All Saints' College of Technology

Sagar Institute of Science & Technology

Opposite Raja Bhoj International Airport, Gandhi Nagar, Bhopal, Madhya Pradesh 462036

LAB MANUAL
OF

ENGINEERING CHEMISTRY

B .Tech (Bachelor of Technology)

First Year
Common for all branches
Academic Session………………..

Name

Enrollment No.

Branch :

Semester Section

Department of Basic Sciences Page 1

 INDEX
Sr. Name of experiment Page Date of Date of Grade Signature
no. no. experiment submission

1 Complexometric titration
[Hardness]

2 Analysis of water :Total

alkalinity

3 Argentometric titration

4 Iodometric titration

5 Viscosity index [Redwood

viscometer no.1]

6 Viscosity index [Redwood

viscometer no.2]

7 Cleveland's open cup

apparatus

8 Abel's closed cup apparatus

9 Penskey Marten's apparatus

10 Cloud and pour point

[Lab Technician ] [Faculty ] [ H.O.D.

2|Page
 First Year
Department Of Basic Science

Course Outcome of Laboratory Experiments

Student will be able to :

CO1: Apply the role of chemistry on water analysis by titrimetric method of

complexometry.

CO2: Apply the role of chemistry on water analysis by titrimetric method of alkalinity and

determination of type and extent of alkalinity.

CO3: Analyze the strength of Copper in the given alloy by Iodometric titration.

CO4: Analyze the properties of Lubricant viz Flash and Fire point and their determination

by using testing apparatus to check their significance.

CO5: Interpret the properties of Lubricant viz Viscosity, Viscosity index along with their

determination by using testing apparatus to check their applicability.

Department of Basic Sciences Page 3

 EXPERIMENT 1

AIM:

To determine the total hardness of given water sample by EDTA method.

APPARATUS AND REAGENTS REQUIRED:

Burette, Pipette, Conical Flask, Measuring Flask, EDTA Solution, EBT indicator, Water
sample.

THEORY:

Hardness of water can be determined by complexometric titration. EDTA is used as

complexing agent. The Ca2+ and Mg++ present in water are titrated with EDTA and EBT is used as
Indicator.

Estimation is based on following steps:

(i) First the indicator EBT forms an unstable complex with free metal ion at pH=10
pH =10
Mg /Ca + EBT
++ ++ [Mg++/Ca++―EBT]
Wine Red complex

(ii) Once the free metal ions are consumed, EDTA replaces EBT from wine Red complex. As a
result EBT becomes free.
pH=10
[Mg /Ca + EBT] +EDTA
++ ++ [Mg++/Ca++―EDTA] + EBT
Colourless Blue

PROCEDURE:

(i) Rinse and fill the burette with the EDTA soln.
(ii) Pipette out 20ml of hard water in to conical flask and add 2 ml of buffer soln.
(iii) Add 2 drops of EBT indicator [ wine red soln. is obtained]
(iv) Titrate against N/100 EDTA soln. till the colour of the soln. changes from wine red to
light blue.
(v) Note the final reading and repeat to get two concordant readings.

Department of Basic Sciences Page 4

OBSERVATION TABLE {1:1}

(i) EDTA against known hard water sample.

S.No. Volume of hard Burette reading for change in colour Vol. of EDTA
water sample(ml) from wine red to blue
consumed (ml)
Initial (ml) Final (ml)

01

02

03

OBSERVATION TABLE {1:2}

(ii) EDTA against unknown hard water sample.

S.No. Volume of hard water Burette reading for change in Vol. of EDTA
sample(ml) colour from wine red to blue
consumed (ml)
Initial (ml) Final (ml)

01

02

03

CALCULATION:

Unknown hard water sample against EDTA

N1V1=N2V2

Where N1= Normality of unknown hard water sample

V1 = Volume of unknown hard water sample taken

N2= Normality of EDTA

V2= Volume of EDTA

Strength in ppm=Normality of hard water (N1) ×Equivalent wt. of CaCO3×1000

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CALCULATION:

RESULT:

The total hardness of given water sample is ………………..ppm

PRECAUTIONS:

(i) Glassware should be rinsed before use.

(ii) Colour change near the end point is very slow and thus should be observed
carefully.

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VIVA VOCE:

Q 1. What is the hardness of water?

Ans:-

Q 2. What is temporary and permanent hardness?

