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VIKAS PRE-UNIVERSITY COLLEGE

CHEMISTRY
PRACTICAL 1
LAB MANUAL

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Index
Experiment No -1
Parts of Bunsen Burner 03

Experiment No -2
Study of glass works 04

Experiment No -3
Preparation of standard oxalic acid solution. 05

Experiment No -4
Estimation of HCl using sodium carbonate 06

Experiment No - 5
Estimation of sodium hydroxide using oxalic acid 08

Experiment No - 6
Estimation of sodium hydroxide using HCl 10

Experiment No - 7
Systematic Semi-micro qualitative analysis of a simple inorganic salt No-1 17

Experiment No - 8
Systematic Semi-micro qualitative analysis of a simple inorganic salt No-2 19

Experiment No - 9
Systematic Semi-micro qualitative analysis of a simple inorganic salt No-3 22

Experiment No - 10
Systematic Semi-micro qualitative analysis of a simple inorganic salt No-4 24

Experiment No -11
Systematic semi-micro qualitative analysis of a simple inorganic salt-5 26

Experiment No -12
Systematic semi-micro qualitative analysis of a simple inorganic salt-6 29

Experiment No -13
Systematic semi-micro qualitative analysis of a simple inorganic salt-7 31

Experiment No -14
Systematic Semi-micro qualitative analysis of a simple inorganic salt No-8 33

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Experiment No -1
Parts of Bunsen Burner

Aim: To study the different parts of Bunsen Burner and nature of Bunsen flame.

Parts of Bunsen burner:

1)The Base

The base consists of a heavy metal with a horizontal side inlet.The side inlet tube is connected
through a rubber tubing to the source of combustible gas. The base has a brass nozzle
through which gas enters the burner tube.

2)The burner tube

It is long tube with two holes diametrically opposite to each other near the lower end.It is
screwed to the base with the nozzle at the centre and carries the air regulator.

3)The air regulator

It is a short metallic cylindrical sleeve that loosely fits on the lower end of the burner tube.It has
two holes diametrically opposite to each other.It can be rotated to regulate the supply of air into
the burner tube by partially or wholly opening or closing the air holes.

b) Working of the Bunsen Burner

The gas tap is opened and the burner is lighted.As the gas escapes through the nozzle ,there
is a fall of pressure and consequently air is sucked in through the air holes.The mixture of air
and the combustible gas burns at the top with a flame.Depending upon the supply of air,the
flame may be luminous or non-luminous.If the air hole is completely open, the maximum air is
sucked in and the gas burns with a pale blue non-luminous flame. If the air holes are
completely closed,the gas burns with a yellow, luminous flame.The non-luminous zone is the
hottest part of the flame.

Fig 1: Bunsen Burner

Fig2: Zones of flame of Bunsen burner. Fig2: Zones of flame of Bunsen burner.

A pale blue outer zone of complete combustion 3 A pale blue outer zone of complete combustion

A luminous region of incomplete combustion

A dark inner region of unburnt gases 2 A dark inner region of unburnt gases
A small blue region at the base of the flame 1 A small blue region at the base of the flame

Luminous flame Non Luminous flame


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Experiment No -2
Study of glass works

Cutting of a glass tube:

Select a glass tube.Hold it firmly and make a single deep scratch by means of a triangular file
without applying much pressure .Place the thumb on each side of the scratch at equal
distances from it.Gently press by givi ng a bending motion until it cuts.

Bending of a glass tube:

Place the tube in the hottest zone of the Bunsen flame and heat that portion where it is to be
bent keeping the tube rotating until it becomes soft and starts bending under its own
weight.Remove the tube from the flame and bend it slowly to a desired angle by pressing it
against a glazed tile to ensure coplanarity of the bend.Allow the bent tube to cool on the glazed
tile.

Drawing into capillary:

Heat the given tube in the hottest zone of the Bu nsen flame holding it at both ends rotating the
tube gently until it becomes soft.Remove the tube from the flame and pull the ends apart slowly
until it becomes narrow in the middle.Cut the tube in the middle and make the jet uniform by
rubbing it with sand paper and by fire polishing.

Figures

Making a scratch

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Experiment No -3
Preparation of standard oxalic acid solution.

Aim: To prepare 100ml of 0.1M standard oxalic acid solution.

Principle:A solution whose concentration is exactly known is called Standard solution. A


standard solution of oxalic acid is used to determine the unknown concentration of an alkali
solution.The formula of hydr ated oxalic acid is (COOH) 2.2H2O and its molar mass is 126g. If
126g of oxalic acid is present in one litre of the solution,it is called as one molar solution.

