Академический Документы
Профессиональный Документы
Культура Документы
DOI 10.1007/978-3-319-05545-9_27-1
# Springer International Publishing Switzerland 2014
Keywords
LPG; Gasolines; Kerosenes; Aviation turbine fuels; Jet fuels; Gas oils; Fuel oils; Lube oils; Heavy
fractions; Test methods; ASTM tests and specifications
Introduction
This chapter is concerned mostly with the laboratory testing for the control of petroleum products. It
will be concerned with those tests that establish the quality of refinery streams and in some finished
and salable products. What are not covered are those specialized tests such as mass spectrometry,
motor road tests, and the like. Where possible, sketches of test apparatus are included. Most of these
tests are performed in the refinery laboratory and generally follow the methods provided by the
respective ASTM numbered tests.
The most common tests to check the quality of finished products cover the following:
• Specific gravity
• ASTM distillations
• Pensky–Martens closed-cup flash point
• Kinematic viscosities
• Octane numbers
• Sulfur content tests
• LPG weathering tests
• Reid vapor pressure
• Bromine number
The chapter begins with some details of typical product specifications. More discussions and
descriptions of modern-day trends in product quality (such as the effect of reformulated gasoline) are
given elsewhere in this book.
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LPG
This category includes the normal specifications for propane and butane LPG. The detailed
requirements for LPG are specified in ASTM D1835. Regular issues are currently available, from
1997 to 2013. Table 1 provides a typical specification.
Gasolines
Two grades of gasoline are given here. They represent the present-day and near-future quality
requirements meeting the environmental parameters already discussed earlier in this volume. The
two grades are:
• Regular grade
• Premium grade (100 octane)
The specifications given in Table 2 cover the present-day quality requirements. Note that only the
major quality items and tests are listed here (also refer to Appendix 1 for updates).
In the United States (Federal Register, vol. 79, no. 81, April 28, 2014) required reductions in the
gasoline sulfur content under the Tier 2 program began in 2004 with refinery and importer caps of
300 wt-ppm and a corporate average cap of 120 ppm. For most refiners and importers, compliance
with the final sulfur standards (30 annual average and 80 per-gallon cap) was required beginning in
2006. The Tier 2 program was fully implemented on January 1, 2011. Under the Tier 3 program,
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gasoline and any ethanol-gasoline blend is required to have a sulfur level of 10 ppm or less on an
annual average basis beginning January 1, 2017. In addition, refiners and importers continue to be
subject to a refinery gate per-gallon sulfur cap of 80 ppm, and gasoline downstream of the refinery
gate subject to a 95 ppm per-gallon sulfur cap (possibly subject to further reductions). Many other
specifications may apply; for example, the vapor lock index, the driveability index, the volatility
specifications (ASTM D4814), etc. which should be consulted as appropriate.
Kerosenes
There are three grades of kerosenes which are common in most refineries. These are:
• Odorless kerosene
• Regular-grade kerosene
• Premium kerosene
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them is their flash point temperature. The minimum flash point for JP-8 is 38 C while that for JP-5 is
60 C. The higher flash point for JP-5 is for the safer handling of the fuel on aircraft carriers.
Appropriate updates should be consulted as they become available. Also, separate specifications
apply to biojet fuel and to synthetic fuels (e.g., Fischer-Tropsch). Detailed descriptions are available
from various oil companies (e.g., Chevron, Shell, etc.)
