ASTM D1078-2011 Standard Test Method for Distillation Range of Volatile Organic Liquids《挥发性有机液馏程的标准试验方法》.pdf

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1、Designation: D1078 11Designation: 195/98Standard Test Method forDistillation Range of Volatile Organic Liquids1This standard is issued under the fixed designation D1078; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l

2、ast revision. A number 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 Department of Defense.1. Scope*1.1 This test method covers the determina

3、tion of the distil-lation range of liquids boiling between 30 and 350C, that arechemically stable during the distillation process, by manual orautomatic distillation procedures.1.2 This test method is applicable to organic liquids such ashydrocarbons, oxygenated compounds, chemical intermedi-ates, a

4、nd blends thereof.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications, test result(s) shall be ro

5、unded off “to the nearestunit” in the last right-hand digit used in expressing thespecification limit, in accordance with the rounding-off methodof Practice E29.1.5 For hazard information and guidance, see the suppliersMaterial Safety Data Sheet.1.6 WarningMercury has been designated by EPA andmany

6、state agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety

7、Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for additional informa-tion. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited bystate law.1.7 This standard does not purport to address all of thesafet

8、y 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. Specific hazardstatements are given in Section 7.2. Referenced Documents2.1

9、 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE133 Specification for Distillation EquipmentE299 Test

10、 Method for Trace Amounts of Peroxides InOrganic Solvents2.2 ASTM Adjuncts:Determination of Precision and Bias for Use in Test Methodsfor Petroleum Products and Lubricants33. Terminology3.1 Definitions:3.1.1 initial boiling point, nthe temperature indicated bythe distillation thermometer at the inst

11、ant the first drop ofcondensate leaves the condenser tube.3.1.2 dry point, nthe temperature indicated at the instantthe last drop of liquid evaporates from the lowest point in thedistillation flask, disregarding any liquid on the side of theflask.3.1.3 decomposition point, nthe thermometer reading t

12、hatcoincides with the first indications of thermal decomposition ofthe liquid in the flask.3.2 Definitions of Terms Specific to This Standard:3.2.1 final boiling point, nthe maximum thermometerreading obtained during the test.3.2.1.1 DiscussionThis usually occurs after the evapora-tion of all liquid

13、 from the bottom of the flask. The term“maximum temperature” is a frequently used synonym.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents, Plasticizers, and

14、Chemical Intermediates.Current edition approved Nov. 15, 2011. Published December 2011. Originallyapproved in 1949. Last previous edition approved in 2005 as D1078 05. DOI:10.1520/D1078-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servic

15、eastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from ASTM International Headquarters. Order Adjunct No.ADJD6300.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International,

16、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.2 end point 5 minutes, nthe thermometer readingobtained 5 min after the 95 % distillation point if no dry or finalboiling point occurs.4. Summary of Test Method4.1 A100-mLspecimen is distilled under conditions eq

17、uiva-lent to a simple batch differential distillation. The temperatureof the thermometer is equilibrated with that of the refluxingliquid before the distillate is taken over. Boiling temperaturesobserved on a partial immersion thermometer are corrected tostandard atmospheric pressure to give true bo

18、iling tempera-tures.5. Significance and Use5.1 This test method provides a method of measurement ofdistillation range of volatile organic liquids. The relativevolatility of organic liquids can be used with other tests foridentification and measurement of quality. Therefore, this testmethod provides

19、a test procedure for assessing compliancewith a specification.5.2 This test method also provides an empirical value ofresidue, solvent recovery capacity, and loss (or non-recovery)on heating. Organic liquids are used as solvents in manychemical processes. As the relative volatility, residual mattera

20、nd recovery capability affect the efficiency of these processes,this test method is useful in manufacturing control.6. Apparatus6.1 Distillation ApparatusSee Condenser and CoolingBath section, Apparatus Assembly Using Gas Burner figure,Apparatus Assembly Using Electric Heater figure, and MetalShield

21、 or Enclosure for Flask section of Specification E133.6.1.1 Manual Distillation ApparatusSee Condenser Cool-ing Bath section, Apparatus Assembly Using Gas Burnerfigure, Apparatus Assemble Using Electric Heater figure, andMetal Shield or Enclosure for Flask section of SpecificationE133.6.1.2 Automate

