Inorganic Finalll

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Lab Manual.

GROUP - 01

• Course Code:
CHEM - 308

• Course Title:
Inorganic Chemistry – llI (PRACTICAL)
• Section:
BS CHEMISTRY-6th (B)
• Course Instructor:
Ma’am Hajra Zafar.

ACKNOWLEDGEMENT
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First of all we would like to thank Ma’am Hajra Zafar for


instructing us during the completion of this course and
performance of experiments. Secondly, we would like to
acknowledge that we have performed all these practicals in lab
and this lab manual is completed by :

• Zarlish Waheed 20011507-001


• Habiba Ashfaq 20011507-057
• Sana Asif 20011507-063
• Anusha Farooqi 20011507-067
• Asad Hussain 20011507-113

Signature Of Instructur

Signature Of Head Of Department:


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Table of Contents.

1. Estimation of anions in a given binary salts mixture

• Estimation of sulfate-phosphate: ----------------------------------------- 10


• Estimation of iodide-nitrate: ----------------------------------------- 12
• Estimation of bromide-nitrate: ----------------------------------------- 15
• Estimation of borate-acetate: ----------------------------------------- 18

2. Gravimetric estimation of Zn2+ ion (g/dm3) in a given sample

• Introduction ----------------------------------------- 21
• Chemicals/Apparatus ----------------------------------------- 21
• Solution preparation ----------------------------------------- 21
• Procedure ----------------------------------------- 22
• Calculations/results ----------------------------------------- 22

3. Determination of chloride ions by argentometric titrations

• Introduction ----------------------------------------- 23
• Chemicals/Apparatus ----------------------------------------- 23
• Procedure ----------------------------------------- 23
• Calculations and observations ----------------------------------------- 24
• Results/Conclusion ---------------------------------------- 24

4. Spectrophotometric determination of cerium

• Introduction ----------------------------------------- 25
• Chemicals/Apparatus ----------------------------------------- 25
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• Procedure ----------------------------------------- 25
• Results/Conclusion ----------------------------------------- 26

5. separation of heavy metals using the solvent extraction technique

• Introduction ----------------------------------------- 28
• Chemicals/Apparatus -------------------------------------- 28
• Procedure -------------------------------------- - 28
• Results/Conclusion ------------------------------------- 29
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Lab Safety Guidelines.

Plan Your Work

• Before conducting any experiment, you should


access the hazards related to the work, including;
what are the worst possible things that could go
wrong, how to deal with them, and what are the
prudent practices, protective facilities and
equipment necessary to minimize the risk of
exposure to the hazards.
• Always know the hazards of the materials used
(e.g., corrosivity, flammability, reactivity, and toxicity). Use the Project Hazard Review
Checklist (in Adobe PDF format) to help you with this assessment.
• Read the Material Safety Data Sheets (MSDS) for information on all chemicals you
plan to use. Make sure all Personal Protective Equipment (PPE) is on hand. Use the
MSDS or Personal Protective Equipment Selection Guide (in Adobe PDF format) to
select the needed equipment.
• Post a sign on the door to notify others of the lab hazards and list emergency contact
numbers.
• Inspect equipment and apparatus for weaknesses, cracks or damage before beginning
work.
• Inspect electrical equipment and cords for frayed wiring or damage before use. Discard
or repair damaged equipment before use.

Follow All Safety procedures

• Always wear chemical splash goggles for eye protection when working with chemicals.
• When pouring large quantities of hazardous chemicals, in addition to goggles, wear a
face shield large enough to protect your ears and neck as well as your face.
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• Always wear gloves when handling chemicals. Select the glove material based on
compatibility with the chemicals you may contact.
• Always wear appropriate clothing: chemically resistant lab coats or aprons are
recommended.
• Do not wear shorts or miniskirts (anything that would leave your legs bare and
unprotected). Do not wear high-heeled shoes, open-toed/heeled shoes, sandals or shoes
made of woven materials. Confine long hair and loose clothing.
• Do not work with hazardous chemicals or processes when alone in the laboratory. An
instructor must supervise undergraduate students at all times.
• Always use chemicals with adequate ventilation or in a chemical fume hood. Do not
allow the release of toxic substances in cold rooms or warm rooms, since these areas
have contained, re-circulated air.
• Use chemicals only as directed and for their intended purpose.
• Never use mouth suction to fill a pipette or siphon. Use a pipette bulb or other suitable
device.
• Handle needles, syringes and other sharps carefully. Use self-sheathing needles or
needless systems whenever possible. Dispose of all sharps in an appropriate sharps
container.
• Do not dispose of chemicals down the drain. Most chemicals must be disposed of as
hazardous waste.
• Compressed gas cylinders must be secured to prevent them from being knocked over.
Cylinders must be capped when the regulator is removed or not in use.
• Inspect the lab weekly for hazardous conditions.
• Shield or wrap pressurized or evacuated equipment (dewars & vacuum flasks).