Ans:-

Q 3. What is the unit of hardness?

Ans:-

Q 4. How can we remove temporary hardness of water?

Ans:-

Q 5. How can we remove permanent hardness of water?

Ans:-

Q 6. What do you mean by complexometric titration?

Ans:-

Q 7. What is the full form of EDTA?

Ans:-

Q 8 .What is EBT?

Ans:-

Q 9. How EDTA titration is done?

Ans:-

Q 10. What is total hardness?

Ans:-

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 EXPERIMENT 2

AIM:

To determine mixed alkalinity of the given water sample.

APPARATUS AND REAGENTS REQUIRED:

Burette, Pipette, Conical Flask, Measuring Flask.N/50 H2SO4, Phenolphthalein indicator, Methyl
orange indicator.

THEORY:

Water has ability to neutralize free acids. In alkalinity all the substances which cause an
increase in hydroxide concentration (OH-) upon dissociation or due to hydrolysis are included.
The water alkalinity is due to the presence of: CO3-,HCO3- and OH-. Alkalinity of water sample
can be determined by estimating the quantity of OH- , CO32-, HCO-3 by titrating water sample
against standard H2SO4 solution. Phenolphthalein and methyl orange are used as indicators. The
determination is based on the following reactions

(i) OH- + H+ H2O

(ii) CO32- + H+ HCO-3

(iii) HCO-3 + H+ H2O + CO2

Reaction (i) and (ii) are completed up to phenolphthalein end point. The amount of acid used
corresponds to hydroxide plus half of the normal carbonate present. While titration of water
sample with methyl orange end point marks the completion of the Reaction (i), (ii) and (iii) the
total amount of acid represents total alkalinity.

Thus P= OH- and 1/2 CO32-

M= OH-, CO32-, HCO-3

The possible combinations of ions causing alkalinity in water are

(i) OH- only

(ii) CO32- only
(iii) HCO-3 only
(iv) OH- and CO32- together
(v) CO32- and HCO-3 together

PROCEDURE:

Take out 10 ml water sample by using pipette and transfer it in to conical flask, add 1-2
drops of phenolphthalein indicator in it, pink colour appears. Now titrate this solution against
N/50 H2SO4 solution until pink colour disappears. Note down the reading as phenolphthalein end
8|Page
point. Now in the same solution add two drops of methyl orange indicator yellow colour appears.
Titrate against N/50 H2SO4 solution till yellow colour changes to pink colour. Note the reading as
methyl orange end point. In both the cases take two concordant readings.

OBSERVATION TABLE:{ 2:1}

S.No. Volume of Volume of H2SO4 solution used up to Volume of acid

unknown used up to methyl
water phenolphthalein end point(ml). orange end
sample(ml) point(ml) (Total
Initial Final(A)
volume of acid
used) (B)

01

02

03

CALCULATION:

(a)Strength of water sample using phenolphthalein as indicator.

N1V1 = N2V2

Where, N1 or Np=Normality of water sample

V1=Volume of water sample

N2= Normality of H2SO4

V2= Volume of H2SO4

Strength in ppm= Np× Equivalent wt.of CaCO3×1000

(b)Strength of water sample using methyl orange as indicator

N1V1 = N2V2(Vp+Vm)

N1 or Nm=Normality of water sample

V1=Volume of water sample

N2= Normality of H2SO4

V2= Volume of H2SO4(Vp+Vm)

Total alkalinity or methyl orange alkalinity.

= Nm × Equivalent wt. of CaCO3×1000ppm

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CALCULATION:

RESULT:

Total alkalinity of water sample is ……………………… ppm.

PRECAUTION:

(i) Before starting the experiment clean all the glassware thoroughly.
(ii) The end point of the titration should be observed carefully.

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VIVA VOCE:

Q 1. What do you mean by alkalinity of water?

Ans:-

Q 2. What do you mean by alkali?

Ans:-

Q 3. What is the difference between alkali and base?

Ans:-

Q4. What is the cause of alkalinity in water?

Ans:-

Q5. What do you mean by phenolphthalein alkalinity?

Ans:-

Q6. What is methyl orange alkalinity?

Ans:-

Q7. What type of alkalinity will be present in water and to what extent?

a. If P >1/2 M

b. If P < 1/2 M

c. If P =O

d. If P =M

Q8. What is normality?

Ans:-

Q 9.What is molarity?

