1、Designation: D4931 06 (Reapproved 2017)Standard Test Method forGross Moisture in Green Petroleum Coke1This standard is issued under the fixed designation D4931; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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 both the preparation procedurefor samples containing free water (air drying loss (ADL) ongross moisture
3、samples) and the determination of the grossmoisture content of green petroleum coke.1.2 The values stated in SI units are to be regarded asstandard.1.2.1 ExceptionThe values given in parentheses are forinformation only.1.3 This standard does not purport to address all of thesafety concerns, if any,
4、associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationall
5、y recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D2013 Practice
6、 for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sampleof CoalD3302 Test Method for Total Moisture in CoalE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 air drying, na proce
7、ss of partial drying of a greenpetroleum coke sample to bring it to near equilibrium with theatmosphere in the room in which further reduction/division ofthe petroleum coke sample is to take place.3.1.2 air dry loss, ADL, nthe loss in mass, expressed as apercentage, resulting from each air drying op
8、eration.3.1.3 free water, nvisible unbound water in the sample.3.1.4 green petroleum coke, nsame as raw petroleumcoke.3.1.5 gross moisture, nthat moisture determined as theloss in mass in an air atmosphere under rigidly controlledconditions of temperature, time, and air flow.3.1.5.1 DiscussionTest M
9、ethod D3302 prescribes theabove controlled conditions.3.1.6 petroleum coke, nsolid, carbonaceous residue pro-duced by thermal decomposition of heavy petroleum fractions,or cracked stocks, or both.3.1.7 residual moisture, nthat moisture remaining in thesample after air drying.3.1.8 total moisture, ns
10、ynonym for gross moisture.4. Summary of Test Method4.1 This test method is based on the loss in mass of a greenpetroleum coke sample in an air atmosphere under controlledconditions of temperature, time, and air flow.4.1.1 Preparation Procedure shall be used when the petro-leum coke sample contains f
11、ree water. The gross moisturesample is weighed and air dried to equilibrate it with theatmosphere. Determination of residual moisture is that deter-mined using the Drying Oven Method. Air drying and residualmoisture losses are combined to report gross moisture.4.1.2 Drying Oven Method shall be used
12、in routine com-mercial practice when the sample does not contain free water.The sample is crushed to at least minus 25 mm (1 in.) top sievesize and divided into analytical portions of at least 500 g each.Determination of total gross moisture is calculated by summingthe results of the Drying Oven Met
13、hod and the results of thePreparation Procedure.5. Significance and Use5.1 Moisture adds mass to the coke and serves no usefulpurpose. A knowledge of the moisture content is important inthe purchase and sale of green petroleum coke, both of whichare conducted on a dry basis.1This test method is unde
14、r the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Oct. 1, 2017. Published November 2017. Originallyapproved in 1989. La
15、st previous edition approved in 2011 as D4931 06 (2011).DOI: 10.1520/D4931-06R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page
16、 onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
17、Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.2 The collection of the sample as specified for the DryingOven Method is intended for the express purpose of determin-ing the total moisture of gre
18、en petroleum coke. The standard isavailable to producers, sellers, and consumers for determina-tion when other techniques or modifications are not mutuallyagreed on.5.3 The Preparation Procedure is used only when samplecontains free water. Obtaining a representative sample of acoke source is compoun
19、ded by the presence of free water.6. Apparatus6.1 Ovens:6.1.1 Air Drying OvenAdevice for passing slightly heatedair over the sample. The oven shall be capable of maintaininga temperature of 10 C to 15 C (18 F to 27 F) above ambientwith a maximum oven temperature of 40 C (104 F) unlessambient tempera
20、ture is above 40 C (104 F), in which caseambient temperature shall be used. Air changes are to be at therate of 1 to 4/min. A typical oven is shown in Fig. 1.6.1.2 Drying Oven (for residual moisture on minus 25 mm(1.0 in.) samples sieve USAstandardforced-air type). It shallbe capable of maintaining
21、a temperature of 105 C 6 5 C andso constructed that fresh air is introduced to all parts of theoven to ensure the removal of moisture-laden air.Air flow shallbe maintained at sufficiently low velocity to prevent loss of fineparticles, (for example, one exchange per minute).6.2 Drying Pans:6.2.1 Pans
22、 for the gross moisture sample (PreparationProcedure) shall be noncorroding, mass-stable at temperatureused, and large enough so that the sample can be spread to adepth of not more than twice the diameter of the largestparticles, or not more than 25 mm (1.0 in.) depth for smallercoke. The pan sides
23、shall be 50 mm to 75 mm (2 in. to 3 in.)high.6.2.2 Pans for crushed and divided sample shall benoncorroding, mass-stable at temperature used, and largeenough so that the sample can be spread to depth of not morethan 50 mm (2 in.). The sides shall be not more than 75 mm(3 in.) high.6.3 Balances:6.3.1
24、 Balance (Gross Sample)A balance with a minimumcapacity of 10 kg and sensitive to 1 g.6.3.2 Balance (Crushed Sample)A balance with a mini-mum capacity of 4 or sufficient to weigh the pan, sample, andcontainer and sensitive to 0.1 g.6.4 Laboratory Sample ContainersNoncorroding canswith airtight, fric
25、tion top or screw top sealed with a rubbergasket and pressure-sensitive tape for use in storage andtransport of the laboratory sample. Glass containers, sealedwith rubber gaskets, can be used, but care must be taken toavoid breakage in transport.6.5 SievesMeeting Specification E11.7. Sampling7.1 The
