Chapter03 - Lab Tests

Petroleum Refining - Chapter 3: Significance of Lab Tests

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Chapter 3 : Significance of lab tests in petroleum refining

Laboratory Standard Test Procedures (ASTM).

Significance of Laboratory Tests.

Product Specifications (ASTM).

Product Quality Upgrading (through operations) - Chapter 7

Table 3.1: The 30 most important ASTM tests in petroleum refining.

No. Test Fraction ASTM Standard

Test Number

Page

No. 1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

13.

14.

15.

16.

17.

18.

19.

20.

21.

22.

23.

24.

25.

26.

27.

28.

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

Crude oil and lighter

Atm resid and heavier

All

Crude Oil Feed

Gasoline

All

Light fractions

All

All

Naphtha & gasoline

Kerosene

kerosene (ATK)

Heavy fractions

Heavy fractions

Diesel and heavier

Diesel and lighter

Diesel and lighter

Naphtha and kerosene

All

All

Diesel

Diesel

Heavy fractions

Heavy fractions

All

All

All

Crude oil

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

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API (specific) gravity

Sample: all

Standard Test Number: ASTM D287-92

Principle: Buoyancy

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

D287

D1070

D1298

D1657

D4052

Specific gravity of bituminous materials, Pycnometer Method

API Gravity of Crude Petroleum & Petroleum Products (Hydrometer

Specific gravity of gaseous fuels

Density, Specific Gravity or API, Hydrometer Method

Density of LPG, hydrometer method

Oscillating frequency, Digital Density Meter

Density Meter - DMA 38

Density Meter - DMA 5000

Figure 3.1: Electronic Density Meters


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= 141.5

131.5

SG API

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.

Figure 3.2: Apparatus for ADTM D86 distillation

Procedure

A 100 ml sample, placed in a flask, is heated in a regulated rate (so that a uniform average rate of condensation in ml/min is maintained). This rate varied from zero to

5V% recovered, from 5 to 10 V% recovered and so on.

When the first drop appears at the lower end of the condenser tube, the thermometer reading (vapor temperature) is recorded as the initial boiling point (IBP).

Temperature readings are recorded at several V% distilled (Table 1) up to the final boiling point (FBP) and heating is discontinued.

After the flask has cooled the volume of remaining liquid is measured and recorded as the recovery.

For heavy fractions, heating is discontinued when decomposition point is observed (the vapor reaches a maximum temperature then starts declining before the end point).


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Table 3.2: Data recording for ASTM D86 test

Vol% T (F)

IBP

5

10

20

30

40

50

60

70

80

90

95

FBP

100

106

112

122

130

139

148

157

166

185

194

202

205

Recovery 98 %

This is usually plotted as follows


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ASTM D86 Atmospheric Distillation

Apparatus

ASTM D1160 Vacuum Distillation Apparatus

Related standards: Table 3.3: Standard test methods for distillation of petroleum products

ASTM test

#

Application

1.

2.

3.

4.

5.

6.

7.

8.

D86-96

D1160

D2887

D3710

D5307

D6352-98

D2892

D5236

Light petroleum fractions (naphtha, kerosene, diesel)

Heavy petroleum fractions (VGO, atm residue, vac residue)

Simulated Distillation (GC method); TBP of petroleum frac. other than gasoline

Simulated Distillation (GC method); TBP of gasoline

Simulated Distillation (GC method); TBP of crude oil.

Simulated Distillation (GC method); TBP of distillates (BP range 174 to 700C)

15/5 distillation; 15theoretical plate column (simulated TBP)

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).


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Figure. D2892: 15/5 distillation


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Simulated Distillation (SimDist) by Gas Chromatography (GC) Analyzers

Figure 3.3: Major components of a Gas Chromatograph

Figure 3.4: Output peaks of a gas chromatograph.


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Figure 3.5: Actual output from a gas chromatograph


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BS&W (Bottom sediments and water)

Sample: Crude oil

Standard Test Number: ASTM D96-88

Principle: centrifuge

D96-88: Standard Test method for Water & Sediment in Crude Oil by Centrifuge

Method

Objective

This test method covers the centrifuge method for determining sediment & water in crude oil.

It is not the most accurate, but the most practical method for field determination. Procedure

Two 50 ml samples are placed in two 100 ml cone-shaped centrifuge tubes.

50 ml solvent is added to each tube to facilitate mixing and demulsifying chemical to facilitate separation then plugged with a stopper.

The tubes are heated to 60 C and inverted a minimum of 10 times to ensure uniform mixing of oil and solvent.

The tubes are then placed in the centrifuge and spin for 5 min.

Immediately after the centrifuge comes to rest the combined volume of sediment & water at the bottom of each tube is recorded

BS&W usually ranges between 0.025, 0.05, and 0.1 for Kuwait Export Crude feed in the refinery (after settling in crude charge tanks).

Both tubes are reheated to 60 C, returned without agitation to the centrifuge and spin for 5 min at the same rate.

This is repeated until two consecutive consistent readings are obtained on each tube.

.

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)


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Octane Number

Sample: gasoline

Standard Test Number: ASTM D357 (Motor)

D908 (Research)

Principle: Combustion in a variable compression ratio motor.

Is a measure of the degree of knocking of (gasoline).

It compares the degree of combustion of gasoline to that of a mixture of n-heptane (zero octane) and iso-octane (100 octane) expressed as V% iso-octane (2,2,4-

trimethylpentane) .

Octane number depends on the structure (branching) of the compound MON = - 17 (n-octane)

MON = 100 (iso-octane) 2,2,4-trimethylpentane

Types of octane number

(Both use same test engine but operate under different conditions. MON at high engine

speed and RON at low engine speed)

(a) Motor method (MON) Represent performance on the highway or heavy load conditions (high speed).

