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ASTM D7679-10

(Test Method)

Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils

Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils

SIGNIFICANCE AND USE
Measuring the total sulfur content of feedstock oil is often a necessary component in calculations for sulfur dioxide emissions.
The carbon black industry measures sulfur content of feedstock oils along with sulfur content of carbon black products per Test Method D1619 in calculations to determine sulfur dioxide emissions for compliance with governmental reporting requirements.
SCOPE
1.1 This test method covers the instrumental determination of sulfur content in samples of carbon black feedstock oils. Values obtained represent the total sulfur content.
1.2 This test method is applicable to carbon black feedstock oils derived from petroleum, coal, and other sources which include fuel oils, residues, tars, pitches, reclaimed oils, and similar materials that are normally handled as liquids. This test method is applicable to products typically containing 0 to 5 mass % sulfur.  
1.3 The results of these tests can be expressed as mass % sulfur.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Nov-2010
ICS
75.080 - Petroleum products in general
Technical Committee
D24 - Carbon Black
Drafting Committee
D24.66 - Environment, Health, and Safety
Current Stage
Ref Project

Relations

Replaced By
ASTM D7679-11 - Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils
Effective Date
01-Nov-2011

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ASTM D7679-10 - Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils
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Standards Content (Sample)


NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D7679–10
Standard Test Method for
Sulfur Content in Carbon Black Feedstock Oils
This standard is issued under the fixed designation D7679; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope content is determined by placing the boat in a tube furnace at
1350°C in an air or oxygen-enriched atmosphere resulting in
1.1 This test method covers the instrumental determination
complete combustion. Sulfur in the sample is completely
of sulfur content in samples of carbon black feedstock oils.
oxidized to sulfur dioxide. Moisture and particulates are
Values obtained represent the total sulfur content.
removed from the gas stream by traps filled with anhydrous
1.2 This test method is applicable to carbon black feedstock
magnesium perchlorate. The gas stream is then passed through
oils derived from petroleum, coal, and other sources which
a cell in which sulfur dioxide concentration is measured by an
include fuel oils, residues, tars, pitches, reclaimed oils, and
infrared (IR) absorption detector at a precise wavelength in the
similar materials that are normally handled as liquids. This test
IR spectrum.The IR absorption detects sulfur dioxide through-
method is applicable to products typically containing 0 to 5
out the entire combustion process. The integral of the detector
mass % sulfur.
signal is the basis for the total sulfur content of a sample.
1.3 The results of these tests can be expressed as mass %
3.2 This test method is for use with commercially available
sulfur.
sulfur analyzers equipped to carry out the combustion and
1.4 The values stated in SI units are to be regarded as
measurement operations automatically.
standard. No other units of measurement are included in this
3.3 The sulfur analyzer shall be calibrated using appropriate
standard.
calibration standards (see 6.7).
1.5 This standard does not purport to address all of the
3.4 The instrument may be configured to analyze more than
safety concerns, if any, associated with its use. It is the
one element such as a carbon-sulfur analyzer. In this case, the
responsibility of the user of this standard to establish appro-
analyzer has individual detectors for each element that are
priate safety and health practices and determine the applica-
arranged in series.
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents
4.1 Measuring the total sulfur content of feedstock oil is
2.1 ASTM Standards:
often a necessary component in calculations for sulfur dioxide
D1619 Test Methods for Carbon Black—Sulfur Content
emissions.
D4057 Practice for Manual Sampling of Petroleum and
4.2 The carbon black industry measures sulfur content of
Petroleum Products
feedstock oils along with sulfur content of carbon black
D4177 Practice for Automatic Sampling of Petroleum and
products per Test Method D1619 in calculations to determine
Petroleum Products
sulfur dioxide emissions for compliance with governmental
3. Summary of Test Method reporting requirements.
3.1 In this test method, a sample of feedstock oil is weighed
5. Apparatus
in a combustion boat containing either a tungsten oxide based
5.1 There are a number of commercially available instru-
accelerator, sand or aluminum oxide absorbent, and the sulfur
ments designed to measure sulfur content in organic materials
including sulfur and carbon-sulfur combustion analyzers. This
This test method is under the jurisdiction ofASTM Committee D24 on Carbon
test method makes no specifications regarding system designs.
Black and is the direct responsibility of Subcommittee D24.66 on Environment,
5.2 Functionally,however,thefollowingarespecifiedforall
Health, and Safety.
instruments:
Current edition approved Dec. 1, 2010. Published January 2011. DOI: 10.1520/
D7679-10.
5.2.1 An analytical balance, or equivalent, that is capable of
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
a weighing sensitivity of 0.1 mg or better resolution.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.2.2 The combustion tube and boat are made of a suitable
Standards volume information, refer to the standard’s Document Summary page on
material such as mullite, porcelain, or zircon.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7679–10
5.2.3 The sample is absorbed onto a solid which may 9. Calibration
include the following materials: (1) tungsten oxide based
9.1 Calibrate the instrument per the manufacturer’s recom-
accelerator; (2) Sea sand; (3) Aluminum oxide. Refer to the
mendation using appropriate sulfur calibration standards.
instrument manufacturer’s recommendations.
9.2 Adjustment of Response of Measurement System—
5.2.4 The sample is combusted at a temperature of 1350 6
Weigh approximately 0.1 to 0.2 g of calibration standard or use
15°C in an air or oxygen-enriched atmosphere.
the recommended mass per manufacturer. Analyze the sample
5.2.5 The combustion gas is passed through an absorbent
(see Section 10). Repeat this procedure. Adjust the instrument
(anhydrous magnesium perchlorate) to remove water vapor.
as recommended by the manufacturer until the absence of drift
5.2.6 Thedetectionsystemmeasuressulfurdioxideusingan
is indicated. Insure the minimum analysis time is sufficient for
IR absorption detector at a wavelength suitable for linear
complete combustion of the sample.
res
...

