1、Designation: C114 11bStandard 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 4. 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 analytes and may be usedalone or as alternates and determinatio
5、ns within the basicscheme at the option of the analyst and as indicated in theindividual 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 Qualifica
6、tion 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 Residue8 S
7、ilicon 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 Sulfid
8、e18 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 Chloride22 Chloroform-Soluble Organic SubstancesAlternative Test Methods23 Calcium Oxide24 Carbon Dioxide25 Mag
9、nesium Oxide26 Loss on Ignition26.1 Portland Blast-Furnace Slag Cement and Slag Cement27 Titanium Dioxide28 Phosphorus Pentoxide29 Manganic Oxide30 Free Calcium OxideAppendices TitleAppendix X1 Example of Determination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2Determinations i
10、n Hydraulic Cements1.3 The values stated in SI units are to be regarded asstandard. 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 standar
11、d to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. See 8.3.2.1 and16.4.1 for specific caution statements.2. Referenced Documents2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone,Quicklime, and Hydrate
12、d LimeD1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis
13、.Current edition approved Aug. 1, 2011. Published August 2011. Originallyapproved in 1934. Last previous edition approved in 2011 as C114 - 11a. DOI:10.1520/C0114-11B.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
14、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.E275 Practice
15、 for Describing and Measuring Performanceof Ultraviolet and Visible SpectrophotometersE350 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
16、for Laboratory Filter Papers3. Terminology3.1 Definitions:3.1.1 analyte, na substance of interest when performing aquantitative analysis.3.1.1.1 DiscussionFor the purposes of this test method,analytes are considered to be those items listed in Column 1 ofTable 1.4. Description of Referee Analyses4.1
17、 Referee AnalysesWhen conformance to chemicalspecification requirements is questioned, perform refereeanalyses as described in 4.1.1. The reference test methods thatfollow in Sections 7-22, or other test methods qualifiedaccording to 5.4, the Performance Requirements for Rapid TestMethods Section, a
18、re 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 result
19、s of referee analyses, specify which testmethods were used.4.1.1 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 result
20、s 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 co
21、mparing 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 determination
22、 (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 analyte.NOTE 1A blank determination is a procedure which follows all stepsof analysis but in the absence of a sample. It is used for detection and
23、compensation of systematic bias.5. Qualification for Different Analyses5.1 Certified Reference MaterialsA Certified ReferenceMaterial (CRM) must be used in the qualification of testmethods and analysts. Acceptable reference cements are NISTCRMs, or other reference cements traceable to the NISTCRMs.
24、The reference cement must have an assigned value forthe analyte being determined. Traceability consists of docu-mentary evidence that the assigned values of the referencecement are compatible with the certified values of NISTCRMs. To demonstrate traceability for a given analyte, per-form a referee a
25、nalysis (as defined in 4.1) on the proposedreference cement, using a NIST CRM for demonstration ofprecision and accuracy. The reference cement is acceptable ifits assigned value agrees with the average referee value withinTABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)M
26、aximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference of theAverage ofDuplicates fromCRM 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.
27、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 (zinc oxide) 0.03 60.03Mn2O3(manganic oxide) 0.03 60.03S (sulfide sulfur) 0.01ECl (chloride) 0.003EIR (insoluble residue) 0.10ECx
28、(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 required, as for demonstrating the perfor-mance of rapid test methods, at least six of the seven shall be within the prescribedlimi
29、ts 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 % shall be within the prescribed limits, and the remainder byno more than twice the value. When a lesser number of CRM cements a
30、rerequired, 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 requirement for differences between duplicates shall apply.CInterelement corrections may be used for any oxide standardization provided
31、improved 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 analys
32、is, 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. Weigh and pr
33、epare two separate specimens 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
34、value) by the mass fraction 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 forStan
35、dard A and for Standard 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 0.2
36、4 % 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.Gw = weight, in grams, of samples used for the test.C114 11b2the limits given in column 3 ofTable 1. If the reference cement,as
37、 supplied, has no documented guarantee of homogeneity,establish its homogeneity by analyzing at least six randomlyselected samples. No result shall deviate from the assignedvalue by more than the limits given in column 2 of Table 1.Anacceptable reference cement must be accompanied by a docu-ment sho
38、wing the data produced in demonstrating traceabilityand homogeneity.5.2 Requirements for Qualification TestingQualified testmethods are required whenever testing is performed for thefollowing reasons: (1) for Referee analyses; (2) for analysesintended for use as a basis for acceptance or rejection o
39、f acement; or, (3) for manufacturers certification. When Refer-ence Methods are used, qualification testing of the analyst isrequired as described in 5.2.1. When Rapid Methods are used,qualification testing of both the analyst and the test method arerequired as described in 5.2.1 and 5.4. Such demon
40、stration maybe made concurrently with analysis of the cement being tested.The requirements for qualification of a test method and analystare summarized in Table 2.5.2.1 Qualification of the analyst shall be demonstrated byanalysis of each analyte of concern using at least one CRMcement in duplicate,
41、 no matter what test method is used (Note2). Duplicate samples shall be tested on different days. Theanalyst is considered qualified when the difference between theduplicate results does not vary by more than the value listed inColumn 2 of Table 1 and the average of the two samples agreeswith the ce
42、rtificate value of the CRM within the limits listed inColumn 3 of Table 1 after correction for minor componentswhen needed. The same test methods to be used for analysis ofcement being tested shall be used for analysis of the CRMcement. If either of the two requirements listed above are notmet, iden
43、tify and correct any problems or errors found in theprocedure. Repeat the determinations until a set of duplicateresults agree within the permissible variations. Requalificationof the analyst is required every two years.NOTE 2When qualifying a Rapid Method with seven CRMs inaccordance with 5.4.2, th
44、e analyst performing the qualification of the testmethod may simultaneously qualify for the requirement of 5.2.1.5.2.2 Qualification data demonstrating that the same opera-tor or analyst making the acceptance determination obtainedprecise and accurate results with CRM cements as per 5.2.1shall be ma
45、de available on request to all parties concernedwhen there is 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.5.3 Alternative AnalysesThe alternative test methods pro-vide, in some cases,
46、 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 bydifferent procedur
47、es 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
48、 the specification requirement. Anychange in test method procedures from those procedures listedin Sections 7-30 requires method qualification in accordancewith 5.4, the Performance Requirements for Rapid Test Meth-ods Section.NOTE 3It is not intended that the use of reference test methods beconfine
49、d 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.5.3.1 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.5.4 Performance Re
