ASTM D233-2002 Standard Test Methods of Sampling and Testing Turpentine《松脂的抽样和测试的标准试验方法》.pdf

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1、Designation: D 233 02Standard Test Methods ofSampling and Testing Turpentine1This standard is issued under the fixed designation D 233; 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 parenthe

2、ses 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 These test methods cover procedures for sampling andtesting turpentine,

3、 as defined by the Code of Federal Regula-tions and Terminology D 804. These test methods are also usedfor the sampling and testing of pinenes, the major componentsof most turpentines.1.2 These test methods primarily measure the physicalrather than the chemical properties of turpentines and pinenes.

4、As turpentines and pinenes are currently used chiefly aschemical raw materials for the production of resins andsynthetic organic chemicals, chemical composition is also veryimportant. Consequently, testing the chemical composition ofturpentines and pinenes by gas chromatography has displacedthese te

5、st methods to a large extent. (See for example TestMethods D 6387.)1.3 The values stated in inch-pound units are to be regardedas the standard. The values given in parentheses are forinformation only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its

6、 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.2. Referenced Documents2.1 ASTM Standards:D86 Test Method for Distillation of Petroleum Products atAtmospheric Pres

7、sure2D 270 Methods of Sampling Petroleum and PetroleumProducts3D 804 Terminology Relating to Naval Stores, Including TallOil and Related Products4D 1193 Specification for Reagent Water5D 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)6D 6166 Test Method for Color of Naval Stores

8、and RelatedProducts (Instrumental Determination of Gardner Color)4D 6387 Test Methods for Composition of Turpentine andRelated Terpene Products by Capillary Gas Chromatogra-phy4E1 Specification for ASTM Thermometers72.2 Other Document:Code of Federal Regulations, Title 7, Part 160, “Regulationsand S

9、tandards for Naval Stores,” 199983. Significance and Use3.1 The test procedures described in this standard weredeveloped when the chief use for turpentine was as a solvent.Currently however, the chief use for turpentine (and pinenes) isas raw materials for the production of resins and syntheticorgan

10、ic chemicals. Thus the chemical composition of turpen-tines and pinenes is extremely important and tests, in additionto the ones described in these test methods, are required inorder to fully characterize turpentines and pinenes. The mostwidely used technique for determining the chemical composi-tio

11、n of turpentines (and pinenes) is gas chromatography (seeTest Methods D 6387).4. Purity of Reagents4.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the Amer

12、ican Chemical Society, where such1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.34 on Naval Stores.Current edition approved May 10, 2002. Published July 2002 Originall

13、ypublished as D 233 26. Last previous edition D 233 97.2Annual Book of ASTM Standards, Vol 05.01.3Discontinued; see 1983 Annual Book of ASTM Standards , Vol 05.01.4Annual Book of ASTM Standards, Vol 06.03.5Annual Book of ASTM Standards, Vol 11.01.6Annual Book of ASTM Standards, Vol 06.04.7Annual Boo

14、k of ASTM Standards, Vol 14.03.8Available from U.S. Government Printing Office, Superintendent of Docu-ments, 732 North Capitol St., NW, Mail Stop: SDE, Washington, DC 204011Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.specificatio

15、ns are available.9Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to

16、 SpecificationD 1193.SAMPLING5. Sampling5.1 The method of sampling specified in 5.2 or 5.3 shall beused, according to the special conditions that apply.5.2 From Loaded Tank Car or Other Large VesselThecomposite sample taken shall be not less than12 gal (1.9 L) andshould consist of small samples of n

17、ot more than 1 qt (0.9 L)each, taken from near the top and bottom by means of a metalor glass container with removable stopper or top.10Thisdevice, attached to a suitable pole, shall be lowered to thedesired depth, the stopper or top removed, and the containerallowed to fill. If a sample from close

18、to the bottom of a tankshows a decided difference in color or appearance fromsamples taken at other depths, an extra bottom sample shall betaken and examined separately from the composite sample. Insuch case, the composite sample shall not include any portionof such bottom sampling.5.3 From Barrels