Ans:-

Q10. What is molality?

Ans:-

Q11. What is molecular weight?

Ans:-

Q12. What is equivalent weight?

Ans:-

Q13. What is acidity of base?

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Ans:-

Q14. What do you mean by strong base or strong acid?

Ans:-

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 EXPERIMENT 3

AIM:

To determine chloride ion in a given water sample by argentometric method.

APPARATUS AND REAGENTS REQUIRED:

Burette, Pipette, Conical Flask, Measuring Flask, standard silver nitrate solution (N/50),
potassium chromate indicator (K2CrO4).

THEORY:
Chloride ions, present in the water sample can be determined by argentometric method. In this
method water sample is titrated against silver nitrate solution using potassium chromate as an
indicator. The solubility product of AgCl is less than that of Ag2CrO4. Until unless Cl- ions are
available, AgCl being less soluble is precipitated. When all the Cl- ion present in the water sample
get precipitated as AgCl, even a drop of AgNO3 added gives a red precipitate of silver chromate.

AgNO3 + Cl- AgCl + NO3-

2AgNO3+ K2CrO4- Ag2CrO4+2KNO3

PROCEDURE:

1. Pipette out 20 ml of given Cl- solution in a conical flask, add 1 ml K2CrO4 indicator.
2. Add N/50 AgNO3 solution slowly from the burette. A white ppt is formed initially.
3. Add silver nitrate solution till a permanent reddish brown colour is obtained. Take two
concordant readings. Let V2 is the volume of AgNO3 used.

CALCULATION : Forrmula

N1V1= N2V2

Where, N1= Normality of water sample

V1= Volume of water sample

N2= Normality of AgNO3 solution

V2= Volume of AgNO3 solution

Strength of Cl- ions = N1 x 35.5 x 1000 ppm

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OBSERVATION TABLE : { 3:1}

S.No. Volume of Burette reading Vol. of AgNO3

water sample(ml) Consumed (ml)

Initial (ml) Final (ml)

01

02

03

CALCULATION:

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RESULT:

The strength of chloride ions present in water sample is……………… ppm.

PRECAUTIONS:

1. Before starting the experiment glassware should be washed with distilled water.
2. The end of point of the titration should be observed carefully.
3. The volume of indicator should be same in all titrations.
4. During titration reaction mixture should be shaked vigorously.

VIVA-VOCE:

Q.1 What do you understand by argentometric titration?

Q.2.What is solubility product?

Q.3.How chloride can be determined in a given water sample?

Q.4.What is redox titration?

Q.5. Why a white precipitate is obtained after adding AgNO3 into the water sample?

Q.6.What is normality?

Q.7.What is strength?

Q.8.What will be the equivalent weight of AgNO3?

Q.9. What do you understand by titration?

Q.10.What is the effect of excess chloride ions on water quality?

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 EXPERIMENT 4

AIM

To determine the strength (gm/l) of unknown copper sulphate CuSO4.5H2O Solution (B) using
intermediate hypo Solution and standard CuSO4.5H2O solution of N/30 normality (A)

APPARATUS AND REAGENTS REQUIRED

Burette, Pipette, Conical Flask, Measuring Flask N/30copper sulphate CuSO4.5H2O

solution(A), unknown copper sulphate CuSO4.5H2O solution (B), hypo solution, potassium
iodide, starch solution.

PRINCIPLE

Iodometry, also known as iodometric titration, is a method of volumetric chemical analysis, a

redox titration where the appearance or disappearance of elementary iodine indicates the end
point. Free iodine is titrated against standard reducing agent such as sodium thiosulfate solution.
Usual reagents are sodium thiosulfate as titrate, starch as an indicator (it forms blue complex with
iodine molecules - though polyvinyl alcohol has started to be used recently as well), and an iodine
compound (iodide or iodate, depending on the desired reaction with the sample).The colour
change at the end point is usually blue to colourless (milky white suspension).