Know Emergency Procedures

• Know where the nearest emergency eyewash and showers are, and how to use them.
• Know at least two exits from the laboratory area in case of an emergency.
• In the event of an emergency, pull the nearest "Pull BOX", evacuate the area, and close
all doors.
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Practice Good Housekeeping and Personal Hygiene

• Avoid direct contact with any chemical.


• Never smell, inhale or taste laboratory chemicals.
• Always wash hands and arms with soap and water after removing gloves and before
leaving the work area.
• Never eat, drink, chew gum or tobacco, smoke or apply cosmetics in the laboratory.
• Do not pick up broken glass with your hands. Use tongs or other mechanical means.
• Remove Personal Protective Equipment (PPE) such as gloves and lab coats before
leaving the lab.
• Remove gloves before handling common items like phones, instruments, door knobs,
etc.
• Keep all work areas clean and uncluttered. Wipe down benches with cleaners or
disinfectants regularly.
• Do not block emergency showers, eye washes, exits or hallways.

Transport Chemicals Safely

• Use secondary containers such as acid buckets or plastic totes.


• Secure containers on carts.
• Wear appropriate PPE.
• Use freight elevators or limit access in passenger elevators.
• Use a hand truck with a safety chain when moving compressed gas cylinders.

Unattended Operations

• Provide for containment of materials in the event of spills or failures.


• Label all containers and process equipment.
• Post emergency numbers on the lab door.
• Keep lab lights on.

Report Dangerous Activities or Situations


Page |8

• Report all accidents, no matter how minor.


• Never perform unauthorized work, preparations or experiments.
• Never engage in horseplay, pranks or other acts of mischief in laboratories.
• Never remove chemicals from the facility without proper authorization.

• Report suspicious people or activities in lab areas to University Police.

“Salt analysis of anions”

Theory:

Inorganic salts can be obtained with a base through complete or partial neutralization of acid.
The part that the acid contributes is called anion in the formation of a salt and the part that the
base contributes is called cation.

Anion is basically having more electrons than a cation or a proton thus providing it with a
negative charge. For forming an anion the atom needs to gain one or more electrons. The
number of electrons that will be gained tells about the charge on the anion. Suppose if an anion
is formed by gaining one electron it will have one negative charge, if it is forked by gaining
two electrons then 2 negative charges and so on. These electrons are basically pulled away
from other atoms that have less affinity for them. For finding out about the anion in a particular
sample anion analysis is done.
Analysis of anions may indicate what kind of anions is present in a sample and also the amount
of anions that are present in the given sample provided to you. To identify and quantify the
anion composition in the sample traditional chemistry uses methods known as colorimetric
methods. In modern chemistry, there is a method known as anion exchange chromatography
or ion chromatography. In this method, you can not only separate the ions present in the given
samples but also quantify the individual anion that is present in the given sample. It takes nearly
10 to 30 minutes in order to find multiple anions in a single run.
Page |9

Categories of acid radicals


• Dilute acid group radicals
It includes CO32-, HCO3-, SO3-, S2O32-
• Conc. Acid group radicals
It includes Cl-, Br-, I-, CH3COO-, NO3-, C2O42- .
• Special group radicals
It includes sulfate, phosphate and borate
Glassware required:

• Test tubes.
• Rod.
• Measuring cylinder.
• Beaker.
• Spatula.
• Pipette.
• Bunsen burner

Examination:

• Dry test.
• Wet test.
• Confirmatory test.
P a g e | 10

Experiment no. 01

Estimate anions in the mixture: Sulfate-phosphate, iodide-nitrate, bromide-


nitrate, and borate-acetate.

1. Salt analysis for sulfate-phosphate


“For sulfates’’

i. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added No gas evolved Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a Br-, CH3COO-) is absent.
test tube, and heated it.

