ASTM_C_114-18.pdf

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.Designation:C114-18NTERNATIONALStandard 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 parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope9Ammonium Hydroxide Group1.1 These test methods cover the chemical analyses of10Ferric OxidePhosphorus Pentoxidehydraulic cements.Any test methods of demonstrated accept-12Titanium Dioxideable precision and bias may be used for analysis of hydraulic13Zinc Oxide14Aluminum Oxidecements,including analyses for referee and certification15Calcium Oxidepurposes,as explained in Section 4.Specific chemical testMagnesium Oxidemethods are provided for ease of reference for those desiring to17Sulfuruse them.They are grouped as Reference Test Methods and17.1Sulfur Trioxide17.2SulfideAlternative Test Methods.The reference test methods are long18Loss On Ignitionaccepted classical chemical test methods which provide a18.1Portland Cement18.2Portland Blast-Fumace Slag Cement and Slag Cementreasonably well-integrated basic scheme of analysis for hy-19Sodium and Potassium Oxidesdraulic cements.The alternative test methods generally provide19.1Total Alkalisindividual determination of specific analytes and may be used19.2Water-Soluble Alkalisalone or as alternates and determinations within the basic20Manganic Oxidescheme at the option of the analyst and as indicated in theChlorideChloroform-Soluble Organic Substancesindividual method.Altemnative Test Methods1.2 Contents:23Calcium Oxide24Carbon DioxideSectionSubject25Magnesium Oxide2Referenced Documents26Loss on Ignition4Description of Referee Analyses26.1Portland Blast-Furnace Slag Cement and Slag Cement4.1Referee Analyses27Titanium Dioxide5Qualification for Different Analyses28Phosphorus Pentoxide5.1Certified Reference Materials9Manganic Oxide5.2Requirements for Qualification Testing30Free Calcium Oxide5.3Altemative Analyses5.4Performance Requirements for Rapid Test MethodsAppendices6GeneralAppendix X1Example of Determination of Equivalence Point6.1Interferences and Limitationsfor the Chloride Determination6.2Apparatus and MaterialsAppendix X2CO.Determinations in Hydraulic Cements6.3Reagents6.4Sample Preparation1.3 The values stated in SI units are to be regarded as6.5General Proceduresstandard.No other units of measurement are included in this6.6Recommended Order for Reporting Analysesstandard.Reference Test Methods1.4 This standard does not purport to address all of the7Insoluble Residue8Silicon Dioxidesafety concerns,if any,associated with its use.It is the8.2Cements with Insoluble Residue Less Than 1%responsibility of the user of this standard to establish appro-8.3Cements with Insoluble Residue Greater Than 1%priate safety,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-These test methods are under the jurisdiction of ASTM Committee Col ondance with internationally recognized principles on standard-Cement and are the direct responsibility of Subcommittee C01.23 on Compositionalization established in the Decision on Principles for theAnalysis.Development of International Standards,Guides and Recom-Current edition approved May 1.2018.Published May 2018.Originallyapproved in 1934.Last previous edition approved in 2015 as C114-15.DOI:mendations issued by the World Trade Organization Technical10.1520/C0114-18.Barriers to Trade(TBT)Committee.*A Summary of Changes section appears at the end of this standardCopyright ASTM Intemational,100 Barr Harbor Drive,PO Box C700.West Conshohocken.PA 19428-2959.United States1C114-18NorE 3-It is not intended that the use of reference test methods beshall be assumed to be a significant number.When sevenconfined to referee analysis.A reference test method may be used inCRMs are used in the qualification procedure,at least six of thepreference to an alternative test method when so desired.A reference testmethod must be used where an alternative test method is not provided.seven averages for each analyte shall not differ from thecertified concentrations by more than the value shown in5.3.1 Duplicate analyses and blank determinations are notcolumn 3 of Table 1,and the remaining average by more thanrequired when using the alternative test methods.If,however.twice that value.When more than seven CRMs are used in thea blank determination is desired for an alternative test method,qualification procedure,at least 77 of the averages for eachone may be used and it need not have been obtained concur-analyte shall not differ from the certified concentrations byrently with the analysis.The final results,when corrected formore than the value shown in column 3 of Table 1,and theblank values,should,in either case,be so designated.remaining average(s)by more than twice that value.5.4 Performance Requirements for Rapid Test Methods:3.45.4.2.4 The standardization,if needed,used for qualification5.4.I Definition and Scope-Where analytical data obtainedand for analysis of each constituent shall be determined byin accordance with this test method are required,any testvalid curve-fitting procedures.A point-to-point,saw-toothmethod may be used that meets the requirements of 5.4.2,thecurve that is artificially made to fit a set of data points does notQualification of a Test Method section.A test method isconstitute a valid curve-fitting procedure.A complex polyno-considered to consist of the specific procedures,reagents,mial drawn through the points is similarly not valid.For thesupplies,equipment,instrument,and