ASTM D850-2018 Standard Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials.pdf

1、Designation: D850 16D850 18Standard Test Method forDistillation of Industrial Aromatic Hydrocarbons and RelatedMaterials1This standard is issued under the fixed designation D850; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the

2、year of last 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 U.S. Department of Defense.1. Scope*1.1 This test method covers

3、 the distillation of industrial aromatic hydrocarbons and related materials of relatively narrow boilingranges from 30 to 250C.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.2 The following applies to all specified limi

4、ts in this test method: for the purposes of determining conformance to this testmethod, an observed or calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressingthe specification limit, in accordance with the rounding-off method of Practice E29.1.3 Wa

5、rningMercury has been designated by EPA and many state agencies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury-containing pro

6、ducts. See the applicable product Safety Data Sheet (SDS) fordetails and EPAs website (http:/www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that sellingmercury or mercury-containing products, or both, in your state may be prohibited by state law.1.4 The values stated

7、in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safe

8、ty, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. For specific hazard statements, see 6.5.2, 6.6.1 and Section 7.1.6 This international standard was developed in accordance with internationally recognized principles on standardizatio

9、nestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1078 Test Method for Distillation Range of Volatile Orga

10、nic LiquidsD3437 Practice for Sampling and Handling Liquid Cyclic ProductsD4790 Terminology of Aromatic Hydrocarbons and Related ChemicalsD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE1 Specification for ASTM Liquid-in-Glass Thermome

11、tersE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE133 Specification for Distillation EquipmentE220 Test Method for Calibration of Thermocouples By Comparison TechniquesE691 Practice for Conducting an Interlaboratory Study to Determine the Precisi

12、on of a Test Method1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of Subcommittee D16.04 on Instrumental Analysis.Current edition approved June 1, 2016June 1, 2018. Publ

13、ished July 2016June 2018. Originally approved in 1945. Last previous edition approved in 20112016 asD850 11.D850 16. DOI: 10.1520/D0850-16.10.1520/D0850-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM

14、 Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically pos

15、sible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCo

16、pyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200 33. Terminology3.1 Definitions:3.1.1 See Terminology D4790 for definitions of terms used in this test method.

17、4. Summary of Test Method4.1 The distillation of a 100-mL sample of industrial aromatic hydrocarbons and related materials is carried out via a carefullycontrolled distillation wherein temperature readings are noted for the first drop of distillate and when 5, 10, and each additional10 up to 90, and

18、 95 % of the sample has distilled over. The temperature corresponding to the dry point is also noted.5. Significance and Use5.1 This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in developmentor research work on industrial aromatic hydr

19、ocarbons and related materials.5.2 This test method gives a broad indication of general purity and can also indicate presence of excessive moisture. It will notdifferentiate between products of similar boiling range.6. Apparatus6.1 Distillation FlaskAstandard 200-mL side-tube, heat-resistant glass d

20、istillation flask as shown in Fig. 1, conforming to thefollowing dimensions:Diameter of bulb, outside, mm 76 1.5Diameter of neck, inside, mm 21 1Height of flask, outside, mm 179 3Vertical distance from bottom of bulb outside tobottom of vapor-tube opening in neck, mm120 3Length of side tube, mm 100

21、3Diameter of side tube, outside, mm 7 0.5Angle of side tube with vertical axis of bulb andneck, 75 3The flask does not comply with Flask C of Specification E133.6.2 Temperature Measurement Devices:6.2.1 Manual Distillation ThermometerThe ASTM Solvents Distillation Thermometer used in the test shall

22、be as prescribedin the specifications for the material being tested. If no thermometer is specified in the material specification, select one from Table1 with the smallest graduations that will cover the entire distillation range of the material being tested. Table 1 lists severalASTMsolvents distil

23、lation thermometers which are suitable for testing industrial aromatic hydrocarbons, and which meet the requirementsof Specification E1.3 Available 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

24、.FIG. 1 Distillation FlaskD850 1826.2.2 Automatic Distillation Temperature SensorTemperature measurement systems using thermocouples or resistancethermometers, otherwise referred to as the “temperature measuring devices,” must exhibit the same temperature lag and accuracyas the equivalent mercury gl

25、ass thermometer. Confirmation of the calibration of these temperature sensors is to be done at regularintervals. This may be accomplished as prescribed in Test Method E220, or some similar means using a precision resistance decadebox. Another technique is to distill pure toluene and compare the temp

26、erature indicated by the thermocouple or resistancethermometer with that shown by the thermometer. When installing a new automatic distillation analyzer, a toluene sample witha known distillation range of approximately 1.0C must be used to verify the dry point and distillation range.4 It is recommen

27、dedthat such a material be used when replacing a temperature measuring device. Alternatively a material of known distillation rangeand dry point may be used when replacing a temperature measuring device.6.2.2.1 Automatic Distillation Temperature Sensor Centering DeviceThe temperature sensor shall be

28、 mounted through asnug-fitting device designed to mechanically center the sensor in the neck of the flask. The use of a cork or silicone stopper witha hole drilled through the center is not acceptable for this purpose. Examples of acceptable centering devices are shown in Fig.2.6.2.2.2 The electroni

29、c circuitry or algorithms, or both, used shall include the capability to simulate the temperature lag of amercury-in-glass thermometer. For that reason the known toluene sample with a distillation range of approximately 1.0C mustbe used to verify the algorithm and dampening software.6.2.2.3 Alternat

30、ively, the sensor can also be placed in a casing with the tip of the sensor covered, so that the assembly, becauseof its adjusted thermal mass and conductivity, has a temperature lag similar to that of a mercury-in-glass thermometer.4 Such a material is available from Spectrum Quality Standards.TABL

