Faculty of Chemical &

Energy Engineering

RESERVOIR ENGINEERING LAB REPORT

SESSION/SEM: 2016/17 – SEM 2

Experiment no. 8
Title WATER CONTENT (BY
DISTILLATION)
Section 03
Group no. 7(G)
Group members 1. RAM KUMAR RAO A/L
NAGARAJAN
2. SANJIHUEN A/L SELVAMANI
3. SARAVIN A/L SELLEYITOREEA
4. SASIKUMAR A/L BAKAVATHEI
Lecturer DR. MOHD AKHMAL MUHAMAD
SIDEK
Technician 1. MR. ROSLAN JAS
2. MR. ZULKIFLE NASIR
Date of experiment 27TH FEBRUARY 2017

Date of submission 6TH FEBRUARY 2017

(through email*)
 TABLE OF CONTENTS

NO CONTENT PAGE

1 SUMMARY 2

2 INTRODUCTION 3

3 THEORY 3

4 METHODOLOGY 4

5 RESULTS 5-6

6 DISCUSSION 7

7 CONCLUSION 8

8 SUGGESTION 8

9 REFERENCES 8

10 APPENDICES 9-10

1
SUMMARY
“Water Content by Distillation” experiment is about testing the negative impact of
water in oils to the mechanical equipment. Therefore, we use used crude oil to determine the
water content in it as water increases the oxidation rate of oil and thus decreasing the oil’s
oxygen inhibitors and thus shorten the ‘life’ of the oil. The objective of this experiment is to
determine the percent of water in crude oil, in our case used car oil by using Dean Stark
Distillation-Extraction. However, there were still have some of the crude oil in the measuring
cylinder after the crude oil was put into the Dean-Stark apparatus. So the reading was accurate.
The conclusion of this experiment is that the water content of the crude oil used is very low
may be because the oil is changed constantly or it is still new.

The apparatus for this experiment is the Dean Stark Apparatus whereas the materials
used are solvent or petroleum spirit with 100°C-200°C boiling point and also oil sample which
is crude oil.

2
Introduction

In this experiment, the oil sample and an immiscible solvent in this case petroleum ether
was used in the Dean Stark apparatus is heated until it boils. Evaporated water and the solvent
being cooled by condenser to form water and petroleum ether again. The water and the
petroleum ether are collected in a graduated cylinder. As water has a higher density than the
petroleum spirit, water will settle below the graduated cylinder and the solvent will be at the
top. Water content on any petroleum product is very important to determine the purity and
safety and also the compatibility of the product in its usage, such as in refinery and others.

This experiment is purely conducted using distillation process. Distillation is a method

of separating mixtures based on the differences in volatilities in a boiling point mixture. Dean
Stark Distillation-Extraction is a laboratory glassware used to collect water from a reactor. The
major result of this experiment is the collected water result from heating the solvent which is
petroleum spirit and the crude oil.

Theory

Water content in any petroleum product is very important to determine the purity and safety
and also the compatibility of the product in its usage, such as being used in refinery. In this
experiment, the oil samples and an immiscible solvent in the Dean-Stark apparatus is heated
until it boils. Evaporated water and the solvent being cooled by condenser to form water and
solvent again. The water and the solvent are collected in a graduated cylinder.

Percentage of water in sample can be calculated by:

𝑤𝑎𝑡𝑒𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 𝑐𝑜𝑙𝑙𝑒𝑐𝑡𝑒𝑑

% 𝑤𝑎𝑡𝑒𝑟 = × 100 =
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒

3
Methodology

1. 100 ml used lubricant oil sample and 100 ml solvent measured using graduated cylinder.

2. The used lubricant oil sample and the solvent mixed into the Dean-Stark apparatus.

3. 5-10 glass beads were put into the apparatus.

