ASTM D4530-00

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An American National Standard
Designation: D 4530 – 00
Standard Test Method for
Determination of Carbon Residue (Micro Method)
This standard is issued under the fixed designation D 4530; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope priate safety practices and to determine the applicability of
regulatory limitations prior to use. For specific hazard state-
1.1 This test method covers the determination of the amount
ments see 8.2.3 and 8.4.
of carbon residue (see Note 1) formed after evaporation and
pyrolysis of petroleum materials under certain conditions and
2. Referenced Documents
is intended to provide some indication of the relative coke
2.1 ASTM Standards:
forming tendency of such materials.
D 189 Test Method for Conradson Carbon Residue of
1.2 The test results are equivalent to the Conradson Carbon
Petroleum Products
Residue test (see Test Method D 189).
D 482 Test Method for Ash from Petroleum Products
NOTE 1—This procedure is a modification of the original method and
D 4046 Test Method for Alkyl Nitrate in Diesel Fuels by
apparatus for carbon residue of petroleum materials, where it has been
Spectrophotometry
demonstrated that thermogravimetry is another applicable technique.
D 4057 Practice for Manual Sampling of Petroleum and
However, it is the responsibility of the operator to establish operating
Petroleum Products
conditions to obtain equivalent results when using thermogravimetry.
D 4177 Practice for Automatic Sampling of Petroleum and
1.3 This test method is applicable to petroleum products that
Petroleum Products
partially decompose on distillation at atmospheric pressure and
E 1 Specification for ASTM Thermometers
was tested for carbon residue values of 0.10 to 30 % (m/m).
E 133 Specification for Distillation Equipment
Samples expected to be below 0.10 weight % (m/m) residue
2.2 IP Standard:
should be distilled to remove 90 % (V/V) of the flask charge
Specification for IP Standard Thermometers
(see Section 9). The 10 % bottoms remaining is then tested for
carbon residue by this test method.
3. Terminology
1.4 Ash-forming constituents, as defined by Test Method
3.1 Definitions:
D 482, or non-volatile additives present in the sample will add
3.1.1 carbon residue, n— in petroleum products, the part
to the carbon residue value and be included as part of the total
remaining after a sample has been subjected to thermal
carbon residue value reported.
decomposition.
1.5 Also in diesel fuel, the presence of alkyl nitrates, such as
3.1.1.1 Discussion—The amount of residue is dependent on
amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher
the test conditions of evaporation and pyrolysis. The term may
carbon residue value than observed in untreated fuel, which
be misleading here in that the residue may contain other than
may lead to erroneous conclusions as to the coke-forming
carbon decomposition products. However, the term is retained
propensity of the fuel. The presence of alkyl nitrate in the fuel
due to its wide common usage.
may be detected by Test Method D 4046.
1.6 The values stated in SI units are to be regarded as the
4. Summary of Test Method
standard. The values given in parentheses are for information
4.1 A weighed quantity of sample is placed in a glass vial
only.
and heated to 500°C under an inert (nitrogen) atmosphere in a
1.7 This standard does not purport to address all of the
controlled manner for a specific time. The sample undergoes
safety concerns, if any, associated with its use. It is the
coking reactions, and volatiles formed are swept away by the
responsibility of the user of this standard to establish appro-
Annual Book of ASTM Standards, Vol 05.01.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on Annual Book of ASTM Standards, Vol 05.02.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 14.03.
D02.06 on Analysis of Lubricants. Annual Book of ASTM Standards, Vol 14.04.
Current edition approved May 10, 2000. Published August 2000. Originally Methods for Analysis and Testing, Institute of Petroleum Standard Methods for
published as D 4530 – 85. Last previous edition D 4530 – 85. Petroleum and Its Products, Part I, Vol 2. Available from Institute of Petroleum, 61
See Fuel, Vol 63, July 1984, pp. 931–934. New Cavendish St., London, WIM 8AR, UK.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D4530–00
nitrogen. The carbonaceous-type residue remaining is reported 6.3 Eyedropper or Small Rod, for sample transfer.
as a percent of the original sample as “carbon residue (micro).”
