Chapter03 - Lab Tests
Chapter03 - Lab Tests
Chapter03 - Lab Tests
Atm Distillation
Vac Distillation
API & specific gravity
BS&W
Octane Number (Motor/Research)
Molecular Weight
RVP
Lamp Sulfur
Doctor test
Flash point
Freezing point
Smoke point
Viscosity (Saybolt universal)
Viscosity (Kinematic)
Pour point
Cloud Point
Color (clear liquids)
PNA/PINA/ PONA/PIONA
Refractive Index (RI)
Aniline point
Cetane Index
Cetane number
Conradson carbon
Ramsbottom carbon
H/C ratio
Heating value (net/gross)
Flammability Limits (upper/lower)
Salt, PTB
Page
No.
D 86
D 1160
D287-92
D 96-88
D 357/D 908
D2503
D323-94
D1266
D325
D56-97A
D2386
D1322
D88
D445
D97-96a
D2500
D1209-93
D544393
D1218-92
D611
D976
D613
D189-97
D524
D5291
D240/D4809
E681
D3230/D6470
KOEHLER INSTRUMENTS
http://www.koehlerinstrument.com/index.html
FXG
http://fxg-ent.com/
GECIL
http://www.gecil.com/index.php?pageID=74
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Objective:
To determine the API gravity of crude petroleum and petroleum products normally
handled as liquids and having a Reid vapor pressure of 26 psi or less and at constant
temperature of 60 F.
Procedure
The temperature of the sample is adjusted according to the type of sample.
The sample is then transferred into the clean hydrometer cylinder (volatile samples
are transferred by siphoning)
The hydrometer is lowered gently into the sample and when it has settled, depressed
about two scales divisions into the liquid and released.
When the hydrometer has come to the rest, floating freely and the temperature of the
sample is constant to 0.2 F the hydrometer reading is recorded.
Related Standards
D70
Specific gravity of bituminous materials, Pycnometer Method
D287
API Gravity of Crude Petroleum & Petroleum Products (Hydrometer
D1070
Specific gravity of gaseous fuels
D1298
Density, Specific Gravity or API, Hydrometer Method
D1657
Density of LPG, hydrometer method
D4052
Oscillating frequency, Digital Density Meter
SG API
141.5
131.5
ASTM distillation
Sample: Crude oil & Light to medium fractions
Standard Test Number: ASTM D86-96, D1160
Principle: physical separation (vaporization)
Scope
This test method covers the distillation of natural gasoline, motor gasoline, aviation
gasoline, aviation turbine fuels, special boiling point spirits, naphtha, white spirit
kerosene, gas oils, distillate fuel oils and similar petroleum products, utilizing either
manual or automated equipment.
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
T (F)
100
106
112
122
130
139
148
157
166
185
194
202
205
98 %
Related standards:
Table 3.3: Standard test methods for distillation of petroleum products
ASTM test
Application
#
1. D86-96
Light petroleum fractions (naphtha, kerosene, diesel)
2. D1160
Heavy petroleum fractions (VGO, atm residue, vac residue)
3. D2887
Simulated Distillation (GC method); TBP of petroleum frac. other than gasoline
4. D3710
Simulated Distillation (GC method); TBP of gasoline
5. D5307
Simulated Distillation (GC method); TBP of crude oil.
6. D6352-98
Simulated Distillation (GC method); TBP of distillates (BP range 174 to 700C)
7. D2892
15/5 distillation; 15theoretical plate column (simulated TBP)
8. D5236
Distillation of heavy HC mixtures (Vacuum Potstill Method)
Notes:
1. Tests 1 & 2 may be combined together for wide boiling range materials.
2. Test 2 is used for fractions heavier than diesel.
3. Test 3 can replace test 1 for white products (namely gasoline, Naphtha, and kerosene).
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
.
Centrifuge
Tube
Related Standards
D95 (water in petroleum products and bituminous products by azeotropic distillation)
D473 (Sediment in crude oil and fuel oil by extraction)
D1744 (water by Karl Fischer Method electrometric, after addition of KF reagent)
D1796 (water and sediment in fuel oils, mix with toluene and centrifuge)
D2709 (Water and Sediment in Distillate Fuels by Centrifuge)
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Octane Number
Sample: gasoline
Standard Test Number: ASTM D357 (Motor)
D908 (Research)
Principle: Combustion in a variable compression ratio motor.
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Compression Ratio
The ratio of the maximum to minimum volume in the cylinder of an internal-combustion
engine.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
n-heptane
Iso-octane (2,2,4-trimethylpentane)
Octane rating does not relate to the energy content of the fuel (that is the heating value). It is
only a measure of the fuel's tendency to burn rather than explode.
Octane rating does not mean better power output or fuel economy or cleaner burning. It is
only a measure of the fuels combustion quality. Since switching to a higher octane fuel does
not add any more hydrocarbon content or oxygen, the engine cannot produce more power.
