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Saltanalysis & Volumetric
Saltanalysis & Volumetric
Saltanalysis & Volumetric
Aim: To analyze the given salt for acidic and basic radicals.
PRELIMINARY EXAMINATION of salt No: _____:
3. Confirmation of nitrate(NO3-):
(i) Brown ring test:
To the water extract, add equal A brown ring[FeSO4.NO] Presence of
amount of freshly prepared (nitroso ferrous sulphate) is -
NO3 is
FeSO4 soln followed by conc. formed at the junction of two
liquids. confirmed
H2SO4 along the sides of test
tube without disturbing the
solution.
(ii) Diphenylamine Test: Deep blue coloration. Presence of NO3-
To the water extract, add few drops of is confirmed.
diphenylamine.
4. Confirmation of
acetate(CH3COO-):
Oxalic acid Test: Smell like that of vinegar Presence of
Make a paste of the salt with oxalic CH3COO-
acid. Rub the paste and smell.
Ethyl Acetate/Ester Test: Heat a
pinch of salt with few drops of Pleasant fruity smell of Presence of
Conc. H2SO4 and 1 ml of ester[CH3COOC2H5] CH3COO-
C2H5OH. Then pour the is confirmed.
contents of the test tube in
beaker full of water.
Ferric Chloride Test: Take about Deep red coloration Presence
2ml of the water extract in a test [Fe(COOCH3)3] produced. of
tube and add neutral FeCl3 CH3COO--
solution and boil it. is
Filter, if required, and divide the confirmed
solution or the filtrate in two
parts:
(i) To one part add dil.HCl
(ii) To the second part add Red coloration disappears.
water and boil. Reddish brown ppt.
No ppt. Absence of
group 1(Pb2+)
2+
Dissolve the above ppt in hot H2O Yellow ppt (PbI2) Pb is confirmed
and divide into three parts
(i). To the first part, add KI
solution.
(ii). To the second portion, add Yellow ppt (PbCrO4) Pb2+ is confirmed
K2CrO4 solution.
(iii) Cool the third portion under the White crystalline ppt(PbCl2/PbSO4) Pb2+ is confirmed
tap. separates out.
III Analysis of Group II – Cu2+/ Pb2+/
As3+/Cd2+
To the salt solution, add dil.HCl and Black ppt(CuS) Cu2+/Pb2+
pass H2S gas.
Yellow ppt Cd2+/As3+
No ppt. Absence of
group II
Group II precipitate is boiled with *White precipitate soluble in *Presence of
dil.HNO3 and NH4OH is added in excess NH4OH. Cd2+ is
drops and then in excess.(or) NaOH is confirmed.
added to original salt solution.
No ppt. Absence of
group V
cation(Ba2+/Ca
2+
/Sr2+ )
Flame Test:
(i)
Perform flame test with the Brick red flame
original salt.
VII Analysis of Group VI – Mg2+
Result:
The given salt no _________has acid radical_____, basic radical_______. The salt
is ________.
Volumetric Analysis / Quantitative analysis
Experiment No. 1
Chemical Equation:
Reduction half reaction: 2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
Oxidation half reaction: [2FeSO4 (NH4)2SO4.6H2O + H2SO4 + 5[O] →
Fe2(SO4)3 + 2(NH4)2SO4 + 13H2O] x 5
---------------------------------------------------------------------------------------
Overall reaction: 2KMnO4 + 10FeSO4(NH4)2SO4.6H2O+8H2O →
K2SO4+ 2MnSO4+ 5Fe2(SO4)3+ 10(NH4)2SO4+ 68H2O
--------------------------------------------------------------------------------------------
Ionic equation:
Oxidation half reaction: [Fe2+ → Fe3+ + e–] x 5
Reduction half reaction: MnO4– + 8H+ + 5e– → Mn2+ + 4H2O
---------------------------------------------------------------
Overall ionic equation: MnO4– + 8H+ + 5Fe2+ → Mn2+ + 5Fe3+ + 4H2O
----------------------------------------------------------------
Procedure:
1. Mohr’s salt[FeSO4(NH4)2SO4.6H2O] being a primary standard; its solution can be
prepared by direct weighing. Take a square piece of paper, weigh it accurately and tare
its weight. Now put crystalline Mohr’s salt in the paper and weigh till the weight of
Mohr’s salt is 4.9g.
2. Add 10 ml of dil.H2SO4 to 250ml volumetric flask through a glass funnel kept over
it. H2SO4 is added to prevent the hydrolysis of Mohr’s salt.
Transfer the weighed Mohr’s salt from the paper to a glass funnel placed above 250ml
volumetric flask. Give fine spray of water from wash bottle to the funnel so that
everything comes down to the volumetric flask.
3.Dissolve the Mohr’s salt by shaking the volumetric flask when the salt dissolves
completely add distilled water up to just a little below the mark on the flask. Now add
the last drops of water carefully until the lower meniscus just touches the graduated
mark. Close the measuring flask and shake to get a uniformly concentrated solution.
4. Rinsed and filled the clean burette with potassium permanganate solution upto 0.0
mark without any air bubble.