BaCl2 test: To the O.S of salt add Ppts formed, which were SO42- is indicated.
barium chloride in equal dissolved when conc. HCl was
proportion. added

i. Confirmatory test:

Experiment Observation Inference


1. To the O.S add lead acetate White ppts. of PbSO4 soluble SO42- is confirmed.
solution. in ammonium acetate.
e.g, Na2SO4 + (CH3COO)2Pb PbSO4 + 2CH3COONa
PbSO4 + 2CH3COONH4 (CH3COO)2Pb + (NH4)2SO4
P a g e | 11

2. To the O.S add SrCl2 solution. White ppts. Of SrSO4 soluble SO42- is confirmed.
in all acids.
e.g, Na2SO4 + SrCl2
SrSO4 + 2NaCl

Possible basic radicals:


A. Al3+, Zn2+, Na+, K+, Mg+, NH4+
B. Cu2+, Fe3+, Ni2+, Mn2+, Cr3+
Respective salts: ZnSO4, Mn2SO4, (NH4)2SO4, SrSO4 etc.

“For Phosphate’’

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added No gas evolved Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a Br-, CH3COO-) is absent.
test tube, and heated it.

To the O.S. add a few drops of Yellow ppts of ammonium PO43- is indicated.
conc. HNO3 boil and add phosphomolybdate.
ammonium molybdate.

iii. Confirmatory test:


P a g e | 12

Experiment Observation Inference


1. To the O.S add AgNO3 Yellow ppt soluble in dil. PO43- is confirmed.
solution. HNO3.
e.g, Na3PO4 + 3AgNO3 Ag3PO4 + 3NaNO3

2. To the O.S add BaCl2 solution. White ppt. soluble in conc PO43- is confirmed.
HCl but do not give SO2.
e.g, 2 Na3PO4 + 3BaCl2
Ba3(PO4) +6NaCl

3.To the O.S add FeCl3 solution. Yellow ppt. of FePO4 PO43- is confirmed.
e.g, (NH4)3PO4 + FeCl3 FePO4 + 3NH4Cl

Possible base radicals: Na+, NH4+, Mg2+


Respective salts: Na3PO4, (NH4)3PO4

Conclusion: From the above confirmatory tests of given binary mixture it was confirmed that
acid radicals like, sulfate and phosphate are present in given binary mixture of salts.

2. Salt analysis for iodide-nitrate


“For Iodide’’
iv. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

v. Wet test:
P a g e | 13

Experiment Observation Inference


Made a solution of salt, added Violet fumes evolved and Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a condensed near the mouth of Br-, CH3COO-) is present.
test tube and heated it. test tube. Maybe I2 gas.

Starch test: made a solution of The starch solution turns I- is identified.


salt and added an equimolar blue.
starch solution in it.
2KI + H2SO4 → K2SO4 + 2HI
2HI + H2SO4 → H2S +K2SO4+
2H2O + I2

vi. Confirmatory test:

Experiment Observation Inference


Silver nitrate test: Made a salt Precipitates insoluble in I- Is confirmed.
solution and added it to the dilute nitric acid as well as
equimolar solution of silver ammonium hydroxide.
nitrate.
KI + AgNO3 → KNO3 + AgI

Layers test: made a salt CS2 layer turns violet. I- Is confirmed.


solution, added carbon
disulfide reagent in the
required quantity, a few
crystals of KMnO4, dilute
sulfuric acid, and shook it.
2KMnO4 + 10KI + 8H2SO4 →
2MnSO4 + 5I2 + 8H2O + K2SO4

Possible basic radicals: Na+ K+ Al3+


Respective salts: NaI, KI, AlI3.

“For Nitrates”
P a g e | 14

i. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added White fumes having a Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a pungent smell evolved. Br-, NO3-, CH3COO-) is
test tube, and heated it. present. May be HNO3
gas.
2NaNO3 + H2SO4 → Na2SO4 +
2HNO3

Added paper pallets to the Reddish brown fumes of NO2 NO3- is identified.
above contents and heated. appear at the mouth of the
test tube.
4HNO3 + C → CO2 + 2H2O + 4NO2

iii. Confirmatory test:

Experiment Observation Inference


Ring test: To the salt solution A deep blue color ring NO3- is confirmed.
added a few drops of biphenyl formed.
amine and conc. H2SO 4.
2NaNO3 + H2SO4 → Na2SO4 +
2HNO3
2HNO3 + 6FeSO4 + 3H2SO4 →
3Fe2(SO4)3 + 4H2O + 2NO
FeSO4 + NO → [𝐹𝑒(𝑁𝑂)𝑆𝑂4]
P a g e | 15

To the salt solution added Pungent smell of ammonia NO3- is confirmed.


aluminum foil, NaOH solution evolved.
and heated.
NaNO3 + 3Al + 3NaOH →
3NaAlO2 + NH3

Possible basic radicals: (a) Pb2+, Ag+, Bi3+, Cd2+, Al3+, Ba2+, Sr2+, Na+, K+, NH4+
Colored: (b) Cu2+, Co2+
Respective salts: Pb((NO3)2, AgNO3, Bi(NO3)3, Cd(NO3)2, Al(NO3)3, Ba(NO3)2, Sr(NO3)2,
Ca(NO3)2, NaNO3, KNO3, NH4NO3

Colored: (b) Cu (NO3)2, Co (NO3)2,


Conclusion: From the above confirmatory tests of the given binary mixture it was confirmed
that acid radicals like, iodide and nitrate are present in given binary mixture of salts.

3. Salt analysis for bromide-nitrate


“For Bromide”
i. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added White fumes of HBr along Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a with reddish brown vapors Br-, CH3COO-) is present.
test tube, and heated it. having a pungent smell are May be Br2 gas.
evolved.
P a g e | 16

Treated the fumes with ferric No effect on ferrous Br- is indicated.


sulfates by using a rod dipped in sulphates solution
ferrous sulphates.

2KBr + H2SO4 → K2SO4 + 2HBr

HBr + H2SO4 → H2O + Br2 + SO2

iii. Confirmatory test:

Experiment Observation Inference


Silver nitrate test: Made a salt Light yellow precipitates Br- is confirmed.
solution and added it to soluble in dilute nitric acid
equimolar solution of silver but partially soluble in
nitrate. ammonium hydroxide.
KBr+AgNO3 → AgBr+ KNO3

Took these yellow precipitates In the first test tube Br- is confirmed.
in two test tubes. Treated one precipitates are partially
with ammonium hydroxide and soluble while in the second
other with dilute nitric acid. test tube solution will turn
completely transparent.

Layers test: made a salt Layers will form where CS2 Br- is confirmed.
solution, added carbon layer will be of orange colour.
disulphide reagent in required
quantity, few crystal of KMnO4,
dilute sulphuric acid and shook
it.
3KMnO4 + 4KBr + 2H2SO4 →
3K2SO4 + 2MnBr2 + 2H2O + 5Br2

Possible basic radicals: Na+, K+, NH4+


Respective salts: NaBr, KBr, NH4Br.

“For Nitrates”
i. Dry test:
P a g e | 17

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added White fumes having pungent Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a smell evolved. Br-, NO3-, CH3COO-) is
test tube and heated it. present. May be HNO3
gas.
2NaNO3 + H2SO4 → Na2SO4 +
2HNO3

Added paper pallets to above Reddish brown fumes of NO2 NO3- is identified.
contents and heated. appear at the mouth of test
tube.
4HNO3 + C → CO2 + 2H2O + 4NO2

iii. Confirmatory test:

Experiment Observation Inference


Ring test: To the salt solution Deep blue colour ring NO3- is confirmed.
added few drops of biphenyl formed.
amine and conc. H2SO4.
2NaNO3 + H2SO4 → Na2SO4 +
2HNO3
2HNO3 + 6FeSO4 + 3H2SO4 →
3Fe2(SO4)3 + 4H2O + 2NO
FeSO4 + NO → [Fe(NO)SO4]

To the salt solution added A pungent smell of ammonia NO3- is confirmed.


aluminum foil, NaOH solution evolved.
and heated.
P a g e | 18

NaNO3 + 3Al + 3NaOH →


3NaAlO2 + NH3

Possible basic radicals: (a) Pb2+, Ag+, Bi3+, Cd2+, Al3+, Ba2+, Sr2+, Na+, K+, NH4+
Coloured: (b) Cu2+, Co2+
Respective salts: Pb((NO3)2, AgNO3, Bi(NO3)3, Cd(NO3)2, Al(NO3)3, Ba(NO3)2, Sr(NO3)2,
Ca(NO3)2, NaNO3, KNO3, NH4NO3

Coloured: (b) Cu (NO3)2, Co (NO3)2


Conclusion: From the above confirmatory tests of given binary mixture it was confirmed
that acid radicals like, bromide and nitrate are present in given binary mixture of salts.