120
pure
isooctane
100
Octane Number
80
60
pure
n-heptane
40
20
0
-20
-20
20
40
60
80
100
120
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under controlled conditions, and comparing the results with those for mixtures of iso-octane
and n-heptane.
There is another type of octane rating, called Motor Octane Number (MON) or the aviation
lean octane rating, which is a better measure of how the fuel behaves when under load. MON
testing uses a similar test engine to that used in RON testing, but with a preheated fuel
mixture, a higher engine speed, and variable ignition timing to further stress the fuel's knock
resistance. Depending on the composition of the fuel, the MON of a modern gasoline will be
about 8 to 10 points lower than the RON. Normally fuel specifications require both a
minimum RON and a minimum MON.
Regional variations
Generally, octane ratings are higher in Europe than they are in North America and most other
parts of the world. This is especially true when comparing the lowest available octane level in
each country.
Country
Octane number
Many parts of Europe
95 RON (90-91 AKI) and 97/98
United Kingdom
95 RON, 97 RON, 99 RON, 102 RON
Germany
100 RON
Australia
91 RON, 95 RON, 98 RON, 100 RON
Malaysia
92 RON, 97 RON, 99 RON
In other countries
85 RON, 95 RON, 98 RON
Russia and CIS countries
76 MON, 80 RON
In most countries (including all of Europe and Australia) the "headline" octane rating, shown
on the pump, is the RON, but in the United States, Canada and some other countries the
headline number is the average of the RON and the MON, sometimes called the Anti-Knock
Index (AKI), Road Octane Number (RdON), posted octane number, Pump Octane Number
(PON), or (R+M)/2. Because of the 8 to 10 point difference noted above, the octane shown in
the United States is 4 to 5 points lower than the same fuel elsewhere: 87 octane fuel, the
"regular" gasoline in the US and Canada, is 91-92 in Europe. However most European pumps
deliver 95 (RON) as "regular", equivalent to 90-91 US (R+M)/2, and some even deliver 98
(RON) or 100 (RON).
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
It is possible for a fuel to have a RON greater than 100, because iso-octane is not the most
knock-resistant substance available. Racing fuels, AvGas, LPG, and alcohol fuels such as
methanol or ethanol can have octane ratings of 110 or significantly higher - ethanol's RON is
129 (MON 102, AKI 116).
Typical "octane booster" gasoline additives include tetra-ethyl lead, MTBE and toluene.
Tetra-ethyl lead (the additive used in leaded gasoline) is easily decomposed to its component
radicals, which react with the radicals from the fuel and oxygen that start the combustion,
thereby delaying ignition, leading to an increased octane number.
Examples of octane ratings
For some other hydrocarbons, the following table gives the 'AKI' ratings.
Compound
ON
Compound
ON
Compound
hexadecane
< -30
1-pentene
84
methanol
n-octane
-10
n-butanol
87
toluene
n-heptane
0
E10 gasoline
8790
ethanol
diesel fuel
1525 n-butane
91
xylene
2-methylheptane
23
t-butanol
97
E85 gasoline
n-hexane
25
cyclohexane
97
methane
2-methylhexane
44
iso-octane
100
ethane
1-heptene
60
benzene
101
n-pentane
62
propane
103
ON
113
114
116
117
105
107
108
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
16
The apparatus is withdrawn from the bath and the procedure is repeated as needed.
The (uncorrected) RVP reading is recorded when the difference between two readings
is 0.05psi.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Related Standards:
D129 (Bomb Method; for heavy petroleum fractions; oxidation in pressurized bomb
and gravimetric analysis)
D325 (Doctor Test, detection of H2S and mercaptans Sodium plumnite test,
coloration of interface)
D1552 (combustion in high temperature, induction furnace, and analysis)
D1072 (Total Sulfur in Fuel Gases)
D2622 (X-ray Spectrographic)
D2784 (sulfur in LPG; combustion in lamp and analysis of sulfur oxides formed)
D2785 (combustion in Wickbold burner and analysis)
D3120 (Trace quantities of Sulfur in Light petroleum hydrocarbons by Oxidative
Microcoulometry)
D3227 (Mercaptan Sulfur in Destillate Fuels, Potentiometric method?-silver nitrate
analysis?)
D4294 (Non-dispersive X-ray fluorescence)
ASTM D703915 (Standard Test Method for Sulfur in Gasoline, Diesel Fuel, Jet
Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol Blends by
Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry)
Flash point
Sample: gasoline, naphtha, kerosene, diesel, and others
Standard Test Number: ASTM D56-97a (Tag closed tester)
Definition:
Flash point is the lowest temperature, corrected to a pressure of 101.3 kpa (760
mmHg), at which application of an ignition source causes the vapors of a specimen of
the sample to ignite.
The specimen is deemed to have flashed when a flame appears and instantaneously
propagates itself over the entire surface of the fluid.
Significance
It is affected by the amount of light materials present the fraction. This is very important
for the safe handling of petroleum products (transfer and storage) and ease of ignition of
fuel.