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Table 5 Compares several of the specification properties of the major civilian jet fuels
Fuel Jet A Jet A-1 TS-1 Jet B
Specification ASTM D DEF STAN GOST 10227 CGSB-3.22
1655 91-91
Acidity, mg KOH/g 0.10 0.015 0.7 (mg KOH/100 0.10
ml)
Aromatics, % vol, max 25 25.0 22 (% mass) 25.0
Sulfur, mass% 0.30 0.30 0.25 0.40
Sulfur, mercaptan, mass% 0.003 0.003 0.005 0.003
Distillation, °C
Initial boiling point – Report 150 Report
10 % recovered, max 205 205 165 Report
50 % recovered, max Report Report 195 Min 125;
max 190
90 % recovered, max Report Report 230 Report
End point 300 300 250 270
Vapor pressure, kPa, max – – – 21
Flash point, °C, min 38 38 28 –
Density, 15 °C, kg/m3 775–840 775–840 Min 774 at 20 °C 750–801
Freezing Point, °C, max −40 −47.0 −50 (Chilling point) −51
Viscosity, –20 °C, mm2/s, max 8 8.0 8.0 at −40 °C –
Net Heat of combustion, MJ/kg, min 42.8 42.8 42.9 42.8
Smoke point, mm, min 18 19.0 25 20
Naphthalenes, vol%, max 3.0 3.00 – 3.0
Copper corrosion, 2 h at 100 °C, max No. 1 No. 1 Pass (3 h at 100 °C) No. 1
rating
Thermal stability
Filter pressure drop, mmHg, max 25 25 – 25
Visual tube rating, max <3 <3 – <3
Static test 4 h at 150 °C, mg/100 ml, – – 18 –
max
Existent gum, mg/100 ml, max 7 7 5 –
Gas Oils
Three grades of gas oils are considered here. They are:
Heating oil is used predominately as domestic heating oil in many countries. Its most important
properties are the pour point and sulfur content. A full specification of the gas oil is given in Table 6.
The specification for automotive-grade gas oil (diesel fuel) is given in Table 7. Certain properties
of this product are more stringent than those for heating oil to meet the present environmental
requirements and the present design features of the diesel engines. The one item that stands out as
being very stringent is the sulfur content of the diesel. This specification became effective in 2002.
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More stringent specifications have applied since 2006. In the past, diesel engine manufacturers
have produced engines to meet the increasingly stringent emissions standards through improve-
ments to the combustion process itself. In order to meet additional regulatory standards (U.S. 2007+,
Europe 2009+), most new diesel engines will need to employ some type of advanced exhaust after-
treatment technology. Because most exhaust after-treatment devices are very sensitive to sulfur
(some devices can be permanently damaged by prolonged exposure to fuel sulfur levels as low as
50 ppm), vehicles so equipped must use ultra-low sulfur diesel (ULSD) fuel, officially designated as
S15 in the ASTM diesel fuel standard. The term “ultra-low sulfur diesel” may refer to different levels
of sulfur in different parts of the world. However, for the purposes of this review (Chevron, Diesel
Fuels Technical Review, 2007), ULSD refers to diesel fuel containing less than 15 ppm sulfur in the
U.S. and less than 10 ppm sulfur in Europe and the Asia-Pacific region.
In California, the Air Resources Board (ARB) has regulated an additional requirement. All diesel
fuel sold in this state must have an aromatics content of 10 mass percent or less. Alternatively, a fuel
supplier can test and certify a fuel with higher aromatics level, if emissions are equivalent to those of
a specific reference fuel with a 10 mass percent aromatics level. In that case, other fuel properties
(cetane number, sulfur, nitrogen, aromatics, and polynuclear aromatics) are recorded. Fuel marketed
under this certification must be within the recorded limits of these five properties.
