ASTM D1078-99

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 1078 – 99
Designation: 195/98
Standard Test Method for
Distillation Range of Volatile Organic Liquids
This standard is issued under the fixed designation D 1078; 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 (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 * sate leaves the condenser tube.
3.1.2 dry point—the temperature indicated at the instant the
1.1 This test method covers the determination of the distil-
last drop of liquid evaporates from the lowest point in the
lation range of liquids boiling between 30 and 350°C, that are
distillation flask, disregarding any liquid on the side of the
chemically stable during the distillation process, by manual or
flask.
automatic distillation procedures.
3.1.3 decomposition point—the thermometer reading that
1.2 This test method is applicable to organic liquids such as
coincides with the first indications of thermal decomposition of
hydrocarbons, oxygenated compounds, chemical intermedi-
the liquid in the flask.
ates, and blends thereof.
3.2 Definitions of Terms Specific to This Standard:
1.3 For hazard information and guidance, see the supplier’s
3.2.1 final boiling point—the maximum thermometer read-
Material Safety Data Sheet.
ing obtained during the test.
1.4 This standard does not purport to address all of the
3.2.1.1 Discussion—This usually occurs after the evapora-
safety concerns, if any, associated with its use. It is the
tion of all liquid from the bottom of the flask. The term
responsibility of the user of this standard to establish appro-
“maximum temperature” is a frequently used synonym.
priate safety and health practices and determine the applica-
3.2.2 end point 5 minutes—the thermometer reading ob-
bility of regulatory limitations prior to use. Specific hazard
tained 5 min after the 95 % distillation point if no dry or final
statements are given in Section 7.
boiling point occurs.
2. Referenced Documents
4. Summary of Test Method
2.1 ASTM Standards:
4.1 A 100-mL specimen is distilled under conditions equiva-
D 86 Test Method for Distillation of Petroleum Products at
lent to a simple batch differential distillation. The temperature
Atmospheric Pressure
of the mercury in the thermometer is equilibrated with that of
E 1 Specification for ASTM Thermometers
the refluxing liquid before the distillate is taken over. Boiling
E 133 Specification for Distillation Equipment
temperatures observed on a partial immersion thermometer are
E 299 Test Method for Trace Amounts of Peroxides in
corrected to standard atmospheric pressure to give true boiling
Organic Solvents
temperatures.
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
5. Significance and Use
3. Terminology 5.1 This test method provides a method of measurement of
distillation range of volatile organic liquids. The relative
3.1 Definitions:
volatility of organic liquids can be used with other tests for
3.1.1 initial boiling point—the temperature indicated by the
identification and measurement of quality. Therefore, this test
distillation thermometer at the instant the first drop of conden-
method provides a test procedure for assessing compliance
with a specification.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
5.2 This test method also provides an empirical value of
and Related Coatings, Materials, and Applications and is the direct responsibility of
residue, solvent recovery capacity, and loss (or non-recovery)
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
on heating. Organic liquids are used as solvents in many
Current edition approved July 10, 1999. Published September 1999. Originally
published as D 1078 – 49 T. Last previous edition D 1078 – 97.
chemical processes. As the relative volatility, residual matter
Annual Book of ASTM Standards, Vol 05.01.
and recovery capability affect the efficiency of these processes,
Annual Book of ASTM Standards, Vol 14.03.
this test method is useful in manufacturing control.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 15.05.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 1078
6. Apparatus and accuracy as the appropriate and calibrated mercury-in-
glass thermometer. Confirmation of the calibration of these
6.1 Distillation Apparatus—See Condenser and Cooling
temperature sensors shall be done at regular intervals. This can
Bath section, Figs. 1 and Figs. 2, and Metal Shield or Enclosure
be accomplished potentiometrically by the use of standard
for Flask section of Specification E 133.
precision resistance, depending on the type of probe. Another
6.2 Distillation Flasks, 200-mL of borosilicate glass com-
technique is to distill pure toluene (99.9 + % purity) and
plying with the specifications given in Distillation Flask
compare the temperature indicated by the thermocouple or
section, Fig. 3, and Flask C of Specification E 133.
resistance thermometer with that shown by the mercury-in-
NOTE 1—Liquid superheating in a new flask may be prevented by
glass thermometer.
depositing a small amount of carbon in the bottom of the flask. This may
be accomplished by heating and decomposing a pinch of tartaric acid in NOTE 2—Toluene is shown in reference manuals as boiling at 110.6°C
the bottom of the flask. The flask is then prepared for use by washing with (corrected for barometric pressure) under the conditions of a manual
water, rinsing with acetone, and drying. D 1078 distillation that uses a partial immersion thermometer.
