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Expt5 Solemne
Expt5 Solemne
Abstract
A laboratory experiment was carried out to determine the proportion of a petroleum product
that will evaporate at various temperatures through the distillation of natural gasoline. A
straightforward distillation process was utilized in two trials. The second trial collected more
distillate than the first, but distillation was successful. It is believed that the cause is the
variation in heating rates between the trials.
I. Introduction
Based on their varying boiling points, the constituent elements of a fluid combination can
be separated using a method called distillation. It entails boiling a mixture inside of a flask.
The element with the lowest boiling point will evaporate since the mixture's components have
differing boiling points. The vapor is then allowed to fall inside a cooled tube, where it
condenses back into a liquid and flows into a receiving container. The unevaporated
substances remaining that can be seen in the flask are referred to as the residue, while the
condensed liquid is known as the distillate.
Petroleum products are liquid mixtures comprised of various metals, sulfur, nitrogen, and
hydrocarbons with varying melting points. Natural gas contains the same hydrocarbons that
are present in petroleum products. So it is possible to distill natural gasoline from petroleum
products using the distillation process.
The purpose of this experiment is to quantify the proportion of petroleum products that will
evaporate at various temperatures. Two repetitions of the experiment will be conducted using a
straightforward distillation technique. To demonstrate his comprehension of the subject, the
researcher will examine the temperature and volume data acquired from the experiment.
II. Scope and Limitations
The distillation of natural gasoline is covered by this procedure. The measurements
given in inch-pound units should be taken as the norm. There may be restrictions in the
experiment's approach. To achieve the appropriate rate of distillation, the heat of the gas
burner must be controlled during the distillation. However, to get the correct quantity of
heat, the gas burner being utilized had to be adjusted using a gas valve. As seen in table 5,
improper heat regulation might result in variations in the rate of distillation between
experiments. This will also result in variations in the volume of the final distillate. It would
be simpler to achieve the desired distillation rate if you used an easily adjustable heating
device, like an electric heater.
Thermometer Number
Temperature Range
ASTM IP
30 to 580 7°F …
IV. Procedure
1. A. Apparatus
1. Fill the condenser bath with cracked ice (Note 1) and add enough water
to cover the condenser tube. Maintain the temperature between 32 and
34°F (0-1.1°C). Agitation with air gently aids in maintaining the required
temperature range.
Note 1 – Any other cooling medium may be used.
2. Swab the condenser tube to remove any liquid remaining from the
previous test. A piece of soft lint-free cloth, attached to a cord or copper
wire may be used for this purpose.
3. Measure a 100-ml sample in a 100-ml cylinder at 32 to 40°F (0 to 4.5°C)
and transfer it directly to the distillation flask. Both the flask and the
graduated cylinder shall have been cooled to a temperature from 32 to
40°F (0 to 4.5°C) before use. Do not permit any of the liquid to flow into
the vapor tube.
4. Make a record of the room at the time of each distillation. The heating
apparatus including the shield and the flask support shall be at room
temperature at the start of each distillation.
5. Fit the thermometer (previously cooled at a temperature of 32 to 40°F (0
to 4.5°C) and dried tightly into the flask with a suitable cork so that
lower of the capillary tube is on a level with the inside of the bottom of
the vapor outlet tube at its junction with the neck of the flask.
6. Place the charged flask at the 1 14-in (32mm) opening in the 6 by 6-in
(150 by 150-mm) asbestos board with the vapor outlet tube inserted into
the condenser tube. A tight connection must be made by means of a cork
thru which the vapor tube passes. Adjust the position of the flask so that
the vapor tube extends into the condenser tube not less than 1 in
(25.4mm) nor more than 2 in (50mm).
7. Place the graduated cylinder in measuring the charge without drying, the
outlet of the condenser tube in such a position that the condensed tube
shall extend into the cylinder at least l-in (25.4mm), but not below the
100-ml mark. Immerse the graduated cylinder up to the level of the outlet
of the condenser tube in a transparent bath, maintained between the
temperatures of 32 to 34°F (0 to 1.1°C). Cover the top of the cylinder
closely during the distillation with a piece of blotting paper, or its
equivalent so cut as to fit the condenser tube tightly. A lead washer or
other suitable materials, resting on the blotting paper tightly against the
top of the cylinder and also provides the additional weight necessary to
overcome the buoyant effect of the liquid in the cooling bath.
B. Test Procedure
1. When. everything is in readiness, apply heat immediately at a uniform
rate, so regulated that the first group of the condensate falls from the
condenser in not less than a min nor 5 min. When the first drop falls
from the end of the condenser, move the receiving cylinder so that the
end of the condenser tube shall touch the side of the cylinder. Then
regulate the heat so that the first 10 ml distillate shall be recovered in not
less than 3 min or more than 4 min. Therefore, thereafter, maintain the
rate of distillation at not less than 4 ml/min nor more than 5 ml/min.