High flash point means higher temperature is required for the fuel to flash.
The fuel therefore does not ignite easily and is safe.
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There are two basic types of flash point measurement of a substance or fuel: open cup and
closed cup, which differ according to the characteristics of the liquid under study. Standard
ASTM (2002) closed-cup test methods include Tag (D56-01), small scale (D3828-98),
Setaflash (D3828), Pensky-Martens (D93-00), and the equilibrium method (D3941-90).
Standard ASTM (2002) open-cup test methods include Cleveland (D92-01) and Tag (D1310).
Generally closed cup testers normally give lower values for the flash point than open cup
(typically 510 C or 918 F lower).
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Tag
closed cup
flash tester
Pensky-Martens closedcup
flash tester
Cleveland
open-cup
flash tester
Rapid Flash
Closed-Cup
flash tester
Tag
Open-Cup
Flash Tester
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Fully Automatic
Setaflash
Significance
In aircraft, the temperature of the fuel tank normally falls during flight depending on
aircraft speed, altitude and flight duration. So, the freezing point of the fuel must always be
lower than the minimum operational tank temperature.
Apparatus:
The apparatus consists of jacketed sample tube, unsilvered vessel, sample tube,
collers, stirrer, vacuum flask and thermometer.
Procedure:
A 25 ml of the fuel is transferred to the dry, jacketed tube. The tube is closed
tightly with cork holding the stirrer, thermometer and moisture proof color.
The thermometer is adjusted in the tube and its bulb not touching the walls.
The jacketed sample tube and its set are clamped in the vacuum flask containing
the coolant as for as possible.
Solid carbon dioxide is added to maintain the coolant level in the vacuum flask.
The fuel sample is stirred continuously at rate 1.5 cycles/s.
The temperature at which crystals of hydrocarbon appear is recorded.
The jacketed sample tube is removed from the coolant, warmed then stirred.
The temperature at which the crystals completely disappear is recorded.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
A sample is filtered at a temperature at least 14C above the expected cloud point
until oil is perfectly clear.
The sample is then poured into the test jar to the level mark.
The test jar is tightly closed by the cork carrying the test thermometer then placed
in a jacket into a cooling medium maintained at about 0 C.
At every thermometer reading increment of 1C the test jar is removed from the
jacket and inspected for cloud and replaced in the jacket (in not more than 3 sec).
The oil is transferred to a lower temperature bath if it does not show a cloud at the
lowest temperature as shown in Table 1.
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The specimen is poured to the level mark into a test jar having a cork holding a
thermometer.
The specimen is heated without stirring to 9C above the expected pour point (or 45C
whichever is higher) in a bath maintained at 12 C above the expected pour point (or
48C whichever is higher).
The test jar is transferred to a water bath maintained at a lower temperature to cool the
sample and is observed for pour point.
Care is taken as not to disturb the specimen as paraffin wax crystals are formed after
cooling the specimen.
The jar is then tilted to check for movement of the specimen.
If the specimen still flows when its temperature reaches 27C the jar is transferred
from one bath to another with a lower temperature until the specimen in the test jar
does not flow when tilted.
The jar is then held in a horizontal position for 5 seconds. If the specimen shows any
movement, the test jar is replaced in the jacket and the test is repeated for flow at the
next temperature 3C lower.
This is continued until the specimen in the jar does not move and temperature is
reported as the pour point.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
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Viscosity
Sample: All
Standard Test Number: D445
ASTM D445: Standard Test Method for Kinematic Viscosity of Transparent and Opaque
Liquids (the Calculation of Dynamic Viscosity)
Principle: Measurement of time required to flow between 2 marks in a tube
Objective
To determine the kinematic viscosity, , of both transparent and opaque petroleum
products.
To calculate the dynamic viscosity using kinematic viscosity.
Definition
The dynamic viscosity is a ratio between the applied shear stress and the rate of shear
of the liquid.
The Kinematic viscosity is the resistance of fluid flowing under gravity.
Kinematic viscosity is determined by measuring the time of a fixed volume of fluid
takes to flow under gravity through a capillary viscometer.
The kinematic viscosity is directly proportional to the dynamic viscosity as described
by the following equation
= /
where:
=C.t
C= Viscometer constant
Apparatus
The apparatus consists of a viscometer, viscometer holder, temperature control bath,
temperature controller, temperature measuring device and timing device.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Procedure
For transparent products; a viscometer bath is maintained at a required test
temperature.
The viscometer is charged and placed in the bath where it is maintained until its
temperature reaches the test temperature.
Once it reaches the test temperature the level of the sample in the viscometer is
marked.
The head level is adjusted to a position 7 mm above the first mark. The time taken by
the fluid to reach the new position is measured.
For Opaque Products; the test sample is first heated and stirred until it becomes
sufficiently fluid then introduced in the viscometer which is placed in the viscometer
bath.
