Cd+2
white residue, glows on heating Ca+2, Ba+2 ,Sr+2 , Mg+2 , Al+3,K+
Black (when hot) to Rusty red or brown Fe2O3
(when cold)
Orange or Red (when hot) to yellow (when Bi+3, Pb+2
cold)
Black (when hot) to Black (when cold) MnO2,CuO,CoO,NiO,FeS ,CoS
Violet (when hot) to Blue (when cold) Co+2
Yellow (when hot) to yellow (when cold) Pb+2

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 e) Gas evolved
Colourless gas turns lime water milky CO3-2 or SO4-2
Characteristic vinegar like smell CH3COO-
Greenish yellow gas with suffocating odour, Cl-
smell of chloride, bleaches moist litmus
paper
Red brown vapours turn starch paper yellow Br-
Violet vapours turn starch paper blue I-
Dark brown or reddish fumes, acidic in NO3-
reaction
Colourless gas with smell of burnt sulphur Sulphites salts
and turns K2Cr2O7 paper green
Colourless gas with smell of rotten eggs, Sulphide salts
blackens lead acetate paper
Colourless gas turns blue litmus red and
produces fumes over glass rod dipped in Cl-
ammonia solution
Smell of ammonia, turns red litmus blue NH4+

2. Charcoal cavity a) fusion and sinking in the cavity Na+, K+, NH4+
test:-Mix.0.05gm of b) Decrepitationi.e,crackling sound and NaCl, KCl, KNO3, KI, Pb(NO3)2
mixture with double flying about of particles.
quantity of Na2CO3 c) Deflagration with the sparks and residue NO3- salts
and fill in cavity of turns green
charcoal. Add 2-3 d) Fumes and incrustation (the fumes NH4+, S-2, I-1
drops of water. Heat evolved get deposited on the cooler sides
cavity with blow pipe round about the cavity)
in a reducing e) Metal beads formed
flame(yellow). i) Rusty red Fe2O3
ii) Yellow incrustation with brittle bead Bi+3, Pb+2
iii) Malleable bead that marks the paper Pb+2
black
iv) Yellow malleable bead that does not Sn+2
mark paper black
v) Red flakes Cu+2
vi) Grey metallic particles without Fe2+, Co2+, Ni2+
incrustation.
vii) White infusible mass Mg2+,Ba2+,Sr2+,Ca2+,Al3+,Zn2+
3. Co(NO3)2 test:- a) Blue mass Al3+,PO43- salts.
This test is performed b) green mass Zn2+ salts etc.
only when residue in c) pale pink or indistinct mass Mg2+,Ba2+,Sr2+,Ca2+salts etc.
charcoal test remains
white.Add one drop
of 5%Co(NO3)2
solution and heat
residue in an

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oxidizing flame
(blue).
4.Flame test:- a) crimson K+
Mixture 0.05 g of the b) Bluish green Ba2+
mixture with 2-3 drop c) Light green Ca2+
of conc. HCl on clean d) Purple Sr2+
watch glass and e) Blue Cu2+
prepare a paste of it. f) White Bi3+,pb2+,Sn2+,As3+,sb3+,Cd2+etc
Take it on a match
stick head
(Nick chrome) and
heat in an oxidizing
flame.
Observe the color of
the flame with naked
eye and then through
cobalt glass.
5.NaOH test a) Evolution of ammonia gas but NH4+ may be present
(Sodalime Test):- turmeric paper remain unchanged.
Mixture +NaOH b) Smell of garlic salt
solution and boil

Test Observation Inference

Dry tests for acidic radical(Can be identified by volatile products except SO 4-2):-

1. Action of dilute acid (HCl or Evaluation of gases

H2SO4):-
Little mixture in a test tube +
3-4 ml dil. H2SO4
2. Mixturewith double the
quantity of MnO2 and 4-5
drops of conc. H2SO4. Warm it
gently
a) Colourless ,odourless gas evolved with CO3-2, SO4-2 may be
brisk effervescence turning freshly present.
prepared lime water milky.
b) Colourless gas with effervescence and SO3- -
with suffocating odour, turning
acidified potassium dichoromate paper
green.
c) Colourless gas with little S- -
effervescence. Smell of rotten eggs,
turning moist lead acetate paper black
brown or shining.
d) brown fume with little effervescence. NO2-
a) Greenish yellow gas bleaches moisten Cl-
litmus paper
b) Reddish brown gas with characteristics Br-
odour turns starch paper yellow
c) Voiletvapour with characteristics odour I-
turns starch paper bluish back. Forms a

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 black crystalline deposit on cooler parts
of the test tube
3. Mixture +Cu filling + Con. Dark brown fumes of evolved NO3-
H2SO4+ warm
4. 4. Chromyl Chloride Test:- Yellow coloured solution. Add 2-3 drops of Cl-
the mixture initially with solution to it. Yellow precipitate
double the quantity of solid of PbCr
on a piece of paper.
Take this mixture in a test tube
add 3-4 drops of conc.
and heat it. Collect the gas
evolved in another test tube
containing a few drops of
dilute NaOH solution

Wet Tests andConfirmetory test for Anions or acidic radicals:-

(i) Wet test for anions are done first as it helps us to confirm anions. It also helps us in preparation of
original solution for cations, because some of the anions interfere in the separation of groups and
analysis.
(ii) For each test ,4-5 drops of extact should be used in a test tube.
(iii) and are detected and confirmed in dry test test.

A) If mixture is water soluble then use Water Extractfor detection of anions.

B) If mixture is water insoluble then use sodium carbonate extract (S.C.E)and neutral sodium carbonate
extract(N.E)for detection of anions.

A) Preparation of Water Extract (W.E.): Take about 0.05 g of the mixture in a 25 ml beaker containing 10ml
of distilled water. Boil it strongly and Filter. Fitrate is W.E. Perform the wet tests for anions like ,
and analysis the VIth group for , and from this W. E.
B) Preparation of sodium carbonate extract (S.C.E)and neutral sodium carbonate extract(N.E) :-
1. Add about 2gm of pure sodium carbonate to about 1gm of mixture.
2. Add about 25ml distilled water and boil for 10 min. in a Conical flask.
3. Filter of reject the residue. Add 20-25 ml distilled water to the filtrate(S.C.E) .keep 10-15ml extract for
detection of S - -,NO2- -,NO3- -.
4. Neutralize the remaining filtrate by adding dil.HNO3and make it little acidic , then add NH4OH till the
extract become basic to litmus

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 5. Boil the solution to completely evolve NH3and CO2,and cool. Use this neutral solution(N.E) for
detection of halide.

