1、Designation: D 1045 08Standard Test Methods forSampling and Testing Plasticizers Used in Plastics1This standard is issued under the fixed designation D 1045; 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.1. Scope*1.1 These test methods cover sampling and testing of liquidplasticizers used in compounding of plastics. Acid number,ester content, sp
3、ecific gravity, color, refractive index, and watercontent are determined.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its u
4、se. 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 hazardsinformation is given in Section 5.NOTE 1There is no similar or equivalent ISO standard.2. Referenced
5、 Documents2.1 ASTM Standards:2D70 Test Method for Density of Semi-Solid BituminousMaterials (Pycnometer Method)D 287 Test Method forAPI Gravity of Crude Petroleum andPetroleum Products (Hydrometer Method)D 792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Plastics by Displacem
6、entD 883 Terminology Relating to PlasticsD 1193 Specification for Reagent WaterD 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D 1218 Test Method for Refractive Index and RefractiveDispersion of Hydrocarbon LiquidsD 1544 Test Method for Color of Transparent Liquids(Gardner Color
7、 Scale)D 1600 Terminology for Abbreviated Terms Relating toPlasticsD 3465 Test Method for Purity of Monomeric Plasticizersby Gas ChromatographyD 4052 Test Method for Density and Relative Density ofLiquids by Digital Density MeterD 5386 Test Method for Color of Liquids Using TristimulusColorimetryE1
8、Specification for ASTM Liquid-in-Glass ThermometersE 203 Test Method for Water Using Volumetric Karl FischerTitration3. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nology D 883 and Terminology D 1600, unless otherwiseindicated.4. Significance and Use4.1 These test methods shal
9、l be used in establishing andconfirming quality control standards for liquid plasticizers usedin the compounding of plastics.5. Hazards5.1 Chemical Hazard of ReagentsIt is possible that someof the chemicals used in this test method are hazardous.Accepted laboratory safety procedures must be followed
10、. Seesuppliers material safety data sheets for further information.6. Sampling6.1 The method of sampling specified in 6.2 or 6.3 shall beused, according to the special conditions that exist.6.2 From Loaded Tank Car or Other Large VesselThecomposite sample taken shall be not less than 2 L (12 gal). I
11、t isimportant that the composite sample consists of small samplesof not more than 1 L (1 qt) each, taken from near the top andbottom by means of a metal or glass container with removablestopper or top. This device, attached to a suitable pole, shall belowered to the desired depth, when the stopper o
12、r top shall be1These methods are under the jurisdiction of ASTM Committee D20 on Plasticsand are the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials (Section D20.15.11 on Plasticizers).Current edition approved Aug. 1, 2008. Published September 2008. Originallyapproved in 1949.
13、 Last previous edition approved in 2001 as D 1045 - 95(2001).2For referenced ASTM standards, visit 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.
14、1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.removed and the container allowed to fill. A bomb samplerattached to a chain is convenient to use; adjust the opening s
15、othat the bomb will fill on the way down.6.3 From Barrels and DrumsAt least 5 % of the packagesin any shipment shall be represented in the sample. It ispermissible for the purchaser to increase the percentage ofpackages to be sampled at his discretion; in the case ofplasticizers that are purchased i
16、n small quantity, it is permis-sible to sample and analyze each package, if desired. A portionshall be withdrawn from near the center of each packagesampled by means of a “thief” or other sampling device andcomposited. The composite sample thus obtained shall be notless than 1 L (1 qt) and shall con
17、sist of equal portions of notless than 250 mL (12 pt) from each package sampled.7. Purity of Reagents7.1 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 on Analytica
18、l Reagents of the American Chemical Society,where such specifications are available.37.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD 1193.ACID NUMBER8. Thermometers8.1 All temperature measurements shall be made withASTM thermo
19、meters of suitable range, accurate to within0.1C and conforming to the requirements prescribed inSpecification E1.9. Reagents9.1 AlcoholDenatured alcohol, Formula No. 3A of the U.S. Bureau of Alcohol, Tobacco, and Firearms.9.2 Alkali, Standard Solution ( 0.01 N)Prepare and stan-dardize a 0.01 N aque
20、ous solution of sodium hydroxide(NaOH) or a 0.01 N alcoholic solution of potassium hydroxide(KOH).9.3 Alkali, Standard Solution (0.1 N)Prepare and stan-dardize a 0.1 N aqueous solution of sodium hydroxide (NaOH)or a 0.1 N alcoholic solution of potassium hydroxide (KOH).9.4 Acetone.9.5 Bromthymol Blu
21、e Indicator Solution.10. Procedure10.1 Weigh 25 g of the sample into a 125-mL Erlenmeyerflask and dissolve in 50 mL of alcohol. If the sample is notcompletely soluble in alcohol, use 50 mL of a mixture of equalparts of alcohol and acetone. With certain samples it willpotentially be necessary first t
22、o add 25 mL of acetone, warm toeffect solution, and then add 25 mL of alcohol.10.2 Add a few drops of bromthymol blue indicator solutionand titrate with 0.01 N NaOH or KOH solution. If the titrationexceeds 10 mL, repeat the determination using 0.1 N NaOH orKOH solution.10.3 BlankMake a blank titrati