5. Taken 20 mL of 0.05 M Mohr’s salt solution in a clean conical flask using
measuring cylinder and added full test tube dil. H2SO4 to it.
6. Titrated the Mohr’s salt solution against potassium permanganate solution with
constant swirling of conical flask until a permanent pale pink colour is obtained.
7. Repeated the titration for concordant titre value and tabulated the readings.
8. Molarity and strength of given KMnO4 soluttion is calculated.
Scheme of Titration:
Conical flask: 20mL Mohr’s salt solution + 1 test tube dil.H2SO4 solution.
Burette: KMnO4 solution.
Indicator: KMnO4 self-indicator.
End point: Colorless to permanent pale pink.
Tabular Column:
1. 20 0 9.7 9.7
2. 20 0 9.8 9.8
3. 20 0 9.8 9.8
Calculation:
To prepare Mohr’s salt solution:
Mass of Mohr’s salt = Molarity X Molar mass of Mohr′s salt X Volume of Solution (mL)
1000
= 1 𝑿 𝟑𝟗𝟐 𝑿 𝟐𝟓𝟎
20X𝟏𝟎𝟎𝟎
= 4.9g
Molarity and strength of KMnO4 solution (𝐚𝟏𝐌𝟏𝐕𝟏)𝐌𝐨𝐡𝐫′𝐬 𝐬𝐚𝐥𝐭= (𝐚𝟐𝐌𝟐𝐕𝟐)𝐊𝐌𝐧𝐎𝟒
𝒂𝟏= The number of electrons lost per formula unit of Mohr’s salt = 1
𝑴𝟏= Molarity of Mohr’s salt solution = 1/20M OR 0.05M
𝑽𝟏= Volume of Mohr’s salt solution = 20 mL
𝒂𝟐= The number of electrons gained per formula unit of KMnO4 = 5
𝑴𝟐= Molarity of KMnO4 solution = ?
𝑽𝟐= Volume of KMnO4 solution = ________ mL (titre value)
PRECAUTIONS:
1. Weighing should be accurate.
2. Add 10 ml of conc H2SO4 to prevent hydrolysis of Mohr’s Salt solution.
3. While titrating, the funnel should not be placed at the top of the burette.
4. For preparing standard solution, apparatus should be clean.
5. Standard solution should be prepared in distilled water.
6. Last drops in the measuring flask must be added accurately.
Experiment No. 2
Estimation of KMnO4 solution using standard 0.02M (M/50) Oxalic acid
solution
Aim : 1. To prepare 0.02M Oxalic acid solution.
2. To calculate the molarity and strength of given KMnO4 solution by titrating it
against oxalic acid solution
Theory:
Oxalic acid acts as a reducing agent. The oxidation number of Carbon in oxalic acid is
+3. Carbon is oxidised during the reaction and its oxidation number changes from +3
to +4.
Potassium permanganate acts as oxidising agent. MnO4− is reduced to Mn2+. Potassium
permanganate acts as a self indicator. Initially colour of potassium permanganate is
discharged due to its reduction by oxalic acid. After complete consumption of oxalate
ions, the end point is indicated by the appearance of a pale pink colour produced by
the addition of a little excess of unreacted potassium permanganate. during the
titration of oxalic acid against potassium permanganate, warming of oxalic acid
solution (50°–60°C) along with dilute H2SO4 is required.
Chemical Equation:
Reduction Half reaction: - 2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
Oxidation Half reaction: - 5H2C2O4 + 5[O] → 5H2O + 10CO2↑
--------------------------------------------------------------------------------------- --
---------------------------------------------------------------------------------------------
Ionic equation:
Reduction Half reaction: - [MnO4– + 8H+ + 5e– → Mn2+ + 4H2O] x 2
Oxidation Half reaction: - [C2O42- → 2CO2 + 2e–] x 5
------------------------------------------------------------------
Overall reaction: - 2MnO4– + 16H+ + 5C2O42- → 2Mn2+ + 10CO2 + 8H2O
-------------------------------------------------------------------------
Procedure:
1. Being a primary standard oxalic acid(C2H2O4.2H2O) can be prepared by direct
weighing. Take a square piece of paper, weigh it accurately and tare its weight. Now
put oxalic acid crystals in the paper and weigh till the weight is 0.63g.
2. Transfer the weighed oxalic acid crystals from the paper to a glass funnel placed
above 250ml volumetric flask. Give fine spray of water from wash bottle to the funnel
so that everything comes down to the volumetric flask.
3.Dissolve oxalic acid by shaking the volumetric flask when the salt dissolves
completely add distilled water up to just a little below the mark on the flask. Now add
the last drops of water carefully until the lower meniscus just touches the graduated
mark. Close the volumetric flask and shake to get a uniformly concentrated solution.
4. Rinsed and filled the clean burette with potassium permanganate solution upto 0.0
mark without any air bubble.
5. Taken 20 mL of 0.02 M oxalic acid solution in a clean conical flask using measuring
cylinder and added full test tube dil. H2SO4 to it. Heated the oxalic acid solution upto
50°– 60°C before titrating.
