1、Standard Method of Test for Chemical Analysis of Hydraulic Cement AASHTO Designation: T 105-161 Release: Group 1 (April 2016) ASTM Designation: C114-15 American Association of State Highway and Transportation Officials 444 North Capitol Street N.W., Suite 249 Washington, D.C. 20001 TS-3a T 105-1 AAS
2、HTO Standard Method of Test for Chemical Analysis of Hydraulic Cement AASHTO Designation: T 105-161Release: Group 1 (April 2016) ASTM Designation: C114-15 1. SCOPE 1.1. These test methods cover the chemical analyses of hydraulic cements. Any test methods of demonstrated acceptable precision and bias
3、 may be used for analysis of hydraulic cements, including analyses for referee and certification purposes, as explained in Section 4. Specific chemical test methods are provided for ease of reference for those desiring to use them. They are grouped as Reference Test Methods and Alternate Test Method
4、s. The reference test methods are long accepted classical chemical test methods, which provide a reasonably well-integrated basic scheme of analysis for hydraulic cements. The alternative test methods generally provide individual determination of specific analytes and may be used alone or as alterna
5、tes and determinations within the basic scheme at the option of the analyst and as indicated in the individual method. The individual analyst must demonstrate achievement of acceptable precision and bias, as explained in Section 4, when these methods are used. 1.2. Contents: Section Subject 2 Refere
6、nced Documents 3 Terminology 4 Description of Referee Analyses 4.1 Referee Analyses 5 Qualification for Different Analyses 5.1 Certified Reference Materials 5.2 Requirements for Qualification Testing 5.3 Alternative Analyses 5.4 Performance Requirements for Rapid Test Methods 6 General 6.1 Interfere
7、nces and Limitations 6.2 Apparatus and Materials 6.3 Reagents 6.4 Sample Preparation 6.5 General Procedures 6.6 Recommended Order for Reporting Analyses Reference Test Methods 7 Insoluble Residue 8 Silicon Dioxide 8.1 Selection of Test Method 8.2 Silicon Dioxide in Portland Cements and Cements with
8、Low Insoluble Residue 2016 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.TS-3a T 105-2 AASHTO Section Reference Test Methods (continued) 8.3 Silicon Dioxide in Cements with Insoluble Residue Greater Than 1
9、Percent 9 Ammonium Hydroxide Group 10 Ferric Oxide 11 Phosphorus Pentoxide 12 Titanium Dioxide 13 Zinc Oxide 14 Aluminum Oxide 15 Calcium Oxide 16 Magnesium Oxide 17 Sulfur 17.1 Sulfur Trioxide 17.2 Sulfide 18 Loss on Ignition 18.1 Portland Cement 18.2 Portland Blast-Furnace Slag Cement and Slag Cem
10、ent 19 Sodium and Potassium Oxides 19.1 Total Alkalies 19.2 Water-Soluble Alkalies 20 Manganic Oxide 21 Chloride 22 Chloroform-Soluble Organic Substances Alternative Test Methods 23 Calcium Oxide 24 Carbon Dioxide 25 Magnesium Oxide 26 Loss on Ignition 26.1 Portland Blast-Furnace Slag Cement and Sla
11、g Cement 27 Titanium Dioxide 28 Phosphorus Pentoxide 29 Manganic Oxide 30 Free Calcium Oxide Appendixes Appendix X1 Example of Determination of Equivalence Point for the Chloride Determination Appendix X2 CO2Determinations in Hydraulic Cements 1.3. The values stated in SI units are to be regarded as
12、 the standard. 1.4. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations
13、prior to use. See Sections 8.3.2.1 and 16.4.1 for specific caution statements. 2016 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.TS-3a T 105-3 AASHTO 2. REFERENCED DOCUMENTS 2.1. ASTM Standards: C25, Stand
14、ard Test Methods for Chemical Analysis of Limestone, Quicklime, and Hydrated Lime D1193, Standard Specification for Reagent Water E29, Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications E275, Standard Practice for Describing and Measuring Perform
15、ance of Ultraviolet and Visible Spectrophotometers E350, Standard Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and Wrought Iron E617, Standard Specification for Laboratory Weights and Precision Mass Standards E832, Standard Specification
16、for Laboratory Filter Papers 3. TERMINOLOGY 3.1. Definition: 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. DESCRIPTION OF REFEREE A
17、NALYSES 4.1. Referee AnalysesWhen conformance to chemical specification requirements is questioned, perform referee analyses as described in Section 4.1.1. The reference test methods that follow in Sections 7 through 22, or other test methods qualified according to Section 5.4, Performance Requireme
18、nts for Rapid Test Methods, are required for referee analysis. A cement shall not be rejected for failure to conform to chemical requirements unless all determinations of constituents involved and all necessary separations prior to the determination of any one constituent are made entirely by these