Usually measured at a certain temperature depending on sample (commonly 122 or
210 F)
Types;
1. Kinematic Viscosity, Centistokes (cSt). [= mm2/s]
2. Saybolt Universal Seconds (SUS).
3. Saybolt Furol Seconds (SFS)
Related standards:
D88 (Saybolt Viscosity)
D341-93 (viscosity temperature chart)
D2270 (Viscosity index, calculation based on kinematic viscosity)
D2983 (Viscosity Brookfield, rotation of a bob in a sample)
ASTM D446-07 (Standard Specifications and Operating Instructions for Glass Capillary
Kinematic Viscometers)
D2161 (Conversion of Kinematic viscosity to Saybolt Universal Viscosity or to Saybolt Furol
Viscosity)
Color
Sample: Clear liquids, mostly diesel.
Standard Test Number: D1209-93
D1209-93: Standard test method for color of clear liquids (Platinum-cobalt scale)
Significance
The presence of color in material gives an indication
of the degree of refinement of solution or the
cleanliness of the of the storage container that is
handled. It applies to materials in which the color
producing bodies have light absorption
characteristics close to those of the platinum cobalt
color standards used.
Procedure
A 100 ml of sample is introduced in to a Nessler tube (after filtration if there is visible
turbidity).
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
Definition:
Aniline point is defined as the minimum equilibrium solution temperature for equal
volume of aniline sample.
The mixed aniline point is the minimum equilibrium solution temperature for a
mixture of two volumes of aniline.
Method A (for clear sample)
Apparatus
The apparatus consists of test tube, jacket tube, stirrer and thermometer.
Procedure
Equal amount of aniline and the dried sample is introduced in a test tube, placed in the
center of a jacket tube.
The mixture is stirred rapidly until it becomes homogeneous.
If the mixture is not miscible at room temperature heat is applied to the jacket tube.
The temperature is raised with a continuous stirring until the dried sample becomes
miscible.
Then the stirrer is stopped and the mixture is cooled.
The point at which the mixture becomes cloudy is the aniline point.
Method B (for light, intermediate and vary dark samples)
Method C (for clear sample with low IBP)
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Cetane number
Sample: Diesel
Standard Test Number: D613
ASTM D613-01 Standard Test Method for Cetane Number of Diesel Fuel Oil.
Scope:
This test method determines the rating of diesel fuel oil in terms of an arbitrary scale of
Cetane numbers using standard single cylinder, four-stroke cycle, variable compression ratio,
and indirect injected diesel engine.
Significance:
The cetane number provides a measure of ignition characteristics of diesel fuel oil in
compression ignition engines.
Diesel Ignition quality
Very similar to the octane number.
Compares the degree of combustion of diesel fuel to that of a mixture of cetane
(C16H34, high-ignition quality) and alpha-methyl-naphthalene (C11 H10, low ignition
quality) expressed as V% cetane.
The fuel is used to operate a standard diesel test engine.
Related standards
ASTM D6890 13: Standard Test Method for Determination of Ignition Delay and Derived
Cetane Number (DCN) of Diesel Fuel Oils by Combustion in a Constant Volume Chamber
Cetane number or CN is a measure of the combustion quality of diesel fuel via the
compression ignition process. Cetane number is a significant expression of diesel fuel quality.
Cetane number of a fuel is defined as the percentage by volume of normal cetane in a mixture
of normal cetane and alpha-methyl napthalene which has the same ignition characteristics
(ignition delay) as the test fuel when combustion is carried out in a standard engine under
specified operating conditions.
Cetane number is actually a measure of a fuel's ignition delay; the time-period between the
start of injection and start of combustion (ignition) of the fuel. In a particular diesel engine,
higher cetane fuels will have shorter ignition delay periods than lower cetane fuels. Cetane
numbers are only used for the relatively light distillate diesel oils. For heavy (residual) fuel
oil two other scales are used CCAI and CII.
Generally, diesel engines run well with a CN from 40 to 55. Fuels with higher cetane number
which have shorter ignition delays provide more time for the fuel combustion process to be
completed. Hence, higher speed diesels operate more effectively with higher cetane number
fuels. There is no performance or emission advantage when the CN is raised past
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
approximately 55; after this point, the fuel's performance hits a plateau. In North America,
diesel at the pump can be found in two CN ranges: 40-46 for regular diesel, and 45-50 for
premium. Premium diesel may have additives to improve CN and lubricity, detergents to
clean the fuel injectors and minimize carbon deposits, water dispersants, and other additives
depending on geographical and seasonal needs. In Europe, diesel Cetane numbers was set at a
minimum of 51 in 2000.
Chemical relevance
Cetane is an alkane molecule that ignites very easily under compression, so it was assigned a
Cetane number of 100. All other hydrocarbons in diesel fuel are indexed to Cetane as to how
well they ignite under compression. The Cetane number therefore measures how quickly the
fuel starts to burn (auto-ignites) under diesel engine conditions. Since there are hundreds of
components in diesel fuel, with each having a different Cetane quality, the overall Cetane
number of the diesel is the average Cetane quality of all the components. There is very little
actual Cetane in diesel fuel.
