1、Designation: C114 10aStandard Test Methods forChemical Analysis of Hydraulic Cement1This standard is issued under the fixed designation C114; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in pa
2、rentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods cover the chemical analyses ofhydraulic cements. Any test methods of demonstrated accept-able precision and bias may be used fo
3、r analysis of hydrauliccements, including analyses for referee and certification pur-poses, as explained in Section 3. Specific chemical testmethods are provided for ease of reference for those desiring touse them. They are grouped as Reference Test Methods andAlternative Test Methods. The reference
4、 test methods are longaccepted classical chemical test methods which provide areasonably well-integrated basic scheme of analysis for hy-draulic cements. The alternative test methods generally provideindividual determination of specific analytes and may be usedalone or as alternates and determinatio
5、ns within the basicscheme at the option of the analyst and as indicated in theindividual method.1.2 Contents:Section Subject2 Referenced Documents3 Description of Referee Analyses3.1 Referee Analyses4 Qualification for Different Analyses4.1 Certified Reference Materials4.2 Requirements for Qualifica
6、tion Testing4.3 Alternative Analyses4.4 Performance Requirements for Rapid Test Methods5 General5.1 Interferences and Limitations5.2 Apparatus and Materials5.3 Reagents5.4 Sample Preparation5.5 General Procedures5.6 Recommended Order for Reporting AnalysesReference Test Methods6 Insoluble Residue7 S
7、ilicon Dioxide7.2 Cements with Insoluble Residue Less Than 1 %7.3 Cements with Insoluble Residue Greater Than 1 %8 Ammonium Hydroxide Group9 Ferric Oxide10 Phosphorus Pentoxide11 Titanium Dioxide12 Zinc Oxide13 Aluminum Oxide14 Calcium Oxide15 Magnesium Oxide16 Sulfur16.1 Sulfur Trioxide16.2 Sulfide
8、17 Loss On Ignition17.1 Portland Cement17.2 Portland Blast-Furnace Slag Cement and Slag Cement18 Sodium and Potassium Oxides18.1 Total Alkalis18.2 Water-Soluble Alkalis19 Manganic Oxide20 Chloride21 Chloroform-Soluble Organic SubstancesAlternative Test Methods22 Calcium Oxide23 Carbon Dioxide24 Magn
9、esium Oxide25 Loss on Ignition25.1 Portland Blast-Furnace Slag Cement and Slag Cement26 Titanium Dioxide27 Phosphorus Pentoxide28 Manganic Oxide29 Free Calcium OxideAppendices TitleAppendix X1 Example of Determination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2Determinations in
10、 Hydraulic Cements1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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
11、 to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. See 7.3.2.1 and15.4.1 for specific caution statements.2. Referenced Documents2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone,Quicklime, and Hydrated
12、 LimeD1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.
13、Current edition approved Dec. 1, 2010. Published January 2011. Originallyapproved in 1934. Last previous edition approved in 2010 as C11410. DOI:10.1520/C0114-10a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book
14、 of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E275 Practice for
15、 Describing and Measuring Performanceof Ultraviolet and Visible SpectrophotometersE350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE617 Specification for Laboratory Weights and PrecisionMass StandardsE832 Specification for
16、Laboratory Filter Papers3. Description of Referee Analyses3.1 Referee AnalysesWhen conformance to chemicalspecification requirements is questioned, perform refereeanalyses as described in 3.1.1. The reference test methods thatfollow in Sections 6-21, or other test methods qualifiedaccording to 4.4,
17、the Performance Requirements for Rapid TestMethods Section, are required for referee analysis. A cementshall not be rejected for failure to conform to chemicalrequirements unless all determinations of constituents involvedand all necessary separations prior to the determination of anyone constituent
18、 are made entirely by these methods. Whenreporting the results of referee analyses, specify which testmethods were used.3.1.1 Referee analyses shall be made in duplicate and theanalyses shall be made on different days. If the two results donot agree within the permissible variation given in Table 1,
19、 thedetermination shall be repeated until two or three results agreewithin the permissible variation. When two or three results doagree within the permissible variation, their average shall beaccepted as the correct value. When an average of either two orthree results can be calculated, the calculat
20、ion shall be based onthe three results. For the purpose of comparing analyses andcalculating the average of acceptable results, the percentagesshall be calculated to the nearest 0.01 (or 0.001 in the case ofchloroform-soluble organic substances), although some of theaverage values are reported to 0.
