Saltanalysis & Volumetric

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New Indian Model School, Dubai

Systematic Procedure for Inorganic Qualitative Analysis:

Aim: To analyze the given salt for acidic and basic radicals.
PRELIMINARY EXAMINATION of salt No: _____:

S.NO EXPERIMENT OBSERVATION INFERENCE


.
1. Color of the substance Blue/bluish green 2+
Cu2+. 2+
Color of the salt is noted. Light Green Ni Fe
Dark green Cr3+
Brown Fe3+
Light pink/flesh Color Mn
2+

Rose red/Violet Co2+


Colorless Absence of transition metal
cations like Cu2+, Ni2+, Mn2+,
Co2+etc.
2 Odor of salt
A pinch of the salt is Vinegar like smell CH3COO-
taken and rubbed with Ammoniacal smell NH4+
a drop of water. No characteristic smell Absence of NH4+ or
CH3COO-
3. Solubility: Soluble in water NH4+ may be present.
Insoluble in dil.HCl Pb2+may be present
4. Flame Test
2+
Make a paste of the salt Bluish white colored flame Pb
with Con.HCl in a watch Light/Pale Green flame 2+
glass and introduce into Ba
the non-luminous flame
Crimson Red flame Sr
2+
using a glass rod
Brick Red flame or Ca
2+

Golden Yellow flame Na+


Lilac K+
Blue surrounded by green Cu2+
No distinct colour of the flame seen. Absence of Ba2+, Ca2+, Sr2+
5. Dry heating test: Colorless odorless gas CO32- may be present.
A small amount of salt is turns lime water milky.
heated in a dry test tube. Pungent smelling gas, white fumes Cl- may be present.
with NH4OH
Reddish brown vapors Presence of NO3-
Vinegar smell CH3COO- may be present.
Colorless gas with smell of ammonia NH4+ may be present.
gives white fumes with HCl
Brown when hot & yellow when cold Pb2+ may be present
with crackling sound
Yellow when hot and Zn2+may be present.
white when cold.
6. Ash Test
A little of the salt is *Blue tinted ash Presence of Al3+
dissolved in few drops of
conc. HNO3 and boiled *Green ash Presence of Zn2+
with cobalt nitrate
[CO(NO3)2.6H2O] *Pale pink ash Presence of Mg2+
solution. A filter paper
soaked in this solution
and burnt to ashes.

Systematic Analysis of Anion (ANIONIC RADICALS):

S.N EXPERIMENT OBSERVATION INFERENCE


O
1. Action of dil.HCl
a)To a little of the salt 1-2 *Brisk effervescence with the *Presence of CO 2_
3
ml. of dil.HCl is added. liberation of colorless, odorless gas
b)A little of the salt is turns lime water milky(CaCO3).
rubbed with dil.HCl in a *Presence of CH3COO-
watch glass *Vinegar smell. (acetate)
*No brisk effervescence *Absence of CO 2_
3

2. Action of Con. H2SO4


To a little of the White fuming pungent smelling Presence of Cl-
substance add Con. gas(HCl), that intensify when glass
H2SO4 and warm it. rod dipped in NH4OH is brought near
the mouth of test tube

Yellowish brown gas having pungent Br-


smell turns starch paper yellow

Copious evolution of reddish brown Presence of NO3-


fumes(NO2) with pungent smell,
which intensify on adding paper
balls/Cu turnings.
Violet vapor I-
Colorless vapors having smell of Presence of CH3COO-
vinegar turns moist blue litmus red.
No characteristic gas is evolved. Absence of Cl-, NO3-,
CH3COO-
3. Action of dil.HCl &
BaCl2:
A little of the salt is White ppt(BaSO4) insoluble in Presence of SO42-
acidified with dil.HCl and con.HCl & con. HNO3.
BaCl2 solution is added.
CONFIRMATORY TESTS FOR ANIONS
S.No EXPERIMENT OBSERVATION INFERENCE
1. Confirmation of Carbonate:
(CO32-)
(i) To the water extract, add few White ppt soluble in dil.HCl / CO32-
drops of BaCl2 solution. dil.HNO3 with effervescence. confirmed
(ii) To the water extract, add White ppt soluble in dil.HCl. CO32-
MgSO4 solution. confirmed

2. Confirmation of Chloride (Cl-):


(i) Silver Nitrate test: Curdy white ppt(AgCl) Presence of Cl-
To the water extract, add soluble[Ag(NH3)2+Cl-] in excess is confirmed
dil.HNO3 and AgNO3. NH4OH solution.
(ii) Chromyl chloride test: Evolution of red Presence of Cl-
Heat the salt with solid K2Cr2O7 fumes(CrO2Cl2) which gives is confirmed
and 2-3 drops con. H2SO4. Pass yellow solution(Na2CrO4).
the red fumes through NaOH
solution taken in another test tube.
To this yellow solution, add lead Yellow ppt(PbCrO4) is formed.
acetate.

