ASTM D233-13(2017) Standard Test Methods of Sampling and Testing Turpentine.pdf

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1、Designation: D233 13 (Reapproved 2017)Standard 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 nu

2、mber in parentheses 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 U.S. Department of Defense.1. Scope1.1 These test methods cover procedures for sampling an

3、dtesting turpentine, as defined by the Code of Federal Regula-tions and Terminology D804. 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 turpe

4、ntines and pinenes.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 ha

5、s displacedthese test methods to a large extent. (See for example TestMethods D6387.)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.

6、1.4 This standard does 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use

7、.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers t

8、o Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products andLiquid Fuels at Atmospheric PressureD270 Methods of Sampling Petroleum and Petroleum Prod-ucts (Withdrawn 1984)3D804 Terminology Relating to Pine Chemicals, IncludingTall Oil

9、and Related ProductsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D6166 Test Method for Color of Pine Chemicals and Re-lated Products (Instrumental Determination of GardnerColor)D6387 Test Methods for Composition of Turpentine andRelated Ter

10、pene Products by Capillary Gas Chromatogra-phyE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 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 weredevelope

11、d 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 syntheticorganic chemicals. Thus the chemical composition of turpen-tines and pinenes is extremely important and tests, in additionto

12、 the ones described in these test methods, are required inorder to fully characterize turpentines and pinenes. The most1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.3

13、4 on Pine Chemicals and HydrocarbonResins.Current edition approved Dec. 1, 2017. Published December 2017. Originallyapproved in 1926. Last previous edition approved in 2013 as D233 13. DOI: 10.1520/D0233-13R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custo

14、mer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from U.S. Government Printing Office Superintendent of D

15、ocuments,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized pri

16、nciples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1widely used technique for determining the chemical composi-tion of turpen

17、tines (and pinenes) is gas chromatography (seeTest Methods D6387).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 American Chemica

18、l 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 the accuracy ofthe determination.4.2 Unless otherwise indicated, references to water shall beunderstood to

19、 mean reagent water conforming to SpecificationD1193.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) andshou

20、ld 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 suitable pole, shall be lowered to the desireddepth, the stopper or top removed, and the container allowed

21、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 separately from the composite sample. In such case,the composite sample shall not include any portion of suchbo

22、ttom 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 direction, and it is recommended that everypackage be sampled in the case of expensive terpene hydro-carbon

23、s 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 shall be not less than 1 qt (0.9 L) andshall consist of equal portions of not less than12 pt (0.24 L)from ea

24、ch 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 thelowest part of the container, or by opening the bottom valve ofthe perfectly level tank car. If water is found in

25、 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 whether its appearance conforms to specifications.ODOR8. Procedure8.1 Compare the odor of the sample with an

26、 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.SPECIFIC GRAVITY9. Procedure9.1 Determine the specific gravity at 15.6/15.6C by anyconvenient method having

27、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 each degree Celsius thatthe temperature of the liquid is above or below 15.6C. If thedetermination is made w

28、ith 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 applying the above factor,and finally converted to specific gravity by dividing thecalculated density by 0.99

29、9 (the density of water at 15.6C).REFRACTIVE INDEX10. Procedure10.1 Determine the refractive index with an accurateinstrument, at 20C if possible. If determined at any othertemperature, correct the reading obtained to 20C by adding orsubtracting 0.00045 for each degree Celsius that the tempera-ture

30、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 exceptions:11.1.1 For testing turpentine or pinene use an ASTM Tur-pentine Distillation Thermometer, 3-in. (76-

31、mm) partialimmersion, having a range from 147 to 182C, and conformingto the requirements for Thermometer 27C as prescribed in5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Ch

32、emical 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 D270.D233

33、13 (2017)2Specification E1, or an ASTM Solvents DistillationThermometer, 3.94-in. (100-mm) partial immersion, having arange from 95 to 255C, and conforming to the requirementsfor Thermometer 27C as prescribed in Specification E1 or from95 to 255C and conforming to the requirements for Thermom-eter 4

34、2C as prescribed in Specification E1. Thermometricdevices such as RTDs, thermistors and liquid-in-glass ther-mometers of equal or better accuracy in the specified tempera-ture range, may be used.11.1.2 Ice is not necessary in the condenser bath. It ispermissible to use a glass Liebig condenser 22 in

35、. (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.12. Procedure12.1 Using the receiving graduate, transfer exactly 100 mLof the sample directly into the flask, allowing none to run intothe side tube

36、. 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 thethermometer, so that the top of the bulb (or the top of thecontraction chamber if the Solvents Distillation Thermometeris used) is level w

37、ith 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 less than 5nor m

38、ore 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 rate of not less t

39、han 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 percentage distilled.1

40、2.2 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 temperature of tu

41、rpentine (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, corrected to 0C, were ex

42、actly 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 to these atmosphe

43、ricconditions, 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 must be subtracted f

44、romthe 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, thecorrected bo

45、iling 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 discontinued at 169.2C to de

46、termine 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 D6166 and the platinum-cobalt scal

47、efound in Test Method D1209.15. 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 toredetermine the

48、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 0.84 0.81770 0.52 0.

49、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 + 3.33AThese corrections are calculated as follows: The observed barometric pressureis first corrected to what it would be at 0C, by means of the table in Circular F,Instrument Division, U. S. Weather Bureau. The corrected barometric pressure isthen subtrac