Duhok polytechnic university

Faculty of Petrochemical Engineering

School of Petroleum Refinery

Laboratory of petroleum Refinery

 EXPERIMENT NUMBER TWO(2)

WATER IN CRUDE OIL BY DISTILLATION

Instructor: Mr. alaa
Author Name: Muhammad Akram
Experiment Contacted on: 24/Feb/2018
Report Submitted on: 3/MAR /2018
Group: A
Objective:
To find the percentage of water in a sample of crude oil by
distillation (Dean Stark) method.

INTRODUCTION:
Crude is mixed with water immiscible solvent (toluene)
„The mixture is boiled (refluxed) forcing water and
solvent overhead „Condenser condenses solvent and
water into trap „Trap returns solvent to crude while
retaining water The sample is heated under reflux
conditions with a water immiscible solvent (toluene),
which co-distills with the water in the sample. Condensed
solvent and water are continuously separated in a trap; the
water settles in the graduated section of the trap, and the
solvent returns to the distillation flask, This test method
covers the determination of water in the range from 0 to
25 % volume in petroleum products, tars, and other
bituminous materials by the distillation method
Significance and Use:
 A knowledge of the water content of petroleum products is
important in the refining, purchase, sale, and transfer of
products.
 The amount of water as determined by this test method (to
the nearest 0.05 volume %) may be used to correct the
volume involved in the custody transfer of petroleum
products and bituminous materials.
 The allowable amount of water may be specified in
contracts.

Solvent-Carrier Liquid:
Aromatic Solvent—The following aromatic solvents are
acceptable:
 Industrial Grade Xylene.
 A blend of 20 volume % industrial grade toluene and
80 volume % industrial grade xylene.
 Petroleum or Coal Tar Naphtha.
Apparatus & Materials:
1. A glass distillation flask-a 1000-mL (or 500ml) round-
bottom, glass, distillation flask
2. A 5-mL calibrated, graduated water trap with 0.05-mL
graduations connected to the distillation flask.
3. A 400-mm condenser fitted with the trap.
4. A drying tube filled with desiccant (to prevent entrance
of atmospheric moisture) is placed on top of the
condenser.
5. An electric heating mantle that can uniformly distribute
heat to the entire lower half of the flask
6. Solvent: different solvents can be used. Toluene,
xylene or a mixture of both or naphtha. The solvent is
miscible with oil but immiscible with water.
7. A sample of crude oil.
Procedure:
1. Measure (100 ml) of the crude oil sample in a graduated
cylinder and transfer it to the distillation flask.
2. Add 100 ml solvent to the flask in three stages 50 ml, 25ml
and 25ml using the graduated cylinder of step one (total solvent
volume 100 ml).
3. Use glass beads or other boiling aids to reduce bumping
distillation flask.
4. Assemble the apparatus as shown in Fig. 1, making sure all
connections flask. are vapor and liquid-tight.
5. Insert a drying tube containing an indicating desiccant into the
end of the condenser to prevent condensation of atmospheric
moisture inside the condenser.
6. Circulate water, between 20 and 25°C, through the condenser
jacket.
7. Apply heat to the flask. Heat should be applied slowly during
the initial stages of the distillation (condensation rate 2-5 drops/
second) to prevent bumping and possible loss of water from the
system.
8. Continue heating until no water is visible in the condenser and
the volume of water in the trap remains constant for at least 5
min.
9. Allow the trap and contents to cool to 20°C. Dislodge any
drops of water adhering to the sides of the trap and transfer them
to the water layer. Read the volume of the water in the trap.
Result & calculation:

volume of water = 3.2 ml

water volume
Water volume% = sample volume × 100

3.2
Water volume% = 100 × 100 = 3.2%
Discussion:
1- What is the source of water and sediments in crude oil?
 Natural water in oil underground
 We can add water to oil
2- What are the factors affecting accuracy of the result?
 Temperature
 viscosity
3- What are the disadvantages of the presence of water with
crude oil?
 The water and sediment content of crude oil is significant
because it can cause corrosion of equipment and problems
in processing. It leads to high pressure in the tower to loss
of energy used to heat the oil.
4- How is oil - water emulsion treated in oil industry?

 Dehydration chemicals, or demulsifiers, are chemical compounds

that are widely used to destabilize, and assist in coalescence of,
crude-oil emulsions. This treatment method is popular because the
chemicals are easily applied, usually are reasonable in cost, and
usually minimize the amount of heat and settling time required.
5- Is the process of separating the water in this experiment
physical or chemical and why the solvent is used?
 The process is chemical and the solvent is used to
separate water and immiscible solvent in a trap.