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OBJECTIVE
To determine the cloud point and pour point of given oil sample
CHEMICAL
Coconut oil
APPARATUS
THEORY
1. Cloud point :-
● It is a temp. at which oil becomes cloudy or hazy when oil is cooled at specific rate.
2. Pour point
OBSERVATION TABLE:
1. 43 Non-Hazy
2. 40 Non-Hazy
3. 37 Non-Hazy
4. 34 Non-Hazy
5. 31 Non-Hazy
6. 28 Non-Hazy
7. 25 Non-Hazy
8. 22 Hazy
9. 19 Non-Hazy
10. 16 Non-Hazy
11. 13 Solid
12. 10 -
CALCULATIONS:
CONCLUSION:-
Ideal cloud and pour point of coconut oil is 30°c & 17°c, the variation in a
reading is due to improper isolation and some measuring error.
QUESTIONS:
1. Write a note on the importance of cloud point & pour point for a
given oil.
The pour point of a liquid is the temperature below which the liquid loses
its flow characteristics. The pour point of a liquid is the temperature at which it
becomes semi solid and loses its flow characteristics. In crude oil a high pour
point is generally associated with a high paraffin content, typically found in crude
deriving from a larger proportion of plant material. Two pour points can be
derived which can give an approximate temperature window depending on its
thermal history. Within this temperature range, the sample may appear liquid or
solid.
2. Industrial application of cloud point & pour point.
♦ Cloud Point:
➢ The cloud point of petroleum products and biodiesel fuels is an index of the
lowest temperature of their utility for certain applications. Wax crystals of
sufficient quantity can plug filters used in some fuel systems.
♦ Pour Point:
➢ Oil and gas companies pay close attention to pour point because it has
an impact on drilling and transport. If a petroleum deposit has a high pour point,
usually reflecting a high paraffin content, it may be ifficult to extract. Drilling teams
need the oil to flow so they can pull it up with drilling rigs. Transport can also
become a problem; in some cases, oil pipelines need to be heated to keep the oil at
pour point and ensure it moves smoothly from oil fields to shipping terminals and
other destinations
4. How can the pour point of an oil be lowered? Explain the action of pour
point depressants.
• The pour point of a lubricant is the lowest temperature that fluid will flow
under standard conditions. A pour point depressant lowers that temperature. Pour
point depressants (also known as PPDs) are polymers that are designed to control
wax crystal formation in lubricants resulting in lower pour point and improved low
temperature flow performance.
• Pour point depressants do not lower the temperature at which wax crystals
begin to form, called the cloud point, or the amount of wax that is formed—pour
point depressants work by altering the crystal shape and size, which inhibits lateral
crystal growth. There are two known methods by which this may be achieved:
surface adsorption and co-crystallization.
EXPERIMENT: 2
AIM:
To figure out Flash point and Fire point of oil sample.
APPARATUS:
OBSERVATION:
Temperature(ºC) Remark
60 No flame
61 No flame
62 No flame
63 No flame
64 No flame
65 Flash point
66 No flame
67 No flame
68 No flame
69 Fire point
PRECAUSION:
● Rate of heat transfer should be control.
● Moisture removed from sample.
● Vapour of sample is harmful.
● Stay away from device during experiment.
RESULT:
● Flash point of given oil sample = 65ºC
● Fire point of given oil sample = 69ºC
CONCLUSION:
Ideal flash point and fire point of diesel is 65ºC and 78ºC respectively, the
variation in reading is due to improper isolation and some measuring error.
ADDITIONAL QUESTIONS:
1) WRITE A NOTE ON THE IMPORTANCE OF FLASH AND FIRE POINT FOR A
GIVEN OIL.
➢ FLASH POINT
- FUEL OIL FLASH POINT IS TO BE HIGH BECAUSE IF IT IS LOW,
THERE WOULD BE A POSSIBILITY OF FIRE IN STORAGE.
- ENGINE CRANKCASE LUBRICATING OIL FLASH POINT SHOULD BE AS HIGH
AS POSSIBLE TO PREVENT CRANKCASE EXPLOSION.
- FOR SAFE STORAGE, OIL STORAGE TANK HEATING TEMPERATURE TO BE
LIMITED TO AT LEAST 14°C LOWER THAN FLASH POINT TO PREVENT FIRE.
➢ FIRE POINT
- THE FIRE POINT IS USED TO ASSESS THE RISK OF THE MATERIALS ABILITY
TO SUPPORT COMBUSTION.
- THESE VALUES CAN ALSO AFFECT HOW THE FLUID MAY BE SHIPPED,
STORED, AND DISCARDED.
2) WHAT FACTORS AFFECT FLASH AND FIRE POINT AND WHAT IS THE
EFFECT THEY GIVE ON THE READING?
➢ FREQUENCY OF APPLICATION OF TEST FRAME
➢ RATE OF HEATING
➢ RATE OF STIRRING
➢ SIZE OF TEST FLAME
➢ TIME
➢ PRESSUREZ
3. WHAT IS MAIN DIFFERENCE BETWEEN OPEN CUP AND CLOSED CUP
FLASH POINT APPARATUS?