To prepare one litre of 0.1M oxalic acid solu tion,we require 126/10=12.6g of hydrated oxalic
acid. Therefore for preparing 100ml of 0.1M ox alic acid solution we require 12.6×100/1000=
1.26g of hydrated oxalic acid. In general Molarity can be calculated using the formula

M=mass of the solute in grams × 1000/molar mass of the solute × volume of the solute to be
prepared in ml

Procedure:

Weigh an empty clean dry watch glass.Accurately weigh 1.26g of oxalic acid by placing
it on the watch glass.
Transfer oxalic acid carefully from the watch glass into a clean and dry 100ml of
standard flask using a funnel. Add a little amount of distilled water and swirl the flask
until the oxalic acid is completely dissolved. Add more distilled water with shaking and
make the solution upto the mark carefully by adding the last few ml dropwise. Stopper
the flask and shake it thoroughly to make the solution uniform throughout.
Calculate the molarity of the solution using the above mentioned formula.

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Experiment No -4
Estimation of HCl using sodium carbonate

Aim: Determination of concentration (s trength)of a given solution of dilute Hydrochloric acid by


titrating against standard solution of sodium carbonate.

Principle: Sodium carbonate reacts with hydrochloric acid as follows:

Na2CO3+2HCl →2NaCl +H 2O+CO 2

1 mole of Na 2CO3≡2 mole of HCl

Acidity of the base Na 2CO3 =2

Basicity of the acid=1

Aqueous solution of Sodium carbonate is a weak alkali while Hydrochloric acid is a strong
acid.Therefore methyl orange is used as the in dicator during the titration.Methyl orange gives
yellow colour in alkaline solution while it turns red in acidic solutions. In neutral solutions it gives
an orange red colour.

Procedure:

Titration of standard Sodium carbonate solution against Hydrochloric Acid

Wash a burette with tap water,rinse it with distilled water and then rinse it with the given
hydrochloric acid care should be taken to see that no air bubbles are trapped in the
burette and its nozzle. Note the initial reading of the solution in the burette clamp the
burette stand.
Wash a 10cm3 pipette with tap water,rinse it with distilled water and then rinse it with the
standard sodium carbonate solution.
Pipette out exactly 10cm 3 of standard sodium carbonate solution into a clean conical
flask.Add 2-3 drops of methyl orange indicator . The solution turns yellow. Place the
conical flask on a white glazed tile.Titrate the solution against hydrochloric acid taken in
the burette.Initially add small amounts of hydrochloric acid keeping the conical flask
swirled and then add the acid drop wise until the solution in the conical flask shows a
sharp change in colour from yellow to orange red. Now, note the final reading of the
solution in the burette.
Repeat the titration for concordant values.

Result: concentration of the given HCl solution =……….M

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Tabulation and calculation:

In burette: HCl solution

In conical flask: Na 2CO3 solution

Indicator: Methyl Orange

Colour Change: yellow to orange red.

Titration of 10cm 3 of Na2CO3 vs HCl

Trial No 1 2 3
Final Burette reading
Initial Burette reading
Volume of HCl added
in cm 3
3
V2 =…….cm

Na2CO3 HCl

a1M1V1 = a 2M2V2

where, a1= Acidity of Na 2CO3

a2=Basicity of HCl

M1=Molarity of Na 2CO3

M2=Molarity of HCl

V1=Volume of Na 2CO3

V2=Volume of HCl

a1m1v1
Strength of Hcl (M2) =
a2v2

=
=_________M.

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Experiment No - 5
Estimation of sodium hydroxide using oxalic acid

Aim:

To determine the concentration of the given solution of sodium hydroxide by titrating against
standard solution of oxalic acid.

Principle:

Sodium hydroxide reacts with oxalic acid as follows:

COOH COONa

COOH +2NaOH→ +2H 2O

COONa

1 mole of oxalic acid ≡2 mole of NaOH

The molarity of the solution can be can be calculated using the formula,

a1M1V1=a 2M2V2

Where a1M1V1 are respectively the basicity, molarity and volume of the acid while a 2 ,M2 and V2
are the acidity , molarity and the volume of the base.

Molecular mass of oxalic acid crystals , H 2C2O4 .2H2O is 126 g mol -1


-1
Molecular mass of NaOH = 40 gmol .

A known volume of sodium hydroxide is titrated against standard oxalic acid.Oxalic acid is a
weak acid while sodium hydroxide is a strong base.Therefore, phenolphthalein is used as the
indicator. Phenolphthalein turns pink in alkaline solution while it remains colourless in neutral
and acidic solutions.The end point is reached when the last drop of oxalic acid added from the
burette turns the colour of NaOH solution in the conical flask from pink to colourless.