19、and DrumsAt least 5 % of the packagesin any shipment shall be represented in the sample. Thepurchaser may increase the percentage of packages to besampled at his direction, and it is recommended that everypackage be sampled in the case of expensive terpene hydro-carbons that are bought in small quan

20、tity. A portion shall bewithdrawn from about the center of each package sampled bymeans of a “thief” or other sampling device. The compositesample thus obtained shall be not less than 1 qt (0.9 L) andshall consist of equal portions of not less than12 pt (0.24 L)from each package sampled.DETECTION AN

21、D REMOVAL OF SEPARATEDWATER6. Procedure6.1 Draw a portion by means of a glass or metal containerwith a removable stopper or top,10or with a “thief,” from thelowest part of the container, or by opening the bottom valve ofthe perfectly level tank car. If water is found in this sample,draw it all out,

22、record the quantity, and deduct it from the totalvolume of liquid delivered.APPEARANCE7. Procedure7.1 Examine a portion of the sample after agitation todetermine whether its appearance conforms to specifications.ODOR8. Procedure8.1 Compare the odor of the sample with an agreed-uponwater-free referen

23、ce sample kept in the dark in a completelyfilled, well-stoppered bottle. In 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 anyconvenient method having a precision of 0.0005. Determi

24、na-tions made at any other temperature using apparatus standard-ized at 15.6C shall be corrected by adding to or subtractingfrom the observed reading 0.00082 for each degree Celsius thatthe temperature of the liquid is above or below 15.6C. If thedetermination is made with apparatus calibrated for a

25、 tempera-ture other than 15.6C, the observed reading shall first becalculated to density at the temperature of observation, thenconverted to density at 15.6C by applying the above factor,and finally converted to specific gravity by dividing thecalculated density by 0.999 (the density of water at 15.

26、6C).REFRACTIVE INDEX10. Procedure10.1 Determine the refractive index with an accurate instru-ment, at 20C if possible. If determined at any other tempera-ture, correct the reading obtained to 20C by adding orsubtracting 0.00045 for each degree Celsius that the tempera-ture at which the determination

27、 was made is, respectively,above or below 20C.DISTILLATION11. Apparatus11.1 Use the type of distillation apparatus described in TestMethod D86, with the following exceptions:11.1.1 For testing turpentine or pinene use an ASTM Tur-pentine Distillation Thermometer, 3-in. (76-mm) partial im-mersion, ha

28、ving a range from 147 to 182C, and conforming tothe requirements for Thermometer 27C as prescribed in Speci-fication E1, or an ASTM Solvents Distillation Thermometer,3.94-in. (100-mm) partial immersion, having a range from 95to 255C, and conforming to the requirements for Thermom-eter 42C as prescri

29、bed in Specification E1.11.1.2 Ice is not necessary in the condenser bath. It ispermissible to use a glass Liebig condenser 22 in. (560 mm) inlength with 16 in. (410 mm) in contact with the cooling waterand filled with an adapter to extend 1 in. (51 mm) into thereceiving graduate.9Reagent Chemicals,

30、 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.K., and the United States Pharmacopeiaand National Form

31、ulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.10Detailed description of equipment suitable for such sampling is given inMethods D 270.D23302212. Procedure12.1 Using the receiving graduate, transfer exactly 100 mLof the sample directly into the flask, allowing none to run intothe si

32、de tube. If the sample contains dissolved or suspendedwater it is advisable to add a few small pieces of pumice orbroken glass to promote smooth distillation. Insert the ther-mometer, so that the top of the mercury bulb (or the top of thecontraction chamber if the Solvents Distillation Thermometeris

33、 used) is level with the bottom of the side tube. Connect theside tube to the condenser, with the bottom of the flask restingsecurely in the opening of the ceramic or other heat resistantboard. Apply heat cautiously, and regulate it so that the firstdrop of condensate falls from the condenser in not

34、 less than 5nor more than 10 min. Record as the initial boiling point thethermometer reading when the first drop falls from the end ofthe condenser, correcting for barometric pressure as describedin Section 13. When the distillation begins, regulate the heat sothat the distillate is collected at a r