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Table 7 Specification for diesel fuels (also refer to Appendix 1 for updates)
Properties Method of test
Specific gravity at 60 F 0.820–0.860 ASTM D1298
Color NPA 3 max ASTM D155
Pour point ASTM D97
Summer, F 15
Winter, F 7
Cloud point ASTM D97
Summer, F N/A
Winter, F N/A
Sulfur, wt% 0.1a ASTM D129
Diesel index 54 min IP 21
Cetane number 47 min ASTM D613
Distillation
Recovered at 230 C, vol% 10 min ASTM D158
Recovered at 240 C, vol% 50 max
Recovered at 347 C, vol% 50 min
Recovered at 370 C, vol% 95 max
FBP, C 385 max
Flash point (PM), F 140 min ASTM D93
Copper strip (3 h at 100 C) 1 max ASTM D130
Viscosity at 100 F, SUS 35.9 max ASTM D88
Carbon residue (Conradson) on 10 % Btms, wt% 0.25 max ASTM D189
Ash, wt% 0.1 max ASTM D482
Water by distillation, wt% 0.02 max ASTM D95
Sediment by extraction, wt% 0.005 max ASTM D473
Calorific value (gross), Btu/lb Not specified ASTM D240
a
Down to 50 wt-ppm (0.005 wt%) for ultra-low-sulfur diesel
ULSD became widely available in Western Europe and Japan (10 ppm sulfur maximum) starting
in 2005; the U.S. (15 ppm sulfur maximum) followed in 2006. Full transition to ULSD has occurred
over a period of several years, with 100 % of on-highway and off-road diesel meeting ULSD
specifications by 2009 in Europe and by 2010–2014 in the U.S. While ULSD enables use of
advanced exhaust after-treatment technology on new diesel engines, it is also fully compatible
with, and will help reduce sulfate emissions from, existing older technology diesel engines.
The third gas oil product is really a blend of the gas oil distillate and atmospheric residuum. Its
color is black and has the following much reduced specification. This is given in Table 8.
A variety of fuels are available for marine diesel engines (Chevron, Diesel Fuels Technical
Review, 2007). There is a set of four marine distillate fuels, some of which contain small amounts
of resid, and a set of 15 marine residual fuels in which resid is the majority constituent.
Marine fuels range in viscosity from less than one centistoke (cSt) to about 700 cSt at 50 C (122 F)
(1 cSt=1 mm2/s). The higher viscosity grades are preheated during use to bring their viscosity into
the range suitable for injection (8–27 cSt). Marine fuels also contain more sulfur than on-road diesel
fuel, although, in some areas and ports, only low sulfur fuels are permitted. The maximum sulfur
limit varies from 1 % to 4.5 % by mass for different grades and Sulfur Emission Control Areas
(SECAs).
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Table 8 Specification for marine diesel fuel (subject to revisions, especially sulfur content)
Properties Method of test
Specific gravity at 60 F 0.840 min ASTM D1298
Pour point – winter, F 15 max ASTM D97
Sulfur, wt% N/A ASTM D129
Diesel index 50 min IP 21
Flash point (PM), F 150 min ASTM D93
Viscosity at 100 F, SUS 32.0–43.9 ASTM D88
Carbon residue (Conradson) on 10 % Btms, wt% 0.2 max ASTM D189
Several organizations issue marine fuel specifications. ISO 8217 of the International Standards
Organization (ISO) is the primary standard. The International Maritime Organization (IMO) also
develops regulations for shipping. Among the measures adopted within IMO is MARPOL (the
International Convention for the Prevention of Pollution from Ships); this is the main international
convention covering the prevention of operational or accidental pollution of the marine environment
by ships. MARPOL Annex VI also limits the usage of fuels to prevent air pollution.
The shipping industry prefers higher viscosity residual fuels because they are less expensive.
Although residual fuels do not burn as readily as distillate fuels, the slow speeds (60–200 rpm) of the
large marine engines allow more time for combustion to occur.
Lube Oils
Most marketable lube oils produced in a refinery are graded by their viscosity. Proprietary brands of
these lube oil grades will contain additives as provided by their particular marketing outlets. These basic
grades and their specification are given in Table 10. Other specifications apply for multigrade lube oils.
These grades and their processing are described in some detail in the discussion of “non-energy
refineries.”
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Asphalts
The production of the asphalt grades and their specification have been described and discussed under
“non-energy refineries.” A good source of information is the Asphalt Paving Design Guide available
from the Asphalt Paving Association of Iowa (undated).