19、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 on different days. If the two results do not agree within the permissible variation given in Table 1, the determination shall be repeated until two or
20、 three results agree within the permissible variation. When two or three results do agree within the permissible variation, their average shall be accepted as the correct value. When an average of either two or three results can be calculated, the calculation shall be based on the three results. For
21、 the purpose of comparing analyses and calculating the average of acceptable results, the percentages shall be calculated to the nearest 0.01 (or 0.001 in the case of chloroform-soluble organic substances), although some of the average values are reported to 0.1 as indicated in the test methods. Whe
22、n a blank determination (see Note 1) is specified, one shall be made with each individual analysis or with each group of two or more samples analyzed on the same day for a given analyte. Note 1A blank determination is a procedure that follows all steps of analysis, but in the absence of a sample. It
23、 is used for detection and compensation of systematic bias. 2016 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.TS-3a T 105-4 AASHTO Table 1Maximum Permissible Variation in Resultsa(Column 1) Analyte (Column
24、 2) Maximum Difference between Duplicatesb(Column 3) Maximum Difference of the Average of Duplicates from CRM Certificate Valuesb ,c ,dSiO2(silicon dioxide) 0.16 0.20 Al2O3(aluminum oxide) 0.20 0.20 Fe2O3(ferric oxide) 0.10 0.10 CaO (calcium oxide) 0.20 0.30 MgO (magnesium oxide) 0.16 0.20 SO3(sulfu
25、r trioxide) 0.10 0.10 LOI (loss on ignition) 0.10 0.10 Na2O (sodium oxide) 0.03 0.05 K2O (potassium oxide) 0.03 0.05 TiO2(titanium dioxide) 0.02 0.03 P2O5(phosphorus pentoxide) 0.03 0.03 ZnO (zinc oxide) 0.03 0.03 Mn2O3(manganic oxide) 0.03 0.03 S (sulfide sulfur) 0.01 e Cl (chloride) 0.003 0.005e I
26、R (insoluble residue) 0.10 e Cx (free calcium oxide) 0.20 e CO2(carbon dioxide) 0.12 e,fAlksol(water-soluble alkali)g0.75/w ge Chlsol(chloroform-soluble organic substances) 0.004 e a When all seven Certified Reference Material (CRM) cements are required, as for demonstrating performance of rapid tes
27、t methods, at least six of the seven shall be within the prescribed limits, and the seventh shall differ by no more than twice that value. When more than seven CRMs are used, as for demonstrating the performance of rapid test methods, at least 77 percent shall be within the prescribed limits, and th
28、e remainder no more than twice the value. When a lesser number of CRM cements are required, all of the values shall be within the prescribed limits. b Where no value appears in Column 3, CRM certificate values do not exist. In such cases, only the requirement for differences between duplicates shall
29、 apply. c Interelement corrections may be used for any oxide standardization provided improved accuracy can be demonstrated when correction is applied to all seven CRM cements.d Where a CRM certificate value includes a subscript number, that subscript number shall be treated as a valid significant f
30、igure. e Not applicable. No certificate value given. f Demonstrate performance by analysis, in duplicate, of at least one portland cement. Prepare three standards, each in duplicate: Standard A shall be selected portland cement, Standard B shall be Standard A containing 2.00 percent Certified CaCO3(
31、e.g., NIST 915a), Standard C shall be Standard A containing 5.00 percent Certified CaCO3. Weigh and prepare two separate specimens of each standard. Assign the CO2content of Standard A as the average of the two values determined, provided they agree within the required limit of Column 2. Assign CO2v
32、alues to Standards B and C as follows: Multiply the Certified CaCO3value (Y) for CO2(from the certificate value) by the mass fraction of Certified CaCO3 added to that standard (percentage added divided by 100); multiply the value determined for Standard A by the mass fraction of Standard A in each o
33、f the other standards (i.e., 0.98 and 0.95 for Standards B and C, respectively); add the two values for Standards A and B, respectively; 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 percent B = 0.98A + 0.80 percent by mass. C = 0.95A
34、 + 2.00 percent by mass. Maximum difference between the duplicate CO2values for Standards B and C, respectively, shall be 0.17 and 0.24 percent by mass. Averages of the duplicate values for Standards B and C shall differ from their assigned values (B and C) by no more than 10 percent of those respec