(b) Research method (RON) Represent performance during city driving (low speed and acceleration is

relatively frequent)

(c) Posted octane number (PON)

2RON MONPON

Sensitivity of the fuel Sensitivity = (RON MON)

The sensitivity of the performance of the fuel to the two types of driving conditions (Low

Sensitivity fuels are better; equal performance is all conditions is desirable).

The octane rating is a measure of the resistance of gasoline and other fuels to detonation

(engine knocking) in spark-ignition internal combustion engines. High-performance engines

typically have higher compression ratios and are therefore more prone to detonation, so they

require higher octane fuel. A lower-performance engine will not generally perform better

with high-octane fuel, since the compression ratio is fixed by the engine design.

The octane number of a fuel is measured in a test engine, and is defined by comparison with

the mixture of iso-octane and normal heptane, which would have the same anti-knocking

quality as the fuel under test: the percentage, by volume, of iso-octane in that mixture is the

octane number of the fuel. For example, gasoline with the same knocking characteristics as a

mixture of 90% iso-octane and 10% n-heptane would have an octane rating of 90. Because

some fuels are more knock-resistant than iso-octane, the definition has been extended to

allow for octane numbers higher than 100.


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Compression Ratio

The ratio of the maximum to minimum volume in the cylinder of an internal-combustion

engine.

Figure. Stroke cycles in internal combustion engines

TDC = Top dead center

BDC = Bottom dead center

Volume at BDC = 10 in3

Volume at TDC = 1 in3

Compression ratio = 10 to 1

Figure. Compression ratio of internal combustion engines

Video. Compression Ratio


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Definition of octane rating

The octane rating of a spark ignition engine fuel is the detonation resistance (anti-knock

rating) compared to a mixture of iso-octane (2,2,4-trimethylpentane, an isomer of octane) and

n-heptane. By definition, iso-octane is assigned an octane rating of 100 and heptane is

assigned an octane rating of zero. An 87-octane gasoline, for example, possesses the same

anti-knock rating of a mixture of 87% (by volume) iso-octane and 13% (by volume) n-

heptane. This does not mean, however, that the gasoline actually contains these hydrocarbons

in these proportions. It simply means that it has the same detonation resistance as the

described mixture.

Iso-octane (2,2,4-trimethylpentane)

n-heptane

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.

Measurement methods

The most common type of octane rating worldwide is the Research Octane Number (RON).

RON is determined by running the fuel in a test engine with a variable compression ratio

-20

0

20

40

60

80

100

120

-20 0 20 40 60 80 100 120

Oct

ane

Num

ber

V% isooctane in (isooctane & n-heptane mixture)

pure

n-heptane

pure

isooctane


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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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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 ON

hexadecane < -30

n-octane -10

n-heptane 0

diesel fuel 1525 2-methylheptane 23

n-hexane 25

2-methylhexane 44

1-heptene 60

n-pentane 62

1-pentene 84

n-butanol 87

E10 gasoline 8790 n-butane 91

t-butanol 97

cyclohexane 97

iso-octane 100

benzene 101

propane 103

methanol 113

toluene 114

ethanol 116

xylene 117

E85 gasoline 105

methane 107

ethane 108

Effects of octane rating

Higher octane ratings correlate to higher activation energies. Activation energy is the amount

of energy necessary to start a chemical reaction. Since higher octane fuels have higher

activation energies, it is less likely that a given compression will cause detonation.

It might seem odd that fuels with higher octane ratings explode less easily and can therefore

be used in more powerful engines. However, an explosion is not desired in an internal

combustion engine. An explosion will cause the pressure in the cylinder to rise far beyond the

cylinder's design limits, before the force of the expanding gases can be absorbed by the piston

traveling downward. This actually reduces power output, because much of the energy of

combustion is absorbed as strain and heat in parts of the engine, rather than being converted

to torque at the crankshaft.

However, burning fuel with a lower octane rating than required by the engine often reduces

power output and efficiency one way or another. If the engine begins to detonate (knock),

that reduces power and efficiency. Many modern car engines feature a knock sensor a small piezoelectric microphone which detects knock and then sends a signal to the engine control

unit to retard the ignition timing. Retarding the ignition timing reduces the tendency to

detonate, but also reduces power output and fuel efficiency.


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Figure 6.1: ASTM Octane Number Standard Engine

Figure. Digital control panel


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Other relevant standards

D909 (knock characteristics for Aviation fuels)

D2699 (knock characteristics of motor fuels by research method)

D2700 (knock characteristics of motor and aviation fuels by motor method)

D2623 (knock characteristics of LPG by the motor (LP) method)

D2885 (Research and Motor Method Octane Ratings Using Online Analyzers)

Figure. Portable octane number analyzer

Reid Vapor Pressure (RVP)

Sample: Naphtha, Gasoline and others

Standard Test Number: D323-94

Principel: Pressure in a sample bob held at 100 F

D323-94: Standard Test Method for Vapor Pressure of Petroleum Products

(Reid Method)

Objective

This test method is used to determine the vapor pressure (in absolute units) at 100 F (37.8 C) of petroleum products and crude oils with initial boiling point (IBP) above

32F (0C).

Procedure

The sample is placed in a liquid chamber (cylinder) which is filled to the tip then coupled to a vapor chamber as quickly as possible. (this is done in such a way that

vaporization losses are avoided)

The sample is drained from the liquid to the vapor chamber and the whole assembly is immersed in constant temperature bath (100F) for 5 minutes.

The reading is observed after taping the pressure gage lightly.


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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.

Other standards related

D1267 (vapor pressure of LPG - Bomb Method)

D2551 (Vapor pressure by micromethod) D5191: Standard Test Method for Vapor Pressure of Petroleum Products (Mini Method)

Figure. RVP Bath and cylinder

Sulfur

Sample: all

Standard Test Number: ASTM D1266 (Lamp Sulfur)

Principle: Combustion in lamp and analysis

Sulfur Content (wt%)

Ranges from 0.1 to 5 % or more.

