1、Designation: C114 15C114 18Standard 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
2、 in parentheses 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 of hydraulic cements. Any test methods of demonstrated acceptableprecision and bias may be us
3、ed for analysis of hydraulic cements, including analyses for referee and certification purposes, asexplained in Section 4. Specific chemical test methods are provided for ease of reference for those desiring to use them. They aregrouped as Reference Test Methods andAlternative Test Methods. The refe
4、rence test methods are long accepted classical chemicaltest methods which provide a reasonably well-integrated basic scheme of analysis for hydraulic cements. The alternative testmethods generally provide individual determination of specific analytes and may be used alone or as alternates and determ
5、inationswithin the basic scheme at the option of the analyst and as indicated in the individual method.1.2 Contents:Section Subject2 Referenced Documents4 Description of Referee Analyses4.1 Referee Analyses5 Qualification for Different Analyses5.1 Certified Reference Materials5.2 Requirements for Qu
6、alification Testing5.3 Alternative Analyses5.4 Performance Requirements for Rapid Test Methods6 General6.1 Interferences and Limitations6.2 Apparatus and Materials6.3 Reagents6.4 Sample Preparation6.5 General Procedures6.6 Recommended Order for Reporting AnalysesReference Test Methods7 Insoluble Res
7、idue8 Silicon Dioxide8.2 Cements with Insoluble Residue Less Than 1 %8.3 Cements with Insoluble Residue Greater Than 1 %9 Ammonium Hydroxide Group10 Ferric Oxide11 Phosphorus Pentoxide12 Titanium Dioxide13 Zinc Oxide14 Aluminum Oxide15 Calcium Oxide16 Magnesium Oxide17 Sulfur17.1 Sulfur Trioxide17.2
8、 Sulfide18 Loss On Ignition18.1 Portland Cement18.2 Portland Blast-Furnace Slag Cement and Slag Cement19 Sodium and Potassium Oxides19.1 Total Alkalis19.2 Water-Soluble Alkalis20 Manganic Oxide21 Chloride1 These test methods are under the jurisdiction ofASTM Committee C01 on Cement and are the direc
9、t responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition approved April 15, 2015May 1, 2018. Published April 2015May 2018. Originally approved in 1934. Last previous edition approved in 20132015 asC114 13.C114 15. DOI: 10.1520/C0114-15.10.1520/C0114-18.This document is not an
10、 ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. I
11、n all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States122 Chl
12、oroform-Soluble Organic SubstancesAlternative Test Methods23 Calcium Oxide24 Carbon Dioxide25 Magnesium Oxide26 Loss on Ignition26.1 Portland Blast-Furnace Slag Cement and Slag Cement27 Titanium Dioxide28 Phosphorus Pentoxide29 Manganic Oxide30 Free Calcium OxideAppendicesAppendix X1 Example of Dete
13、rmination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2 Determinations in Hydraulic Cements1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety
14、 concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.See 8.3.2.1 and 16.4.1 for specific caution stateme
15、nts.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers t
16、o Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated LimeD1193C219 Specification for Reagent WaterTerminology Relating to Hydraulic CementE29 Practice for Using Significant Digits in Test Data to Determine Con
17、formance with SpecificationsE275 Practice for Describing and Measuring Performance of Ultraviolet and Visible SpectrophotometersE350 Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and WroughtIronE617 Specification for Laboratory Weights and
18、 Precision Mass StandardsE832 Specification for Laboratory Filter Papers3. Terminology3.1 Definitions of Terms Specific to This StandardThe terms used in this standard are defined in Terminology C219.3.2 Definitions:3.2.1 analyte, na substance of interest when performing a quantitative analysis.3.2.
