ASTM D233-2012 Standard Test Methods of Sampling and Testing Turpentine《松脂的取样和测试的标准试验方法》.pdf

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1、Designation: D233 08 D233 12Standard Test Methods ofSampling and Testing Turpentine1This standard is issued under the fixed designation D233; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in pa

2、rentheses 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 Department of Defense.1. Scope1.1 These test methods cover procedures for sampling and testing turpe

3、ntine, as defined by the Code of Federal Regulations andTerminology D804. These test methods are also used for the sampling and testing of pinenes, the major components of mostturpentines.1.2 These test methods primarily measure the physical rather than the chemical properties of turpentines and pin

4、enes. Asturpentines and pinenes are currently used chiefly as chemical raw materials for the production of resins and synthetic organicchemicals, chemical composition is also very important. Consequently, testing the chemical composition of turpentines and pinenesby gas chromatography has displaced

5、these test methods to a large extent. (See for example Test Methods D6387.)1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not considered standard.1.4 This

6、 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 establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.

7、1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products at Atmospheric PressureD270 Methods of Sampling Petroleum and Petroleum Products (Withdrawn 1984)3D804 Terminology Relating to Pine Chemicals, Including Tall Oil and Related ProductsD1193 Specification for Reagent WaterD1209 Te

8、st Method for Color of Clear Liquids (Platinum-Cobalt Scale)D6166 Test Method for Color of Naval StoresPine Chemicals and Related Products (Instrumental Determination of GardnerColor)D6387 Test Methods for Composition of Turpentine and Related Terpene Products by Capillary Gas ChromatographyE2251 Sp

9、ecification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids2.2 Other Document:Code of Federal Regulations, Title 7, Part 160, “Regulations and Standards for Naval Stores,” 199943. Significance and Use3.1 The test procedures described in this standard were developed when the c

10、hief use for turpentine was as a solvent. Currentlyhowever, the chief use for turpentine (and pinenes) is as raw materials for the production of resins and synthetic organic chemicals.Thus the chemical composition of turpentines and pinenes is extremely important and tests, in addition to the ones d

11、escribed inthese test methods, are required in order to fully characterize turpentines and pinenes. The most widely used technique fordetermining the chemical composition of turpentines (and pinenes) is gas chromatography (see Test Methods D6387).1 These test methods are under the jurisdiction of AS

12、TM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.Current edition approved June 1, 2008Nov. 1, 2012. Published June 2008December 2012 . Originally approved in 1926. Last previou

13、s edition approved in 20022008 asD233 02.D233 08. DOI: 10.1520/D0233-08.10.1520/D0233-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Su

14、mmary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.4 Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.This document is n

15、ot 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 appropria

16、te. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Purity of Reagents4.1 Reagent grade chemicals shall be used in

17、all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.5 Other grades may be used, provided it is first ascertained that the reagent is

18、 of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to SpecificationD1193.SAMPLING5. Sampling5.1 The method of sampling specified in 5.2 or 5.3 shall

19、 be used, according to the special conditions that apply.5.2 From Loaded Tank Car or Other Large VesselThe composite sample taken shall be not less than 12 gal (1.9 L) and shouldconsist of small samples of not more than 1 qt (0.9 L) each, taken from near the top and bottom by means of a metal or gla

20、sscontainer with removable stopper or top.6 This device, attached to a suitable pole, shall be lowered to the desired depth, the stopperor top removed, and the container allowed to fill. If a sample from close to the bottom of a tank shows a decided difference in coloror appearance from samples take

21、n at other depths, an extra bottom sample shall be taken and examined separately from thecomposite sample. In such case, the composite sample shall not include any portion of such bottom sampling.5.3 From Barrels and DrumsAt least 5 % of the packages in any shipment shall be represented in the sampl

22、e. The purchasermay increase the percentage of packages to be sampled at his direction, and it is recommended that every package be sampled inthe case of expensive terpene hydrocarbons that are bought in small quantity. A portion shall be withdrawn from about the centerof each package sampled by mea

23、ns of a “thief” or other sampling device. The composite sample thus obtained shall be not lessthan 1 qt (0.9 L) and shall consist of equal portions of not less than 12 pt (0.24 L) from each package sampled.DETECTION AND REMOVAL OF SEPARATED WATER6. Procedure6.1 Draw a portion by means of a glass or

24、metal container with a removable stopper or top,6 or with a “thief,” from the lowestpart of the container, or by opening the bottom valve of the perfectly level tank car. If water is found in this sample, draw it allout, record the quantity, and deduct it from the total volume of liquid delivered.AP

25、PEARANCE7. Procedure7.1 Examine a portion of the sample after agitation to determine whether its appearance conforms to specifications.ODOR8. Procedure8.1 Compare the odor of the sample with an agreed-upon water-free reference sample kept in the dark in a completely filled,well-stoppered bottle. In

26、the absence of such a sample, compare with samples of known purity similarly preserved.SPECIFIC GRAVITY9. Procedure9.1 Determine the specific gravity at 15.6/15.6C by any convenient method having a precision of 0.0005. Determinations madeat any other temperature using apparatus standardized at 15.6C