21、1 as indicated in the testmethods. When a blank determination (See Note 1) is speci-fied, one shall be made with each individual analysis or witheach group of two or more samples analyzed on the same dayfor a given analyte.NOTE 1A blank determination is a procedure which follows all stepsof analysis
22、 but in the absence of a sample. It is used for detection andcompensation of systematic bias.4. Qualification for Different Analyses4.1 Certified Reference MaterialsA Certified ReferenceMaterial (CRM) must be used in the qualification of testmethods and analysts. Acceptable reference cements are NIS
23、TCRMs, or other reference cements traceable to the NISTCRMs. The reference cement must have an assigned value forthe analyte being determined. Traceability consists of docu-mentary evidence that the assigned values of the referencecement are compatible with the certified values of NISTCRMs. To demon
24、strate traceability for a given analyte, per-form a referee analysis (as defined in 3.1) on the proposedreference cement, using a NIST CRM for demonstration ofprecision and accuracy. The reference cement is acceptable ifits assigned value agrees with the average referee value withinthe limits given
25、in column 3 ofTable 1. If the reference cement,as supplied, has no documented guarantee of homogeneity,establish its homogeneity by analyzing at least six randomlyselected samples. No result shall deviate from the assignedvalue by more than the limits given in column 2 of Table 1.Anacceptable refere
26、nce cement must be accompanied by a docu-ment showing the data produced in demonstrating traceabilityand homogeneity.4.2 Requirements for Qualification TestingQualified testmethods are required whenever testing is performed for thefollowing reasons: (1) for Referee analyses; (2) for analysesintended
27、 for use as a basis for acceptance or rejection of acement; or, (3) for manufacturers certification. When Refer-ence Methods are used, qualification testing of the analyst isrequired as described in 4.2.1. When Rapid Methods are used,qualification testing of both the analyst and the test method arer
28、equired as described in 4.2.1 and 4.4. Such demonstration maybe made concurrently with analysis of the cement being tested.The requirements for qualification of a test method and analystare summarized in Table 2.4.2.1 Qualification of the analyst shall be demonstrated byanalysis of each analyte of c
29、oncern using at least one CRMcement in duplicate, no matter what test method is used (Note2). Duplicate samples shall be tested on different days. Theanalyst is considered qualified when the difference between theduplicate results does not vary by more than the value listed inColumn 2 of Table 1 and
30、 the average of the two samples agreeswith the certificate value of the CRM within the limits listed inColumn 3 of Table 1 after correction for minor componentswhen needed. The same test methods to be used for analysis ofcement being tested shall be used for analysis of the CRMcement. If either of t
31、he two requirements listed above are notmet, identify and correct any problems or errors found in theprocedure. Repeat the determinations until a set of duplicateresults agree within the permissible variations. Requalificationof the analyst is required every two years.NOTE 2When qualifying a Rapid M
32、ethod with seven CRMs inaccordance with 4.4.2, the analyst performing the qualification of the testmethod may simultaneously qualify for the requirement of 4.2.1.4.2.2 Qualification data demonstrating that the same opera-tor or analyst making the acceptance determination obtainedprecise and accurate
33、 results with CRM cements as per 4.2.1shall be made available on request to all parties concernedwhen there is a question of acceptance of a cement. If the CRMused is not a NIST cement, the traceability documentation ofthe CRM used shall also be made available on request.4.3 Alternative AnalysesThe
34、alternative test methods pro-vide, in some cases, procedures that are shorter or moreconvenient to use for routine determination of certain constitu-ents than are the reference test methods (Note 3). Longer, moreC114 10a2complex procedures, in some instances, have been retained asalternative test me
35、thods to permit comparison of results bydifferent procedures or for use when unusual materials arebeing examined, where unusual interferences may be sus-pected, or when unusual preparation for analysis is required.Test results from alternative test methods may be used as abasis for acceptance or rej