Measuring Cetane number
To measure Cetane number properly is rather difficult, as it requires burning the fuel in a
special, hard-to-find, diesel engine called a Cooperative Fuel Research (CFR) engine, under
standard test conditions. The operator of the CFR engine uses a hand-wheel to increase the
pressure within the cylinder of the engine until the time between fuel injection and ignition is
2.407ms. The resulting Cetane number is then calculated by determining which mixture of
Cetane (hexadecane) and alpha-methyl napthalene will result in the same ignition delay.
Cetane Index
Sample: Distillate fuels
Standard Test Number: ASTM D976
ASTM D976: Calculated Cetane Index of Distillate Fuels
Sometimes Cetane Index is erroneously referred to as Diesel Index
Another method that fuel-users control quality is by using the Cetane index (CI), which is a
calculated number based on the density and distillation range of the fuel. There are various
versions of this, depending on whether you use metric or imperial units, and how many
distillation points are used. These days most oil companies use the '4-point method'.
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Since cetane index is an indicator of the H/C ratio, it is also an indication of the
aromatic content of the diesel fuel. Therefore, frequently a minimum cetane index
specification is used as an alternative to max aromatic content.
This is not to be confused with the Watson (UOP) characterization factor or the US
Bureau of Mines Correlation index (CI)
Significance
The calculated Cetane index formula represents a means for directly estimating ASTM
Cetane number of distillate fuels from API gravity and mid-boiling point.
Equations for calculated Cetane Index
In British units
CI = 420.34 + 0.016G2 + 0.192G log M + 65.01(log M)2 0.0001809 M2
In SI units
CI = 454.74 1641.416 D + 774.74 D2 0.554 B + 97.803(log B)2
Where:
G = API gravity.
M = MiDboiling temperature, F.
D = Density at 15 C, g/ml.
B = MiDboiling temperature, C
Limitations:
1. Cannot be applied for fuels containing additives for raising Cetane number.
2. Cannot be applied for pure hydrocarbons such as products derived from shale oils and
tar sands.
3. Substantial inaccurate in correlation may occur if used for crude oil, residuals or
products having volatility of below 500 F end point. However,
Related Standards:
D4737 (Standard Test Method for Calculated Cetane Index by Four Variable Equation)
Related Standards
ASTM D189-06 Standard Test Method for Conradson carbon residue of Petroleum
Products
ASTM D524-04 Standard Test Method for Ramsbottom carbon residue of Petroleum
Products
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D4530-06e1 Standard Test Method for determination of carbon residue (Micro
Method) - The test results are equivalent to the Conradson Carbon Residue test (see
Test Method D 189)
Conradson carbon
Sample: crude oil and heavier fractions.
Standard Test Number: D18997
D18997: Standard Test Method for Conradson Carbon Residue of Petroleum Products
Objective
To determination the amount of carbon residue left after evaporation and pyrolysis of
oil.
It is applicable to relatively nonvolatile petroleum products (heavy) which partially
decompose on distillation at atmospheric pressure.
Procedure
A sample is heated to about 50 C and shaken for 30 min. then filtered through a mesh
screen.
A 10 g sample is weighed (free of moisture & suspended matter) into a tarred
porcelain or silica crucible containing 2 glass beads 2.5 mm in diameter.
The crucible is placed in the center of skidmore crucible which is set at the center of
the iron crucible and covers are applied to both of skidmore & iron crucible.
A strong flame is applied from meker-type gas burner to have high heat for a period
of 10 min.
When smoke appears form the chimney the burner is moved or tilted to ignite the
vapor then removed temporarily.
When the vapors cease to burn the heat is reapplied until the bottom of the sheet iron
crucible is cherry red.
The burner is removed and the apparatus is cooled until no smoke appears then the
cover of skidmore crucible is removed (about 15 min)
The porcelain or silica crucible is removed and placed in the desiccators, cooled and
weighed and the % of carbon residue is calculated based on the original sample.
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Calculation
Carbon residue = A 100 / W
Where
A = Mass of carbon residue in g
W = Mass of sample in g
Ramsbottom carbon
Sample: crude oil and heavier fractions.
Test Number: ASTM D524
ASTM D524: Ramsbottom Carbon Residue of Petroleum Products
Objective
The objective of this test is to determine the amount of residue resulting from
evaporation and pyrolysis of oil.
Significance
Provides an indication of oil tendency toward coke formation.
Apparatus
The apparatus consists of a glass-coking bulb, control bulb, sample charging syringe,
metal control furnace and temperature measuring device.
Procedure
A new glass-coking bulb is placed in the coking furnace that operates at 550 F for
about 20 min to remove any water, foreign or organic matters then dried in a closed
dissector.
