1、Designation: D7662 13D7662 15Standard Test Method forCarbon Content in Carbon Black Feedstock Oils1This standard is issued under the fixed designation D7662; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the instrumental determination of carbon content in samples of carbon black feedstock oils. Valuesobtained
3、represent the total carbon content.1.2 This test method is applicable to carbon black feedstock oils derived from petroleum, coal, and other sources which includefuel oils, residues, tars, pitches, reclaimed oils, and similar materials that are normally handled as liquids. This test method isapplica
4、ble to products that typically contain 75 to 94 mass % carbon.1.3 The results of these tests can be expressed as mass % carbon.1.4 UnitsThe values stated in SI units are to be regarded as standard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to addre
5、ss all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4057 Practice fo
6、r Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD7633 Test Method for Carbon BlackCarbon Content3. Su
7、mmary of Test Method3.1 In this test method, a sample of feedstock oil is weighed in a combustion boat containing a tungsten oxide based acceleratorand the carbon content is determined by placing the boat in a tube furnace at 1350C in an air- or oxygen-enriched atmosphereresulting in complete combus
8、tion. Carbon in the sample is completely oxidized to carbon dioxide. Moisture and particulates areremoved from the gas stream by traps filled with anhydrous magnesium perchlorate. The gas stream is then passed through a cellin which carbon dioxide concentration is measured by an infrared (IR) absorp
9、tion detector at a precise wavelength in the IRspectrum.3.2 This test method is for use with commercially available carbon analyzers equipped to carry out the combustion andmeasurement operations automatically.3.3 The carbon analyzer shall be calibrated using an appropriate calibration standard (see
10、 6.5).3.4 The instrument may be configured to analyze more than one element such as a carbon-sulfur analyzer. In this case, theanalyzer has individual detectors for each element that are arranged in series.4. Significance and Use4.1 Measuring the total carbon content of feedstock oil is often a nece
11、ssary component in calculations for carbon dioxideemissions, estimating yield of a process, or assessing product quality.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.66 on Environment, Health,and Safety.Curren
12、t edition approved Nov. 1, 2013June 15, 2015. Published December 2013September 2015. Originally approved in 2010. Last previous edition approved in 20112013as D7662 11.D7662 13. DOI: 10.1520/D7662-13.10.1520/D7662-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM
13、 Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made
14、to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyri
15、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 The carbon black industry measures carbon content of feedstock oils along with carbon content of carbon black productsper Test Method D7633 for Carbon Black-Carbon Content in calculations
16、to determine carbon dioxide emissions for compliancewith governmental greenhouse-gas-reporting requirements.5. Apparatus5.1 There are a number of commercial instruments available that are designed to measure carbon content in organic materialsincluding carbon and carbon-sulfur analyzers. This test m
17、ethod makes no specifications regarding system designs.5.2 Functionally, however, the following are specified for all instruments:5.2.1 An analytical balance, or equivalent, that is capable of a weighing sensitivity of 0.1 mg or better resolution.5.2.2 The combustion tube and boat are made of a suit
18、able material such as mullite, porcelain, or zircon.5.2.3 The sample is absorbed onto tungsten oxide based accelerator to control the sample combustion rate.5.2.4 The sample is combusted at a temperature of 1350C in an air- or oxygen-enriched atmosphere.5.2.5 The combustion gas is passed through an
19、absorbent (anhydrous magnesium perchlorate) to remove water vapor.5.2.6 The detection system measures carbon dioxide using an IR absorption detector at a wavelength suitable for linearresponses with respect to the concentration over the full range of possible concentrations.6. Reagents6.1 Purity of
20、ReagentsReagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society wheresuch specifications are available.3 Other grades may be used, prov
21、ided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.6.2 Magnesium Perchlorate.6.3 Oxygen, high purity, 99.9 %.6.4 Tungsten (VI) Oxide Accelerator containing potassium dihydrogen-phosphate.6.5 Calibration St
22、andard. 47. Sampling7.1 Collect a feedstock oil as specified in Practices D4057 or D4177.7.2 SampleThis is the portion or aliquot of the feedstock oil for use in obtaining a result.7.3 PreparationWarm viscous samples until they are fluid and shake for 5 s.7.4 TransferUse any convenient, clean syring
23、e or pipet to transfer a sample to the combustion boat as described in Section10.8. Preparation of Apparatus8.1 Assemble the apparatus according to the manufacturers instructions.8.2 Stabilize the furnace temperature at 1350 6 15C.8.3 Make a minimum of two determinations to condition the equipment o
24、r follow the manufacturers recommendation tocondition equipment before calibrating the instrument.9. Calibration9.1 Calibrate the instrument per the manufacturers recommendation using appropriate carbon calibration standards.9.2 Adjustment of Response of Measurement SystemWeigh approximately 0.1 g o
25、f calibration standard or use therecommended mass per manufacturer. Analyze the sample (see Section 10). Repeat this procedure. Adjust the instrument asrecommended by the manufacturer until the absence of drift is indicated. Insure the minimum analysis time is sufficient forcomplete combustion of th
