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CHEMISTRY PRACTICAL 1
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LAB MANUAL
CY OTI LS LER GE EVI MNU A- NE GR
AP LS UA RKI U
V
VIKAS PRE-UNIVERSITY COLLEGE
Experiment No -1 Parts of Bunsen Burner 03
Experiment No -2Study of glass works 04
Experiment No -3 Preparation of standard oxalic acid solution. 05
Experiment No -4Estimation 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 - 7Systematic Semi-micro qualitative analysis of a simple inorganic salt No-1 17
Experiment No - 8Systematic Semi-micro qualitative analysis of a simple inorganic salt No-2 19
Experiment No - 9Systematic Semi-micro qualitative analysis of a simple inorganic salt No-3 22
Experiment No - 10Systematic Semi-micro qualitative analysis of a simple inorganic salt No-4 24
Experiment No -11Systematic semi-micro qualitative analysis of a simple inorganic salt-5 26
Experiment No -12Systematic semi-micro qualitative analysis of a simple inorganic salt-6 29
Experiment No -13Systematic semi-micro qualitative analysis of a simple inorganic salt-7 31
Experiment No -14Systematic Semi-micro qualitative analysis of a simple inorganic salt No-8 33
Index
CHEMISTRY PRACTICAL 1
LAB MANUAL
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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
CHEMISTRY PRACTICAL 1
LAB MANUAL
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Fig2: Zones of flame of Bunsen burner.
A small blue region at the base of the flame
A dark inner region of unburnt gases
A luminous region of incomplete combustion
A pale blue outer zone of complete combustion
Luminous flame
Fig2: Zones of flame of Bunsen burner.
A small blue region at the base of the flame
A dark inner region of unburnt gases
A pale blue outer zone of complete combustion
Non Luminous flame
3
2
1
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 Bunsen 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
Experiment No -2
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Making a scratch
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 hydrated 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 oxalic 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.
CHEMISTRY PRACTICAL 1
LAB MANUAL
Experiment No -3
5
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 Na2CO ≡3 2 mole of HCl
Acidity of the base Na2CO3 =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 indicator 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
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 10cm3 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
Experiment No -4
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solution in the burette.
Repeat the titration for concordant values.
Result: concentration of the given HCl solution =……….M
burette stand.
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Tabulation and calculation:
In burette: HCl solution
In conical flask: Na2CO3 solution
Indicator: Methyl Orange
Colour Change: yellow to orange red.
Titration of 10cm 3 of Na2CO3 vs HCl
Trial No 1 2 3 F i nal Burette reading I n itial Burette reading Volume of HCl added in cm3
V2 =…….cm 3
Na2CO3 HCl
a M V1 1 1 = a M V 2 2 2
where, a1= Acidity of Na2CO3
a2=Basicity of HCl
M1=Molarity of Na 2CO 3
M2=Molarity of HCl
V1=Volume of Na 2CO 3
V2=Volume of HCl
CHEMISTRY PRACTICAL 1
LAB MANUAL
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Strength of Hcl (M ) =2
a m v1 1 1
a v2 2
=
=_________M.
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
+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,
a M V1 1 1=a M V 2 2 2
Where a M V1 1 1 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 C O2 2 4 .2H2O is 126 g mol-1
Molecular mass of NaOH = 40 gmol -1 .
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.
Experiment No - 5
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COOH
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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
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LAB MANUAL
9
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 F i nal Burette reading
I n itial Burette reading
Volume of Oxalic acid
added in cm 3
V1 =…….cm3
Oxalic acid NaOH
a M V1 1 1 = a M V2 2 2
=
=…………M
10
Estimation of sodium hydroxide using HCl
Aim:
To estimate the concentration of NaOH using 0.1M. HCl.
Experiment No - 6
Principle :
A known volume NaOH solution is titrated against standard HCl solution using phenolpthalein.
Molarity of solution is calculated using the formula a M V = a M V1 1 1 2 2 2
NaOH + HCl NaCl + H 02
Where a and a are the acidity and basicity of the base and acid respectively.1 2
M and M are the molarities. V and V are the volume of base and acid respectively.1 2 1 2
Procedure :
A clean burette is washed with the water and rinsed with 0.1 M HCl solution. It is then filled with 3HCl solution. Initial burette reading is noted. A 10cm of cleaned pepette is washed with
3H 0 and rinsed with NaOH solution. Exactly 10cm of NaOH solution is pipetted to a cleaned2
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 pinkcolour of solution changes to colourless. Final burette reading is noted. The titration is repeatedto get agreeing values.
