D86-16a Distillation of Petroleum Products at Atmospheric Pressure

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Designation: D86 − 16a
Standard Test Method for

Distillation of Petroleum Products and Liquid Fuels at
Atmospheric Pressure1
This standard is issued under the fixed designation D86; 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* its vapor, may be hazardous to health and corrosive to

1.1 This test method covers the atmospheric distillation of materials. Caution should be taken when handling mercury and
petroleum products and liquid fuels using a laboratory batch mercury containing products. See the applicable product Ma-
distillation unit to determine quantitatively the boiling range terial Safety Data Sheet (MSDS) for details and EPA’s
characteristics of such products as light and middle distillates, website—http://www.epa.gov/mercury/faq.htm—for addi-
automotive spark-ignition engine fuels with or without oxy- tional information. Users should be aware that selling mercury
genates (see Note 1), aviation gasolines, aviation turbine fuels, and/or mercury containing products into your state or country
diesel fuels, biodiesel blends up to 20 %, marine fuels, special may be prohibited by law.
petroleum spirits, naphthas, white spirits, kerosines, and
1.6 This standard does not purport to address all of the
Grades 1 and 2 burner fuels.
safety concerns, if any, associated with its use. It is the
NOTE 1—An interlaboratory study was conducted in 2008 involving 11 responsibility of the user of this standard to establish appro-
different laboratories submitting 15 data sets and 15 different samples of priate safety and health practices and determine the applica-
ethanol-fuel blends containing 25 % volume, 50 % volume, and 75 %
volume ethanol. The results indicate that the repeatability limits of these bility of regulatory limitations prior to use.
samples are comparable or within the published repeatability of the
method (with the exception of FBP of 75 % ethanol-fuel blends). On this 2. Referenced Documents
basis, it can be concluded that Test Method D86 is applicable to
ethanol-fuel blends such as Ed75 and Ed85 (Specification D5798) or other 2.1 All standards are subject to revision, and parties to
ethanol-fuel blends with greater than 10 % volume ethanol. See ASTM agreement on this test method are to apply the most recent
RR:D02-1694 for supporting data.2
edition of the standards indicated below, unless otherwise
1.2 The test method is designed for the analysis of distillate specified, such as in contractual agreements or regulatory rules
fuels; it is not applicable to products containing appreciable where earlier versions of the method(s) identified may be
quantities of residual material. required.
1.3 This test method covers both manual and automated
instruments. 2.2 ASTM Standards:3
D97 Test Method for Pour Point of Petroleum Products
1.4 Unless otherwise noted, the values stated in SI units are D323 Test Method for Vapor Pressure of Petroleum Products
to be regarded as the standard. The values given in parentheses (Reid Method)
are provided for information only. D4057 Practice for Manual Sampling of Petroleum and
1.5 WARNING—Mercury has been designated by many Petroleum Products
regulatory agencies as a hazardous material that can cause D4175 Terminology Relating to Petroleum Products, Liquid
central nervous system, kidney and liver damage. Mercury, or Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1
This test method is under the jurisdiction of ASTM Committee D02 on D4953 Test Method for Vapor Pressure of Gasoline and
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.08 on Volatility. Gasoline-Oxygenate Blends (Dry Method)
In the IP, the equivalent test method is published under the designation IP 123.
It is under the jurisdiction of the Standardization Committee.
Current edition approved Aug. 1, 2016. Published August 2016. Originally
3
approved in 1921. Last previous edition approved in 2016 as D86 – 16. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D0086-16A. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
2
Supporting data have been filed at ASTM International Headquarters and may Standards volume information, refer to the standard’s Document Summary page on
be obtained by requesting Research Report RR:D02-1694. the ASTM website.
*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
1
D86 − 16a
D5190 Test Method for Vapor Pressure of Petroleum Prod- a lower temperature than the immersed portion, resulting in a
ucts (Automatic Method) (Withdrawn 2012)4 shrinkage of the mercury thread and a lower temperature
D5191 Test Method for Vapor Pressure of Petroleum Prod- reading.
ucts (Mini Method) 3.1.6 end point (EP) or final boiling point (FBP), n—the
D5798 Specification for Ethanol Fuel Blends for Flexible- maximum corrected thermometer reading obtained during the
Fuel Automotive Spark-Ignition Engines test.
