ChE 402: Chemical Engineering Laboratory-V

Experiment No: 06

Report
On

(A)

(B)

STANDARD TEST METHOD FOR CORROSIVENESS TO

COPPER FROM PETROLEUM PRODUCTS BY COPPER STRIP
TEST
STANDARD TEST METHOD FOR GROSS CALORIFIC VALUE
OF COAL AND COKE BY THE ADIABATIC BOMB
CALORIMETER

Prepared
by
Mir Hasib-Ul-Latif
Student number: 1002058
Level-4 Term-1
Chemical Engineering Department
Bangladesh University of Engineering and Technology

Date of Performance: March 03, 2015

Date of Submission: June 02, 2015

Group No: 05 (A2)

Partners Student number: 1002055
1002056
1002057
1002059
1002060

Summary
The objective of the Copper strip corrosion test is to know the process to determine the
degree of corrosion of copper from petroleum products by comparing with the American
Society of Testing and Materials (ASTM) Copper strip corrosion standards. In this
experiment diesel sample had been used as the petroleum product. It is important to know the
degree of corrosion of copper to handle petroleum products in copper vessels or conduits. The
copper strip found to be slightly tarnished in contact with the sample diesel oil. The
objective of the bomb calorimeter experiment is to get acquainted with the process to
determine the calorific value of solid fuels such as coal, coke etc according to the ASTM
standard testing method. To know the calorific value of a fuel is very important to select the
appropriate fuel that should be used in a certain process. It would give the heat energy
evolved by combustion of each fuel and thus the amount, quality and economy of using a
specific solid fuel can be studied by this experiment. The gross calorific value of the sample
coal was found to be 6740 kcal/kg.

(A)STANDARD TEST METHOD FOR CORROSIVENESS TO

COPPER FROM PETROLEUM PRODUCTS BY COPPER STRIP
TEST
Definition
Corrosiveness: Corrosiveness refers to cause irreversible damage or destroy to a substance
by another substance that has the power to contact.

Scope
This test method covers the detection of the corrosiveness to copper of aviation gasoline,
aviation turbine fuel, automotive gasoline, natural gasoline or other hydrocarbons having a
Reid vapor pressure no greater than 18 psi (124 kPa), cleaners (Stoddard) solvent, kerosine,
diesel fuel, distillate fuel oil, lubricating oil, and certain other petroleum products.
(Warning--Some products, particularly natural gasoline, may have a much higher vapor
pressure than would normally be characteristic of automotive or aviation gasolines. For this
reason, extreme caution must be exercised to ensure that the test bomb containing natural
gasoline or other products of high vapor pressure are not placed in the 100 oC (212oF) bath.
Samples having Reid vapor pressures in excess of 18 psi (124 kPa) may develop sufficient
pressure at 100oC to cause rupture of the test bomb.

Significance
Crude petroleum contains sulfur compounds most of which are removed during refining.
However, of the sulfur compounds remaining in the petroleum product, some can have a
corroding action on various metals and this corrosivity is not necessarily related directly to
the total sulfur content. The effect can vary according to the chemical types of sulfur
compounds present. The copper strip corrosion test is designed to assess the relative degree of
corrosivity of a petroleum product.

Apparatus
The apparatus used in the standard method of copper strip corrosion test are listed below:
Test tubes:
25 by 150 mm test tube is used in the standard test. It is capable of containing enough fuel
to make the copper strip completely submerged.
Constant temperature bath:

A bath capable of being maintained at a constant temperature (here 50 1C) and having
suitable supports to hold the test tubes in a vertical position and immersed to a depth
about 100 mm. Either water, oil, or Aluminum block baths are suitable. The bath
temperature is maintained by an electric heating system inside.
Copper Strip Corrosion Test Bomb:
It is constructed of stainless steel according to the standard dimensions and capable of
withstanding a test a test pressure of 100psi.
Thermometers:
Normal thermometer cpable of measuring the temperature of constant temperature
bath.Thermomters should be of total immersion type, for indicating hereured test
temperatre with smallest graduations of 1oC or less. No more than 25 mm of the mercury
thread should extend above the surface of the bath at the test temperature. The ASTM
12C or 1P 64C thermometer is suitable.
Polishing Vice:
It is used for holding the copper strip firmly without marring the edges while polishing.
Any convenient type of holder may be used provided that the strip is held tightly and that
the surface of the strip being polished is supported above the surface of the holder.
Viewing test tubes:
They are flat and convenient for protection-corroded strip for close inspection or storage.