Result :
concentration of NaOH solution = _________________M
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Tabulation and calculation
3Titration of 10cm of NaOH using HCl.In burette - HCl solutionIn conical glass - NaOH solutionIndication - phenolphthaleinColour Change - pink to colourless
Trial No. 1 2 3
Finalburettereading
Inititalburettereading
Volume ofHCl added in
3(cm )
3V = cm2
a = acidity of NaOH1
a = basicity of HCl2
M = Molarity of NaOH1
M = Molarity of HCl 2
V = Volume of NaOH1
V = Volume of HCl 2
NaOH HCl
a M V a M V1 1 1 = 2 2 2
M1 = a2 M2 V2
a1 v1
M1 =
M1 = _______________ M.
Strength of NaOH,
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 presence of light.
White crystalline Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent in salt.
Light pink crystalline Mn 2+ salts may be present.
White amorphous CO32-,HCO3
-,or S2- may be present 2.Solubility in water: A pinch of salt+ 10 drops of water and shaken.
Soluble No inference possible Insoluble Salts of Na+ ,K+ or NH4
+ may be absent.
DETECTION OF ACID RADICALS: (ANION)
DETECTION OF FIRST GROUP ACID RADICAL: (CO32-)
A pinch of salt +dil.H 2SO4
The gas liberated is passed into the test tube containing lime water.
Brisk effervescence I group acid radicals are present
Lime water turns milky Carbonate is present and confirmed
No brisk effervescence 1 group acid radicals are absent
DETECTION OF SECOND GROUP ACID RADICALS (Cl -,Br-,NO3-)
A pinch of salt+Conc.H 2SO4 Colourless fuming gas is evolved, which gives dense white fumes with a glass rod dipped in NH 4OH
II group acid radicals is present Chloride may be present
Reddish brown fumes and the solution turns brown
II group acid radical is present Bromide may be present
No characteristic observation Chloride and Bromide are absent
Above solution+Copper turnings. Heated strongly.
Reddish brown fumes and the solution turns blue No reddish brown gas
IIgroup acid radicals is present Nitrate may be present Nitrate is absent II group acid radicals absent.
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a)Barium Chloride test: Clear solution of the salt in dil.HCl+2drops of Barium chloride solution.
A white precipitate insoluble in excess of dil.HCl
III group acid radical is present Sulphate is present and confirmed
b)Lead acetate test: Clear solution of the salt in water+Acetic acid+Lead acetate solution.
A white precipitate soluble in ammonium acetate solution
Sulphate is present and confirmed.
CONFIRMATORY TEST FOR CHLORIDE (Cl -)
1.Silver Nitrate test: Clear salt solution in dilute Nitric acid+3 drops of silver nitrate solution
A curdy white precipitate soluble in excess of ammonium hydroxide
Chloride is confirmed.
2.Chromyl Chloride test: A pinch of salt +potassium dichromate crystals +few drops of conc.H 2SO4,mixture is heated The vapours are dissolved in water. To the yellow solution+3 drops of NH4OH+3 drops of acetic acid+2 drops of lead acetate solution
Reddish brown vapours of Chromyl Chloride are evolved Yellow solution. Yellow precipitate
Chloride is confirmed.
CONFIRMATORY TEST FOR BROMIDE (Br -)
1.Silver Nitrate test: Clear salt solution in dilute nitric acid+ boil & cool 3 drops of silver nitrate solution.
A pale yellow precipitate partially soluble in excess of ammonium hydroxide
Bromide is confirmed
2.Orange globule test: Clear salt solution in water+ 3 drops of carbon tetrachloride + Chlorine water, shaken well.