The sample is weighed, heated if necessary to reduce it viscosity then introduced in
the coking bulb by means of hypodermic syringe.
The coking bulb is weighed before placing it in the metal coking furnace.
The sample is kept in the furnace at 550 F for about 20 min to vaporize the volatile
materials and allow the heavier residue to undergo cracking and coke formation.
The bulb is then taken out, cooled in the dissector and weighed.
The carbon residue is calculated by the same equation used in conradson carbon test.
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Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
C/H ratio
Sample:
Standard Test Number:
D5291-96: Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants
D5373: Carbon-hydrogen-nitrogen determination
D1018 11: Standard Test Method for Hydrogen In Petroleum Fractions
D7171 05: Standard Test Method for Hydrogen Content of Middle Distillate Petroleum Products by Low-Resolution
Pulsed Nuclear Magnetic Resonance Spectroscopy
Hydrocarbon type
Sample:
Standard Test Number:
Principle:
Related Standards
D1319 (HC groups, Chromatography on silica gel, Fluorescence indicator Absorption)
D2007 (Hydrocarbon families, Chromatography on clay and silica gel)
Aromatics Content
Sample: kerosene and gasoline
Related Standards
D2267 (Aromatics in light naphthas, and aviation gasolines by GC)
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Nitrogen Content
High Nitrogen Content is undesirable in crude oils.
Organic nitrogen compounds cause catalyst poisoning in refinery downstream
processing units.
Crude containing nitrogen more than 0.25 W% require special processing to remove
Nitrogen.
That is usually done in the hydrodesulfurization units where denitrification catalysts
are also added.
Metals content
These are Nickel / Vanadium / Copper.
Range from few to more than 1,000 ppmw.
Even low concentrations are undesirable
- They can cause catalyst deactivation/poisoning.
- Can affect selectivity producing poor product distribution.
- Can lead to corrosion problems;
1. More than 2ppm Vanadium in fuel oils causes sever corrosion to turbine
blades.
2. Deterioration of Furnace refractory linings and stacks.
Distillation concentrates the metallic constituents of crude in the residue, but some of
the organometallic compounds are actually volatilized and appear in the high-boiling
distillates (i.e. diesel and gasoil).
Desalting, in the oilfields and the refinery CDU, gets red of metals as a bonus along
with salt and water.
Metallic content can also be reduced by solvent extraction with propane or similar
solvents as the organometallic compounds are precipitated with the asphaltenes and
resins.
Heating Value
Sample: All
Standard Test Number: D240-14
Related Standards
ASTM D240 14: Standard Test Method for Heat of Combustion of Liquid Hydrocarbon
Fuels by Bomb Calorimeter
37
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D4809 13: Standard Test Method for Heat of Combustion of Liquid Hydrocarbon
Fuels by Bomb Calorimeter (Precision Method)
ASTM D1826 - 94(2010): Standard Test Method for Calorific (Heating) Value of Gases in
Natural Gas Range by Continuous Recording Calorimeter
ASTM D2015: Standard Test Method for Gross Calorific. Value of Solid Fuel by the
Adiabatic Bomb Calorimeter.
ASTM D3523 - 92(2012): Standard Test Method for Spontaneous Heating Values of Liquids
and Solids (Differential Mackey Test)
ASTM D4891 13: Standard Test Method for Heating Value of Gases in Natural Gas and
Flare Gases Range by Stoichiometric Combustion
ASTM D7314 10: Standard Practice for Determination of the Heating Value of Gaseous
Fuels using Calorimetry and On-line/At-line Sampling
ASTM E711-87(2004): Standard Test Method for Gross Calorific Value of Refuse-Derived
Fuel by the Bomb Calorimeter (Withdrawn 2004)
DIN 51612, testing of liquefied petroleum gases (LPG) and calculation of net calorific value
DIN 51857, testing of gaseous fuel - calculation of calorific value, density , relative density
and wobbe index
Flammability Limits
Sample: All
Standard Test Number: E681
Related Standards
ASTM E681 - 09(2015): Standard Test Method for Concentration Limits of Flammability of
Chemicals (Vapors and Gases)
38
References
1. ASTM Manual on Hydrocarbon Analysis, 6th edition, A.W. Drews, editor , West
Conshohocken, PA 1998. (TP 691 M358 1998)
2. ASTM Manual on Significance of Tests for Petroleum Products, 5th ed., George V.
Dryoff editor, Philadelphia, PA, 1989. (TP 691 M36 1989)
3. ASTM standards for testing (TA736 A736 1990)
4. Arthur, I. Vogel, Quantitative chemical Analysis (QD101.2 V63 1989)
Term Paper
Each student assigned an ASTM designation must:
1. Find the ASTM procedure from the library or the internet
2. Present a legible Xerox copy of the procedure.
3. Summarize the procedure in the same manner and format as above.
4. Present a typed copy of the summary both on paper and on floppy disk.
5. Computer/hand sketch to simplify difficult drawings or obtain simple drawings from
other references.