Petroleum Coke
Petroleum coke is not found in crude oil, but is the carbon compound formed from the thermal
conversion of petroleum containing resins and asphaltenes. Coke is formed in the processes to
convert the residuum fuels to the more desirable distillate products of naphtha and lighter, through to
the middle distillates. There are two routes by which this coking process proceeds. The first and the
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most common is the delayed coking route. The second is the fluid coking method, and this has been
made more attractive to many refiners with the development of ExxonMobil’s proprietary process of
FLEXICOKING. This proprietary process eliminates the coke completely by converting it to
low-Btu fuel gas. By far the largest production of coke is the sponge coke from the delayed coking
process. Uncalcined sponge coke has a heating value of about 14,000 Btu/lb and is used primarily as
a fuel. High-sulfur sponge coke however is popular for use in cement plants since the sulfur reacts to
form sulfates. Sponge coke is calcined to produce a coke grade suitable for anodes in the aluminum
industry. Details of the specifications for green (uncalcined) coke and calcined coke are given in
Table 11.
Sulfur
Sulfur is a by-product of modern-day refineries. By the processes that make up the modern hydrogen
skimming refinery, a significant portion of the sulfur contained in the crude is removed as elemental
sulfur for marketing as a product. It is true to say that as the environmental requirements for the
reduced sulfur levels in products and emissions from the refinery decrease, the sulfur produced as a
product increases. In most countries today, over half of the required sulfur is produced from the
petroleum and gas industries. Sulfur is stored and transported from the refinery as a molten product
or as solid sulfur. Almost half the world’s sulfur production is used in making sulfuric acid and
phosphate fertilizers using the sulfuric acid produced from the sulfur. A typical specification for
sulfur is given in Table 12.
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A
B
F
D E
C
items such as motor vehicle road tests. Those tests described briefly in the following sections are
those listed earlier.
141:5
Specific Gravity ¼
131:5 þ API
The calculation of the weight per unit volume from the specific gravity is based on the US measure of
volume (i.e., US gallons). A summary table of the relationship between specific gravity at 60 F,
API, and lbs per gallon is shown in Table 13.
ASTM Distillations
There are two types of ASTM distillations that are used in the refinery for plant control and finished
product quality. These are the ASTM D86 for naphtha and its equivalent products and for
kerosenesand ASTM D1160. ASTM D1160 is an equivalent method run at reduced pressures.
ASTM D86
The diagram in Fig. 1 is the apparatus used for ASTM distillations. Only the apparatus item sizes
will change and the temperature levels in the condenser bath. The measured sample is introduced
into a glass Engler flask (A) at 100 ml for the D86 test. The liquid fills about two-thirds of the flask,
leaving the space above the liquid to the cork in the vessel neck as vapor space. About halfway along
the neck of the flask, there is a vapor offtake tube. The open end of this tube is connected to the
condenser tube which is routed through the condenser bath (B). This condenser tube emerges from
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the “bath” and the open end is directed into a measuring cylinder. For the lower-boiling-range
samples (i.e., naphthas), this cylinder is placed in a cold water (slightly below room temperature)
bath. The Engler flask rests on an asbestos or similar plate (F) which has a hole 100 in diameter
exposing the bottom of the flask to the heat source. In this case the heat source is shown as a Bunsen
burner (C). A thermometer is introduced into the top of the flask and is positioned so that the bulb is
directly in line with the vapor offtake. The condenser bath is filled with water and ice and allowed to
reach 32 F before heat is applied to the sample flask and the test begun. The temperature of the
sample is increased slowly until the liquid begins to boil. The initial boiling point is read as the
temperature measured by the thermometer located in the flask when the first condensate drop enters
the receiving cylinder (D) at the end of the condensate bath (B). For low-boiling-point samples (i.e.,
naphthas), this receiver is cooled in a water bath (E). For kerosenes, the water bath (E) is not
required. The test is allowed to proceed at a constant rate and temperature readings are taken at
predetermined recovery levels of condensate (usually, these temperatures will be at 10 vol%
recovered and 30, 50, and 90 vol% recovered). When the flask (A) has been boiled apparently
dry, the temperature shown by the thermometer will rise sharply and then begin to fall. The highest
temperature observed in this rise and fall is the final boiling point of the sample.
