1、Designation: C114 09aStandard 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 components and may beused alone or as alternates and determinat
5、ions within the basicscheme at the option of the analyst and as indicated in theindividual method.1.2 Contents:Section Subject2 Referenced Documents3 Number of Determinations and Permissible Variations3.1 Referee Analyses3.2 Optional Analyses3.3 Performance Requirements for Rapid Test Methods3.4 Pre
6、cision and Bias4 General4.1 Interferences and Limitations4.2 Apparatus and Materials4.3 Reagents4.4 Sample Preparation4.5 General Procedures4.6 Recommended Order for Reporting AnalysesReference Test Methods5 Insoluble Residue6 Silicon Dioxide6.2 Cements with Insoluble Residue Less Than 1 %6.3 Cement
7、s with Insoluble Residue Greater Than 1 %7 Ammonium Hydroxide Group8 Ferric Oxide9 Phosphorus Pentoxide10 Titanium Dioxide11 Zinc Oxide12 Aluminum Oxide13 Calcium Oxide14 Magnesium Oxide15 Sulfur15.1 Sulfur Trioxide15.2 Sulfide16 Loss On Ignition16.1 Portland Cement16.2 Portland Blast-Furnace Slag C
8、ement and Slag Cement17 Sodium and Potassium Oxides17.1 Total Alkalis17.2 Water-Soluble Alkalis18 Manganic Oxide19 Chloride20 Chloroform-Soluble Organic SubstancesAlternative Test Methods21 Calcium Oxide22 Carbon Dioxide23 Magnesium Oxide24 Loss on Ignition24.1 Portland Blast-Furnace Slag Cement and
9、 Slag Cement25 Titanium Dioxide26 Phosphorus Pentoxide27 Manganic Oxide28 Free Calcium OxideAppendices TitleAppendix X1 Example of Determination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2Determinations in Hydraulic Cements1.3 The values stated in SI units are to be regarded as
10、standard. 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 to establish appro-priate safety and health practices and determine the
11、applica-bility of regulatory limitations prior to use. See 6.3.2.1 and14.4.1 for specific caution statements.2. Referenced Documents2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone,Quicklime, and Hydrated LimeD1193 Specification for Reagent WaterE29 Practice for Using Signific
12、ant Digits in Test Data toDetermine Conformance with SpecificationsE275 Practice for Describing and Measuring Performance1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition app
13、roved Dec. 1, 2009. Published January 2010. Originallyapproved in 1934. Last previous edition approved in 2009 as C114 09. DOI:10.1520/C0114-09a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards
14、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.of Ultraviolet and Visible Spectrop
15、hotometersE350 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 Laboratory Filter Papers3. Number of Determinations and Permissible Vari
16、ations3.1 Referee AnalysesWhen conformance to chemicalspecification requirements is questioned, perform refereeanalyses as described in 3.1.1. The reference test methods thatfollow in Sections 5-20, or other test methods qualifiedaccording to 3.3, are required for referee analysis. A cementshall not
17、 be rejected for failure to conform to chemicalrequirements unless all determinations of constituents involvedand all necessary separations prior to the determination of anyone constituent are made entirely by these methods. Whenreporting the results of referee analyses, specify which testmethods we
18、re 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, thedetermination shall be repeated until two or three results agreewithin the permissible variation. When two o
19、r 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 calculation shall be based onthe three results. For the purpose of comparing analyses andcalculating the average of acce
20、ptable 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 0.1 as indicated in the testmethods. When a blank determination (See Note 1) is speci-fied, one shall be made with
21、 each individual analysis or witheach group of two or more samples analyzed on the same dayfor a given component.NOTE 1A blank determination is a procedure which follows all stepsof analysis but in the absence of a sample. It is used for detection andcompensation of systematic bias.3.1.2 Referee ana
22、lyses or analyses intended for use as abasis for acceptance or rejection of a cement or for manufac-turers certification shall be made only after demonstration ofprecise and accurate analyses by the test methods in use bymeeting the requirements of 3.1.3, except when demonstratedunder 3.3.2.1. Such
23、demonstration may be made concurrentlywith analysis of the cement being tested and must have beenmade within the preceding two years. The requirements forverification of equipment and personnel are summarized inTable 2. The demonstration is required only for those constitu-ents being used as a basis
24、 for acceptance, rejection, orcertification of a cement, but may be made for any constituentof cement for which a standard exists.3.1.3 Initial qualification of the analyst shall be demon-strated by analysis of each constituent of concern in at least oneCRM cement (Note 2) no matter what test method
25、 is used (forexample, gravimetric, instrumental). Duplicate samples shallbe run on different days. The same test methods to be used foranalysis of cement being tested shall be used for analysis of theCRM cement. If the duplicate results do not agree within thepermissible variation given in Table 1,