6.3 Source of Heat—An adjustable gas burner or electric
7. Hazards
heater so constructed that sufficient heat can be obtained to
7.1 Precaution—Certain solvents and chemical intermedi-
distill the product at the uniform rate specified in Section 8. For
ates, particularly, but not only ethers and unsaturated com-
narrow-range (less than 2°C) liquids, an electric heater may be
pounds, may form peroxides during storage. These peroxides
used only if it has been proven to give results comparable to
may present a violent explosion hazard when the chemical is
those obtained when using gas heat. (See Section 9 for factors
distilled, especially as the dry point is approached. When
that cause superheating, and Appendix X1 for a discussion on
peroxide formation is likely because of chemical type or length
the use of electric heaters.)
of storage, the material should be analyzed for peroxides (See
6.4 Distillation Receiver:
Test Method E 299.) and if they exist in hazardous concentra-
6.4.1 Manual Distillation Receiver—A 100-mL cylinder
tions, appropriate precautions should be taken such as destroy-
graduated in 1 mL subdivision and having an overall height of
ing the peroxide before distillation, shielding, or destroying the
250 to 260 mm.
sample and not running the test.
6.4.2 Automatic Distillation Receiver—A receiver to be
7.2 Most organic solvents and chemical intermediates will
used with automatic distillation in accordance with the instru-
burn. In the operation of the distillation apparatus, use a
ment manufacturer’s instructions, conforming to the dimen-
suitable catch pan and shielding to contain spilled liquid in the
sions given in 6.4.1, with the exception of the graduations.
event of accidental breakage of the distillation flask.
6.4.2.1 Automatic Distillation Level Follower—The level
7.3 Provide adequate ventilation to maintain solvent vapor
follower/recording mechanism of the automatic apparatus shall
concentrations below the lower explosive limit in the immedi-
have a resolution of 0.1 mL with an accuracy of 6 1 mL.
ate vicinity of the distillation apparatus, and below the thresh-
6.5 Temperature Measurement Devices:
old limit value in the general work area.
6.5.1 Manual Distillation Thermometers—Partial immer-
8. Preparation of Apparatus
sion thermometers as listed in Table 1, conforming to Specifi-
cation E 1. Both bore corrections and either ice or steam 8.1 Manual Distillation Apparatus:
standardization corrections are recommended. 8.1.1 Clean and dry the condenser tube by swabbing with a
piece of soft lint-free cloth attached to a wire or cord, or by any
6.5.2 Automatic Distillation Temperature Sensors—
Temperature measurement systems using thermocouples or other suitable means.
resistance thermometers shall exhibit the same temperature lag 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 will
TABLE 1 Thermometers
cover the entire distillation range of the material. Center the
ASTM Sub-
thermometer into the neck of the flask through a tight-fitting
Thermometer IP Range, °C division,
cork stopper so that the upper end of the contraction chamber
Number °C
(or bulb if Thermometer 2C or IP thermometer 62C is used) is
A A
2C 62C −5 to + 300 1.0
A A B
3C 73C −5 to + 400 level with the lower side of the vapor tube at its junction with
14C . 38 to 82 0.1
the neck of the flask. (See Fig. 1 of Test Method D 86.)
37C 77C −2 to + 52 0.2
38C 78C 24 to 78 0.2
NOTE 3—It is far more important that the greatest volume of mercury
39C 79C 48 to 102 0.2
be immersed in the refluxing zone than that the immersion mark on the
40C 80C 72 to 126 0.2
thermometer be placed at any specific point.
41C 81C 98 to 152 0.2
A A
42C 82C 95 to 255 0.5
8.1.3 Position the correct heat shield (see 9.1.3.1 and
102C 83C 123 to 177 0.2
9.1.3.2).
103C 84C 148 to 202 0.2
104C 85C 173 to 227 0.2
NOTE 4—For low-boiling materials, cool the apparatus to room tem-
105C 86C 198 to 252 0.2
perature before starting the test.