D5842 Practice for Sampling and Handling of Fuels for
3.1.6.1 Discussion—This usually occurs after the evapora-
Volatility Measurement
tion of all liquid from the bottom of the flask. The term
D5949 Test Method for Pour Point of Petroleum Products
maximum temperature is a frequently used synonym.
(Automatic Pressure Pulsing Method)
D5950 Test Method for Pour Point of Petroleum Products 3.1.7 front end loss, n—loss due to evaporation during
(Automatic Tilt Method) transfer from receiving cylinder to distillation flask, vapor loss
D5985 Test Method for Pour Point of Petroleum Products during the distillation, and uncondensed vapor in the flask at
(Rotational Method) the end of the distillation.
D6300 Practice for Determination of Precision and Bias 3.1.8 fuel ethanol (Ed75-Ed85), n—blend of ethanol and
Data for Use in Test Methods for Petroleum Products and hydrocarbon of which the ethanol portion is nominally 75 % to
Lubricants 85 % by volume denatured fuel ethanol. D4175
D6708 Practice for Statistical Assessment and Improvement
of Expected Agreement Between Two Test Methods that 3.1.9 initial boiling point (IBP), n—in D86 distillation, the
Purport to Measure the Same Property of a Material corrected temperature reading at the instant the first drop of
E1 Specification for ASTM Liquid-in-Glass Thermometers condensate falls from the lower end of the condenser tube.
E77 Test Method for Inspection and Verification of Ther- 3.1.10 percent evaporated, n—in distillation, the sum of the
mometers percent recovered and the percent loss.
E1272 Specification for Laboratory Glass Graduated Cylin- 3.1.10.1 percent loss, n— in distillation, one hundred minus
ders the percent total recovery.
E1405 Specification for Laboratory Glass Distillation Flasks
2.3 Energy Institute Standards:5 3.1.10.2 corrected loss, n—percent loss corrected for baro-
IP 69 Determination of Vapour Pressure—Reid Method metric pressure.
IP 123 Petroleum Products—Determination of Distillation 3.1.11 percent recovered, n—in distillation, the volume of
Characteristics condensate collected relative to the sample charge.
IP 394 Determination of Air Saturated Vapour Pressure
3.1.11.1 percent recovery, n—in distillation, maximum per-
IP Standard Methods for Analysis and Testing of Petroleum
cent recovered relative to the sample charge.
and Related Products 1996—Appendix A
3.1.11.2 corrected percent recovery, n—in distillation, the
3. Terminology percent recovery, adjusted for the corrected percent loss.
3.1 Definitions: 3.1.11.3 percent total recovery, n—in distillation, the com-
3.1.1 decomposition, n—of a hydrocarbon, the pyrolysis or bined percent recovery and percent residue.
cracking of a molecule yielding smaller molecules with lower
3.1.12 percent residue, n—in distillation, the volume of
boiling points than the original molecule.
residue relative to the sample charge.
3.1.2 decomposition point, n—in distillation, the corrected
temperature reading that coincides with the first indications of 3.1.13 rate of change (or slope), n—the change in tempera-
thermal decomposition of the specimen. ture reading per percent evaporated or recovered, as described
in 13.2.
3.1.3 dry point, n—in distillation, the corrected temperature
reading at the instant the last drop of liquid evaporates from the 3.1.14 sample charge, n—the amount of sample used in a
lowest point in the flask. test.
3.1.4 dynamic holdup, n—in D86 distillation, the amount of 3.1.15 temperature lag, n—the offset between the tempera-
material present in the neck of the flask, in the sidearm of the ture reading obtained by a temperature sensing device and the
flask, and in the condenser tube during the distillation. true temperature at that time.
3.1.5 emergent stem effect, n—the offset in temperature 3.1.16 temperature measurement device, n—a thermometer,
reading caused by the use of total immersion mercury-in-glass as described in 6.3.1, or a temperature sensor, as described in
thermometers in the partial immersion mode. 6.3.2.
3.1.5.1 Discussion—In the partial immersion mode, a por- 3.1.16.1 temperature reading, n—the temperature obtained
tion of the mercury thread, that is, the emergent portion, is at by a temperature measuring device or system that is equal to
the thermometer reading described in 3.1.16.3.