Undesirable pollutant and corrosive.

Crude with S content greater than 0.5 W% requires more extensive processing than those with lower sulfur content.

Almost half of the units in the refinery such as the ARDS, HTU, Merox, sulfur recovery, tail gas treating (TGT), and the Amine all are added because of the high S

content of crude.

Costs more to get rid of (100 %).

Sour crude - Previously, refer to crude containing dissolved H2S independent of total sulfur. - Now, refer to any crude oil with S content > 0.5 wt % thus requiring special

processing.


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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).

Other relevant standards D92 (Flash and Fire points by Cleveland Open Cup).

D93 (Pensky-Martines Closed Tester).

D3828 (Setaflash closed tester).


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Tag

closed cup

flash tester

Pensky-Martens closed-

cup

flash tester

Rapid Flash

Closed-Cup

flash tester

Cleveland

open-cup

flash tester

Tag

Open-Cup

Flash Tester

Setaflash Closed Cup Setaflash Open Cup Fully Automatic

Setaflash

Figure 6.2: Flash Point


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Freezing point Temperature, C (F)

Sample: aviation fuels (kerosene, ATK)

Standard Test Number: ASTM D2386

Principle: Temperature of disappearance of crystals on reheating.

Scope:

This test method covers the determination of the temperature below which solid

hydrocarbon crystals may form in aviation turbine fuels and aviation gasoline.

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.

Figure. Freezing point of kerosene


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Figure. Apparatus for the Freezing point of kerosene

Cloud Point Temperature, C (F)

Sample: diesel


Test Principle:

Observation during cooling under prescribed conditions

Definition:

The temperature of a liquid specimen when the smallest observable duster of wax

crystals first appears upon cooling under prescribed condition.

Procedure:

1. A sample is filtered at a temperature at least 14C above the expected cloud point until oil is perfectly clear.

2. The sample is then poured into the test jar to the level mark. 3. 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.

4. 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).

5. 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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Pour Point Temperature, C (F)

Sample: Diesel and heavier fractions.

Standard Test Number: ASTM D97-96 a (petroleum products)

ASTM D5853-95 (for crude oil)

Test Principle: Observation during gradual cooling

Definition

The pour point is the lowest temperature of the test sample when it becomes a solid. It is

related to the amount of wax content present in the fraction.

It is a rough indicator of the relative paraffinicity and aromacity of the crude.

Lower pour points indicate low paraffin and high aromatic content.

Lower pour points are usually preferred.

Procedure

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.

Cloud and Pour point apparatus


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Smoke point (mm)

Sample: kerosene (both Illuminating and ATK)


Principle: Maximum height of smokeless flame.

Scope:

This test method covers the determination of the smoke point, which is the maximum

height, in millimeters of a smokeless flame of kerosene and aviation turbine fuel burned in a

wick-fed lamp of specified design. Higher smoke point is better.

Significance

The smoke point is related to the hydrocarbon type composition of fuel

Generally, the more aromatic the fuel the smokier the flame.

Gives an indication of the smoke and sooting tendency of burning fuel (kerosene)

Apparatus

Smoke point lamp: (Chimney, Graduated scale and Candle)

Wick of woven solid circular cotton and Pipettes or Burettes.

Procedure:

- A 125 long dried wick is soaked in the sample and placed in the wick tube of the candle.

- A 10-20 ml of the prepared sample is introduced at room temperature into the dry candle.

- The wick tube is placed in the candle firmly. A new, clean, sharp razor is used to cut the wick at the face of the holder and remove wisps and frayed ends.

- The candle is lighted and the wick adjusted so that the flame is approximately 10 mm high within 5 min.

- After burning, the candle is raised until a smoky tail appears, then the candle is lowered slowly through several stages of flame appear once.

- The maximum height of flame that can be achieved without smoking is determined to the nearest 0.5 mm.

- The candle is removed from the lamp arise with heptanes and purged with air to make ready for re-use.

Related Standards

IP57 (for fuel oil)

D187 (burning quality of kerosene)


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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.

Apparatus for the determination of kinematic viscosity


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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.


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).


27

The tube is tightly closed and placed in the comparator.

The comparator reading are observed and compared with a standard.

PFX995-PFX950-PFX880 Automatic Colorimeters

Lovibond PFX195 Automatic Colorimeters

Lovibond 3000 Comparator Series

Lovibond Comparator 2000 System

Related Standards:

D156 (Saybolt color, Height of liquid column for equality with colored glass)

D1500 (comparison with colored glass standard reference)


28


Sample: Transparent and light colored fractions


ASTM D1218-92: Standard Test Method for Refractive Index and Refractive Dispersion of

Hydrocarbon Liquids

Objective:

To measure the refractive index and refractive dispersion of transparent and light-colored

hydrocarbon liquids that has refractive indexes in the range from 1.33 to 1.5, and at

temperature from 20 to 30 C.

Definition:

Refractive index is the ratio of the velocity of light in air, to its velocity in the substance under examination (or it is the sine of the angle of incidence divided by

the sine of the angle of refraction) as light passes from air into the substance.

Refractive dispersion is the difference between the refractive indexes of a substance for light of two different wavelengths, both indexes being measured at

the same temperature.

Apparatus:

The apparatus consists of a refractometer, thermostat and circulating Pump,

thermometer, light sources, and light filters.

Procedure:

The sample is applied to the faces of two prisms after cleaning them.

A light source is applied and the reading is taken from the scale directly.