Procedure:

Wash the burette with tap water,rinse it with distilled water and then rinse it with
the standard oxalic acid solution.Then fill the burette with the standard oxalic
acid solution. Care should be taken to see that there is no air bubbles trapped
inside the burette and its nozzle.Note the initial reading of the burette.Clamp the
burette to the burette stand.

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Wash a 10cm3 pipette with tap water,rinse it with distilled water and then rinse it
with the given Sodium hydroxide solution. Pipette out exactly 10cm3 of the
Sodium hydroxide solution.Add 2-3 drop s of phenolphthalein indicator. The
solution turns pink.Place the conical flas k on a glazed tile. Add oxalic acid from
the burette to the conical flask.Keep the conical flask swirling after each addition
of oxalic acid.Add oxalic acid in small amount initially and then dropwise. Near
the end point the pink colour fades away. Continue to add the acid drop at a
time,swirling the conical flask until the last drop added turns the solution from
light pink to colourless. Note the final reading of the burette.

Result: Concentration of NaOH solution = …………M

Tabulation and Calculation:

In burette: Oxalic Acid solution

In conical flask: NaOH solution

Indicator: phenolphthalein

Colour Change: Pink to colourless

Titration of 10cm 3 of NaOH vs Oxalic acid

Trial No 1 2 3
Final Burette reading
Initial Burette reading
Volume of Oxalic acid
added in cm 3
V1 =…….cm3

Oxalic acid NaOH

a1M1V1 = a 2M2V2

=…………M

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Experiment No - 6
Estimation of sodium hydroxide using HCl

Aim:

To estimate the concentration of NaOH using 0.1M. HCl.

Principle :

A known volume NaOH solution is titrated against standard HCl solution using phenolpthalein.

NaOH + HCl NaCl + H20

Molarity of solution is calculated using the formula


a1 M1 V1 = a2 M2 V2

Where a1 and a2 are the acidity and basicity of the base and acid respectively.

M1 and M2 are the molarities. V1 and V2 are the volume of base and acid respectively.

Procedure :

A clean burette is washed with the water and rinsed with 0.1 M HCl solution. It is then filled with
HCl solution. Initial burette reading is noted. A 10cm3 of cleaned pepette is washed with
H20 and rinsed with NaOH solution. Exactly 10cm3 of NaOH solution is pipetted to a cleaned
conical flask. 2 drops of phenolphthalein is added, the solution turns pink.

The solution in conical flask is titrated against HCl taken in the burette. At the end point pink
colour of solution changes to colourless. Final burette reading is noted. The titration is repeated
to get agreeing values.

Result :

concentration of NaOH solution = _________________M

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Tabulation and calculation

Titration of 10cm3 of NaOH using HCl.


In burette - HCl solution
In conical glass - NaOH solution
Indication - phenolphthalein
Colour Change - pink to colourless

Trial No. 1 2 3

Final
burette
reading

Initital
burette
reading

Volume of
HCl added in
(cm3)

V2 = cm3

a1 = acidity of NaOH
a2 = basicity of HCl
M1 = Molarity of NaOH
M2 = Molarity of HCl
V1 = Volume of NaOH
V2 = Volume of HCl

NaOH HCl
a1M1V1 = a2M2V2

Strength of NaOH, M1 = a2 M2 V2
a1 v1
M1 =

M1 = _______________ M.

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Inorganic salt analysis


Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt.

Experiment Observation Inference


1.The given salt is observed in the White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be
presence of light. absent in salt.
Light pink crystalline Mn 2+ salts may be present.

White amorphous CO 32-,HCO3-,or S2- may be present


2.Solubility in water: Soluble No inference possible
A pinch of salt+ 10 drops of water Insoluble Salts of Na+ ,K+ or NH4+ may be
and shaken. absent.

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt +dil.H 2SO4 Brisk effervescence I group acid radicals are present
Lime water turns milky Carbonate is present and
The gas liberated is passed into confirmed
the test tube containing lime No brisk effervescence 1 group acid radicals are
water. absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO 3-)

A pinch of salt+Conc.H 2SO4 Colourless fuming gas is II group acid radicals is present
evolved, which gives dense
white fumes with a glass rod Chloride may be present
dipped in NH 4OH

Reddish brown fumes and the II group acid radical is present


solution turns brown
Bromide may be present
No characteristic observation Chloride and Bromide are
absent
Above solution+Copper Reddish brown fumes and the IIgroup acid radicals is present
turnings. solution turns blue
Heated strongly. Nitrate may be present

No reddish brown gas Nitrate is absent


II group acid radicals absent.