Materials
Wash solvent :
Any volatile sulphur-free hydrocarbon solvent may be used provided that it shows no tarnish
at all when tested at 50C (122F). In our experiment Acetone had been used to wash the
fresh polished copper strip
Polishing material:
Silicon carbide or alumina grit paper of varying degrees of fineness including 65- m (240grit) silicon carbide paper or cloth: also a supply of 105 m (150 mesh) silicon carbide grain
and pharmaceutical grade absorbent cotton (cotton wool) can be used for this purpose.
Copper strips:
Strips of 12.5 mm wide, 1.5 to 3.0 mm thick, 75 mm long from smooth-surfaced, hardtemper, Cold-finished copper of 99.9+ percent purity is required by standard method of
testing. Electrical bus bar stock is generally suitable. The strips may be used repeatedly but
should be discarded when the surfaces become deformed on handling.

Experimental Setup

Fig-6.A.1: Pressure vessel for copper strip corrosion test.

Procedure
Surface preparation: Surface blemishes from the sides of the strip is removed with
silicon carbide or alumna grit paper of such degrees of fineness as are need to
accomplish the desired results efficiently. All marks that may have been made by
other grades of paper used previously should be removed. The strip is immersed in
wash solvent from which it may be withdrawn immediately for final polishing or in
which it may be stored for future use. As a practical manual procedure for surface
preparation a sheet of the paper on a flat surface is placed, it is moisten with kerosene
or wash solvent, and the strip is rubbed against the paper with a rotary motion,
protection the strip from contact with the fingers with an ash less filter paper.
Alternatively, the surface of the strip may be prepared by use of motor-driven
machines using appropriate grades of dry paper or cloth.
Final polishing: After removing the strip from the wash solvent, holding it in the
fingers protected with ash less filter paper, first the ends and then the sides are
polished with the 105- m (150- mesh) silicon carbide grains picked up from a clean
glass plate with a pad of cotton (cotton wool) moistened with a drop of wash solvent.
It is wiped vigorously with fresh pads of cotton and should be handled only with
stainless forceps and should not be touched with fingers.
Immersing the copper strip in diesel oil:The copper strip is then immersed in the
test tube containing diesel oil and

the test tube is set inside the test bomb by

immersing it in a water bath of (50 1 oC) in such a way so that the test tube is held
firmly and in a vertical position.
The copper strip removed:Then the test bomb is opened, the copper strip is
withdrawn from the test tube. It has to be handled very carefully so that any type of
marking or staining can be avoided.
Strip Examination:After withdrawing the copper strip gently with forceps it is
immersed in the wash solvent and then dried with filter paper by blotting only. Then it
is observed by comparison for the copper strip corrosion stndard to measure he

degree of corrosion if taken place. The oper strip and the standard strip have to be
held in 45o angle twards the light.

ASTM Copper strip corrosion standard:

The American Society of Testing and Materials provided the followingclassification for the
Copper strip corrosion test (ASTM D 130-94)

Table-6.A.1: ASTM Copper strip classifications

Classificatio
n
Freshly
polished strip

Designation

Description

-Light orange, almost the same as a

1a
Slight Tarnish

freshly polished strip

1b

Dark orange

2a

Claret red

2b

Lavender

2c

Moderate

Multi-colored with lavender blue

Tarnish

or silver, or both overlaid on claret

2d

Red Silvery

2e

Brassy or gold

3a

Magenta overcast on brassy strip

Dark Tarnish

3b
4a

Multi-coloured with red and green

showing (peacock), but no grey

Corrosion

Transparent black, dark grey or

brown with peacock green barely
showing

4b

Graphite or lusterless black

4c

Glossy or jet black

Observed Data
Description of corroded copper strip : Dark orange
Designation : Slight tarnish
Classification : 1b