26、the determinations shallbe repeated, following identification and correction of prob-lems or errors, until a set of duplicate results do agree withinthe permissible variation.NOTE 2The term CRM (Certified Reference Material) samples refersto NIST Hydraulic-Cement Chemical Standard Reference Material
27、s, orother acceptable reference cement as defined in 3.1.6.3.1.4 The average of the results of acceptable duplicatedeterminations for each constituent may differ from the CRMassigned value by no more than the value shown in column 2of Table 1 after correction for minor components when needed.3.1.5 Q
28、ualification data demonstrating that the same opera-tor or analyst making the acceptance determination obtainedprecise and accurate results with CRM cements as per 3.1.3shall be made available on request to all parties concernedwhen there is a question of acceptance of a cement. If the CRMused is no
29、t a NIST cement, the traceability documentation ofthe CRM used shall also be made available on request.3.1.6 Acceptable reference cements are NIST CRMs (Note2), or other reference cements traceable to the NIST CRMs.The reference cement must have an assigned value for theanalyte being determined.Trac
30、eability consists of documentaryevidence that the assigned values of the reference cement arecompatible with the certified values of NIST CRMs. Todemonstrate traceability for a given analyte, perform a refereeanalysis (as defined in 3.1) on the proposed reference cement,using a NIST CRM for demonstr
31、ation of precision and accu-racy. The reference cement is acceptable if its assigned valueagrees with the average referee value within the limits given incolumn 3 of Table 1. If the reference cement, as supplied, hasno documented guarantee of homogeneity, establish its homo-geneity by analyzing at l
32、east six randomly selected samples.No result shall deviate from the assigned value by more thanthe limits given in column 2 of Table 1. An acceptablereference cement must be accompanied by a document show-ing the data produced in demonstrating traceability and homo-geneity.3.2 Alternative AnalysesTh
33、e 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, morecomplex procedures, in some instances, have been retained asalternative test methods t
34、o 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.C114 09a2Test results from alternative test methods may be used as abasis for acceptance or r
35、ejection when it is clear that a cementdoes or does not meet the specification requirement. Anychange in test method procedures from those procedures listedin Sections 5-28 requires method qualification in accordancewith 3.3.NOTE 3It is not intended that the use of reference test methods beconfined
36、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.3.2.1 Duplicate analyses and blank determinations are notrequired when using the alternative test
37、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 case, be so designated.3.3 Performance Requirements for Rapid
38、Test Methods:33.3.1 Definition and ScopeWhere analytical data obtainedin accordance with this test method are required, any testmethod may be used that meets the requirements of 3.3.2.Atest method is considered to consist of the specific procedures,reagents, supplies, equipment, instrument, etc. sel
39、ected andused in a consistent manner by a specific laboratory. See Note4 for examples of procedures.NOTE 4Examples of test methods used successfully by their authorsfor analysis of hydraulic cement are given in the list of references.Included are test methods using atomic absorption X-ray spectromet
40、ry,and spectrophotometry-EDTA.3.3.1.1 If more than one instrument, even though substan-tially identical, is used in a specific laboratory for the sameanalyses, use of each instrument shall constitute a separate testmethod and each must be qualified separately.3.3.2 Qualification of a Test MethodPrio
41、r to use foranalysis of hydraulic cement, each test method (see 3.3.1) mustbe qualified individually for such analysis. Qualification data,or if applicable, requalification data, shall be made availablepursuant to the Manufacturers Certification Section of theappropriate hydraulic cement specificati
42、on.3.3.2.1 Using the test method chosen, make single determi-nations for each oxide under consideration on at least sevenCRM samples (Note 2). Complete two rounds of tests ondifferent days repeating all steps of sample preparations.Calculate the differences between values and averages of thevalues f
43、rom the two rounds of tests.3.3.2.2 When seven CRMs are used in the qualificationprocedure, at least six of the seven differences betweenduplicates obtained of any single component shall not exceedthe limits shown in Column 2 of Table 1 and the remaining3Gebhardt, R. F., “Rapid Methods for ChemicalA
44、nalysis of Hydraulic Cement,”ASTM STP 985, 1988.TABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Component(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromSRM CertificateValuesC,D,BSiO2(silicon dioxide) 0.16 60.2Al2O3(aluminum oxide)
45、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 dioxide) 0.02 60.03P2O5(phosphorus pentoxide) 0.03 60.03ZnO (z
46、inc 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 req
47、uired, 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 require
49、ment 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 s