so forth,selected andsame reason,empirical inter-element corrections may be used,used in a consistent manner by a specific laboratory.See Noteonly if(N-3)2 are employed,where N is the number of4 for examples of procedures.different standards used.The qualification testing shall beNorE 4Examples of test methods used successfully by their authorsconducted with specimens newly prepared from scratch,in-for analysis of hydraulic cement are given in the list of references.cluding all the preparation stages applicable for analysis of anIncluded are test methods using atomic absorption X-ray spectrometry andunknown sample,and employing the reagents currently in usespectrophotometry-EDTA.for unknown analyses.5.4.1.1 If more than one instrument,even though substan-5.4.3 Partial Results-Test Methods that provide acceptabletially identical,is used in a specific laboratory for the sameresults for some analytes but not for others may be used onlyanalyses,use of each instrument shall constitute a separate testfor those analytes for which acceptable results are obtained.method and each must be qualified separately.5.4.4 Report of Results-When performing chemical analy-5.4.2 Qualification of a Test Method-Prior to use forsis and reporting results for Manufacturers Certification,theanalysis of hydraulic cement,each test method(see 5.4.1)musttype of method(Reference or Rapid)and the test method usedbe qualified individually for such analysis.Qualification data,along with any supporting qualification testing shall be avail-or if applicable,requalification data,shall be made availableable on request.pursuant to the Manufacturers Certification section of the5.4.5 Rejection of Material-See 4.1,the Referee Analysesappropriate hydraulic cement specification.section,and 5.3,the Alternative Analyses section.5.4.2.1 Using the test method chosen,make single determi-5.4.6 Requalification of a Test Method:nations for each analyte under consideration on at least sevenCRM samples.Requirements for a CRM are listed in 5.1,the5.4.6.1 Requalification of a test method shall be requiredCertified Reference Material section.Complete two rounds ofupon receipt of substantial evidence that the test method maytests on different days repeating all steps of sample prepara-not be providing data in accordance with Table I for one ortions.Calculate the differences between values and averages ofmore constituents.Such requalification may be limited to thoseconstituents indicated to be in error and shall be carried outthe values from the two rounds of tests.5.4.2.2 When seven CRMs are used in the qualificationprior to further use of the method for analysis of thoseprocedure,at least six of the seven differences betweenconstituents.duplicates obtained of any single analyte shall not exceed the5.4.6.2 Substantial evidence that a test method may not belimits shown in column 2 of Table 1 and the remainingproviding data in accordance with Table I shall be considereddifferences by no more than twice that value.When more thanto have been received when a laboratory is informed thatseven CRMs are used,the values for at least 77 of theanalysis of the same material by Reference Test Methods run insamples shall be within the prescribed limits,while the valuesaccordance with 4.1.1,the final average of a CCRL sample,afor the remainder shall differ by no more than twice that value.certificate value of an NIST CRM,the assigned value of an5.4.2.3 For each analyte and each CRM,the average ob-alternate CRM,or an accepted value of a known secondarytained shall be compared to the certified concentrations.Wherestandard differs from the value obtained by the test method ina certificate value includes a subscript number,that subscriptquestion by more than twice the value shown in column 2 ofTable I for one or more constituents.When indirect testmethods are involved,as when a value is obtained by3 Gebhardt.R.F.Rapid Methods for Chemical Analysis of Hydraulic Cement,difference,corrections shall be made for minor constituents inASTM STP 985,1988.order to put analyses on a comparable basis prior to determin-Barger,G.S.A Fusion Method for the X-Ray Fluorescence Analysis ofing the differences.For any constituents affected,a test methodPortland Cements,Clinker and Raw Materials Utilizing Cerium(IV)Oxide inalso shall be requalified after any substantial repair or replaceLithium Borate Fluxes,Proceedings of the Thirty Fourth Annual Conference onApplications of X-Ray Analysis.Denver Conference.Volume 29 pp.581-585.ment of one or more critical components of an instrumentAugust 5,1985.essential to the test method.C114-185.4.6.3 If an instrument or piece of equipment is replaced,6).Conventional two-pan balances shall have a maximumeven if by one of identical make or model,or is significantlysensibility reciprocal of 0.0003 g.Any rapid weighing devicemodified,a previously qualified test method using such new orthat may be provided,such as a chain,damped motion,ormodified instrument or equipment shall be considered a newheavy riders,shall not increase the basic inaccuracy by moremethod and must be qualified in accordance with 5.4.2.than 0.0001 g at any reading and with any load within the rated5.4.7 Precision and Bias-Different analytical test methodscapacity of the balance.are subject to individual limits of precision and bias.It is theNorE 6-The sensitivity of a direct-reading balance is the weightresponsibility of the user to demonstrate that the