6. Titrated the oxalic solution against potassium permanganate solution with constant
swirling of conical flask until a permanent pale pink color is obtained
7. Repeated the titration for concordant titre value and tabulated the readings.
8. Molarity and strength of given KMnO4 solution is calculated.
Scheme of Titration:
Conical flask: 20mL oxalic solution + 1 test tube dil.H2SO4 solution and heated
Burette: KMnO4 solution.
Indicator: KMnO4 self-indicator.
End point: Colorless to permanent pale pink.
Tabular Column:
1. 20 0 7.7 7.7
2. 20 0 7.9 7.9
3. 20 0 7.9 7.9
Concordant titre Value: _7.9 Ml
Calculation:
To prepare oxalic acid solution:
Mass of oxalic acid = Molarity X Molar mass of oxalic acid X Volume of Solution (mL)
1000
= 𝟎.02 𝑿𝟏𝟐𝟔 𝑿 𝟐𝟓𝟎
𝟏𝟎𝟎𝟎
= 0.63g
Molarity and strength of KMnO4 solution (𝐚𝟏𝐌𝟏𝐕𝟏)𝐨𝐱𝐚𝐥𝐢𝐜 𝐚𝐜𝐢𝐝= (𝐚𝟐𝐌𝟐𝐕𝟐)𝐊𝐌𝐧𝐎𝟒
𝒂𝟏= The number of electrons lost per formula unit of oxalic acid = 2
𝑴𝟏= Molarity of oxalic acid solution = 0.02M
𝑽𝟏= Volume of oxalic acid solution = 20 mL
𝒂𝟐= The number of electrons gained per formula unit of KMnO4 = 5
𝑴𝟐= Molarity of KMnO4 solution = ?
𝑽𝟐= Volume of KMnO4 solution = ______mL (titre value)
2x0.02x20 =________M
5x____
PRECAUTIONS:
1. Oxalic acid should not be heated above 700C.
2. For preparing standard solution, apparatus should be clean.
3. Standard solution should be prepared in distilled water.
4. Weighing should be done correctly.
5. Since the lower meniscus of KMnO4 is not visible, read the upper meniscus.
6. Rinse burette and pipette before use.
7. Do not use rubber pinch cork, burette as rubber is an organic matter and gets attached to
KMnO4.
[C] Tests for the functional groups present in organic compounds.
Aim: To identify the functional group present in the given organic compound.
Unsaturation, alcoholic, phenolic, aldehydic, ketonic, carboxylic and amino
(Primary) groups.
Result : The functional group present in organic compound is alcohol group (-OH).
Test for phenol.
1. Organic compound + 2-3ml blue Red coloration Phenolic – (OH)
litmus present
solution.
2. Organic compound +2-3 ml Purple/violet color soln. Phenolic – (OH)
freshly prepared present
neutral FeCl3& shake
Result : The functional group present in the given organic compound is carboxylic acid (-COOH)
CARBOHYDRATE TEST
AIM: To test the presence of carbohydrate in the given food sample.
1. CHO(CHOH)4CH2OH + 2Cu2+ + 5OH- → COOH(CHOH)4CH2OH + Cu2O +3H2O
2.CHO(CHOH)4CH2OH + 2[Ag(NH3)2]+ + 3OH- → COOH(CHOH)4CH2OH
+ 4NH3+ 2Ag ↓ + 2H2O
S.N EXPERIMENT OBSERVATION INFERENCE
O.
1. CONC H2SO4 Test
Food sample + conc. H2SO4. Charring occurs Carbohydrate
∆ with smell of burnt present.
sugar
2. MOLISCH’S TEST
Food sample + A purple ring is Carbohydrate
Molisch’sreagent (1% obtained at the junction present.
alcoholic solution of α of two layers.
naphthol) + conc.
H2SO4along the sides of the
test tube.
3. BENEDICT’S TEST:
4. TOLLEN’S TEST
Aqueous solution of sample + Silver mirror is formed Reducing sugar is
2ml of Tollen’s reagent. Heat along the surface of the present.
on water bath. test tube.
Result : Carbohydrates is present.
PROTEIN TEST:
To test the presence of protein in the given food sample.
BIURET TEST
1. Sample + few drops of NaOH + A bluish violet Protein is
few drops of coloration. present.
1% CuSO4 solution.
2. XANTHOPROTEIC TEST
Sample + few drops of A yellow ppt. Protein is
conc. HNO3. Heat. present.
3. NINHYDRIN TEST
Food sample + few drops of Blue color appears. Protein is
0.15 ninhydrin solution. Boil present.
the contents for 1 min.
Result : Protein is present.
2. SPOT TEST
Put a small amount of sample on A translucent spot Fat is present.
a filter paper and press with appears on the filter
another filter paper. paper.
3. ACROLEIN TEST
Take a few drops of sample in a An irritating odour Fat is present.
test tube. Add few drops of appears due to the
potassium bisulphite(KHSO4) to formation of acrolein
it and heat. vapors.
4. Food sample+ether. Shake Emulsion is obtained Oil / fat present.
both and add to water in a t.t.
Result : Fat is present.
STARCH TEST :