2014
[CHEMISTRY LAB
MANUAL]
JAYPEE UNIVERSITY OF INFORMATION TECHNOLOGY, WAKNAGHAT
Chemistry Lab Manual 2014
In all titrations, you need to take two concordant
readings. Do not take the mean of three readings.
If the solution is same and instrument is same if there is any difference in readings then it is due
to personal error.just to check this three concordant readings are recommended. You can’t have
different concentrations and strength of the same solution so, readings cannot be averaged.
EXPERIMENTS
Contents
Experiment No: 1 To Prepare 0.1 M (Approximately) Hydrochloric Acid And Standardize It. .. 3
Experiment No: 2 To Prepare N/10 Standard Solution Of NaOH .................................................. 5
Experiment No: 3 To Determine Strength Of Given Oxalic Acid Solution ................................... 7
Experiment No: 4 To Determine The Viscosities Of Given Organic Liquids With The Help Of
Viscometer. ..................................................................................................................................... 9
Experiment No: 5 To Determine The Ph Values Of Different Water Samples. ........................... 11
Experiment No: 6 To Determine The Alkalinity Of A Given Water Sample. ............................ 13
Experiment No: 7 To Determine The Acidity Of Given Water Sample. ..................................... 15
Experiment : 8 To Determine The Surface Tension Of Given Organic Liquids With The Help Of
Stalagmometer. ............................................................................................................................. 17
Experiment No: 9 To Determine The Amount Of Carbon Dioxide In A Given Water Sample ... 19
Experiment No: 10 To Determine The Chloride Content Of Given Water Sample ..................... 21
Experiment No: 11 To Determine Total Hardness Of Given Water Sample By EDTA Method. 23
Note: Repeat Exp 3 with different concentrations and Exp 4 with solutions.
Examination:
1. Day To Day Work 50 Marks
2. Mid Term 20 Marks
3. End Term 25 Marks
4. Attendance 5 marks (zero marks for attendance below 80%)
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Experiment No: 1
To Prepare 0.1 M (Approximately) Hydrochloric Acid And
Standardize It.
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Experiment No: 2
To Prepare N/10 Standard Solution Of NaOH
AIM: To prepare N/10 standard solution of NaOH.
REAGENTS: 1.Oxalic acid
2. NaOH
3. Phenolphthalein
APPARATUS REQUIRED: 1.Burette
2. Pipette
3. Volumetric flask
4. Conical flask
5. Funnel
THEORY:
Titration is a common laboratory method of quantitative chemical analysis that is used to
determine the unknown concentration of a known reactant. Because volume measurements play
a key role in titration, it is also known as volumetric analysis. A reagent, called the titrant or
titrator, of known concentration (a standard solution) and volume is used to react with a solution
of the analyte or titrand, whose concentration is not known
PROCEDURE:
1. Dissolve the weigh (grams) NaOH in minimum quantity of distilled water in a volumetric
flask. Make it up to 250 ml.
2. Prepare standard N/10 Oxalic acid solutions in a 250 ml volumetric flask.
3. Fill the Burette with NaOH solution.
4. Pipette out 10 ml of Oxalic acid solution in a conical flask.
5. Add 2 drops of phenolphthalein indicator.
6. Titrate the known Oxalic acid solution against the unknown (conc.) NaOH solution till pink
color appear.
7. Repeat steps 4 to 6 till concordant reading achieved.
8. Dilute NaOH solution up to concentration N/10.
OBSERVATIONS:
S.No. Vol. of Oxalic acid (in mL) Burette Reading Vol of NaOH Used
Initial Final Difference (in mL)
A B C D=C-B
1.
2.
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CALCULATIONS:
Normality of NaOH: N1V1= N2V2
RESULT: The normality of NaOH is …………………………………….