Test Observation Inference

1) 2-3 drops of W.E/N.E +
3-4 drops of 5% BaCl2 or
Ba(NO3)2 solution
2) 2.3 drops of W.E/ N.E+
dilute HNO3 till acidic +
3-4 drops of 5%
AgNO3solution
a) Yellow precipitate soluble in dilute HCl CrO4-2 or Cr2O7-2( If
mixture or W.E. is yellow
CrO4-2present and if it is
orange Cr2O7-2present).
b) White precipitate insoluble in dilute HCl SO42-
a) White or yellow ppt. insoluble in dil. HNO3 Cl- , Br-, I- present.
i) White precipitate soluble in excess NH4OH Cl-
ii) Yellowish White precipitate partially Br-
soluble in excess NH4OH
iii) Yellow precipitate insoluble in NH4OH I-

b) Yellow ppt. soluble in dil. HNO3 PO3-4 present

c) Brick Red soluble in dilute HNO3 CrO2-4 or Cr2O2-7 present
d) White precipitate soluble in dilute HNO3 SO2-4 present
completely
e) White precipitate soluble in dilute HNO3 with CO3- -
effervescences of CO2
f) Black or Blackish Brown precipitate S2- present

Test Observation Inference

3) 2-3 drops of S.C.E/W.E + Brown ring or coloration. NO-2 present
dilute H2SO4 till acidic. Add 1-2
drops of freshly prepared FeSO4
solution from the side of the test
tube.

4) 2-3 drops of S.C.E/W.E + Brown ring forms at the junction. NO3- present
Conc H2SO4 till acidic. Mix
thoroughly and cool the solution. .
Add 1-2 drops of freshly prepared
FeSO4 solution from the side of
the test tube.

Confirmatory Tests For Anions.

1. Acidify 2-3 drops of W.E. a) Violet colored layer I- Confirmed.
or N.S with Conc.H2SO4 forms.
or HNO3 + 1 ml of CHCl3
+ 1 ml of saturated b) Brown Layer forms. Br- confirmed.
chlorine water. Shake
well.
2. Add little solid K2Cr2O7 to Yellow ppt of lead chromate is CI- Confirmed.
the mixture + concentrated formed.
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 H2SO4 warm gently. Pass
the evolved vapours into
lead acetate solution.
3. Water solution +dil. White ppt insoluble in dilute SO42-
CH3COOH till acidic + HNO3.
lead acetate solution.
4. Little mixture in a test Colourless ,odourless gas evolved CO3- -
tube + 3-4 ml dil. H2SO4 with brisk effervescence turning
freshly prepared lime water
milky.
2-3 drops of S.C.E + dilute Brown ring forms at the junction. NO3-
H2SO4 till acidic. Mix thoroughly
and cool the solution. . Add 1-2
drops of freshly prepared FeSO4
solution from the side of the test
tube.+ 3-4 drops conc. H2SO4

WET TEST FOR BASIC RADICALS

Instructions:

Group Seperation :(Salt Solution + Group Reagent → Precipitate) → Filtered → Residue

Group Analysis : (Residue + Reagents → Precipitate of Specific Colour) i.e. Cation is Confirmed
A) Preparation of solution:-
In qualitative analysis when we analyses basic radicals by wet test we have to prepare the solution of the
mixture. When a mixture gives transparent solution with the solvent then it is called Original Solution.
Many solvents are used to prepare the solution. Taking 0.1 gm. of mixture put the solvent in the following
order:
(1) Distilled Water :- In the cold and hot form.
(2) Dilute HCl: - In the cold and hot form.
(3) Concentrated HCl :- In the cold and hot form.
(4) Aqua-regia:- conc. HCl and conc. HNO3 in the ratio 3:1 is tried
(5) Mixture partly soluble in water:-If mixture is partly soluble in water then filter it. The filtrate is used for
group I to VI. The residue is dissolved in acid and is used for analysis of group II to V

NOTE
1) Use very small quantity of solution.
2) Once the particular group detected then remove that group completely from the whole solution.

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 Filter it.Use the filtrate for further group detection and use precipitate for the identification of radical in
that group. Firstly do group analysis of detected group
3) For group II extremely dilute solution is required for precipitation and For group IV extremely
concentrate solution is required for precipitation
Group Separation
Test Observation Inference
1) O.S+ dil. HCl Ppt. obtained. Gr.I present
AgCl-White
Hg2Cl2- White
PbCl2- White
No ppt. Gr.I radicals absent

2) O.S/filtrate + dil. HCl +H2S pass Ppt. obtained. Gr.II present

CuS-Black
PbS-Black
Bi2S3-Brown
SnS-Brown
CdS-Yellow
Sb2S3-Orange
No ppt. Gr.II radicals absent

3) 3) O.S/filtrate + NH4Cl solid (excess)+NH4OH(till Ppt. obtained. Gr.IIIA present

alkaline) Al(OH)3-White Gelatinous
Cr(OH)3-Green
Fe(OH)3-Reddish
MnOH)3-Brown
No ppt. Gr.IIIA radicals absent

4)
4) O.S/filtrate O.S. + NH4Cl(s) (excess)+ NH4OH Ppt. obtained. Gr.III B present
(till alkaline )+ H2S pass ZnS-White
MnS-Green
NiS-Black
No ppt. CoS-Black
Gr.III B radicals absent

5) O.S/filtrate O.S. + NH4Cl(s) (excess)+ NH4OH Ppt. obtained. Gr.IV present

(till alkaline )+ (NH4)2CO3 BaCO3-White
CaCO3-White
SrCO3-White
No ppt. Gr.IV radicals absent

6) O.S/filtrate O.S. + NH4Cl(s) (excess)+ NH4OH Ppt. obtained. Gr.V present

(till alkaline )+ Na2H(PO4) MgNH4PO4- White
No ppt. Gr.V radicals absent
7) If all group absent then - Gr.VI:- NH4+,K+ present

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 Group Analysis

Analysis of group I:-

Transfer the ppt. in a beaker + 5 ml water and boil well, then filter when hot
Residue Filtrate
Residue + conc. NaOH warm and filter It may contain PbCl2 as soluble in water

Residue Filtrate i) Filtrate + KI solution→Yellow ppt.(in cold)

Residue + aqua-regia and
boil + SnCl2→Black ppt.
Hg+ present and
confirmed
Acidify the filtrate with
ii) Filtrate + K2CrO4→Yellow ppt.
dil. HNO3
If white ppt is formed
iii) Filtrate + dil. H2SO4→White ppt.
Ag+ present
Filtrate + KI
Pb+2 present and confirmed
solution→yellow ppt.
Ag+ confirmed

Analysis of Group II

Separation of IIA & IIB:-Black ppt+yellow(NH4)2S+NaOH boil & filter.