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4.1 Measuring the total carbon content of feedstock oil is often a necessary component in calculations for carbon dioxide emissions, estimating yield of a process, or assessing product quality.  
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3.1 Measuring the total sulfur content of feedstock oil is often a necessary component in calculations for sulfur dioxide emissions.  
3.2 The carbon black industry measures sulfur content of feedstock oils along with sulfur content of carbon black products per Test Method D1619 in calculations to determine sulfur dioxide emissions for compliance with governmental reporting requirements.
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5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is performed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamber deposits.  
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1.1 This test method covers the determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis of an oil, and is intended to provide some indication of relative coke-forming propensities. This test method is generally applicable to relatively nonvolatile petroleum products which partially decompose on distillation at atmospheric pressure. Petroleum products containing ash-forming constituents as determined by Test Method D482 or IP Method 4 will have an erroneously high carbon residue, depending upon the amount of ash formed (Note 2 and Note 4).  
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1.3 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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5.1 Many petroleum products, and some non-petroleum materials, are used as lubricants, and the correct operation of the equipment depends upon the appropriate viscosity of the liquid being used. In addition, the viscosity of many petroleum fuels is important for the estimation of optimum storage, handling, and operational conditions. Thus, the accurate determination of viscosity is essential to many product specifications.
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1.1 This test method specifies a procedure for the determination of the kinematic viscosity, ν, of liquid petroleum products, both transparent and opaque, by measuring the time for a volume of liquid to flow under gravity through a calibrated glass capillary viscometer. The dynamic viscosity, η, can be obtained by multiplying the kinematic viscosity, ν, by the density, ρ, of the liquid.  
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ASTM D3415-98(2024)(Practice)
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SIGNIFICANCE AND USE
4.1 Oil from one crude oil field is readily distinguishable from another, and differences in the makeup of oils from the same crude oil field can often be observed as well. Refined oils are fractions from crude oil stocks, usually derived from distillation processes. Two refined oils of the same type differ because of dissimilarities in the characteristics of their crude oil feed stocks as well as variations in refinery processes and any subsequent contact with other oils mixed in during transfer operations from residues in tanks, ships, pipes, hoses, and so forth. Thus, all petroleum oils, to some extent, have chemical compositions different from each other.  
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1.1 This practice covers the broad concepts of sampling and analyzing waterborne oils for identification and comparison with suspected source oils. Detailed procedures are referenced in this practice. A general approach is given to aid the investigator in planning a program to solve the problem of chemical characterization and to determine the source of a waterborne oil sample.  
1.2 This practice is applicable to all waterborne oils taken from water bodies, either natural or man-made, such as open oceans, estuaries or bays, lakes, rivers, smaller streams, canals; or from beaches, marshes, or banks lining or edging these water systems. Generally, the waterborne oils float on the surface of the waters or collect on the land surfaces adjoining the waters, but occasionally these oils, or portions, are emulsified or dissolved in the waters, or are incorporated into the sediments underlying the waters, or into the organisms living in the water or sediments.  
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5.1 ASTM test methods are frequently intended for use in the manufacture, selling, and buying of materials in accordance with specifications and therefore should provide such precision that when the test is properly performed by a competent operator, the results will be found satisfactory for judging the compliance of the material with the specification. Statements addressing precision and bias are required in ASTM test methods. These then give the user an idea of the precision of the resulting data and its relationship to an accepted reference material or source (if available). Statements addressing determinability are sometimes required as part of the test method procedure in order to provide early warning of a significant degradation of testing quality while processing any series of samples.  
5.2 Repeatability and reproducibility are defined in the precision section of every Committee D02 test method. Determinability is defined above in Section 3. The relationship among the three measures of precision can be tabulated in terms of their different sources of variation (see Table 1).  
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5.3 A bias statement furnishes guidelines on the relationship between a set of test results and a related set of accepted reference values. When the bias of a test method is known, a compensating adjustment can be incorporated in the test method.  
5.4 This practice is intended for use by D02 subcommittees in determining precision estimates and bias statements to be used in D02 test methods. Its procedures correspond with ISO 4259 and are the basis for the Committee D02 computer software, Calculation of Precision Data: Petroleum Test Methods. The use of this practice replaces that of Re...
SCOPE
1.1 This practice covers the necessary preparations and planning for the conduct of interlaboratory programs for the development of estimates of precision (determinability, repeatability, and reproducibility) and of bias (absolute and relative), and further presents the standard phraseology for incorporating such information into standard test methods.  
1.2 This practice is generally limited to homogeneous petroleum products, liquid fuels, and lubricants with which serious sampling problems (such as heterogeneity or instability) do not normally arise.  
1.3 This practice may not be suitable for products with sampling problems as described in 1.2, solid or semisolid products such as petroleum coke, industrial pitches, paraffin waxes, greases, or solid lubricants when the heterogeneous properties of the substances create sampling problems. In such instances, consult a trained statistician.  
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4.1 Determination of the color of petroleum products is used mainly for manufacturing control purposes and is an important quality characteristic, since color is readily observed by the user of the product. In some cases, the color may serve as an indication of the degree of refinement of the material. When the color range of a particular product is known, a variation outside the established range may indicate possible contamination with another product. However, color is not always a reliable guide to product quality and should not be used indiscriminately in product specifications.
SCOPE
1.1 This test method covers the visual determination of the color of a wide variety of petroleum products, such as lubricating oils, heating oils, diesel fuel oils, and petroleum waxes.  
Note 1: Test Method D156 is applicable to refined products that have an ASTM color lighter than 0.5.
Note 2: The color of some dyed products may extend outside color range defined by the glass reference standards employed in the testing procedure. Furthermore, samples used to determine the precision and bias did not include dyed products.
Note 3: It is up to the user to determine the suitability of this test method for their dyed products.  
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Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material