31、E 1 ASTM Thermometers for Distillation Test of IndustrialAromatic HydrocarbonsASTMThermometerNo.Name Range, C Subdivision,C39C solvents distillation 48 to 102 0.240C solvents distillation 72 to 126 0.241C solvents distillation 98 to 152 0.242C solvents distillation 95 to 255 0.5102C solvents distill

32、ation 123 to 177 0.2103C solvents distillation 148 to 202 0.2104C solvents distillation 173 to 227 0.2105C solvents distillation 198 to 252 0.2106C solvents distillation 224 to 276 0.2111C solvents distillation 170 to 250 0.2FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck FlasksD8

33、50 183NOTE 1In a region where the temperature is changing rapidly during the distillation, the temperature lag of a thermometer can be as much as3 s.6.3 Condenser and Cooling Bath:6.3.1 Manual Distillation Condenser and Cooling Bath:6.3.1.1 The manual distillation condenser and cooling bath shall be

34、 as specified in Section 5, and Fig. 1 of Specification E133.6.3.1.2 As an alternative, the condenser tube may consist of a straight glass tube 600 to 610 mm in length and 12 mm in insidediameter, of standard wall thickness (about 1.25 mm) with the exit end cut off square and ground flat. It shall b

35、e set in a coolingtrough so that at least 380 mm of the tube is in contact with the water. Clearance between the condenser tube and any parallel sideof the trough shall be not less than 19 mm. The water in the cooling trough shall be maintained at 10 to 20C. This may be doneby adding ice to the wate

36、r or by circulating chilled water through the trough. The trough shall be so mounted that the condensertube is set at an angle of 75 with the vertical. To minimize the turbulence in the receiver during the run, provisions shall be madeto enable the flow of the distillate to run down the side of the

37、receiving cylinder. This can be accomplished by using adrip-deflector, which is attached to the outlet of the tube.6.3.2 Automatic Distillation and Cooling BathThe automatic distillation and cooling bath shall be as specified in Section 5,Fig. 2 of Specification E133.6.4 Distillation Receiver:6.4.1

38、Manual Distillation ReceiverAgraduate of the cylindrical type, of uniform diameter, with a pressed or molded base anda lipped top. The cylinder shall be marked to contain 100 mL, and the 0 to 100 mL receiver portion shall be not less than 178 normore than 203 mm in length. It shall be graduated in s

39、ingle millilitres and each fifth mark shall be distinguished by a longer line.It shall be numbered from the bottom up at intervals of 10 mL. The overall height of the receiver shall not be less than 248 normore than 260 mm. The graduations shall not be in error by more than 1 mLat any point on the s

40、cale. The bottom 1-mLgraduationmay be omitted. The receiver complies with Section 9, Graduate B Fig. 4, of Specification E133.6.4.2 Automatic Distillation ReceiverA receiver to be used with measurements in accordance with the instrumentmanufacturer and conform to the physical specifications describe

41、d in this section, with the exception of the graduations.6.4.2.1 Automatic Distillation Level FollowerFor automatic apparatus, the level follower or recording mechanism of theapparatus will have a resolution of 0.1 mL with an accuracy of 61 mL. The calibration of the assembly should be confirmedacco

42、rding to the manufacturers instructions at regular intervals. The typical calibration procedure involves verifying the outputwith the receiver containing 5 and 100 mL of material respectively.6.5 Flask Support Assembly:6.5.1 For Units Using Electric HeatersThe assembly consists of an adjustable syst

43、em onto which the electric heater ismounted with provision for placement of a flask support board (see 6.5.2) above the electric heater. The whole assembly isadjustable from the outside of the shield.6.5.2 Flask Support BoardThe flask support board shall be constructed of ceramic or other heat-resis

44、tant material with acentrally located opening. For tests of benzene and toluene, the opening shall be 25 mm in diameter; for tests of materials boilingabove toluene but mostly below 145C, the opening shall be 38 mm in diameter, and for higher boiling materials, it shall be 50mm in diameter. The flas

45、k support board shall be of sufficient dimension to ensure that thermal heat to the flask only comes fromthe central opening and that extraneous heat to the flask other than through the central opening is minimized. (WarningHeatresistant-containing materials shall not be used in the construction of

46、the flask support board.)6.5.3 For Units Using Bunsen BurnerThe flask support board is approximately 50 mm higher than the top of the burner.6.6 Heater:6.6.1 Manual Distillation HeaterAn electric heater or a bunsen burner, fully adjustable and capable of giving sufficient heatto distill the product

47、at the required rate. When a bunsen burner is used, as described in 7.1 and Fig. 1 of Specification E133, theburner shall be adjusted so as to produce an entirely blue flame. (WarningSuperheating of the flask can cause erroneous resultsand is more likely to occur with electric heaters than with buns

48、en burners as heat sources. This problem is discussed in the sectionon Preparation of Apparatus in Test Method D1078.)7. Hazards7.1 Consult current OSHAregulations and suppliers Safety Data Sheets, and local regulations, for all materials used in this testmethod.8. Sampling8.1 Sampling should follow

49、 safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations.Refer to Practice D3437 for proper sampling and handling of aromatic hydrocarbons analyzed by this test method.8.2 The sample under test shall be transparent and free of separated water. Any separated water may ordinarily be eliminatedby care in pouring the 100-mL specimen (10.1) into the graduated cylinder. If necessary, any separated water or cloudiness maybe removed by filtration, in which case the following precautions shall be tak