ASTM D1078-11(2019)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:D1078 −11 (Reapproved 2019)
Designation:195⁄98
Standard Test Method for
Distillation Range of Volatile Organic Liquids
This standard is issued under the fixed designation D1078; 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 U.S. Department of Defense.
1. Scope responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.1 This test method covers the determination of the distil-
mine the applicability of regulatory limitations prior to use.
lation range of liquids boiling between 30 and 350 °C, that are
Specific hazard statements are given in Section 7.
chemically stable during the distillation process, by manual or
1.8 This international standard was developed in accor-
automatic distillation procedures.
dance with internationally recognized principles on standard-
1.2 This test method is applicable to organic liquids such as
ization established in the Decision on Principles for the
hydrocarbons, oxygenated compounds, chemical
Development of International Standards, Guides and Recom-
intermediates, and blends thereof.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
2. Referenced Documents
standard.
2.1 ASTM Standards:
1.4 For purposes of determining conformance of an ob-
D86 Test Method for Distillation of Petroleum Products and
served or a calculated value using this test method to relevant
Liquid Fuels at Atmospheric Pressure
specifications, test result(s) shall be rounded off “to the nearest
E1 Specification for ASTM Liquid-in-Glass Thermometers
unit” in the last right-hand digit used in expressing the
E29 Practice for Using Significant Digits in Test Data to
specification limit, in accordance with the rounding-off method
Determine Conformance with Specifications
of Practice E29.
E133 Specification for Distillation Equipment
1.5 For hazard information and guidance, see the supplier’s
E299 Test Method for Trace Amounts of Peroxides In
Material Safety Data Sheet.
Organic Solvents
1.6 Warning—Mercury has been designated by EPA and
2.2 ASTM Adjuncts:
many state agencies as a hazardous material that can cause
Determination of Precision and Bias for Use in Test
central nervous system, kidney, and liver damage. Mercury, or
Methods for Petroleum Products and Lubricants
its vapor, may be hazardous to health and corrosive to
materials. Caution should be taken when handling mercury and 3. Terminology
mercury-containing products. See the applicable product Ma-
3.1 Definitions:
terial Safety Data Sheet (MSDS) for details and EPA’s website
3.1.1 decomposition point, n—the thermometer reading that
(http://www.epa.gov/mercury/faq.htm) for additional informa-
coincideswiththefirstindicationsofthermaldecompositionof
tion. Users should be aware that selling mercury or mercury-
the liquid in the flask.
containingproducts,orboth,inyourstatemaybeprohibitedby
3.1.2 dry point, n—the temperature indicated at the instant
state law.
the last drop of liquid evaporates from the lowest point in the
1.7 This standard does not purport to address all of the
distillation flask, disregarding any liquid on the side of the
safety concerns, if any, associated with its use. It is the
flask.
1 2
This test method is under the jurisdiction of ASTM Committee D01 on Paint For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Related Coatings, Materials, andApplications and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2019. Published April 2019. Originally the ASTM website.
approved in 1949. Last previous edition approved in 2011 as D1078 – 11. DOI: Available from ASTM International Headquarters. Order Adjunct No.
10.1520/D1078-11R19. ADJD6300.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1078−11 (2019)
water, rinsing with acetone, and drying.
3.1.3 initial boiling point, n—the temperature indicated by
the distillation thermometer at the instant the first drop of
6.3 Source of Heat—An adjustable gas burner or electric
condensate leaves the condenser tube.
heater so constructed that sufficient heat can be obtained to
distilltheproductattheuniformratespecifiedinSection8.For
3.2 Definitions of Terms Specific to This Standard:
narrow-range (less than 2 °C) liquids, an electric heater may be
3.2.1 end point 5 minutes, n—the thermometer reading
used only if it has been proven to give results comparable to
obtained5minafterthe95 %distillationpointifnodryorfinal
those obtained when using gas heat. (See Section 9 for factors
boiling point occurs.
that cause superheating, and Appendix X1 for a discussion on
3.2.2 final boiling point, n—the maximum thermometer
the use of electric heaters.)
reading obtained during the test.
6.4 Distillation Receiver:
3.2.2.1 Discussion—This usually occurs after the evapora-
6.4.1 Manual Distillation Receiver—A 100-mL cylinder
tion of all liquid from the bottom of the flask. The term
graduatedin1-mLsubdivisionsandhavinganoverallheightof
“maximum temperature” is a frequently used synonym.
250 to 260 mm.