4. Salt analysis for borate-acetate

‘‘For Borate’’
i. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-,SO3-,S2O32-) is
H2SO 4 and heat. absent.

ii. Wet test:

Experiment Observation Inference


Made a solution of salt, added No gas evolved. Conc. H2SO 4 group (Cl-,
concentrated H2SO4 to it in a Br-, CH3COO-) is absent.
test tube and heated it.
It would be from special
group.
P a g e | 19

BaCl2 test: To the O.S of salt add Ppts formed, which were Borate ions are present.
barium chloride in equal dissolved when HNO3 or NH3
proportion. was added

iii. Confirmatory test:

Experiment Observation Inference


1.AgNO3 test: To the O.S of salt White colored precipitates Silver metaborate is
add silver nitrate in equal formed. confirmed.
proportion.

2. Solubility test: Ppts get dissolved in both Borate ions are


acetic acid and dilute nitric conformed
(i) Added CH3COOH solution to
acid.
silver metaborate ppts.
(ii) Added dil. HNO3 to the ppts
of silver metaborate.

2. Turmeric paper test: Made Paper turned reddish brown. Borate ions are
a solution of turmeric and conformed.
dipped paper into it and dry
it in the air. This paper was
dipped in salt’s O.S then
dried at 100oC.

“For Acetate”
iv. Dry test:

Experiment Observation Inference


Added a pinch of salt and No gas evolved. Dilute acid group (CO32-,
treated this salt with dilute HCO3-, SO3-, S2O32-) is
H2SO4 and heat. absent.

v. Wet test:
P a g e | 20

Experiment Observation Inference


Made a solution of salt, added Colourless vapours with Conc. H2SO 4 group (Cl-,
concentrated H2SO 4 to it in a vinegar smell evolved. Br-, CH3COO-) is present.
test tube and heated it. May be CH3COO-.

Silver nitrate test: Made a salt No precipitates formed. CH3COO- is identified.


solution and added it to
equimolar solution of silver
nitrate.

Barium Chloride test: Made a No precipitates formed. CH3COO- is identified.


salt solution and added it to
equimolar solution of Barium
chloride.

vi. Confirmatory test:

Experiment Observation Inference


To the salt solution added Red colour produced. CH3COO- is confirmed.
neutral FeCl3 solution.
3CH3COONa + FeCl3 →
(CH3COOH)3 Fe+ 3NaCl

To the salt solution added Red precipitates formed. CH3COO- is confirmed.


neutral FeCl3 solution and
added water in it.
3CH3COONa + 3H2O →
Fe(OH)2(CH3COO)

To the salt solution added Fruity smell of ethyl acetate CH3COO- is confirmed.
ethanol, concentrated H2SO4, evolved.
heated and shift contents to ice
chilled cold water.
CH3COONa + C2H5OH →
CH3COOC2H5 + H2O

Possible basic radicals:(a) Pb+, Na+ ,K+ ,NH4+


P a g e | 21

Colored: (b) Cu2+, Co2+, Ni2+


Respective salts:( a) Pb (CH3COO)2, CH3COONa, CH3COOK, CH3COONH4,
Coloured: (b) Cu(CH3COO)2, Co(CH3COO)2, Ni(CH3COO)2,
Conclusion: From the above confirmatory tests of given binary mixture it was confirmed
that acid radicals like, borate and acetate are present in given binary mixture of salts.

Experiment No. 02
“Gravimetric Estimation of Zinc”

Introduction:
Gravimetric analysis is a method in analytical chemistry to determine the quantity of an analyte
based on the mass of a solid. The principle behind the gravimetric analysis is that the mass of
an ion in a pure compound and can be determined. Later, used to find the mass percent of the
same ion in a known quantity of an impure compound.

