I.

OBJECTIVES
1. To determine the carbon residue content of sample lubricating oil.

II. THEORY AND PRINCIPLES

Carbon residue is the residue formed by evaporation and thermal degradation

of a carbon containing material. The residue is not composed entirely of carbon but is
a coke that can be further changed by carbon pyrolysis. The term carbon residue is
retained in deference to its wide common usage. The test method for carbon residue,
as listed in the diesel fuel specification is D 524.

The D 524, Standard Test Method for Ramsbottom Carbon Residue of

Petroleum Products. The sample, after being weighed into a special glass bulb having
a capillary opening, is placed in a metal furnace maintained at approximately 550°C.
The sample is thus quickly heated to the point at which all volatile matter is
evaporated out of the bulb with or without decomposition while the heavier residue
remaining in the bulb undergoes cracking and coking reactions. In the latter portion of
the heating period, the coke or carbon residue is subject to further slow
decomposition or slight oxidation due to the possibility of breathing air into the bulb.
After a specified heating period, the bulb is removed from the bath, cooled in a
desiccator, and again weighed. The residue remaining is calculated as a percentage of
the original sample, and reported as Ramsbottom carbon residue. Provision is made
for determining the proper operating characteristics of the furnace with a control bulb
containing a thermocouple, which must give a specified time-temperature
relationship.

This test method covers the determination of the amount of carbon residue left
after evaporation and pyrolysis of an oil, and is intended to provide some indication
of relative coke-forming propensity. This test method is generally applicable to
relatively nonvolatile petroleum products that partially decompose on distillation at
atmospheric pressure. Petroleum products containing ash-forming constituents as
determined by Test Method D 482 will have an erroneously high carbon residue,

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depending upon the amount of ash formed. Values obtained by this test method are
not numerically the same as those obtained by Test Method D 189, or Test Method D
4530. Approximate correlations have been derived (Fig. 12) but need not apply to all
materials that can be tested because the carbon residue test is applicable to a wide
variety of petroleum products. The Ramsbottom Carbon Residue test method is
limited to those samples that are mobile below 90°C. In diesel fuel, the presence of
alkyl nitratessuch as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher
carbon residue value than observed in untreated fuel, which can lead to erroneous
conclusions as to the coke-forming propensity of the fuel. Test Method D 4046 can
detect the presence of alkyl nitrate in the fuel.

The carbon residue value of burner fuel serves as a rough approximation of

the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type
burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is
performed on the base fuel without additive) the carbon residue of diesel fuel
correlates approximately with combustion chamber deposits. The carbon residue
value of gas oil is useful as a guide in the manufacture of gas from gas oil. In a gas
turbine it can be an indication of the tendency to form carbon deposits in the
combustor.

One of the greatest problems encountered when using a compressor fluid is

the formation and accumulation of sludge, which can lead to a safety problem,
possibly even an explosive situation if coupled with overheating. This will occur if
sufficient quantities of carbon and sludge are formed to cause the valves to stick open
(Reference ISO 5388 part 6.6.1). Therefore, it is desirable to determine the sludge
forming potential of a compressor fluid. Conradson Carbon Residue (Test Method
D189).One method of quantifying the sludge-forming potential of a compressor fluid
involves determination of the Conradson carbon residue (Test Method D189), which
measures the amount of polymeric material remaining in the oil after heating to
elevated temperatures in the absence of sufficient oxygen to burn off all of the
organic compounds present. The Conradson carbon residue is determined by placing
a weighed sample in an iron crucible. The crucible is heated with a Meeker-type gas

2
burner to a sufficiently high temperature to evaporate and bum the oil. The sample is
further heated until the bottom and sides of the crucible are cherry red and is held at
this temperature for 30 min. The crucible is then cooled and weighed. The amount of
tar remaining in the crucible relative to the original amount of the oil define the
Conradson carbon residue value. Test Method D 189 may be affected by some
additives used to formulate the compressor fluid.

Ramsbottom Carbon Residue (Test Method D 524)—Another test that is used

to determine the tendency for a compressor lubricant to form carbonaceous residues is
Test Method D 524, the Ramsbottom Carbon Residue test. In this test, the sample,
after being weighed into a special glass bulb, is placed in a metal furnace and heated
to 550°C. In this way, the sample is quickly heated to the point where all volatile
material is evaporated out of the bulb, with or without decomposition, while the
remaining residue undergoes cracking and coking reactions. After the test, the bulb is
cooled and weighed. The residue remaining is reported as % of original sample and is
called the Ramsbottom Carbon Residue. "Micro Method" for Carbon Residue (Test
Method D 4530). In the "micro method," a weighed sample of the fluid is heated in a
2 mL glass vial at 500°C under an inert atmosphere (nitrogen) in a controlled manner
for a specific time. The sample undergoes coking reactions and the volatiles that are
formed are swept away by the nitrogen. The carbonaceous residue formed is reported
as % of original sample as "carbon residue (micro)." This test method is reported to
be equivalent to the Conradson Carbon Residue.