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DETECTION OF THIRD GROUP ACID RADICAL (SO42-)


a)Barium Chloride test: A white precipitate insoluble III group acid radical is
Clear solution of the salt in in excess of dil.HCl present
dil.HCl+2drops of Barium
chloride solution. Sulphate is present and
confirmed
b)Lead acetate test: A white precipitate soluble in Sulphate is present and
Clear solution of the salt in ammonium acetate solution confirmed.
water+Acetic acid+Lead
acetate solution.

CONFIRMATORY TEST FOR CHLORIDE (Cl -)

1.Silver Nitrate test: A curdy white precipitate Chloride is confirmed.


Clear salt solution in dilute soluble in excess of
Nitric acid+3 drops of silver ammonium hydroxide
nitrate solution
2.Chromyl Chloride test:
A pinch of salt +potassium Reddish brown vapours of
dichromate crystals +few Chromyl Chloride are evolved
drops of conc.H 2SO4,mixture
is heated
Yellow solution.
The vapours are dissolved in
water.
Yellow precipitate Chloride is confirmed.
To the yellow solution+3
drops of NH 4OH+3 drops of
acetic acid+2 drops of lead
acetate solution

CONFIRMATORY TEST FOR BROMIDE (Br -)

1.Silver Nitrate test: A pale yellow precipitate Bromide is confirmed


Clear salt solution in dilute partially soluble in excess of
nitric acid+ boil & cool 3 drops ammonium hydroxide
of silver nitrate solution.
2.Orange globule test: Orange brown globule Bromide is confirmed
Clear salt solution in water+ 3 separates out
drops of carbon tetrachloride
+ Chlorine
water, shaken well.

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CONFIRMATORY TEST FOR NITRATE(NO 3-):


Brown ring test:
3 drops of clear salt solution A brown ring is formed at the Nitrate is confirmed
in dil.H 2SO4+3 drops of junction of two liquids
freshly saturated solution of
Mohr’s salt+conc.H 2SO4 is
added carefully along the
sides of the test tube

DETECTION OF BASIC RADICALS (CATIONS):

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH: A Pungent smell of ammonia


A pinch of the salt is heated which gives dense white NH4+ may be present
with 5 drops of sodium fumes with a glass rod dipped
hydroxide in conc.HCl

No pungent smell of NH 4+ is absent


ammonia

CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:

Nessler’s reagent test:


One drop of salt solution in Brown precipitate is formed NH4+ is confirmed
water+3 drops of Nessler’s
reagent

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a test tube and it is dissolved in minimum amount of water or dil. HCl.

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DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 No precipitate I group cations are absent


of dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added
Group III: 1cm 3 of OS +2cm 3 A Gelatinous white precipitate Al 3+ may be present
of NH4Cl solution +NH 4OH No precipitate III group cations are absent
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 A flesh coloured precipitate Mn 2+ may be present
of NH4Cl solution +NH 4OH
No precipitate IV group cations are absent
solution in excess + H2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 A white precipitate Ba 2+, Sr2+, or ca 2+ may be
of NH4Cl solution +NH 4OH present
solution in excess No precipitate V group cations are absent
+(NH 4)2CO3 Solution

Confirmatory test for Aluminium(Al 3+ )

a)Sodium hydroxide test:


1cm 3 of original Gelatinous white precipitate
solution+NaOH solution soluble in excess of NaOH
dropwise White gelatinous precipitate Al3+ is confirmed
Above solution is treated with reappears
NH4Cl solution.
b)Lake test: Al3+ is confirmed
Original solution+blue litmus Blue precipitate floating in the
solution +NH 4OH drop wise colourless solution
along the sides of the test
tube

Confirmatory test for Manganous (Mn2+ )

a)Sodium hydroxide test: White precipitate formed is Mn2+ is confirmed


1cm 3 of original insoluble in excess of NaOH
solution+NaOH solution and turns brown on exposure
dropwise. to air.
b) Lead dioxide test: Supernatant layer is pink in Mn2+ is confirmed
1cm 3 of OS +conc.HNO 3+a colour.
pinch of lead dioxide,heated
strongly and diluted with
water.

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Confirmatory test for V group cations:

a)Potassium chromate test: Yellow precipitate Ba 2+ is confirmed


1cm3 of original
solution+acetic + acid + No yellow precipitate Ba2+ is absent
potassium chromate solution
b)Ammonium sulphate test: White precipitate Sr2+ is confirmed
1cm 3 of original
solution+ammonium sulphate No white precipitate Sr2+ is absent
solution,warm.

c)Ammonium oxalate test: White precipitate Ca2+ is confirmed


1Cm3 of original solution+5
drops of NH 4OH +Ammonium
oxalate solution.
Flame test: a) Apple green colour is Ba2+ is confirmed
A pinch of salt +few drops imparted to the flame
conc.HCl and made into a b) Crimson red colour is Sr2+ is confirmed
paste. imparted to the flame
The paste is held to the flame c) Brick red colour is imparted Ca2+ is confirmed
with the help of a platinum to the flame
wire.