The principal reaction is the reduction of iodine to iodide by thiosulfate:

I2 + 2 S2O32− S4O62- + 2 I-

Chemical Reactions

[CuSO4+2KI K2SO4+CuI2]×2

2 CuI2 CuI2+ I2

2CuSO4+4KI 2K2SO4 + Cu2I2 + I2

Cuprous iodide (Dark Brown Suspension)

I2 + 2Na2S2O3 2NaI +Na2S4O6 (Milky White)

(Sodium tetrathionate)

16 | P a g e
PROCEDURE

1. Wash the burette with water, rinse with hypo solution and the make up to zero mark.
2. Wash the Pipette with the water. Rinse with CuSO45H2O.Pipette out 10 ml. of acidified
CuSO4.5H2O. Soln. in conical flask and transfer it followed by addition of 1 ml of 10% KI
soln.
3. Cul2 being unstable dissociates to produce Cu2I2 and I2.
4. Due to liberation of I2 the colour of CuSO4.5H2O turns dark brown.
5. Add hypo solution from burette to conical flask. Shake the contents of the conical flask.
Continue the addition of hypo solution to the conical flask, till the appearance of light or
pale yellow colour.
6. Add 1-2 drops of freshly prepared starch indicator in the titrating flask the solution turns
blue. (Adsorption).
7. Continue the addition of hypo solution to the conical flask, till the disappearance of blue
color. (At the end point milky white suspension appears due to Cu2I2 cuprous Iodide
formation).Note the burette reading.
8. Repeat the same procedure to get the concordant reading.
9. Follow the same procedure for the unknown solution (B) and obtain concordant reading.
10. Calculate the strength of CuSO4.5H2O (B) Solution

CALCULATION:-

Standard CuSO4.5H2O Solution Vs Hypo

N1V1 = N2V2
N1 = Normality of Standard CuSO4.5H2O Solution
V1 = Volume of Standard CuSO4.5H2O Solution
N2 = Normality of Intermediate Hypo Solution
V2 = Volume of Intermediate Hypo Solution

(Na2S2O3)
and
N2 V2 = N3 V3
N2 = Normality of Intermediate Hypo
V2 = Volume of Intermediate Hypo
N3 = Normality of Unknown CuSO4 Solution
V3 = Volume of Unknown CuSO4 Solution
Strength gm/l = Normality x Equivalent wt. of CuSO4.5H2

17 | P a g e
 For Sample A (Standard Copper Sulphate Solution)

Titration of standard CuSO4.5H2O Solution (A) with intermediate hypo solution

OBSERVATION TABLE : { 4:1}

S.No. Volume of Burette reading Volume of hypo

CuSO4.5H2O solution used
Initial Final
solution taken in (ml)
ml
1
2
3

For Sample B (Unknown Copper Sulphate Solution)

Titration of unknown CuSO4.5H2O Solution (B) with intermediate hypo solution

OBSERVATION TABLE : { 4:2}

S.No. Volume of Burette reading Volume of hypo

CuSO4.5H2O solution used
Initial Final
Solution taken in (ml)
ml
1
2
3

CALCULATION:-

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CALCULATION

Standard CuSO4.5H2O Solution Vs Hypo

N1V1 = N2V2
N1 = Normality of Standard CuSO4.5H2O Solution
V1 = Volume of Standard CuSO4.5H2O Solution
N2 = Normality of Intermediate Hypo Solution
V2 = Volume of Intermediate Hypo Solution

(Na2S2O3)
and
N2 V2 = N3 V3
N2 = Normality of Intermediate Hypo
V2 = Volume of Intermediate Hypo
N3 = Normality of Unknown CuSO4 Solution
V3 = Volume of Unknown CuSO4 Solution
Strength gm/l = Normality x Equivalent wt. of CuSO4.5H2

RESULT

The strength of unknown solution of CuSO4.5H2O is ………….. gm / lit.

Viva-Voce

Q.1 Why is hypo solution used for Iodometric titration?

Q.2 Why do you need freshly prepared starch solution for Iodometric Titrations?

Q.3 Differentiate between Iodometry and Iodimetry

Q.4 What is hypo solution?

Q.5 What is strength?

Q.6 What are the applications of Iodometry?

Q.7 The colour of the copper sulphate solution becomes blue after adding starch, why?

Q.8 Why milky white suspension is obtained at the end point?

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 EXPERIMENT 5

AIM

To determine the effect of temperature on the viscosity of the given thin oil using Red Wood
Viscometer No. 1.

APPARATUS AND REAGENTS REQUIRED

Redwood Viscometer No.1, Kohlrausch flask, thermometer, beaker, stop watch, lubricating oil
sample etc.

THEORY

Viscosity of the liquid is its property by virtue of which it offers resistance to its own flow. Its
unit is poise.