Residue Filtrate
Wash the ppt with 2% NH4NO3 solution Acidify with dilute HNO3 & heat gently. If
&discard the washings. yellow or orange ppt. then Group IIB present

Use this ppt for analysis of IIA. Sb2+,Sn2+

Cu2+ ,Pb2+,Bi3+,Cd2+

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Analysis of Group II A (Copper group)

Dissolve the precipitate in 1cm3of 2N HNO3 and boil it.Add 1cm3 of 2N H2SO4 to 2-3 drops of this solution. If
white precipitate forms, then add 2N H2SO4 to the whole solution drop wise,till the precipitation is complete,
separate the precipitate by filtration.

Residue Filtrate

Whiteppt of PbSO4 Treat It is made alkaline with 4N NH4OH solution, boiled and Filter it.
it with 0.1g of solid
CH3COONH4, 1ml of
Residue Filtrate
CH3COOH&1cm3 of
H2O.boil strongly and White ppt of Bi(OH)3. It It is boiled with 0.5-1ml of Na2S2O4(sodium
then filter. Acidify the is dissolved in 2N HCl. dithionate) solution and centrifuged.
filtrate with 2N HNO3. 2 2 drops of solution are
poured in 10 ml of Residue Fitrate

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drops of this solution+2- H2O→white ppt or Metallic Cu. Dissolve it in Acidify it with 2N
3drops of 5% turbidity of BiOCl. 1ml conc. HNO3 by boiling HCl. Add 4-5ml of
K2CrO4→yellow ppt of Bi3+ present and neutralize it with 2N H2O to dilute it.2 drops
PbCrO4. C.T. NH4OH.2 drops of soln are of soln,heat and pass
Pb2+ present (a) 2drops of soln +2N acidified with CH3COOH+3 H2S→ yellow ppt of
C.T. HNO3 till acidic+2 drops drops of 5% CdS.
i) Filtrate + KI of 10% Thiourea soln. K4 Fe(CN)6soln-reddish Cd2+ present
solution→Yellow ppt.(in shake well→yellow ppt. brown ppt Cu2Fe(CN)6 C.T.
cold) (b) 2drops of soln +3-4 Cu2+ present (a) 2 drops of
ii) Filtrate +
drops of C.T. soln+2drops of H2O+5
K2CrO4→Yellow ppt.
iii) Filtrate + dil. Na2SnO2→yellow ppt. (a) 2 drops of solution + 2N drops of 0.25%
H2SO4→White ppt. NH4OH till Ferrous dipyridyl
alkaline→bluecolour + one iodide reagent→ red
drop of it on 5% alpha ppt.
benzoin oxime regent (b) 2 drops of
paper→green color solution+ a drop of
(b) A drop of solution on freshly prepared 0.1%
tile + 2-3 drops of 1% Zn Dinitro p-
acetate + drops of 5% diphenylcarbazide
NH4HgSCN→violet color reagent→ violet or
pink colour

Analysis of Group IIB (Tin group )

Ppt. + Conc.HCl + double amount of water and boil for five minute and pass H 2S.Filter it

Residue Filtrate
Orange ppt. of Sb2S3. Disslove it in 2N HCl. Boil off Boil off H2S; add Zn + dilHCl→Sn ppt.
H2S.Two drops of this solution are poured in 10ml of Sn2+ present
water→ white ppt or turbidity of SbOCl Dissolve it in conc. HCl
Sb2+ present C.T.
C.T a) Soltuion + HgCl2→ white ppt. of Hg2Cl2 is
a) 2 drops + Zn dust ( 0.02gm) warm→black ppt. formed
b) Solution + KI+ pyridine→coloured solution b) Solution + dil. I2 Solution→ I2decolorised

Analysis of Group IIIA (Iron Group):

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Precipitate is washed with 2 ml of H2O, filter and washing is rejected. Washed ppt is boiled with 1 ml of 2N
NaOH solution. 1 ml of H2O and 3-4 drops of 20 volume H2O2 and filter.

Residue
Brown ppt of (FeOH)3, Dissolve it. In 2N HCl
and dilute with 1ml of H2O2.
Divide the soln into two parts
Frist Part(for Fe3+)
3 drops of soln +3 drops of 5% KSCN soln
blood red soln or ppt of Fe(SCN)3.
Fe3+ present
C.T:
(a) 2 drops of soln +2-3 drops of
5%K4Fe(CN)6soln→ blue colour or ppt.
(b) 2 drops of soln+ 2 drops of 2N HCl + 2
drops of 2% cupferron reagent→ reddish
brown ppt.
Second parts (for Mn2+)
2 drops of soln + 3 drops of 2N HNO3 + 0.002g
(pinch) of NaBiO3 (sodium bismuthate)→
pink or violet colour of HMnH4.
Mn2+ present.
C.T
(a) 2 drops of soln + 0.001 g of Na2S2O8 + 2-3
drops of 2N H2SO4 + adrop of 0.1N
AgNO3soln boil → reddish violet or purple
colour.
(b) 2-3 drops of soln + 0.002g PbO2 + 5-6 drop
of conc. HNO3→ boil strongly and allow it to
settle→ violet colour.
Filtrate
Divide into two parts
Frist part (for Al3+)
2 drops of soln + 2N HCl till acidic. Make it alkaline with 4N
NH4OH → white gelatinous ppt of Al(OH)3.→Al3+ present
C.T
(a) 2 drops of soln + 2-3 drops of conc. HCl+ 2-3 drops of
0.1% Aluminon reagent → shake well + 5 ml of alkaline
(NH4)2CO3soln (NH4OH : (NH4)2 CO3=14) red colour.
(b) 2 drops of soln + 2N HCl till slightly acidic + 5 drops of
2M CH3COONH4soln + 5 drops of 10% solochrome cyanine
reagent → centrifuge→ after sometime, upper layer
turns intents purple.
Second part(for Cr3+)
3 drops of soln + 5 drops of 2N CH3COOH + 4 drops of 10%
Pb (CH3COO)2soln→ yellow ppt of PbCrO4.→
Cr3+ present
C.T
(a) 2drops of soln + 4N H2SO4 till acidic, cool + adrop of 20
volume H2O2 + 0.5 ml of 1% Ether-butanol mixture. Shake
well → blue organic layer.

Analysis of gorouplll B (Zinc group ):-

Ppt. of III B with 15ml of dil.HCl and allow to stand for five minutes and filter.

