1、Designation: D3042 17Standard Test Method forInsoluble Residue in Carbonate Aggregates1This standard is issued under the fixed designation D3042; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n 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 determination of the percentageof insoluble residue in carbonate aggregates using hydrochloricacid solution to react th
3、e carbonates.1.2 The values stated in SI units are to be regarded asstandard. Regarding sieves, per Specification E11, “The valuesstated in SI units shall be considered standard for the dimen-sions of the wire cloth openings and the diameter of the wiresused in the wire cloth. The values stated in i
4、nch-pound unitsshall be considered standard with regard to the sieve frames.”When sieve mesh sizes are referenced, the alternate inch-pounddesignations are provided for information purposes and en-closed in parentheses.1.3 The text of this standard references notes and footnoteswhich provide explana
5、tory material. These notes and footnotes(excluding those in tables and figures) shall not be consideredas requirements of the standard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to est
6、ablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precautionstatements are given in Section 7.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization es
7、tablished 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:2C136 Test Method for Sieve Analysis of Fine and CoarseAggreg
8、atesC294 Descriptive Nomenclature for Constituents of Con-crete AggregatesC670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsD3666 Specification for Minimum Requirements for Agen-cies Testing and Inspecting Road and Paving MaterialsD4753 Guide for Eva
9、luating, Selecting, and Specifying Bal-ances and Standard Masses for Use in Soil, Rock, andConstruction Materials TestingE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Significance and Use3.1 The amount and size distribution of noncarbonate (in-soluble) material in carbonate aggr
10、egates is of interest to thoseconducting research on the polish susceptibility of stone usedin pavements or on the friction properties of pavement sur-faces. In addition, some agencies utilize the test for acceptancepurposes to delineate carbonate aggregates that polish exces-sively and become slipp
11、ery and those that will not.NOTE 1The quality of the results produced by this standard aredependent upon the competence of the personnel performing the proce-dure and the capability, calibration, and the maintenance of the equipmentused. Agencies that meet the criteria of Specification D3666 are gen
12、erallyconsidered capable of competent and objective testing/sampling/inspection, etc. Users of this standard are cautioned that compliance withSpecification D3666 alone does not completely ensure reliable results.Reliable results depend on many factors: following the suggestions ofSpecification D366
13、6 or similar acceptable guideline provides a means ofevaluating and controlling some of those factors.4. Apparatus4.1 Sieves, U.S. standard 8-in. diameter, conforming toSpecification E11 in the following sizes:9.5-mm (38-in.)4.75-mm (No. 4)2.36-mm (No. 8)1.18-mm (No. 16)600-m (No. 30)300-m (No. 50)1
14、50-m (No. 100)75-m (No. 200)4.2 BalanceA balance having a minimum capacity of15 kg and meeting the requirements of Guide D4753, ClassGP5.4.3 Oven, of appropriate size capable of being maintained at110 6 5 C.1This test method is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials
15、 and is the direct responsibility of Subcommittee D04.51 onAggregate Tests.Current edition approved April 1, 2017. Published April 2017. Originallyapproved in 1972. Last previous edition approved in 2015 as D3042 09 (2015).DOI: 10.1520/D3042-17.2For referenced ASTM standards, visit the ASTM website,
16、 www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThi
17、s international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (T
18、BT) Committee.14.4 Agitation Equipment, such as a jar mill or a magneticstirrer.4.5 Bunsen Burner or Hot Plate.4.6 Receiving Tank, of nonreactive material to receive washwater and residue washed through the 8-in. diameter sieves.4.7 Rapid Filter Paper, acid-resistant.4.8 Safety Eyeglasses, Rubber Gl
19、oves, Aprons, and so forth.4.9 Borosilicate Glass Containers, for performing acidleaching test.4.10 pH Paper or pH Meter.5. Reagent5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications
20、of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Use of other grades ispermitted, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2
21、 Hydrochloric Acid (6 N)Prepare a 6 N solution ofhydrochloric acid (HCl).6. Samples6.1 Samples shall be representative of the sources fromwhich they are obtained and shall be reduced to appropriatesize by use of sample splitters or by quartering in accordancewith the Sampling section of Test Method