4
The last approved version of this historical standard is referenced on
3.1.16.2 corrected temperature reading, n—the temperature
www.astm.org.
5
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, reading, as described in 3.1.16.1, corrected for barometric
U.K., http://www.energyinst.org.uk. pressure.
2
D86 − 16a
3.1.16.3 thermometer reading (or thermometer result),
n—the temperature of the saturated vapor measured in the neck
of the flask below the vapor tube, as determined by the
prescribed thermometer under the conditions of the test.
3.1.16.4 corrected thermometer reading, n—the thermom-
eter reading, as described in 3.1.16.3, corrected for barometric
pressure.
4. Summary of Test Method
4.1 Based on its composition, vapor pressure, expected IBP
or expected EP, or combination thereof, the sample is placed in
one of four groups. Apparatus arrangement, condenser
temperature, and other operational variables are defined by the
group in which the sample falls.
4.2 A 100 mL specimen of the sample is distilled under
prescribed conditions for the group in which the sample falls.
The distillation is performed in a laboratory batch distillation
unit at ambient pressure under conditions that are designed to
provide approximately one theoretical plate fractionation. Sys-
tematic observations of temperature readings and volumes of
condensate are made, depending on the needs of the user of the
data. The volume of the residue and the losses are also
recorded.
4.3 At the conclusion of the distillation, the observed vapor FIG. 1 Apparatus Assembly Using Gas Burner
temperatures can be corrected for barometric pressure and the
data are examined for conformance to procedural
requirements, such as distillation rates. The test is repeated if
any specified condition has not been met. 5.4 Volatility, as it affects rate of evaporation, is an impor-
tant factor in the application of many solvents, particularly
4.4 Test results are commonly expressed as percent evapo- those used in paints.
rated or percent recovered versus corresponding temperature,
either in a table or graphically, as a plot of the distillation 5.5 Distillation limits are often included in petroleum prod-
curve. uct specifications, in commercial contract agreements, process
refinery/control applications, and for compliance to regulatory
5. Significance and Use rules.
5.1 The basic test method of determining the boiling range
of a petroleum product by performing a simple batch distilla- 6. Apparatus
tion has been in use as long as the petroleum industry has 6.1 Basic Components of the Apparatus:
existed. It is one of the oldest test methods under the jurisdic- 6.1.1 The basic components of the distillation unit are the
tion of ASTM Committee D02, dating from the time when it distillation flask, the condenser and associated cooling bath, a
was still referred to as the Engler distillation. Since the test metal shield or enclosure for the distillation flask, the heat
method has been in use for such an extended period, a source, the flask support, the temperature measuring device,
tremendous number of historical data bases exist for estimating and the receiving cylinder to collect the distillate.
end-use sensitivity on products and processes. 6.1.2 Figs. 1 and 2 are examples of manual distillation units.
5.2 The distillation (volatility) characteristics of hydrocar- 6.1.3 In addition to the basic components described in 6.1.1,
bons have an important effect on their safety and performance, automated units also are equipped with a system to measure
especially in the case of fuels and solvents. The boiling range and automatically record the temperature and the associated
gives information on the composition, the properties, and the recovered volume in the receiving cylinder.
behavior of the fuel during storage and use. Volatility is the 6.2 A detailed description of the apparatus is given in Annex
major determinant of the tendency of a hydrocarbon mixture to A2.
produce potentially explosive vapors. 6.3 Temperature Measuring Device:
5.3 The distillation characteristics are critically important 6.3.1 Mercury-in-glass thermometers, if used, shall be filled
for both automotive and aviation gasolines, affecting starting, with an inert gas, graduated on the stem and enamel backed.
warm-up, and tendency to vapor lock at high operating They shall conform to Specification E1 or IP Standard Methods
temperature or at high altitude, or both. The presence of high for Analysis and Testing of Petroleum and Related Products
boiling point components in these and other fuels can signifi- 1996—Appendix A, or both, for thermometers ASTM 7C/IP
cantly affect the degree of formation of solid combustion 5C and ASTM 7F for the low range thermometers, and ASTM
deposits. 8C/IP 6C and ASTM 8F for the high range thermometers.