Orange brown globule separates out
Bromide is confirmed
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DETECTION OF THIRD GROUP ACID RADICAL (SO42-)
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Brown ring test: 3 drops of clear salt solution in dil.H2SO4+3 drops of freshly saturated solution of Mohr’s salt+conc.H 2SO4 is added carefully along the sides of the test tube
A brown ring is formed at the junction of two liquids
Nitrate is 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 with 5 drops of sodium hydroxide
A Pungent smell of ammonia which gives dense white fumes with a glass rod dipped in conc.HCl
NH4
+ may be present
No pungent smell of ammonia
NH4+ is absent
CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:
Nessler’s reagent test: One drop of salt solution in water+3 drops of Nessler’s reagent
Brown precipitate is formed
NH4
+ is confirmed
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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CONFIRMATORY TEST FOR NITRATE(NO 3-):
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DETECTION OF GROUP OF CATIONS:
Group I: 1cm3 of OS + 1cm3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Group III: 1cm3 of OS +2cm 3 of NH4Cl solution +NH 4OH solution in excess
A Gelatinous white precipitate Al3+ may be present
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess + H2S solution is added
A flesh coloured precipitate Mn 2+ may be present
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO3 Solution
A white precipitate Ba2+, Sr2+, or ca2+ may be present
No precipitate V group cations are absent
Confirmatory test for Aluminium(Al 3+ )
a)Sodium hydroxide test: 1cm 3 of original solution+NaOH solution dropwise Above solution is treated with NH4Cl solution.
Gelatinous white precipitate soluble in excess of NaOH White gelatinous precipitate reappears
Al3+ is confirmed
b)Lake test: Original solution+blue litmus solution +NH 4OH drop wise along the sides of the test tube
Blue precipitate floating in the colourless solution
Al3+ is confirmed
Confirmatory test for Manganous (Mn2+ )
a)Sodium hydroxide test: 1cm 3 of original solution+NaOH solution dropwise.
White precipitate formed is insoluble in excess of NaOH and turns brown on exposure to air.
Mn2+ is confirmed
b) Lead dioxide test: 1cm3 of OS +conc.HNO 3+a pinch of lead dioxide,heated strongly and diluted with water.
Supernatant layer is pink in colour.
Mn2+ is confirmed
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CHEMISTRY PRACTICAL 1
LAB MANUAL
Confirmatory test for V group cations:
a)Potassium chromate test: 1cm3 of original solution+acetic + acid +potassium chromate solution
Yellow precipitate Ba 2+ is confirmed
No yellow precipitate Ba2+ is absent
b)Ammonium sulphate test: 1cm 3 of original solution+ammonium sulphate solution,warm.
White precipitate Sr2+ is confirmed
No white precipitate Sr2+ is absent
c)Ammonium oxalate test: 1Cm3 of original solution+5 drops of NH 4OH +Ammonium oxalate solution.
White precipitate Ca2+ is confirmed
Flame test: A pinch of salt +few drops conc.HCl and made into a paste. The paste is held to the flame with the help of a platinum wire.
a) Apple green colour is imparted to the flame b) Crimson red colour is imparted to the flame c) Brick red colour is imparted to the flame
Ba2+ is confirmed Sr2+ is confirmed Ca2+ is confirmed
Analysis of VI group basic radical:
Confirmatory test for Magnesium (Mg2+ ) 1) Disodium hydrogen phosphate test: 1cm3 of original solution+2cm of NH OH+5 4
drops of disodium hydrogen phosphate.The side of the test tube is scratched with glass rod.
White crystalline precipitate
Mg2+ is confirmed.
2) Sodium hydroxide test: 1cm3 of original solution+NaOH Solution.
White precipitate insoluble in NaOH solution
Mg2+ is confirmed.
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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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 the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt+conc.H 2SO4 Colourless fuming gas is evolved, which gives dense white fumes with a glass rod dipped in NH 4OH
II group acid radical is present Chloride may be present
CONFIRMATORY TEST FOR CHLORIDE(Cl -)
1.Silver Nitrate test: Clear salt solution in dilute Nitric acid+3 drops of silver nitrate solution
A curdy white precipitate soluble in excess of ammonium hydroxide
Chloride is confirmed.
2.Chromyl Chloride test: A pinch of salt +potassium dichromate crystals +few drops of conc.H 2SO4,mixture is heated The vapours are dissolved in water. To the yellow solution+3 drops of NH4OH+3 drops of acetic acid+2 drops of lead acetate solution
Reddish brown vapours of Chromyl Chloride are evolved Yellow solution. Yellow precipitate
Chloride is confirmed.