Other standards:

ASTM D1747 - 09(2014) Standard Test Method for Refractive Index of Viscous Materials

Photo of a traditional handheld refractometer Photo of a water-resistant digital handheld

refractometer


29

An illustration of the main types of laboratory refractometers in operation today

Aniline point Temperature

Sample: all


D611-82 Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon

Solvents

Principle: Phase separation temperature of a HC/aniline mixture

Objective

The purpose of this test is to determine the aniline and mixed aniline point of petroleum

products (and hydrocarbon solvents having aniline point below the temperature at which

aniline will crystallize).


30

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)

K10200 Automatic Aniline Point Apparatus K10190 Thin Film Aniline Point Apparatus


31

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 (Hexadecane) C16H34 alpha-methyl naphthalene C11H10

(Cetane number = 100) (Cetane number = 0)

isocetane (2,2,4,4,6,8,8-heptamethylnonane)

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


32

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


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'.

A mathematical expression is developed to estimate the cetane number in the many refineries that do not have cetane test engine.

The number desired is called the cetane index & is calculated from the mid-boiling point and specific gravity of the sample.

It is actually an expression of the hydrogen to carbon (H/C) ratio of the hydrocarbon components in the sample.

The higher the H/C ratio, the better the burning characteristic. (i.e. higher the smoke point and higher the cetane index).


33

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)

Carbon Residue (wt %)

Relates to the asphalt content of crude oil & to the quantity of the lubricating oil fraction that can be recovered.

Determined by distillation to a coke residue in the absence of air.

In most cases (unless want to make lube oil) the lower the carbon residue, (less Carbon) the more valuable the crude.

Expressed by Ramsbottom (RCR) ASTM designation D524. Conradson (CCR) ASTM designation D189.

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


34

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.

Conradson Carbon Residue Apparatus;

Includes: burner, tripod, nickel-chrome

triangle, refractory block, porcelain crucible,

monel crucible and cover; Skidmore

crucible and cover-monel and a monel hood

and bridge

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.


35

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.

Ramsbottom Carbon Residue Apparatus

& Data Acquisition Software

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.


36

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

Salt Content, PTB

Sample: Crude oil

Standard Test Number:

D6470-99 Salt in crude by Potentiometric Method

D3230-99 Salts in Crude Oil (Electrometric Method)

Principle:

Auto Ignition Temperature

Sample: all


Principle:

Figure 6.3: Auto-ignition Apparatus

Hydrocarbon type

Sample:


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)


37

D2600 (Aromatics traces in light saturated hydrocarbons by GC)

D2269 (Aromatic content, UV absorption method)

D4420 (Aromatics in Gasoline)

D3606 (Benzene and Toluene in Gasoline by GC)

Molecular Weight

Sample: All

Standard Test Number: D2503

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


Related Standards

ASTM D240 14: Standard Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter


38

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)


39

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.


40

Table: The most important ASTM tests in Naphtha.

No. Test ASTM Standard

Test Number

1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

Atm Distillation

API & specific gravity

Octane Number

RVP

PNA/ PONA/PIONA(PIANO)

Sulfur, wt% - all

Flash point


Conradson carbon

Ramsbottom carbon

C/H ratio

Heating value (net/gross)

D 86

D 1160

D96-88

D323

D544393 D908

D56-97

D1218-92

D189-97

D524

D5291

D240/D4809

ASTM specifications for products is presented in chapter 4


41

Summary of petroleum related ASTM Standards

Method ASTM Description Common Reference

ASTM C117

Determination of Materials Finer

than 75um (no. 200) Sieve in

Mineral Aggregates by Washing

Mineral Aggregates by Washing

ASTM C136 Sieve Analysis of Course and Fine

Aggregates

Sieve Analysis of Fine and Coarse

Aggregates

ASTM C566 Total Evaporable Moisture Content

of Aggregate by Drying

Moisture Content of Aggregate by

Drying

ASTM D56 Flash Point by Tag Closed Tester Tag Closed Cup Flash

ASTM D86 Distillation of Petroleum Products at

Atmospheric Pressure

Atmospheric Distillation of

Petroleum Products (Gasoline)

(Fuel Oils)

ASTM D87 Melting Point of Petroleum Wax

(Cooling Curve) Melting Point of Wax

ASTM D91 Precipitation Number of Lubricating

Oils

Precipitation Number of

Lubricating Oils

ASTM D92 Flash and Fire Points by Cleveland

Open Cup Tester

Flash Point, COC / Fire Point.

COC

ASTM D93 Flash-Point by Pensky-Martens

Closed Cup Tester

Pensky-Marten Flash Point, Flash

Point PM / Pensky-Marten Fire

Point, Fire Point PM

ASTM D94 Saponification Number of

Petroleum Products

Saponification Number of

Petroleum Products

ASTM D95

Water in Petroleum Products and

Bituminous Materials by

Distillation

Water by Distillation, Water

Content by Distillation

ASTM D96

Test Methods for Water and

Sediment in Crude Oil by

Centrifuge Method (Field

Procedure)

Percent Sediment, Brine,

Sediment and Water

ASTM D97 Pour Point of Petroleum Products Pour Point - Fuels / Pour Point -

Oils

ASTM D127 Drop Melting Point of Petroleum

Wax including Petrolatum

Drop Melting Point, Melting Point

of Wax, Dropping Point

ASTM D128 Analysis of Lubricating Grease Analysis of Lubricating Grease

ASTM D129 Sulfur in Petroleum Product

(General Bomb Method)

Sulfur in Petroleum Product

(General Bomb Method)

ASTM D130

Detection of Copper Corrosion from

Petroleum Products by the Copper

Strip Tarnish Test

Copper Corrosion


42

ASTM D156

Saybolt Color of Petroleum

Products (Saybolt Chromometer

Method)

