ASTM D233-2008 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 08Standard 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 () 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.A

4、s 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 tes

5、t methods to a large extent. (See for example TestMethods D 6387.)1.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4 This standard d

6、oes not purport to address all of thesafety concerns, if any, associated with its 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 St

7、andards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 270 Methods of Sampling Petroleum and PetroleumProducts3D 804 Terminology Relating to Naval Stores, Including TallOil and Related ProductsD 1193 Specification for Reagent WaterD 1209 Test Method for Color of Clea

8、r Liquids (Platinum-Cobalt Scale)D 6166 Test Method for Color of Naval Stores and RelatedProducts (Instrumental Determination of Gardner Color)D 6387 Test Methods for Composition of Turpentine andRelated Terpene Products by Capillary Gas Chromatogra-phyE 2251 Specification for Liquid-in-Glass ASTM T

9、hermom-eters with Low-Hazard Precision Liquids2.2 Other Document:Code of Federal Regulations, Title 7, Part 160, “Regulationsand Standards for Naval Stores,” 199943. Significance and Use3.1 The test procedures described in this standard weredeveloped when the chief use for turpentine was as a solven

10、t.Currently however, the chief use for turpentine (and pinenes) isas raw materials for the production of resins and syntheticorganic 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 requ

11、ired inorder to fully characterize turpentines and pinenes. The mostwidely used technique for determining the chemical composi-tion 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

12、 indicated, it is intended that all reagents shall1These 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 June 1, 2008. Published Ju

13、ne 2008 Originally approvedin 1926. Last previous edition approved in 2002 as D 233 02.2For 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 Summar

14、y page onthe ASTM website.3Withdrawn.4Available 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,

15、 United States.conform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.5Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening

16、 the accuracy ofthe determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to 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

17、 Loaded Tank Car or Other Large VesselThecomposite sample taken shall be not less than12 gal (1.9 L) andshould consist of small samples of not 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.6This device,attached to a

18、 suitable pole, shall be lowered to the desireddepth, the stopper or top removed, and the container allowed tofill. If a sample from close to the bottom of a tank shows adecided difference in color or appearance from samples takenat other depths, an extra bottom sample shall be taken andexamined sep

19、arately from the composite sample. In such case,the composite sample shall not include any portion of suchbottom sampling.5.3 From Barrels 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

20、 direction, and it is recommended that everypackage be sampled in the case of expensive terpene hydro-carbons that are bought in small quantity. A portion shall bewithdrawn from about the center of each package sampled bymeans of a “thief” or other sampling device. The compositesample thus obtained

21、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 AND REMOVAL OF SEPARATEDWATER6. Procedure6.1 Draw a portion by means of a glass or metal containerwith a removable stopper or top,6or with a “thief,” from thelowes

22、t 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, record the quantity, and deduct it from the totalvolume of liquid delivered.APPEARANCE7. Procedure7.1 Examine a portion of the sample after agitation todetermine

23、whether its appearance conforms to specifications.ODOR8. Procedure8.1 Compare the odor of the sample with an agreed-uponwater-free reference 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.

24、SPECIFIC GRAVITY9. Procedure9.1 Determine the specific gravity at 15.6/15.6C by anyconvenient method having a precision of 0.0005. Determina-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

25、each degree Celsius thatthe temperature of the liquid is above or below 15.6C. If thedetermination is made with apparatus calibrated for a 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 a

26、pplying the above factor,and finally converted to specific gravity by dividing thecalculated density by 0.999 (the density of water at 15.6C).REFRACTIVE INDEX10. Procedure10.1 Determine the refractive index with an accurate instru-ment, at 20C if possible. If determined at any other tempera-ture, co

27、rrect the reading obtained to 20C by adding orsubtracting 0.00045 for each degree Celsius that the tempera-ture at which the determination was made is, respectively,above or below 20C.DISTILLATION11. Apparatus11.1 Use the type of distillation apparatus described in TestMethod D86, with the following

28、 exceptions:11.1.1 For testing turpentine or pinene use an ASTM Tur-pentine Distillation Thermometer, 3-in. (76-mm) partial im-mersion, having a range from 147 to 182C, and conforming tothe requirements for Thermometer 27C as prescribed in Speci-fication E 2251, or an ASTM Solvents Distillation Ther

