ASTM D850-03(2008)e1
(Test Method)Standard Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
Standard Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
SIGNIFICANCE AND USE
This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in development or research work on industrial aromatic hydrocarbons and related materials.
This test method gives a broad indication of general purity and can also indicate presence of excessive moisture. It will not differentiate between products of similar boiling range.
SCOPE
1.1 This test method covers the distillation of industrial aromatic hydrocarbons and related materials of relatively narrow boiling ranges from 30 to 250°C.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The following applies to all specified limits in this test method: for the purposes of determining conformance to this test method, an observed or calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
1.4 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA's website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, 6.6.1and Section 7.
General Information
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´1
Designation:D850–03(Reapproved2008)
Standard Test Method for
Distillation of Industrial Aromatic Hydrocarbons and Related
Materials
This standard is issued under the fixed designation D850; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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.
´ NOTE—Mercury warning was editorially added in June 2008.
1. Scope 2. Referenced Documents
1.1 This test method covers the distillation of industrial 2.1 ASTM Standards:
aromatic hydrocarbons and related materials of relatively D1078 Test Method for Distillation Range of Volatile Or-
narrow boiling ranges from 30 to 250°C. ganic Liquids
1.2 The values stated in SI units are to be regarded as the D3437 Practice for Sampling and Handling Liquid Cyclic
standard. The values given in parentheses are for information Products
only. D4790 TerminologyofAromaticHydrocarbonsandRelated
1.3 The following applies to all specified limits in this test Chemicals
method: for the purposes of determining conformance to this E1 Specification for ASTM Liquid-in-Glass Thermometers
test method, an observed or calculated value shall be rounded E29 Practice for Using Significant Digits in Test Data to
off “to the nearest unit” in the last right-hand digit used in Determine Conformance with Specifications
expressing the specification limit, in accordance with the E133 Specification for Distillation Equipment
rounding-off method of Practice E29. E220 Test Method for Calibration of Thermocouples By
1.4 Warning—Mercury has been designated by EPA and Comparison Techniques
many state agencies as a hazardous material that can cause E691 Practice for Conducting an Interlaboratory Study to
central nervous system, kidney and liver damage. Mercury, or Determine the Precision of a Test Method
its vapor, may be hazardous to health and corrosive to 2.2 Other Document:
materials.Cautionshould be taken when handling mercuryand OSHA Regulations, 29 CFR paragraphs 1910.1000 and
mercury-containing products. See the applicable product Ma- 1910.1200
terial Safety Data Sheet (MSDS) for details and EPA’s website
3. Terminology
(http://www.epa.gov/mercury/faq.htm) for additional informa-
3.1 Definitions:
tion. Users should be aware that selling mercury or mercury-
containingproducts,orboth,inyourstatemaybeprohibitedby 3.1.1 See Terminology D4790 for definitions of terms used
in this test method.
state law.
1.5 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 The distillation of a 100-mL sample of industrial aro-
responsibility of the user of this standard to establish appro-
matic hydrocarbons and related materials is carried out via a
priate safety and health practices and determine the applica-
carefully controlled distillation wherein temperature readings
bility of regulatory limitations prior to use. For specific hazard
are noted for the first drop of distillate and when 5, 10, and
statements, 6.6.1 and Section 7.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D16 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Standards volume information, refer to the standard’s Document Summary page on
Subcommittee D16.04 on Instrumental Analysis. the ASTM website.
Current edition approved June 1, 2008. Published June 2008. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
approved in 1945. Last previous edition approved in 2003 as D850 – 03. DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/D0850-03R08E01.
www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D850–03 (2008)
TABLE 1 ASTM Thermometers for Distillation Test of Industrial
each additional 10 up to 90, and 95 % of the sample has
Aromatic Hydrocarbons
distilled over. The temperature corresponding to the dry point
ASTM
is also noted.
Subdivision,
Thermometer Name Range, °C
°C
No.