PRECAUTIONS:
1. Weigh the NaOH properly.
2. Use the instruments properly.
3. Before using the apparatus they should be properly washed with distilled water.
QUESTIONS BASED ON ABOVE EXPERIMENT:
1. What is normality?
2. What do you mean by standardization?
3. Waht is standard solution?
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Experiment No: 3
To Determine Strength Of Given Oxalic Acid Solution
AIM: To Determine strength of given oxalic acid solution
REAGENTS: 1.Oxalic acid
2. NaOH
3. Phenolphthalein
APPARATUS REQUIRED: 1.Burette
2. Pipette
3. Volumetric flask
4. Conical flask
5. Funnel
THEORY:
Titration is a common laboratory method of quantitative chemical analysis that is used to
determine the unknown concentration of a known reactant. Because volume measurements play
a key role in titration, it is also known as volumetric analysis. A reagent, called the titrant or
titrator, of known concentration (a standard solution) and volume is used to react with a solution
of the analyte or titrand, whose concentration is not known
PROCEDURE:
1. Dissolve the weigh (grams) NaOH in minimum quantity of distilled water in a volumetric
flask. Make it up to 250 ml.
2. Prepare standard N/10 Oxalic acid solutions in a 250 ml volumetric flask.
3. Fill the Burette with NaOH solution.
4. Pipette out 10 ml of Oxalic acid solution in a conical flask.
5. Add 2 drops of phenolphthalein indicator.
6. Titrate the known Oxalic acid solution against the unknown (conc.) NaOH solution till pink
color appear.
7. Repeat steps 4 to 6 till concordant reading achieved.
8. Dilute NaOH solution up to concentration N/10.
OBSERVATIONS:
A. Standardization of NaOH Solution
S.No. Vol.of Oxalic acid (in mL) Burate Reading Vol of NaOH Used
Initial Final Difference (in mL)
V1 A B C=B-A V2
1.
2.
3
Normality of Oxalic Acid N1=
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Volume of Oxalic Acid V1=
Volume of of NaOH Solution V2 =
The Strength of NaOH Solution N2 = N1V1/ V2
B. Strength of unknown Oxlalic acid Solution
S.No. Vol.of Oxalic acid (in mL) Burate Reading Vol of NaOH Used
Initial Final Difference (in mL)
V3 A B C=B-A V4
1.
2.
3
The Strength of NaOH Solution N2 = ---------
Volume of of NaOH Solution V4 =
Volume of Oxalic Acid V3=
Normality of Oxalic Acid N3 = N2V4/ V3
RESULT: The normality of givin oxalic acid solution is …………………………………….
PRECAUTIONS:
1. Weigh the NaOH properly.
2. Use the instruments properly.
3. Before using the apparatus they should be properly washed with distilled water.
QUESTIONS BASED ON ABOVE EXPERIMENT:
4. What is normality?
5. What do you mean by standardization?
6. Waht is standard solution?
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Experiment No: 4
To Determine The Viscosities Of Given Organic Liquids With The
Help Of Viscometer.
AIM: To determine the viscosities of given organic liquids with the help of viscometer.
REAGENTS:
1. Distilled water
2. Acetone
3. Ethyl Alcohol
4. Methyl alcohol
5. Carbon Tetrachloride
6. Benzene
APPARATUS REQUIRED: 1.Beakers
2. Pipette
3. Ostwald Viscometer
4. Stop watch
5. Specific gravity bottle
PROCEDURE:
With the help of pipette pour water into viscometer. Suck it from the end having
rubber tube and pull it until it reaches second mark. Now allow the water to flow from
upper mark to lower mark and note down the time taken by water to reach from one
mark to another.
Repeat the process to take at least three concordant readings. Then clean and
dry specific gravity bottle and weigh the empty bottle. Now fill it with water and weigh.
Now repeat the whole process to take reading for different organic liquids.
GENERAL CALCULATIONS:
Temperature of water = ToC
Density of water at this temperature = dw gm/lt
Time of flow of water = tw
Viscosity of water = w
(a) To calculate the density of liquid (ds)
Weight of empty bottle = W 1
Weight of empty bottle + water = W 2
Weight of empty bottle + solvent =W 3
Density of liquid (ds)= (Wt. of solvent/Wt. of water)X Density of water
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X dw gm/cm3
(b) To calculate the viscosity of liquid
Or X centipoise
OBSERVATION TABLE:
S. No. Organic Time of Density Viscosity Viscosity Error
Liquid flow (s) (ds) from
gm/l (cp) Literature
PRECAUTIONS:
1. Wash viscometer and specific gravity bottle thoroughly with water and then with
acetone respectively after each reading.