106C 87C 223 to 277 0.2
107C 88C 248 to 302 0.2
8.1.4 Fill the condenser bath with water of the appropriate
A
These thermometers have more temperature lag than the other thermometers
temperature shown in Table 2.
listed herein and are not satisfactory for use with narrow-boiling range liquids.
B
1 to 301°C; 1.5°C above 301°C. NOTE 5—When distilling pure compounds always ensure that the
D 1078
TABLE 2 Temperatures
collection of the first drop of distillate within 15 min of the start
Initial Boiling Condenser, Sample, of heating.
Point,° C °C °C
9.1.4 Adjust the heat input so that the distillation proceeds at
Below 50 0 to 3 0 to 3
a rate of 4 to 5 mL/min (approximately 2 drops per second),
50 to 70 0to10 10to20
and move the receiving cylinder so that the tip of the condenser
70 to 150 25 to 30 20 to 30
tube touches one side of the cylinder after the first drop falls
Above 150 35 to 50 20 to 30
(initial boiling point). Record the readings of the distillation
thermometer after collecting 5, 10, 20, 30, 40, 50, 60, 70, 80,
90, and 95 mL of distillate.
condenser bath temperature is above the crystallizing point of the
9.1.5 Without changing the heater setting, continue distilla-
compound.
tion beyond the 95 % point until the dry point is observed.
8.1.5 Adjust the temperature of the appropriate portion of
Record the temperature at this point as the dry point (Section
the sample to the applicable temperature shown in Table 2.
3). If a dry point is not obtained (that is, if active decomposi-
8.2 Automatic Distillation Apparatus—For assembly of au-
tion should occur before the dry point is reached, as evidenced
tomatic distillation apparatus, consult instrument manufactur-
by a rapid evolution of vapor or heavy fumes; or if there is
er’s operating manual.
liquid remaining on the bottom of the flask when the maximum
temperature is observed on the distillation thermometer),
9. Procedure
record this fact.
9.1 Manual Distillation Procedure:
9.1.6 When a dry point cannot be obtained, report as the end
9.1.1 Using the graduated receiver measure 100 6 0.5 mL
point the maximum temperature observed on the distillation
of the temperature-adjusted sample. Remove the flask from the
thermometer or final boiling point (Section 3). When active
apparatus and transfer the fresh specimen directly to the flask,
decomposition is encountered, the rapid evolution of vapor and
allowing the graduate to drain for 15 to 20 s.
heavy fumes is usually followed by a gradual decrease in the
NOTE 6—For viscous liquids, a longer drainage period may be neces- distillation temperature. Record the temperature and report as
sary to complete the transfer of the specimen to the flask, but the drainage
the decomposition point (Section 3). If the expected drop in
time should not exceed 5 min. Do not allow any of the specimen to enter
temperature does not occur, record the maximum temperature
the vapor tube.
observed on the distillation thermometer 5 min after the 95 %
9.1.2 Connect the flask to the condenser by inserting the
point has been reached, and report as “end point, 5 min.” This
vapor tube of the flask into the condenser, making a tight
notation shows that a true end point could not be reached
connection with a well-rolled cork or similar material. Adjust
within the given time limit. In any event, the end point should
the position of the heat shield so that the neck of the flask is
not exceed 5 min after the 95 % point.
vertical and the vapor tube extends into the condenser tube a
9.1.7 Read and record the barometric pressure.
distance of 25 to 50 mm. Have the bottom of the flask resting
9.1.8 After the condenser tube has drained, read the total
firmly in the hole of the heat shield. Insert the thermometer as
volume of distillate and record it as recovery. The total yield of
described in 8.1.2. Place the receiver, without drying, at the
distillate from a material having a distillation range of 10°C or
outlet of the condenser tube in such a position that the
less should be not less than 97 % for nonviscous liquids. For
condenser tube extends into the graduate at least 25 mm but
viscous liquids and materials having a wider distillation range
does not extend below the 100-mL mark. If the initial boiling
than 10°C, a yield of 95 volume % is satisfactory. If yields are
point of the material is below 70°C, immerse the cylinder in a
not obtained within these limits, repeat the test.
transparent bath and maintain at a temperature of 10 to 20°C
9.1.9 If any residue is present, cool to room temperature and
throughout the distillation. Place a flat cover on the top of the
pour into a small cylinder graduated in 0.1-mL subdivisions.
graduate to prevent condensed moisture from entering the
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