Inorganic Finalll
Inorganic Finalll
Inorganic Finalll
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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Signature Of Instructur
Table of Contents.
• Introduction ----------------------------------------- 21
• Chemicals/Apparatus ----------------------------------------- 21
• Solution preparation ----------------------------------------- 21
• Procedure ----------------------------------------- 22
• Calculations/results ----------------------------------------- 22
• Introduction ----------------------------------------- 23
• Chemicals/Apparatus ----------------------------------------- 23
• Procedure ----------------------------------------- 23
• Calculations and observations ----------------------------------------- 24
• Results/Conclusion ---------------------------------------- 24
• Introduction ----------------------------------------- 25
• Chemicals/Apparatus ----------------------------------------- 25
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• Procedure ----------------------------------------- 25
• Results/Conclusion ----------------------------------------- 26
• Introduction ----------------------------------------- 28
• Chemicals/Apparatus -------------------------------------- 28
• Procedure -------------------------------------- - 28
• Results/Conclusion ------------------------------------- 29
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• 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.
Page |6
• 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 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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Unattended Operations
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.
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• Test tubes.
• Rod.
• Measuring cylinder.
• Beaker.
• Spatula.
• Pipette.
• Bunsen burner
Examination:
• Dry test.
• Wet test.
• Confirmatory test.
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Experiment no. 01
i. Dry test:
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:
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
“For Phosphate’’
To the O.S. add a few drops of Yellow ppts of ammonium PO43- is indicated.
conc. HNO3 boil and add phosphomolybdate.
ammonium molybdate.
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
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.
v. Wet test:
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“For Nitrates”
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i. Dry test:
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
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
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
“For Nitrates”
i. Dry test:
P a g e | 17
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
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
‘‘For Borate’’
i. Dry test:
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
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:
v. Wet test:
P a g e | 20
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
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.
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• 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.
• 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+
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+ :
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.
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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.
Experiment No. 04
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:
Apparatus:
• UV-Vis spectrophotometer
• Quartz cuvettes
• Pipettes and pipette tips
• Volumetric flask
• Graduated cylinder
Procedure:
• 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.
Results:
Conclusion:
P a g e | 28
Experiment No. 04
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.