1、Designation: C 114 07Standard Test Methods forChemical Analysis of Hydraulic Cement1This standard is issued under the fixed designation C 114; 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 p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、for 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 referen
4、ce 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 determin
5、ations 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 P
6、recision 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 Ceme
7、nts 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
8、 Cement 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 a
9、nd 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
10、as thestandard.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 applica-bility of regulatory limitations prior to use.
11、 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 LimeD 1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with
12、SpecificationsE 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near-Infrared Spectrophotom-eters1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current e
13、dition approved July 15, 2007. Published August 2007. Originallyapproved in 1934. Last previous edition approved in 2006 as C 114 06e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inf
14、ormation, 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.E 350 Test Methods for ChemicalAnalysis of Ca
15、rbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 617 Specification for Laboratory Weights and PrecisionMass StandardsE 832 Specification for Laboratory Filter PapersTABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Component(Column 2)MaximumDifferenceBetwe
16、enDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromSRM CertificateValuesC,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 ignitio
17、n) 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 (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)
18、0.20ECO2(carbon dioxide) 0.12E,FAlksol(water-soluble alkali)G0.75/wEChlsol(chloroform-soluble 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 sh
19、all 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 % 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 th
20、e values shall be within the prescribed limits.BWhere no value appears in Column 3, CRM certificate 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
21、 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
22、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. Weigh and prepare two separate sp
23、ecimens of each standard.Assign the CO2content of Standard A as the average of the two valuesdetermined, 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 fr
24、action of Certified CaCO3added tothat standard (percentage added divided by 100); multiply 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 Standa
25、rd B, respectively; call these values B and C.Example:B=0.98A+0.02Y.C=0.95A+0.05Y.Where for 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
26、 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.Gw = weight, in grams, of samples used for the test.C1140723. Number of Determinations and Permissible Variations3.1 Referee Analyses The reference
27、test methods thatfollow in Sections 5-20, or other test methods qualifiedaccording to 3.3, are required for referee analysis in those caseswhere conformance to chemical specification requirements arequestioned. In these cases, a cement shall not be rejected forfailure to conform to chemical requirem
28、ents unless all deter-minations of constituents involved and all necessary separa-tions prior to the determination of any one constituent are madeentirely by reference test methods prescribed in the appropriatesections of this test method or by other qualified test methods,except when specific test
29、methods are prescribed in thestandard specification for the cement in question. The testmethods actually used for the analysis shall be designated.3.1.1 Referee analyses, when there is a question regardingacceptance, shall be made in duplicate and the analyses shall bemade on different days. If the
30、two results do not agree withinthe permissible variation given in Table 1, the determinationshall be repeated until two or three results agree within thepermissible variation. When two or three results do agreewithin the permissible variation, their average shall be ac-cepted as the correct value. W
31、hen 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 acceptable results, the percentagesshall be calculated to the nearest 0.01 (or 0.001 in the case ofchloroform-solubl
32、e organic substances), although some of theaverage values are reported to 0.1 as indicated in the testmethods. When a blank determination is specified, one shall bemade with each individual analysis or with each group of twoor more samples analyzed on the same day for a givencomponent.3.1.2 Referee
33、analyses 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. Su
34、ch 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 ba
35、sis 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 operator/analyst shall bedemonstrated by analysis of each constituent of concern in atleast one CRM cement (Note 1) no matter what t
36、est method isused (for example, gravimetric, instrumental). Duplicatesamples shall be run on different days. The same test methodsto be used for analysis of cement being tested shall be used foranalysis of the CRM cement. If the duplicate results do notagree within the permissible variation given in
37、 Table 1, thedeterminations shall be repeated, following identification andcorrection of problems or errors, until a set of duplicate resultsdo agree within the permissible variation.NOTE 1The term CRM (Certified Reference Material) samples refersto NIST Hydraulic-Cement Chemical Standard Reference
38、Materials, 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
39、.3.1.5 Data demonstrating that precise and accurate resultswere obtained with CRM cements by the same analyst makingthe acceptance determination shall be made available onrequest to all parties concerned when there is a question ofacceptance of a cement. If the CRM used is not a NIST cement,the trac
40、eability documentation of the CRM used shall also bemade available on request.3.1.6 Acceptable reference cements are NIST CRMs (Note1), or other reference cements traceable to the NIST CRMs.The reference cement must have an assigned value for theanalyte being determined.Traceability consists of docu
41、mentaryevidence 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 demonstration of precision and ac
42、cu-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 least six randomly selecte
43、d 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 Optional AnalysesThe alternative test methods p
44、ro-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 2). Longer, morecomplex procedures, in some instances, have been retained asalternative test methods to permit comparison of resul
45、ts 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 rejection when it is clear that a ceme
46、ntdoes or does not meet the specification requirement. AnyTABLE 2 Minimum Number of CRMs Required for Qualificationof Chemical TestingMethod TypeReferenceAOtherBEquipment Qualification None 7Operator QualificationC11AReference Methods are those outlined in Sections 5-20.BThese may be any test method
47、 as described in 3.2 or any instrumental or rapidtest method, which must be qualified in accordance with 3.3.CEach operator performing acceptance or reference analyses must be qualifiedin accordance with 3.1.3 at a frequency of two years. If qualification of theinstrument is completed by a single op
48、erator, the operator has demonstratedindividual qualifications per 3.1.3.C114073change in test method procedures from those procedures listedin Sections 5-28 requires method qualification in accordancewith 3.3.NOTE 2It is not intended that the use of reference test methods beconfined to referee anal
49、ysis. 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 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