Residue Fitrate
Ppt. + 2 ml aqua regia ( 3:1 conc. HCl: conc. Filtrate is boil to expel H2S gas. Filtrate +NaOH
HNO3)+ evaporate slowly nearly to dryness then (excess).Filter
cool extract with 2 ml water and divide in two Residue Filtrate

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parts White residue turning a) Acidify the filtrate with
brown due to atmosphere acetic acid and pass H2S
Part I :- for Ni+2 oxidation. gas.→ White ppt.
3-4 drops of solution + 2N NH4OH till alkaline+ 3 Disslove the ppt. in conc. b) Acidify the filtrate with
drops of 1% DMG ( excess)→Scarlet red/rosy red HNO3 + pinch of PbO2 or acetic acid + few drops
ppt. NaBiO3→pink or violet K4[Fe(CN)6] + few drops of
Ni+2is present and confirmed. colour diphenyl amine in
Mn+2is present and H3CCOOH→ Green ppt.
Part II :- for Co+2 confirmed. c) Acidify the filtrate with
a) 4-5 drops of solution + solid NH4Cl + NH3 till dil.HNO3+ few drops
Co(NO3)2 and heat to
alkaline + K3[Fe(CN)6] →reddish brown ppt
dryness→ Green mass
or solution
Zn+2is present and
b) 2 drops of solution on watch glass + one
confirmed.
crystal of Na2S2O3→blue colour around the
crystal
Co+2 is present and confirmed

Analysis of group IV(Barium group ):-

Dissolve the precipitate in hot 2 ml of 2N CH3COOH. Test 2-3 drops of the solution with 0.5 ml of freshly
prepared saturated K2CrO4 solution. If yellow precipitate forms, then add 2 ml of K2CrO4 solution to the whole
solution and filter.

Residue Filtrate

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 Yellow ppt of BaCrO4. Add 2N NH4OH till the solution becomes alkaline. Test 2-3 drops of the solution
Dissolve the ppt in 2N with 0.5 ml of freshly prepared saturated (NH4)2C2O4 solution. If white
HCl. 2 drops of soln + precipitate forms, then treat the whole solution with (NH4)2SO4, warm and filter.
3-4 drops of 2N H2SO4
– white ppt of BaSO4.
Residue Filtrate
Ba2+ present.
White ppt of SrSO4. Boil the ppt with 4N 2-3 drops of soln + 3-4 drops of
C.T.
HCl. filter it. Take 2-3 drops of filtrate + saturated (NH4)2C2O4soln – white
(a) Obtained solution +
(NH4)2C2O4→ white 4 drops of NH4OH + 0.5 ml of saturated ppt of CaC2O4.
ppt. (NH4)2C2O4 solution – white ppt of Ca2+ present
(b) 2 drops of soln + 3 SrC2O4. C.T.
drops of freshly Sr2+ present 2 drops of soln + 4 drops of 1%
prepared 10% sodium C.T. Glyoxalbis reagent + a drop of 2N
rhodizoate reagent –
(a) 2 drops of soln + 5 drops of 5% NaOH + a drop of 10% Na2CO3 –
bright red colour.
K2CrO4soln + 2N NH4 OH soln till alkaline soln + 4 drops of CHCl3. Shake
– yellow coloured precipitate. well and allow it to settle – red
(b) 2 drops of soln on a tile + 3 drops of organic layer.
freshly prepared 10% sodium rhodizoate
reagent – brownish red colour.

Analysis of Group V(Magnesiumgroup ):-

Dissolve the ppt. in dilHCl/Dil H2SO4
C.T for Mg+2
a) 2 drops of solution + 2 drops 0.1% Titan Yellow solution + 4 drops dilNaOH → red ppt
b) 2 drops of solution + Hypoiodite reagent ( NaOH + equal amount of KI + iodine solution till the
solution becomes just yellow)→reddish brown ppt

Analysis of Group VI:-

Use water solution or original water extract
Part I
2-3 drops of W.E. + 5-6 drops of NaOH solution, boil
it and cover the mouth of test tube with moist turmeric
paper→smell of NH3and Turmeric paper turns
brown/red→ NH4+ present
Solution + Nessler’s reagent. .:=(Two drops of HgCl2 + few seconds.→ Yellow precipitate of
KI till scarlet red ppt. is formed and dissolved then add
equal amount of NaOH)→ Brown ppt is
formed→NH4+ confirmed
Part II
If is present, take 3 drops of W.E. + 5-6
drops of NaOH solution boil it to remove .
Then acidify it with acetic acid and add 3-4
drops of 5% sodium cobaltinitrite
solution. Shake well and allow it to stand for a
→K+ present
Water solution + perchloric acid → white ppt. of
KClO4→K+ confirmed

Cation NaOH(aq) NH3(aq)

Little Excess Little Excess
Al+3 White ppt Ppt. dissolve to form White ppt Ppt. remain insoluble
colorless solution

T.V.Rajale Page 15
 Ca+2 White ppt Ppt. remain insoluble No ppt or Very No Change
slight ppt
Zn+2 White ppt Ppt. dissolve to form White ppt Ppt. dissolve to form
colorless solution colorless solution
Cr+3 Green ppt Ppt dissolves
Co+2 Blue ppt Blue ppt turning pink Green ppt Brown
Pb+2 White ppt Ppt. dissolve to form White ppt Ppt. remain insoluble
colorless solution
Cu+2 Blue ppt Ppt. remain insoluble Blue ppt Ppt. dissolve to form
( turns brown on standing) dark blue solution
Fe+2 Dirty Green ppt Ppt. remain insoluble Dirty Green ppt Ppt. remain insoluble
Fe+3 Reddish Brown ppt Ppt. remain insoluble Reddish Brown Ppt. remain insoluble
ppt
NH4+ No ppt. When No Change No ppt. No Change
warm NH3 smell

 Result :-

1) Acidic radical :- ________and _________

2) Basic radicals :- ________and _________

Probable mixture is:-

a) _____________+______________b)._____________ +____________

T.V.Rajale Page 16
Aim :-Estimation ofironfromhematite ore
Principle:Hematite ore contains mainly iron oxide Fe2O3with impurities such as Al2O3 and SiO2.
Fe content above 65-70%. It has little gangue (<6% SiO2 and 3-4% Al2O3)
Chemicals :- Conc. HCl ,Conc. HNO3,Perchloric acid 60% ,K3Fe(CN)6 , K2Cr2O7 (0.025N) ,SnCl2 sol.(4%) ,
HgCl2 sol.(saturated).
Procedure:
The dissolution of Ore:
About 0.3-0.4 g of ore is accurately weighed in 250 ml conical flask add to it 15 ml con. HCl. Place a
stem-cut funnel in the mouth of the flask. Heat the flask till the ore is completely dissolved. Cool and add to it
con.HNO3 about 5 ml and heat for 10 minutes. Cool thoroughly and add 5 ml 60% perchloric acid and heat till
white fumes starts evolving. Cool the flask. Filter the above solution through Whattman filter paper No. 41.
Pour and wash the residue with hot water till it is free from acid as tested with litmus paper. Collect the Filtrate
and washing. Dilute-it to 250 ml and reuse for estimation of iron