Viscosity index is defined as the rate at which the viscosity of oil falls rapidly changes with
temperature. If the viscosity of an oil falls rapidly as the temperature is raised then it has low
viscosity index.

Units of Viscosity

C.G.S. System: 1 poise = 1 dyne/sec/cm2

1 centipoise = 1/100 poise
S.I. System: Newton second/m2 (NS/ m2)
1 NS/ m2 = 10 poise
Viscosity is the most important property of any lubricating oil and helpful in the selection of good
lubricants oil.

Redwood Viscometer No. 1

Fig. 5.1

Department of Basic Sciences Page 20

 OBSERVATION TABLE 5.1

S.No. Temperature (°C) Time (Sec)

1.

2.

3.

4.

GRAPH BETWEEN TEMPERATURE AND TIME OF FLOW (VISCOSITY)

Fig 5.2

21 | P a g e
PROCEDURE

1. Level the viscometer with the help of leveling screws.

2. Fill the outer bath with water and connect to the electric mains.

3. Clean the oil cup and discharged jet with xylol or benzene followed by passing a small
amount of the test oil through the jet.

4. Place the ball valve on the agate jet to close it and pour the test oil in to the cup to such a
level that the metal indicator fixed on the wall of the cup just dips in the coil.

5. Insert the thermometer and a stirrer. Keep stirring the water in the bath and oil in the cup
and adjust the bath temperature until the oil attains the desired constant temperature.

6. Place a clean and dry kohlrausch flask immediately below and directly in line with the
discharge jet.

7. Remove the ball valve with one hand, simultaneously starting the stop watch with the
other.

8. Oil from the jet flows into the flask. Record the time of flow of oil in seconds.

9. Repeat the experiment to take number of readings at different temperatures.

10. Report the time of flow in seconds mentioning the test temperature.

11. Plot a graph between time of flow in seconds and temperature.

RESULT

The graph was plotted between the temperature and time of flow of the given lubricating
oil. From the graph it is concluded that viscosity decreases as temperature increases.

PRECAUTIONS

1. The oil cup and receiver should be properly washed every time.

2. The temperature of water and oil should be same.

3. The oil flowing into receiver should not slide down through wall of receivers.

4. Oil sample should be filtered through filter paper to remove solid particles that may clog
the jet.

22 | P a g e
VIVA VOCE

Q1. What is viscosity?

Q2. What is the unit of viscosity?

Q3. On what factors do the viscosity depends?

Q4.What is the effect of temperature on viscosity?

Q5. How can we determine the viscosity of lubricating oil (thin oil)?

Q6. How can we determine the viscosity of thick oil?

Q7. What is the difference between Redwood Viscometer No.1 and No.2?

Q8. What is viscosity index?

Q9. Whether RW1 or RW2 should be used for determining the viscosity of mustard oil?

Q10. What is the procedure adopted for determining the effect of change in temperature on

Viscosity with the help of Redwood viscometer?

23 | P a g e
 EXPERIMENT 6

AIM
To determine the effect of temperature on the viscosity of thick oil with the help of Redwood
Viscometer No.2

APPARATUS AND REAGENTS REQUIRED

Redwood Viscometer No.2, oil, water, flask (50ml), thermometer, stop watch.

THEORY

Viscosity of the liquid is its property by virtue of which it offers resistance to its own flow. Its
unit is poise.

Viscosity index is defined as the rate at which the viscosity of oil falls rapidly changes with
temperature. If the viscosity of an oil falls rapidly as the temperature is raised then it has low
viscosity index.

Units of Viscosity

C.G.S. System: 1 poise = 1 dyne/sec/cm2

1 centipoise = 1/100 poise
S.I. System: Newton second/m2 (NS/ m2)
1 NS/ m2 = 10 poise
Viscosity is the most important property of any lubricating oil and helpful in the section of good
lubricants oil.

Redwood Viscometer No. 2

Fig 6.1

Fig. Redwood Viscometer No. 2

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OBSERVATION TABLE : { 6.1}

S.No. Temperature (°C) Time (Sec)

1.

2.

3.

4.

5.

6.

7.

GRAPH BETWEEN TEMPERATURE AND TIME OF FLOW (VISCOSITY)

Fig 6.2

25 | P a g e
PROCEDURE

1. Level the viscometer with the help of leveling screws.

2. Fill the outer bath with water and connect to the electric mains.

3. Clean the oil cup and discharged jet with xylol or benzene followed by passing a small
amount of the test oil through the jet.