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.

5. Confirmation of sulphate (SO42-):


To the water extract, add White ppt(PbSO4) Presence of
dil.CH3COOH and lead insoluble in Con. SO42- is
acetate solution HCl/HNO3 but soluble in Confirmed
[(CH3COO)2Pb] excess of hot ammonium
acetate solution
[CH3COONH4].
Systematic Analysis of Cations (BASIC RADICALS):

S.N EXPERIMENT OBSERVATION INFERENCE


O.
I Analysis of Zero Group-NH4+
(Ammonium )
NaOH Test: A little of the salt is Smell of ammonia(NH3) and gives NH4+ is
heated with few drops of NaOH dense white fumes(NH4Cl) when a Present.
solution.
glass rod dipped in Con.HCl is
shown on the mouth of the test tube.
(Or)
A moist red litmus paper is shown at
the mouth of the test tube.NH3 gas
released turns damp red litmus paper
blue.
No smell of NH3. Absence of zero
group (NH4+)
1. To a little of the salt solution, No ppt, a clear soln. NH4+ is
add Na2CO3 solution. Confirmed
2.To a little of the salt solution
NaOH is added and then Reddish brown ppt NH4+
Nessler's reagent, K2[HgI4]. [HgO.Hg(NH2)I]. Confirmed
II Analysis of Group I – Pb2+ (lead): Dissolve salt in
H2O/dil.HCl/Con.HCl to make o.s.
1.To the salt solution, add White ppt(PbCl2) dissolve on Presence of
2+
dil HCl. warming with water. Pb

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.

To a little of the salt solution, *Pale blue/Bluish white/Greenish


K4[Fe(CN)6] is added. white precipitate *Presence of
changes to deep blue Cu2+ is
solution. Confirmed

IV Analysis of Group III – Al3+


To the salt solution, add solid Gelatinous white ppt[Al(OH)3] Presence of Al3+
NH4Cl followed by excess
NH4OH solution and agitate.
No Gelatinous white ppt Absence of group
III cation(Al3+)
1.Lake Test: A blue lake is formed on the Al3+ is confirmed.
Dissolve the ppt in minimum surface of the solution.
quantity of dil.HCl and add two
drops of blue litmus solution
followed by NH4OH dropwise till
blue color develops.
2. Add excess NaOH drop by White ppt [Al(OH)3] Al3+ is confirmed.
drop to the salt solution. soluble(NaAlO2) in excess NaOH.
3. Ash Test: Blue tinted ashes. Al3+ is confirmed.
A little of the salt is
dissolved in few drops of conc.
HNO3 and boiled with
cobalt nitrate [CO(NO3)2.6H2O]
solution. A filter paper soaked in this
solution and burnt to ashes.
V Analysis of Group IV – Zn2+
2+
1. To the salt solution, add excess Dirty/dull white ppt(ZnS) Presence of Zn
solid NH4Cl and excess of NH4OH
and pass H2S gas.
No ppt.
Absence of
group IV
2+
cation(Zn )
Dissolve the above ppt in dil.HCl
to boil off H2S and divide into two
parts.
(i) To the first part, add NaOH White ppt[Zn(OH)2]
drop by drop and then excess. soluble[Na2ZnO2] in excess Zn2+ confirmed
(ii) To the second part, add NH4OH NaOH .
and Potassium ferrocyanide White /bluish white ppt,
K4[Fe(CN)6] Zn2[Fe(CN)6]
3. Ash Test:
A little of the salt is Green ashes Zn2+ confirmed
dissolved in few drops of
conc. HNO3 and boiled with
cobalt nitrate [CO(NO3)2.6H2O]
solution. A filter paper soaked in this
solution and burnt to ashes.
VI Analysis of Group V - Ca2+ /
Ba 2+/Sr 2+:
To the salt solution, add excess White ppt(BaCO3/CaCO3/SrCO3) Ba2+/Ca2+/Sr2+
solid NH4Cl, NH4OH and excess may be
(NH4)2CO3 solution. present.

