1、Designation: D1045 14Standard Test Methods forSampling and Testing Plasticizers Used in Plastics1This standard is issued under the fixed designation D1045; 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, spec
3、ific 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 use
4、. 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 known ISO equivalent to this standard.2. Reference
5、d Documents2.1 ASTM Standards:2D70 Test Method for Density of Semi-Solid BituminousMaterials (Pycnometer Method)D287 Test Method for API Gravity of Crude Petroleum andPetroleum Products (Hydrometer Method)D792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Plastics by Displacem
6、entD883 Terminology Relating to PlasticsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1218 Test Method for Refractive Index and RefractiveDispersion of Hydrocarbon LiquidsD1544 Test Method for Color of Transparent Liquids (Gard-ner Color Sc
7、ale)D1600 Terminology forAbbreviated Terms Relating to Plas-ticsD3465 Test Method for Purity of Monomeric Plasticizers byGas ChromatographyD4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterD5386 Test Method for Color of Liquids Using TristimulusColori
8、metryE1 Specification for ASTM Liquid-in-Glass ThermometersE203 Test Method for Water Using Volumetric Karl FischerTitrationE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids3. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nology D883 an
9、d Terminology D1600, unless otherwise indi-cated.4. Significance and Use4.1 These test methods shall 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 chem
10、icals used in this test method are hazardous.Accepted laboratory safety procedures must be followed. 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 Lo
11、aded Tank Car or Other Large VesselThecomposite sample taken shall be not less than 2 L (12 gal). It 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.
12、 This device, attached to a suitable pole, shall belowered to the desired depth, when the stopper or top shall beremoved and the container allowed to fill. A bomb samplerattached to a chain is convenient to use; adjust the opening sothat the bomb will fill on the way down.6.3 From Barrels and DrumsA
13、t least 5 % of the packagesin any shipment shall be represented in the sample. It is1These methods are under the jurisdiction of ASTM Committee D20 on Plasticsand are the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials (Section D20.15.07 on Vinyl Chloride Polymers).Current edi
14、tion approved March 1, 2014. Published March 2014. Originallyapproved in 1949. Last previous edition approved in 2008 as D1045 - 08. DOI:10.1520/D1045-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS
15、tandards volume information, refer to the standards Document Summary page onthe ASTM website.*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 States1permissible for the purchase
16、r to increase the percentage ofpackages to be sampled at his discretion; in the case ofplasticizers that are purchased in 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” o
17、r other sampling device andcomposited. The composite sample thus obtained shall be notless than 1 L (1 qt) and shall consist 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
18、 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.37.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water co
19、nforming to SpecificationD1193.8. Thermometers8.1 All temperature measurements shall be made withASTM thermometers of suitable range, accurate to within0.1C and conforming to the requirements prescribed inSpecification E1. Thermometric devices such as RTDs,thermistors, thermocouples, and liquid-in-g
20、lass thermometers(as in Specification E2251), with appropriate temperaturerange and equal or better accuracy as the selected thermometer,are acceptable for use.9. Acid Number9.1 Reagents:9.1.1 AlcoholDenatured alcohol, Formula No. 3A of theU. S. Bureau of Alcohol, Tobacco, and Firearms.9.1.2 Alkali,
21、 Standard Solution (0.01 N)Prepare and stan-dardize a 0.01 N aqueous solution of sodium hydroxide(NaOH) or a 0.01 N alcoholic solution of potassium hydroxide(KOH).9.1.3 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 s
22、olution of potassium hydroxide (KOH).9.1.4 Acetone.9.1.5 Bromthymol Blue 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 an
23、d acetone. With certain samples it willpotentially be necessary first to 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 deter
24、mination using 0.1 N NaOH orKOH solution.10.3 BlankMake a blank titration 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!N 356.1#/C (1)where:A = NaOH or KOH solution re
25、quired for titration of thesample, mL,B = NaOH or KOH solution required 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 ac
26、id, by using the proper factor in the equation in11.1 or by using the conversion factors below:Acid Number Mg KOH/g! 5 Milliequivalent Meq!/100 g 30.561% Acid 5 Meq/100 g 3milliequivalent weight of acidTABLE Milliequivalent Weight of Various AcidsMaleic = 0.058Acetic = 0.060Phthalic = 0.083Hydrochlo
27、ric = 0.037Phosphoric = 0.049Adipic = 0.07312. Ester Content12.1 Selection of Test Method:12.1.1 Ester content shall be determined using either the gaschromatographic method (Test Method D3465) or the titrimet-ric method (Section 13).13. Titrimetric Method13.1 Reagents:13.1.1 Bromthymol Blue Indicat
28、or Solution.13.1.2 Hydrochloric Acid, Standard (0.5N)Prepare and stan-dardize a 0.5 N aqueous 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 Procedure:13.2.1 Weigh accurately
29、 about2gofthesample into a250-mL Erlenmeyer flask with ground-glass joint. By means ofa constant 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 sapo
30、nification is complete.13.2.2 After the apparatus has cooled, wash down thecondenser with water and disconnect. Add a few drops ofbromthymol blue indicator solution to contents of the flask andtitrate with 0.5 N HCl.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Socie
31、ty, 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.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.