Estimation of Iron volumetrically

Pipette out 100 ml diluted solution in 500 ml beaker add 3 ml conc. HNO 3, 7.5 g of ammonium
Chloride, 5 to 6 drops of bromocresol purple indicator and heat to boiling and add slowly to the above solution
1:1 ammonia till iron is completely precipitated. (i.e. supernent liquid turns purple). Filter through ordinary
filter paper and wash with hot water three times. Dissolve the precipitate in hot 1:1 HCl (About 10 ml) and
wash the filter paper with hot water till free from acid. Dilute the filtrate to 100 ml in volumetric flask. Fill it in
burette 2.
Take out 10 ml of above solution, heat to boiling and add to it 4% SnCl2 solution dropwise till becomes
colourless, add a drop or two drops SnCl2 in excess to ensure the complete reduction. Cool thoroughly and add
solution of HgCl2 till slight turbidity is obtained. Finally titrate with standard K2Cr2O7(0.025 N) using
potassium ferricyanide solution as an external indicator. Calculate % of iron present in Ore.
Iron is estimated using K 2Cr2O7 solution by two methods:
A. External Indicator: K3Fe(CN)6 Potassium ferricynide.
1. Fill burette no.1 with diluted solution of iron and burette no.2 with 0.025N K2Cr2O7 solution.
2. Take by burette no.1, 10 ml. of diluted iron solution in a100 ml. conical flask.
3. Add to it 2 ml. conc. HCl and boil it. It becomes yellow in colour.
4. To this hot solution add drop by drop 4% SnCl2 in excess to ensure complete reduction of ferric iron to ferrous
iron.
5. Cool the solution in the flask thoroughly under tap water.
6. To this cooled solution add drop wise saturated solution of HgCl 2 till a slight turbidity is just obtained. (Caution:
Avoid excess of HgCl2 otherwise it will oxidize Fe2+ to Fe3+).
7. Titrate this solution with 0.025N K2Cr2O7 using K3[Fe(CN)6] as an external indicator. The end point of the
titration is noted when there is no change in colour of the indicator. Call this reading as X1 ml.
8. In a similar way take two more reading. Find the constant burette reading as X ml.

B. Internal indicator: Diphenyl amine.

Potassium dichromate acts as an oxidizing agent in acidic medium and oxidizes Fe (II) to Fe (III) ions.
Diphenylamine is colorless, so long as K2Cr2O7 is completely used up in the reaction. At the end point, a slight
excess of K2Cr2O7 oxidizes the indicator to intense violet colour.
Reactions:
Fe2O3 + 6HCl 2FeCl3 + 3H2O
2FeCl3 + SnCl2 2FeCl2+ SnCl4
SnCl2+ 2HgCl2 SnCl4 +Hg2Cl2
SnCl2+ HgCl2 SnCl4 +Hg (Gray ppt.)
6FeCl2+14HCl+K2Cr2O7 6FeCl3+2KCl+2CrCl3 +7H2O

T.V.Rajale Page 17
Observations:
Weight of Ore taken :W=_____gm
a) Burette 2- 0.025K2Cr2O7solution
b) Burette 1 solution – Diluted solution
c) Indicator – K3[Fe (CN) 6]
d) End point –

Sr. Burette 1 Solution Burette 2 reading Constant Burette reading

No. (in ml) (in ml) (in ml)
1. 10 X1=_____
2. 10 X2=_____ X ml
3. 10 X3=_____

Calculations:
1000 ml 1N K2Cr2O7 = 55.85 g of Iron.
XxN 1 x55.85
 X ml N1 Normal K2Cr2O7 =? 
1000 = A g of Iron
10 ml solution = A g of Iron
100 xA
100 ml solution =? 
10 = B g of Iron
250 xB
 250 ml solution =? 
100 = C g of Iron
W g ore samplecontains = C g of Iron
100 xC
 100 g of sample =? 
W
% of Iron in Ore simple = -------% Fe

Result Table:

Sr.No. Description Values

1. Weight of Hematite ore taken W=

2. Amount of Fe in sample

3. % of Fe

T.V.Rajale Page 18
Aim: Estimation of manganese frompyrolusite ore.
Theory :Pyrolusite ore contains a large amount of manganese in the form of manganese dioxide, MnO 2, and
little silica. It is a black mineral. Its MnO2 content is between 60 to 63 % and silica content is between l0 to l5%
.Thedissolution of the ore is done in the mixture of conc. HCl and conc.HNO3. The insoluble residue contains
silica (SiO2) and soluble part contains largelymanganese. Silica is estimated gravimetrically while manganese is
estimated volumetrically, using KMnO4. Potassium permanganate is a powerful oxidizingagent in acidic
medium and hence can be used to estimate Mn volumetrically. Themethod is called Volhard's method.
Chemicals: conc. HCl , conc. HNO3 , conc. H2SO4 , Zinc oxide paste (emulsion) ,KMnO4 solution
(approx. 0.1 N) oxalic acid
Apparatus : Stem-cut funnel, Silica crucible , 100 ml. Volumetric flask,burette,etc
Procedure :
Dissolution of the ore :
1. Weigh accurately about 0.3 to 0.4 g of the ore. call it as w g. Transfer it in aconical flask.
2. Add to it l0 ml. conc. HCl and 3 ml. conc. HNO3. cover it with a stem-cut funnel which actsas an air
condenser.
3. Heat the flask in a fuming cupboard on a low flame till black particles of the ore dissolve. Ifthe ore does
not dissolve, again add 2 ml. conc.HCI and 1 ml. conc. HNO 3 and heat it again.
4. Repeat the procedure till the ore dissolves.
5. Cool the flask and add 2 ml. conc. H2SO4 slowly from the sides of flask.
6. Heat the flask again till white copious fumes of SO3 start evolving.
7. Cool the solution and rinse the funnel and its stem with little distilled water in the same flask.Add to it
about 20 ml. distilled water.