5. Significance and Use
39C solvents distillation 48 to 102 0.2
5.1 Thistestmethodissuitableforsettingspecifications,for
40C solvents distillation 72 to 126 0.2
41C solvents distillation 98 to 152 0.2
use as an internal quality control tool, and for use in develop-
42C solvents distillation 95 to 255 0.5
mentorresearchworkonindustrialaromatichydrocarbonsand
102C solvents distillation 123 to 177 0.2
related materials. 103C solvents distillation 148 to 202 0.2
104C solvents distillation 173 to 227 0.2
5.2 This test method gives a broad indication of general
105C solvents distillation 198 to 252 0.2
purity and can also indicate presence of excessive moisture. It
willnotdifferentiatebetweenproductsofsimilarboilingrange.
turemeasuringdevices,”mustexhibitthesametemperaturelag
6. Apparatus
and accuracy as the equivalent mercury glass thermometer.
6.1 Distillation Flask—A standard 200-mL side-tube, heat-
Confirmation of the calibration of these temperature sensors is
resistant glass distillation flask as shown in Fig. 1, conforming
to be done at regular intervals. This may be accomplished as
to the following dimensions:
prescribed in Test Method E220, or some similar means using
Diameter of bulb, outside, mm 76 6 1.5
a precision resistance decade box. Another technique is to
Diameter of neck, inside, mm 21 6 1
distill pure toluene and compare the temperature indicated by
Height of flask, outside, mm 179 6 3
Vertical distance from bottom of bulb outside to 120 6 3
the thermocouple or resistance thermometer with that shown
bottom of vapor-tube opening in neck, mm
by the thermometer. When installing a new automatic distilla-
Length of side tube, mm 100 6 3
tion analyzer, a toluene sample with a known distillation range
Diameter of side tube, outside, mm 7 6 0.5
Angle of side tube with vertical axis of bulb and 75 6 3
of approximately 1.0°C must be used to verify the dry point
neck, °
and distillation range. It is recommended that such a material
The flask does not comply with Flask C of Specification
be used when replacing a temperature measuring device.
E133. Alternatively a material of known distillation range and dry
6.2 Temperature Measurement Devices:
point may be used when replacing a temperature measuring
6.2.1 Manual Distillation Thermometer—The ASTM Sol- device.
vents Distillation Thermometer used in the test shall be as
6.2.2.1 Automatic Distillation Temperature Sensor Center-
prescribed in the specifications for the material being tested. If ing Device—The temperature sensor shall be mounted through
no thermometer is specified in the material specification, select
a snug-fitting device designed to mechanically center the
one from Table 1 with the smallest graduations that will cover sensor in the neck of the flask. The use of a cork or silicone
the entire distillation range of the material being tested. Table
stopper with a hole drilled through the center is not acceptable
1 lists severalASTM solvents distillation thermometers which
for this purpose. Examples of acceptable centering devices are
are suitable for testing industrial aromatic hydrocarbons, and
shown in Fig. 2.
which meet the requirements of Specification E1.
6.2.2.2 The electronic circuitry or algorithms, or both, used
6.2.2 Automatic Distillation Temperature Sensor—
shall include the capability to simulate the temperature lag of
Temperature measurement systems using thermocouples or
a mercury-in-glass thermometer. For that reason the known
resistancethermometers,otherwisereferredtoasthe“tempera- toluenesamplewithadistillationrangeofapproximately1.0°C
must be used to verify the algorithm and dampening software.
6.2.2.3 Alternatively, the sensor can also be placed in a
casing with the tip of the sensor covered, so that the assembly,
because of its adjusted thermal mass and conductivity, has a
temperature lag similar to that of a mercury-in-glass thermom-
eter.
NOTE 1—In a region where the temperature is changing rapidly during
the distillation, the temperature lag of a thermometer can be as much as
3s.
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 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
FIG. 1 Distillation Flask Such a material is available from Spectrum Quality Standards.