Analysis of VI group basic radical:

Confirmatory test for


Magnesium (Mg 2+ )

1) Disodium hydrogen
phosphate test:
1cm 3 of original White crystalline precipitate Mg 2+ is confirmed.
solution+2cm3 of NH4OH+5
drops of disodium hydrogen
phosphate.The side of the
test tube is scratched with
glass rod.
2) Sodium hydroxide test:
1cm 3 of original White precipitate insoluble in Mg 2+ is confirmed.
solution+NaOH Solution. NaOH solution

Report: The given inorganic salt contains,

Anion is ……………………(……..).It belongs to group……….

Cation is…………………….(…….).It belongs to group……….

Hence the given salt is…………………………(……….)

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Experiment No - 7
Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-1

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO 3-)

A pinch of salt+conc.H 2SO4 Colourless fuming gas is II group acid radical is


evolved, which gives dense present
white fumes with a glass rod Chloride may be present
dipped in NH 4OH

CONFIRMATORY TEST FOR CHLORIDE(Cl -)

1.Silver Nitrate test: A curdy white precipitate Chloride is confirmed.


Clear salt solution in dilute soluble in excess of
Nitric acid+3 drops of silver ammonium hydroxide
nitrate solution
2.Chromyl Chloride test:
A pinch of salt +potassium Reddish brown vapours of
dichromate crystals +few Chromyl Chloride are evolved
drops of conc.H 2SO4,mixture
is heated
Yellow solution.
The vapours are dissolved in
water.
Yellow precipitate Chloride is confirmed.
To the yellow solution+3
drops of NH 4OH+3 drops of
acetic acid+2 drops of lead
acetate solution

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DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH: A Pungent smell of ammonia


A pinch of the salt is heated which gives dense white NH4+ may be present
with 5 drops of sodium fumes with a glass rod dipped
hydroxide in conc.HCl

CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:

Nessler’s reagent test:


One drop of salt solution in Brown precipitate is formed NH4+ is confirmed
water+3 drops of Nessler’s
reagent

Result: The given inorganic salt contains

Anion is Chloride(Cl -). It belongs to II group

Cation is Ammonium(NH 4+ ).It belongs to 0 th group

Hence the given salt is Ammonium Chloride(NH 4Cl).

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Experiment No - 8
Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-2

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICAL: (Cl -,Br-,NO 3-)

A pinch of salt +conc.H 2SO4 No characteristic observation Chloride and Bromide are
absent
Above solution+Copper No reddish brown gas Nitrate is absent
turnings.Heated strongly. II group acid radicals are
absent.

DETECTION OF THIRD GROUP ACID RADICAL(SO 42-)

a)Barium Chloride test: A white precipitate insoluble III group acid radical is
Clear solution of the salt in in excess of dil.HCl present
dil.HCl+2drops of Barium
chloride solution. Sulphate is present and
confirmed
b)Lead acetate test: A white precipitate soluble in Sulphate is present and
Clear solution of the salt in ammonium acetate solution confirmed.
water+Acetic acid+Lead
acetate solution.

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DETECTION OF BASIC RADICALS (CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of water.

DETECTION OF THE GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 of No precipitate I group cations are absent


dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added
Group III: 1cm 3 of OS +2Cm 3 A Gelatinous white precipitate III group cation is present
of NH4Cl solution +NH 4OH Al3+ may be present
solution in excess

Confirmatory test for Aluminium(Al3+ )

a)Sodium hydroxide test:


1Cm3 of original Gelatinous white precipitate
solution+NaOH solution soluble in excess of NaOH
dropwise White gelatinous precipitate Al3+ is confirmed
Above solution is treated with reappears
NH4Cl solution.
b)Lake test: Al3+ is confirmed
Original solution+blue litmus Blue precipitate floating in the
solution +NH 4OH drop wise colourless solution
along the sides of the test tube

Result:

The given inorganic salt contains

Anion is Sulphate (SO4 2-) It belongs to Group III

Cation is Aluminium(Al 3+ )It belongs to Group III

Hence the given salt is Aluminium Sulphate Al 2(SO4)3

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Experiment No - 9
Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-3

Experiment Observation Inference


1.Colour &Appearance
Thegivensaltisobservedin White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO 3-)

A pinch of salt+conc.H 2SO4 Colourless fuming gas is II group acid radical is


evolved, which gives dense present
white fumes with a glass rod Chloride may be present
dipped in NH 4OH

CONFIRMATORY TEST FOR CHLORIDE(Cl -)

1.Silver Nitrate test: A curdy white precipitate Chloride is confirmed.