ASTM D93
A brass test cup is filled to an inside mark with the test specimen. A cover is fitted of specified
dimensions; see Fig. 2. The specimen is heated and stirred at specified rates. An ignition source in the
form of a small flame is directed into the cup at regular intervals. When the specimen is seen to flash,
the temperature of the specimen is noted as the flash point of the sample.
Significance and Use The flash point is a measure of the tendency of the material to form a
flammable mixture with air under controlled laboratory conditions. It is however only one of several
properties that must be considered in assessing the overall flammable hazard of the material. The
flash point is used to establish the flammable criteria in transporting the material. Generally, shipping
and safety regulations will be based on the flash point criteria. The flash point should NOT however
be used to describe or appraise the fire hazard or risk under actual fire conditions. This test method
(D93) provides the only closed-cup flash point test procedures for temperatures up to 698 F.
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PILOT SHUTTER
FRONT
HANDLE (OPTIONAL)
(MUST NOT TIP EMPTY CUP)
LID THERMOMETER
IR GAP
A
DISTANCE PIECE
D
B C
TEST CUP
E
TOP PLATE
STOVE mm in.
min max min max
AIR BATH A 4.37 5.16 0.172 0.203
B 41.94 42.06 1.651 1.656
F MIN THICKNESS C 1.58 3.18 0.062 0.125
OVER CUP AREA D ... 9.52 . . . 0.375
IE,METAL SURROUNDING E 57.23 57.86 2.253 2.278
THE CUP F 6.35 . . . 0.25 . . .
HEATER FLAME-TYPE
OR ELECTRIC RESISTANCE
TYPE {FLAME TYPE SHOWN}
ASTM D97
The apparatus used to determine pour point (and cloud point) consists of a cylindrical glass jar with a
flat bottom and a cork stopper at its top. A thermometer is inserted through the cork stopper so that
the bulb is immersed up to 3 mm of the capillary in the specimen. The sample is inserted into the jar
up to a prescribed level. The apparatus is shown in the following Fig. 3 and is self-explanatory.
The sample is first heated as follows:
Material with an estimated pour point above 33 C – heat to a temperature of expected pour point
plus 9 C but at least 45 C in a bath controlled to at least 48 C. Material with an expected pour point
of below 33 C – heat to at least 45 C and cool to 15 C in a bath controlled at 6 C.
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THERMOMETER
30 - 32.4 ID.
CORK 33.2 - 34.8 OD.
JACKET
25 MAX.
COOLANT LEVEL
TEST JAR
115 - 125
FILL LEVEL
115
5
CASKET
COOLING BATH
6
DISK
NOTE 1- Dimensions are in millimetres (not to scale).
Commence the test then by sequential cooling and observing the flow of the specimen using
cooling baths as follows:
The specimen is checked at regular intervals of cooling (every 3–5 C) for flow. This checking
must be done with great care by just slowly tilting the jar to the horizontal position for not more than
5 s and observing if there is flow. The moving of the sample from bath to bath should be at the
following schedule:
Specimen at 27 C Move to bath 1
Specimen at 9 C Move to bath 2
Specimen at 6 C Move to bath 3
Specimen at 24 C and below Move to bath 4
The pour point is reported as the temperature where no flow is observed plus 3 C.
Kinematic Viscosity
The kinematic viscosity of oil is obtained by measuring the time required for a sample of the oil to
flow, under gravity, through a capillary. The capillary is a part of the calibrated viscometer and the
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18
L N
16. 5 16. 5
K
L − 11
k−6
N−6
75
D
E
35 C−
F
300
R
1 45
15
5
A−26
A
45
P
flow of the oil through it is at a known temperature. These viscometers come in several sizes and
differing designs. The configuration and size of the capillary are calibrated and tested to provide a
constant value for that particular viscometer.
ASTM D446
The viscometer shown in Fig. 4 is one of many types. It is used for obtaining the viscosity of
transparent liquids. The viscometer shown in Fig. 4 is designated as SIL. Its important features and
its calibration constants are given in Table 14.
