1、Designation: D 1078 05Designation: 195/98Standard Test Method forDistillation Range of Volatile Organic Liquids1This standard is issued under the fixed designation D 1078; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 last revision. A number in parentheses 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. Scope*1.1 This test method covers the determ
3、ination 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
4、, and 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
5、 rounded 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 This standard does not purport to address all o
6、f 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. Specific hazardstatements are given in Section 7.2. Referenced Do
7、cuments2.1 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 SpecificationsE 133 Specification for Distillation Equipme
8、ntE 299 Test 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
9、 at the instant 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 thermomet
10、er reading thatcoincides 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 o
11、f all liquid from the bottom of the flask. The term“maximum temperature” is a frequently used synonym.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 u
12、nder conditions equiva-lent to a simple batch differential distillation. The temperatureof the mercury in the thermometer is equilibrated with that of1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsi
13、bility ofSubcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved May 15, 2005. Published June 2005. Originallyapproved in 1949. Last previous edition approved in 2003 as D 1078 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orconta
14、ct ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from ASTM International Headquarters. Request Adjunct No.ADJD6300.1*A Summary of Changes section appears at the end of this sta
15、ndard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the refluxing liquid before the distillate is taken over. Boilingtemperatures observed on a partial immersion thermometer arecorrected to standard atmospheric pressure to give true
16、 boilingtemperatures.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
17、 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 matter
18、and 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 MetalShiel
19、d or Enclosure for Flask section of Specification E 133.6.1.1 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 SpecificationE 133.6.1.2 Autom
20、ated 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
21、, and Flask C of Specification E 133.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 b
22、y washing 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 beus
23、ed only 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
24、1 mL 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
25、.1 Automatic Distillation Level FollowerThe levelfollower/recording mechanism of the automatic apparatus shallhave a resolution of 0.1 mL with an accuracy of 6 1 mL.6.5 Temperature Measurement Devices:6.5.1 Manual Distillation ThermometersPartial immer-sion thermometers as listed in Table 1, conform
26、ing to Specifi-cation E1. Both bore corrections and either ice or steamstandardization corrections are recommended.6.5.2 Automatic Distillation Temperature SensorsTemperature measurement systems using thermocouples orresistance thermometers shall exhibit the same temperature lagand accuracy as the a
27、ppropriate and calibrated mercury-in-glass thermometer. Confirmation of the calibration of thesetemperature sensors shall be done at regular intervals. This canbe accomplished potentiometrically by the use of standardprecision resistance, depending on the type of probe. Anothertechnique is to distil
28、l pure toluene (99.9 + % purity) andcompare the temperature indicated by the thermocouple orresistance thermometer with that shown by the mercury-in-glass thermometer.NOTE 2Toluene is shown in reference manuals as boiling at 110.6C(corrected for barometric pressure) under the conditions of a manualD
29、 1078 distillation that uses a partial immersion thermometer.7. Hazards7.1 WarningCertain solvents and chemical intermedi-ates, particularly, but not only ethers and unsaturated com-pounds, may form peroxides during storage. These peroxidesmay present a violent explosion hazard when the chemical isd
30、istilled, especially as the dry point is approached. Whenperoxide formation is likely because of chemical type or lengthof storage, the material should be analyzed for peroxides (SeeTest Method E 299.) and if they exist in hazardous concentra-tions, appropriate precautions should be taken such as de
31、stroy-ing the peroxide before distillation, shielding, or destroying thesample and not running the test.7.2 Most organic solvents and chemical intermediates willburn. In the operation of the distillation apparatus, use asuitable catch pan and shielding to contain spilled liquid in theevent of accide
32、ntal breakage of the distillation flask.TABLE 1 ThermometersASTMThermometerNumberIP Range, CSub-division,C2CA62CA5 to + 300 1.03CA73CA5 to + 400B14C . 38 to 82 0.137C 77C 2 to + 52 0.238C 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
33、 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 thermometerslisted herein and are not satisfactory for use with narrow-boiling range liquids.B1 to 301C; 1.5C abo
34、ve 301C.D10780527.3 Provide adequate ventilation to maintain solvent vaporconcentrations below the lower explosive limit in the immedi-ate vicinity of the distillation apparatus, and below the thresh-old limit value in the general work area.8. Preparation of Apparatus8.1 Manual Distillation Apparatu
35、s: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.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
36、the smallest graduations that willcover the entire distillation range of the material. Center thethermometer into the neck of the flask through a tight-fittingcork stopper so that the upper end of the contraction chamber(or bulb if Thermometer 2C or IP thermometer 62C is used) islevel with the lower
37、 side of the vapor tube at its junction withthe neck of the flask. (See Apparatus Assembly Using GasBurner figure of Test Method D86.)NOTE 3It is far more important that the greatest volume of mercurybe immersed in the refluxing zone than that the immersion mark on thethermometer be placed at any sp
38、ecific point.8.1.3 Position the correct heat shield (see 9.1.3.1 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
39、always ensure that thecondenser bath temperature is above the crystallizing 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,
40、consult instrument manufactur-ers operating manual.9. Procedure9.1 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 t
41、o drain for 15 to 20 s.NOTE 6For viscous liquids, a longer drainage 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 insert
42、ing thevapor tube of the flask into the condenser, making a tightconnection 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
43、flask restingfirmly in the hole of the heat shield. Insert the 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
44、initial boilingpoint of the material is below 70C, immerse the 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 i
45、s necessary in choosingthe best operating conditions to get acceptable 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)
46、Heat ShieldHole size, 32-mm diameter.(b) Heating RateTime from 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
47、 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 star
48、tof heating.9.1.4 Adjust the heat input so that the distillation proceeds ata rate of 4 to 5 mL/min (approximately 2 drops per second),and move the receiving cylinder so that the tip of the condensertube touches one side of the cylinder after the first drop falls(initial boiling point). Record the r
49、eadings of the distillationthermometer after collecting 5, 10, 20, 30, 40, 50, 60, 70, 80,90, and 95 mL of distillate.9.1.5 Without changing the heater setting, continue distilla-tion beyond the 95 % point until the dry point is observed.Record the temperature at this point as the dry point (Section3). If a dry point is not obtained (that is, if active decomposi-tion should occur before the dry point is reached, as evidencedby a rapid evolution of vapor or heavy fumes; or if there isliquid remaining on the bottom of the flask when the max