Clear salt solution in dilute soluble in excess of
Nitric acid+3 drops of silver ammonium hydroxide
nitrate solution
2.Chromyl Chloride test:
A pinch of salt +potassium Reddish brown vapours of
dichromate crystals +few Chromyl Chloride are evolved
drops of conc.H 2SO4,mixture
is heated
Yellow solution.
The vapours are dissolved in
water.
Yellow precipitate Chloride is confirmed.
To the yellow solution+3
drops of NH 4OH+3 drops of
acetic acid+2 drops of lead
acetate solution

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VIKAS PRE-UNIVERSITY COLLEGE

DETECTION OF BASIC RADICALS (CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of water.

DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 No precipitate I group cations are absent


of dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added
Group III: 1cm 3 of OS +2Cm 3 No precipitate III group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 No precipitate IV group cations are absent
of NH4Cl solution +NH 4OH
solution in excess+H 2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 A white precipitate V group cations is present
of NH4Cl solution +NH 4OH
solution in excess Ba2+ ,Sr2+ ,or ca 2+ may be
+(NH 4)2CO3 Solution present

Confirmatory test for V group cations:

a)Potassium chromate test:


1cm3 of original Yellow precipitate Ba2+ is confirmed
solution+acetic acid +
potassium chromate solution
Flame test:
A pinch of salt +few drops Apple green colour is Ba2+ is confirmed
conc.HCl and made into a imparted to the flame
paste.
The paste is held to the flame
with the help of a platinum
wire.

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Result: The given inorganic salt contains

Anion is Chloride(Cl -). It belongs to group II.

Cation is Barium (Ba2+ ).It belongs to groupV.

Hence the given salt is Barium Chloride(BaCl 2)

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VIKAS PRE-UNIVERSITY COLLEGE

Experiment No - 10
Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-4

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White amorphous CO3 2-,HCO3- ,Or S2- may be
the presence of light present.
2.Solubility in water:
A pinch of salt+10 drops of Insoluble Salts of Na+ ,K+ , or NH4+ may
water and shaken well be absent.
DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt +dil.H 2SO4 Brisk effervescence I group acid radicals are
present
The gas liberated is passed Lime water turns milky
into the test tube containing Carbonate is present and
lime water. confirmed

DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of dil.HCl

DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 No precipitate I group cations are absent


of dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added

24
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Group III: 1cm 3 of OS +2Cm 3 No precipitate III group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 No precipitate IV group cations are absent
of NH4Cl solution +NH 4OH
solution in excess+H 2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 A white precipitate V group cations is present
of NH4Cl solution +NH 4OH
solution in excess Ba2+ ,Sr2+ ,or ca 2+ may be
+(NH 4)2CO3 Solution present

Confirmatory test for V group cations:

a)Potassium chromate test:


1Cm3 of original No yellow precipitate Ba2+ is absent
solution+potassium chromate
solution
b)Ammonium sulphate test:
1Cm3 of original No white precipitate Sr2+ is absent
solution+ammonium sulphate
solution,warm.

c)Ammonium oxalate test:


1Cm3 of original solution+5 White precipitate Ca2+ is confirmed
drops of NH 4OH +Ammonium
oxalate solution.
Flame test:
A pinch of salt +few drops Brick red colour is imparted to Ca2+ is confirmed
conc.HCl and made into a the flame
paste.
The paste is held to the flame
with the help of a platinum
wire.

Report:

Anion is Carbonate (CO 32-).It belongs to group I.

Cation is Calcium (Ca2+ ).It belongs to groupV.

Hence the given salt is Calcium Carbonate (CaCO 3).

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VIKAS PRE-UNIVERSITY COLLEGE

Experiment No -11
Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-5

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICAL: (Cl -,Br-,NO 3-)

A pinch of salt +conc.H 2SO4 No characteristic observation Chloride and Bromide are
absent
Above solution+Copper No reddish brown gas Nitrate is absent
turnings.Heated strongly. II group acid radicals are
absent.

DETECTION OF THIRD GROUP ACID RADICAL(SO 42-)

a)Barium Chloride test: A white precipitate insoluble III group acid radical is
Clear solution of the salt in in excess of dil.HCl present
dil.HCl+2drops of Barium
chloride solution. Sulphate is present and
confirmed
b)Lead acetate test: A white precipitate soluble in Sulphate is present and
Clear solution of the salt in ammonium acetate solution confirmed.
water+Acetic acid+Lead
acetate solution.