4. Summary of Test Method 6.4.2 Automatic Distillation Receiver—A receiver to be
used with automatic distillation in accordance with the instru-
4.1 A100-mLspecimenisdistilledunderconditionsequiva-
ment manufacturer’s instructions, conforming to the dimen-
lent to a simple batch differential distillation. The temperature
sions given in 6.4.1, with the exception of the graduations.
of the thermometer is equilibrated with that of the refluxing
6.4.2.1 Automatic Distillation Level Follower—The level
liquid before the distillate is taken over. Boiling temperatures
follower/recording mechanism of the automatic apparatus shall
observed on a partial immersion thermometer are corrected to
have a resolution of 0.1 mL with an accuracy of 61 mL.
standard atmospheric pressure to give true boiling tempera-
tures.
6.5 Temperature Measurement Devices:
6.5.1 Manual Distillation Thermometers—Partial immer-
5. Significance and Use
sion thermometers as listed in Table 1, conforming to Speci-
fication E1. Other liquid-in-glass thermometers or temperature
5.1 This test method provides a method of measurement of
measuring devices that provide equivalent range, accuracy, lag
distillation range of volatile organic liquids. The relative
time, and precision may be used. Both bore corrections and
volatility of organic liquids can be used with other tests for
either ice or steam standardization corrections are
identification and measurement of quality. Therefore, this test
recommended, as appropriate.
method provides a test procedure for assessing compliance
6.5.2 Automatic Distillation Temperature Sensors—
with a specification.
Temperature measurement systems using thermocouples or
5.2 This test method also provides an empirical value of
resistance thermometers shall exhibit the same temperature lag
residue, solvent recovery capacity, and loss (or non-recovery)
and accuracy as the appropriate and calibrated mercury-in-
on heating. Organic liquids are used as solvents in many
glass thermometer. Confirmation of the calibration of these
chemical processes. As the relative volatility, residual matter
temperature sensors shall be done at regular intervals. This can
and recovery capability affect the efficiency of these processes,
be accomplished potentiometrically by the use of standard
this test method is useful in manufacturing control.
precision resistance, depending on the type of probe. Another
technique is to distill pure toluene (99.9+ % purity) and
6. Apparatus
6.1 Distillation Apparatus—See Condenser and Cooling
Bath section, Apparatus Assembly Using Gas Burner figure,
TABLE 1 Thermometers
Apparatus Assembly Using Electric Heater figure, and Metal
Shield or Enclosure for Flask section of Specification E133.
ASTM Sub-
Thermometer IP Range, °C division,
6.1.1 Manual Distillation Apparatus—See Condenser Cool-
Number °C
ing Bath section, Apparatus Assembly Using Gas Burner
A A
2C 62C −5 to + 300 1.0
figure, Apparatus Assemble Using Electric Heater figure, and A A B
3C 73C −5 to + 400
Metal Shield or Enclosure for Flask section of Specification 14C . 38 to 82 0.1
37C 77C −2 to + 52 0.2
E133.
38C 78C 24 to 78 0.2
6.1.2 Automated Distillation Apparatus—Any automated
39C 79C 48 to 102 0.2
40C 80C 72 to 126 0.2
instrument that complies with 6.2 – 6.5, and is capable of
41C 81C 98 to 152 0.2
achieving the operating parameters given in 9.1.3 and 9.1.4,is
A A
42C 82C 95 to 255 0.5
acceptable.
102C 83C 123 to 177 0.2
103C 84C 148 to 202 0.2
6.2 Distillation Flasks, 200-mL of borosilicate glass com-
104C 85C 173 to 227 0.2
plying with the specifications given in Distillation Flask
105C 86C 198 to 252 0.2
106C 87C 223 to 277 0.2
section, Fig. 3, and Flask C of Specification E133.
107C 88C 248 to 302 0.2
NOTE 1—Liquid superheating in a new flask may be prevented by A
These thermometers have more temperature lag than the other thermometers
depositing a small amount of carbon in the bottom of the flask. This may
listed herein and are not satisfactory for use with narrow-boiling-range liquids.
B
be accomplished by heating and decomposing a pinch of tartaric acid in
1 to 301 °C; 1.5 °C above 301 °C.
the bottom of the flask.The flask is then prepared for use by washing with
D1078−11 (2019)
TABLE 2 Temperatures
compare the temperature indicated by the thermocouple or
resistance thermometer with that shown by the mercury-in- Initial Boiling Condenser, Sample,
Point,°C °C °C
glass thermometer.