Experiment No - 7
17
CHEMISTRY PRACTICAL 1
LAB MANUAL
DETECTION OF BASIC RADICALS(CATIONS)
TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)
Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide
A Pungent smell of ammonia which gives dense white fumes with a glass rod dipped in conc.HCl
NH4
+ may be present
CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:
Nessler’s reagent test: One drop of salt solution in water+3 drops of Nessler’s reagent
Brown precipitate is formed
NH4
+ is confirmed
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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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 the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt +conc.H 2SO4 No characteristic observation Chloride and Bromide are absent
Above solution+Copper turnings.Heated strongly.
No reddish brown gas Nitrate is absent II group acid radicals are absent.
DETECTION OF THIRD GROUP ACID RADICAL(SO 42-)
a)Barium Chloride test: Clear solution of the salt in dil.HCl+2drops of Barium chloride solution.
A white precipitate insoluble in excess of dil.HCl
III group acid radical is present Sulphate is present and confirmed
b)Lead acetate test: Clear solution of the salt in water+Acetic acid+Lead acetate solution.
A white precipitate soluble in ammonium acetate solution
Sulphate is present and confirmed.
Experiment No - 8
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CHEMISTRY PRACTICAL 1
LAB MANUAL
DETECTION OF BASIC RADICALS (CATIONS)
TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)
Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
A Gelatinous white precipitate III group cation is present Al3+ may be present
Confirmatory test for Aluminium(Al3+ )
a)Sodium hydroxide test: 1Cm3 of original solution+NaOH solution dropwise Above solution is treated with NH4Cl solution.
Gelatinous white precipitate soluble in excess of NaOH White gelatinous precipitate reappears
Al3+ is confirmed
b)Lake test: Original solution+blue litmus solution +NH 4OH drop wise along the sides of the test tube
Blue precipitate floating in the colourless solution
Al3+ is confirmed
Result:
The given inorganic salt contains
Anion is Sulphate (SO 42-) It belongs to Group III
Cation is Aluminium(Al3+ )It belongs to Group III
Hence the given salt is Aluminium Sulphate Al 2(SO )4 3
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Aim: Systematic Semi-micro qualitative analysis of a simple inorganic salt No-3
Experiment Observation Inference 1.Colour &Appearance The given sal tis observed in the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt+conc.H 2SO4 Colourless fuming gas is evolved, which gives dense white fumes with a glass rod dipped in NH 4OH
II group acid radical is present Chloride may be present
CONFIRMATORY TEST FOR CHLORIDE(Cl -)
1.Silver Nitrate test: Clear salt solution in dilute Nitric acid+3 drops of silver nitrate solution
A curdy white precipitate soluble in excess of ammonium hydroxide
Chloride is confirmed.
2.Chromyl Chloride test: A pinch of salt +potassium dichromate crystals +few drops of conc.H 2SO4,mixture is heated The vapours are dissolved in water. To the yellow solution+3 drops of NH4OH+3 drops of acetic acid+2 drops of lead acetate solution
Reddish brown vapours of Chromyl Chloride are evolved Yellow solution. Yellow precipitate
Chloride is confirmed.
Experiment No - 9
21
CHEMISTRY PRACTICAL 1
LAB MANUAL
DETECTION OF BASIC RADICALS (CATIONS)
TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)
Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4
+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess+H 2S solution is added
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO3 Solution
A white precipitate
V group cations is present Ba2+ ,Sr2+ ,or ca2+ may be present
Confirmatory test for V group cations:
a)Potassium chromate test: 1cm3 of original solution+acetic acid + potassium chromate solution
Yellow precipitate
Ba2+ is confirmed
Flame test: A pinch of salt +few drops conc.HCl and made into a paste. The paste is held to the flame with the help of a platinum wire.
Apple green colour is imparted to the flame
Ba2+ is confirmed
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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(BaCl2)
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CHEMISTRY PRACTICAL 1
LAB MANUAL
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 the presence of light
White amorphous
CO 3
2-,HCO3- ,Or S2- may be
present. 2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Insoluble
Salts of Na+ ,K+ , or NH4
+ may be absent.
DETECTION OF ACID RADICALS: (ANION)
DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)
A pinch of salt +dil.H 2SO4
The gas liberated is passed into the test tube containing lime water.