6. Staple each test alone with you name and test name and number on the cover sheet.
7. You may not require any assistance from the TA.
39
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
40
ASTM C117
ASTM C136
ASTM C566
ASTM D56
ASTM D86
ASTM D87
ASTM D91
ASTM D92
ASTM D93
ASTM D94
ASTM D95
ASTM D96
ASTM D97
ASTM D127
ASTM D128
ASTM D129
ASTM D130
ASTM Description
Determination of Materials Finer
than 75um (no. 200) Sieve in
Mineral Aggregates by Washing
Sieve Analysis of Course and Fine
Aggregates
Total Evaporable Moisture Content
of Aggregate by Drying
Flash Point by Tag Closed Tester
Common Reference
41
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D156
ASTM D189
ASTM D217
ASTM D240
ASTM D287
ASTM D322
ASTM D323
ASTM D381
ASTM D396
ASTM D439
ASTM D445
ASTM D471
ASTM D473
ASTM D482
ASTM D483
ASTM D524
ASTM D525
ASTM D566
42
ASTM D611
ASTM D613
Cetane No.
ASTM D664
ASTM D665
ASTM D721
ASTM D808
ASTM D854
ASTM D874
ASTM D892
ASTM D893
ASTM D924
ASTM D937
ASTM D938
ASTM D943
ASTM D971
ASTM D972
ASTM D974
ASTM D975
ASTM D976
Rust-Preventing Characteristics of
Inhibited Mineral Oil in the
Presence of Water
Oil Content of Petroleum Waxes
43
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D1067
ASTM D1119
ASTM D1120
ASTM D1121
ASTM D1122
ASTM D1123
ASTM D1133
ASTM D1160
ASTM D1177
ASTM D1217
ASTM D1218
ASTM D1275
ASTM D1287
ASTM D1293
ASTM D1298
Hardness in Water
Kauri Butanol Value of
Hydrocarbon Solvents
Vacuum Distillation of Petroleum
Products
Refractive Index and Refractive
Freezing Point of Aqueous Engine
Dispersion of Hydrocarbon
Coolants
Liquids
Density and Relative Density
Density and Relative Density
(Specific Gravity) of Liquids by
(Specific Gravity) of Liquids by
Bingham Pycnometer
Pycnometer
Refractive Index and Refractive
Refractive Index and Refractive
Dispersion of Hydrocarbon
Dispersion of Hydrocarbon Liquids
Liquids
Corrosive Sulfur in Electrical
Corrosive Sulfur in Electrical
Insulating Oils
Insulating Oils
The pH of Engine Coolants and
pH of Antifreeze
Antirusts
pH of Water
pH of Water
Density, Relative Density (Specific
Gravity), or API Gravity of Crude Density, Specific Gravity and API
Petroleum and Liquid Petroleum
Gravity by Hydrometer
Products by Hydrometer Method
44
ASTM D1319
ASTM D1321
ASTM D1384
ASTM D1401
ASTM D1403
ASTM D1480
ASTM D1481
ASTM D1500
ASTM D1662
ASTM D1747
ASTM D1796
ASTM D1832
ASTM D1835
ASTM D1837
ASTM D1881
Hydrocarbon Types by
Fluorescent Indicator Absorption
Needle Penetration
Corrosion in Glassware
Demulsibility
Quarter Scale Cone Penetration
Density and Relative Density
(Specific Gravity) of Viscous
Materials by Pycnometer
Density and Relative Density
(Specific Gravity) of Viscous
Materials by Lipkin Bicapillary
Pycnometer
Color, ASTM
Active Sulfur in Cutting Oils
Refractive Index
Water and Sediment
ASTM D1882
ASTM D1959
45
Iodine Value
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D2007
ASTM D2008
ASTM D2158
ASTM D2161
ASTM D2163
ASTM D2257
ASTM D2265
ASTM D2266
ASTM D2270
ASTM D2272
ASTM D2273
ASTM D2386
ASTM D2500
Cloud Point
ASTM D2501
Calculation of Viscosity-Gravity
Constant (VGC) of Petroleum Oils
ASTM D2274
46
ASTM D2509
ASTM D2533
ASTM D2549
ASTM D2570
ASTM D2596
ASTM D2602
ASTM D2619
ASTM D2669
ASTM D2699
ASTM D2700
ASTM D2709
ASTM D2766
ASTM D2782
Hydrolytic Stability
(Discontinued)
Hydrolytic Stability
Measurement of Extreme-Pressure
Properties of Lubricating Fluids
(Timken Method)
47
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D2783
Measurement of Extreme-Pressure
Properties of Lubricating Fluids
(Four-Ball Method)
ASTM D2809
ASTM D2879
ASTM D2880
ASTM D2882
ASTM D2887
ASTM D2889
ASTM D2896
ASTM D2982
ASTM D2983
ASTM D3120
ASTM D3147