Below 50 0to3 0to3
NOTE 2—Toluene is shown in reference manuals as boiling at 110.6 °C 50 to 70 0to10 10to20
70 to 150 25 to 30 20 to 30
(corrected for barometric pressure) under the conditions of a manual
Above 150 35 to 50 20 to 30
D1078 distillation that uses a partial immersion thermometer.
7. Hazards
8.1.5 Adjust the temperature of the appropriate portion of
7.1 Warning—Certain solvents and chemical
the sample to the applicable temperature shown in Table 2.
intermediates, particularly, but not only ethers and unsaturated
compounds, may form peroxides during storage. These perox-
8.2 Automatic Distillation Apparatus—For assembly of au-
ides may present a violent explosion hazard when the chemical
tomatic distillation apparatus, consult instrument manufactur-
is distilled, especially as the dry point is approached. When
er’s operating manual.
peroxide formation is likely because of chemical type or length
9. Procedure
of storage, the material should be analyzed for peroxides (see
Test Method E299) and if they exist in hazardous
9.1 Manual Distillation Procedure:
concentrations, appropriate precautions should be taken such
9.1.1 Using the graduated receiver, measure 100 6 0.5 mL
as destroying the peroxide before distillation, shielding, or
of the temperature-adjusted sample. Remove the flask from the
destroying the sample and not running the test.
apparatus and transfer the fresh specimen directly to the flask,
allowing the graduate to drain for 15 to 20 s.
7.2 Most organic solvents and chemical intermediates will
burn. In the operation of the distillation apparatus, use a
NOTE 6—For viscous liquids, a longer drainage period may be
suitable catch pan and shielding to contain spilled liquid in the
necessary to complete the transfer of the specimen to the flask, but the
drainage time should not exceed 5 min. Do not allow any of the specimen
event of accidental breakage of the distillation flask.
to enter the vapor tube.
7.3 Provide adequate ventilation to maintain solvent vapor
9.1.2 Connect the flask to the condenser by inserting the
concentrations below the lower explosive limit in the immedi-
vapor tube of the flask into the condenser, making a tight
ate vicinity of the distillation apparatus, and below the thresh-
connection with a well-rolled cork or similar material. Adjust
old limit value in the general work area.
the position of the heat shield so that the neck of the flask is
vertical and the vapor tube extends into the condenser tube a
8. Preparation of Apparatus
distance of 25 to 50 mm. Have the bottom of the flask resting
8.1 Manual Distillation Apparatus:
firmly in the hole of the heat shield. Insert the thermometer as
8.1.1 Clean and dry the condenser tube by swabbing with a
described in 8.1.2. Place the receiver, without drying, at the
pieceofsoftlint-freeclothattachedtoawireorcord,orbyany
outlet of the condenser tube in such a position that the
other suitable means.
condenser tube extends into the graduate at least 25 mm but
8.1.2 Use the thermometer listed in the material specifica-
does not extend below the 100-mL mark. If the initial boiling
tionfortheproductunderstudy.Ifnothermometerisspecified,
point of the material is below 70 °C, immerse the cylinder in a
select one from Table 1 with the smallest graduations that will
transparent bath and maintain at a temperature of 10 to 20 °C
covertheentiredistillationrangeofthematerial.Preferably,an
throughout the distillation. Place a flat cover on the top of the
equivalent non-mercury thermometer should be used if avail-
graduate to prevent condensed moisture from entering the
able. Center the thermometer into the neck of the flask through
graduate.
a tight-fitting cork stopper so that the upper end of the
9.1.3 Acertainamountofjudgmentisnecessaryinchoosing
contraction chamber (or bulb if Thermometer 2C or IP ther-
the best operating conditions to get acceptable accuracy and
mometer 62C is used) is level with the lower side of the vapor
precision for materials having different distilling temperatures.
tube at its junction with the neck of the flask. (See Apparatus
As a general guide, it is recommended that:
Assembly Using Gas Burner figure of Test Method D86.)
9.1.3.1 For materials having an initial boiling point below
150 °C, the following conditions be established:
NOTE 3—It is far more important that the bulb and contraction chamber
(a) Heat Shield—Hole size, 32-mm diameter.
be immersed in the refluxing zone than that the immersion mark on the
thermometer be placed at any specific point. (b) Heating Rate—Time from application of heat to first
drop of distillate, 5 to 10 min, and time of rise of vapor column
8.1.3 Position the correct heat shield (see 9.1.3.1 and
1 1
in neck of flask to side arm, 2 ⁄2 to 3 ⁄2 min.