2. Viscometer should be placed vertical
3. Time should be noted properly
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Experiment No: 5
To Determine The Ph Values Of Different Water Samples.
AIM: To determine the pH values of different water samples.
REAGENTS: 1. pH 7.0 and pH 4.0 buffer solutions,
2. Distilled water,
3. pH meter
4. Different water samples
APPARATUS: pH meter
THEORY:
pH is a measure of the acidity or basicity of a solution. It is defined as the cologarithm of the
activity of dissolved hydrogen ions (H+). The pH scale is not an absolute scale; it is relative to a
set of standard solutions whose pH is established by international agreement. The concept of pH
was first introduced by Danish chemist Søren Peder Lauritz Sørensen at the Carlsberg
Laboratory in 1909. Pure water is said to be neutral. The pH for pure water at 25 °C is close to
7.0. Solutions with a pH less than 7 are said to be acidic and solutions with a pH greater than 7
are said to be basic or alkaline. pH measurements are important for medicine, biology, chemistry,
food science, environmental science, oceanography and many other applications.
PROCEDURE:
1. Prepare the buffer solutions (7.0 pH and 4.0 pH) by dissolving 1 tablet of each buffer in
distilled water and make up to 100 ml in two separate volumetric flasks.
2. Switch on the pH meter for 15 minutes.
3. After washing and wiping the pH electrode and the temperature probe dip it in a solution of
pH 7.0 buffers. Change knob from standby to pH.
4. With the CAL knob set the pH value to 7.0
5. With a pH 4.0 buffers, set the pH value to 4.0 using the slope knob.
6. Repeat steps 2-3 till the pH meter is standardized with respect to both pH 4.0 and 7.0
7. Take the pH values of the different water samples with the pH meter.
OBSERVATIONS:
S.No. Water sample pH value
(pH meter)
1
2
3
4
RESULT: The pH of HA+ & HB+ are ………………………………………….
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PRECAUTIONS:
1. Before starting the experiments apparatus should be rinsed with distilled water.
2. Prepare the buffer solutions carefully.
3. Take the readings carefully.
QUESTIONS BASED ON ABOVE EXPERIMENT:
1. How is the hydrogen ion concentration of any solution expressed? Explain.
2. How does a glass electrode measure pH
3. Which electrodes other than the glass electrode can be used to measure pH.?
4. What are buffers?
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Experiment No: 6
To Determine The Alkalinity Of A Given Water Sample.
AIM: To determine the alkalinity of a given water sample.
REQUIREMENTS: 1.Burette,
2. Pipette,
3. Conical flask (250 ml capacity),
4. Measuring flask
INDICATORS: 1. Methyl Orange indicator
2. Phenolphthalein indicator
3. N/50 H2SO4 solution
THEORY:
The alkalinity of natural waters is due to the presence of salts of weak acids. There are three
normal forms of alkalinity, hydroxide (OH-), carbonate (CO3-2), and bicarbonate (HCO3-).
Bicarbonate presents the major form since they are formed in considerable amounts from the
action of CO2 upon the basic materials in the soil.
CO2 + CaCO3 + H2O → Ca (HCO3)2
Natural waters may also contain appreciable amounts of carbonates and hydroxide alkalinities,
particularly surface waters are blooming with algal growth. The algae take up CO2 for its
photosynthetic activities and raise the pH.
The carbonate alkalinity may be present with either hydroxide or bicarbonate alkalinity, but
hydroxide and bicarbonate alkalinity can not be present in the same sample because they
combine together to form CO3-2 ions. The total alkalinity of water sample is determined by
titration with a strong acid to the end point of methyl orange indicator (pH 4.5) and expressed as
CaCO3 scale.
The knowledge of alkalinity of water is necessary for calculating the amounts of lime and soda
needed for water softening and also in neutralizing the acidic solution produced by hydrolysis of
salts. In boilers for steam generation, high alkalinity of water may not only lead to caustic
embitterment but also to the precipitation of sludge and deposition of scales.
PROCEDURE:
1. Take 100 ml of water sample into a conical flask.
2. Add 1-2 drops of phenolphthalein indicator.
3. Titrate this sample against N/50 H2SO4 until the pink color caused by phenolphthalein just
disappears.