4. Place the ball valve on the agate jet to close it and pour the test oil in to the cup to such a
level that the metal indicator fixed on the wall of the cup just dips in the coil.

5. Insert the thermometer and a stirrer. Keep stirring the water in the bath and oil in the cup
and adjust the bath temperature until the oil attains the desired constant temperature.

6. Place a clean and dry kohlrausch flask immediately below and directly in line with the
discharge jet.

7. Remove the ball valve with one hand, simultaneously starting the stop watch with the
other.

8. Oil from the jet flows into the flask. Record the time of flow of oil in seconds.

9. Repeat the experiment to take number of readings at different temperatures.

10. Report the time of flow in seconds mentioning the test temperature.

11. Plot a graph between time of flow in seconds and temperature.

RESULT

The graph was plotted between the temperature and time taken. From the graph it is
concluded that viscosity decreases with raise in temperature.

PRECAUTIONS
1. The oil cup and receiver must be washed properly.
2. The temperature of water and oil should almost be same.
3. Oil should fall directly in the receiver bed and not stick to the walls.

26 | P a g e
VIVA VOCE

Q1. What is viscosity?

Q2. What is the unit of viscosity?

Q3. On what factors do the viscosity depends?

Q4.What is the effect of temperature on viscosity?

Q5. How can we determine the viscosity of lubricating oil (thin oil)?

Q6. How can we determine the viscosity of thick oil?

Q7. What is the difference between Redwood Viscometer No.1 and No.2?

Q8. What is viscosity index?

Q9. Whether RW1 or RW2 should be used for determining the viscosity of mustard oil?

Q10. What is the procedure adopted for determining the effect of change in temperature on

Viscosity with the help of Redwood viscometer?

27 | P a g e
 EXPERIMENT 7

AIM

To determine flash and fire point of the given oil sample using Cleveland’s open cup
apparatus.

REQUIRMENTS

Cleveland’s apparatus, sprit lamp, match box, thermometer and oil sample.

THEORY

Good lubricating oil should not vapourize much at its working temperature and should not give
enough vapours that could lead to a fire breakout. Flash point is that temperature at which oil
sample gives sufficient vapours with a flash when a flame is brought near it. Fire point is that
temperature at which oil vapours give sufficient vapors which burn continuously for a period of
at least 5 seconds when a flame is brought near it. In most of the cases fire point is 5 to 400 C
higher than the flash point. At flash point and fire point the vapours of oil form an inflammable
mixture with air.

Fig 7.1 : Cleveland’s Apparatus

28 | P a g e
 OBSERVATION TABLE : { 7:1}

Temperature in increasing order

S.No. Temperature in 0C Observations

OBSERVATION TABLE : { 7:2}

Temperature in decreasing order

S.No. Temperature in 0C Observations

29 | P a g e
PROCEDURE

1. Fill the oil cup up to the mark with the oil sample provided.
2. The apparatus is heated at a rate of 1-2o C rise per minute.
3. When the temperature rises up to 150 C below the anticipated flash point, the flash
is introduced near the oil vapours for about 2 seconds at every degree rise in
temperature.
4. The lowest temperature at which distinct flame is observed on exposure to flame is
noted down as flash point
5. The oil is again heated at rate of 1o C rise in temperature, until oil vapor burn
continuously up to at least 5 seconds this temperature is noted down as fire point.

RESULTS

The flash point of the given oil sample is……………oC

The fire point of the given oil sample is……………oC

PRECAUTIONS

1. The moisture should not be present inside the oil cup.

2. The bulb of the thermometer should be dipped inside the oil sample.

VIVA VOCE

Q1 what is flash point?

Q2 what is fire point?

Q3 what is the importance of determining flash and fire point of oil?

Q4 which apparatus is employed for determining flash and fire point of oil?

Q5 what is the difference between the Cleveland’s open cup apparatus’, Pensky martin and
able cup apparatus?

Q6 Explain the working of Cleveland’s open cup apparatus’?

Q7 Explain the working of Pensky Martin’s closed cup apparatus’?

Q8 Explain the working of Abel’s closed cup apparatus’?

Q9 If we reuse the oil sample what will be the effect observed on flash and fire point. ?

Q10 what will be the effect on flash and fire point if moisture is present in water?