22、C136.6.1.1 Normally, the aggregate used in the test sample shallbe retained after washing over the 4.75-mm (No. 4) sieve, andpassing the 9.5-mm (38-in.) sieve.6.1.2 Test separate fractions or combined aggregate grad-ings as appropriate.6.2 Dry sample aggregates to constant mass at 110 6 5 C.6.3 Use
23、an oven-dry sample having a minimum mass of500 g.7. Procedure for Determining Only the Plus 75-m (No.200) Size Fraction of Insoluble Residue7.1 For many applications, only the plus 75-m (No. 200)size insoluble residue fraction is of interest. This sectionprovides a procedure for determination of the
24、 amount and sizedistribution of only the plus 75-m (No. 200) size insolubleresidue. If the total amount of insoluble residue is desired,follow the procedure in Section 8 and only such portions ofSection 7 as are indicated in Section 8.7.2 Prepare and test samples in triplicate for each aggregatesamp
25、led.7.3 WarningHydrogen chloride gas is released duringthis procedure. Exercise extreme care to prevent corrosive gasfrom entering the laboratory atmosphere. The hydrogen chlo-ride gas that may be produced in the chemical reaction can bedestructive to laboratory equipment and can also be a definites
26、afety hazard to laboratory personnel. Under no circumstancesshall the test be performed without proper and adequateventilation. Operators shall be required to wear appropriatepersonal protective equipment (PPE) when performing thistest.7.4 Place an aggregate sample weighing a minimum of500 g in a su
27、itable borosilicate glass container. The containershall be vented to allow gas from the reaction to escape and tobe drawn away. Slowly add 1000 mL of 6 N hydrochloric acid(HCl) allowing for excessive effervescence or foaming tosubside before further addition of solution. Agitate the con-tainer and c
28、ontents gently by hand until excessive efferves-cence has subsided.7.5 Place the container and contents on an agitating device.7.6 Check the container periodically, and when the reactionappears to have subsided (no obvious bubbling), decant thesolution and add approximately 300 mL of the 6 N HCl and
29、check for a reaction. Collect all decant solution in a receivingtank for future use only if determination of the total residuecontent is desired as in Section 8.7.6.1 If a reaction (bubbling) is observed, continue agitationuntil the reaction subsides and repeat the procedure beginningat 7.6.7.7 When
30、 no reaction is observed, heat the container gentlyover a Bunsen burner or hot plate. Some carbonate materialswill require heating to temperatures of up to 110 C andmaintaining this temperature level for approximately1hinorder to completely react the carbonate fraction.7.7.1 If no reaction is observ
31、ed upon heating, proceed withthe remainder of the test procedure.7.7.2 If a reaction is observed upon heating, continue theagitation and repeat the procedure beginning at 7.7.7.8 When the reaction has stopped, decant the acid solutionand add water to the aggregate in the glass container tothoroughly
32、 dilute the acid. The residue in the container shallhave a pH as indicated by pH paper or pH meter of more than5.5.7.9 Wash the diluted solution and residue from the aggre-gate sample over a preweighed 75-m (No. 200) sieve placedover a receiving tank.7.10 Thoroughly rinse the material on the 75-m (N
33、o. 200)sieve and into the receiving tank. Dry the sieve and the residueina1106 5 C oven.7.11 When the sieve and residue have cooled to roomtemperature, weigh the sieve plus the residue and subtract theoriginal mass of the dry clean sieve to obtain the mass of theplus 75-m (No. 200) sieve size residu
34、e.7.12 Visually inspect the residue to determine if there isparticle agglomeration because of the presence of plastic clayfractions.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the Amer
35、ican Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D3042 1727.12.1 If agglomeration has occurred, physical reduction ofthe agglomerated
36、particles shall be performed by use of amortar and rubber-tipped pestle. Exercise care to preventcrushing of individual particle grains during this process.7.12.2 If no agglomeration has occurred, proceed with theremainder of the test procedure.7.13 Dry sieve the residue from the aggregate sample ov
37、erpreweighed nested sieves. The nested sieves shall be of thefollowing series:4.75-mm (No. 4)2.36-mm (No. 8)1.18-mm (No. 16)600-m (No. 30)300-m (No. 50)150-m (No. 100)75-m (No. 200)8. Procedure for Determining the Total Acid InsolubleResidue Content8.1 Perform the steps in 7.1 7.8.8.2 Wash the dilut
38、ed solution and residue from the aggre-gate sample over pre-weighed nested sieves placed over areceiving tank. The nested sieves shall be of the followingseries:4.75-mm (No. 4)2.36-mm (No. 8)1.18-mm (No. 16)600-m (No. 30)300-m (No. 50)150-m (No. 100)75-m (No. 200)8.3 Rinse each sieve with water indi
39、vidually and thoroughlyover the lower sieves and into the receiving tank. Dry thesieves and the residue in a 110 6 5 C oven.8.4 When the sieves have cooled to room temperature,weigh each sieve plus the residue and subtract the originalmass of the dry, clean sieve to obtain the mass of the residue.8.