´1
D850–03 (2008)
FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck Flasks
inside diameter, of standard wall thickness (about 1.25 mm) firmed according to the manufacturer’s instructions at regular
with the exit end cut off square and ground flat. It shall be set intervals. The typical calibration procedure involves verifying
in a cooling trough so that at least 380 mm of the tube is in the output with the receiver containing 5 and 100 mL of
contact with the water. Clearance between the condenser tube material respectively.
andanyparallelsideofthetroughshallbenotlessthan19mm.
6.5 Flask Support Assembly:
The water in the cooling trough shall be maintained at 10 to
6.5.1 For Units Using Electric Heaters—The assembly
20°C. This may be done by adding ice to the water or by
consists of an adjustable system onto which the electric heater
circulating chilled water through the trough. The trough shall
is mounted with provision for placement of a flask support
be so mounted that the condenser tube is set at an angle of 75°
board(see6.5.2)abovetheelectricheater.Thewholeassembly
with the vertical.
is adjustable from the outside of the shield.
6.3.2 Automatic Distillation and Cooling Bath—The auto-
6.5.2 Flask Support Board—The flask support board shall
matic distillation and cooling bath shall be as specified in
be constructed of ceramic or other heat-resistant material with
Section 5, Fig. 2 of Specification E133.
a centrally located opening. For tests of benzene and toluene,
6.4 Distillation Receiver:
the opening shall be 25 mm in diameter; for tests of materials
6.4.1 Manual Distillation Receiver—A graduate of the cy-
boiling above toluene but mostly below 145°C, the opening
lindrical type, of uniform diameter, with a pressed or molded
shall be 38 mm in diameter, and for higher boiling materials, it
base and a lipped top. The cylinder shall be marked to contain
shall be 50 mm in diameter.The flask support board shall be of
100 mL, and the 0 to 100 mLreceiver portion shall be not less
sufficient dimension to ensure that thermal heat to the flask
than 178 nor more than 203 mm in length. It shall be graduated
only comes from the central opening and that extraneous heat
in single millilitres and each fifth mark shall be distinguished
to the flask other than through the central opening is mini-
by a longer line. It shall be numbered from the bottom up at
mized. (Warning—Heat rsisitant-containing materials shall
intervals of 10 mL. The overall height of the receiver shall not
not be used in the construction of the flask support board.)
be less than 248 nor more than 260 mm. The graduations shall
6.5.3 For Units Using Bunsen Burner—The flask support
notbeinerrorbymorethan1mLatanypointonthescale.The
board is approximately 50 mm higher than the top of the
bottom 1-mL graduation may be omitted. The receiver com-
burner.
plies with Section 9, Graduate B Fig. 4, of Specification E133.
6.6 Heater:
6.4.2 Automatic Distillation Receiver—A receiver to be
used with measurements in accordance with the instrument 6.6.1 Manual Distillation Heater—An electric heater or a
manufacturer and conform to the physical specifications de- bunsen burner, fully adjustable and capable of giving sufficient
scribed in this section, with the exception of the graduations. heat to distill the product at the required rate. When a bunsen
6.4.2.1 Automatic Distillation Level Follower—For auto- burner is used, as described in 7.1 and Fig. 1 of Specification
matic apparatus, the level follower or recording mechanism of E133, the burner shall be adjusted so as to produce an entirely
theapparatuswillhavearesolutionof0.1mLwithanaccuracy blue flame. (Warning—Superheating of the flask can cause
of 61 mL. The calibration of the assembly should be con- erroneous results and is more likely to occur with electric
´1
D850–03 (2008)
heaters than with bunsen burners as heat sources.This problem 9.1.2 Assemble the apparatus. Mount the flask on the
is discussed in the section on Preparation of Apparatus in Test insulation board of appropriate dimensions, with the side tube
Method D1078.)
extending through a tightly fitting silicone or cork stopper
about 50 mm into the condenser tube.