A KEY VARIABLE IN THIS TEST IS THE HEIGHT OF THE IGNITION SOURCE OVER
THE CUP.
AIM:
CHEMICAL:
● N/2 NaOH
● formaldehyde (1:1)
● 1 g ammonia sulphate
● phenolphthalein (Indicator)
APPARATUS:
● Flask
● Burette
● weight measuring device
PROCEDURE:
• Add 50 ml DM water.
• Add 30 ml Formaldehyde.
• Wait for 15-20 min & then titrate against N/2 NaOH using Phenolphthalein
as indicator.
OBSERVATION:
• Burette Reading: 30 ml
CALCULATION:
RESULT:
THEORY QUESTIONS
1.) REACTIONS:
(NH4)2SO4 + HCHO (NH2)4(CH2)6 + H+
● titration
H2BO3- + H+ H3BO3
AIM:
CHEMICAL:
● NaCl(Saturated)
● KOH(30-35% Concentrated)
● Methyl Red
● Sample gas (H, N, CO2)
APPARATUS:
● ORSAT INSTRUMENT
DIAGRAM:
100
0
PURGE OUTLET
SMALL
AMOU
NT OF
GLYCE
ROL
KOH
NaCl
NEW SAMPLE
ABSORBER BURETTE
GAS
PROCEDURE:
• First open all the nobs & then increase the level of NaCl in burette. So,
previously trapped air is removed from system. Now close all nobs except sample
gas and burette.
• Now Insert sample gas so that it directly goes to burette. And the close
sample gas nob.
• Level in the absorber is set to 0 and then the increase in the level of Nacl
in the burette shows the % of CO2 absorbed in KOH.
OBSERVATION:
CALCULATION:
% of CO2 absorbed
= (Final Burette reading × 100) / Max. Burette Reading
= (9 ml * 100) / 100
= 9%
RESULT:
9% OF CO2 IS ABSORBED.
THEORY QUESTIONS :
1. EXPLAIN LIMITIATIONS OF USING ORSAT APPARATUS?
B.) Oxygen
The four liquid absorbents which are commanly employed for the absorption of oxygen.
Are strongly alkaline solution of pyrogallol, acid solution of chromous cloride , alkaline
solution of sodium dithionate and ammoniacal cuprous chloride.
ADDITIONAL QUESTIONS :
I.The reagents in the absorption bulb are brought to the etched mark levels one by one by operating
the receiver bottle and the value of each bulb then their respective valves are closed.
II.All the air in receiver bottle is expelled to atmosphere by lifting the receiver bottle and opening
the three way to atmosphere.
III. It is quite necessary to follow the order of absorbing gases: CO2 first O2 second and CO last .
this is because the absorbent used for O2 can absorb only some CO2 and the % CO2 left would be
less ; while the % of O2 thus detected would be more. The absorbent used for CO2 , however,
doesn’ t absorb O2 or CO2.
IV.The percentage of CO in the flue gas is very small and this should be measured carefully.
When you drop a solid object such as a bead or a stone into a liquid, the object
either floats on top of the liquid or sinks to the bottom. In this bead bottle, the
beads neither float nor sink completely. The beads are suspended in the middle
of the liquid.
The beads appear suspended in the middle of the liquid because the bottle
contains not one, but two liquids. One of the liquids floats on top of the other
liquid. The beads sink in the top liquid, but float on the bottom one. This gives
the appearance that the beads are suspended in the middle of the liquid, but in
fact the beads rest where the two liquids meet.
Furthermore, when this bottle is shaken and set to rest, some of the beads float to
the top, while others sink to the bottom. As the bottle rests, the beads that sank to
the bottom begin to rise, while those that rose to the top begin to sink. After a
short while, the beads return to rest at the middle
EXPERMENT -5
AIM:
To determine COD of water sample.
CHEMICAL:
● Potassium dichromate Solution(K2Cr2O7)
● Sulfuric Acid
● DM water
● Ferrous Ammonium Sulphate
● Ferroin (Indicator)
● Mercuric Sulphate (HgSo4)
● Silver Sulphate (AgSo4)
● Water Sample
APPARATUS:
Digestion apparatus, Air condenser
THEORY:
● Chemical oxygen demand determination provide measure of oxygen
equipment of that portion organic matter in sample that is suspectable to oxidation
by strong chemical oxidant.
● Use of exactly same technology each time is important cause only part of
organic matter in included the portion depending on chemical use in structure of
organic compound and manipulative procedure.
● The dichromate reflux method has been selected for COD determination cause
it has advantage over oxidant in oxidability.
● Straight chain aliphatic compound aromatic hydrocarbon and pyridine are not
oxidised to any applicable,the straight chain compond are more effectively oxidised
when silver sulphate is added catalyst.
4) ferroin indicator:
PROCEDURE:
• Take 20 ml of sample in flask with fitted reflux condenser.
• Add 10 ml of 0.25N K2Cr2O7 solution and 0.1N H2SO4.
• Acid should be added in small amount carefully mixing after each addition.
• Add 0.4 gm AgSo4 and few glass beads.
