1、Designation: C114 11b1C114 13Standard 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 numb
2、er in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEEq 14 was corrected editorially in August 2013.1. Scope*1.1 These test methods cover the chemical analyses of hydraulic cements. Any test methods
3、 of demonstrated acceptableprecision and bias may be used for analysis of hydraulic cements, including analyses for referee and certification purposes, asexplained in Section 4. Specific chemical test methods are provided for ease of reference for those desiring to use them. They aregrouped as Refer
4、ence Test Methods andAlternative Test Methods. The reference test methods are long accepted classical chemicaltest methods which provide a reasonably well-integrated basic scheme of analysis for hydraulic cements. The alternative testmethods generally provide individual determination of specific ana
5、lytes and may be used alone or as alternates and determinationswithin the basic scheme at the option of the analyst and as indicated in the individual method.1.2 Contents: Contents:Section Subject2 Referenced Documents4 Description of Referee Analyses4.1 Referee Analyses5 Qualification for Different
6、 Analyses5.1 Certified 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
7、Order for Reporting AnalysesReference 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
8、 Calcium Oxide16 Magnesium 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 Oxides1 These test methods are under the jurisdiction ofASTM Committee C01 on Cement and are the direct respo
9、nsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition approved Aug. 1, 2011Oct. 1, 2013. Published August 2011November 2013. Originally approved in 1934. Last previous edition approved in 2011 asC114 - 11a.C114 - 11b1. DOI: 10.1520/C0114-11B.10.1520/C0114-13.This document is not
10、an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate.
11、 In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*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 States119.1
12、 Total Alkalis19.2 Water-Soluble Alkalis20 Manganic Oxide21 Chloride22 Chloroform-Soluble Organic SubstancesAlternative Test Methods23 Calcium Oxide24 Carbon Dioxide25 Magnesium Oxide26 Loss on Ignition26.1 Portland Blast-Furnace Slag Cement and Slag Cement27 Titanium Dioxide28 Phosphorus Pentoxide2
13、9 Manganic Oxide30 Free Calcium OxideAppendices TitleAppendix X1 Example of Determination of Equivalence Pointfor the Chloride DeterminationAppendix X2 CO2 Determinations in Hydraulic Cements1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included
14、in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.
15、 See 8.3.2.1 and 16.4.1 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 Significant Digits in Test Data to Determine Conformance wit
16、h SpecificationsE275 Practice for Describing and Measuring Performance of Ultraviolet and Visible SpectrophotometersE350 Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and WroughtIronE617 Specification for Laboratory Weights and Precision M
17、ass StandardsE832 Specification for Laboratory Filter Papers3. Terminology3.1 Definitions:3.1.1 analyte, na substance of interest when performing a quantitative analysis.3.1.1.1 DiscussionFor the purposes of this test method, analytes are considered to be those items listed in Column 1 of Table 1.4.
18、 Description of Referee Analyses4.1 Referee AnalysesWhen conformance to chemical specification requirements is questioned, perform referee analyses asdescribed in 4.1.1. The reference test methods that follow in Sections 7 22, or other test methods qualified according to 5.4, thePerformance Requirem
19、ents for Rapid Test Methods Section, are required for referee analysis. A cement shall not be rejected forfailure to conform to chemical requirements unless all determinations of constituents involved and all necessary separations priorto the determination of any one constituent are made entirely by
20、 these methods. When reporting the results of referee analyses,specify which test methods were used.4.1.1 Referee analyses shall be made in duplicate and the analyses shall be made on different days. If the two results do not agreewithin the permissible variation given in Table 1, the determination
21、shall be repeated until two or three results agree within thepermissible variation. When two or three results do agree within the permissible variation, their average shall be accepted as thecorrect value. When an average of either two or three results can be calculated, the calculation shall be bas
22、ed on the three results.For the purpose of comparing analyses and calculating the average of acceptable results, the percentages shall be calculated to thenearest 0.01 (or 0.001 in the case of chloroform-soluble organic substances), although some of the average values are reported to2 For referenced
23、ASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.C114 1320.1 as indicated in the test methods. When a blank determination (See
24、 Note 1) is specified, one shall be made with each individualanalysis or with each group of two or more samples analyzed on the same day for a given analyte.TABLE 1 Maximum Permissible Variations in ResultsA(Column 1)Analyte(Column 2)MaximumDifferenceBetweenDuplicatesB(Column 3)MaximumDifference oft
25、heAverage ofDuplicates fromCRMCertificateValuesC,D,BSiO 2 (silicon dioxide) 0.16 0.2Al 2 O3 (aluminum oxide) 0.20 0.2Fe 2 O3 (ferric oxide) 0.10 0.10CaO (calcium oxide) 0.20 0.3MgO (magnesium oxide) 0.16 0.2SO 3 (sulfur trioxide) 0.10 0.1LOI (loss on ignition) 0.10 0.10Na 2 O (sodium oxide) 0.03 0.0
26、5K 2 O (potassium oxide) 0.03 0.05TiO 2 (titanium dioxide) 0.02 0.03P 2 O5 (phosphorus pentoxide) 0.03 0.03ZnO (zinc oxide) 0.03 0.03Mn 2 O3 (manganic oxide) 0.03 0.03S (sulfide sulfur) 0.01 ECl (chloride) 0.003 EIR (insoluble residue) 0.10 ECx (free calcium oxide) 0.20 ECO 2 (carbon dioxide) 0.12 E
27、 ,FAlk sol (water-soluble alkali)G 0.75/w EChl sol (chloroform-soluble organicsubstances)0.004 EA When 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 tha