22、d Distillation ApparatusAny automatedinstrument that complies with 6.2-6.5, and is capable ofachieving the operating parameters given in 9.1.3 and 9.1.4,isacceptable.6.2 Distillation Flasks, 200-mL of borosilicate glass com-plying with the specifications given in Distillation Flasksection, Fig. 3, a

23、nd Flask C of Specification E133.NOTE 1Liquid superheating in a new flask may be prevented bydepositing a small amount of carbon in the bottom of the flask. This maybe accomplished by heating and decomposing a pinch of tartaric acid inthe bottom of the flask. The flask is then prepared for use by wa

24、shing withwater, rinsing with acetone, and drying.6.3 Source of HeatAn adjustable gas burner or electricheater so constructed that sufficient heat can be obtained todistill the product at the uniform rate specified in Section 8. Fornarrow-range (less than 2C) liquids, an electric heater may beused o

25、nly if it has been proven to give results comparable tothose obtained when using gas heat. (See Section 9 for factorsthat cause superheating, and Appendix X1 for a discussion onthe use of electric heaters.)6.4 Distillation Receiver:6.4.1 Manual Distillation ReceiverA 100-mL cylindergraduated in 1 mL

26、 subdivision and having an overall height of250 to 260 mm.6.4.2 Automatic Distillation ReceiverA receiver to beused with automatic distillation in accordance with the instru-ment manufacturers instructions, conforming to the dimen-sions given in 6.4.1, with the exception of the graduations.6.4.2.1 A

27、utomatic Distillation Level FollowerThe levelfollower/recording mechanism of the automatic apparatus shallhave a resolution of 0.1 mL with an accuracy of 61 mL.6.5 Temperature Measurement Devices:6.5.1 Manual Distillation ThermometersPartial immer-sion thermometers as listed in Table 1, conforming t

28、o Specifi-cation E1. Other liquid-in-glass thermometers or temperaturemeasuring devices that provide equivalent range, accuracy, lagtime and precision may be used. Both bore corrections andeither ice or steam standardization corrections are recom-mended as appropriate.6.5.2 Automatic Distillation Te

29、mperature SensorsTemperature measurement systems using thermocouples orresistance thermometers shall exhibit the same temperature lagand accuracy as the appropriate and calibrated mercury-in-glass thermometer. Confirmation of the calibration of thesetemperature sensors shall be done at regular inter

30、vals. This canbe accomplished potentiometrically by the use of standardprecision resistance, depending on the type of probe. Anothertechnique is to distill pure toluene (99.9 + % purity) andcompare the temperature indicated by the thermocouple orresistance thermometer with that shown by the mercury-

31、in-glass thermometer.NOTE 2Toluene is shown in reference manuals as boiling at 110.6C(corrected for barometric pressure) under the conditions of a manualD1078 distillation that uses a partial immersion thermometer.7. Hazards7.1 WarningCertain solvents and chemical intermedi-ates, particularly, but n

32、ot only ethers and unsaturated com-pounds, may form peroxides during storage. These peroxidesmay present a violent explosion hazard when the chemical isTABLE 1 ThermometersASTMThermometerNumberIP Range, CSub-division,C2CA62CA5 to + 300 1.03CA73CA5 to + 400B14C . 38 to 82 0.137C 77C 2 to + 52 0.238C

33、78C 24 to 78 0.239C 79C 48 to 102 0.240C 80C 72 to 126 0.241C 81C 98 to 152 0.242CA82CA95 to 255 0.5102C 83C 123 to 177 0.2103C 84C 148 to 202 0.2104C 85C 173 to 227 0.2105C 86C 198 to 252 0.2106C 87C 223 to 277 0.2107C 88C 248 to 302 0.2AThese thermometers have more temperature lag than the other t

34、hermometerslisted herein and are not satisfactory for use with narrow-boiling range liquids.B1 to 301C; 1.5C above 301C.D1078 112distilled, especially as the dry point is approached. Whenperoxide formation is likely because of chemical type or lengthof storage, the material should be analyzed for pe

35、roxides (SeeTest Method E299.) and if they exist in hazardous concentra-tions, appropriate precautions should be taken such as destroy-ing the peroxide before distillation, shielding, or destroying thesample and not running the test.7.2 Most organic solvents and chemical intermediates willburn. In t

36、he operation of the distillation apparatus, use asuitable catch pan and shielding to contain spilled liquid in theevent of accidental breakage of the distillation flask.7.3 Provide adequate ventilation to maintain solvent vaporconcentrations below the lower explosive limit in the immedi-ate vicinity

37、 of the distillation apparatus, and below the thresh-old limit value in the general work area.8. Preparation of Apparatus8.1 Manual Distillation Apparatus:8.1.1 Clean and dry the condenser tube by swabbing with apiece of soft lint-free cloth attached to a wire or cord, or by anyother suitable means.

