1、Designation: E449 08 (Reapproved 2013)E449 18Standard Test Methods forAnalysis of Calcium Chloride1This standard is issued under the fixed designation E449; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、 A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope Scope*1.1 These test methods cover the analysis o
3、f calcium chloride and solutions.1.2 Procedures are given for the determination of calcium chloride, magnesium chloride, potassium chloride, sodium chloride,and calcium hydroxide. The test methods appear in the following order:SectionsCalcium Chloride 8 to 16Calcium Chloride 8 to 17Magnesium Chlorid
4、e, Potassium Chloride,and Sodium Chloride17 to 26Magnesium Chloride, Potassium Chloride,and Sodium Chloride18 to 28Calcium Hydroxide 27 to 33Calcium Hydroxide 29 to 361.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.1.4 Review
5、 the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first aid procedures, handling, andsafety precautions.1.5 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
6、establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. Specific hazard statements are given in Section 5.1.5 Review the current Material Safety Data Sheet (MSDS) for detailed information concerning toxicit
7、y, first aid procedures,handling, and safety precautions.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issue
8、dby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D345 Test Method for Sampling and Testing Calcium Chloride for Roads and Structural ApplicationsD1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality Ass
9、urance Procedures for Aromatic Hydrocarbons and Related MaterialsE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions fo
10、r Chemical AnalysisE663 Practice for Flame Atomic Absorption Analysis (Withdrawn 1997)31 These test methods are under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and are thedirect responsibility of Subcommittee D16.16 on Indus
11、trial and Specialty Product Standards.Current edition approved June 1, 2013Feb. 1, 2018. Published June 2013April 2018. Originally approved in 1972. Last previous edition approved in 20082013 asE449 08.E449 08 (2013). DOI: 10.1520/E0449-08R13.10.1520/E0449-18.2 For referencedASTM standards, visit th
12、eASTM 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.3 The last approved version of this historical standard is referenced on www.astm.org.This document i
13、s not 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 approp
14、riate. 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 State
15、s13. Significance and Use3.1 Calcium chloride is available in various forms and purities. A major use is the de-icing and dust control of roads. It is alsoused in the coal industry for dustproofing and freezeproofing, in foods, in electrolytic cells, and in refrigeration brines. The testmethods list
16、ed in 1.2 provide procedures for analyzing calcium chloride to determine if it is suitable for its intended use.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, these shall conform tothe specifications of the Committee on Analytical Rea
17、gents of the American Chemical Society, where such specifications areavailable.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.4.2 Purity of WaterUnless otherwise indicat
18、ed, references to water shall be understood to mean Type II or Type III reagentwater conforming to Specification D1193.5. Hazards5.1 While calcium chloride is a relatively harmless material, some of the reagents used in these methods present possible safetyhazards. Potassium cyanide is extremely haz
19、ardous and must be handled with great care. In addition to being poisonous, solutionscontaining cyanide should never be mixed with acids to preclude the release of poisonous hydrogen cyanide gas. Concentratedhydrochloric acid and sodium hydroxide also are hazardous chemicals which may produce seriou
20、s burns on contact.6. Atomic Absorption Spectrophotometers6.1 Photometers and photometric practice used in these methods shall conform to Practice E663.7. Sampling7.1 Sampling of calcium chloride is not within the scope of these test methods. See the appropriate sections of Test MethodD345.7.2 The s