32、D1045 14213.2.3 BlankRun a blank, containing 50 mL of the 0.5 NKOH solution, along with the sample.13.3 Calculation:13.3.1 Calculate the ester content, expressed in milligramsof KOH per gram of sample, as follows:Ester content 5 D 2 E!N 356.1#/G 2 F (2)where:D = HCl required for titration of the bla
33、nk, mL,E = HCl required for titration of the sample, mL,F = correction for acidity of sample (Section 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 equ
34、ation in 13.3.1.14. Specific Gravity14.1 Selection of Test Method:14.1.1 Specific gravity of low viscosity plasticizers shall bedetermined using a hydrometer (Test Method D287), Westphalbalance, pycnometer (Section 15) or Digital Density Meter(Test Method D4052). Extremely viscous plasticizers shall
35、 betested by Test Methods D792 or Test Method D70.15. Procedure Using Pycnometer15.1 Determine the weight 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,
36、 taking care toavoid introduction of air bubbles. Set the pycnometer in aconstant-temperature water 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 we
37、igh.15.2 Calculation:15.2.1 Calculate the specific gravity as follows:Specific gravity at 23/23C 5 A/B (3)where:A = grams of sample used, andB = water capacity of pycnometer in grams.16. Color16.1 Selection of Test Method:16.1.1 The color of plasticizers shall be determined usingeither Test Methods
38、D5386 or D1209 for color less than 200APHA and Test Method D1544 for color higher than 200APHA.17. Refractive Index17.1 Procedure:17.1.1 The refractive index of plasticizers shall be deter-mined using Test Method D1218.18. Water Content18.1 Procedure:18.1.1 The water content shall be measured using
39、TestMethod E203.19. Report19.1 Report the results for acid number, ester content,specific gravity, color, refractive index, and water content in atable along with the identification of the plasticizer tested andthe test methods used.20. Precision and Bias20.1 Precision and bias statements are an int
40、egral part ofreferenced test procedures used in this test method. Thesestatements are to be considered applicable to test resultsobtained by use of this test method.20.2 Attempts to develop precision and bias statements forAcid Number, Ester Content-Titrimetric, Specific Gravity-Pycnometer, Color, a
41、nd Refractive Index have not been suc-cessful. 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.21. Keywords21.1 plasticizer; plasticizer acid number; plasticizer color;plasticizer
42、ester content; plasticizer refractive index; sampling;test methodsSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D1045 - 08)that may impact the use of this standard. (March 1, 2014)(1) Updated ISO equivalency statement in Note 1
43、.(2) Updated Subcommittee information.(3) Updated thermometers to include Specification E2251,aswell as Section 8.(4) Moved Section 8 to precede “Acid Number.”(5) Assigned section numbers to tests: Acid Number, EsterContent, etc.(6) Added a Report section (Section 19).D1045 143ASTM International tak
44、es 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 such rights, are entirely their own re
45、sponsibility.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 revision of this standard or for additional standardsand should be addres
46、sed 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 shouldmake your views known to the ASTM Committee on Standards, at th
47、e 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1045 144
