1、Designation: D 3042 03Standard Test Method forInsoluble Residue in Carbonate Aggregates1This standard is issued under the fixed designation D 3042; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 the carbonates.1.2 The values stated in SI units are to be regarded asstandard.1.3 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 establish appro-priate safety and health practices and det
4、ermine the applica-bility of regulatory limitations prior to use. Specific precautionstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:C 136 Test Method for Sieve Analysis of Fine and CoarseAggregates2C 294 Descriptive Nomenclature for Constituents of Natu-ral Mineral Aggre
5、gates2C 670 Practice for Preparing Precision and Bias Statementsfor Test Methods of Construction Materials2D 4753 Specification for Evaluating, Selecting, and Speci-fying Balances and Scales for Use in Soil, Rock, andConstruction Materials Testing3E 11 Specification for Wire- Cloth and Sieves for Te
6、stingPurposes43. Significance and Use3.1 The amount and size distribution of noncarbonate (in-soluble) material in carbonate aggregates 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,
7、some agencies utilize the test for acceptancepurposes to delineate carbonate aggregates that polish exces-sively and become slippery and those that will not.4. Apparatus4.1 Sieves, U.S. standard 203.2-mm (8-in.) diameter, con-forming to Specification E 11 in the following sizes:9.5-mm (38-in.)4.75-m
8、m (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)4.2 BalanceA balance having a minimum capacity of 15kg and meeting the requirements of Specification D 4753,Class GP5.4.3 Oven, of appropriate size capable of being maintained at110 6 5C (230 6 9F).4.4 A
9、gitation 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 203.2-mm (8-in.)diameter sieves.4.7 Rapid Filter Paper, acid-resistant.4.8 Safety Eyeglasses, Rubber Gloves, Apro
10、ns, 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 of the Com
11、mit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Use 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.1This test me
12、thod is under the jurisdiction of ASTM Committee D04 on Roadand Paving Materials and is the direct responsibility of Subcommittee D04.51 onAggregate Tests.Current edition approved July 10, 2003. Published September 2003. Originallyapproved in 1972. Last previous edition approved in 1997 as D 3042 97
13、.2Annual Book of ASTM Standards, Vol 04.02.3Annual Book of ASTM Standards, Vol 04.08.4Annual Book of ASTM Standards, Vol 14.02.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American
14、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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1
15、9428-2959, United States.5.2 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 Samp
16、ling Section of Test Method C 136.6.1.1 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 consta
17、nt mass at 110 6 5C(230 6 9F).6.3 Use an oven-dry sample having a minimum mass of 500g.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 sectionprovide
18、s a procedure for determination of the 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 sample
19、s in triplicate for each aggregatesampled.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
20、 equipment and can also be a definitesafety hazard to laboratory personnel. Under no circumstancesshall the test be performed without proper and adequateventilation. Operators shall be required to wear a mask whenperforming this test.7.4 Place an aggregate sample weighing a minimum of 500g in a suit
21、able borosilicate glass container. The container shallbe vented to allow gas from the reaction to escape and to bedrawn 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 con
22、tents 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 andche
23、ck 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 no
24、 reaction is observed, heat the container gentlyover a bunsen burner or hot plate. Some carbonate materialswill require heating to temperatures of up to 110C (230F) andmaintaining this temperature level for approximately1hinorder to completely react the carbonate fraction.7.7.1 If no reaction is obs
25、erved 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 tothoroug
26、hly 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
27、 (No. 200)sieve and into the receiving tank. Dry the sieve and the residueina1106 5C (230 6 9F) 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) siev
28、e size residue.7.12 Visually inspect the residue to determine if there isparticle agglomeration because of the presence of plastic clayfractions.7.12.1 If agglomeration has occurred, physical reduction ofthe agglomerated particles shall be performed by use of amortar and rubber-tipped pestle. Exerci
29、se 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 overpreweighed nested sieves. The nested sieves shall be of thefollowing series:4
30、.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 through 7.8.8.2 Wash the diluted solution and residue from the aggre-gate sample over pre-weighed nes
31、ted 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 individually and thoroughlyover the lower sieves and into the receiving tan
32、k. Dry thesieves and the residue in a 110 6 5C (230 6 9F) 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.D30420328.5 Dilute the decant acid solution in the receiving tan
33、k 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 placed in glass funnels. Thoroughly rinse withadditional
34、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 5C (230 6 9F) for24 h.8.8 Weigh the dish, dried filters, and residue. Subtract
35、 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) in a 110 6 5C (230 6 9F)oven.8.10 When the 75-m (No. 200) si
36、eve 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 thequantity established in 8.2.8.11 Exami
37、ne the residue and describe it with the aid ofsuch mineral and rock identification tests as are necessary andappropriate. Refer to Descriptive Nomenclature C 294.9. Calculation9.1 Calculate the cumulative percent of insoluble residueretained on each of the sieves listed in 8.2 expressed as apercenta
38、ge 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 residueretained on each of the sieves in the
39、 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 triplicate tests.11. Precision an
40、d Bias611.1 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 non-linear relationship ofinsoluble residue between standard deviations and the amountscontained in t
41、he 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 %.7Therefore, results of two properly conducted tests bythe same operator
42、are not expected to differ by more than 4.2.7The 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 4.9.811.3.2 Multilaboratory PrecisionThe multilaboratorystandard dev
43、iation (one-sigma limit) has been found to be 3.1percent.7Therefore, results of two properly-conducted tests indifferent laboratories on the same material should not differ bymore than 8.9.7The averages of three test results in twodifferent laboratories should not differ by more than 5.1.811.4 BiasN
44、o information can be presented on the bias ofthe procedure in this test method for measuring the insolubleresidue in carbonate aggregates, because no material having anaccepted reference value is available.12. Keywords12.1 aggregates; carbonate aggregates; friction; insolubleresidue; polish suscepti
45、bility6A Research Report is available from ASTM International headquarters. RequestRR: D041009.7These numbers represent the (1s) and (d2s) limits as described in PracticeC 670.8Calculated as described in the Definitions of Terms Specific to This Standard ofPractice C 670, for the term acceptable ran
46、ge of more than two results.D3042033APPENDIX(Nonmandatory Information)X1. PRECISION AT DIFFERENT INSOLUBLE RESIDUE LEVELSX1.1 Three carbonate aggregates, selected to represent low,intermediate, and high insoluble residue contents were tested.Data analysis was confined to the plus 75-m (No. 200) size
47、fraction of the insoluble residue.X1.2 The precision was found to vary with insolubleresidue level, with the intermediate level having the highestvariability. Data analyses by individual material provides theresults: described in Table X1.1 and Table X1.2.ASTM International takes no position respect
48、ing the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This stan
49、dard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved 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 you feel that your comments have not received a fair hearing you shouldmake your views known to th