The viscometer(s) shown may be one of many. These are suspended using a specially designed
holder in a bath containing water with some glycol added to reduce vaporization or prevent boiling.
The bath is maintained at a constant temperature at which the viscosity is to be reported. The test
temperature may be as high as 100 C, thus the use of glycol in the bath water to prevent actual boiling.
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Bourdon Pressure
Gage
Screw Connection
The oil sample is introduced into the viscometer through tube L by tilting the viscometer to about
30 from the vertical with bulb A below capillary R. After introducing the sample, attach the
viscometer into the holder and insert the viscometer into the bath so that it is vertical. Allow
the sample to reach the bath temperature, usually about 30 min before starting the test. Using suction
(all laboratories should have a vacuum system), draw up the sample through bulb C to about 5 mm
above the upper timing mark E. Release the vacuum and allow the sample to flow by gravity.
Measure the time for the sample to flow from the timing mark E to the lower timing mark F. This is
the time t in the equation
V ¼Ct
where
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38 mm (1 1/2 in.)
TOLERANCE
3 mm (1/8 in.)
ARMORED
THERMOMETER
SLOTTED CORK
25 mm (1 in.)
MINIMUM
100
90
80
TOLERANCE 3 mm (1/8 in.)
70
203 mm (8 in.)
60
50
40
30
20
TOLERANCE 9.5 mm (3/8 in.)
15
10
86 mm (3 3/8 in.)
INSIDE TOL. 8 mm (1/32 in.)
8
6
5
4
3
(27/32 in.)
21 mm
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ASTM D323
In the above diagram, A represents the vapor chamber which has a length of 254 mm and a diameter
of 51 mm. The ratio of the volume of the vapor chamber A to the liquid chamber B shall be between
3.8 and 4.2. The diameters of both the vapor chamber and the liquid chamber shall be the same. The
liquid test sample is placed in the liquid chamber to fill the vessel. The liquid chamber is then
connected to the vapor chamber and the pressure gauge inserted as shown in the diagram. The
assembled apparatus is then immersed vertically in a water bath up to a level of 190 mm of the vapor
chamber. The water bath is kept at a temperature of 100 F for 30 min and then removed, tilted once
or twice, and replaced for 15 min further. At the end of this time, the vapor pressure of the test sample
is read from the pressure gauge to the nearest 0.2 psi.
ASTM D1837
Testing a Butane or a Butane–Propane Mixture If the sample is at a temperature of 10 F or
below, allow it to weather in the atmosphere to 10 F then introduce the thermometer and assemble
the apparatus as shown in Fig. 6. Place the weathering tube vertically in a water bath (temperature
between 60 F and 70 F), submerging it to the 1.5 ml mark on the tube. Record the temperature
when 95 % of the sample has evaporated.
Weathering Propane-Type LPG Allow the test sample to weather in the atmosphere. Clean off the
frost that will accumulate on the vessel outer surface with a swab containing acetone or alcohol.
Read off the temperature at 95 % as in the case for butane.
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CHIMNEY
SCALE
WICK
GUIDE
GALLERY
CANDLE
SOCKET
CANDLE
maximum height of flame that can be achieved without smoking. The apparatus that is used for this
test is shown in Fig. 7.
ASTM D1322
Calibrating the Apparatus The apparatus is calibrated daily against known aromatic compound
smoke points to establish a correction factor. The two reference fuel blends are toluene and 2,2,4-
trimethyl pentane, and details of these fuels are given in Table 16.
The smoke points of the blends are determined in the same way as the test procedure given below.
From the calibrating readings, the correction factor f is determined from the equation
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40mm
H
81mm
50 50 130mm
40 40
30 30
20 20 G
10 10
0 0
F
E C
23.8
mm
Dimensions in mm
Candle Socket C internal diameter 23.8
Wick Guide C internal diameter 6.0
Air inlets 20 in number E diameter 2.9
Galary F internal diameter 35.0
Air inlets 20 in number 3.5
Lamp Body G internal diameter 81.0
Internal depth 81.0
Chimney H internal diameter 40
Top of chimney to center
of lamp body 130
where
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47mm
22mm
60mm
90mm 109mm
21.25mm
3.5mm
Dimensions in mm
Candle Body: Internal diameter 21.25
External diameter Sliding fit in holder
Length without cap 109
9.5 mm dia 1.0 mm
Thread on cap
screw pitch
1.0 Soak a piece of extracted and dried wick about 125 mm in length in the test sample, and place it
in the wick tube of the candle. Carefully ease out any twists arising from this operation.