4. Note down this reading as phenolphthalein end point A ml.
5. Now add 2 drops of methyl orange in the same solution. It will give light yellow color.
6. Continue the titration against N/50 H2SO4 until the yellow color changes to red.
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7. Note down the total volume of acid as B. This is methyl orange end point.
8. The experiment is repeated for at least one more sample till reproducible results are obtained.
OBSERVATION TABLE:
S.NO. Volume of sample Volume of N/50H2SO4 used Volume of N/50H2SO4 used
(ml) Phenolphthalein end point Methyl orange end point
1.
2.
CALCULATION:
Volume of sample taken for each titration = 100 ml
Volume of N/50H2SO4 used to phenolphthalein end-point = A ml
Additional Volume of N/50 H2SO4 acid used to methyl orange end-point = B ml
N1 V1 = N2 V2
Sample N/50H2SO4 N1×100 = A/50 = N1 = A/5000
Strength (asCaCO3) or phenolphthalein alkalinity = A×50/5000 gm/l
= 10A mg/l = 10A ppm
Similarly, Total alkalinity or methyl orange alkalinity = 10× (A+B) gm/l
= 10× (A+B) ppm
Hydroxide alkalinity = 10(A-B) mg/l
= 10 × (A-B) ppm
Carbonate Alkalinity = 2 B×50×1000/5000 = 10×2B ppm when A> B
= 2 A×50×1000/5000 = 10×2A ppm when A< B
Bicarbonate Alkalinity = (B-A) ×50 ×1000/5000 mg/l
= 10 × (B-A) ppm
RESULT: The carbonate alkalinity, hydroxide alkalinity, bicarbonate alkalinity is
…………………………………………………..
PRECAUTIONS:
1. The glass apparatus should be perfectly cleaned before the start of the experiment.
2. Since phenolphthalein and methyl orange indicators are used in determination of alkalinity
the end point of the titration should be observed carefully.
QUESTION BASED ON EXPERIMENT:
1. What is the significance of determining alkalinity in water?
2. Explain the action of phenolphthalein’s an acid base indicator?
3. In what form does methyl orange exit in acid & alkaline medium?
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Experiment No: 7
To Determine The Acidity Of Given Water Sample.
AIM: To determine the acidity of given water sample.
APPARATUS REQUIRED: 1.Pippete
2. Dropper
3. Titration Flask (250 ml capacity)
4. Burette
REAGENTS: 1. Methyl Orange
2. Phenolpthalein
3. N/50 Sodium Hydroxide
4. N/10 Sodium Thiosulphate
THEORY:
The acidity in natural waters is primarily due to dissolved carbon dioxide. However in waters
polluted by industrial wastes may be because of mineral acids (below pH 4.5)
PROCEDURE:
1. Place 100 ml of given water sample.
2. Add to it one drop of Methyl Orange Indictor.
3. If it gives an orangish red color it means mineral acidity is available.
4. Titrate with N/50 Sodium Hydroxide Solution till Yellow end point.
5. Note the ml of N/ 50 NaOH solution used.
6. In another flask place 100 ml water and add 0.5 ml Phenolphthalein indicator.
7. If it does not give any color titrate with N/50 NaOH to a Pink end point.
8. Note the ml of solution used.
9. If phenolphthalein gives a pink color on addition in the sample, acidity is not available.
OBSERVATION:
S.No. Volume of Volume of N/50 NaOH used Volume of N/50H2SO4 used
sample (ml) Methyl orange end point (A) Phenolphthalein end point (B)
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CALCULATION:
Mineral Acidity (mg/l) as CaCO3 = (ml of NaOH solution used with methyl Orange x 1000) / ml
sample
Carbon Dioxide acidity (mg/l) = (ml of NaOH solution used with phenolphthalein x 1000) / ml
sample
RESULT: The acidity of given sample is………….
PRECAUTIONS:
1. The glass apparatus should be perfectly cleaned before the start of the experiment.
2. Since phenolphthalein and methyl orange indicators are used in determination of acidity
the end point of the titration should be observed carefully.
QUESTIONS BASED ON ABOVE EXPERIMENT:
1. What is the significance of determining acidity in water?
2. What causes acidity in natural waters?
3. What pH range is used to measure mineral acidity in water?
4. How are methyl orange and phenolphthalein acidity related to mineral and total acidity?
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Experiment : 8
To Determine The Surface Tension Of Given Organic Liquids With
The Help Of Stalagmometer.