19、1.1 DiscussionFor the purposes of this test method, analytes are considered to be those items listed in Columncolumn 1 of Table 1.3.2.2 reagent water, nwater purified by the process of distillation, deionization, reverse osmosis, or any combination of thethree processes.3.2.2.1 distillation, nthe pr
20、ocess of purification by the evaporation and vaporization of water and its subsequent condensationand collection.3.2.2.2 deionization, nthe process of purification using the two-step process of converting soluble salts into acids by passingthem through a hydrogen exchanger after which they are remov
21、ed by an acid absorbent or synthetic resin.3.2.2.3 reverse osmosis, nwater purification technology that uses a semipermeable membrane to remove ions, molecules, andlarger particles from drinking water.3.2.3 water (potable), nwater that is suitable for drinking.4. Description of Referee Analyses4.1 R
22、eferee AnalysesWhen conformance to chemical specification requirements is questioned, perform referee analyses asdescribed in 4.1.1. The reference test methods that follow in Sections 7 22, or other test methods qualified according to 5.4, the2 For referencedASTM standards, visit theASTM website, ww
23、w.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.C114 182TABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)MaximumDifferenceBetweenDuplicate
24、sB(Column 3)MaximumDifference oftheAverage ofDuplicates fromCRMCertificateValuesC,D,BSiO2 (silicon dioxide) 0.16 0.2Al2O3 (aluminum oxide) 0.20 0.2Fe2O3 (ferric oxide) 0.10 0.10CaO (calcium oxide) 0.20 0.3MgO (magnesium oxide) 0.16 0.2SO3 (sulfur trioxide) 0.10 0.1LOI (loss on ignition) 0.10 0.10Na2
25、O (sodium oxide) 0.03 0.05K2O (potassium oxide) 0.03 0.05TiO2 (titanium dioxide) 0.02 0.03P2O5 (phosphorus pentoxide) 0.03 0.03ZnO (zinc oxide) 0.03 0.03Mn2O3 (manganic oxide) 0.03 0.03S (sulfide sulfur) 0.01 ECl (chloride) 0.003 0.005IR (insoluble residue) 0.10 ECx (free calcium oxide) 0.20 ECO2 (c
26、arbon dioxide) 0.12 E,FCO2 (carbon dioxide) 0.12 E,FAlksol (water-soluble alkali)G 0.75/w EChlsol (chloroform-soluble organicsubstances)0.004 EA When seven CRM cements are required, as for demonstrating the performanceof rapid test methods, at least six of the seven shall be within the prescribed li
27、mitsand the seventh shall differ by no more than twice that value. When more thanseven CRMs are used, as for demonstrating the performance of rapid testmethods, at least 77 % shall be within the prescribed limits, and the remainder byno more than twice the value. When a lesser number of CRM cements
28、arerequired, all of the values shall be within the prescribed limits.B Where no value appears in Columncolumn 3, CRM certificate values do notexist. In such cases, only the requirement for differences between duplicates shallapply.C Interelement corrections may be used for any oxide standardization
29、providedimproved accuracy can be demonstrated when the correction is applied to allseven CRM cements.D Where an CRM certificate value includes a subscript number, that subscriptnumber shall be treated as a valid significant figure.E Not applicable. No certificate value given.F Demonstrate performanc
30、e by analysis, in duplicate, of at least one Portlandcement. Prepare three standards, each in duplicate: Standard A shall be selectedPortland cement; Standard B shall be Standard A containing 2.00 % CertifiedCaCO3 (such as NIST 915a); Standard C shall be Standard A containing 5.00 %Certified CaCO3 .