2.0 Introduce about 20 ml of the test sample into the clean dry candle; place the wick tube into the
candle and screw and secure. Then, insert the candle into the lamp.
3.0 Light the candle and adjust the wick so that the flame is approximately 10 mm high. Allow the
lamp to burn for 5 min. Raise the candle until a smoky tail appears, and then lower the candle
slowly until the following stages occur:
• First stage: An elongated pointed tip as shown in Flame A in Fig. 10.
• Second stage: The pointed tip just disappears, leaving a slightly blunted flame shown as
Flame B in Fig. 10.
• Third stage: A well-rounded flame tip as shown in Flame C in Fig. 10.
The correct flame profile is Flame B. Determine the height of this flame and record to the
nearest 5 mm.
4.0 Make three separate observations using the same flame sequence as given in item 3.0 above. If
these values vary by more than 1.0 mm, repeat the test with a fresh sample.
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A - Too High
B - Correct
c - Too Low
Base of
Flame
5.0 The smoke point is calculated to the nearest 1.0 mm using the following equation
Smoke point ¼ L f
where
L = the average value of Flame B over the three individual test readings (item 0.4)
f = the correction factor rounded to the nearest 0.01
ASTM D189
The apparatus consists of a porcelain crucible containing a weighed sample of the oil. This crucible
is placed in the center of an iron crucible which is itself placed in a larger iron crucible. Both iron
crucibles are fitted with covers and are vented through a metallic hood. This assembly is placed on a
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Handbook of Petroleum Processing
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# Springer International Publishing Switzerland 2014
3
DIA
50
89 DIA
50–60
HOOD
78–82
DIA
60–67
HORIZONTAL DIA
125–130
OPENING 53–57 L DIA
6-5 APPROX 46–49
L DIA
IRON CRUCIBLE
50–53
0-8 THICK
58–60
37–39
IRON CRUCIBLE
65–82mL CAPACITY
32–38
PORCELAIN
CRUCIBLE
29–31mL CAPACITY
WIRE SUPPORT
BARE NICHROME
30–32
(No 13 B & S GAUGE INSULATOR
DIA
APPROX) OR
EQUIVALENT 83 DIA
stand with a supporting wire mesh. The crucibles are partially surrounded by insulating brickwork
on which the metallic hood rests. Heat is supplied to the crucibles by a burner located below the wire
mesh support. The sample is heated for a specified period of time until all the volatile content of the
oil has evaporated, leaving the carbon as residue. The carbon content of the oil is calculated as the
weight of the carbon left as a percentage of the weight of the original sample.
ASTM D1159
The apparatus used in this test is any apparatus that can perform titration to a preset end point. Such
an apparatus may include an electrical meter with two polarized electrodes of sufficient voltage to
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Handbook of Petroleum Processing
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# Springer International Publishing Switzerland 2014
indicate the end point. The titration vessel is a jacketed glass vessel about 120 mm high and with
45 mm internal diameter. The sample contained in the vessel will be kept at 32–45 F. The burette
will be a normal titration burette capable of measuring the titration reagent in graduations of 0.05 ml
or smaller. Place 10 ml of 1,1,1-trichloroethane or dichloromethane in the titration vessel, and
introduce the test specimen as indicated in Table 17.