21、ample to be analyzed shall be considered to be that sample in a single bottle submitted to the analytical laboratory.7.3 The size of the sample shall be sufficient to perform all analyses without the reuse of any portion of the sample.CALCIUM CHLORIDE8. Scope8.1 This test method covers the determina
22、tion of calcium chloride in the range from 0 to 100 %.8. Scope8.1 This test method covers the determination of calcium chloride in the range from 0 to 100 %.9. Summary of Test Method9.1 Calcium in an alkaline solution is titrated with standard ethylenediaminetetraacetate solution, using modified cal
23、cein II asan indicator. The color change is from green to purple. -hydroxynaphthol blue is also suitable as an indicator, in which case thecolor change is from red to blue.10. Interferences10.1 Strontium and other cations not complexed with cyanide at pH of at least 10 will consume ethylenediaminete
24、traacetatesolution and will affect the accuracy of this test method.11. Apparatus11.1 Buret, 50-mL, Class A.11.2 Weighing Bottle, glass-stoppered, 100-mL.12. Reagents12.1 Calcium Chloride, Standard Solution (1 mL = 0.00832 g CaCl2)Weigh 7.500 g of primary standard calcium carbonate(CaCO3). Transfer
25、to a 600-mL beaker and add 300 mL of water. Cover with a watch glass and slowly add to the beaker, while4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see
26、 Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.E449 182stirring, 15 mL of concentrated hydrochloric acid (HCl) delivered from a pipet inserted between the
27、lip of the beaker and the edgeof the watch glass. When dissolution of the CaCO3 is complete, boil gently to expel CO2. Cool, and transfer to a 1-L volumetricflask. Dilute to volume with water and mix.12.2 Ethylenediaminetetraacetate, Standard Solution (0.1 mol/L (M)Dissolve 37.22 g of disodium dihyd
28、rogen ethylenedi-aminetetraacetate dihydrate (EDTA) in water. Transfer to a 1-Lvolumetric flask, dilute to volume with water, and mix. Standardizeas follows:Transfer a 50-mLaliquot of CaCl2 standard solution (1 mL = 0.00832 g CaCl2) to a 500-mLErlenmeyer flask and diluteto 200 mL with water. Proceed
29、 as directed in 13.2. Calculate the CaCl2 equivalent of the EDTA solution as follows:Calcium chloride equivalent,g/mL50.416/A (1)where:A = millilitres of EDTA solution required for the titration of the CaCl2 solution.12.3 Hydrochloric Acid (1 + 3)Mix 1 volume of concentrated hydrochloric acid (HCl,
30、sp gr 1.19) and 3 volumes of water.12.4 Hydroxylamine Hydrochloride Solution(10 %)Dissolve 10 g of hydroxylamine hydrochloride (NH2OHHCl) in 90 mLof water.12.5 -Hydroxynaphthol Blue. 512.6 Modified Calcein Indicator. 612.7 Potassium Cyanide (KCN).12.8 Sodium Hydroxide Solution (80 g/L)Add slowly 80
31、g of sodium hydroxide (NaOH) in 300 mL of water stirringconstantly. Cool, transfer to a 1-L volumetric flask, dilute to volume with water, and mix.12.9 Sugar, granulated.13. Procedure13.1 Solid SamplesWeigh 100.0 g of sample and wash into a 1000-mLvolumetric flask with water.Add 10 mLof HCl (1 + 3)a
32、nd swirl to dissolve the sample. Cool to room temperature, make to volume with water, and mix. Pipet a 20-mL aliquot into a500-mL volumetric flask, dilute to volume, and mix. Proceed as in 13.3.13.2 Liquid SamplesWeigh 100.0 g of sample and wash into a 1000-mL volumetric flask with water. Add 10 mL
33、of HCl(1 + 3) and mix. Cool to room temperature, make up to volume with water, and mix. Pipet an aliquot containing about 2 g of CaCl2into a 500-mLvolumetric flask, dilute to volume, and mix.Appropriate aliquot volumes are indicated in the table below. Interpolateif necessary.Expected CaCl2Concentra
34、tion, %AliquotSize, mL10 20020 10030 7540 5050 4013.3 Pipet a 100-mL aliquot of the solution prepared in 13.1 or 13.2 into a 500-mL Erlenmeyer flask and dilute to about 200mL with water. Add in order 10 mL of hydroxylamine hydrochloride solution and 3 g of sugar. Swirl to dissolve. Add 40 mL ofNaOH
35、solution (12.8) and swirl to mix. Add 0.1 g of KCN, and swirl to dissolve and mix. Add about 0.2 g of calcium indicator.13.4 Titrate with 0.1 M EDTA solution until the indicator changes from green to purple.NOTE 1If -hydroxynaphthol blue indicator is used, 0.4 g should be added and the solution titr