23、on on 50 mL of the solventused to dissolve the sample.11. Calculation11.1 Calculate the acid number, expressed as milligrams ofKOH per gram of sample, as follows:Acid number 5 A 2 B!N3 56.1/C (1)where:A = NaOH or KOH solution required for titration of thesample, mL,B = NaOH or KOH solution required
24、for titration of theblank, mL,N = normality of the NaOH or KOH solution, andC = sample used, g.11.2 Conversion FactorsIn the case of esters, it is accept-able to express the results as a percentage by weight of theappropriate acid, by using the proper factor in the equation in11.1 or by using the co
25、nversion factors below:Acid Number Mg KOH/g! 5 Milliequivalent Meq!/100 g 3 0.561% Acid 5 Meq/100 g 3 milliequivalent weight of acidTABLE Milliequivalent Weight of Various AcidsMaleic = 0.058Acetic = 0.060Phthalic = 0.083Hydrochloric = 0.037Phosphoric = 0.049Adipic = 0.07312. Selection of Test Metho
26、d12.1 Ester content shall be determined using either the gaschromatographic method (Test Method D 3465) or the titrimet-ric method (Section 13).13. Titrimetric Method13.1 Reagents13.1.1 Bromthymol Blue Indicator Solution.13.1.2 Hydrochloric Acid, Standard (0.5 N) Prepare andstandardize a 0.5 N aqueo
27、us solution of hydrochloric acid(HCI).13.1.3 Potassium Hydroxide, Standard Solution (0.5 N)Prepare and standardize a 0.5 N alcoholic solution of potassiumhydroxide (KOH).13.2 Procedure13.2.1 Weigh accurately about2gofthesample into a250-mL Erlenmeyer flask with ground-glass joint. By means ofa const
28、ant delivery pipet or buret, add 50 mL of 0.5 N KOHsolution. Connect to a water-cooled condenser with ground-glass joint and reflux for a period of 1 to 4 h, depending on theester being tested, or until saponification is complete.13.2.2 After the apparatus has cooled, wash down thecondenser with wat
29、er and disconnect. Add a few drops of3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U
30、.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D1045082bromthymol blue indicator solution to contents of the flask andtitrate with 0.5 N HCl.13.2.3 BlankRun a blank, containing 50 mL of the 0.5 NKOH solution, along with the sa
31、mple.13.3 Calculation13.3.1 Calculate the ester content, expressed in milligramsof KOH per gram of sample, as follows:Ester content 5 D 2 E!N 3 56.1/G 2 F (2)where:D = HCl required for titration of the blank, mL,E = HCl required for titration of the sample, mL,F = correction for acidity of sample (S
32、ection 11),N = normality of the HCl, andG = sample used, g.13.3.2 If desired, it is acceptable to express the results as apercentage of the appropriate ester by weight, by using theproper factor in the equation in 13.3.1.SPECIFIC GRAVITY14. Selection of Test Method14.1 Specific gravity of low viscos
33、ity plasticizers shall bedetermined using a hydrometer (Test Method D 287), Westphalbalance, pycnometer (Section 15) or Digital Density Meter(Test Method D 4052). Extremely viscous plasticizers shall betested by Test Methods D 792 or Test Method D70.15. Procedure Using Pycnometer15.1 Determine the w
34、eight capacity of the pycnometer withwater at 23 6 1C. Fill this standardized pycnometer with aportion of the sample that has been cooled to approximately20C. Insert the thermometer or capillary tube, taking care toavoid introduction of air bubbles. Set the pycnometer in aconstant-temperature water
35、bath maintained at 23 6 1C (73.46 1.8F) for a period of at least 30 min. Remove the droplet ofsample from the overflow capillary and cover with the glasscap. Clean the outside of the pycnometer and weigh.15.2 Calculation15.2.1 Calculate the specific gravity as follows:Specific gravity at 23/23C 5 A/
36、B (3)where:A = grams of sample used, andB = water capacity of pycnometer in grams.COLOR16. Selection of Test Method16.1 The color of plasticizers shall be determined usingeither Test Methods D 5386 or D 1209 for color less than 200APHA and Test Method D 1544 for color higher than 200APHA.REFRACTIVE
37、INDEX17. Procedure17.1 The refractive index of plasticizers shall be determinedusing Test Method D 1218.WATER CONTENT18. Procedure18.1 The water content shall be measured using TestMethod E 203.19. Precision and Bias19.1 Precision and bias statements are an integral part ofreferenced test procedures
38、 used in this test method. Thesestatements are to be considered applicable to test resultsobtained by use of this test method.19.2 Attempts to develop precision and bias statements forAcid Number, Ester Content-Titrimetric, Specific Gravity-Pycnometer, Color, and Refractive Index have not been suc-c
39、essful. For this reason, data on precision and bias cannot begiven. If anyone wishes to participate in the development ofprecision and bias data, contact the ASTM headquarters.20. Keywords20.1 plasticizer; plasticizer acid number; plasticizer color;plasticizer ester content; plasticizer refractive i
40、ndex; sampling;test methodsSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D 1045 - 95(2001) that may impact the use of this standard. (August 1, 2008)(1) Removed permissive language.(2) Added D 1209, D 1218, D 1544, D 5386 to the
41、 ReferencedDocuments section.(3) Added conversion factors for acid number in 11.(4) Added D 5386, D 1209, and D 1544 for color measure-ment and eliminated the Color Measurement procedure fromthe standard.(5) Replaced D 1807 with D 1218 and eliminated the Refrac-tive Index procedure from the standard
42、.(6) Renumbered sections as appropriate.D1045083ASTM 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,
43、 and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for rev
44、ision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you
45、 shouldmake your views known to the 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 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D1045084