AIM:To determine the Surface tension of given organic liquids with the help of
Stalagmometer.
Requirements:
Stalagmometer, specific gravity bottle, a small rubber tubing with screw pinch-
cock, pipette, acetone, organic liquids.
Procedure:
Thoroughly clean the stalagmometer. To the top of the stalagmometer, attach the
rubber tubing with the screw-pinch-cork. Immerse the lower end of the stalagmometer
into distilled water and suck through the rubber tubing until the level of water rises
above the mark X. Close the screw-pinch-cock and fit the rubber stopper carrying the
stalagmometer into the mouth of the beaker. Hold the stalagmometer vertical with the
help of clamp. Slightly open the screw-pinch-cock and count the number of drops as the
liquid from the mark X to Y. Repeat the process to record a number of observations.
Then clean and dry specific gravity bottle and weigh the empty bottle. Now fill it
with water and weigh.
Now repeat the whole process to take reading for different organic liquids.
General calculations:
Temperature of water = ToC
Density of water at this temperature = dw gm/lt
Number of drops of water = nw
Surface tension of water = w
(a) To calculate the density of liquid (ds)
Weight of empty bottle = W 1
Weight of empty bottle + water = W 2
Weight of empty bottle + solvent =W 3
Density of liquid (ds)= (Wt. of solvent/Wt. of water)X Density of water
X dw gm/cm3
(b) To calculate the surface tension of liquid
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Or X dyne/cm
Observation Table:
S. No. Organic Number Density Surface Surface Error
Liquid of drops (ds) Tension Tension
gm/l from
Literature
Precautions:
1. Wash stalagmometer and specific gravity bottle thoroughly with water and then
with acetone respectively after each reading.
2. Stalagmometer should be placed vertical
3. While counting the drops, all vibrations or disturbances of the stalagmometer
should be avoided.
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Experiment No: 9
To Determine The Amount Of Carbon Dioxide In A Given Water
Sample
AIM: To determine the amount of Carbon Dioxide in a given water sample
REAGENTS: 1. Beaker
2. Funnel
3. Pipette
4. Burette
APPARATUS REQUIRED: 1. N/50 Sodium Carbonate
2. Phenolphthalein
THEORY:
Chemical Reactions:
CO2 + 2OH- CO32- + H2O
CO2 + CO3 + H2O 2HCO3
PROCEDURE:
1. Rinse and fill the burette with Sodium Carbonate solution.
2. Note the initial reading and pipette out 100 ml of water sample to titration flask.
3. Add 5 drops of phenolphthalein indicator.
4. Titrate it against Sodium Carbonate solution until pink color persists for 30 sec.
5. Note the final reading.
OBSERVATIONS:
S.No. Initial Burette Final Burette ml of titrant used
Reading Reading
1.
2.
3.
CALCULATIONS:
USE N1V1 = N2V2
RESULT: The amount of free carbon dioxide is given as………….
PRECAUTIONS:
1. Before using the apparatus they should be properly washed with distilled water.
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2. Don’t blow air in pipette.
3. Be careful while noting down the readings.
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Experiment No: 10
To Determine The Chloride Content Of Given Water Sample
AIM: To determine the Chloride content of given water sample
REAGENTS: 1. N/ 35.5 Silver Nitrate solution
2. Potassium Chromate Indicator
APPARATUS: 1. Burette
2. Pipette
3. Titration flask (250 ml)
THEORY:
Chlorides occur in all natural waters in widely varying concentration. Upland and mountain
streams are usually low in chloride concentration. Chlorides gain access in many ways viz.,
solvent power of water dissolves salts from top soil, spray from oceaness, invading fresh waters
during tides, underground formations and seepage, domestic and industrial wastes.
Chemical reactions:
When pH is low:
2CrO42- + 2H+ HCrO4 Cr2O72- + H2O
When pH is high:
Ag+ + OH- AgOH
When AgNO3 is added to sample:
Ag+ + Cl- AgCl
2Ag + + CrO4 2- AgCrO4
PROCEDURE:
1. Take 100 ml of sample in a conical flask.
2. Place the same quantity of chloride free distilled water in another flask.
3. Add to both 0.5 ml of Potassium Chromate indicator.
4. Titrate with N/ 35.5 Silver Nitrate solution.
5. Note the amount of titrant used.
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OBSERVATIONS:
S.No.
