1、Designation: D3444 00 (Reapproved 2015)Standard Test Method forTotal Acid Number of Trichlorotrifluoroethane1This standard is issued under the fixed designation D3444; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of totalacidity in trichlorotrifluoroethane and other halocarbons thatare liqui
3、d at room temperature.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this stan
4、dard 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 6.2. Summary of Test Method2.1 The total acidity of the solvent is determined by titrationwith standard alcoholi
5、c potassium hydroxide solution usingphenolphthalein solution as the indicator.3. Significance and Use3.1 This test method determines the total acidity of trichlo-rotrifluoroethane by titration with alcoholic potassium hydrox-ide using phenolphthalein for an indicator.3.2 This test method can be used
6、 to develop production andpurchasing specifications.4. Apparatus4.1 Buret, 2-mL in 0.01-mL subdivisions, self-leveling, with1000-mL reservoir.4.2 Vinyl Tubing.24.3 Two Indicating Carbon Dioxide Absorbent Tubes, 3050mesh.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tes
7、ts. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on 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 ofsuffi
8、ciently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean halide-free distilled water.5.3 Isopropyl Alcohol.5.4 Phenolphthalein Indicator Solution (0.05 g in 100 mL ofisopropy
9、l alcohol).5.5 Potassium Acid Phthalate, U.S. National Bureau ofStandards primary standard. Dry this chemical in a 120C ovenfor several hours prior to use. Store the dry chemical in adesiccator.5.6 Potassium Hydroxide Pellets.5.7 Potassium Hydroxide Solution in Isopropyl Alcohol(0.01 N)Add approxima
10、tely1gofsolid KOH to approxi-mately 1 L of anhydrous isopropyl alcohol in a 2-L Erlenmeyerflask. Boil the mixture gently for 5 to 10 min, stirring toprevent the solids from forming a cake on the bottom. Add atleast 2 g of barium hydroxide Ba(OH)2 and boil again gentlyfor 5 to 10 min. Cool to room te
11、mperature. Allow to stand forseveral hours and filter the supernatant liquid through a finesintered glass or porcelain filtering funnel. Avoid unnecessaryexposure to CO2during filtration. Store the solution out ofcontact with cork or rubber. Protect the solution from CO2bya guard tube containing car
12、bon dioxide adsorbent. Standardizeagainst pure potassium acid phthalate in about 25 mL ofCO2-free water using phenolphthalein to detect the end point.6. Hazards6.1 Trichlorotrifluoroethane removes natural oils from skin.Avoid skin contact. The solvent is not flammable and has athreshold limit value
13、of 1000 ppm by volume in air. See themanufacturers MSDS.1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 1, 2015. Publish
14、ed June 2015. Originallyapproved in 1975. Last previous edition approved in 2010 as D3444 00(2010)1.DOI: 10.1520/D3444-00R15.2Tygon has been found satisfactory. An equivalent may be used.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For sugge
15、stions 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.Copyright ASTM International,
16、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.2 Isopropyl alcohol is flammable, and has a thresholdlimit value of 400 ppm by volume in air. See the manufactur-ers MSDS.6.3 Potassium hydroxide is corrosive to body tissue. Avoidcontact with the solid and its sol
17、ution. Should this chemicalcontact the person, immediately flush the affected area withcopious amounts of water. See the manufacturers MSDS.7. Procedure7.1 For sample analysis, add 50 mL of isopropyl alcohol toa 250-ml Erlenmeyer flask, add 5 drops of phenolphthaleinindicator solution and titrate to
18、 a pink end point with alcoholicKOH solution.7.1.1 Swirl flask contents gently during titration. The endpoint should last for 10 to 15 s. Stopper the flask until thesample is added to minimize CO2contamination.7.2 Pour a weighed sample (about 50.00 6 0.02 g) into theflask containing the pretitrated
19、alcohol.7.3 Titrate the sample with the standard alcoholic KOHsolution to a 15-s pink end point. Record the amount of titrantrequired.7.4 For standardization of 0.01 N KOH in isopropyl alcohol,proceed as follows:7.4.1 Weigh (60.0001 g) 0.142 6 0.005 g of dry (NationalBureau of Standards) primary sta
20、ndard potassium acid phtha-late into a 1-L volumetric flask containing about 500 mL ofdeionized CO2-free water, then stopper the flask.7.4.2 Swirl the flask to dissolve the potassium acid phtha-late.7.4.3 Fill the flask to volume with deionized, CO2-freewater, stopper the flask then mix the solution
21、 thoroughly.7.4.4 Place 25 mL (transfer pipet) of deionized, CO2-freewater and 5 drops of phenolphthalein indicator solution into a250-mL Erlenmeyer flask.7.4.5 Pipet 25 mL (transfer pipet) of the potassium acidphthalate standard solution into the flask, then seal the flaskwith a stopper.NOTE 1Neopr
22、ene has been found satisfactory. An equivalent may beused.7.4.6 Treat the blank and standard alike from this point on.7.4.7 Titrate the standard with the approximate 0.01 Npotassium hydroxide solution to the phenolphthalein indicatorend point. Record the titer.8. Calculation8.1 Calculate the acid nu
23、mber of the solvent as follows:Total acid number in 1 mg of KOH/g sample5 A 3 N 356.1!/W (1)where:A = millilitres of KOH solution required for titration ofsample, mL,N = normality of KOH solution, andW = weight of sample, g.8.2 Calculate the normality of the potassium hydroxidestandard as follows:N,
24、 KOH 5 G 3 V!/204.224 3 A 2 B!# (2)where:A = standard titer, mL,B = blank titer, mL,G = potassium acid phthalate, g,V = potassium acid phthalate aliquot, mL, and204.224 = potassium acid phthalate/mole, g.8.3 Average the normality values obtained from triplicateanalyses to the nearest 0.0001 unit. Us
25、e the average normalityfor sample calculation.9. Precision and Bias49.1 Repeatability (Single Analyst): At a mean value of0.0018 mg-KOH/g the standard deviation of results (each theaverage of triplicates obtained by the same analyst on twodifferent days) has been estimated to be 0.0010 mg-KOH/g atth
26、ree degrees of freedom. Two such values should be consid-ered suspect (95 % confidence level) if they differ by more than0.0045 mg-KOH/g.9.2 Reproducibility (Multilaboratory): At a mean value of0.0018 mg-KOH/g the standard deviation of results (each theaverage of triplicates in three different labor
27、atories), obtainedby analysts in different laboratories, has been estimated to be0.0036 mg-KOH/g at two degrees of freedom. Two such valuesshould be considered suspect (95 % confidence level) if theydiffer by more than 0.0219 mg-KOH/g.10. Keywords10.1 acidity; CFC-113; total acid number; trichlorotr
28、ifluo-roethaneASTM International takes no position respecting the validity of any patent rights asserted in connection with 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 su
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31、e ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor 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
32、 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D26-1011.D3444 00 (2015)2