If lubricating oil is heated to a high temperature in an enclosure where there is

a limited supply of air, the greater part of the oil will be distilled and there will remain
a residue of carbon. The amount of this carbon residue in lubricating oil is an
indication of the extent of its decomposition when used for high-temperature
lubrication.

Carbon residue determinations are generally made by the method introduced

by Conradson and the apparatus being used consists of the following equipment:

1. Porcelain crucible glazed throughout, 25 to 26 cubic centimetre capacity, 46

millimetres in diameter.

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2. Skidmore iron crucible, 45 cubic centimetres capacity, 65 millimetres in diameter,
37 to 39 millimetres high with cover, without delivery tubes and one opening
closed.
3. Wrought iron crucible formed from spun sheet iron with cover, about 180 cubic
centimetres capacity, 80 millimetres in diameter, 58 to 60 millimetres high. At the
bottom of this crucible a layer of sand is placed about 10 millimetres deep or
sufficient to bring the Skidmore crucible with cover on, nearly to the top of the
wrought iron crucible.
4. Triangle, pipe stem covered, with a projection so as to follow the flame to reach
the crucible on all sides.
5. Sheet iron or asbestos hood provided with a chimney about 2 to 2 ½ inches high,
2 1/8 to 2 ¼ inches in diameter, to distribute the heat uniformly during the
process.
6. Asbestos or hollow sheet iron block (insulator), 6 to 7 inches square, 1 ¼ to 1 ½
inches high, provided with opening in the centre, 3 ¼ inches in diameter at the
bottom, and 3 ½ inches in diameter at the top.

To determine carbon residue by Conradson apparatus, the oil sample, in the

crucible, is heated at a state rate and caused to vaporize. After ignition and further
heating for a specified time, the residue is cooled and weighed. Duplicate tests should
agree within 10 per cent if the carbon residue is about 2 per cent or within 20 per cent
if the residue is above 0.5 per cent (see ASTM D-189).

For oils without detergency additives, carbon residue by the Conradson test is
a rough index of the tendency of the oil to decompose in service and to leave carbon
residue on hot surfaces.

In order to get accurate results, the dimensions of the apparatus used must be
as nearly as possible the same as those specified in this description. Special
precautions must be taken to observe the first appearance of vapours. In order to
make this observation as accurate as possible the gas burner may occasionally be
momentarily removed to facilitate this observation. If, at any time during the test the
vapours from the oil exceeds the 3-inch specification above the chimney of the hood,

4
 the gas burner may be removed for a short interval until the size of the gas flame can
be reduced sufficiently to keep the vapour flame about 2 inches above the top of the
chimney.

To solve for the Percentage of Carbon Residue:

Weight of Residue
% Carbon Residue= ×100 %
Weight of Lube Oil

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III. LIST OF APPARATUS

1. Conradson Apparatus
2. Meker Burner
3. Tripod
4. Wire Gauze/mesh
5. Chimney

6
IV. PROCEDURES
1. Measure the weight of the porcelain crucible. Make sure that the crucible is dry

and free from impurities.

2. Pour 10 grams of SAE 10 into the porcelain crucible.

3. Put the porcelain crucible inside the skidmore crucible. Then, put the skidmore

crucible inside the nickel crucible.

4. Cover the nickel crucible.

5. Put the wire triangle at the top of the tripod. Then, the refractory block insulator

ring on top of it.

6. Place the nickel crucible with the covers inside the refractory block insulator ring.

Then, put the carbon residue apparatus hood.

7. Set up the flame. Make sure that the flame is blue.

8. Start the timer after placing the burner below the center of the carbon residue

apparatus.

9. Wait until the smoke comes out of the carbon residue apparatus hood.

10. Stop the timer when the smoke is gone.

11. Remove the flame and let the crucible cool down.

12. Measure the weight of the porcelain crucible and compare it with the first
measurement.

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V. SET UP

Experiment Set-up as Stated by Instructor

Porcelain Crucibles with Covers and Hood

8
Actual Experimental Set-Up

Weighing of the Residue

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 VI. FINAL DATA SHEET

Percent
Weight of Weight of Weight of
SN Oil Specs Carbon Time
Crucible Lubricant Oil Residue
Residue

12 min 29
1-12 SAE40 21.76g 10g 0.0605g 0.605%
sec

9 min 25
13-25 SAE10 21.77g 10 0g 0%
sec

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VII. SAMPLE COMPUTATION

SAE10

Weight of Residue: 0 g

Weight of Lubricant Oil: 10 g

Weight of Residue
% Carbon Residue= ×100 %
Weight of Lube Oil

0g
% Carbon Residue= ×100 %
10 g

% Carbon Residue=0 %

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VIII. DISCUSSION OF RESULTS

The experiment was performed in the foundry using the Conradson apparatus.
The class performed each test oil, working on different lubricant oils. Morlina Oil- 10
Shell and Rev-X Diesel Engine Oil HD SAE40 were used as the lubricant oils in the
experiment.

The first group started with SAE40 and the next group used SAE10. The
procedure was uniform. After setting up the apparatus and recording all the necessary
measurements, the group started heating up the lube oil. After the gas was released,
we observed what happened inside the lube oil container.