27、 shall be corrected by adding to or subtracting from the observedreading 0.00082 for each degree Celsius that the temperature of the liquid is above or below 15.6C. If the determination is madewith apparatus calibrated for a temperature other than 15.6C, the observed reading shall first be calculate

28、d to density at thetemperature of observation, then converted to density at 15.6C by applying the above factor, and finally converted to specificgravity by dividing the calculated density by 0.999 (the density of water at 15.6C).5 Reagent Chemicals, American Chemical Society Specifications, American

29、 Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC

30、), Rockville, MD.6 Detailed description of equipment suitable for such sampling is given in Methods D270.D233 122REFRACTIVE INDEX10. Procedure10.1 Determine the refractive index with an accurate instrument, at 20C if possible. If determined at any other temperature,correct the reading obtained to 20

31、C by adding or subtracting 0.00045 for each degree Celsius that the temperature at which thedetermination was made is, respectively, above or below 20C.DISTILLATION11. Apparatus11.1 Use the type of distillation apparatus described in Test Method D86, with the following exceptions:11.1.1 For testing

32、turpentine or pinene use an ASTM Turpentine Distillation Thermometer, 3-in. (76-mm) partial immersion,having a range from 147 to 182C, and conforming to the requirements for Thermometer 27C as prescribed in Specification E2251,or an ASTM Solvents Distillation Thermometer, 3.94-in. (100-mm) partial i

33、mmersion, having a range from 95 to 255C, andconforming to the requirements for Thermometer 42C as prescribed in Specification E2251.11.1.2 Ice is not necessary in the condenser bath. It is permissible to use a glass Liebig condenser 22 in. (560 mm) in lengthwith 16 in. (410 mm) in contact with the

34、cooling water and filled with an adapter to extend 1 in. (51 mm) into the receivinggraduate.12. Procedure12.1 Using the receiving graduate, transfer exactly 100 mL of the sample directly into the flask, allowing none to run into theside tube. If the sample contains dissolved or suspended water it is

35、 advisable to add a few small pieces of pumice or broken glassto promote smooth distillation. Insert the thermometer, so that the top of the bulb (or the top of the contraction chamber if theSolvents Distillation Thermometer is used) is level with the bottom of the side tube. Connect the side tube t

36、o the condenser, withthe bottom of the flask resting securely in the opening of the ceramic or other heat resistant board. Apply heat cautiously, andregulate it so that the first drop of condensate falls from the condenser in not less than 5 nor more than 10 min. Record as the initialboiling point t

37、he thermometer reading when the first drop falls from the end of the condenser, correcting for barometric pressureas described in Section 13. When the distillation begins, regulate the heat so that the distillate is collected at a rate of not less than4 nor more than 5 mL/min (approximately 2 drops/

38、s). Discontinue the distillation when the temperature reaches that specified forthe minimum percentage requirement (usually 170C for turpentine), after correcting for barometric pressure. Allow the condenserto drain and read the percentage distilled.12.2 The percentages distilled below successive se

39、lected temperatures and the temperature at which each successive 10 mLdistills may also be determined, if desired, making the necessary correction of the temperature for barometric pressure.13. Barometric Correction13.1 The distilling temperature of turpentine (and pinene) is affected by 0.052C for

40、each millimetre (1.32C for each inch)variation of the atmospheric pressure. Therefore, the distillation temperatures observed or specified shall be corrected to permitdistillation to be conducted as though the barometer reading, corrected to 0C, were exactly 760 mm (30 in.).13.2 When about to begin

41、the distillation, observe and record the barometric pressure and the temperature of the barometer. (Notemperature correction is necessary for aneroid-type barometers.) From Table 1 determine the proper temperature correctioncorresponding to these atmospheric conditions, interpolating to the nearest

42、0.1C. If the barometric pressure, corrected to 0C, isbelow 760 mm, the temperature correction must be added to the initial boiling point and subtracted from the minimum percentagerequirement temperature; if above 760 mm, the correction must be subtracted from the initial boiling point and added to t

43、heminimum percentage requirement temperature.NOTE 1ExampleSuppose the observed barometric pressure is 748 mm at 32C, and the initial boiling point is observed to be 155.2C. From Table1 the temperature correction is seen to be 0.8C. Therefore, the corrected boiling point is 155.2 + 0.8 = 156C. Furthe

44、rmore, the temperature observationpoint at the minimum percentage requirement (170C at 760 mm) must be altered to the same extent. Since the turpentine is distilling 0.8C below whatit would at normal pressure, distillation must be discontinued at 169.2C to determine the percentage distilling below 1

45、70C at 760 mm pressure.14. Color14.1 Compare the color of the sample in any suitable or designated apparatus with the accepted or specific color standard.Accepted color standards are the Gardner color scale found in Test Method D6166 and the platinum-cobalt scale found in TestMethod D1209.15. Precis

46、ion and Bias15.1 The procedures described in these test methods were developed many years ago and were once widely used for thesampling and testing of turpentines and pinenes. Currently they are not widely used and it is not considered practical to redeterminethe precision and bias of the individual

47、 methods at this time.D233 12316. Keywords16.1 pinene; samplingsampling; turpentineASTM 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

48、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 technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your

49、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 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 the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,Uni