ASTM D3228
Vapor Pressure-Temperature
Relationship and Initial
Decomposition Temperature of
Liquids by Isoteniscope
Specification for Gas Turbine Fuel
Oils
Indicating the Wear Characteristics
of Petroleum and Non-Petroleum
Hydraulic Fluids in Constant
Volume Vane Pump
Boiling Range Distribution of
Petroleum Fractions by Gas
Chromatography
Vapor Pressure-Temperature
Relationship and Initial
Decomposition Temperature of
Liquids by Isoteniscope,
Determination of Pressure by
Isoteniscope
Specification for Gas Turbine
Fuel Oils
Hydraulic Pump Test
Simulated Distillation (Fuels),
Volatility by D2887 (Oils,Crude
Oil)
Brookfield Viscosity
48
ASTM D3230
ASTM D3233
ASTM D3235
ASTM D3306
ASTM D3321
ASTM D3427
ASTM D3524
ASTM D3525
ASTM D3606
ASTM D3634
Benzene/Toluene
ASTM D3699
ASTM D3828
ASTM D3829
ASTM D3944
ASTM D3945
ASTM D4006
49
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D4007
ASTM D4052
ASTM D4053
ASTM D4055
ASTM D4172
ASTM D4291
ASTM D4294
ASTM D4310
ASTM D4327
ASTM D4340
ASTM D4377
Sulfur by X-Ray
Determination of the Sludging and
Corrosion Tendencies of Inhibited
Mineral Oils
Anions in Water by Ion
Chromatography
Corrosion of Cast Al @ Hot
Surface
Water in Crude oil by Karl Fisher
ASTM D4485
ASTM D4530
ASTM D4539
50
ASTM D4629
ASTM D4682
ASTM D4683
ASTM D4684
ASTM D4737
ASTM D4739
ASTM D4740
ASTM D4807
ASTM D4809
ASTM D4814
ASTM D4815
ASTM D4929
ASTM D4929
ASTM D4950
Oxygenates in Fuel
51
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D4951
ASTM D4980
Determination of Additive
Elements in Lubricating Oils by
ICP-AES
Standard Test Methods for
Screening of pH in Waste
ASTM D5133
ASTM D5134
ASTM D5185
Determination of Additive
Elements, Wear Metals, and
Contaminants in Used Lubricating
Oils and Determination of Selected
Elements in Base Oils by
Inductively Coupled Plasma Atomic
Emission Spectrometry (ICP-AES)
ASTM D5190
ASTM D5293
ASTM D5307
Vapor Pressure
Cold Crank Simulator, Cold
Cranking Simulator Viscosity
Boiling Range, Boiling Range
Distribution of Crude Petroleum
by GC
Analysis of Petroleum Waxes by
GC, Analysis of Petroleum Wax
by Gas Chromatography (Carbon
Number Distribution)
ASTM D5442
ASTM D5599
Determination of Oxygenates in
Gasoline by Gas Chromatography
and Oxygen Selective Flame
Ionization Detection
ASTM D5621
Sonic Shear
ASTM D5762
52
ASTM D5771
ASTM D5800
ASTM D5828
ASTM D6082
HiTemp Foam
ASTM D6107
Stop Leak
ASTM D6184
ASTM D6278
ASTM D6293
ASTM D6352
ASTM D6371
ASTM D6375
PONA or PIANO
Boiling Range
ASTM D6417
ASTM D6448
ASTM D6470
53
Copyrights 2001 2015, Dr. Tareq Albahri, Chem. Eng. Dept., Kuwait University
ASTM D6560
ASTM D6584
ASTM D6616
ASTM D6751
ASTM E168
ASTM E 202
ASTM E 659
ASTM E1064
ASTM E1148
ASTM E1687
ASTM E1719
ASTM ES 15
ASTM PS 121
Determination of Asphaltenes
(Heptane Insolubles) in Crude
Petroleum and Petroleum Products
Determination of Free and Total
Glycerine in B-100 Biodiesel
Methyl Esters by Gas
Chromatography
Measuring Viscosity at High Shear
Rate by Tapered Bearing Simulator
Viscometer At 100C
Asphaltenes
Free and Total Glycerine,
Determination of Free and Total
Glycerine in B-100 Biodiesel by
GC
High Temperature/ High Shear
Viscosity at 100C
Measurements of Aqueous
Solubility
Determining Carcinogenic Potential
of Virgin Base Oils in
Metalworking Fluids
Vapor Pressure of Liquids by
Ebulliometry
Vapor Pressure of Petroleum
Products (Mini-Method)
[Discontinued in 1992, Replaced by
ASTM5291 D5191]
Measurements of Aqueous
Solubility
Determining Carcinogenic
Potential of Virgin Base Oils in
Metalworking Fluids
Vapor Pressure
Vapor Pressure
WITHDRAWN STANDARD:
PS121-99 Provisional Specification
Biodiesel Specs
for Biodiesel Fuel (B100) Blend
Stock for Distillate Fuels
54