Before the experiment, the professor said that one of the lubricant oils will
have 0% carbon residue. Proven by the experiment, it was found that the SAE10 oil
has 0% carbon residue. For SAE 40, however, results show that 0.67% carbon residue
was present, classifying it as Extra heavy-duty oil. Studies shows that SAE 40 is
considered heavy duty oil for having a range of 0.55% - 0.69% carbon residue must
have been obtained. There might be some error in our procedure. We also noticed that
the time recorded for SAE10 is much less than the time for SAE40. It only shows that
it is easier to burn SAE10 compared to SAE40. This may account to the viscosity of
the lubricant oils.

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IX. QUESTIONS AND ANSWERS
1. How many methods to calculate carbon residue?

There are three methods to calculate carbon residue. It may be expressed as Rams
bottom Carbon Residue(RCR), Conradson Carbon Residue(CCR) or Micro Carbon
Residue(MCR). Numerically, the CCR value is the same as that of MCR. Sometimes
the carbon residue value can be listed as Residual Carbon Content, RCC, which is
normally the same as MCR/CCR.

2. What are the disadvantages of carbon residues on engines?

It causes erosion and corrosion of the internal parts of the engines.

3. The value of carbon residue of a fuel depends on what?

The carbon residue value of a fuel depends on the refinery processes employed in
its manufacture. For straight run fuels, the value is typically 10-12% m/m, while for fuels
from secondary refining processing the value depends on the severity of the processes
applied. In some areas it can be as high as 20% m/m.

4. Differentiate octane rating and cetane rating.

Cetane number (diesel fuel) and octane number (gasoline) both measure the

tendency of the fuel to ignite spontaneously. In the cetane number scale, high values

represent fuelsthat ignite readily and, therefore, perform better in a diesel engine. In

the octane number scale, high values represent fuels that resist spontaneous ignition

and, therefore, have less tendency to knock in a gasoline engine. Because both scales

were developed so that higher numbers represent higher quality for the respective use,

high cetane number fuels have low octane numbers, and vice versa.

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5. Define cracking in the petroleum industry.

Cracking splits larger molecules into smaller ones, or breaks the bonds of a

larger, more complex material into smaller matter. Cracking can be done in a variety

of methods, including hydrocracking, fluid catalytic cracking and steam cracking.

6. What is carbon residue?

Carbon residue is the residue formed by evaporation and thermal degradation

of a carbon containing material. The residue is not composed entirely of carbon but is
a coke that can be further changed by carbon pyrolysis.

7. What is the importance of the carbon residue number?

The carbon residue value of burner fuel serves as a rough approximation of

the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type
burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is
performed on the base fuel without additive) the carbon residue of diesel fuel
correlates approximately with combustion chamber deposits. The carbon residue
value of gas oil is useful as a guide in the manufacture of gas from gas oil. In a gas
turbine it can be an indication of the tendency to form carbon deposits in the
combustor.

8. What is the formula to solve for the carbon residue of a lubricant or fuel when
using the Conradson Method?

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 The formula used for the Conradson Method is:

Weight of Residue
% Carbon Residue= ×100 %
Weight of Lube Oil

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X. CONCLUSION

In this experiment we were able to determine the carbon residue and the
percent carbon residue of lubricating oil. The same weight of different types of oil we
used and burn it until all the test samples of lubricant were all burn up. The result of
the experiment shows that the SAE 40 produce the higher percentage of carbon
residue. The carbon residue indicates the extent of its decomposition when used for
high-temperature lubrication.

We used the Conradson’s carbon residue test. Conradson’s carbon residue test
is used for finding out the amount of carbon to be released by lubricating oil.
Lubricating oils contain high percentage of carbon in combined form. On heating the
decompose deposits a certain amount of carbon, the deposits of such carbon in the
machine is intolerable. A good lubricant should deposit least amount of carbon in use.
The apparatus consists of a silica crucible, skid more iron crucible and wrought iron
crucible, a chimney and a tripod stand. The crucible is heated by means of Bunsen
burner.

The possible sources of error in this experiment are the collecting of the
residue, weighing of the crucible as well as the oil. The inaccurate measurement will
cause a small defect or error in terms of the percent carbon residue computation.
Aside from this, there are also errors such as spilling of carbon residue after burning
which may cause the percentage of carbon residue to change by just a little.

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XI. REFERENCE/S
 http://www.cpeo.org/techtree/ttdescript/pyrols.htm

 http://www.frtr.gov/matrix2/section4/4-25.html

 http://en.wikipedia.org/wiki/Pyrolysis#Biochar

 http://en.wikipedia.org/wiki/Ramsbottom_Carbon_Residue

 http://global.britannica.com/EBchecked/topic/122944/coal-utilization

 http://en.wikipedia.org/wiki/Cetane_number

 http://nzic.org.nz/ChemProcesses/energy/7B.pdf

 http://www.wisegeek.com/what-is-carbon-residue.htm

 http://www.mandieselturbo.de/files/news/filesof9981/5510-0041-01ppr.pdf
 http://www.ags.gov.ab.ca/publications/INF/PDF/INF_001.pdf

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