29、mom-eter, 3.94-in. (100-mm) partial immersion, having a range from95 to 255C, and conforming to the requirements for Ther-mometer 42C as prescribed in Specification E 2251.11.1.2 Ice is not necessary in the condenser bath. It ispermissible to use a glass Liebig condenser 22 in. (560 mm) inlength wit

30、h 16 in. (410 mm) in contact with the cooling waterand filled with an adapter to extend 1 in. (51 mm) into thereceiving graduate.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the America

31、n 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.6Detailed description of equipment suitable for such sampling is given inMethods D 270.

32、D23308212. Procedure12.1 Using the receiving graduate, transfer exactly 100 mLof the sample directly into the flask, allowing none to run intothe side tube. If the sample contains dissolved or suspendedwater it is advisable to add a few small pieces of pumice orbroken glass to promote smooth distill

33、ation. Insert the ther-mometer, so that the top of the bulb (or the top of thecontraction chamber if the Solvents Distillation Thermometeris 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 cera

34、mic or other heat resistantboard. Apply heat cautiously, and regulate it so that the firstdrop of condensate falls from the condenser in not 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

35、for barometric pressure as describedin Section 13. When the distillation begins, regulate the heat sothat the distillate is collected at a rate of not less than 4 normore than 5 mL/min (approximately 2 drops/s). Discontinuethe distillation when the temperature reaches that specified forthe minimum p

36、ercentage requirement (usually 170C forturpentine), after correcting for barometric pressure. Allow thecondenser to drain and read the percentage distilled.12.2 The percentages distilled below successive selectedtemperatures and the temperature at which each successive 10mL distills may also be dete

37、rmined, if desired, making thenecessary correction of the temperature for barometric pres-sure.13. Barometric Correction13.1 The distilling temperature of turpentine (and pinene) isaffected by 0.052C for each millimetre (1.32C for each inch)variation of the atmospheric pressure. Therefore, the disti

38、lla-tion temperatures observed or specified shall be corrected topermit distillation to be conducted as though the barometerreading, corrected 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.

39、 (No temperature correction is necessary foraneroid-type barometers.) From Table 1 determine the propertemperature correction corresponding to these atmosphericconditions, interpolating to the nearest 0.1C. If the barometricpressure, corrected to 0C, is below 760 mm, the temperaturecorrection must b

40、e added to the initial boiling point andsubtracted from the minimum percentage requirement tempera-ture; if above 760 mm, the correction must be subtracted fromthe initial boiling point and added to the minimum percentagerequirement temperature.NOTE 1ExampleSuppose the observed barometric pressure i

41、s 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, thecorrected boiling point is 155.2 + 0.8 = 156C. Furthermore, the tempera-ture observation point at the minimum percentage requirement (170C at760 mm) must b

42、e altered to the same extent. Since the turpentine isdistilling 0.8C below what it would at normal pressure, distillation mustbe discontinued 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 appar

43、atus with the accepted or specific colorstandard. Accepted color standards are the Gardner color scalefound in Test Method D 6166 and the platinum-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 o

44、nce widely used for thesampling and testing of turpentines and pinenes. Currently theyare not widely used and it is not considered practical toredetermine the precision and bias of the individual methods atthis time.16. Keywords16.1 pinene; sampling; turpentineTABLE 1 Temperature Corrections for Bar

45、ometric PressureAObservedBarometricPressure,mmAneroidBarometerMercurial BarometerTemperature of Barometer20C 25C 30C 35C780 1.04 0.91 0.88 0.84 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 +

46、 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 + 3.33AThese 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

47、, Instrument Division, U. S. Weather Bureau. The corrected barometric pressureis then subtracted from 760 mm (or vice versa) and the difference multiplied by0.052C to give the temperature correction shown in this table. The correctionfactor, C, of 0.052C was calculated using the Sydney-Young equatio

48、n:C = 0.00012(760 P)(273 + T)where:P = observed pressure, corrected to 0C, in millimetres, andT = median boiling temperature for turpentine, 160C.D233083ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. U

49、sers 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 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 commen