1、Designation:C11410a Designation: C114 11Standard 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 revis
2、ion. A number 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 b
3、ias may be used for analysis of hydraulic cements, including analyses for referee and certification purposes, asexplained in Section 3. Specific chemical test methods are provided for ease of reference for those desiring to use them. They aregrouped as Reference Test Methods andAlternative Test Meth
4、ods. The reference 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 alternat
5、es and determinationswithin the basic scheme at the option of the analyst and as indicated in the individual method.1.2 Contents:Section Subject2 Referenced Documents3 Description of Referee Analyses3.1 Referee Analyses4 Qualification for Different Analyses4.1 Certified Reference Materials4.2 Requir
6、ements for Qualification 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
7、Insoluble Residue7 Silicon 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
8、Trioxide16.2 Sulfide17 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 Substances1These test methods are under the jurisdicti
9、on ofASTM Committee C01 on Cement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition approved Dec.Feb. 1, 2010.2011. Published JanuaryMarch 2011. Originally approved in 1934. Last previous edition approved in 2010 as C114 10a. DOI:10.1520/C0114-10a.10.1
10、520/C0114-11.1This document is not an 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 con
11、sult prior editions as appropriate. In 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 standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
12、n, PA 19428-2959, United States.Alternative Test Methods22 Calcium Oxide23 Carbon Dioxide24 Magnesium 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
13、Determination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2Determinations 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 saf
14、ety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. See 7.3.2.1 and 15.4.1 for specific caution statements.2. Referenced Documen
15、ts2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated LimeD1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE275 Practice for Describing and Measuring Performance of Ult
16、raviolet 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 Precision Mass StandardsE832 Specification for Laboratory Filter Papers3. Description of
17、 Referee Analyses3.1 Referee AnalysesWhen conformance to chemical specification requirements is questioned, perform referee analyses asdescribed in 3.1.1. The reference test methods that follow in Sections 6-21, or other test methods qualified according to 4.4, thePerformance Requirements for Rapid
18、Test Methods Section, are required for referee analysis. A cement shall not be rejected forfailure to conform to chemical requirements unless all determinations of constituents involved and all necessary separations priorto the determination of any one constituent are made entirely by these methods.
19、 When reporting the results of referee analyses,specify which test methods were used.3.1.1 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 be repeat
20、ed 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 the three
21、 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 test me
22、thods. When a blank determination (See Note 1) is specified, one shall be made with each individualanalysis 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 absence of a sa
23、mple. It is used for detection andcompensation of systematic bias.4. Qualification for Different Analyses4.1 Certified Reference MaterialsACertified Reference Material (CRM) must be used in the qualification of test methods andanalysts. Acceptable reference cements are NIST CRMs, or other reference
24、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 traceability fora
25、given analyte, perform a referee analysis (as defined in 3.1) 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 referee2For referencedASTM standards, visit theASTM website, w
26、ww.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 112value within the limits given in column 3 of Table 1. If the reference cement, as supplied, has no documented
27、 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 cement must be accompanied bya document showing the data produced in d
28、emonstrating traceability and homogeneity.4.2 Requirements for Qualification TestingQualified test methods are required whenever testing is performed for thefollowing reasons: (1) for Referee analyses; (2) for analyses intended for use as a basis for acceptance or rejection of a cement;or, (3) for m
29、anufacturers certification. When Reference Methods are used, qualification testing of the analyst is required asTABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromSRM CertificateVa
30、luesC,D,BSiO2(silicon dioxide) 0.16 60.2Al2O3(aluminum oxide) 0.20 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
31、dioxide) 0.02 60.03P2O5(phosphorus pentoxide) 0.03 60.03ZnO (zinc 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-sol
32、uble organic substances) 0.004EAWhen seven CRM cements are required, 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 de
33、monstrating 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 arerequired, all of the values shall be within the prescribed limits.BWhere no value appears in Column 3, CRM c
34、ertificate values do not exist. Insuch cases, only the requirement 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 cer
35、tificate 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
36、 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. Weigh and prepare two separate specimens of each standard.Assign the CO2content of Standard A as the average of the two va
37、luesdetermined, provided they agree within the required limit of Column 2.Assign CO2values to Standards B and C as follows: Multiply the Certified CaCO3value (Y) forCO2(from the certificate value) by the mass fraction of Certified CaCO3added tothat standard (percentage added divided by 100); multipl
38、y the value determined forStandard A by the mass fraction of Standard A in each of the other standards (thatis, 0.98 and 0.95 for Standards B and C, respectively); add the two values forStandard A and for Standard B, respectively; call these values B and C.Example:B=0.98A+0.02Y.C=0.95A+0.05Y.Where f
39、or Certified CaCO3,ifY=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,respectively, 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
40、and C) by no morethan 10 % of those respective assigned values.Gw = weight, in grams, of samples used for the test.C114 113described in 4.2.1. When Rapid Methods are used, qualification testing of both the analyst and the test method are required asdescribed in 4.2.1 and 4.4. Such demonstration may
41、be made concurrently with analysis of the cement being tested. Therequirements for qualification of a test method and analyst are summarized in Table 2.4.2.1 Qualification of the analyst shall be demonstrated by analysis of each analyte of concern using at least one CRM cementin duplicate, no matter
42、 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 in Column 2of Table 1 and the average of the two samples agrees with the certifica
43、te value of the CRM within the limits listed in Column 3of Table 1 after correction for minor components when needed. The same test methods to be used for analysis of cement beingtested shall be used for analysis of the CRM cement. If either of the two requirements listed above are not met, identify
44、 and correctany problems or errors found in the procedure. Repeat the determinations until a set of duplicate results agree within thepermissible variations. Requalification of the analyst is required every two years.NOTE 2When qualifying a Rapid Method with seven CRMs in accordance with 4.4.2, the
45、analyst performing the qualification of the test method maysimultaneously qualify for the requirement of 4.2.1.4.2.2 Qualification data demonstrating that the same operator or analyst making the acceptance determination obtained preciseand accurate results with CRM cements as per 4.2.1 shall be made
46、 available on request to all parties concerned when there is aquestion of acceptance of a cement. If the CRM used is not a NIST cement, the traceability documentation of the CRM used shallalso be made available on request.4.3 Alternative AnalysesThe alternative test methods provide, in some cases, p
47、rocedures that are shorter or more convenientto use for routine determination of certain constituents than are the reference test methods (Note 3). Longer, more complexprocedures, in some instances, have been retained as alternative test methods to permit comparison of results by differentprocedures
48、 or for use when unusual materials are being examined, where unusual interferences may be suspected, or when unusualpreparation for analysis is required. Test results from alternative test methods may be used as a basis for acceptance or rejectionwhen it is clear that a cement does or does not meet
49、the specification requirement. Any change in test method procedures fromthose procedures listed in Sections 6-29 requires method qualification in accordance with 4.4, the Performance Requirements forRapid Test Methods Section.NOTE 3It is not intended that the use of reference test methods be confined to referee analysis. A reference test method may be used in preferenceto an alternative test method when so desired. A reference test method must be used where an alternative test method is not provided.4.3.1 Duplicate analyses and blank determinations are not required when us