31、 Weigh and prepare two separate specimens of each standard.Assign the CO2 content of Standard A as the average of the two valuesdetermined, provided they agree within the required limit of Columncolumn 2.Assign CO2 values to Standards B and C as follows: Multiply the Certified CaCO3value (Y) for CO2
32、 (from the certificate value) by the mass fraction of CertifiedCaCO3 added to that standard (percentage added divided by 100); multiply thevalue determined for StandardAby the mass fraction of StandardAin each of theother standards (that is, 0.98 and 0.95 for Standards B and C, respectively); addthe
33、 two values for Standard A and for Standard B, respectively; call these valuesB and C. Example:B = 0.98A + 0.02Y.C = 0.95A + 0.05Y.Where for Certified CaCO3, if Y = 39.9 %B = 0.98A + 0.80 % by mass.C = 0.95A + 2.00 % by mass.Maximum difference between the duplicate CO2values for Standards B and C,re
34、spectively, shall be 0.17 and 0.24 % by mass. Averages of the duplicate valuesfor Standards B and C shall differ from their assigned values (B and C) by no morethan 10 % of those respective assigned values.G w = weight, in grams, of samples used for the test.C114 183Performance Requirements for Rapi
35、d Test Methods Section,section, are required for referee analysis.Acement shall not be rejectedfor failure to conform to chemical requirements unless all determinations of constituents involved and all necessary separationsprior to the determination of any one constituent are made entirely by these
36、methods. When reporting the results of refereeanalyses, specify which test methods were used.4.1.1 Referee analyses shall be made in duplicate and the analyses shall be made on different days. If the two results do not agreewithin the permissible variation given in Table 1, the determination shall b
37、e repeated until two or three results agree within thepermissible variation. When two or three results do agree within the permissible variation, their average shall be accepted as thecorrect value. When an average of either two or three results can be calculated, the calculation shall be based on t
38、he three results.For the purpose of comparing analyses and calculating the average of acceptable results, the percentages shall be calculated to thenearest 0.01 (or 0.001 in the case of chloroform-soluble organic substances), although some of the average values are reported to0.1 as indicated in the
39、 test methods. When a blank determination (See(see Note 1) is specified, one shall be made with eachindividual analysis or with each group of two or more samples analyzed on the same day for a given analyte.NOTE 1A blank determination is a procedure which follows all steps of analysis but in the abs
40、ence of a sample. It is used for detection andcompensation of systematic bias.5. Qualification for Different Analyses5.1 Certified Reference MaterialsACertified Reference Material (CRM) must be used in the qualification of test methods andanalysts. Acceptable reference cements are NIST CRMs, or othe
41、r reference cements traceable to the NIST CRMs. The referencecement must have an assigned value for the analyte being determined. Traceability consists of documentary evidence that theassigned values of the reference cement are compatible with the certified values of NIST CRMs. To demonstrate tracea
42、bility fora given analyte, perform a referee analysis (as defined in 4.1) on the proposed reference cement, using a NIST CRM fordemonstration of precision and accuracy. The reference cement is acceptable if its assigned value agrees with the average refereevalue within the limits given in column 3 o
43、f Table 1. If the reference cement, as supplied, has no documented guarantee ofhomogeneity, establish its homogeneity by analyzing at least six randomly selected samples. No result shall deviate from theassigned value by more than the limits given in column 2 of Table 1. An acceptable reference ceme
44、nt must be accompanied bya document showing the data produced in demonstrating traceability and homogeneity.5.2 Requirements for Qualification TestingQualified test methods are required whenever testing is performed for the followingreasons: (1) for Referee analyses; (2) for analyses intended for us
45、e as a basis for acceptance or rejection of a cement; or, (3) formanufacturers certification. When Reference Methods are used, qualification testing of the analyst is required as described in5.2.1. When Rapid Methods are used, qualification testing of both the analyst and the test method are require
46、d as described in 5.2.1and 5.4. Such demonstration may be made concurrently with analysis of the cement being tested.The requirements for qualificationof a test method and analyst are summarized in Table 2.5.2.1 Qualification of the analyst shall be demonstrated by analysis of each analyte of concer
47、n using at least one CRM cementin duplicate, no matter what test method is used (Note 2). Duplicate samples shall be tested on different days. The analyst isconsidered qualified when the difference between the duplicate results does not vary by more than the value listed inColumncolumn 2 of Table 1
48、and the average of the two samples agrees with the certificate value of the CRM within the limits listedin Columncolumn 3 of Table 1 after correction for minor components when needed. The same test methods to be used for analysisof cement being tested shall be used for analysis of the CRM cement. If
49、 either of the two requirements listed above are not met,identify and correct any problems or errors found in the procedure. Repeat the determinations until a set of duplicate results agreewithin the permissible variations. Requalification of the analyst is required every two years.NOTE 2When qualifying a Rapid Method with seven CRMs in accordance with 5.4.2, the analyst performing the qualification of the test method maysimultaneously qualify for the requirement of 5.2.1.TABLE 2 Minimum Number of CRMs Required for Qualification ofChemical Testing