38、8.1.2 Use the thermometer listed in the material specifica-tion for the product under study. If no thermometer is specified,select one from Table 1 with the smallest graduations that willcover the entire distillation range of the material. Preferably, anequivalent non-mercury thermometer should be u

39、sed if avail-able. Center the thermometer into the neck of the flask througha tight-fitting cork stopper so that the upper end of thecontraction chamber (or bulb if Thermometer 2C or IP ther-mometer 62C is used) is level with the lower side of the vaportube at its junction with the neck of the flask

40、. (See ApparatusAssembly Using Gas Burner figure of Test Method D86.)NOTE 3It is far more important that the bulb and contraction chamberbe immersed in the refluxing zone than that the immersion mark on thethermometer be placed at any specific point.8.1.3 Position the correct heat shield (see 9.1.3.

41、1 and9.1.3.2).NOTE 4For low-boiling materials, cool the apparatus to room tem-perature before starting the test.8.1.4 Fill the condenser bath with water of the appropriatetemperature shown in Table 2.NOTE 5When distilling pure compounds always ensure that thecondenser bath temperature is above the c

42、rystallizing point of thecompound.8.1.5 Adjust the temperature of the appropriate portion ofthe sample to the applicable temperature shown in Table 2.8.2 Automatic Distillation ApparatusFor assembly of au-tomatic distillation apparatus, consult instrument manufactur-ers operating manual.9. Procedure

43、9.1 Manual Distillation Procedure:9.1.1 Using the graduated receiver measure 100 6 0.5 mLof the temperature-adjusted sample. Remove the flask from theapparatus and transfer the fresh specimen directly to the flask,allowing the graduate to drain for 15 to 20 s.NOTE 6For viscous liquids, a longer drai

44、nage period may be neces-sary to complete the transfer of the specimen to the flask, but the drainagetime should not exceed 5 min. Do not allow any of the specimen to enterthe vapor tube.9.1.2 Connect the flask to the condenser by inserting thevapor tube of the flask into the condenser, making a tig

45、htconnection with a well-rolled cork or similar material. Adjustthe position of the heat shield so that the neck of the flask isvertical and the vapor tube extends into the condenser tube adistance of 25 to 50 mm. Have the bottom of the flask restingfirmly in the hole of the heat shield. Insert the

46、thermometer asdescribed in 8.1.2. Place the receiver, without drying, at theoutlet of the condenser tube in such a position that thecondenser tube extends into the graduate at least 25 mm butdoes not extend below the 100-mL mark. If the initial boilingpoint of the material is below 70C, immerse the

47、cylinder in atransparent bath and maintain at a temperature of 10 to 20Cthroughout the distillation. Place a flat cover on the top of thegraduate to prevent condensed moisture from entering thegraduate.9.1.3 Acertain amount of judgment is necessary in choosingthe best operating conditions to get acc

48、eptable accuracy andprecision for materials having different distilling temperatures.As a general guide, it is recommended that:9.1.3.1 For materials having an initial boiling point below150C, the following conditions be established:(a) Heat ShieldHole size, 32-mm diameter.(b) Heating RateTime from

49、application of heat to firstdrop of distillate, 5 to 10 min, and time of rise of vapor columnin neck of flask to side arm, 212 to 312 min.9.1.3.2 For materials having an initial boiling point above150C, the following conditions should be established:(a) Heat ShieldHole size, 38-mm diameter.(b) Heating RateTime from application of heat to firstdrop of distillate, 10 to 15 min, and time of rise of vaporcolumn in neck of flask to side arm, sufficiently rapid to permitcollection of the first drop of distillate within 15 min of the starto