35、tive assigned values. g w = mass, in grams, of samples used for the test. TS-3a T 105-5 AASHTO 5. QUALIFICATION FOR DIFFERENT ANALYSES 5.1. Certified Reference MaterialsA Certified Reference Material (CRM) must be used in the qualification of test methods and analysts. Acceptable reference cements a
36、re National Institute of Standards and Technology (NIST) CRMs or other reference cements traceable to the NIST CRMs. The reference cement must have an assigned value for the analyte being determined. Traceability consists of documentary evidence that the assigned values of the reference cement are c
37、ompatible with the certified values of NIST CRMs. To demonstrate traceability for a given analyte, perform a referee analysis (as defined in Section 4.1) on the proposed reference cement, using an NIST CRM for demonstration of precision and accuracy. The reference cement is acceptable if its assigne
38、d value agrees with the average referee value within the limits given in Column 3 of Table 1. If the reference cement, as supplied, has no documented guarantee of homogeneity, establish its homogeneity by analyzing at least six randomly selected samples. No result shall deviate from the assigned val
39、ue by more than the limits given in Column 2 of Table 1. An acceptable reference cement must be accompanied by a document showing the data produced in demonstrating traceability and homogeneity. 5.2. Requirements for Qualification TestingQualified test methods are required whenever testing is perfor
40、med for the following reasons: (1) Referee analyses, (2) analyses intended for use as a basis for acceptance or rejection of a cement, or (3) manufacturers certification. When Reference methods are used, qualification testing of the analyst is required as described in Section 5.2.1. When Rapid metho
41、ds are used, qualification testing of both the analyst and the test method are required as described in Sections 5.2.1 and 5.4. Such demonstration may be made concurrently with analysis of the cement being tested. The requirements for qualification of a test method and analyst are summarized in Tabl
42、e 2. Table 2Minimum Number of CRMs Required for Qualification of Chemical Testing Equipment Qualification Operator QualificationcMethod Type ReferenceaOtherbNone 7 1 1 a Reference methods are those outlined in Sections 7 through 22. b These may be any test method as described in Section 5.3, Alterna
43、tive Analyses, or any instrumental or rapid test method, which must be qualified in accordance with Section 5.4, Performance Requirements for Rapid Test Methods. c Each analyst performing acceptance or reference analyses must be qualified in accordance with Section 5.2.1, Performance Requirements fo
44、r Rapid Test Methods, at a frequency of 2 years. If qualification of the instrument is completed by a single analyst, the analyst has demonstrated individual qualifications per Section 5.2.1. Initial qualification of the analyst shall be demonstrated by analysis of each constituent of concern in at
45、least one CRM cement in duplicate, no matter what test method is used (Note 2). Duplicate samples shall be run on different days. The same test methods to be used for analysis of cement being tested shall be used for analysis of the CRM cement. If the duplicate results do not agree within the permis
46、sible variation given in Table 1, the determinations shall be repeated, following identification and correction of problems or errors, until a set of duplicate results do agree within the permissible variation. Requalification of the analyst is required every two years. Note 2When qualifying a rapid
47、 method with seven CRMs in accordance with Section 5.4.2, the analyst performing the qualification of the test method may simultaneously qualify for the requirement of Section 5.2.1. 5.2.1. The average of the results of acceptable duplicate determinations for each constituent may differ from the CRM
48、 assigned value by no more than the value shown in Column 3 of Table 1 after necessary corrections for minor analytes are made. 5.2.2. Qualification data demonstrating that the same operator or analyst making the acceptance determination obtained precise and accurate results with CRM cements as per
49、Section 5.4 shall be made available on request to all parties concerned when there is a question of acceptance of a 2016 by the American Association of State Highway and Transportation Officials.All rights reserved. Duplication is a violation of applicable law.TS-3a T 105-6 AASHTO cement. If the CRM used is not an NIST cement, the traceability documentation of the CRM used shall also be made available on request. 5.3. Alternative AnalysesThe alternative test methods provide, in so