Filter the above solution through whatman No. 41 filter paper collect the filtrate in a
50ml.beaker. Transfer all the silica in a filter paper. Wash it with hot water till theresidueis
free from chloride (test with AgNO3) and acid (test by blue litmus paper).Collect the filtrate
and washings in the same beaker. Dilute it to exactly 100 ml in avolumetric flask. Preserve it
for the volumetric estimation of Mn.
Estimation of Mnyolumetrically (Volhards method)
Principle:
This method is based on the oxidation of divalent manganese with potassium permanganate in a hot (not less than 80°C)
solution neutralised with zinc oxide and containing a little excess of the latter. The endpoint is indicated by the persistent
pink colour.
Solid zinc oxide have a tendency to adsorb manganese ion. Potassium permanganate was stable in boiling hot solution at
pH 7.08 which was obtained by saturation with zinc oxide. Fading in pink of potassium permanganate observed near the
end point of the titration
During the dissolution of pyrorusite ore, MnO2 gets converted to MnSO4 i,e, Mn (IV) gets
converted to Mn (II). Volhard,s method is based on the principle that when manganous
salt solution is warmed and titrated with standard KMnO4 solution turns to brown and dark precipitate of
hydrated manganesedioxide is obtained. During the reaction manganous ion is
oxidized and permanganate ion is reduced giving hydrous manganese dioxide.
2KMnO4 + 3MnSO4 + 2H2O K2SO4+ 5MnO2 +2H2SO4
2+ 4-
i.e. 3Mn + 2MnO + 2H2O 5MnO2 + 4H+

Hydrated manganese dioxide has acidic properties and absorbs manganous hydroxide
Preventing complete oxidation. This difficulty is avoided by introducing sufficient amount of
ZnO paste.
FunctionofZnOpaste(emulsion):
i) The precipitate hydrated of MnO2 settles very quickly.

T.V.Rajale Page 19
ii) It neutralisesH2SO4 which is added during the titration of manganese
iii) It avoids formation of potassium permanganate.
iv) It avoids formation of manganous acid, hence prevents precipitation of manganous manganite.
v) It forms Zn ferrite with Fe if present as an impurity in MnSO 4. Thus interference of Fe is
masked.
Reactions:
MnO2 + 4HC1 MnC12 + 2H2O + Cl2

MnO2 + 4HNO3 Mn(NO3)2 + 2H2O + 2NO2 +O2

MnCl2 + H2SO4 MnSO4 + 2HC1

Mn(NO3)2 + H2SO4 MnSO4 + 2HNO3

2KMnO4 + 3MnSO4 + 2H2O 5MnO2 + K2SO4 +2H2SO4

Atomic Wt.x 3
5 xchange in oxidation state
ZnO + H2SO4ZnSO4 + H2O

Procedure:
Part I -Preparation of standard 0.1N Oxalic acid solution (Eq. Wt.63)
1000 ml 1N oxalic acid solution contains 63 g of oxalic acid.
1000 ml 0.1N oxalic acid solution contain 6.3 g of oxalic acid.
250ml 0.1N oxalic acid solution contain 1.575 g of oxalic acid.
Weigh accurately 1.575 g of oxalic acid (H2C2O4.2H2O) on a watch glass. Transfer it in a beaker and rinse the
watch glass with little water in the same beaker. Dissolve it in about 50ml distilled water. Transfer it into 250 ml
volumetric flask. Dilute it up to the mark using distilled water. Use of this solution for standardization KMnO 4
solution.
Part II :Standardisation of KMnO4solution :

1. Fill burette no.1 by 0.1 N (approx.)KMnO4solution.Fill burette no.2 by 0.1 N oxalic acid Take by burette no.2, 10
ml of 0.1 N oxalic acid and add to it 15 ml 2N H2SO4solution
2. Heat the solution on a wire gauze to 70o C and titrate this hot solution with KMnO 4 solution added from burette
no.1.
3. The end point of the titration is noted when permanent faint pink colourappears.Call this
4. burette reading as X1 ml.
5. To the same solution, add 2 ml oxalic acid solution by burette no.2 and heat the flask to
6. 70oC.The solution becomes colorless.
7. To this hot solution, add KMnO4solution from burette no.1 till faint pink colour appears.
8. Call this burette reading as X2 ml.
9. To the same solution, add 2 ml oxalic acid solution by burette no. 2 and heat the flask to 70 oC.The solution
becomes colorless.
10. To this hot solution, add KMnO4 solution from burette no.1 till faint pink colour appears.
11. Call this burette reading as X3 ml.
12. From these three burette readings find out the exact normality of KMnO 4 solution.

T.V.Rajale Page 20
Part III : Estimation of Manganese :
Fill the burette no.1 by standardized KMnO 4solution.and burette no.2 with diluted solution
of MnSO4.
1. Take by burette no.2, 10 ml of the diluted solution of MnSO4. Add 1/2 test tube of ZnO paste.
2. Add one test tube water to it.
3. Heat the solution on water bath between 40 and 600C and add 2 to 3 drops of 2N HNO3 solution (which promotes
the settling of the ppt. of MnO2 at the bottom).
4. Titrate this hot solution with standardised KMnO4 solution from burette no.1 with constant
shaking.The end point is faint pink colour to supernatant liquid which persists even after vigorousshaking. Note
down this burette reading . The faint pink colour should remain as it is even after heating, if not add one or two
drops of KMnO4 solution.

5. Take two more readings. Find the constant burette reading as Y ml.

Imp. Note : During the titration it is necessary allow the ppt. to settle down and see the colour of
the supernatant liquid against white background after each reading.
Observation and Observation Table –

Standardisation of KMnO4 solution –

Burette 1 : 0.1 N (approx) KMnO4 solution
Burette 2 : 0.1 N H2C2O4 . 2H2O solution
Indicator : KMnO4 act as a self-indicator
End Point : Colourless to pink

Burette – 2 10 ml 12 ml 14 ml
Burette – 1 X1 = ml X2 = ml X3 = ml

Calculations:-

Find out exact normality of KMnO4

KMnO4 = Oxalic acid
0.1 x 10
N1x X1 = 0.1 x 10 ∴N1 =
X1

0.1 x 12
N2 x X2 = 0.1 x 12 ∴N2 =
X2

0.1 x 14
N3 x X3 = 0.1 x 14 ∴N3 =
X3

N1  N 2  N 3
Exact normality of KMnO4= mean N4 =
3

T.V.Rajale Page 21
Estimation of Mn from a given solution –
Observation and Observation Table –
Burette 1 : 0.1 N (approx) KMnO4 solution
Burette 2 : diluted Mn2+ solution
Indicator : KMnO4 act as a self-indicator
End Point : Colourless to pink

Burette – 2 10 ml 10 ml 10 ml C.B.R
Burette – 1 Y1 = ml Y2 = ml Y3 = ml Y=___ml

Estimation of Manganese: (Volumetrically)

1000 ml 1 N KMnO4 = 16.462 g of Mn.
YxN 4 x16.46
Y ml N4Normal KMnO4 = ? 
1000 = Z g of Mn.

10 ml dil. solution = Z g of Mn.