26、e sample.9.3 Calibration ProcedureFollow the calibration procedure recommended by the manufacturer. Confirm the calibration byanalyzing a reference material of known carbon concentration. Reference standards should be similar to feedstock oils with carbon3 Reagent Chemicals, American Chemical Societ
27、y Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopei
28、al Convention, Inc. (USPC), Rockville, MD4 Carbon calibration and reference standards are typically available from the instrument manufacturer, and are also available from Alpha Resources, 3090 Johnson Road,Stevensville, MI 49127, .D7662 152content in the range of approximately 75 to 94 %. The measu
29、red value should be within allowable limits of the known value. Ifnot, repeat the procedure. If acceptable results are not obtained, refer to the manufacturers instructions for calibration.10. Procedure10.1 Stabilize and verify calibration of the analyzer (see 8.1 8.3 and 9.1 9.3).10.2 Confirm the f
30、urnace temperature is 1350 6 15C.10.3 Weigh approximately 0.5 to 1 g of tungsten oxide based accelerator into the combustion boat (or use a mass recommendedby the manufacturer), spreading evenly.10.4 Weigh approximately 0.1 to 0.15 g of the sample into the combustion boat (on top the accelerator).10
31、.5 Record the sample weight.10.6 Cover the sample with approximately 0.5 to 1 g of tungsten oxide based accelerator.10.7 Initiate the analysis and place the boat in the instrument using a boat puller or an auto-sampler mechanism.10.8 When the analysis is complete, the instrument should indicate the
32、carbon value. Refer to the manufacturers recommendedprocedure.11. Report11.1 The percent carbon value is obtained directly from the apparatus.11.2 Report results to the nearest 0.1 %.12. Precision and Bias512.1 These precision statements have been prepared in accordance with Practice D4483. Refer to
33、 this practice for terminologyand other statistical details.12.2 The precision results in this precision and bias section give an estimate of the precision of this test method with thematerials used in the particular inter-laboratory program described below. The precision parameters should not be us
34、ed foracceptance or rejection testing of any group of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols of the test method. Any appropriate value may be used from Table 1 for the HighTemperature Combustion Method. A common altern
35、ate method for carbon content, CHN, was included in the inter-laboratoryprogram used to generate this precision statement since a number labs use this instrumental method. Precision data specific to theCHN method is found in Table 2.12.3 A type 1 inter-laboratory precision program was conducted. Bot
36、h repeatability and reproducibility represent short-term(daily) testing conditions. The testing was performed in each laboratory performing the test twice on each of two days (total offour tests). A test result is the value obtained from a single determination. Acceptable difference values were not
37、measured.12.4 The results of the precision calculations for this test are given in Table 1. The materials are arranged in ascending “meanlevel” order.12.5 RepeatabilityThe pooled absolute repeatability, r, of this test has been established as 1.80 %. Any other value in Table1 may be used as an estim
38、ate of repeatability, as appropriate. The difference between two single test results (or determinations)found on identical test material under the repeatability conditions prescribed for this test will exceed the repeatability on an averageof not more than once in 20 cases in the normal and correct
39、operation of the method. Two single test results that differ by morethan the appropriate value from Table 1 must be suspected of being from different populations and some appropriate action taken.NOTE 1Appropriate action may be an investigation of the test method procedure or apparatus for faulty op
40、eration or the declaration of a significant5 A research report is pending.forthcoming.TABLE 1 Precision Parameters for Test Method D7662, Type 1 Precision, High Temperature Combustion, Carbon Content of FeedstockUnitsPercentMaterial Number ofLaboratories Mean Level Sr r (r) SR R (R)5. NA Tar Oil 5 8
41、0.10 0.843 2.39 2.94 2.240 6.34 7.836. Leco 502-816(85.7 % C)5 86.52 0.502 1.42 1.64 0.925 2.62 3.037. Asian Coal Tar 5 90.70 0.454 1.29 1.42 0.547 1.55 1.718. NA Coal Tar 5 91.75 0.671 1.90 2.07 0.841 2.38 2.59Average 87.49Pooled Values 0.636 1.80 2.06 1.312 3.71 4.24D7662 153difference in the two
42、materials, samples, etc., which generated the two test results.12.6 ReproducibilityThe pooled absolute reproducibility, R, of this test has been established as 3.71 %. Any other value inTable 1 may be used as an estimate of reproducibility, as appropriate. The difference between two single and indep
43、endent testresults found by operators working under the prescribed reproducibility conditions in different laboratories on identical testmaterial will exceed the reproducibility on an average of not more than once in 20 cases in the normal and correct operation ofthe method. Two single test results
44、produced in different laboratories that differ by more than the appropriate value from Table 1must be suspected of being from different populations and some appropriate investigative action taken.12.7 BiasIn test method terminology, bias is the difference between an average test value and the refere
45、nce (true) test propertyvalue. Reference values do not exist for this test method since the value or level of the test property is exclusively defined by thetest method. Bias, therefore, cannot be determined.13. Keywords13.1 carbon black; carbon content; combustion; feedstock; hydrocarbon oilASTM In
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