Technical College of Engineering

Department of Petrochemical
COURSE: refinery
Class: Second 2018 - 2019

Name of Experiment: Standard Test Method for

Water in Crude Oil by Distillation D 4006 – 81 (Reapproved 2000)

Submitted by: Bryar Husen

Experiment No: 2
Date of experiment: 23 /02 /2019

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EVALUATION

Activity During Experiment & Procedure

Data & Results

Discussion, Conclusion & Answer to the Questions

Neat and tidy report writing

Overall Mark
Title
Standard Test Method for
Water in Crude Oil by Distillation D 4006 – 81 (Reapproved 2000)

Objective: To find the percentage of water in a sample of crude oil by

distillation (Dean Stark) method.

Introduction
The sample is heated under reflux conditions with a water immiscible
solvent (xylene,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.
Water is present with crude oil in reservoir rocks and it enters the pores
with oil during some stimulation processes which are carried to
stimulate the well, such as Acidizing and Fracturing. The water forms
with oil emulsions of two types: Hydrophilic (water in oil) and
Hydrophobic (oil in water). The stability of petroleum emulsions
depends on the nature and composition of the film material
surrounding the water droplets, which prevents their mixing with each
other.
This test method covers the determination of water in crude oil by
distillation.
The sample is heated under reflux conditions with a water immiscible
solvent 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.
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 and to loss of energy used to heat the oil in
addition to the salts in water which deposit on the distillation devices
and inside the pipes.
A determination of water and sediment content is required to measure
accurately net volumes of actual oil in sales, taxation, exchanges, and
custody transfers.
If the water content in oil is more than 2%, it complicates the process of
distillation to a large extent. The presence of water in petroleum
products and fuels is also undesirable, especially in cold weather
conditions.
Apparatus & Materials:

The apparatus, shown in Fig. 1, consists of:

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 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.

Results & Calculations:

1. Record the final volume of water in the trap to the nearest 0.025
ml.
2. Calculate the water in the sample as follows:

Water volume % = (water volume / sample volume) * 100

Discussion:
1-What is the source of water and sediments in crude oil?
- Basic sediment and water (BS&W) is a technical specification of certain
impurities in crude oil. When extracted from an oil reservoir, the crude oil will
contain some amount of water and suspended solids from the reservoir
formation. The particulate matter is known as sediment or mud. The water
content can vary greatly from field to field, and may be present in large quantities
for older fields, or if oil extraction is enhanced using water injection technology.
The bulk of the water and sediment is usually separated at the field to minimize
the quantity that needs to be transported further.

2-What are the factors affecting accuracy of the result?

- Water can adhere to glassware if it’s not cleaned properly
„ Incomplete refluxing of crude „
Improper reading of trap
3-What are the disadvantages of the presence of water with crude oil?
- 1.Money – Water displaces crude which costs money
2. Processability – Water content can cause difficulties in refining and
transportation; corrosion
3. Environmental – Water must be treated before it can be disposed of
4-How is oil – water emulsion treated in oil industry?
- The heat input and thus the fuel required for treating depends on the temperature
rise, the amount of water in the oil, and the flow rate. Because heating a given
volume of water requires approximately twice the energy needed to heat the same
volume of oil, it is beneficial to separate free water from the emulsion to be treated.
Often this is done in a separate free-water-knockout (FWKO) vessel upstream of
where heat is added. Sometimes it is accomplished in a separate section of the
same vessel.
5-Is the process of separating the water in this experiment physical or
chemical and why the solvent is used?
References
D95 Test Method for Water in Petroleum Products and Bituminous Materials by
Distillation (API MPMS Chapter 10.5)
D473 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method
(API MPMS Chapter 10.1)
D665 Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the
Presence of Water
D1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method
(Laboratory Procedure) (API MPMS Chapter 10.6)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products (API
MPMS Chapter 8.1)
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API
MPMS Chapter 8.2)
D4928 Test Method for Water in Crude Oils by Bolometric Karl Fischer Titration (API MPMS Chapter 10.9)
E123 Water
2.2 API Standards:
MPMS Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM
Practice D4057)
MPMS Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM
Practice D4177)
MPMS Chapter 10.1 Test Method for Sediment in Crude Oils and Fuel Oils by the
Extraction Method (ASTM Test Method D473)
MPMS Chapter 10.4 Determination of Water and/or Sedi-ment in Crude Oil by the
Centrifuge Method (Field Procedure)
MPMS Chapter 10.5 Test Method for Water in Petroleum Products and Bituminous
Materials by Distillation (ASTM Test Method D95)
MPMS Chapter 10.6 Test Method for Water and Sediment in Fuel Oils by the
Centrifuge Method (Laboratory Proce-dure) (ASTM Test Method D1796)
MPMS Chapter 10.9 Test Method for Water in Crude Oils by Coulometric Karl Fischer
Titration (ASTM Test Method D4928)