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DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of Water

DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 of No precipitate I group cations are absent


dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added
Group III: 1cm 3 of OS +2Cm 3 No precipitate III group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 No precipitate IV group cations are absent
of NH4Cl solution +NH 4OH
solution in excess+H 2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 No precipitate V group cations are absent
of NH4Cl solution +NH 4OH
solution in excess +(NH 4)2CO3
Solution

Analysis of VI group basic radical:

Confirmatory test for


Magnesium (Mg 2+ )

1)Disodium hydrogen
phosphate test:
1Cm3 of original White crystalline precipitate Mg 2+ is confirmed.
solution+2Cm3 of NH4OH+5
drops of disodium hydrogen
phosphate.The side of the test
tube is scratched with glass
rod.
2) Sodium hydroxide test:
1Cm3 of original White precipitate insoluble in Mg 2+ is confirmed.
solution+NaOH Solution. NaOH solution

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VIKAS PRE-UNIVERSITY COLLEGE

Report: The given inorganic salt contains,

Anion is Sulphate(SO42-).It belongs to groupIII

Cation isMagnesium(Mg 2+ ).It belongs to groupVI.

Hence the given salt isMagnesium Sulphate (MgSO 4.)

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Experiment No -12
Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-6

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO 3-)

A pinch of salt+conc.H 2SO4 Reddish brown fumes and the II group acid radical is
solution turns brown present
Bromide may be present

CONFIRMATORY TEST FOR BROMIDE (Br -)

1.Silver Nitrate test: A pale yellow precipitate Bromide is confirmed


Clear salt solution in dilute partially soluble in excess of
nitric acid+3 drops of silver ammonium hydroxide
nitrate solution.
2.Orange globule test: Orange brown globule Bromide is confirmed
Clear salt solution in water+3 separates out
drops of carbon
tetrachloride+Chlorine
water,shaken well.

DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

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VIKAS PRE-UNIVERSITY COLLEGE

Action of NaOH: A Pungent smell of ammonia


A pinch of the salt is heated which gives dense white NH4+ may be present
with 5 drops of sodium fumes with a glass rod dipped
hydroxide in conc.HCl

CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:

Nessler’s reagent test:


One drop of salt solution in Brown precipitate is formed NH4+ is confirmed
water+3 drops of Nessler’s
reagent

Result: The given inorganic salt contains

Anion is Bromide(Br -). It belongs to II group

Cation is Ammonium(NH 4+ ).It belongs to 0 th group

Hence the given salt is Ammonium Bromide(NH 4Br).

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Experiment No -13
Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-7

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White amorphous CO3 2-,HCO3- ,Or S2- may be
the presence of light present.
2.Solubility in water:
A pinch of salt+10 drops of Insoluble Salts of Na+ ,K+ , or NH4+ may
water and shaken well be absent.
DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt +dil.H 2SO4 Brisk effervescence I group acid radicals are
present
The gas liberated is passed Lime water turns milky Carbonate is present and
into the test tube containing confirmed
lime water.

DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of dil.HCl

DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 No precipitate I group cations are absent


of dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added

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VIKAS PRE-UNIVERSITY COLLEGE

Group III: 1cm 3 of OS +2Cm 3 No precipitate III group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 No precipitate IV group cations are absent
of NH4Cl solution +NH 4OH
solution in excess+H 2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 No precipitate V group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
+(NH 4)2CO3 Solution

Analysis of VI group basic radical:

Confirmatory test for


Magnesium (Mg 2+ )

1)Disodium hydrogen
phosphate test:
1cm 3 of original White crystalline precipitate Mg 2+ is confirmed.
solution+2cm3 of NH4OH+5
drops of disodium hydrogen
phosphate.The side of the
test tube is scratched with
glass rod.
2) Sodium hydroxide test:
1cm 3 of original White precipitate insoluble in Mg 2+ is confirmed.
solution+NaOH Solution. NaOH solution

Report: The given inorganic salt contains,

Anion is Carbonate (CO 32-). It belongs to groupI

Cation isMagnesium(Mg 2+ ).It belongs to groupVI.

Hence the given salt isMagnesium Carbonate(MgCO 3)

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Experiment No -14
Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-8

Experiment Observation Inference


1.Colour &Appearance
The given salt is observed in White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may
the presence of light be absent.
2.Solubility in water:
A pinch of salt+10 drops of Soluble No inference possible
water and shaken well

DETECTION OF ACID RADICALS: (ANION)

DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)

A pinch of salt+dil.H 2SO4 No brisk effervescence I group acid radicals absent

DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO 3-)

A pinch of salt+conc.H 2SO4 Colourless fuming gas is II group acid radical is


evolved, which gives dense present
white fumes with a glass rod Chloride may be present
dipped in NH 4OH

CONFIRMATORY TEST FOR CHLORIDE(Cl -)

1.Silver Nitrate test: A curdy white precipitate Chloride is confirmed.