28、n twice that value. When more thanseven 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 the values shall be within
29、the prescribed limits.B Where no value appears in Column 3, CRM certificate values do not exist. Insuch cases, only the requirement for differences between duplicates shall apply.C Interelement corrections may be used for any oxide standardization providedimproved accuracy can be demonstrated when t
30、he correction is applied to allseven CRM cements.D Where an CRM certificate value includes a subscript number, that subscriptnumber shall be treated as a valid significant figure.E Not applicable. No certificate value given.F Demonstrate performance by analysis, in duplicate, of at least one Portlan
31、dcement. 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 specimens of each st
32、andard.Assign the CO2 content 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 CaCO3 value (Y) forCO2 (from the certificate value) by the mass fraction of Certi
33、fied CaCO3 added tothat standard (percentage added divided by 100); multiply the value determined forStandardAby the mass fraction of StandardAin 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
34、; call these values B and C.Example:B = 0.98A + 0.02Y.C = 0.95A + 0.05Y.Where for Certified CaCO3 , if Y = 39.9 %B = 0.98A + 0.80 % by mass.C = 0.95A + 2.00 % by mass.Maximum difference between the duplicate CO2 values for Standards B and C,respectively, shall be 0.17 and 0.24 % by mass. Averages of
35、 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.G w = weight, in grams, of samples used for the test.C114 133NOTE 1A blank determination is a procedure which follows all steps of analysis but in the
36、absence of a sample. It is used for detection andcompensation of systematic bias.5. Qualification for Different Analyses5.1 Certified Reference MaterialsACertified Reference Material (CRM) must be used in the qualification of test methods andanalysts. Acceptable reference cements are NIST CRMs, or o
37、ther reference cements traceable to the NIST CRMs. The referencecement must have an assigned value for the analyte being determined. Traceability consists of documentary evidence that theassigned values of the reference cement are compatible with the certified values of NIST CRMs. To demonstrate tra
38、ceability fora given analyte, perform a referee analysis (as defined in 4.1) on the proposed reference cement, using a NIST CRM fordemonstration of precision and accuracy. The reference cement is acceptable if its assigned value agrees with the average refereevalue within the limits given in column
39、3 of Table 1. If the reference cement, as supplied, has no documented guarantee ofhomogeneity, establish its homogeneity by analyzing at least six randomly selected samples. No result shall deviate from theassigned value by more than the limits given in column 2 of Table 1. An acceptable reference c
40、ement must be accompanied bya document showing the data produced in demonstrating traceability and homogeneity.5.2 Requirements for Qualification TestingQualified test methods are required whenever testing is performed for the followingreasons: (1) for Referee analyses; (2) for analyses intended for
41、 use as a basis for acceptance or rejection of a cement; or, (3) formanufacturers certification. When Reference Methods are used, qualification testing of the analyst is required as described in5.2.1. When Rapid Methods are used, qualification testing of both the analyst and the test method are requ
42、ired as described in 5.2.1and 5.4. Such demonstration may be made concurrently with analysis of the cement being tested.The requirements for qualificationof a test method and analyst are summarized in Table 2.5.2.1 Qualification of the analyst shall be demonstrated by analysis of each analyte of con
43、cern using at least one CRM cementin duplicate, no matter what test method is used (Note 2). Duplicate samples shall be tested on different days. The analyst isconsidered qualified when the difference between the duplicate results does not vary by more than the value listed in Column 2of Table 1 and
44、 the average of the two samples agrees with the certificate value of the CRM within the limits listed in Column 3of Table 1 after correction for minor components when needed. The same test methods to be used for analysis of cement beingtested shall be used for analysis of the CRM cement. If either o
45、f the two requirements listed above are not met, identify and correctany problems or errors found in the procedure. Repeat the determinations until a set of duplicate results agree within thepermissible variations. Requalification of the analyst is required every two years.NOTE 2When qualifying a Ra
46、pid Method with seven CRMs in accordance with 5.4.2, the analyst performing the qualification of the test method maysimultaneously qualify for the requirement of 5.2.1.5.2.2 Qualification data demonstrating that the same operator or analyst making the acceptance determination obtained preciseand acc
47、urate results with CRM cements as per 5.2.1 shall be made available on request to all parties concerned when there is aquestion of acceptance of a cement. If the CRM used is not a NIST cement, the traceability documentation of the CRM used shallalso be made available on request.5.3 Alternative Analy
48、sesThe alternative test methods provide, in some cases, procedures that are shorter or more convenientto use for routine determination of certain constituents than are the reference test methods (Note 3). Longer, more complexprocedures, in some instances, have been retained as alternative test metho
49、ds to permit comparison of results by differentprocedures or for use when unusual materials are being examined, where unusual interferences may be suspected, or when unusualpreparation for analysis is required. Test results from alternative test methods may be used as a basis for acceptance or rejectionwhen it is clear that a cement does or does not meet the specification requirement. Any change in test method procedures fromthose procedures listed in Sections 7 30 requires method qualification in accordance with 5.4, the Performance Requirements forR