6.4 Coking Oven with circular heating chamber approxi-
4.1.1 When the test result is expected to be below 0.10 % 3
mately 85 mm (3 ⁄8 in.) in diameter by 100-mm (4-in.) deep,
(m/m), the sample can be distilled to produce a 10 % (V/V)
for top loading, with heating capability from 10 to 40°C/min
bottoms, prior to performing the test. 1
rate to 500°C, with exhaust port 13-mm ( ⁄2-in.) inside diameter
for nitrogen purge of oven chamber (inlet near top, exhaust at
5. Significance and Use
bottom center) with thermocouple sensor located in oven
5.1 The carbon residue value of the various petroleum
chamber next to but not touching sample vials, with lid capable
materials serves as an approximation of the tendency of the
of sealing out air, and with removable condensate trap located
material to form carbonaceous type deposits under degradation
at the oven chamber base. A schematic diagram is given in Fig.
conditions similar to those used in the test method, and can be
2.
useful as a guide in manufacture of certain stocks. However,
6.5 Sample Vial Holder—Cylindrical aluminum block, ap-
care needs to be exercised in interpreting the results.
proximately 76 mm (3 in.) in diameter by 16-mm ( ⁄8-in.) thick,
5.2 This test method offers advantages of better control of
with twelve evenly spaced holes (for vials) each 13 mm ( ⁄2 in.)
test conditions, smaller samples, and less operator attention
in diameter by 13-mm ( ⁄2-in.) deep. The holes are arranged in
compared to Test Method D 189, to which it is equivalent.
a circular pattern approximately 3 mm ( ⁄8 in.) from the
5.3 Up to twelve samples may be run simultaneously,
perimeter. The holder has legs 6-mm ( ⁄4-in.) long, with guides
including a control sample when the vial holder shown in Fig.
to center in oven chamber, and an index mark on the side to use
1 is used exclusively for sample analysis.
as position reference. The sample vial holder is shown in Fig.
1.
6. Apparatus
6.6 A modified version of the standard sample vial holder
6.1 Glass Sample Vials, 2-mL capacity, 12-mm outside
(see Fig. 1) is required when larger glass sample vials (see 6.2)
diameter by approximately 35-mm high.
are used. The modified sample vial holder is similar in nature
6.2 Larger 4 dram glass sample vials, with a 15-mL capacity
to the twelve hole vial holder, except that there are six evenly
(20.5 to 21-mm outside diameter by 70 6 1-mm high), may be
spaced holes (for vials) each 21.2 6 0.1 mm in diameter by
used for samples that are expected to yield residues < 0.10 %
approximately 16-mm deep, arranged in a circular pattern.
(m/m) so that a more appreciable mass difference can be
determined. It should be noted that the precision statements for
the test method were determined using the 2-mL capacity vials
only (with sample residues between 0.3 and 26 % (V/V)), and
A satisfactory oven with associated automatic controls that performs this
that the precision associated with using the larger sample vials
carbon residue test is available from ALCOR, INC., 10130 Jones-Maltsberger Road,
has not been determined. San Antonio, TX 78216. This commercial unit is known as the MCRT.
FIG. 1 Sample Vial Holder and Vial
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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D4530–00
FIG. 2 Coking Oven and Lid
6.7 Thermocouple, suitable for controller and temperature Practice D 4057 or similar method, and that the laboratory has
range of interest, with exterior temperature readout, degrees received a sample of about a gallon or less. Stir the sample to
Celsius. be tested, first warming if necessary to reduce its viscosity.
6.8 Analytical Balance, with 60.1 mg sensitivity to 20 g Samples that are homogeneous liquids can be transferred
minimum weighing capacity. directly to vials using a rod or syringe. Solid materials may
6.9 Cylinder of Zero Grade Nitrogen (Industrial), with also be heated; or frozen with liquid nitrogen, and then
2-stage regulator, for delivery pressure of 0 to 200 kPa (0 to 30 shattered to provide manageable pieces.
psig). 8.1.4 Transfer an appropriate mass of the sample (see Table
1) into a tared-sample vial, reweigh to nearest 0.1 mg, and
7. Sampling
record. Place the loaded sample vials into vial holder (up to
7.1 Using the practices outlined in Practice D 4057 (manual twelve), noting position of each sample with respect to index
sampling) or Practice D 4177 (automatic sampling), ensure that mark.
a representative sample of material to be tested is obtained.
NOTE 2—A control sample can be included in each batch of samples
8. Procedure
TABLE 1 Guide for Sample Size
8.1 Sample Preparation:
Expected Carbon Recommended
8.1.1 Determine the mass of each clean sample vial being
Sample Description Residue, (m/m) % Sample Size, g
used in the sample analysis, and record the mass to nearest 0.1
Black, viscous or solid >5 0.15 6 0.05
mg.
Brown, viscous 1–5 0.5 6 0.1
8.1.2 During weighing and filling, handle vials with forceps
Lube oil consistency and 0.1–<1 1.5 6 0.5
to help minimize weighing errors. Discard the sample vials appearance, 10 % bottoms on
distillate material
after use.
Large vials only <0.1 5.0 6 1.0
8.1.3 It is assumed that a representative sample of the stock
Small vials only <0.1 1.5 6 0.5
or process has been obtained for laboratory use following
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D4530–00
being tested. This control sample should be a typical sample that has been
a 100-mL distillation, assemble the distillation
...