SIGNIFICANCE AND USE
5.1 This practice can be used to determine if a constant, proportional, or linear bias correction can improve the degree of agreement between two methods that purport to measure the same property of a material.  
5.2 The bias correction developed in this practice can be applied to a single result (X) obtained from one test method (method X) to obtain a predicted result ( Y^) for the other test method (method Y).
Note 5: Users are cautioned to ensure that  Y^ is within the scope of method Y before its use.  
5.3 The between methods reproducibility established by this practice can be used to construct an interval around  Y^ that would contain the result of test method Y, if it were conducted, with approximately 95 % probability.  
5.4 This practice can be used to guide commercial agreements and product disposition decisions involving test methods that have been evaluated relative to each other in accordance with this practice.  
5.5 The magnitude of a statistically detectable bias is directly related to the uncertainties of the statistics from the experimental study. These uncertainties are related to both the size of the data set and the precision of the processes being studied. A large data set, or, highly precise test method(s), or both, can reduce the uncertainties of experimental statistics to the point where the “statistically detectable” bias can become “trivially small,” or be considered of no practical consequence in the intended use of the test method under study. Therefore, users of this practice are advised to determine in advance as to the magnitude of bias correction below which they would consider it to be unnecessary, or, of no practical concern for the intended application prior to execution of this practice.
Note 6: It should be noted that the determination of this minimum bias of no practical concern is not a statistical decision, but rather, a subjective decision that is directly dependent on the application requirements of the users.
SCOPE
1.1 This practice covers statistical methodology for assessing the expected agreement between two different standard test methods that purport to measure the same property of a material, and for the purpose of deciding if a simple linear bias correction can further improve the expected agreement. It is intended for use with results obtained from interlaboratory studies meeting the requirement of Practice D6300 or equivalent (for example, ISO 4259). The interlaboratory studies shall be conducted on at least ten materials in common that among them span the intersecting scopes of the test methods, and results shall be obtained from at least six laboratories using each method. Requirements in this practice shall be met in order for the assessment to be considered suitable for publication in either method, if such publication includes claim to have been carried out in compliance with this practice. Any such publication shall include mandatory information regarding certain details of the assessment outcome as specified in the Report section of this practice.  
1.2 The statistical methodology is based on the premise that a bias correction will not be needed. In the absence of strong statistical evidence that a bias correction would result in better agreement between the two methods, a bias correction is not made. If a bias correction is required, then the parsimony principle is followed whereby a simple correction is to be favored over a more complex one.
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ASTM
ASTM D6749-24(Test Method)
Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure Method)