• Attach flask to air condenser for 2 hours and 150º C.
• After 2 hours, cool and washdown with DM water.
• After cooldown sample, titrate against FAS using 2-3 drops of Ferroin
indicator.
• Colour change from bluish green to reddish brown.
REACTION:
OBSERVATION:
For NPH,
COD = (25.6-17.2) * 8000 * 0.0977 / (20)
= 328.272 ppm
For OPH,
COD = (25.6-24.7) * 8000 * 0.0977 / (20)
= 35.172 ppm
CONCLUSION:
COD of Mixed discharge is less than 250 ppm as per GPCB & CPCB norms.
Theory Questions:
1) What is COD and how it affects environment?
BOD (Biologocal Oxygen Demand) means the amount of oxygen (in mg/l)
microorganisms like bacteria need to 'eat' the organic polution (sugars, fat,
proteins, ...). Note that not all polution can be removed (eaten) by bacteria.
BOD value in polluted water is normally higher than the fresh water.
Increased BOD can be resulted due to domestic sewage, petroleum residues
and wastes of animals and crops.
4) Write the reaction and how it’ s a redox process and explain it briefly.
5) Explain the formula and reason for the terms used it in.
COD (in ppm) = (A-B) * M * 8000 / Volume of original sample
Where,
A =Volume of FAS used for blank solution (in ml)
B =Volume of FAS used for sample (in ml)
M =Multiplication factor
= 2.5 / Volume of FAS used for blank solution
Additional Questions:
1) Importance of each reagent in the experiment
● Potassium dichromate Solution(K2Cr2O7)
Potassium dichromate is a strong oxidizing agent under acidic conditions.
Acidity is usually achieved by the addition of sulfuric acid.
In the process of oxidizing the organic substances found in the water sample,
potassium dichromate is reduced (since in all redox reactions, one reagent is
oxidized and the other is reduced), forming Cr3+. The amount of Cr3+ is
determined after oxidization is complete, and is used as an indirect measure
of the organic contents of the water sample.
● DM water
For decreasing the temperature upto room temperature, After reaction at a
150ºC temperature.
● Ferroin (Indicator)
For detect to completion the reaction
● Mercuric Sulphate (HgSo4)
To reduce the halogen attack
● Silver Sulphate (AgSo4)
For increasing rate of reaction as a catalyst
● Safety Precautions
Make sure you are wearing a lab coat, latex gloves, and eye protection since
you are working with very hazardous chemicals.
● Apparatus
● Oven: Use an oven for culture-tube digestion only when it has been
determined that 2 hours of exposure at 150°C will not damage the caps. Whenever
you digest sample with potassium dichromate (K2Cr2O7), make sure you turn on
the hood to prevent hazardous chemicals from leaking.
3) GSFC maintains COD compliance by diluting high COD effluent stream with
low COD effluent stream. Similarly ,What are the other methods to reduce COD
content in effluent sample?
in the previous article, we will find that most of the COD is sourced from the
TSS or no dissolved solids commonly called sludge. The most important way
to get rid of the sludge is to use coagulants and flocculants.
The principle is to bind the sludge to one another so that a larger clumps of
sludge and then be deposited in a sedimentation tank.
This deposition process, will greatly affect the value of COD. Especially in
wastewater with a high enough amount of TSS. For additional information for
the 1 mg / L TSS you can get a drop of up to 10 mg / L COD.
In the aeration process, COD reduceed by making the bacteria can break down
organic compounds in water. These bacteria are called heterotrophic bacteria
break down organic compounds due to the use of oxygen. This process is
usually used in waste water with a COD of less than 3000 mg / L.
The anaerobic process is suitable for waste water with BOD levels over 2000
mg / L.
Some processes similar to this is the process of using MBR, SBR or SMBR
Some chemicals, can help you to reduce the COD of waste water. Chlorine,
Hydrogen peroxide and Ozone will mengoksdiasikan chemicals in the water
so that the automatic COD value will go down. But of course you should limit
dose usage of Oxidiser, because oxidiser possess sufficient betray especially
for living organisms.
COD reduction technique is suitable for waste have COD values derived from
non-biodegradable waste such as Phenol, surfactants, etc.
Fenton reaction is a reaction that has been widely known is able to reduce the
COD value. The principle is the formation of free radicals that are created
from the reaction between Fenton reagent is FeSO4 with Hydrogen peroxide.
Fenton reaction is what will be the forerunner of the birth of AOP system.
AOP is the latest technology that is able to reduce the COD value of the
wastewater. Even of COD with a value above 100 thousand though.
AOP was created from the added refinement of Fenton reaction in the
presence of ozone injection so adding reproduce free hydroxyl finally able to
oxidize chemicals in water.
Another plus is also located in the area used for this system is very small is
compared with other systems.
Moreover, this process does not require a lot of chemicals to be added in the
wastewater.
The latter method is widely used in the finishing process or post treatment
after primary treatment process. Usually used as an activated carbon filter.
Activated carbon will absorb organic substances, ozone or chlorine substances
remaining on the processing results. So safe effluent to be discharged into the
environment.