 100 ml dil. solution = ?
Zx100

10
= A g of Mn
W g of ore = A g of Mn
Ax100
100 g of ore = ? 
W

 % of Mn = ---- %

Result Table:

Sr.No. Description Values

1. Weight of Pyrolusite taken

2. Exact Normality of KMnO4

3. Amount of Mn in sample

4. % of MnO2

T.V.Rajale Page 22
 Aim: Estimation of calciumfromdolomite ore.

Principle :The mineral dolomite has a theoretical composition of 40-65% CaCO3 and 40-45% MgCO3.
Part I -Preparation of standard 0.1N Oxalic acid solution (Eq. Wt.63)
1000 cm3 1N oxalic acid solution contains 63 g of oxalic acid.
1000 cm3 0.1N oxalic acid solution contain 6.3 g of oxalic acid.
250cm3 0.1N oxalic acid solution contain 1.575 g of oxalic acid.
Weigh accurately 1.575 g of oxalic acid (H2C2O4.2H2O) on a watch glass. Transfer it in a beaker and
rinse the watch glass with little water in the same beaker. Dissolve it in about 50 cm3 distilled water.
Transfer it into 250 cm3 volumetric flask. Dilute it up to the mark using distilled water. Use of this
solution for standardization KMnO4 solution.
Part II :Standardisation of KMnO4solution :
i) Wash and clean burette I and burette II with water.
ii) Rinse and fill the burette I with approx. KMnO4 solution (remove the air bubble) and place it at LHS.
iii) Rinse and fill the burette II with 0.1N oxalic acid solution (remove the air bubble) and place it at RHS.
iv) Take by burette II, 10 cm3 of 0. 1 N oxalic acid and add to it 15 cm3 2N H2SO4solution in conical flask
v) Heat the solution on a wire gauze to 70oC( just bubbles starts) and titrate this hot solution with
KMnO4solution added from burette I. The end point of the titration is noted when permanent faint pink
color appears. Call this burette reading as X1cm3.
vi) To the same solution, add twocm3 oxalic acid solution by burette II and heat the flask to 70oC.The
solution becomes colorless.
vii) To this hot solution, add KMnO4solution from burette I till faint pink colour appears. Call this burette
reading as X2cm3.
viii) To the same solution, add twocm3 oxalic acid solution by burette II and heat the flask to70oC.The
solution becomes colorless.
ix) To this hot solution, add KMnO4 solution from burette I till faint pink colour appears. Call this burette
reading as X3cm3.
x) From these three burette readings find out the exact normality of KMnO4 solution.
Part III : Estimation of Calcium:
i) Weigh about 0.3-04g of ore accurately and record the weight of the ore.Transfer the powder in 250 cm 3
beaker.
ii) Dissolve the ore in 10 cm3conc.HCl and 20-30cm3 distilled water .Heat the solution to boil for
10minutes.Cool the solution and filter it.
iii) Collect the filtrate in beaker. Discard the residue. 2.5 per cent oxalic acid are added and the solution is
brought to the boiling point and kept gently boiling until the calcium oxalate is coarsely granular.
Three per cent ammonium oxalate is then added, a few drops at a time, to the boiling solution, waiting
after each addition until the resulting precipitate has become coarsely crystalline. The amount of
ammonium oxalate to be added depends on the amount of calcium in solution. Twice the amount
necessary to combine with all the calcium is sufficient. After the calcium oxalate has become coarsely
crystalline and has settled to the bottom of the flask, it should be frequently stirred up in the liquid to
prevent the latter from boiling over suddenly. After the precipitate has become crystalline and has
settled, the solution is allowed to cool to room temperature.
iv) Again dissolve the precipitate.10 cm3conc.HCl and 20-30cm3distilled water .Heat the solution to boil for
10minutes.Cool the solution.
v) Transfer it to 100cm3 volumetric flask. Wash the beaker and rod with distilled water and transfer the
washings to volumetric flask. Dilute the solution to 100cm3 with distilled water. Shake the solution.
vi) Wash and clean burette II with water.
vii) Rinse and fill the burette II with diluted solution of calcium (remove the air bubble) and place it at RHS.

T.V.Rajale Page 23
 viii) Fill the burette I with approx. KMnO4 solution.
ix) Take by burette II, 10 cm3 of diluted solution of calcium and add to it 15 cm3 2N H2SO4solution in
conical flask
x) Heat the solution on wire gauze to 70o C (just bubble starts) and titrate this hot solution with KMnO 4
solution added from burette I.
xi) The end point of the titration is noted when permanent faint pink color appears. Call this burette reading
as Y cm3.
xii) Repeat the step vii to ix for two more reading and record the constant burette reading as Y cm3
Observation
Weight of ore =________ g
Observation table
For standardization of KMnO 4
i) Solution in burette I (LHS)= KMnO4 solution
ii) Solution in burette II (RHS)= 0.1N oxalic acid solution
iii) Indicator = KMnO4 ( Self indicator)
iv) End point = Colorless to pink.
Burette II (RHS) 10cm3 12cm3 14cm3
0.1N oxalic acid

Burette I (LHS) X1 = X2 = X3 =
KMnO4

2KMnO4+CaC2O4+4H2SO4⟶ 2MnSO4+K2SO4+CaSO4+2CO2+4H2O

Calculations:-

Find out exact normality of KMnO4

KMnO4 = Oxalic acid
0.1 x 10
N1x X1 = 0.1 x 10 ∴N1 =
X1

0.1 x 12
N2 x X2 = 0.1 x 12 ∴N2 =
X2

0.1 x 14
N3 x X3 = 0.1 x 14 ∴N3 =
X3

N1  N 2  N 3
Exact normality of KMnO4= mean N4 =
3

T.V.Rajale Page 24
Observation table

For Estimation of Calcium:

i) Solution in burette I (LHS)= KMnO4 solution
ii) Solution in burette II (RHS)= diluted solution of calcium
iii) Indicator = KMnO4 ( Self indicator)
iv) End point = Colorless to pink.
Burette II (RHS) 10cm3 10cm3 10cm3 C.B.R
diluted solution of calcium

Burette I (LHS) ____ cm3 ____ cm3 ____ cm3 Y= ____ cm3
KMnO4

1000 cm3 1N KMnO4 = Equivalent weight of calcium

= 20.04g

20.04 x N 4 xY
∴ Y cm3 N4 N KMnO4 = = A g of calcium
1000

i.e. 10 cm3 diluted solution contains = A g of calcium

∴100 cm3 diluted solution contains = A x 10= B g of calcium

i.e. W g of ore contains = B g of calcium

B x 10 x100
∴ 100 g of ore contains = = % of Ca
W

Result :