30 | P a g e
 EXPERIMENT 8

AIM

To determine flash & fire point of given oil sample using Abel’s apparatus.

REQUIREMENTS

Abel’s apparatus, sprit lamp, match box, thermometer and oil sample.

THEORY

Good lubricating oil should not vapourize much at its working temperature and should not
give enough vapours that could lead to a fire breakout. Flash point is the temperature at which oil
sample gives sufficient vapours with a flash when a flame is brought near it. Fire point is the
temperature at which oil vapours give sufficient vapours which burn continuously for a period of
at least 5 seconds, when a flame is brought near it. In most of the cases fire point is 5 to 400 C
higher than the flash point. At flash point and fire point the vapours of oil form an inflammable
mixture with air.

Significance

Flash &fire point of a lubricating oil should be higher than the working temperature. Otherwise it
could leads to a fire break out.

So it is very necessary to calculate flash and fire point of a lubricating oil to provide a safe guard
against the fire hazards and such lubricating oil is selecting which have a flash & fire point above
the working temperature. Liquids having flash point less then 1400 F are called flammable liquids
and liquids with flash point above 1400 F are called combustible liquids.

Fig 8.1: Abel’s apparatus.

31 | P a g e
PROCEDURE

1.Fill the oil cup up to the mark with the oil sample provided.
2.Fill water in the jacket provided for it
3.Cover the oil cup with lid and introduce thermometer to the opening provided for it.
4. The apparatus is heated at a rate of 1-2o C rise per minute and the stirrer is rotated at a
rate of 60 revolutions per minute.
5. When the temperature rises up to 150 C below the anticipated flash point, the flash is
introduced near the oil vapors for about 2 second at every degree rise in temperature.
6. The lowest temperature at which distinct flame is observed on exposure to flame is noted
down as flash point.
7. The oil is again heated at rate of 1o C rise in temperature, until oil vapour burn
continuously up to at least 5 second this temperature is noted down as fire point.

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OBSERVATION

OBSERVATION TABLE : {8:1}

Temperature in increasing order

S.No. Temperature in 0C Observations

OBSERVATION TABLE : { 8:2}

Temperature in decreasing order

S.No. Temperature in 0C Observations

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RESULT

The flash point of the given oil sample is…………… oC

The fire point of the given oil sample is…………… oC

PRECAUTIONS:

(i) The moisture should not be present inside the oil cup.
(ii) The bulb of the thermometer should be dipped inside the oil sample.
(iii) Oil sample should be stirred continuously for uniform heating.
(iv) At the time of application of test flame, stirring must be stopped.

VIVA-VOCE

Q1 what is flash point?

Q2 what is fire point?

Q3 what is the importance of determining flash and fire point of oil?

Q4 which apparatus is employed for determining flash and fire point of oil?

Q5 what is the difference between the Cleveland’s open cup apparatus’, Pensky martin and
able cup apparatus?

Q6 Explain the working of Cleveland’s open cup apparatus’?

Q7 Explain the working of Pensky Martin’s closed cup apparatus’?

Q8 Explain the working of Abel’s closed cup apparatus’?

Q9 If we reuse the oil sample what will be the effect observed on flash and fire point. ?

Q10 what will be the effect on flash and fire point if moisture is present in water?

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 EXPERIMENT NO. 9

AIM

To determine Flash & fire point of given oil sample using Pensky Martin’s apparatus.

REQUIREMENT

Pensky Martin’s apparatus, Sprit lamp, match box, thermometer and oil sample.

THEORY

Good lubricating oil should not vapourize much at its working temperature and should not
give enough vapours that could lead to a fire breakout. Flash point is the temperature at which oil
sample gives sufficient vapour with a flash when a flame is brought near it fire point is that
temperature at which oil vapours give sufficient vapour which burn continuously for a period of
at least 5 seconds when a flame is brought near it. In most of the cases fire point is 5 to 40 0 C
higher than the flash point. At flash point and fire point the vapour of oil form a inflammable
mixture with air.

Significance

Flash &fire point of a lubricating oil should be higher than the working temperature.
Otherwise it could leads to a fire break out.

So it is very necessary to calculate flash and fire point of a lubricating oil to provide a safe
guard against the fire hazards and such lubricating oil is selecting which have a flash & fire point
above the working temperature. Liquids having flash point less than 1400 F are called flammable
liquid and liquids with flash point above 1400F are called combustible liquids.