26、 principles, terms, and procedures as set forth inPractice D2234/D2234M shall apply to the collection of thetotal moisture sample. Particular attention is directed to thesection on Sampling Coal for Total Gross Moisture Determi-nation.7.2 Proceed with determination of moisture without unnec-essary d
27、elay to minimize the loss (or gain) of moisture to air orthe walls of the sample container. Visible condensation on thewalls of the sample container indicates a moisture loss by thesample. Determine the moisture on the gross sample andinclude the sample container in the drying process adding themass
28、 loss of the container to G (mass of sample) to determinethe total moisture.8. Procedure8.1 Preparation ProcedureWhen the sample contains freemoisture, a conditioning step is needed before determininggross moisture. If the sample does not contain free water, go to8.2.8.1.1 Distribute the required nu
29、mber of increments of thegross moisture sample in a series of preweighed pans. Thesample is spread to a depth of not more than 50 mm (2 in.) ortwice the diameter of the largest particle for cokes smaller than25 mm (1.0 in.).FIG. 1 Air Drying OvenD4931 06 (2017)28.1.2 Weigh each pan with sample as it
30、 is filled from thegross sample and record the masses. Place each in an air dryingoven that has been adjusted to maintain temperature no morethan 15 C (27 F) above ambient to a maximum of 40 C(104 F). Maintain air circulation through oven at a rate of atleast one air exchange per minute, but in no c
31、ase is it to be sohigh as to blow fine particles from the pans. Gently stir thesample occasionally to ensure uniform drying.8.1.3 When the coke surfaces appear dry, remove thesample pans from the oven, cool to ambient, weigh, and recordmass to the nearest gram. Return the pans with sample to theoven
32、 and repeat the drying and weighing at two hour intervalsuntil the mass loss is less than 0.1 % h.8.1.4 Allow the sample to reach equilibrium with ambienttemperature and humidity before the final air dry mass isrecorded. Avoid excess drying. Calculate the air dry moistureloss as shown in Step 9.1.1.
33、8.1.5 Proceed with sample reduction to at least 25 mm(1 in.) and division into minimum 500 g lots in accordancewith the procedures listed in Practice D2013. Use enclosedequipment where possible to minimize moisture change.8.1.6 The crushed and divided sample, 500 g minimumshall remain in an airtight
34、 container with minimum unusedvolume until starting the determination for Residual Moistureon Prepared Sample.8.2 Residual Moisture on Prepared Sample (Drying OvenMethod):8.2.1 Determine and record the mass of the drying pan andsample container. Transfer the crushed and weighed sample,including samp
35、le container and pan, to an oven maintained at105 C 6 5 C. Dry sample to a constant mass (see Note 1).NOTE 1Time required to achieve constant mass is estimated to beapproximately 1 h per 100 g of sample. However, do not assume 5 h issufficient to dry a 500 g sample to constant mass.9. Calculation9.1
36、 Total Moisture:9.1.1 Calculate air dry losses (ADL) as follows:ADL 5 L2 2 L1!/G# 3100 (1)where:ADL = air dry loss, mass %,L1 = mass of sample after air drying,L2 = mass of sample before air drying, andG = mass of gross sample.9.1.2 Calculate the percent residual moisture, R, as followswhen the Air
37、Drying Procedure is used:R 5 L2 2 L1!/G# 3100 (2)where:R = residual moisture,L1 = mass of sample after drying,L2 = mass of sample before drying, andG = mass of sample.9.1.3 Calculate the percent total moisture, M, as followswhen the Air Drying Procedure has been used:M 5 R100 2 ADL!/100#1ADL (3)wher
38、e:M = total moisture, of sample mass %,ADL = air dry loss, of sample mass %, andR = residual moisture.9.2 Calculate the percent total moisture, M, as follows whenthe air drying stage is not used:M 5 WL2 2 WL1!/G# 3100 (4)where:M = total moisture, mass %,WL1 = mass of sample after drying,WL2 = mass o
39、f sample before drying,G = mass of sample.10. Precision and Bias10.1 PrecisionThe precision of total moisture as deter-mined in 9.1.3 by the statistical examination of the interlabo-ratory test results is as follows:10.1.1 RepeatabilityThe difference between successiveresults obtained by the same op
40、erator with the same apparatusunder constant operating conditions on identical test materialswould, in the long run, in the normal and correct operation ofthe test method, exceed the following values only one case intwenty.Repeatability 5 0.34 % (5)10.1.2 ReproducibilityThe difference between two si
41、ngleand independent results obtained by different operators work-ing in different laboratories on identical material would, in thelong run, exceed the following values only in one case intwenty.Reproducibility 5 0.58% (6)NOTE 2The values in the statements were determined in a cooperativeprogram foll
42、owing RR:D02-1007.310.2 The precision for ADL moisture as determined by Step8.1 was not determined in this program. It is believed that therewould be no difference in the precision.10.3 The interlaboratory program included six duplicatepetroleum coke samples with nine laboratories participating.10.4
43、 BiasSince there is no accepted reference material fordetermining the bias for this test method for measuring thegross moisture in green petroleum coke, no statement on biasis being made.11. Keywords11.1 air drying loss (ADL); free water; green petroleumcoke; residual moisture; total moisture3Filed
44、at ASTM International Headquarters and may be obtained by requestingResearch Report RR:D02-1007.D4931 06 (2017)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advis
45、ed that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either r
46、eapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If
47、you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individu
48、al reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 06 (2017)4