7. Hazards
9.1.3 Support the distillation thermometer in the neck of the
7.1 Consult current OSHAregulations and supplier’s Mate-
flask by means of a cork or silicone stopper with the thermom-
rial Safety Data Sheets, and local regulations, for all materials
eter vertical and centered in the neck of the flask and in such
used in this test method.
a position that the top of the bulb (or top of contraction bulb if
present) is level with the lowest point of juncture between the
8. Sampling
side tube and the neck of the flask (see Fig. 3).
8.1 Sampling should follow safe rules in order to adhere to
9.1.4 Place the burner directly under the center of the hole
all safety precautions as outlined in the latest OSHA regula-
in the insulation board.
tions. Refer to Practice D3437 for proper sampling and
9.2 Automatic Distillation Apparatus—For assembly of au-
handling of aromatic hydrocarbons analyzed by this test
tomatic distillation apparatus, consult the instrument manufac-
method.
turer’s operating manual.
8.2 The sample under test shall be transparent and free of
separated water. Any separated water may ordinarily be elimi-
NOTE 2—The centering device must be as stated in 6.2.2.1 (Fig. 2).
nated by care in pouring the 100-mL specimen (10.1) into the
9.3 Carefullymeasurea100-mLspecimenofthematerialto
graduated cylinder. If necessary, any separated water or cloudi-
be tested in the 100-mL graduated cylinder at room tempera-
ness may be removed by filtration, in which case the following
ture and transfer to the distillation flask, dr
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
e1
Designation:D850–03(Reapproved2008)
Designation:D850–02
Standard Test Method for
Distillation of Industrial Aromatic Hydrocarbons and Related
Materials
This standard is issued under the fixed designation D 850; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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.
e NOTE—Research report was added editorially September 2002.
—Mercury warning was editorially added in June 2008.
1. Scope *
1.1 Thistestmethodcoversthedistillationofindustrialaromatichydrocarbonsandrelatedmaterialsofrelativelynarrowboiling
ranges from 30 to 250°C.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The following applies to all specified limits in this test method: for the purposes of determining conformance to this test
method, an observed or calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing
the specification limit, in accordance with the rounding-off method of Practice E 29.
1.4
1.4 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central
nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet
(MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware
that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements, 6.6.1and Section 7.
2. Referenced Documents
2.1 ASTM Standards:
D 1078 Test Method for Distillation Range of Volatile Organic Liquids
D 3437 Practice for Sampling and Handling Liquid Cyclic Products
D 4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
E 1 Specification for ASTM Liquid-in-Glass Thermometers
E 29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E 133 Specification for Distillation Equipment
E 220 Test Method for Calibration of Thermocouples byBy Comparison Techniques
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Document:
OSHA Regulations, 29CFRCFR, paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 Definitions:
This test method is under the jurisdiction ofASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.04 on Instrumental Analysis.
Current edition approved Feb. 10, 2002. Published April 2002. Originally published as D850–45. Last previous edition D850–00.
Current edition approved June 1, 2008. Published June 2008. Originally approved in 1945. Last previous edition approved in 2003 as D 850 – 03.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 06.04.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 14.03.
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.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D850–03 (2008)
D850–02
3.1.1 See Terminology D 4790 for definitions of terms used in this test method.
4. Summary of Test Method
4.1 The distillation of a 100-mL sample of industrial aromatic hydrocarbons and related materials is carried out via a carefully
controlled distillation wherein temperature readings are noted for the first drop of distillate and when 5, 10, and each additional
10 up to 90, and 95 % of the sample has distilled over. The temperature corresponding to the dry point is also noted.
5. Significance and Use
5.1 This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in development
or research work on industrial aromatic hydrocarbons 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 not
differentiate between products of similar boiling range.