Fig 9.1: Pensky Martin’s apparatus

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OBSERVATION

OBSERVATION TABLE : { 9:1}

Temperature in increasing order

S.No. Temperature in 0C Observations

OBSERVATION TABLE : { 9:2}

Temperature in decreasing order

S.No. Temperature in 0C Observations

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PROCEDURE

1. Clean and dry all parts of the apparatus before starting the experiments.
2. Fill the oil up with the oil to be tested up to the mark.
3. Cover the oil cup with lid and introduce thermometer to the opening provided for it.
4. Start heating the oil at a rate of about 5-6oC per minute.
5. When the temperature rises up to 150 C below the anticipated flash point, the flash is
introduced near the oil vapours for about 2 second at every degree rise in temperature.
6. The lowest temperature at which distinct flame is observed on exposure to flame is noted
down as flash point.
7. The oil is again heated at rate of 1o C rise in temperature, until oil vapours burn
continuously up to at least 5 second this temperature is noted down as fire point.

RESULT

The flash point of the given oil sample is found to be……………oC

The fire point of the given oil sample is found to be ……………oC

PRECAUTIONS

1. The moisture should not be present inside the oil cup.

2. The bulb of the thermometer should be dipped inside the oil sample.
3. Oil sample should be stirred continuously for uniform heating.
4. At the time of application of test flame, stirring must be stopped.

VIVA-VOCE

Q1 what is flash point?

Q2 what is fire point?

Q3 what is the importance of determining flash and fire point of oil?

Q4 which apparatus is employed for determining flash and fire point of oil?

Q5 what is the difference between the Cleveland’s apparatus, Pensky Martin’s apparatus and
Abel’s cup apparatus?

Q6 Explain the working of Cleveland’s open cup apparatus?

Q7 Explain the working of Pensky Martin’s closed cup apparatus’?

Q8 Explain the working of Abel’s closed cup apparatus’?

Q9 If we reuse the oil sample what will be the effect observed on flash and fire point. ?

Q10 What will be the effect on flash and fire point if moisture is present in wa

37 | P a g e
 EXPERIMENT 10

AIM

To determine Cloud and Pour point of the given lubricating oil.

REQUIREMENT

Cloud and Pour point apparatus, thermometer, freezing mixture, oil sample.

THEORY

Cloud Point is the temperature at which waxy crystals in an oil or fuel form a cloudy
appearance. The pour point can be defined as the minimum temperature of a liquid, particularly a
lubricant, after which, on decreasing the temperature, the liquid ceases to flow. These
temperatures are important for transportation and storage of fuels.

Significance

Cloud and pour point indicated the suitability of lubricants in cold condition. The lubricants used
in cold climate should have the points lower than the atmosphere or operating temperature,
otherwise it will solidify inside the machine and cause jamming of the machine.

Fig 10.1: Cloud and Pour Point Apparatus

PROCEDURE

(i) Clean and dry the test jars and fill the oil sample in it.
(ii) Fit the thermometer in the test jar also fit another thermometer in the cooling bath.
(iii) Prepare a freezing mixture by mixing ice and. CaCl2.
(iv) The tube is taken out from the freezing mixture after each 1o fall in temperature.
(v) The temperature at which cloudiness appears is noted down as cloud point.
(vi) Keep the jar again in freezing mixture and inspect after each 3o fall in temperature.
(vii) When oil stops flowing, after tilting the test jar for 30 seconds, note down the
corresponding temperature as pour point.

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 OBSERVATION TABLE : { 10.1}

Temperature in decreasing order

S.No. Temperature in 0C Observations

RESULT

The cloud point of the given oil sample is found to be……………oC.

The Pour point of the given oil sample is found to be ……………oC

PRECAUTIONS

(i) The observation of the tube should be completed within 3 to 4 seconds.

(ii) Choose a suitable freezing mixture for the particular lubricating oil.
(iii) The flat bottomed tube should not be kept directly in the freezing mixture.
(iv) Pour point should be note down with great care without disturbing the mass of the oil.

VIVA-VOCE

Q.1 What do you understand by Cloud and Pour point of a Lubricant?

Q.2 What is the significance of determining this point?

Q.3 What is freezing mixture?

Q.4 Why a lubricant ceases to flow at low temperature?

Q.5 How CaCl2 play important role in maintaining the temperature of ice bath below zero

degree centigrade?

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