1、Designation: D 2989 01 (Reapproved 2006)Standard Test Method forAcidity-Alkalinity of Halogenated Organic Solvents andTheir Admixtures1This standard is issued under the fixed designation D 2989; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test me
3、thod covers the determination of acidity inhalogenated organic solvents and admixtures thereof. Thealkalinity may be determined utilizing Test Method D 2106,bysubstituting the end point measured at pH 7 by bromothymolblue or pH meter.1.2 This standard does not purport to address all of thesafety con
4、cerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 7.2. Referenced Document
5、s2.1 ASTM Standards:2D 2106 Test Methods for Determination of Amine AcidAcceptance (Alkalinity) of Halogenated Organic SolventsD2110 Test Method for pH of Water Extractions of Halo-genated Organic Solvents and Their Admixtures3. Summary of Test Method3.1 A sample of halogenated solvent or admixture
6、is mea-sured for pH using Test Method D2110. If the pH of thesample is above 7.0, the alkalinity is determined using TestMethod D 2106 (to an end point of pH 7). If the pH is below7.0, the free acid content of the halogenated organic solvent oradmixture is determined after water extraction using Pro
7、cedureA, or can be determined directly using Procedure B.3.1.1 Procedure A, using glass electrode pH meter, or3.1.2 Procedure B, anhydrous methanolic sodium hydroxidetitration.4. Significance and Use4.1 This test method can be used to establish manufacturingand purchasing specifications. It can also
8、 be used to determinethe condition of solvents in use.5. Apparatus5.1 Separatory Funnel, 250-mL.5.2 Graduated Cylinder, 100 mL.5.3 Volumetric Pipets, 1 mL, 10 mL, 25 mL, 50 mL.5.4 Beaker, 100 mL.5.5 Borosilicate or Stainless Steel Beaker,2L.5.6 Erlenmeyer Flask, 100 mL.5.7 pH Meter with pH Electrode
9、s.5.8 Buret,10mL.5.9 Volumetric Flask, 100 mL, 1 L.5.10 Micro Buret, 5 mL, Class A or Syringe, 100 L.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee o
10、n Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 WaterPrepare neutral, dist
11、illed or deionized water asfollows: Boil 1 L of distilled or deionized water for 5 min in aborosilicate glass or stainless steel container, then cover andcool to room temperature. Titrate to a pH of 7.0 to 7.3 with1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organi
12、c Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1971 as D 2989 71 T. Last previous edition approved in 2001 asD298901e1.2For referenced ASTM standards, vi
13、sit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washing
14、ton, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright A
15、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.either 0.01 N sodium hydroxide (NaOH) solution or 0.01 Nhydrochloric acid (HCl), depending upon whether the initialpH is above or below 7.6.3 Bromothymol Blue Indicator Solution (0.1 %)Indicator so
16、lution may be purchased from a laboratory supplyhouse or prepared as follows: Dissolve 0.1 g of dibromothymolsulfonephthalein in 1.6 mL of 0.1 N NaOH solution and diluteto 100 mL with methanol.6.4 Sodium Hydroxide Solution (0.01 N), ProcedureADissolve4gofsodium hydroxide (NaOH) in boiled,neutral, di
17、stilled or deionized water and dilute to 1000 mL.Prepare 0.01 N NaOH solution by diluting 10.0 mL of the 0.1N NaOH to 100 mL with boiled, neutral, distilled or deionizedwater in a calibrated volumetric flask. Standardize this 0.01 NNaOH by any accepted procedure to determine the exactnormality. This
18、 reagent is also available from most supplyhouses. Protect the reagent from absorption of atmosphericcarbon dioxide and standardize weekly.6.5 Sodium Hydroxide Methanolic Solution (0.01 N), Pro-cedure BDissolve4gofACSreagent grade sodium hydrox-ide (NaOH) in ACS reagent grade anhydrous methanol andd
19、ilute to 1000 mL with ACS reagent grade anhydrous metha-nol. Prepare 0.01 N methanolic NaOH solution by diluting 10.0mL of the 0.1 N NaOH to 100 mL with ACS reagent gradeanhydrous methanol in a calibrated volumetric flask. Standard-ize this 0.01 N NaOH by any accepted procedure to determinethe exact
20、 normality. This reagent is also available from mostsupply houses. Protect the reagent from absorption of atmo-spheric carbon dioxide and standardize weekly.7. Hazards7.1 Solvent HazardsContact with skin should be avoidedto prevent removal of natural oils. Solvents are not flammable,but each has a t
21、hreshold limit value for contact with vapors.These threshold limits should be determined before a solvent islisted.7.2 NaOH as a solid or in solution can be hazardous if thereis skin contact.8. Procedure8.1 Procedure APipet 50 mL of halogenated organicsolvent or admixture into a 250 mL separatory fu
22、nnel contain-ing 50 mL of freshly boiled, neutral (pH 7.0 to 7.3), distilled ordeionized water. Shake the mixture for 2 min, then let standand allow the layers to separate. Drain and discard the lower,organic layer from the separatory funnel and transfer the waterlayer to a 100mL beaker. Titrate the
23、 sample, with stirring,with 0.01 N NaOH using a 5 mL Class A buret until the pH isstable between 7.0 and 7.3 for 30 s. A 100 L syringe can besubstituted for the micro buret. This technique is often used tomeasure very low levels of acidity, below 1 ppm. Technique isvery important. Titrate slowly, ma
24、king sure the titrant fallscleanly into the water being titrated. Record the titer andcalculate the acidity in accordance with 9.1.8.2 Procedure BPipet 50 mL of halogenated organicsolvent or admixture into a clean, dry, 100-mL Erlenmeyerflask. Add 1 mL of bromothymol blue indicator solution andtitra
25、te, with stirring, with 0.01 N methanolic NaOH solution tothe bromothymol blue end point (see Note 1).NOTE 1The bromothymol blue end point may be interpreted as anaqua (blue-green) to light blue color.9. Calculation9.1 ProcedureCalculate the acidity of halogenated or-ganic solvents or admixtures as
26、equivalent hydrochloric acid inweight percent or weight ppm as follows:equivalent HCl, weight % 5 V3 N 3 0.0365!/W 3 100 (1)equivalent HCl, ppm 5 V 3 N 3 0.0365!/W 3 1 000 000where:V = Volume in mL, NaOH solution required for titration ofthe sample,N = Normality of the NaOH solution, andW = Weight o
27、f the sample used, in g as weighed or g =sample volume in mL times its density in g per mL.10. Precision410.1 Using Method A, one standard deviation betweenresults of a sample run by different laboratories should be nomore than about 60.5 ppm. Within a laboratory, one standarddeviation between resul
28、ts should be no more than about 0.2ppm. Bias was not determined in this study.10.2 Using Method B, one standard deviation betweenresults of a sample run by different laboratories should be nomore than about 61.0 ppm. Within a laboratory, one standarddeviation between results should be no more than a
29、bout 0.1ppm. Bias for this method is approximately +1 ppm.11. Keywords11.1 acidity; alkalinity; bromothymol blue; halogenated sol-vents; hydrochloric acid; pH meter; sodium hydroxide; titrationASTM International takes no position respecting the validity of any patent rights asserted in connection wi
30、th any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible tech
31、nical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful considerat
32、ion at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Ha
33、rbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).4A research report is available from ASTM headquarters. Request RR:D261016.D 2989 01 (2006)2