No ppt. Absence of
group V
cation(Ba2+/Ca
2+
/Sr2+ )

Dissolve white ppt in hot [Ba(CH3COO)2]/


dil.acetic acid and divide into 3 [(CH3COO)2Ca]/[Sr(CH3COO)2]
parts.
(i)
To the first part add K2CrO4. Yellow ppt(BaCrO4) Ba2+is
Flame Test: confirmed
Perform flame test with the original
salt. Apple green flame

(ii) To the second part add White ppt(SrSO4) Sr2+ is


(NH4)2SO4 solution and warm it. confirmed
Flame Test: Crimson red flame
Perform flame test with the original
salt.

(iii) To the third part add White crystalline ppt(CaC2O4) Ca2+is


(NH4)2C2O4 (ammonium oxalate) confirmed
and NH4OH soln to make soln
alkaline. Then scratch the sides of
the test tube with glass rod.

Flame Test:
(i)
Perform flame test with the Brick red flame
original salt.
VII Analysis of Group VI – Mg2+

To the salt solution, add solid White crystalline ppt[Mg(NH4)PO4] Presence of


NH4Cl, excess of NH4OH and Mg2+
(NH4)3PO4[or (NH4)2HPO4or
Na2HPO4]. Heated and the inner
side of the test tube is scratched
with a glass rod.
1. To the above ppt, add Violet/ Purple solution. Mg2+is
CO(NO3)2.6H2O. confirmed.
2.To the original solution, add 3 drops Blue coloration. Mg2+ is
of Magneson reagent[(4-(4- confirmed.
Nitrophenylazo)-resorcinol)] and 3
drops of con.NaOH to make it
alkaline.
3. Perform ash test with the original Pink tinted ash. Mg2+ is
salt. confirmed.

Result:

The given salt no _________has acid radical_____, basic radical_______. The salt
is ________.
Volumetric Analysis / Quantitative analysis

Experiment No. 1

Estimation of KMnO4 solution using standard 0.05M (M/20) Ferrous


Ammonium Sulphate (Mohr’s salt) solution
Aim : 1. To prepare 0.05M Mohr’s salt solution.
2. To calculate the molarity and strength of given KMnO4 solution by titrating it
against Mohr’s salt solution
Theory:
Ferrous ammonium sulphate (Mohr’s salt) acts as a reducing agent. The oxidation
number of iron in Mohr’s salt is +2. Iron is oxidised during the reaction and its
oxidation number changes from +2 to +3.
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 Mohr’s salt. After complete
consumption of ferrous 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.

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:

Trial Volume of Mohr’s Burette reading (ml) Volume of


No. salt Solution (mL) Initial Final KMnO4 Used (mL)

1. 20 0 9.7 9.7
2. 20 0 9.8 9.8
3. 20 0 9.8 9.8

Concordant titre Value: 9.8 mL

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)

Strength of KMnO4 solution = Molarity X Molar mass of KMnO4


= ______ X 158.03
= _______ gL−1
Result: (i) Molarity of KMnO4 solution is _______M.
(ii) Strength of KMnO4 solution is _______gL−1

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↑
--------------------------------------------------------------------------------------- --

Overall reaction: - 2KMnO4+3H2SO4+5H2C2O4 → K2SO4+2MnSO4+8H2O+ 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:

Trial Volume of Burette reading (ml) Volume of


No. oxalic acid Initial Final KMnO4 Used (mL)
Solution (mL)

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____

Strength of KMnO4 solution = Molarity X Molar mass of KMnO4


= ______ X 158.03
= _______ gL−1
Result: (i) Molarity of KMnO4 solution is _______M.
(ii) Strength of KMnO4 solution is _______gL−1

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.

Functional Group Identification:


S. Experiment Observation Inference
No
Test for unsaturation.
1. Organic compound +2ml Brown color of Compound is
CCl4+Br2 water bromine water is not saturated
R3C-CR3+Br2 discharged
CR2=CR2+Br2→CR2Br-CR2Br Pink color of Br2 H2O Compound is
changed to colorless unsaturated
Test for alcohol.
1. Ester Test: Organic compound Fruity smell of ester. -OH group
+CH3COOH+Con.H2SO4(2 drops) present
+ heat with occasional stirring
in water bath.

2. Cerric ammonium nitrate Red coloration -OH group


Test: present
Organic compound +Cerric
ammonium
Nitrate & shake the contents

3. Organic compound +piece of Na H2 gas evolved with -OH group


metal (dried in effervescence present
folds of filter paper)

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 given organic comp. contains phenolic (-OH) grp.