Results and Discussion

The copper strip found to be slightly tarnished in contact with the sample diesel oil, which
refers to that the sample diesel oil causes a little change by reacting with Copper.
This slight tarnish of a copper strip represents a very minute amount of S present in the
sample that does not cause corrosion to the copper strip. And this copper strip can be reused
and also can be used as a container or conduit of such diesel oil or petroleum products
possessing similar properties. From the Moderate Tarnish classification range the sample oil
becomes hazardous for the metallic copper vessels, and should not be used as a container or
conduit for long term. If it goes to the Corrosion range of classification i.e. black or grey
layer is found on the copper strip then the oil is extremely hazardous for copper vessels and
some other metallic or plastic containers should be tested for using as the container or a
conduit. So this test proves to be very useful for selecting a copper made vessel or tube to
contain different petroleum products.
The contaminants in the oil enhance the corrosion tendencies to metal. The corrosiveness of
the oils like aviation gasoline, automatic gasoline, tractor oil, kerosene, diesel, lubricating oil
etc. to copper can be accomplished by copper corrosion test. Corrosiveness must be avoided
for safe and economical operation. While selecting materials for the construction of various
equipments the important consideration is the prevention of corrosion. And so a material
should be chosen which remains unaffected by the fuel used.
The Copper strip has to be well prepared according to the method and shouldnt have any
blemishes or stain on it. The test should be repeated if the sharp edges along the flat faces of
the strip appear to be in a classification higher than the greater portion of the strip.
When a strip is in the obvious transition state between that indicated by any two adjacent
standard strips, the sample is taken to be in the more tarnished classification.
The limitation of this experiment that the test result is observed compared with naked eyes
and can be erroneous and the result can vary for different observers. It is quite difficult to

distinguish between the colors in the slight and moderate tarnish ranges. So the test should be
run several times to be assured of the final result.

(B)STANDARD TEST METHOD FOR GROSS CALORIFIC VALUE

OF COAL AND COKE BY THE ADIABATIC BOMB
CALORIMETER
Definition
Calorific Value:
The heat produced by combustion of a unit quantity of a substance under specified
conditions. In the ASTM standard test method it is express in Btu/lb units. Calorific value
may also be expressed in (cal/g) or in SI units (J/g) when required.
Gross calorific value:
Gross heat of combustion at constant volume, Qv (gross)
Energy Equivalent/heat capacity/water equivalent:
The energy required to raise the temperature of the calorimeter one arbitrary unit. This is the
quantity that when multiplied by the temperature rise , then adjusted for extraneous heat
effects and divided by the mass of the sample gives the gross calorific value.

So, Gross Calorific value of Coal, Hc =

wT e1 e2 e3
m

Where,
w = energy equivalent of the sample, cal/oC
T= temperature rise in the calorimeter, oC
e1, e2 ,e3 = Thermochemical energy corrections for the test
m= mass of sample(coal) taken , g

For calculation of the correct gross calorific value, proper allowances for heat contributed by
other processes and thermochemical corrections should be made. The thermochemical
corrections related to this experiment are discussed below shortly.

Scope
This test method covers the determination of the gross calorific value of coal and coke
by the adiabatic bomb calorimeter
The values stated in SI units and British thermal units are to be regarded as the
standr
This standard does not purport to address the safety concerns f any, associated with
its use. It is the responsibilit of the user of this standard to establish appropriate
safety and healt practices and determine the applicability and regulatoylimittions
prior to use
All accountability and quality control aspecs of ASTM Guide D 4621 apply to this
standard

Significance
The gross calorific value is used to compute the total calorific content of the quantity of coal
represented by the sample for payment purposes, provided the buyer and the seller mutually
agree upon this. It is also used in computing the calorific value versus sulfur contentto
determine if the coal meets regulatory requirements for industrial fuels. It can also be used for
evaluating the effectiveness of beneficiation processes or for research purposes.

