1、Designation: C114 11b1Standard 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 p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEq 14 was corrected editorially in August 2013.1. Scope*1.1 These test methods cover the chemical analyses ofhydraulic cements. Any test methods of demon
3、strated accept-able precision and bias may be used for analysis of hydrauliccements, including analyses for referee and certificationpurposes, 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
4、 Methods andAlternative Test Methods. The reference 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
5、 may be usedalone or as alternates and determinations 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 Certifie
6、d Reference Materials5.2 Requirements for Qualification 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 A
7、nalysesReference Test Methods7 Insoluble Residue8 Silicon 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 Magn
8、esium Oxide17 Sulfur17.1 Sulfur Trioxide17.2 Sulfide18 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
9、Test Methods23 Calcium Oxide24 Carbon Dioxide25 Magnesium 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 Ch
10、loride DeterminationAppendix X2 CO2Determinations in 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.
11、It is the1These test methods are under the jurisdiction of ASTM Committee C01 onCement and are the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition approved Aug. 1, 2011. Published August 2011. Originallyapproved in 1934. Last previous edition approved in 2011 as
12、 C114 - 11a. DOI:10.1520/C0114-11B.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1responsibility of the user of this standard to establish appro-priate safety and healt
13、h 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 Hydrated LimeD1193 Specification for Reagent WaterE
14、29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE275 Practice for Describing and Measuring Performance ofUltraviolet and Visible SpectrophotometersE350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot
15、 Iron, andWrought IronE617 Specification for Laboratory Weights and PrecisionMass StandardsE832 Specification 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 metho
16、d,analytes are considered to be those items listed in Column 1 ofTable 1.4. Description of Referee Analyses4.1 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,
17、or other test methods qualifiedaccording to 5.4, the Performance Requirements for Rapid TestMethods Section, 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
18、 prior to the determination of anyone constituent are made entirely by these methods. Whenreporting the results 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 w
19、ithin the permissible variation given in Table 1, thedetermination shall be repeated until two or three results 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 tw
20、o 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-soluble organic substances), alth
21、ough some of theaverage values are reported to 0.1 as indicated in the testmethods. When a blank determination (See Note 1)isspecified, one shall be made with each individual analysis or2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
22、tm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.TABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference oftheAverage ofDuplicates fromCRMCe
23、rtificateValuesC,D,BSiO2(silicon dioxide) 0.16 0.2Al2O3(aluminum oxide) 0.20 0.2Fe2O3(ferric oxide) 0.10 0.10CaO (calcium oxide) 0.20 0.3MgO (magnesium oxide) 0.16 0.2SO3(sulfur trioxide) 0.10 0.1LOI (loss on ignition) 0.10 0.10Na2O (sodium oxide) 0.03 0.05K2O (potassium oxide) 0.03 0.05TiO2(titaniu
24、m dioxide) 0.02 0.03P2O5(phosphorus pentoxide) 0.03 0.03ZnO (zinc oxide) 0.03 0.03Mn2O3(manganic oxide) 0.03 0.03S (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-solub
25、le organicsubstances)0.004EAWhen seven CRM cements are required, as for demonstrating the performanceof rapid test methods, at least six of the seven shall be within the prescribed limitsand the seventh shall differ by no more than twice that value. When more thanseven CRMs are used, as for demonstr
26、ating 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 certifi
27、cate 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 certifica
28、te 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 se
29、lectedPortland 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 valuesde
30、termined, 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); multiply the
31、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 for Cer
32、tified 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 and C)
33、 by no morethan 10 % of those respective assigned values.Gw = weight, in grams, of samples used for the test.C114 11b12with each group of two or more samples analyzed on the sameday for a given analyte.NOTE 1A blank determination is a procedure which follows all stepsof analysis but in the absence o
34、f a sample. It is used for detection andcompensation 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 refer
35、ence cements traceable to the NISTCRMs. 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 f
36、or a given analyte, per-form a referee analysis (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 withinthe limits given in column 3 of Table
37、1. If the reference cement,as 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 a
38、ccompanied by a docu-ment showing 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
39、for acceptance or rejection of 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
40、 in 5.2.1 and 5.4. Such demonstration 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 leas
41、t one CRMcement in duplicate, 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
42、two samples agreeswith the certificate 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
43、listed above are notmet, identify 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 CRM
44、s inaccordance with 5.4.2, the 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 ce
45、ments as per 5.2.1shall be made 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 met
46、hodsprovide, 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 to permit comparison of r
47、esults bydifferent procedures or for use when unusual materials arebeing examined, where unusual interferences may besuspected, 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 ce
48、mentdoes or does not meet 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 referen
49、ce test methods beconfined 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