Brisk effervescence Lime water turns milky
I group acid radicals are present Carbonate is present and 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 with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4
+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Experiment No - 10
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Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess+H 2S solution is added
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO3 Solution
A white precipitate
V group cations is present Ba2+ ,Sr2+ ,or ca2+ may be present
Confirmatory test for V group cations:
a)Potassium chromate test: 1Cm3 of original solution+potassium chromate solution
No yellow precipitate
Ba2+ is absent
b)Ammonium sulphate test: 1Cm3 of original solution+ammonium sulphate solution,warm.
No white precipitate
Sr2+ is absent
c)Ammonium oxalate test: 1Cm3 of original solution+5 drops of NH 4OH +Ammonium oxalate solution.
White precipitate
Ca2+ is confirmed
Flame test: A pinch of salt +few drops conc.HCl and made into a paste. The paste is held to the flame with the help of a platinum wire.
Brick red colour is imparted to the flame
Ca2+ is confirmed
Report:
Anion is Carbonate (CO32-).It belongs to group I.
Cation is Calcium (Ca2+ ).It belongs to groupV.
Hence the given salt is Calcium Carbonate (CaCO3).
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CHEMISTRY PRACTICAL 1
LAB MANUAL
Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-5
Experiment Observation Inference 1.Colour &Appearance The given salt is observed in the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt +conc.H 2SO4 No characteristic observation Chloride and Bromide are absent
Above solution+Copper turnings.Heated strongly.
No reddish brown gas Nitrate is absent II group acid radicals are absent.
DETECTION OF THIRD GROUP ACID RADICAL(SO 42-)
a)Barium Chloride test: Clear solution of the salt in dil.HCl+2drops of Barium chloride solution.
A white precipitate insoluble in excess of dil.HCl
III group acid radical is present Sulphate is present and confirmed
b)Lead acetate test: Clear solution of the salt in water+Acetic acid+Lead acetate solution.
A white precipitate soluble in ammonium acetate solution
Sulphate is present and confirmed.
Experiment No -11
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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 with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4
+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess+H 2S solution is added
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO 3
Solution
No precipitate
V group cations are absent
Analysis of VI group basic radical:
Confirmatory test for Magnesium (Mg2+ ) 1)Disodium hydrogen phosphate test: 1Cm3 of original solution+2Cm3 of NH4OH+5 drops of disodium hydrogen phosphate.The side of the test tube is scratched with glass rod.
White crystalline precipitate
Mg2+ is confirmed.
2) Sodium hydroxide test: 1Cm3 of original solution+NaOH Solution.
White precipitate insoluble in NaOH solution
Mg2+ is confirmed.
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CHEMISTRY PRACTICAL 1
LAB MANUAL
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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Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-6
Experiment Observation Inference 1.Colour &Appearance The given salt is observed in the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt+conc.H 2SO4 Reddish brown fumes and the solution turns brown
II group acid radical is present Bromide may be present
CONFIRMATORY TEST FOR BROMIDE (Br -)
1.Silver Nitrate test: Clear salt solution in dilute nitric acid+3 drops of silver nitrate solution.
A pale yellow precipitate partially soluble in excess of ammonium hydroxide
Bromide is confirmed
2.Orange globule test: Clear salt solution in water+3 drops of carbon tetrachloride+Chlorine water,shaken well.
Orange brown globule separates out
Bromide is confirmed
DETECTION OF BASIC RADICALS(CATIONS)
TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)
Experiment No -12
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CHEMISTRY PRACTICAL 1
LAB MANUAL
Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide
A Pungent smell of ammonia which gives dense white fumes with a glass rod dipped in conc.HCl
NH4
+ may be present
CONFIRMATORY TEST FOR AMMONIUM (NH 4+ ) RADICAL:
Nessler’s reagent test: One drop of salt solution in water+3 drops of Nessler’s reagent
Brown precipitate is formed
NH4
+ is confirmed
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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Aim: Systematic semi-micro qualitative analysis of a simple inorganic salt-7
Experiment Observation Inference 1.Colour &Appearance The given salt is observed in the presence of light
White amorphous
CO 3
2-,HCO3- ,Or S2- may be
present. 2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Insoluble
Salts of Na+ ,K+ , or NH4
+ may be absent.