1
2
3
CALCULATION:
ml of AgNO3 used for sample- ml of AgNO3 used for blank x 1000
Chlorides as Cl- =
ml of sample
RESULT: The chloride content of given sample is …………………………..
PRECAUTIONS:
1. Titrant should be freshly prepared
2. Before using the apparatus they should be properly washed with distilled water.
3. Don’t blow air in pipette.
QUESTION BASED ON EXPERIMENT:
1. Discuss the significance of the presence of high chloride concentration in water supplies?
2. Explain why blank correction must be applied to the titration values in the calculation of
chloride content.
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Experiment No: 11
To Determine Total Hardness Of Given Water Sample By EDTA
Method.
AIM: To determine total hardness of given water sample by EDTA method.
APPARATUS: 1.Burettes
2. Conical flasks
3. Measuring cylinders etc
REAGENTS:
1.Standard N/100 EDTA Solution – Take 5 gm of EDTA, heat it to 80°C for 1.5 hours. Cool. Take
3.72 gm of this salt (disodium salt) and add to it distilled water to make 1 liter.
2.Eriochrome Black T indicator – Dissolve 0.2 gm of pure solid to 15 ml of tri-ethanol amine. This
indicator readily comes in powder or tablet form.
3.Ammonium buffer solution – Take 70gm of NH4Cl, add to it 568 ml of concentrated ammonia
solution, stir and make 12 liters by adding distilled water.
THEORY:
Hardness in water is defined as soap consuming capacity of water. This is mainly due to presence of
calcium and magnesium ions in water. The hardness of water is taken as a measure of Ca++ and Mg++
contents. The hardness is temporary and permanent. When water is boiled, bicarbonates are
decomposed to form carbonate ions and CO2 is driven off. Thus temporary hardness is eliminated.
The permanent hardness is not removed by boiling.
Hardness of water is determined by complexometric titration method by using EDTA solution.
EDTA forms a complex with Ca++ and Mg++. The complexes exist at pH 8 to 10. The indicator used
is Eriochrome Black T. The color change with Eriochrome Black T is in the presence of these ions.
PROCEDURE:
Standardization of EDTA solution:
1. Take 25 ml of CaCl 2 sample in a conical flask.
2. Add 5 ml of buffer solution.
3. Add 3 drops of Eriochrome Black T indicator. The color becomes wine red.
4. Titrate with EDTA solution till the color changes to blue.
5. Take at least three readings. Let the volume of EDTA solution used in titration = V1 ml.
Determination of unknown hard water:
1. Take 25 ml of hard water sample in a conical flask.
2. Add 5 ml of buffer solution.
3. Add 3 drops of Eriochrome Black T indicator. The color becomes wine red.
4. Titrate with EDTA solution till the color changes to blue.
5. Take at least three readings. Let the volume of EDTA solution used in titration = V2 ml.
OBSERVATION TABLE FOR CaCl2
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Sr.no. Volume of CaCl2 taken in conical Volume of EDTA solution used ml
flask ml
1. 25 ml
2. 25 ml
OBSERVATION TABLE FOR HARD WATER:
Sr.no. Volume of hard water taken in Volume of EDTA solution used ml
conical flask ml
1. 25 ml
2. 25 ml
CALCULATION:
Use N1V1 = N2V2
RESULT: Hardness of water is …………………….ppm
PRECAUTIONS:
1. Glass wares namely burette, pipette, beakers should be rinsed only with the distilled water.
2. All the solutions should be checked with care before used
3. Distilled water should be checked with care before use.
4. The same amount of indicator must be added each time.
5. The reaction mixture should be briskly shaken during the titration.
6. The end point should be observed carefully.
7. pH10 should be maintained during the titration.
QUESTIONS BASED ON ABOVE EXPERIMENT:
1. What is EDTA? Give its right chemical name?
2. What is the role of Eriochrome black –T in EDTA titrations?
3. What is the role of buffer solution in EDTA titrations?
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