Chemicals Required:

• NaHCO3
• ZnSO4
• Anthranilic Acid (2-Amino Benzoic Acid)
• dil. HCl
• liq.NH3 or NH4 OH
• Distilled water

Apparatus Required:

• Beaker
• Funnel
• Burette
• Stirrer
• Filter paper
• Weighing balance
Solution Preparation:
1. Organic Reagent Preparation:
• 5% w/v NaHCO3 solution was made by adding 5g of NaHCO3 in 100ml distilled water.
• This solution was taken in burette.
P a g e | 22

• 3g of Anthranilic Acid was taken in a Beaker and it was titrated against 5% w/v
NaHCO3 solution.
• 5% w/v NaHCO3 solution was added dropwise in the beaker.
• Effervescence occurred and CO2 was liberated.
• pH of the solution was maintained to neutral.
• 5% w/v NaHCO3 solution was continuously adding until no further effervescence
occurred.
• There, Anthranilic Acid had been converted to its ionized form i.e., sodium anthranilate.
Na[C7 H6 O2 N].
• Organic reagent had been prepared.

2. Sample solution Preparation:

• To prepare 0.1M ZnSO4 in 1000ml, 28,8g of ZnSO4 was taken in 1000ml volumetric
flask and small quantity of distilled water was added.
• Shake the mixture and more water was added to make the volume up to 1000ml.
• Sample solution had been prepared.
Chemical Equation:

+ Zn2+

Anthranilic acid Zinc-anthranilate complex

Procedure:
• Sodium Anthranilate level was risen up to 100ml and it was added in burette
• 20ml of ZnSO4 solution out of 1000ml was taken in the beaker and titration was
performed.
• Sodium Anthranilate was added drop by drop in ZnSO4 solution.
• Precipitation occurred and it started to settle in bottom of the beaker.
• With time, Superlative layer was formed in the bottom of beaker which was a thick
distinct layer of precipitates.
• At this point, titration was stopped.
• Superlative layer formation indicated complex formation which is stable at neutral
pH.
• Here pH was checked.
if it is above 8, few drops of dil. HCl was added.
if it is below 6, few drops of liq.NH3 or NH4 OH were added.
• Filtered the layer formed with the help of filter paper.
• Dried the crystals and calculated the weight.
P a g e | 23

Observations:
Weight of filter paper = 1.4g
Weight of complex + filter paper = 2.0g
Weight of complex = 0.6g
Calculations:
Theoretical Yield:
2[C6H4 (NH2 )(COOH)] + Zn Zn2+. 2[C6H4 (NH2 )(COO-)]
2(137.14g) + 65.40g = 337.32g
Amount of Zn2+ :

337.32g of Zinc Anthranilate contains Zn2+ = 65.40g


1g of Zinc Anthranilate contains Zn2+ = 65.40/337.32
= 0.19g
2+
0.6g of Zinc Anthranilate contains Zn = 0.19 x 0.6
= 0.114g
In Solution:
20ml of Zinc Anthranilate contains Zn2+ = 0.114g
1ml Zinc Anthranilate contains Zn2+ = 0.114 / 20 = 0.0057ml
2+
1000ml Zinc Anthranilate contains Zn = 0.0057 x 1000 = 5.7ml

Result:
The amount of zinc in zinc anthranilate complex is found to be 0.114g, whereas in
1000ml of zinc anthranilate solution its amount is 5.7ml.
P a g e | 24

Experiment No. 03
“Argentometric Titration”
Introduction:
Argentometry is a type of titration involving the silver(I) ion. Typically, it is used to determine
the amount of chloride present in a sample. The sample solution is titrated against a solution of
silver nitrate of known concentration.
It is a type of precipitation titration which involves the use of silver ion which is taken from its
Latin name argentum. So, the word argentometric is also taken from Latin word argentum. The
titrations with silver nitrate are known as argentometric titration.
Chemicals:
• Silver Nitrate
• Sodium Chloride
• Fluorescence
• Water
Apparatus:
• Beaker
• Burette
• Pipette
• Burette Stand
Procedure:

1) Take Silver Nitrate solution in Burette and sodium chloride solution in beaker.
2) Add a drop of fluorescence indicator in sodium chloride solution.
3) Fluorescence is in salt form hence make a solution by adding 1g of it in 1000 ml of water.
4) Two layers will be formed. Primary layer will be of Sodium and Secondary layer will be of
Chloride.
5) As titration starts, Primary layer will be replaced by Silver and Secondary will be replaced
by Nitrate.
6) End point is achieved when color changed. Pink color will be achieved.
7) This experiment is repeated 3 times to get concordant readings.

