1、Designation: C 114 09Standard 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 () 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 f
3、or 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 referenc
4、e 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 determina
5、tions 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 Pr
6、ecision 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 Cemen
7、ts 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 an
9、d 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 a
10、sstandard. 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 LimeD 1193 Specification for Reagent WaterE29 Practice for Using Signif
12、icant Digits in Test Data toDetermine Conformance with SpecificationsE 275 Practice for Describing and Measuring Performanceof Ultraviolet and Visible Spectrophotometers1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01
13、.23 on CompositionalAnalysis.Current edition approved Feb. 1, 2009. Published February 2009. Originallyapproved in 1934. Last previous edition approved in 2007 as C 114 07.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For An
14、nual Book 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.Copyrigh
15、t by ASTM Intl (all rights reserved); Mon Apr 27 01:49:29 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.E 350 Test Methods for ChemicalAnalysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 6
16、17 Specification for Laboratory Weights and PrecisionMass StandardsE 832 Specification for Laboratory Filter PapersTABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Component(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromSRM Certific
17、ateValuesC,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(tita
18、nium 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(chlorofor
19、m-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 shall differ by no more than twice that value. When morethan seven CRMs are used, as f
20、or 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 the values shall be within the prescribed limits.BWhere no value appears in Column 3,
21、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 be demonstrated when the correction is applied to allseven CRM cements.DWhere an CR
22、M 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
23、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 specimens of each standard.Assign the CO2content of Standard A as the average of the t
24、wo 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 fraction of Certified CaCO3added tothat standard (percentage added divided by 100); mu
25、ltiply 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.Wh
26、ere 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 of the duplicate valuesfor Standards B and C shall differ from their assigned value
27、s (B and C) by no morethan 10 % of those respective assigned values.Gw = weight, in grams, of samples used for the test.C114092Copyright by ASTM Intl (all rights reserved); Mon Apr 27 01:49:29 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions autho
28、rized.3. Number of Determinations and Permissible Variations3.1 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
29、, 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 are made entirely by these methods. Whenreporting the res
30、ults 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, thedetermination shall be repeated until two or three res
31、ults 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 calculation shall be based onthe three results. For the purpose of
32、 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 0.1 as indicated in the testmethods. When a blank determinat
33、ion (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 component.NOTE 1A blank determination is a procedure which follows all stepsof analysis but in the absence of a sample. It is used for detectio
34、n andcompensation of systematic bias.3.1.2 Referee 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
35、of 3.1.3, except when demonstratedunder 3.3.2.1. Such 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 requi
36、red only for those constitu-ents being used as a basis 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
37、in atleast one CRM cement (Note 2) no matter what test 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
38、 notagree within the permissible variation given in 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 2The term CRM (Certified Reference Material) samples refersto
39、 NIST Hydraulic-Cement Chemical Standard Reference 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
40、1 after correction for minor components when needed.3.1.5 Qualification 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
41、 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.3.1.6 Acceptable reference cements are NIST CRMs (Note2), or other reference cements traceable to the NIST CRMs.The reference cement must
42、have an assigned value for theanalyte being determined.Traceability 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
43、the proposed reference cement,using a NIST CRM for demonstration 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 o
44、f homogeneity, establish its homo-geneity by analyzing at least six randomly selected samples.TABLE 2 Minimum Number of CRMs Required for Qualificationof Chemical TestingMethod TypeReferenceAOtherBEquipment Qualification None 7Operator QualificationC11AReference Methods are those outlined in Section
45、s 5-20.BThese may be any test method 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 thein
46、strument is completed by a single operator, the operator has demonstratedindividual qualifications per 3.1.3.C114093Copyright by ASTM Intl (all rights reserved); Mon Apr 27 01:49:29 EDT 2009Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.No re
47、sult 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 AnalysesThe alternative test methods pro-vide, in
48、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 to permit comparison of results bydiffere
49、nt 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 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 to referee analysis. A refere