Color-Saybolt; Saybolt Color,

Color by Saybolt method

ASTM D189 Conradson Carbon Residue of

Petroleum Products

Conradson Carbon; Conradson

Carbon Residue

ASTM D217 Cone Penetration of Lubricating

Grease Full Scale Cone Penetration

ASTM D240

Heat of Combustion of Liquid

Hydrocarbon Fuels by Bomb

Calorimeter


Hydrocarbon Fuels

ASTM D287

API Gravity of Crude Petroleum

and Petroleum Products

(Hydrometer Method)

API Gravity, Specific Gravity,

Density

ASTM D322 Gasoline Diluent in Used Gasoline

Engine Oils by Distillation Fuel Dilution by Distillation

ASTM D323 Vapor Pressure of Petroleum

Products (Reid Method) Reid Vapor Pressure

ASTM D381 Gum Content in Fuels by Jet

Evaporation

Gum Content in Fuels by Jet

Evaporation

ASTM D396 Standard Specification for Fuel Oils Fuel Oils Specification

ASTM D439

Specification for Automotive Spark-

Ignition Engine Fuel [Replaced

ASTM D439 with ASTM D4814]

Anti-Knock Index (R+M)/2

Octane

ASTM D445

Kinematic Viscosity of Transparent

and Opaque Liquids (the

Calculation of Dynamic Viscosity)

Kinematic Viscosity at Non

Standard Temperatures /

Kinematic Viscosity at 40C and

Kinematic Viscosity at100C

ASTM D471 Rubber Properties - Effects of

Liquids Effect of Liquids on Rubber

ASTM D473 Sediment in Crude Oils and Fuel

Oils by the Extraction Method

Sediment in Crude Oils and Fuel

Oils by Extraction

ASTM D482 Ash from Petroleum Products Ash, Ash Content

ASTM D483 Unsulfonated Residue of Petroleum

Plant Spray Oils

Unsulfonated Residue of

Petroleum Plant Spray Oil

ASTM D524 Ramsbottom Carbon Residue of

Petroleum Products Ramsbottom Carbon Residue

ASTM D525 Oxidation Stability of Gasoline

(Induction Period Method) Oxidation Stability

ASTM D566 Dropping Point of Lubricating

Grease Dropping Point


43

ASTM D611

Aniline Point and Mixed Aniline

Point of Petroleum Products and

Hydrocarbon Solvents

Aniline Point, Aniline Point of

Petroleum Products

ASTM D613 Cetane Number of Diesel Fuel Oil Cetane No.

ASTM D664 Acid Number of Petroleum Products

by Potentiometric Titration TAN, Total Acid No.

ASTM D665

Rust-Preventing Characteristics of

Inhibited Mineral Oil in the

Presence of Water

Rust Prevention Characteristics

ASTM D721 Oil Content of Petroleum Waxes Oil in Wax

ASTM D808 Chlorine in New and Used

Petroleum Products (Bomb Method) Chlorine in Lubricating Oils

ASTM D854 Specific Gravity of Soil Solids by

Water Pycnometer Specific Gravity of Soils

ASTM D874 Sulfated Ash from Lubricating Oils

and Additives Sulfated Ash

ASTM D892 Foaming Characteristics of

Lubricating Oils Foam

ASTM D893 Insolubles in Used Lubricating Oils Insolubles

ASTM D924

Dissipation Factor (or Power

Factor) and Relative Permittivity

(Dielectric Constant) of Electrical

Insulating Liqui

Test Method for Dissipation

Factor (or Power Factor) of

Electrical Insulating Liquids.

ASTM D937 Cone Penetration of Petrolatum Cone Penetration of Petrolatum

ASTM D938 Congealing Point of Petroleum

Waxes, including Petrolatum Congealing Point of Wax

ASTM D943 Oxidation Characteristics of

Inhibited Mineral Oils Oxidation

ASTM D971

Test Method for Interfacial Tension

of Oil against Water by Ring

Method

Test Method for Interfacial

Tension of Oil against Water by

Ring Method

ASTM D972 Evaporation Loss of Lubricating

Greases and Oils

Evaporation Loss of Lubricating

Greases and Oils

ASTM D974 Acid and Base Number by Color-

Indicator Titration

Neutralization Number

Neutralization No.; Acid and Base

No.