Calculations and Observations:


P a g e | 25

Sr. No. Initial Volume Final Volume (cm) Volume Used


(cm) (cm)
1 10 20 10
2 20 30.5 10.5
3 30.5 40 9.5

Titrant Molarity = 0.1M


M1 V1 = M2 V2
M1 × 15 = 0.1 × 10
M1 = 0.1 × 10
M1 = 0.06M

Strength of NaCl = 0.06 × 53.44 g/mol


= 3.5064 g/mol
Strength of Cl- = 0.06 × 35.5
= 2.13 g/dm3
Result:
The strength of chloride ion in given solution, determined by argentometric titration is found
to be 2.13g/dm3
P a g e | 26

Experiment No. 04

“Spectrophotometric Determination of Cerium”

Introduction:
UV-Vis spectrophotometry is a powerful analytical technique used to study the interaction
between light and matter. This method is particularly valuable for determining the
concentration of certain compounds, including cerium, which exhibit distinct absorption
properties in the UV and visible regions. By employing a spectrophotometer, we can measure
the absorbance of cerium-containing solutions, allowing us to establish a calibration curve and
ultimately quantify the concentration of an unknown cerium solution.

Chemicals:

• Cerium salt solution (unknown concentration)


• Distilled water

Apparatus:

• UV-Vis spectrophotometer
• Quartz cuvettes
• Pipettes and pipette tips
• Volumetric flask
• Graduated cylinder

Procedure:

1) Blank Solution Preparation:

• Add distilled water to a quartz cuvette.


• Insert the cuvette into the spectrophotometer and set the wavelength to the UV or visible
range.
• Record the baseline absorbance if it is showing straight line, it means apparatus is
working properly.
P a g e | 27

Figure 5.1 Calibration curve in distilled water

2) Analysis of Unknown Solution:

• Transfer a small volume of the unknown cerium solution into a quartz cuvette.
• Measure the absorbance of the unknown solution at the same wavelength as before.
• It is measured to be λmax= 303nm.

Figure 5.2; Absorption spectrum of cerium oxide

Results:

Cerium oxide has UV absorption at 380nm.

Conclusion:
P a g e | 28

UV-Vis spectrophotometry proved to be an effective method for determining the concentration


of cerium in a solution. The established calibration curve facilitated the accurate quantification
of the unknown cerium solution's concentration, which was validated by comparing it with
literature values. This experiment highlights the importance of spectrophotometric techniques
in quantitative analysis and demonstrates their application in various fields requiring precise
concentration measurements.

Experiment No. 04

“Separation of heavy metals using the solvent extraction technique”


Theory:
For the extraction of metal solvent is necessary but metal cannot be separated in aqueous
solution so we have to make the metal organic in nature. For that purpose we either do chelation
in which metal reacts with chelates in aqueous medium and resulting chelating agent will be
organic in nature and metal is inorganic in nature so it will dissolve in water so through
chelation using chelating agent we will make it organic in nature. Secondly, we will take a high
molecular weight organic molecule and make ion pair of counter ion of metal and organic part
in this way our solution containing aqueous medium, water and metal has organic metal.
Now we will use a solvent that will separate metal that is organic in nature. The solvent used
should have more miscibility in organic part. We will perform extraction and add chelating
agent to metal solution further add solvent, shake, let it sit and organic part will be on top as a
result. Discard the aqueous layer and all we are left with is organic layer. Evaporate the solvent
and metal has been extracted.

Chemical reagents:
• NaOH solution as solvent.
• ZnSO4 solution.
• Triphenylamine.

Apparatus:
• Beaker.
• Stirrer.
• Separatory funnel.
• Funnel.
P a g e | 29

• Filter paper.
• Bunsen burner.

Procedure:
1. Take a known volume of the prepared zinc sulphate solution in a beaker.
2. Add a known volume of the prepared EDTA solution to the beaker containing the zinc
sulphate solution.
3. Slowly add NaOH solution drop by drop to the mixture while stirring continuously with a
glass rod.
4. Observe the formation of a precipitate of zinc hydroxide.
5. Continue adding NaOH until no more precipitate forms and the solution appears clear.
6. Allow the precipitate to settle down, then carefully decant the supernatant liquid.
7. Transfer the precipitate to a filter paper in a funnel, and wash it with distilled water to remove
any impurities.
8. Let the filtered precipitate dry in open air.
Result:
The desired metal has been extracted from aqueous layer.

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