SIGNIFICANCE AND USE
5.1 The pour point of a petroleum product is an index of the lowest temperature of its utility for certain applications. Flow characteristics, like pour point, can be critical for the correct operation of lubricating systems, fuel systems, and pipeline operations.  
5.2 Petroleum blending operations require precise measurement of the pour point.  
5.3 Test results from this test method can be determined at either 1 °C or 3 °C intervals.  
5.4 This test method yields a pour point in a format similar to Test Method D97/IP 15 when the 3 °C interval results are reported. However, when specification requires Test Method D97/IP 15, do not substitute this test method.
Note 2: Since some users may wish to report their results in a format similar to Test Method D97/IP 15 (in 3 °C intervals), the precision data were derived for the 3 °C intervals. For statements on bias relative to Test Method D97/IP 15, see 13.3.1.  
5.5 This test method has better repeatability and reproducibility relative to Test Method D97/IP 15 as measured in the 1998 interlaboratory test program (see Section 13).
SCOPE
1.1 This test method covers the determination of pour point of petroleum products by an automatic apparatus that applies a slightly positive air pressure onto the specimen surface while the specimen is being cooled.  
1.2 This test method is designed to cover the range of temperatures from −57 °C to +51 °C; however, the range of temperatures included in the (1998) interlaboratory test program only covered the temperature range from −51 °C to −11 °C.  
1.3 Test results from this test method can be determined at either 1 °C or 3 °C testing intervals.  
1.4 This test method is not intended for use with crude oils.
Note 1: The applicability of this test method on residual fuel samples has not been verified. For further information on the applicability, refer to 13.4.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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