Fill the titration vessel to the mark with the selected solvent. Mix the contents well. Titrate the
sample with the standard bromine–bromate solution – stir the specimen well during the titration. The
end point is noted by a sudden change in potential on an electrometric end point indicator due to the
presence of bromine. The bromine number is calculated by the following equation
ðA BÞðM 1 Þð15:98Þ
Bromine number ¼
W
where
The olefin content of the test sample can be calculated from the bromine number by the equation
where
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Handbook of Petroleum Processing
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# Springer International Publishing Switzerland 2014
ASTM D1266
The sample is burned in a closed system using a suitable lamp (Fig. 12) and an artificial atmosphere
of 70 % carbon dioxide and 30 % oxygen to prevent the formation of nitrogen oxides (Fig. 13). The
oxides of sulfur are absorbed and oxidized to sulfuric acid by means of a hydrogen peroxide
solution. This solution is flushed with air to remove carbon dioxide. The sulfur as sulfate in the
absorbent is determined by titration of the sulfuric acid with standard sodium hydroxide. The sample
size for direct combustion is 10–15 g; if the predicted sulfur content is below 0.05 % for a predicted
sulfur content of 0.05–0.4 %, the sample size should be 5–10 g.
The calculation of the sulfur content from the titration is given by the following equation
Note 1: The calculation can be simplified by adjusting the molarity of the NaOH solution to 0.624.
Then, 1 ml of the solution will be equivalent to 0.001 g of sulfur. In this case the factor 16.03 M in the
calculation becomes 1.0.
Octane Number: Research and Motor (Details of this Test Are Given in ASTM
Standards, Part 7)
By definition, an octane number is that percentage of isooctane in a blend of isooctane and normal
heptane that exactly matches the knock behavior of the gasoline. Thus, a 90-octane gasoline matches
the knock characteristic of a blend containing 90 % isooctane and 10 % n-heptane.
The knock characteristics are determined in the laboratory using a standard single-cylinder test
engine equipped with a super sensitive knock meter. The reference fuel (isooctane and C7 blend) is
run and compared with a second run using the gasoline sample. Two octane numbers are usually
given: the first is the research octane number (RON) and the second is the motor octane number
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Handbook of Petroleum Processing
DOI 10.1007/978-3-319-05545-9_27-1
# Springer International Publishing Switzerland 2014
To Vacuum Monifold
Spray Trap
Absorber
Chimney
CO2 – O2
to
Chimney
CO2 – O2
to
Burner
Glass Rod
Support
(MON). The same basic equipment is used for both octane numbers, but the engine speed is
increased for the motor octane number. The actual octane number obtained in a commercial engine
would be somewhere between the two numbers. The significance of the two octane numbers is to
evaluate the sensitivity of the gasoline to the severity of the operating conditions in the engine.
Invariably, the research octane number is higher than the motor octane number; the difference
between them is quoted as the “sensitivity” of the gasoline.
Conclusion
The specifications and the selected tests given here represent the control measures used to establish
product quality control. Much of the testing described here is used for plant control, while all the
tests are necessary to ensure that the product quality of finished products is met. In modern refinery
practice, much of the plant control is achieved using “in-line” analyzers tied to control system
computers. These computers automatically adjust plant conditions to meet the set product quality
criteria. A similar “in-line” analysis is used for blending run-down streams for finished products.
Invariably, though, laboratory testing is still used to “spot-check” plant intermediate product quality,
and laboratory testing is always used as a final check on finished product quality.
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Handbook of Petroleum Processing
DOI 10.1007/978-3-319-05545-9_27-1
# Springer International Publishing Switzerland 2014
Pressure
Regulator Vacumm
Vacuum Manifold Manometer Supply
Flow
Lamp meter
Unit Trap
20 cm
2 cm
40 cm
Trap (10 psi)
(0.70 kg per sq cm)
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Handbook of Petroleum Processing
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# Springer International Publishing Switzerland 2014
Typical 2-D diesel fuel specifications in the United States (December 2012)
Cetane number, min 40
Cetane index, min 40a
Sulfur, ppm, max 15
Total aromatics, vol%, max 35a
Polyaromatics, wt%, max
Density at 15 C, kg/m3, min–max
Viscosity at 40 C, cSt, min–max 1.9–4.1
a
Either specification must be met
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