Record the reading of the distillation thermometer when the level of the
distillate reaches each 10-ml mark on the cylinder. In case a product is
being tested to ascertain whether or not it conforms with a given
specification, make and record all necessary observations, whether or not
they are included in the series ordinarily employed by the laboratory
making the test.
2. When liquid residue in the distillation flask is approximately 5 ml, heat
may be increased because of the presence of heavy ends, which may
have relatively high boiling points. However, do not apply any further
increases of heat after this adjustment. The 4 to 5-ml rate cannot always
be maintained from this point to the end of the distillation but in no case
should the period between the point when approximately 5 ml ·of the
liquid remains in the flask and the net point is more than 5 min.
3. Continue the heating until the mercury reaches a maximum and starts to
fall consistently after the bottom of the flask has become dry. Record the
highest temperature observed on the distillation thermometer as the
maximum temperature or endpoint.
4. Observe the total volume of the distillate collected in the receiving at the
conclusion of the distillation and therefore at not less than 2-min
intervals, until successive observations agree. Then record this volume as
the recovery.
5. Pour the cooled residue from the flask into a small graduated cylinder 0.1
ml. Measure when cool and record the vo1ume as residue at 32 to 40°F
(0 to 4.5°C).
6. Calculate the difference between 100 ml and the sum of the recovery and
the residue and record all distillation loss.
Note 2 - Abnormal distillation losses, when caused by low barometric
pressure, may be corrected by the equation given below to an approximation
of the loss to be expected under normal pressure. The corrected losses shall
not be used in the calculation of percentage evaporated.
𝐶𝑜𝑟𝑟𝑒𝑐𝑡𝑒𝑑 𝐿𝑜𝑠𝑠 = 𝐴𝐿 + 𝐵
Where:
L = Observed distillation loss
A & B = empirical constants, as given in table 2, for various values of the
observed barometric pressure
°C °F °C °F
10 to 30 50 to 86 0.35 0.63
30 to 50 86 to 122 0.38 0.68
The necessary temperature and volume information acquired during the sample's distillation
are shown in Table 4. Table 1 shows that the distillate recovered during the second trial (86.5
vs. 81.5%) is 5 mL more than the distillate collected during the first trial. However, the amount
of residue left over after distillation was the same (at 6%) in both instances. Both experiments
resulted in the same endpoint temperature. Table 4 also shows that more distillate vapor was
lost during the first trial than during the second trial. If the rate of distillation across trials is
compared, an explanation for this can be observed.
When the level of the distillate hits each 10-mL mark on the graduated cylinder, the
temperature readings from the distillation thermometer are shown in Table 5. It can be seen that
the sample heated up significantly more quickly in the first trial than it did in the second. It was
also noticeable during the experiment that the distillate vapor flowed significantly more quickly
during the first attempt than it did during the second. The difference in recovered distillate seen
in table 4 is explained by increased vapor flow speed during the first trial, which led to more
vapor failing to condense and instead escaping into the atmosphere. Additionally, it may be
deduced that slower heating during distillation will result in greater distillate recovery than
faster heating.
VI. Conclusion
During two distillation trials, the various temperatures at which a petroleum product will
evaporate were identified. In the first trial, 81.5 mL of natural gasoline was distilled from the
100 mL petroleum sample, and in the second trial, 86.5 mL was distilled. This resulted from
the sample heating up significantly more quickly during the first trial than it did during the
second. The distillate variation across experiments would be lessened by the use of
conveniently adjustable heating units. These results suggest that if the rate of distillation can
be regulated, natural gasoline may be extracted from petroleum with little loss.
Questions
A. Plot the distillation curve (temp vs percent evaporated) for the given sample. What is
the significance of this curve?
C. If the endpoint temp for two trials differs more than 6°F (3.5°C), list the possible
reasons or causes for this discrepancy.
- The presence of another chemical with a higher boiling point in one of the
samples could explain different endpoint temperatures for the same sample.
References
[1] R.-J. Yang, C.-C. Liu, Y.-N. Wang, H.-H. Hou, L.-M. Fu, “A comprehensive review of
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Oct. 4, 2022. doi: 10.1016/j.cej.2016.11.041. [Online]. Available:
https://www.sciencedirect.com/science/article/pii/S1385894716316011
[2] G. Yasin, M. I. Bhanger, et al., “Quality and chemistry of crude oils,” J. Pet. Technol.
Altern. Fuels, vol. 4, pp. 53–63, March 2013. Accessed: Oct. 2, 2022. doi:
10.5897/JPTAF12.025. [Online]. Available:
https://academicjournals.org/journal/JPTAF/article-stat/CE9D1489251
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https://www.eia.gov/energyexplained/oil-and-petroleum-products/ (accessed Oct. 2,
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[4] "Distillation." chem.ucla.edu.
http://www.chem.ucla.edu/~bacher/Specialtopics/Distillation.html (accessed Oct. 2,
2022).