Clear salt solution in dilute soluble in excess of
Nitric acid+3 drops of silver ammonium hydroxide
nitrate solution
2.Chromyl Chloride test:
A pinch of salt +potassium Reddish brown vapours of
dichromate crystals +few Chromyl Chloride are evolved
drops of conc.H 2SO4,mixture
is heated
Yellow solution.
The vapours are dissolved in
water.
Yellow precipitate Chloride is confirmed.
To the yellow solution+3
drops of NH 4OH+3 drops of
acetic acid+2 drops of lead
acetate solution

33
VIKAS PRE-UNIVERSITY COLLEGE

DETECTION OF BASIC RADICALS(CATIONS)

TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)

Action of NaOH:
A pinch of the salt is heated No pungent smell of ammonia NH4+ is absent.
with 5 drops of sodium
hydroxide

PREPARATION OF ORIGINAL SOLUTION:

The given salt is taken in a clean test tube and it is dissolved in minimum amount of Water

DETECTION OF GROUP OF CATIONS:

Group I: 1cm 3 of OS + 1cm 3 No precipitate I group cations are absent


of dil.HCl in a test tube
Group II: 1cm 3 of OS + 1cm 3 No precipitate II group cations are absent
of dil.HCl+H 2S solution is
added
Group III: 1cm 3 of OS +2Cm 3 No precipitate III group cations are absent
of NH4Cl solution +NH 4OH
solution in excess
Group IV: 1cm 3 of OS +2Cm 3 No precipitate IV group cations are absent
of NH4Cl solution +NH 4OH
solution in excess+H 2S
solution is added
Group V: 1cm 3 of OS +2Cm 3 A white precipitate V group cations is present
of NH4Cl solution +NH 4OH
solution in excess Ba2+ ,Sr2+ ,or ca 2+ may be
+(NH 4)2CO3 Solution present

Confirmatory test for V group cations:

a)Potassium chromate test:


1Cm3 of original No yellow precipitate Ba2+ is absent
solution+potassium chromate
solution
b)Ammonium sulphate test:
1Cm3 of original White precipitate Sr2+ is confirmed
solution+ammonium sulphate
solution,warm.

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Flame test:
A pinch of salt +few drops Crimson red colour is Sr2+ is confirmed
conc.HCl and made into a imparted to the flame
paste.
The paste is held to the flame
with the help of a platinum
wire.

Report: The given inorganic salt contains,

Anion is Chloride(Cl -). It belongs to groupII

Cation is Strontium (Sr 2+ ).It belongs to groupV

Hence the given salt is Strontium Chloride(SrCl 2)

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VIKAS PRE-UNIVERSITY COLLEGE

SAFETY PROCEDURE IN LAB


1. Do not enter the laboratory when an instructor/lab assistant is not present or
the lab door is closed. Finish your lab work on time to clean up before the end of
the scheduled lab period.

2. Perform only authorized experiments. Parents, Visitors are not permitted to be


with you while you do your lab work.

3. Wear personal protective equipment (PPE) at all times in the chemistry


laboratory including when cleaning up following an experiment.

4. Shoes which offer reasonable protection will be worn while in the laboratory.
Shoes must cover the entire foot, including the toes, the top of the foot, and the
heel.

5. Hair that is longer than shoulder-length must be tied back at all times.

6. Eating, drinking, mouth rinsing, applying cosmetics or lip balm or handling


contact lenses is prohibited in the lab areas. No chewing gum is allowed.

7. Be considerate of others working in the laboratory. Do not distract others while


conducting experiments or accomplishing lab activities. When finished with
equipment or materials to be shared with others, make the equipment or
materials available to others as quickly as possible.

8. Before leaving the lab, clean all equipment, glassware and the work area you
have been using. Return equipment and glassware to their proper places in
the laboratory.

9. Know the location and proper use of safety equipment in the laboratory.

10. Immediately notify the lab instructor of chemical spills, broken glass or other
hazards. Do not attempt to clean up such mishaps/materials by yourself
without first alerting your instructor/lab supervisor.

11. Immediately notify the instructor/lab supervisor of any accidents, injuries, or


situations in which exposure to human blood or other potentially infectious
materials in the laboratory has occurred, regardless of how minor they may
appear to be.

12. You may be exposed to potentially hazardous materials in the process of


completing your required laboratory activities. Persons with specific health
concerns such as wearers of contact lenses, persons with known
hypersensitivities, etc. should consult their personal physician for advisement
about potential risks before continuing in the course.

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