9.1.3.2).
9.1.3.2 For materials having an initial boiling point above
NOTE 4—For low-boiling materials, cool the apparatus to room tem-
150 °C, the following conditions should be established:
perature before starting the test.
(a) Heat Shield—Hole size, 38-mm diameter.
8.1.4 Fill the condenser bath with water of the appropriate
(b) Heating Rate—Time from application of heat to first
temperature shown in Table 2.
drop of distillate, 10 to 15 min, and time of rise of vapor
column in neck of flask to side arm, sufficiently rapid to permit
NOTE 5—When distilling pure compounds, always ensure that the
collectionofthefirstdropofdistillatewithin15minofthestart
condenser bath temperature is above the crystallizing point of the
compound. of heating.
D1078−11 (2019)
9.1.4 Adjusttheheatinputsothatthedistillationproceedsat 10. Factors Causing Superheating
a rate of 4 to 5 mL/min (approximately 2 drops per second),
10.1 In general, any condition whereby the temperature
andmovethereceivingcylindersothatthetipofthecondenser
surrounding the vapor exceeds the temperature of the vapor in
tube touches one side of the cylinder after the first drop falls
equilibrium with the liquid will cause superheating. Specific
(initial boiling point). Record the readings of the distillation
factorsconducivetosuperheatingareasfollows,andshouldbe
thermometer after collecting 5, 10, 20, 30, 40, 50, 60, 70, 80,
avoided:
90, and 95 mL of distillate.
10.2 Flame in Contact With the Flask—The applied gas
9.1.5 Without changing the heater setting, continue distilla-
flame should be prevented from contacting more than the
tion beyond the 95 % point until the dry point is observed.
specified portion of the flask by the following procedures:
Record the temperature at this point as the dry point (Section
10.2.1 Maintain the correct overall dimensions and speci-
3). If a dry point is not obtained (that is, if active decomposi-
fied hole diameter of the heat resistant board.The hole must be
tion should occur before the dry point is reached, as evidenced
perfectly circular, with no irregularities.
by a rapid evolution of vapor or heavy fumes; or if there is
10.2.2 Use a board that is free of cracks and checks.
liquidremainingonthebottomoftheflaskwhenthemaximum
10.2.3 Settheflasksnuglyintheholeintheupperinsulating
temperature is observed on the distillation thermometer),
board.
record this fact.
10.3 Application of Heat—Attention should be given to
9.1.6 Whenadrypointcannotbeobtained,reportastheend
burner placement, position, and character of flame, as follows:
point the maximum temperature observed on the distillation
10.3.1 Apply the source of heat directly beneath the flask.
thermometer or final boiling point (Section 3). When active
Any variation would result in heating a larger portion of
decomposition is encountered, the rapid evolution of vapor and
surrounding air to a higher temperature than that of the flask.
heavy fumes is usually followed by a gradual decrease in the
10.3.2 The flame should not have a larger cross section than
distillation temperature. Record the temperature and report as
is necessary, and should be nonluminous.
the decomposition point (Section 3). If the expected drop in
10.3.3 Place the burner at a level such that the complete
temperature does not occur, record the maximum temperature
combustion area of a nonluminous flame is approximately ⁄4
observed on the distillation thermometer 5 min after the 95 %
in. (20 mm) below the board.
point has been reached, and report as “end point, 5 min.” This
notation shows that a true end point could not be reached
10.4 Extraneous Heat Source—An extraneous source of
within the given time limit. In any event, the end point should
heat, such as sunlight falling directly on the flask, can cause
not exceed 5 min after the 95 % point.
superheating.
9.1.7 Read and record the barometric pressure.
10.5 Condition of Equipment—Observe caution in employ-
9.1.8 After the condenser tube has drained, read the total
ing the apparatus for immediate reuse. For low-boiling
volume of distillate and record it as recovery.The total yield of
materials, cool the heating unit to room temperature before
distillate from a material having a distillation range of 10 °C or
starting the test.
less should be not less than 97 % for nonviscous liquids. For
10.6 Use of Electric Heaters—Electric heaters generally
viscous liquids and materials having a wider distillation range
cause superheating. These should be used only after they have
than 10 °C, a yield of 95 volume % is satisfactory. If yields are
been proven to give results comparable to those obtained when
not obtained within these limits, repeat the test.
using gas heat. The superheating effect obtained from electric
9.1.9 Ifanyresidueispresent,cooltoroomtemperatureand
heaters may be minimized, but not completely eliminated, by
pour into a s
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