1. Weight of Ore W =_____ g

2. Exact normality of KMnO4 N4 =______N
3. Weight of calcium in ore =______g
4. % Ca in given ore = ____%.

T.V.Rajale Page 25
Aim:-Estimation of tin by gravimetric from solder alloy
Requirements: Conc. HN03, Whatman filter paper No. 40 Silica crucible ,
Procedure: Dissolution of the alloy :
i) Weigh accurately about 0.3 to 0.5 g of the ore.Call it as W g. Transfer it in a conical flask.
ii) Add to it 15 ml. conc. HNO3 and 10 ml. of distilled water. Cover it with a stem-cut funnel which acts as an
air condenser.
iii) When the vigorous reaction stops, then evaporate solution on a sand bath, till metallic and white precipitate
forms. (Take care that the solution does not evaporate alloy dissolves completely).
iv) Add 50 ml of distilled water to the precipitate in the beaker. Boil for 20 minutes with constant stirring on
water bath. Allow it to cool.
v) Filter the solution through a Whatman filter paper No. 40 and collect the filtrate in a 250 ml volumetric flask.
vi) Wash the precipitate on the filter paper 3-4 times with1% HNO3 solution and then with distilled
water.(Preserve residue).
(A) Estimation of Tin:
(1) Dry the residue obtained from step Nos. v and vi in an electric oven at 110 oC.
(2) Ignite the dried residue along with the filter paper in a previously weighed silica crucible. Heat
it for about 30 minutes and then cool'
(3) Weigh the residue of tin as SnO2.

Amount of tin :
1) Weight of empty crucible =w1=
2) Weight of crucible+residue =w2=
3) weight of residue (SnO2) be = w2-w1= x g.
Now, 150.7 g of SnO2 = 118.7 gms of Tin.
118.7 X x
... x g of SnO2 = --------------- gms of Tin
150.7
= A gm of Tin.
W g of the alloy contains = A gm of Tin.
A x 100
... 100 g of the alloy contain =- ---------------
W
... Percentage of tin = ………….. %

Results:-
Sr.No. Description Values
1. Weight of Solder
2. Amount of Sn in sample
3. % of Sn

T.V.Rajale Page 26
Estimation of Znvolumetrically from brass alloy
Requirements: Brass sample, Conc. HN03, 0.01M EDTA solution, hexamine , indicator Xylenol orange,
EBT indicator, buffer solution

Dissolution of the alloy :

1) Weigh accurately about 0.3 to 0.5 g of the ore.Call it as W g. Transfer it in a conical flask.
2) Add to it 15 ml. conc. HNO3 and 10 ml. of distilled water. Cover it with a stem-cut funnelwhich acts as an
air condenser.
3) When the vigorous reaction stops, then evaporate solution on sand bath add 5mlconcHCl
4) Cool the flask and add 50 ml of distilled water to it.
5) Pass H2S gas for complete precipitation of copper and filter it and collect the filtrate (colorless).
6) Check filtrate by passing H2S gas to remove copper completely.
7) Dilute the filtrate up to the mark in 100ml volumetric flask and use as diluted Zn stock solution.

Part II :Standardisation of EDTA solution :

1) Fill burette no.1 by 0.01 M (approx.) EDTA solution.
2) Fill burette no.2 by 0.01 M ZnSO4
3) Take by burette no.2, 10 ml of 0.01 M ZnSO4 and add to it one test tube distilled water Add half test
4) tube buffer solution ( pH=10) and 2-3 drops of EBT indicator
5) Titrate this solution with EDTA solution added from burette no.1.
6) The end point of the titration is noted from wine red to blue colour appears. Call thisburette reading as X1
ml.
7) To the same solution, add 2 ml ZnSO4solution by burette no.2 and The solution becomeswine red.
8) Add EDTAsolution from burette no.1 till faint wine red to blue colourappears.Call this burette reading as X 2
ml.
9) To the same solution, add 2 ml ZnSO4 solution by burette no. 2 and.The solutionbecomes wine red.
10) Add EDTA solution from burette no.1 till wine red to blue colourappears.Call this burette reading as X 3 ml.
11) From these three burette readings find out the exact molarity of EDTA solution.

Estimation of Zn by EDTA method:

1. Fill the burette no.1 by standardized EDTA solution and burette no.2 with diluted solution of Zn
2. Take 10ml of stock solution from burette no.2 in conical flask. Add one test tube distilled water to it.
Add 5-6 drops of Xylenol orange indicator to it
3. Now add hexamine powder till color changes from yellow to wine red which indicates that pH is raised to
about 6.
4. Titrate it against 0.01M EDTA solution from the burette no.1 End point will be form wine red to Yellowof
color. Call this burette reading as Y1 ml.
5. Repeat steps 2 to 4 for two more reading Y2 ml and Y3 ml.

T.V.Rajale Page 27
 Weight of Brass alloy taken W= _____________gm ( after decimal three digit)
Observation table
For standardization of EDTA
i) Solution in burette I (LHS)= EDTA solution
ii) Solution in burette II (RHS)= 0.01N ZnSO4solution
iii) Indicator =EBT indicator
iv) End point = wine red to blue
Burette II (RHS) 10cm3 12cm3 14cm3

Burette I (LHS) X1 = X2 = X3 =

Calculations:-

Find out exact normality of EDTA

EDTA ≡ ZnSO4.7H2O

M1V1 = M2V2

M1x X= 0.01x 10

M 2 V2 0.01 x 10
M1 = =
X1 X1

0.01 x 12
M2 =
X2 ’

0.01 x 14
M3 =
X3

Exact morality of EDTA = M1+M2+M3 =M4

For Estimation of Zinc:

i) Solution in burette I (LHS)= EDTA solution
ii) Solution in burette II (RHS)= diluted solution of Zinc
iii) Indicator = Xylenol orange indicator
iv) End point = wine red to Yellow

Burette II (RHS) 10cm3 10cm3 10cm3 C.B.R

Burette I (LHS) ____ cm3 ____ cm3 ____ cm3 Y= ____ cm3

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 A) Amount of Zn :
10 ml of the stock solution required y ml of M4 EDTA solution.
1000 ml of 1M EDTA = 65.37 gms of Zn
65.37 x Y x M4
...y ml of M4 EDTA = 1000 x 1 gms of Zn

= A g of Zn
... 100 ml Zn diluted solution contains =Ax 10 =B gms of Zinc
__W___ g of the alloy contains = B gams of Zn

B x 100
... 100 g of the alloy contain = -------------------------
W weight of the alloy

= ………. %

Results:-

Sr.No. Description Values

1. Weight of Brass
2. Exact Molarity of EDTA
3. Amount of Zn in sample
4. % of Zn

T.V.Rajale Page 29