ASTM D975 Standard Specification for Diesel

Fuel Oils

Standard Specification for Diesel

Fuel Oils

ASTM D976

Calculated Cetane Index of

Distillate Fuels - requires API

Gravity and D86 Distillation

Calculated Cetane Index


44

ASTM D1067 Acidity or Alkalinity of Water Acidity or Alkalinity of Water

ASTM D1119 Percent Ash Content of Engine

Coolants and Antirusts Ash Content of Engine Coolants

ASTM D1120 Boiling Point of Engine Coolants

Boiling Point of Engine Coolants

(neat and 50/50 mixture) /

Equilibrium Reflux Boiling Point

at atmospheric pressure

ASTM D1121 Reserve Alkalinity of Engine

Coolants and Anti-rust

Reserve Alkalinity of Antifreeze,

Determination of the Reserve

Alkalinity of Antifreeze

ASTM D1122

Density or Relative Density of

Engine Coolant Concentrates and

Engine Coolants By The

Hydrometer

Specific Gravity of Engine

Coolant Concentrates and Engine

Coolants by The Hydrometer,

Specific Gravity of Coolants,

Specific Gravity of Antifreeze

ASTM D1123

Water in Engine Coolant

Concentrate by the Karl Fischer

Reagent Method

Water %: by Karl Fischer Method

Hardness in Water Hardness in Water

ASTM D1133 Kauri-Butanol Value of


Kauri Butanol Value of


ASTM D1160 Distillation of Petroleum Products at

Reduced Pressure

Vacuum Distillation of Petroleum

Products

ASTM D1177 Freezing Point of Aqueous Engine

Coolants

Refractive Index and Refractive

Dispersion of Hydrocarbon

Liquids

ASTM D1217

Density and Relative Density

(Specific Gravity) of Liquids by

Bingham Pycnometer


(Specific Gravity) of Liquids by

Pycnometer

ASTM D1218 Refractive Index and Refractive

Dispersion of Hydrocarbon Liquids

Refractive Index and Refractive

Dispersion of Hydrocarbon

Liquids

ASTM D1275 Corrosive Sulfur in Electrical

Insulating Oils

Corrosive Sulfur in Electrical

Insulating Oils

ASTM D1287 The pH of Engine Coolants and

Antirusts pH of Antifreeze

ASTM D1293 pH of Water pH of Water

ASTM D1298

Density, Relative Density (Specific

Gravity), or API Gravity of Crude

Petroleum and Liquid Petroleum

Products by Hydrometer Method

Density, Specific Gravity and API

Gravity by Hydrometer


45

ASTM D1319

Hydrocarbon Types in Liquid

Petroleum Products by Fluorescent

Indicator Adsorption

Hydrocarbon Types by

Fluorescent Indicator Absorption

ASTM D1321 Needle Penetration of Petroleum

Waxes Needle Penetration

ASTM D1384 Corrosion Test for Engine Coolants

in Glassware Corrosion in Glassware

ASTM D1401 Water Separability of Petroleum

Oils and Synthetic Fluid Demulsibility

ASTM D1403

Cone Penetration of Lubricating

Grease Using One-Quarter and One-

Half Scale Cone Equipment

Quarter Scale Cone Penetration

ASTM D1480


(Specific Gravity) of Viscous

Materials by Bingham Pycnometer



Materials by Pycnometer

ASTM D1481



Materials by Lipkin Bicapillary

Pycnometer



Materials by Lipkin Bicapillary

Pycnometer

ASTM D1500 ASTM Color of Petroleum Products

(ASTM Color Scale) Color, ASTM

ASTM D1662 Standard Test Method for Active

Sulfur in Cutting Oils Active Sulfur in Cutting Oils

ASTM D1747 Refractive Index of Viscous

Materials Refractive Index

ASTM D1796

Water and Sediment in Fuel Oils by

the Centrifuge Method (Laboratory

Procedure)

Water and Sediment

ASTM D1832 Peroxide Number of Petroleum Wax Peroxide No. of Petroleum Wax

ASTM D1835 Specifications for Liquid Petroleum

(LP) Gases

LPG Specifications,

Specifications for Liquid

Petroleum Gas (LPG) / Analysis

of Liquified Petroleum Gas (LPG)

by Gas Chromatography

ASTM D1837 Volatility of Liquefied Petroleum

(LP) Gases

Volatility of LPG / LPG

Volatility

ASTM D1881 Foaming Tendencies of Engine

Coolants in Glassware Foaming Tendencies of Antifreeze

ASTM D1882

Effect of Cooling System Chemical

Solutions on Organic Finishes for

Automotive Vehicles

Auto Finish Effect; Surface Finish

by Antifreeze

ASTM D1959 Iodine Value of Drying Oils and

Fatty Acids Iodine Value


46

ASTM D2007

Characteristic Groups in Rubber

Extender and Processing Oils and

Other Petroleum - Derived Oils by

the Clay-Gel Absorption

Chromatographic Method

Hydrocarbon Type analysis by

Clay-Gel Absorption

Chromatography / Percent

Hydrocarbon / Hydrocarbon Type

with Asphalenes / Hydrocarbon

Type with Aromatics recovered

ASTM D2008 Ultraviolet Absorbance and

Absorptivity of Petroleum Products

Ultraviolet Absorbance and

Absorptivity of Petroleum

Products, UV Absorbance and

Absorptivity

ASTM D2158 Residues in Liquified Petroleum

(LP) Gases

LPG Residue, Residues in

Liquified Petroleum Gas (LPG)

ASTM D2161

Standard Practice for Conversion of

Kinematic Viscosity to Saybolt

Universal Viscosity or to Saybolt

Furol Viscosity

Conversion of Kinematic

Viscosity to Saybolt Universal of

Saybolt Furol

ASTM D2163

Analysis of Liquified Petroleum

(LP) Gases and Propene

Concentrates by Gas

Chromatography

LPG Composition, (LP) Gases

and Propane Concentrates by Gas

Chromatography, Analysis of

Liquified Petroleum Gas (LPG)

by Gas Chromatography

ASTM D2257 Extractable Matter in Textiles Extractable Matter in Textiles

ASTM D2265

Dropping Point of Lubricating

Grease over Wide Temperature

Range

Dropping Point of Lubricating

Grease over Wide Temperature

Range

ASTM D2266

Wear Preventive Characteristics of

Lubricating Grease (Four-Ball

Method)

Four Ball Wear test for Greases

ASTM D2270

Standard Practice for Calculating

Viscosity Index From Kinematic

Viscosity at 40 and 100C

Calculating Viscosity Index From

Kinematic Viscosity at 40 and

100C

ASTM D2272

Oxidation Stability of Steam

Turbine Oils by Rotating Pressure

Vessel

Oxidation Stability of Steam

Turbine Oils by Rotating Bomb

ASTM D2273 Trace Sediment in Lubricating Oils Trace Sediment

ASTM D2274 Oxidation Stability of Distillate Fuel

Oil (Accelerated Method)

Oxidation Stability of Distillate

Fuel Oil (Accelerated Method)

ASTM D2386 Freezing Point of Aviation Fuels Freeze Point

ASTM D2500 Cloud Point of Petroleum Products Cloud Point

ASTM D2501 Calculation of Viscosity-Gravity

Constant (VGC) of Petroleum Oils

Calculation of Viscosity Gravity

Constant (VGC) of Petroleum

Oils


47

Estimation of Molecular Weight

(Relative Molecular Mass) of

Petroleum Oils From Viscosity

Measurements

Mol Weight from Viscosity

ASTM D2509

Measurement of Load-Carrying

Capacity of Lubricating Grease

(Timken Method)