Test for Carbonyl group.


1. Organic comp + 2 ml of 2, 4 DNP shake & Orange red ppt Carbonyl group
allow it to stand.
is present, may
RCHO+(NO2)2C6H3HNNH2
be
→(NO2)2C6H3HNN=CRH(ye
aldehyde/keton
ll.orange)+H2O
e.

2. Sodium bisulphite Test: White ppt Carbonyl


Organic compound + 2-3ml group is
sat’d Soln of Sodium present
bisulphite & shake
well& leave for 10 min.
Test for aldehyde.
1. Organic compound + 1ml Silver mirror is formed in -CHO group
Tollen’s reagent. Keep t.t in the inner side of the t.t. present
water bath

2. Fehling’s solution test : Red ppt of Cu2O -CHO group


Organic compound + Fehling’s present
solution (A + B) + boil in a water
bath.

3. Schiff's solution test : Pink color obtained. -CHO group


Organic compound + 2ml of present
Schiff’s reagent

Result : Given organic compound contains aldehydic grp. (- CHO)

Test for Ketone.


1. Sodium nitroprusside Test: Red coloration/wine red Ketonic
Organic compound + sodium color group(>C=O)
nitro prusside + 2 – 3 drops of present
NaOH and shake.
Result : Given organic compound contains Ketonic group (>C = 0)

Test for Carboxylic acid.


1. Organic compound +Blue litmus Soln turns red -COOH group
soln present
Red soln+NaHCO3 Gas with brisk -COOH group
RCOOH+NaHCO3→RCOO effervescence present
Na+H2O+CO2↑ evolved, which turns
lime water milky.

2. Ester Test: Pleasant fruity smell -COOH group


Organic compound + present
C2H5OH+Con.H2SO4
+ heat with occasional stirring
in water bath.

3. FeCl3 Test : Red color appears. -COOH group is


Organic compound + dil FeCl3 present.
solution .

Result : The functional group present in the given organic compound is carboxylic acid (-COOH)

Test for amino group.


1. Carbylamine Test: Offensive smelling gas Amino
Organic compound + 1 ml R-NH2+HCl→RNH4 Cl group
Con.HCl+few drops CHCl3+ 2 ml RNH2+CHCl3+3KOH→RN≡C
present
+
alc. KOH+ ∆ + - 3KCl+3H2O

2. LITMUS TEST: Red litmus turns blue Amino group


Organic compound +Red litmus present
soln
SOLUBILITY TEST: Organic Amino
Organic compound +1-2 ml compound group
dil.HCl. Shake well dissolves present
3. Nitrous acid Test: Soln turns clear & N2 gas Amine present
Organic compound + 2-3 ml is liberate with brisk
dil.HCl+ mix ice cold H2O.+ effervescence.
Cold soln of 0.1g NaNO2
in 2ml dil.HCl. Observe
carefully
4. AZO DYE TEST. Primary
Organic compound +dil.HCl, Red orange dye aromatic
cool in ice. Add ice cold NaNO2. amino group
Mix well+Beta naphthol+NaOH present
NaNO2+HCl→HNO2+NaCl.
Ar-NH2+HNO2+HCl
→ArN+≡N-Cl+2H2O
Beta naphthol+ArN+≡N- Orange color dye
Cl→Azo dye+NaCl+2H2O

TESTS OF CARBOHYDRATES, FATS AND PROTEINS IN PURE SAMPLES AND

DETECTION OF THEIR PRESENCE IN GIVEN FOOD STUFFS

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:

Aqueous solution of sample + A red ppt. is obtained. Reducing sugar is


Benedict’s reagent. Heat on present.
water bath.
FEHLING’S TEST: A red ppt. is obtained. Reducing sugar is
Sample solution + present.
+ 1 ml of Fehling A + 1 ml of Fehling B .
Heat on water bath.

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.

OIL /FAT TEST :


To test the presence of oil or fat in the given food sample.
Oil/ fat --> glycerol + fatty acid
CH2 (OH)CH(OH) CH2 (OH) + KHSO4, --> CH2═CHCHO (acrolein) + 2H2O
1. SOLUBILITY TEST
Take a small amount of sample in 3 Sample does not dissolve in H2O Fat is present.
test tubes. Add water, alcohol and but is soluble in alcohol on
chloroform in 1, 2, 3 test tube heating and soluble in
respectively. chloroform.

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 :

1. Sample solution +few drops of I2 Violet color. Starch present.


solution.

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