1、Designation: D3042 09 (Reapproved 2015)Standard 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 re
2、vision. 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 determination of the percentageof insoluble residue in carbonate aggregates using hydrochloricacid so
3、lution to react the 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
4、values stated in inch-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 This standard does not purport to address all of thesafety
5、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 determine the applica-bility of regulatory limitations prior to use. Specific precautionstatements are given in Section 7.2. Referenced Documents2
6、.1 ASTM Standards:2C136 Test Method for Sieve Analysis of Fine and CoarseAggregatesC294 Descriptive Nomenclature for Constituents of Con-crete AggregatesC670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsD3666 Specification for Minimum Requirements fo
7、r Agen-cies Testing and Inspecting Road and Paving MaterialsD4753 Guide for Evaluating, 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 amoun
8、t 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, some agencies utilize the test for acceptancepurpo
9、ses to delineate carbonate aggregates that polish exces-sively and become slippery 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 th
10、e equipmentused. Agencies that meet the criteria of Practice D3666 are generallyconsidered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance withPractice D3666 alone does not completely assure reliable results. Reliableresults de
11、pend on many factors: following the suggestions of PracticeD3666 or similar acceptable guideline provides a means of evaluating andcontrolling 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.
12、 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 D4753, ClassGP5.4.3 Oven, of appropriate size capable of being maintained at110 6 5C.4.4 Agitation Equipment
13、, 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 Gloves, Aprons, and so forth.1This test
14、method 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 Dec. 1, 2015. Published February 2016. Originallyapproved in 1972. Last previous edition approved in 2009 as D3042 09.
15、 DOI:10.1520/D3042-09R15.2For 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 onthe ASTM website.Copyright ASTM International, 100 Ba
16、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.9 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 th
17、atall reagents shall conform to the specifications 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 wit
18、hout lessening theaccuracy of the determination.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
19、accordancewith the Sampling Section of Test Method 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 sampl
20、e aggregates to constant mass at 110 6 5C.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 se
21、ctionprovides 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
22、 test samples 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 t
23、o laboratory 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 50
24、0g in a suitable 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-ta
25、iner and contents 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
26、N HCl andcheck 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
27、.7.7 When no reaction is observed, heat the container gentlyover a bunsen burner or hot plate. Some carbonate materialswill require heating to temperatures of up to 110C andmaintaining this temperature level for approximately1hinorder to completely react the carbonate fraction.7.7.1 If no reaction i
28、s observed 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 toth
29、oroughly 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
30、 75-m (No. 200)sieve and into the receiving tank. Dry the sieve and the residueina1106 5C 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
31、 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. Exercise car
32、e 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:3Reagen
33、t Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand N
34、ational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D3042 09 (2015)24.75-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
35、7.8.8.2 Wash the diluted 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
36、 sieve with water individually and thoroughlyover the lower sieves and into the receiving tank. Dry thesieves and the residue in a 110 6 5C 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 ma
37、ss of the residue.8.5 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 rapi
38、dfiltering paper placed 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 5C f
39、or 24 h.8.8 Weigh the 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
40、.6)ina1106 5C oven.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 qua
41、ntity to thequantity 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 o
42、f the sieves listed 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 insol
43、uble residueretained 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 ave
44、rageresults for triplicate 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 non-linear relationship ofinsoluble residue between
45、standard deviations 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
46、two properly conducted 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 Multila
47、boratory 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 test results in twodifferent laboratori
48、es should not differ by more than 5.1.611.4 BiasNo 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 aggreg
49、ates; friction; insolubleresidue; polish susceptibility4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D04-1009.5These numbers represent the (1s) and (d2s) limits as described in PracticeC670.6Calculated as described in the Definitions of Terms Specific to This Standard ofPractice C670, for the term acceptable range of more than two results.D3042 09 (2015)3APPENDIX(Nonmandatory Information)X1. PRECISION AT DIFFERENT INSOLUBLE RESIDUE LEVELSX1.1 Three carbonate aggregat