Load Caring Capacity of

Lubricating Greases (Timken

Method)

ASTM D2533 Vapor-Liquid Ratio of Spark-

Ignition Engine Fuels

Vapor-Liquid Ratio, Vapor Liquid

Ratio for Gasoline

ASTM D2549

Separation of Representative

Aromatics and Nonaromatics

Fractions of High-Boiling Oils by

Elution Chromatography

Aromatics, Aromatics and Non-

Aromatics in High Boiling Oils

ASTM D2570 Simulated Service Corrosion

Testing of Engine Coolants Simulated Service of Coolant

ASTM D2596

Measurement of Extreme-Pressure

Properties of Lubricating Grease

(Four-Ball Method)

Four Ball EP Tesing for Greases

ASTM D2602

Hydrolytic Stability of Hydraulic

Fluids (Beverage Bottle Method)

[Discontinued 1993, Replaced by

D5293}

Hydrolytic Stability

(Discontinued)

ASTM D2619 Hydrolytic Stability of Hydraulic

Fluids (Beverage Bottle Method) Hydrolytic Stability

ASTM D2669

Viscosity of Petroleum Waxes

Compounded with Additives (Hot

Melts)

Apparent Viscosity of Petroleum

Waxes compounded with

additives (hot melt), ASTM

D2669

ASTM D2699 Research Octane Number of Spark-

Ignition Engine Fuel

Research Octane Number;

Research Octane No., Knock

Characteristics of Motor Fuel by

Research Method

ASTM D2700 Motor Octane Number of Spark-

Ignition Engine Fuel

Motor Octane Number, Motor

Octane No., Knock Characteristics

of Motor and Aviation Fuels by

Motor Method

ASTM D2709 Water and Sediment in Middle

Distillate Fuels by Centrifuge

Water and Sediment in Middle

Distillate Fuels by Centrifuge

ASTM D2766 Specific Heat of Liquids and Solids Specific Heat of Liquids and

Solids

ASTM D2782


Properties of Lubricating Fluids

(Timken Method)

Timken EP for Gear Oils


48

ASTM D2783


Properties of Lubricating Fluids

(Four-Ball Method)

Four Ball EP for Gear Oils

ASTM D2809

Cavitation Corrosion and Erosion-

Corrosion Characteristics of

Aluminum Pumps With Engine

Coolants

Cavitation, Pump Cavitation

ASTM D2879

Vapor Pressure-Temperature

Relationship and Initial

Decomposition Temperature of

Liquids by Isoteniscope

Vapor Pressure-Temperature

Relationship and Initial

Decomposition Temperature of

Liquids by Isoteniscope,

Determination of Pressure by

Isoteniscope

ASTM D2880 Specification for Gas Turbine Fuel

Oils

Specification for Gas Turbine

Fuel Oils

ASTM D2882

Indicating the Wear Characteristics

of Petroleum and Non-Petroleum

Hydraulic Fluids in Constant

Volume Vane Pump

Hydraulic Pump Test

ASTM D2887

Boiling Range Distribution of

Petroleum Fractions by Gas

Chromatography

Simulated Distillation (Fuels),

Volatility by D2887 (Oils,Crude

Oil)

ASTM D2889 Calculation of True Vapor Pressures

of Petroleum Distillate Fuels True Vapor Pressure

ASTM D2896

Base Number of Petroleum Products

by Potentiometric Perchloric Acid

Titration

TBN; Total Base No., Total Base

Number

ASTM D2982 Detecting Glycol-Base Antifreeze in

Used Lubricating Oils Glycol in Oil

ASTM D2983

Method for Low-Temperature

Viscosity of Lubricants Measured

by Brookfield Viscometer / Low-

Temperature Viscosity of

Lubricants Measured by Brookfield

Viscometer

Brookfield Viscosity

ASTM D3120

Trace Quantities of Sulfur in Light

Liquid Petroleum Hydrocarbons by

Oxidative Microcoulometry

Sulfur, Sulfur Content by

Coulometric Titration / Sulfur

Content by Dohrmann

ASTM D3147 Testing Stop-Leak Additives for

Engine Coolants Coolant Stop Leak Test Machine

ASTM D3228

Total Nitrogen in Lubricating Oils

and Fuel Oils by Modified Kjeldahl

Method

Kjeldahl Nitrogen


49

ASTM D3230 Salts in Crude Oil (Electrometric

Method) Salts in Crude Oil

ASTM D3233

Measurement of Extreme Pressure

Properties of Fluid Lubricants

(Falex Pin and Vee Block Methods)

Measurement of Extreme Pressure

Properties of Fluid Lubricants

(Falex Pin and Vee Block

Methods), Falex EP for

Lubricating Oil

ASTM D3235 Solvent Extractables in Petroleum

Waxes Solvent Extractibles from Wax

ASTM D3306

Standard Specification for Glycol

Base Engine Coolant for

Automobile and Light-Duty Service

Specification for Ethylene Glycol

Base Engine Coolants

ASTM D3321

Use of the Refractometer for Field

Test Determination of the Freezing

Point of Aqueous Engine Coolants

Refractive Index Freezing Point,

ASTM D3427 Air Release Properties of Petroleum

Oils

Gas Bubble Separation Time of

Petroleum Oils

ASTM D3524

Diesel Fuel Diluent in Used Diesel

Engine Oils by Gas

Chromatography

Fuel Dilution (Diesel)

ASTM D3525

Gasoline Diluent in Used Gasoline

Engine Oils by Gas

Chromatography

Fuel Dilution (Gasolline)