35、ate of not less than 4 normore than 5 mL/min (approximately 2 drops/s). Discontinuethe distillation when the temperature reaches that specified forthe minimum percentage requirement (usually 170C forturpentine), after correcting for barometric pressure. Allow thecondenser to drain and read the perce

36、ntage distilled.12.2 The percentages distilled below successive selectedtemperatures and the temperature at which each successive 10mL distills may also be determined, if desired, making thenecessary correction of the temperature for barometric pres-sure.13. Barometric Correction13.1 The distilling

37、temperature of turpentine (and pinene) isaffected by 0.052C for each millimetre (1.32C for each inch)variation of the atmospheric pressure. Therefore, the distilla-tion temperatures observed or specified shall be corrected topermit distillation to be conducted as though the barometerreading, correct

38、ed to 0C, were exactly 760 mm (30 in.).13.2 When about to begin the distillation, observe andrecord the barometric pressure and the temperature of thebarometer. (No temperature correction is necessary foraneroid-type barometers.) From Table 1 determine the propertemperature correction corresponding

39、to these atmosphericconditions, interpolating to the nearest 0.1C. If the barometricpressure, corrected to 0C, is below 760 mm, the temperaturecorrection must be added to the initial boiling point andsubtracted from the minimum percentage requirement tempera-ture; if above 760 mm, the correction mus

40、t be subtracted fromthe initial boiling point and added to the minimum percentagerequirement temperature.NOTE 1ExampleSuppose the observed barometric pressure is 748mm at 32C, and the initial boiling point is observed to be 155.2C. FromTable 1 the temperature correction is seen to be 0.8C. Therefore

41、, thecorrected boiling point is 155.2 + 0.8 = 156C. Furthermore, the tempera-ture observation point at the minimum percentage requirement (170C at760 mm) must be altered to the same extent. Since the turpentine isdistilling 0.8C below what it would at normal pressure, distillation mustbe discontinue

42、d at 169.2C to determine the percentage distilling below170C at 760 mm pressure.14. Color14.1 Compare the color of the sample in any suitable ordesignated apparatus with the accepted or specific colorstandard. Accepted color standards are the Gardner color scalefound in Test Method D 6166 and the pl

43、atinum-cobalt scalefound in Test Method D 1209.15. Precision and Bias15.1 The procedures described in these test methods weredeveloped many years ago and were once widely used for thesampling and testing of turpentines and pinenes. Currently theyare not widely used and it is not considered practical

44、 toredetermine the precision and bias of the individual methods atthis time.16. Keywords16.1 pinene; sampling; turpentineTABLE 1 Temperature Corrections for Barometric PressureAObservedBarometricPressure,mmAneroidBarometerMercurial BarometerTemperature of Barometer20C 25C 30C 35C780 1.04 0.91 0.88 0

45、.84 0.81770 0.52 0.39 0.36 0.32 0.29760 0.00 + 0.13 + 0.16 + 0.19 + 0.22750 + 0.52 + 0.65 + 0.68 + 0.71 + 0.74740 + 1.04 + 1.17 + 1.20 + 1.23 + 1.26730 + 1.56 + 1.68 + 1.71 + 1.75 + 1.78720 + 2.08 + 2.20 + 2.23 + 2.26 + 2.29710 + 2.62 + 2.72 + 2.75 + 2.78 + 2.81700 + 3.16 + 3.24 + 3.27 + 3.30 + 3.33

46、AThese corrections are calculated as follows: The observed barometric pres-sure is first corrected to what it would be at 0C, by means of the table in CircularF, Instrument Division, U. S. Weather Bureau. The corrected barometric pressureis then subtracted from 760 mm (or vice versa) and the differe

47、nce multiplied by0.052C to give the temperature correction shown in this table. The correctionfactor, C, of 0.052C was calculated using the Sydney-Young equation:C = 0.00012(760 P)(273 + T)where:P = observed pressure, corrected to 0C, in millimetres, andT = median boiling temperature for turpentine,

48、 160C.D233023ASTM 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 suc

49、h 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 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