36、ection when it is clear that a cementdoes or does not meet the specification requirement. Anychange in test method procedures from those procedures listedin Sections 6-29 requires method qualification in accordancewith 4.4, the Performance Requirements for Rapid Test Meth-ods Section.NOTE 3It is not
37、 intended that the use of reference test methods beconfined to referee analysis. A reference test method may be used inpreference to an alternative test method when so desired. A reference testmethod must be used where an alternative test method is not provided.4.3.1 Duplicate analyses and blank det
38、erminations are notrequired when using the alternative test methods. If, however,a blank determination is desired for an alternative test method,one may be used and it need not have been obtained concur-rently with the analysis. The final results, when corrected forblank values, should, in either ca
39、se, be so designated.4.4 Performance Requirements for Rapid Test Methods:3,44.4.1 Definition and ScopeWhere analytical data obtainedin accordance with this test method are required, any testmethod may be used that meets the requirements of 4.4.2, theQualification of a Test Method Section. A test met
40、hod isconsidered to consist of the specific procedures, reagents,supplies, equipment, instrument, etc. selected and used in aconsistent manner by a specific laboratory. See Note 4 forexamples of procedures.NOTE 4Examples of test methods used successfully by their authorsfor analysis of hydraulic cem
41、ent are given in the list of references.Included are test methods using atomic absorption X-ray spectrometry,and spectrophotometry-EDTA.4.4.1.1 If more than one instrument, even though substan-tially identical, is used in a specific laboratory for the sameanalyses, use of each instrument shall const
42、itute a separate testmethod and each must be qualified separately.4.4.2 Qualification of a Test MethodPrior to use foranalysis of hydraulic cement, each test method (see 4.4.1) mustbe qualified individually for such analysis. Qualification data,3Gebhardt, R. F., “Rapid Methods for ChemicalAnalysis o
43、f Hydraulic Cement,”ASTM STP 985, 1988.4Barger, G. S., “A Fusion Method for the X-Ray Fluorescence Analysis ofPortland Cements, Clinker and Raw Materials Utilizing Cerium (IV) Oxide inLithium Borate Fluxes,” Proceedings of the Thirty Fourth Annual Conference onApplications of X-Ray Analysis, Denver
44、Conference, Volume 29 pg 581-585,August 5, 1985.TABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromSRM CertificateValuesC,D,BSiO2(silicon dioxide) 0.16 60.2Al2O3(aluminum oxide) 0.
45、20 60.2Fe2O3(ferric oxide) 0.10 60.10CaO (calcium oxide) 0.20 60.3MgO (magnesium oxide) 0.16 60.2SO3(sulfur trioxide) 0.10 60.1LOI (loss on ignition) 0.10 60.10Na2O (sodium oxide) 0.03 60.05K2O (potassium oxide) 0.03 60.05TiO2(titanium dioxide) 0.02 60.03P2O5(phosphorus pentoxide) 0.03 60.03ZnO (zin
46、c oxide) 0.03 60.03Mn2O3(manganic oxide) 0.03 60.03S (sulfide sulfur) 0.01ECl (chloride) 0.003EIR (insoluble residue) 0.10ECx (free calcium oxide) 0.20ECO2(carbon dioxide) 0.12E,FAlksol(water-soluble alkali)G0.75/wEChlsol(chloroform-soluble organic substances) 0.004EAWhen seven CRM cements are requi
47、red, as for demonstrating the perfor-mance of rapid test methods, at least six of the seven shall be within the prescribedlimits and the seventh shall differ by no more than twice that value. When morethan seven CRMs are used, as for demonstrating the performance of rapid testmethods, at least 77 %
48、shall be within the prescribed limits, and the remainder byno more than twice the value. When a lesser number of CRM cements arerequired, all of the values shall be within the prescribed limits.BWhere no value appears in Column 3, CRM certificate values do not exist. Insuch cases, only the requireme
49、nt for differences between duplicates shall apply.CInterelement corrections may be used for any oxide standardization providedimproved accuracy can be demonstrated when the correction is applied to allseven CRM cements.DWhere an CRM certificate value includes a subscript number, that subscriptnumber shall be treated as a valid significant figure.ENot applicable. No certificate value given.FDemonstrate performance by analysis, in duplicate, of at least one Portlandcement. Prepare three standards, each in duplicate: Standard A shall be selectedPortland cement; Standard B sha