ASTM D3606

Determination of Benzene and

Toluene in Finished Motor and

Aviation Gasoline by Gas

Chromatography

Benzene/Toluene

ASTM D3634 Trace Chloride Ion in Engine

Coolants Chloride: titration, Trace Chloride

ASTM D3699 Standard Specification for Kerosine Kerosene Specification

ASTM D3828 Flash Point by Small Scale Closed

Tester

Flash Point by Small Scale Closed

Tester

ASTM D3829 Predicting the Borderline Pumping

Temperature of Engine Oil

MRV 20 hr, Mini Rotary

Viscosity by the 20hr cycle

ASTM D3944 Solidification Point of Petroleum

Wax

Solidification Point of Petroleum

Wax

ASTM D3945

Shear Stability of Polymer-

Containing Fluids Using a Diesel

Injector Nozzle (Discontinued 1998

[replaced by ASTM D6278]

Orbahn Shear

ASTM D4006 Water in Crude Oil by Distillation Water in Crude Oil by Distillation


50

ASTM D4007

Water and Sediment in Crude Oil by

the Centrifuge Method (Laboratory

Procedure)

Water and Sediment in Crude Oil

by the Centrifuge Method

(Laboratory Procedure)

ASTM D4052 Density and Relative Density of

Liquids by Digital Density Meter Density

ASTM D4053 Benzene in Motor and Aviation

Gasoline by Infrared Spectroscopy

Benzene in Motor and Aviation

Gasoline by Infrared

Spectroscopy, Benzene Content of

Crude Oil

ASTM D4055 Pentane Insolubles by Membrane

Filtration

Pentane Insolubles by Membrane

Filtration

ASTM D4172

Wear Preventive Characteristics of

Lubricating Fluid (Four Ball

Method)

Four Ball Wear Test, Four Ball

Wear for Gear Oils

ASTM D4291 Trace Ethylene Glycol in Used

Engine Oil

Glycol in Lube Oils / Foaming

Tendencies of Engine Coolants at

Room Temperature

ASTM D4294

Sulfur in Petroleum Products by

Energy-Dispersive X-Ray

Fluorescence Spectroscopy

Sulfur by X-Ray

ASTM D4310

Determination of the Sludging and

Corrosion Tendencies of Inhibited

Mineral Oils

Determination of the Sludging and

Corrosion Tendencies of Inhibited

Mineral Oils

ASTM D4327 Anions in Water by Chemically

Suppressed Ion Chromatography

Anions in Water by Ion

Chromatography

ASTM D4340

Corrosion of Cast Aluminum Alloys

in Engine Coolants under Heat-

Rejecting Conditions

Corrosion of Cast Al @ Hot

Surface

ASTM D4377

Water in Crude Oils by

Potentiometric Karl Fischer

Titration

Water in Crude oil by Karl Fisher

ASTM D4485 Standard Specifications for

Performance of Engine Oils

Standard Specifications for

Performance of Engine Oils

ASTM D4530 Determination of Carbon Residue

(Micro Method)

Determination of Carbon Residue

(Micro Method)

ASTM D4539

Filterability of Diesel Fuels by the

Low Temperature Flow Test

(LTFT) Method

Low Temperature Flow Test,

Single Temp. or Full Range

Temperatures,, Low Temperature

Flow Test of Fuel Oil


51

ASTM D4629

Trace Nitrogen in Liquid Petroleum

Hydrocarbons by Syringe/Inlet

Oxidative Combustion and

Chemiluminescence Detection

Nitrogen by Chemiluminescence

ASTM D4682

Miscibility with Gasoline and

Fluidity of Two-Stroke-Cycle

Gasoline Engine Lubricants

Miscibility with Gasoline

ASTM D4683

Measuring Viscosity at High Shear

Rate and High Temperature by

Tapered Bearing Simulator

High Temp/High Shear, High

Temperature/High Shear

Viscosity

ASTM D4684

Determination of Yield Stress and

Apparent Viscosity of Engine Oils

at Low Temperature

MRV (TP1)[2-day test], MRV-

TP1 Viscosity

ASTM D4737 Calculated Cetane Index by Four

Variable Equation

Calculated Cetane Index by Four

Variable Equation

ASTM D4739 Base Number Determination by

Potentiometric Titration

TBN, Total Base Number; Total

Base No.

ASTM D4740 Cleanliness and Compatibility of

Residual Fuels by Spot Test

Spot Test, Stability and

Compatibility of Residual Fuels

by Spot Test

ASTM D4807 Sediment in Crude Oil by

Membrane Filtration

Sediment in Crude Oil by

Membrane Filtration

ASTM D4809


Hydrocarbon Fuels by Bomb

Calorimeter (Precision Method)

Heat of Combustion by Bomb

Calorimeter

ASTM D4814

Standard Specification for

Automotive Spark-Ignition Engine

Fuel

Anti-Knock Index (R+M)/2

Octane Specification

ASTM D4815

Determination of MTBE, ETBE,

TAME, DIPE, tertiary-Amyl

Alcohol and C1 to C4 Alcohols in

Gasoline by Gas Chromatography

Oxygenates in Fuel

ASTM D4929

Methods for Determination of

Organic Chloride Content in Crude

Oil

Chlorine Content by Coulometric

Titration

ASTM D4929

Test Method B covers the

determination of organic chloride in

the washed naphtha fraction of

crude oil by oxidative combustion

followed by microcoulometric

titration

Test Method B, Chlorine Content

by Oxidative Combustion

ASTM D4950

Standard Classification and

Specification of Automotive Service

Greases

Standard Classification and

Specification of Automotive

Service Greases


52

ASTM D4951

Determination of Additive Elements

in Lubricating Oils by Inductively

Coupled Plasm

Documents

Chapter03 - Lab Tests