test methodsrequired to change the reading one graduation.The sensibility reciprocalused at least meet the limits of precision and bias shown infor a conventional balance is defined as the change in weight required onTable 1.either pan to change the position of equilibrium one division on the pointerscale at capacity or at any lesser load.6.General6.2.2 Weights-Weights used for analysis shall conform to6.1 Interferences and Limitations:Types I or II,Grades S or O,Classes 1,2,or 3 as described in6.1.1 These test methods were developed primarily for theSpecification E617.They shall be checked at least once a year,analysis of portland cements.However,except for limitationsor when questioned,and adjusted at least to within allowablenoted in the procedure for specific constituents,the referencetolerances for Class 3 weights(Note 7).For this purpose eachtest methods provide for accurate analyses of other hydrauliclaboratory shall also maintain,or have available for use,acements that are completely decomposed by hydrochloric acid,reference set of standard weights from 50 g to 10 mg,whichor where a preliminary sodium carbonate fusion is made toshall conform at least to Class 3 requirements and be calibratedensure complete solubility.Some of the alternative test meth-at intervals not exceeding five years by the National Institute ofods may not always provide accurate results because ofStandards and Technology(NIST).After initial calibration,interferences from elements which are not removed during therecalibration by the NIST may be waived provided it can beprocedure.shown by documented data obtained within the time intervalNorE 5-Instrumental analyses can usually detect only the elementspecified that a weight comparison between summations ofsought.Therefore,to avoid controversy,the actual procedure used for thesmaller weights and a single larger weight nominally equal toelemental analyses should be noted when actual differences with referencethat summation,establishes that the allowable tolerances haveprocedures can exist.For example,P2Os and TiO,are included withnot been exceeded.All new sets of weights purchased shallAlO in the usual wet test method and sulfide sulfur is included in mostinstrumental procedures with SO.have the weights of I g and larger made of stainless steel orother corrosion-resisting alloy not requiring protective coating.6.1.2 When using a test method that determines total sulfur,and shall meet the density requirements for Grades S or O.such as most instrumental test methods,sulfide sulfur will bedetermined with sulfate and included as such.In most hydrau-NoTE 7-The scientific supply houses do not presently list weights aslic cements,the difference resulting from such inclusion will bemeeting Specification E617.They list weights as meeting NIST or OIMLstandards.The situation with regard to weights is in a state of flux becauseinsignificant,less than 0.05 weight%In some cases,notablyof the trend toward internationalization.Hopefully this will soon beslags and slag-containing cements but sometimes other ce-resolvedments as well,significant levels of sulfide may be present.InNIST Classes S and S-1 and OIML Class F weights meet thesuch cases,especially if there is a question of meeting or notrequirements of this standard.meeting a specification limit or when the most accurate results6.2.3 Glassware and Laboratory Containers-Standardare desired,analytical test methods shall be chosen so thatvolumetric flasks,burets,and pipets should be of precisionsulfate and sulfide can be reported separately.grade or better.Standard-taper,interchangeable,ground-glass6.1.2.1 Where desired,when using instrumental test meth-joints are recommended for all volumetric glassware andods for sulfate determination,if sulfide has been determineddistilling apparatus,when available.Wherever applicable,theseparately,correct the total sulfur results(expressed as anuse of special types of glassware,such as colored glass for theoxide)in accordance with the following calculation:protection of solutions against light,alkali-resistant glass,andS03=Saa-(2.5.)(1)high-silica glass having exceptional resistance to thermal shockis recommended.Polyethylene containers are recommendedwhere:for all aqueous solutions of alkalies and for standard solutionsSO:sulfur trioxide excluding sufide sulfur,where the presence of dissolved silica or alkali from the glassStotaltotal sulfur in the sample,expressed as the oxide,would be objectionable.Such containers shall be made offrom instrumental results,high-density polyethylene having a wall thickness of at least2.5molecular ratio of SOS to express sulfur as SO,1 mm.and6.2.4 Desiccators-Desiccators shall be provided with aSsulfide sulfur presentgood desiccant,such as magnesium perchlorate,activated6.2 Apparatus and Materials:alumina,or sulfuric acid.Anhydrous calcium sulfate may also6.2.1 Balance-The analytical balance used in the chemicalbe used provided it has been treated with a color-changedeterminations shall conform to the following requirements:indicator to show when it has lost its effectiveness.Calcium6.2.1.1 The balance shall be capable of reproducing resultschloride is not a satisfactory desiccant for this type of analysis.within 0.0002 g with an accuracy of+0.0002 g.Direct-reading6.2.5 Filter Paper-Filter paper shall conform to the re-balances shall have a sensitivity not exceeding 0.0001 g(Notequirements of Specification E832,Type II,Quantitative.When5