Apparatus

Combustion Bomb: It should be constructed of materials that are not affected by the
combustion process or products sufficiently to introduce measurable heat input or
alteration of end products. There must be no gas leakage during the test. The bomb
must be capable of withstanding a hydrostatic pressure test of 20 MPa at room
temperature.
Calorimeter vessel:It should be made of metal with a tarnish resistant coating, and
with all outer surface highly polished. Its size shall be such that the bomb will be
completely immersed in water when the calorimeter is assembled. It has an electric
stirring system at a uniform rate but minimum heat input.
Jacket: There is a double-walled, water filled jacket fully enclosing the calorimeter.
Thermometers: used to measure temperature in the calorimeter and jacket. Here a
liquid-in glass type thermometer. ASTM standard thermometers 56C,56F,116C or
117F types can be used.
Thermometeraccessories: A magnifier is used for reading the thermometer to one
tenth of the smallest scale division.
Sample holder: It is an open crucible of platinum, quartz or acceptable base-metal
alloy.
Ignition wire
Ignition circuit: used for ignition purpose provides 6 to 16 V alternating or direct
current to the ignition wire. A pilot light is required in the circuit to indicate the
current is moving.

Experimental Setup

Fig-6.B.1: Schematic diagram of standard test method for gross calorific value of coal and
coke by the adiabatic bomb calorimeter.

Procedure
The bomb is rinsed, inverted to drain and left to dry
A measured length of ignition wire is connected to the terminals, with enough slack to
allow the ignition wire to maintain contact with sample.
The bomb is assembled and O2 is charged at a pressure of 32 atm.
The calorimeter is filled with measured quantity of water(2000 g)adjusted from 1.0 to
2.0 oC below from room temperature.
The assembled bomb is placed in the calorimeter vessel. It is checked that no O 2
bubbles are leaking from the bomb. The calorimeter vessel is then placed inside the
water jacket. Then the electrodes are connected. The stirrer, thermometer and cover of
the vessel are placed in definite positions. The stirrer is started then
The initial temperature reading just before igniting the wire is taken.
When 3 consecutive readings became same within one-tenth of smallest thermometer
subdivisions then it can be assumed that the temperature has risen to its final
equilibrium value and that reading is taken.
The cover is opened then, the bomb is removed and pressure is released. The interior
of the bomb is washed with distilled water containing titration indicator.
The combined pieces of unburned ignition wire are measured and subtracted drom the
original length.

Observed Data
Weight of sample ( coke+coal) = 1.2622 g
Initial temperature = 24.89oC
Final temperature = 28.44oC

Calculated Data
Temperature difference = 3.55oC
Calorific value= 6740 kcal/kg

Sample Calculation
Temperature difference = (28.44-24.89) oC
= 3.55oC
Calorific value = (2405 3.55 -30) / 1.2622
= 6740 kcal/kg

Results and Discussion

The gross calorific value of the sample coal was found to be 6740 kcal/kg.
The gross calorific value of a solid fuel is a very important characteristic property of any
petroleum product or fuel as this value determines the quality or grade of the fuel. The higher
the calorific value, the better the quality or grade of the fuel as the calorific value refers to the
heat content of the fuel. And by burning a fuel through combustion reaction, heat energy is
evolved and transformed to many other useful forms.
So for selection of solid fuel when designing equipments or a plant, determination of its
calorific value is necessary to find out that whether it can serve the purpose for that definite
process and also proves to be an efficient and economic one.
Compared to the literature gross calorific value for general Anthracite coal which is
approximately 8600 kcal/kg, the calculated value for the given sample was 6814.26 kcal/kg
varied quite a bit, may be of composition difference and due to heat loss which are neglected
during the calculation.
According to the ASTM standard testing method all the apparatus handling and procedure
steps should have been maintained very strictly. It was required according to the calculation
steps that the calorimeter vessel and the test bomb are adiabatic fully, but it is not possible, a
little amount of heat loss cannot be prevented.
While ignition of the wire , the wire should be in definite contact with the sample fuel,
otherwise the circuit would not be closed, and the pilot light would show that no current is
passing through thus no ignition occurring. In our experiment we had to fix the wire 2 times
to ignite it properly.
While charging pressurized O2 gas in the bomb for combustion reaction, the supply rate
should be a uniform one and. The gas had to be admitted into the bomb so as not to blow
powdered material from the sample holder. If the pressure exceeds the specified pressure,
then the combustion reaction should not be continued anymore.

While handling the O2 cylinder and other pressurized vessels and some safety measures had
to be taken, and the vessels should contain some safety valve or rupture discs.