40、5 Dilute the decant acid solution in the receiving tank withwater. The solution in the receiving tank shall have a pH asindicated by pH paper (or a pH meter) of more than 5.5.8.6 Pour the solution contained in the receiving tankthrough a 75-m (No. 200) sieve and then through rapidfiltering paper pla
41、ced in glass funnels. Thoroughly rinse withadditional water. Pre-weigh the filter papers and the evaporat-ing dish.8.7 When filtration is complete, rinse by filtering cleanwater, then transfer the paper and the residue into an evapo-rating dish and place in the oven at 110 6 5 C for 24 h.8.8 Weigh t
42、he dish, dried filters, and residue. Subtract themass of the clean filters and dish from the mass of the dish,filters, and residue to obtain the mass of the residue passing the75-m (No. 200) sieve.8.9 Dry the 75-m (No. 200) sieve and residue obtainedduring filtering process (see 8.6)ina1106 5 C oven
43、.8.10 When the 75-m (No. 200) sieve and residue havecooled to room temperature, weigh the sieve plus the residueand subtract the original mass of the dry, clean sieve to obtainthe mass of the residue (if any) retained on the 75-m (No.200) sieve from the decant solution. Add this quantity to thequant
44、ity established in 8.2.8.11 Examine the residue and describe it with the aid ofsuch mineral and rock identification tests as are necessary andappropriate. Refer to Descriptive Nomenclature C294.9. Calculation9.1 Calculate the cumulative percent of insoluble residueretained on each of the sieves list
45、ed in 8.2 expressed as apercentage of that portion of the original sample mass retainedon the 75-m (No. 200) sieve.9.2 Calculate the total percent of insoluble residue ex-pressed as a percentage of the total original aggregate samplemass.9.3 Calculate the cumulative percent of insoluble residueretai
46、ned on each of the sieves in the indicated series, expressedas a percentage of the total original aggregate sample mass.10. Report10.1 Report the following information:10.1.1 Identification and description of the aggregatesamples, and10.1.2 Calculated results for each sample and averageresults for t
47、riplicate tests.11. Precision and Bias411.1 Precision has been established only for determinationof the plus 75-m (No. 200) size fraction.11.2 Tests of three materials having widely different levelsof insoluble residue indicated a nonlinear relationship ofinsoluble residue between standard deviation
48、s and the amountscontained in the samples. These data are shown in AppendixX1.11.3 Precision Based on Weighted Average Variance for AllMaterials:11.3.1 Single-Operator PrecisionThe single-operatorstandard deviation (one-sigma limit) has been found to be1.5 %.5Therefore, results of two properly condu
49、cted tests bythe same operator are not expected to differ by more than 4.2.5The test method calls for reporting three test results. The range(difference between highest and lowest) of the three test resultsobtained by the same operator are not expected to exceed 4.9.611.3.2 Multilaboratory PrecisionThe multilaboratorystandard deviation (one-sigma limit) has been found to be 3.1percent.5Therefore, results of two properly conducted tests indifferent laboratories on the same material should not differ bymore than 8.9.5The averages of three tes