6. Apparatus
6.1 Distillation Flask—Astandard 200-mLside-tube, heat-resistant glass distillation flask as shown in Fig. 1, conforming to the
following dimensions:
Diameter of bulb, outside, mm 76 6 1.5
Diameter of neck, inside, mm 21 6 1
Height of flask, outside, mm 179 6 3
Vertical distance from bottom of bulb outside to 120 6 3
bottom of vapor-tube opening in neck, mm
Length of side tube, mm 100 6 3
Diameter of side tube, outside, mm 7 6 0.5
Angle of side tube with vertical axis of bulb and 75 6 3
neck, °
The flask does not comply with Flask C of Specification E 133.
6.2 Temperature Measurement Devices :
6.2.1 Manual Distillation Thermometer— TheASTM Solvents Distillation Thermometer used in the test shall be as prescribed
in the specifications for the material being tested. If no thermometer is specified in the material specification, select one fromTable
1 with the smallest graduations that will cover the entire distillation range of the material being tested. Table 1 lists severalASTM
solventsdistillationthermometerswhicharesuitablefortestingindustrialaromatichydrocarbons,andwhichmeettherequirements
of Specification E 1.
6.2.2 Automatic Distillation Temperature Sensor—Temperature measurement systems using thermocouples or resistance
thermometers, otherwise referred to as the “temperature measuring devices,” must exhibit the same temperature lag and accuracy
as the equivalent mercury glass thermometer. Confirmation of the calibration of these temperature sensors is to be done at regular
intervals.ThismaybeaccomplishedasprescribedinTestMethodE 220,orsomesimilarmeansusingaprecisionresistancedecade
box. Another technique is to distill pure toluene and compare the temperature indicated by the thermocouple or resistance
thermometer with that shown by the thermometer. When installing a new automatic distillation analyzer, a toluene sample with
a known distillation range of approximately 1.0°C must be used to verify the dry point and distillation range. It is recommended
Annual Book of ASTM Standards, Vol 14.02.
FIG. 1 Distillation Flask
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D850–03 (2008)
D850–02
TABLE 1 ASTM Thermometers for Distillation Test of Industrial
Aromatic Hydrocarbons
ASTM
Ther- Subdivision,
Name Range, °C
mometer °C
No.
39C solvents distillation 48 to 102 0.2
40C solvents distillation 72 to 126 0.2
41C solvents distillation 98 to 152 0.2
42C solvents distillation 95 to 255 0.5
102C solvents distillation 123 to 177 0.2
103C solvents distillation 148 to 202 0.2
104C solvents distillation 173 to 227 0.2
105C solvents distillation 198 to 252 0.2
that such a material be used when replacing a temperature measuring device.Alternatively a material of known distillation range
and dry point may be used when replacing a temperature measuring device.
6.2.2.1 Automatic Distillation Temperature Sensor Centering Device—The temperature sensor shall be mounted through a
snug-fitting device designed to mechanically center the sensor in the neck of the flask. The use of a cork or silicone stopper with
a 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 electronic circuitry or algorithms, or both, used shall include the capability to simulate the temperature lag of a
mercury-in-glass thermometer. For that reason the known toluene sample with a distillation range of approximately 1.0°C must
be used to verify the algorithm and dampening software.
6.2.2.3 Alternatively, the sensor can also be placed in a casing with the tip of the sensor covered, so that the assembly, because
of its adjusted thermal mass and conductivity, has a temperature lag similar to that of a mercury-in-glass thermometer.
NOTE 1—In a region where the temperature is changing rapidly during the distillation, the temperature lag of a thermometer can be as much as
3s.
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 as specified in Section 5, and Fig. 1 of Specification E 133.
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 inside
diameter, of standard wall thickness (about 1.25 mm) with the exit end cut off square and ground flat. It shall be set in a cooling
Such a material is available from Spectrum Quality Standards.
FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck Flasks
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D850–03 (2008)
D850–02
trough so that at least 380 mm of the tube is in contact with the water. Clearance between the condenser tube and any parallel side
of the trough shall be not less than 19 mm. The water in the cooling trough shall be maintained at 10 to 20°C. This may be done
by adding ice to the water or by circulating chilled water through the trough. The trough shall be so mounted that the condenser
tube is set at an angle of 75° with the vertical.
6.3.2 Automatic Distillation and Cooling Bath—The automatic distillation and cooling bath shall be as specified in Section 5,
Fig. 2 of Specification E 133.
6.4 Distillation Receiver:
6.4.1 Manual Distillation Receiver —A graduate of the cylindrical type, of uniform diameter, with a pressed or molded base
and a lipped top. The cylinder shall be marked to contain 100 mL, and the 0 to 100 mLreceiver portion shall be not less than 178
nor more than 203 mm in length. It shall be graduated in single 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
nor more than 260 mm. The graduations shall not be in error by more than 1 mL at any point on the scale. The bottom 1-mL
graduation may be omitted. The receiver complies with Section 9, Graduate B Fig. 4, of Specification E 133.
6.4.2 Automatic Distillation Receiver —A receiver to be used with measurements in accordance with the instrument
manufacturer and conform to the physical specifications described in this section, with the exception of the graduations.
6.4.2.1 Automatic Distillation Level Follower—For automatic apparatus, the level follower or recording mechanism of the
apparatus will have a resolution of 0.1 mL with an accuracy of 61 mL. The calibration of the assembly should be confirmed
according to the manufacturer’s instructions at regular intervals. The typical calibration procedure involves verifying the output
with the receiver containing 5 and 100 mL of material respectively.
6.5 Support for Flask—A sheet of 3 to 6-mm hard insulation board approximately 152 mm square with a circular hole in the
center, supported on a circular metal shield enclosing the bunsen burner, and approximately 50 mm higher than the top of the
burner. For tests of benzene and toluene, the hole shall be 25 mm in diameter; for tests of materials boiling above toluene but
mostly below 145°C, the hole shall be 38 mm in diameter, and for higher boiling materials, it shall be 50 mm in diameter. Flask
Support Assembly:
6.5.1 For Units Using Electric Heaters— The assembly consists of an adjustable system onto which the electric heater is
mounted with provision for placement of a flask support board (see 6.5.2) above the electric heater. The whole assembly is
adjustable from the outside of the shield.
6.5.2 Flask Support Board—The flask support board shall be constructed of ceramic or other heat-resistant material with a
centrally located opening. For tests of benzene and toluene, the opening shall be 25 mm in diameter; for tests of materials boiling
above toluene but mostly below 145°C, the opening shall be 38 mm in diameter, and for higher boiling materials, it shall be 50
mm in diameter. The flask support board shall be of sufficient dimension to ensure that thermal heat to the flask only comes from
the central opening and that extraneous heat to the flask other than through the central opening is minimized. (Warning—Heat
rsisitant-containing materials shall not be used in the construction of the flask support board.)
6.5.3 For Units Using Bunsen Burner— The flask support board is approximately 50 mm higher than the top of the burner.
6.6 Heater:
6.6.1 Manual Distillation Heater—An electric heater or a bunsen burner, fully adjustable and capable of giving sufficient heat
to distill the product at the required rate. When a bunsen burner is used, as described in 7.1 and Fig. 1 of Specification E 133, the
burner shall be adjusted so as to produce an entirely blue flame. (Warning—Superheating of the flask can cause erroneous results
and is more likely to occur with electric heaters than with bunsen burners as heat sources. This problem is discussed in the section
on Preparation of Apparatus in Test Method D 1078.)
7. Hazards
7.1 Consult current OSHAregulations and supplier’s Material Safety Data Sheets, and local regulations, for all materials used
in this test method.
8. Sampling
8.1 Sampling should follow safe rules in order to adhere to all safety precautions as outlined in the latest OSHA regulations.
Refer to Practice D 3437 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 eliminated
by care in pouring the 100-mL
...
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