3
D86 − 16a
1–Condenser bath 11–Distillation flask

2–Bath cover 12–Temperature sensor
3–Bath temperature sensor 13–Flask support board
4–Bath overflow 14–Flask support platform
5–Bath drain 15–Ground connection
6–Condenser tube 16–Electric heater
7–Shield 17–Knob for adjusting level
8–Viewing window of support platform
9a–Voltage regulator 18–Power source cord
9b–Voltmeter or ammeter 19–Receiver cylinder
9c–Power switch 20–Receiver cooling bath
9d–Power light indicator 21–Receiver cover
10–Vent
FIG. 2 Apparatus Assembly Using Electric Heater
4
D86 − 16a
FIG. 3 PTFE Centering Device for Ground Glass Joint
6.3.1.1 Thermometers that have been exposed for an ex-

tended period above an observed temperature of 370 °C shall
not be reused without a verification of the ice point or checked
as prescribed in Specification E1 and Test Method E77.
NOTE 2—At an observed thermometer reading of 370 °C, the tempera-
ture of the bulb is approaching a critical range in the glass and the
thermometer may lose its calibration.
6.3.2 Temperature measurement systems other than those
described in 6.3.1 are satisfactory for this test method, pro- FIG. 4 Example of Centering Device Designs for Straight-Bore
vided that they exhibit the same temperature lag, emergent Neck Flasks
stem effect, and accuracy as the equivalent mercury-in-glass
thermometer.
6.3.2.1 The electronic circuitry or the algorithms, or both,
used shall include the capability to simulate the temperature lag
of a mercury-in-glass thermometer.
6.3.2.2 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 time similar to that of a mercury-in-glass
thermometer.
NOTE 3—In a region where the temperature is changing rapidly during
the distillation, the temperature lag of a thermometer can be as much as 3
s.
6.3.3 In case of dispute, the referee test method shall be
carried out with the specified mercury-in-glass thermometer. FIG. 5 Position of Thermometer in Distillation Flask
6.4 Temperature Sensor Centering Device:
6.4.1 The temperature sensor shall be mounted through a 6.5 Automated equipment manufactured in 1999 and later
snug-fitting device designed for mechanically centering the shall be equipped with a device to automatically shut down
sensor in the neck of the flask without vapor leakage. Examples power to the unit and to spray an inert gas or vapor in the
of acceptable centering devices are shown in Figs. 3 and 4. chamber where the distillation flask is mounted in the event of
(Warning—The use of a plain stopper with a hole drilled fire.
through the center is not acceptable for the purpose described
NOTE 6—Some causes of fires are breakage of the distillation flask,
in 6.4.1.) electrical shorts, and foaming and spilling of liquid sample through the top
NOTE 4—Other centering devices are also acceptable, as long as they opening of the flask.
position and hold the temperature sensing device in the proper position in 6.6 Barometer—A pressure measuring device capable of
the neck of the distillation column, as shown in Fig. 5 and described in measuring local station pressure with an accuracy of 0.1 kPa
10.5.
NOTE 5—When running the test by the manual method, products with (1 mm Hg) or better, at the same elevation relative to sea level
a low IBP may have one or more readings obscured by the centering as the apparatus in the laboratory. (Warning—Do not take
device. See also 10.14.3.1. readings from ordinary aneroid barometers, such as those used
5
D86 − 16a
TABLE 1 Group Characteristics provided the operator ensures that the sample container is tightly closed
Group 1 Group 2 Group 3 Group 4 and leak-free.
Sample 7.3.4 Groups 3 and 4—Store the sample at ambient or lower
characteristics temperature.
Distillate type
Vapor pressure at 7.4 Sample Conditioning Prior to Analysis:
37.8 °C, kPa $65.5 <65.5 <65.5 <65.5
100 °F, psi $9.5 <9.5 <9.5 <9.5 7.4.1 Samples shall be conditioned to the temperature
(Test Methods D323, D4953, D5190, D5191, shown in Table 2 before opening the sample container.
D5842, IP 69 or IP 394) 7.4.1.1 Groups 1 and 2—Samples shall be conditioned to a
Distillation, IBP °C #100 >100
°F #212 >212 temperature of less than 10 °C (50 °F) before opening the
EP °C #250 #250 >250 >250 sample container, except when the sample is to be immediately
°F #482 #482 >482 >482 tested and is already at the prescribed sample temperature in
Table 3.