36、ated to a blue end point.13.5 Analyze sample in duplicate.14. Calculation14.1 Calculate the calcium chloride concentration as follows:Calcium chloride,%5A 3B!/C#31002D (2)where:A = millilitres of EDTA solution required for titration of the sample,B = calcium chloride equivalent of the EDTA solution,
37、 g/mL,C = mass of sample in the aliquot used, andD = percent calcium hydroxide expressed as calcium chloride (see 31.1.1).D = percent calcium hydroxide expressed as calcium chloride (see 33.1.1).14.2 Average the duplicate results. Duplicate determinations that agree within 0.3 % absolute are accepta
38、ble for averaging(95 % confidence level).E449 18315. Report15.1 Report the percentage of CaCl2 to the nearest 0.1 %. Duplicate determinations that agree within 0.3 % absolute areacceptable for averaging (95 % confidence level).16. Precision and Bias516.1 The following criteria should be used An ILS
39、was conducted which included eight laboratories analyzing two samples.Each sample was analyzed in duplicate on two different days. Practice E180 was followed for judging the acceptability of results(seethe design and analysis of the data; Note 2).the details are given is ASTM Research Report RR:E15-
40、1015.16.1.1 Intermediate Precision, formerly called Repeatability (Single Analyst)The standard deviation of results (each theaverage of duplicates), obtained by the same analyst on different days, has been estimated to be 0.139 % absolute at 28 degreesof freedom. Two such values should be considered
41、 suspect (95 % confidence level) if they differ by more than 0.4 %.16.1.2 Reproducibility (Multilaboratory)The standard deviation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be 0.229 % absolute at 6 degrees of freedom. Two such va
42、lues should beconsidered suspect (95 % confidence level) if they differ by more then 0.8 % absolute.NOTE 2The precision statements are based on an interlaboratory study performed in 1970 on two samples of solid calcium chloride. Eight laboratoriesparticipated in the study analyzing each sample in du
43、plicate on each of two days. Practice E180 was used in developing these precision statements.716.2 The bias of the test this method has not yet been determined.17. Quality Guidelines17.1 Laboratories shall have a quality control system in place.17.1.1 Confirm the performance of the test instrument o
44、r test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.17.1.2 Aquality control sample is a stable material isolated from the production process and representative of the sample beinganalyzed.17.1.3 When QA/QC protocols are alread
45、y established in the testing facility, these protocols are acceptable when they confirmthe validity of test results.17.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines described in Guide D6809 orsimilar statistical quality control practices.MAGNESIUM CHLO
46、RIDE, POTASSIUMCHLORIDE, AND SODIUM CHLORIDE17. Scope17.1 This test method covers the determination of magnesium chloride, potassium chloride, and sodium chloride in the rangesnormally encountered in calcium chloride.18. Scope18.1 This test method covers the determination of magnesium chloride, pota
47、ssium chloride, and sodium chloride in the rangesnormally encountered in calcium chloride.19. Summary of Test Method19.1 A solution of the sample is aspirated into the air-acetylene flame of an atomic absorption spectrometer. The absorption ofa resonance line from the spectrum of each cation is meas
48、ured and compared with the response of the instrument to calibrationsolutions of the same elements. Recommended lines are: magnesium (2852 ), potassium (7664 ), and sodium (5889 ).20. Concentration Range20.1 The concentration range for each cation must be selected to correspond with the optimum rang
49、e of the instrumentemployed. Higher or lower concentration ranges may be required for different instruments or different source lamps.21. Interferences21.1 Elements normally present in calcium chloride do not interfere with these determinations.22. Apparatus22.1 Atomic Absorption Spectrophotometer, capable of isolating the resonance line chosen for each cation sufficiently to avoidinterference from other elements in the samples being analyzed.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Resear