DETECTION OF ACID RADICALS: (ANION)
DETECTION OF FIRST GROUP ACID RADICAL: (CO 32-)
A pinch of salt +dil.H 2SO4
The gas liberated is passed into the test tube containing lime water.
Brisk effervescence Lime water turns milky
I group acid radicals are present Carbonate is present and 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 with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4
+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Experiment No -13
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CHEMISTRY PRACTICAL 1
LAB MANUAL
Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess+H 2S solution is added
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO3 Solution
No precipitate
V group cations are absent
Analysis of VI group basic radical:
Confirmatory test for Magnesium (Mg2+ ) 1)Disodium hydrogen phosphate test: 1cm 3 of original solution+2cm3 of NH OH+5 4
drops of disodium hydrogen phosphate.The side of the test tube is scratched with glass rod.
White crystalline precipitate
Mg2+ is confirmed.
2) Sodium hydroxide test: 1cm 3 of original solution+NaOH Solution.
White precipitate insoluble in NaOH solution
Mg2+ is confirmed.
Report: The given inorganic salt contains,
Anion is Carbonate (CO32-). It belongs to groupI
Cation isMagnesium(Mg 2+ ).It belongs to groupVI.
Hence the given salt isMagnesium Carbonate(MgCO 3)
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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 the presence of light
White crystalline
Cu2+, Fe3+, Mn2+, Co2+, Ni2+, may be absent.
2.Solubility in water: A pinch of salt+10 drops of water and shaken well
Soluble
No inference possible
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-,NO3-)
A pinch of salt+conc.H 2SO4 Colourless fuming gas is evolved, which gives dense white fumes with a glass rod dipped in NH 4OH
II group acid radical is present Chloride may be present
CONFIRMATORY TEST FOR CHLORIDE(Cl -)
1.Silver Nitrate test: Clear salt solution in dilute Nitric acid+3 drops of silver nitrate solution
A curdy white precipitate soluble in excess of ammonium hydroxide
Chloride is confirmed.
2.Chromyl Chloride test: A pinch of salt +potassium dichromate crystals +few drops of conc.H 2SO4,mixture is heated The vapours are dissolved in water. To the yellow solution+3 drops of NH4OH+3 drops of acetic acid+2 drops of lead acetate solution
Reddish brown vapours of Chromyl Chloride are evolved Yellow solution. Yellow precipitate
Chloride is confirmed.
Experiment No -14
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CHEMISTRY PRACTICAL 1
LAB MANUAL
DETECTION OF BASIC RADICALS(CATIONS)
TEST FOR AMMONIUM (NH 4+ ) RADICAL: (ZERO GROUP ANALYSIS)
Action of NaOH: A pinch of the salt is heated with 5 drops of sodium hydroxide
No pungent smell of ammonia
NH4
+ is absent.
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: 1cm3 of OS + 1cm 3 of dil.HCl in a test tube
No precipitate I group cations are absent
Group II: 1cm3 of OS + 1cm 3 of dil.HCl+H 2S solution is added
No precipitate II group cations are absent
Group III: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess
No precipitate III group cations are absent
Group IV: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess+H 2S solution is added
No precipitate IV group cations are absent
Group V: 1cm3 of OS +2Cm 3 of NH4Cl solution +NH 4OH solution in excess +(NH )4 2CO3 Solution
A white precipitate
V group cations is present Ba2+ ,Sr2+ ,or ca2+ may be present
Confirmatory test for V group cations:
a)Potassium chromate test: 1Cm3 of original solution+potassium chromate solution
No yellow precipitate
Ba2+ is absent
b)Ammonium sulphate test: 1Cm3 of original solution+ammonium sulphate solution,warm.
White precipitate
Sr2+ is confirmed
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Flame test: A pinch of salt +few drops conc.HCl and made into a paste. The paste is held to the flame with the help of a platinum wire.
Crimson red colour is imparted to the flame
Sr2+ is confirmed
Report: The given inorganic salt contains,
Anion is Chloride(Cl -). It belongs to groupII
Cation is Strontium (Sr2+ ).It belongs to groupV
Hence the given salt is Strontium Chloride(SrCl 2)
35
CHEMISTRY PRACTICAL 1
LAB MANUAL
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.
SAFETY PROCEDURE IN LAB
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