4. The apparatus then was put on an electric heater.

5. A retort stand used to hold the apparatus.

6. The apparatus was assembled as in Fig 1.

7. Water was flow through the condenser.

8. The sample heated and regulated the heat such that the liquid drop was around 3 drops per
second.

9. The collected water heated until volume does not change with time.

10. The condenser then rinsed with solvent to collect the water on the inner condenser wall.

11. The reading of the water volume recorded in the graduated tube water collector.

4
Data and Results

Group G
Sample Crude oil
Collector size 10 ml
Solvent type Petroleum Ether

Table 1 : Measurement of Water Volume

Time (sec) Collected water Observation Note

volume (ml)
60 1.10 The water droplets There are about 3
drop very quickly on droplets per second
this period
120 1.40 Water droplets begin The time between
to drop slowly two drops are
slightly higher
180 3.80 The time taken The time between
between two water two drops increased
droplets are high dramatically
240 6.00 The water reaches The graduated tube
above the maximum was shaken slightly
measurements and to make sure all the
fall back into the water droplets to
flask accumulate at the
bottom.
300 6.00 The water reaches
above the maximum
measurements and
fall back into the
flask

5
 600 6.00 The water reaches
above the maximum
measurements and
fall back into the
flask
900 6.00 The water reaches
above the maximum
measurements and
fall back into the
flask
1200 6.00 The water reaches
above the maximum
measurements and
fall back into the
flask

Sample volume : 200 ml

Water volume collected : 6.00 ml

𝑤𝑎𝑡𝑒𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 𝑐𝑜𝑙𝑙𝑒𝑐𝑡𝑒𝑑

% 𝑤𝑎𝑡𝑒𝑟 = × 100 = 3 %
𝑠𝑎𝑚𝑝𝑙𝑒 𝑣𝑜𝑙𝑢𝑚𝑒

6
Discussion

1. State two other methods to determine water content in oil.

Fourier transform infrared (FTIR) spectroscopy and the Karl Fischer titration test. Of
these two methods, FTIR is generally less expensive but also not as accurate. FTIR
uses an infrared light, which is passed through an oil sample. The light absorption at
different wavelengths in the spectra is then measured to indicate the concentration of
water. This test is restricted to lower detection limits of approximately 1,000 parts per
million (ppm).

The Karl Fischer titration test is much more accurate and has the ability to measure as
little as 1 ppm of water in oil when used correctly. This method uses two types of
titration to identify trace amounts of water in a given sample: coulometric or
volumetric. The principles are the same for each, except volumetric uses a titrant
solution. This testing method can be very beneficial because it allows you to analyse
solids, liquids or gases. The disadvantages of the Karl Fischer titration test include its
cost and the amount of time required when water concentrations are high.

2. Why solvent is used in this experiment.

The solvent, petroleum ether, was used in order to minimize the vaporisation process
that undergoes very vigorously so that the experiment can be determined.

3. List down several problems if crude oil were polluted with water.
The water sometimes containing salts which can be deposited in the refinery and if
high – temperature is applied, the hydrolysis of water can be happened. Besides, the
water will affect its purity and distillation process cannot be undergoing properly.

7
Conclusion

As conclusion for our water content experiment, we conclude that the collected water
from the mixture of benzene and used crude oil after a certain time is 6.0ml. While, the
percentages of the collected water which has been distilled out from Dean-Stark apparatus
that contain 200ml of mixture is 3 %.

Suggestion

We have some suggestions to improve and overcome the problems occurred during the
experiment. There were some error that occurred during this experiment.

 Firstly, parallax error is caused by the wrong position of the eyes during taking the
reading will make the reading taken is not accurate. Therefore, we have the make sure
the reading is taken at the meniscus level of the scale to obtain a more accurate
reading.
 Then, there were still have some of the crude oil in the measuring cylinder after the
crude oil was put into the Dean-Stark apparatus. So the reading will not be accurate.
At one point, it was difficult to differentiate the difference between oil and water
making the reading to be inaccurate.

References
1. McCain, William, D. (1990). The Properties of Petroleum Fluids. Penn Well Books.
2. Amyx, J.W., Bass, D.M & Whiting, R.L. (1960). Petroleum Reservoir Engineering.
McGraw-Hill, New York.

8
Appendices

There is only one formula used for this experiment.

Percentage of water present in oil sample

= water volume collected X 100%

Sample volume

9
10