7.4.1.2 Groups 3 and 4—If the sample is not fluid at ambient
temperature, it is to be heated to a temperature of 9 °C to 21 °C
at weather stations and airports, since these are precorrected to above its pour point (Test Method D97, D5949, or D5985)
give sea level readings.) prior to analysis. If the sample has partially or completely
solidified during storage, it shall be vigorously shaken after
7. Sampling, Storage, and Sample Conditioning melting prior to opening the sample container to ensure
7.1 Determine the Group characteristics that correspond to homogeneity.
the sample to be tested (see Table 1). Where the procedure is 7.4.1.3 If the sample is not fluid at room temperature, the
dependent upon the group, the section headings will be so temperature ranges shown in Table 2 for the flask and for the
marked. sample do not apply.
7.2 Sampling: 7.5 Wet Samples:
7.2.1 Sampling shall be done in accordance with Practice 7.5.1 Samples of materials that visibly contain water are not
D4057 or D4177 and as described in Table 2. suitable for testing. If the sample is not dry, obtain another
7.2.1.1 Group 1—Condition the sample container to below sample that is free from suspended water.
10°C, preferably by filling the bottle with the cold liquid 7.5.2 Groups 1 and 2—If such a sample cannot be obtained,
sample and discarding the first sample. If this is not possible the suspended water can be removed by maintaining the
because, for instance, the product to be sampled is at ambient sample at 0 °C to 10 °C, adding approximately 10 g of anhy-
temperature, the sample shall be drawn into a bottle prechilled drous sodium sulfate per 100 mL of sample, shaking the
to below 10 °C, in such a manner that agitation is kept at a mixture for approximately 2 min, and then allowing the mix-
minimum. Close the bottle immediately with a tight-fitting ture to settle for approximately 15 min. Once the sample shows
closure. (Warning—Do not completely fill and tightly seal a no visible signs of water, use a decanted portion of the sample,
cold bottle of sample because of the likelihood of breakage on maintained between 1 °C and 10 °C, for the analysis. Note in
warming.) the report that the sample has been dried by the addition of a
7.2.1.2 Groups 2, 3, and 4—Collect the sample at ambient desiccant.
temperature. After sampling, close the sample bottle immedi- NOTE 9—Suspended water in hazy samples in Groups 1 and 2 can be
ately with a tight-fitting closure. removed by the addition of anhydrous sodium sulfate and separating the
7.2.1.3 If the sample received by the testing laboratory has liquid sample from the drying agent by decanting without statistically
been sampled by others and it is not known whether sampling affecting the results of the test.6
has been performed as described in 7.2, the sample shall be 7.5.3 Groups 3 and 4—In cases in which a water-free
assumed to have been so sampled. sample is not practical, the suspended water can be removed by
7.3 Sample Storage: shaking the sample with anhydrous sodium sulfate or other
7.3.1 If testing is not to start immediately after collection, suitable drying agent and separating it from the drying agent by
store the samples as indicated in 7.3.2, 7.3.3, and Table 2. All decanting. Note in the report that the sample has been dried by
samples shall be stored away from direct sunlight or sources of the addition of a desiccant.
direct heat.
7.3.2 Group 1—Store the sample at a temperature below 8. Preparation of Apparatus
10 °C. 8.1 Refer to Table 3 and prepare the apparatus by choosing
NOTE 7—If there are no, or inadequate, facilities for storage below the appropriate distillation flask, temperature measuring
10°C, the sample may also be stored at a temperature below 20 °C, device, and flask support board, as directed for the indicated
provided the operator ensures that the sample container is tightly closed group. Bring the temperature of the receiving cylinder, the
and leak-free. flask, and the condenser bath to the indicated temperature.
7.3.3 Group 2—Store the sample at a temperature below
10 °C.
NOTE 8—If there are no, or inadequate, facilities for storage below 6
Supporting data have been filed at ASTM International Headquarters and may
10°C, the sample may also be stored at a temperature below 20 °C, be obtained by requesting Research Report RR:D02-1455.
6
D86 − 16a
TABLE 2 Sampling, Storage, and Sample Conditioning
Group 1 Group 2 Group 3 Group 4
Temperature of sample bottle °C <10
°F <50
Temperature of stored sample °C <10A <10 ambient ambient
°F <50A <50 ambient ambient
Temperature of sample after °C <10B <10B Ambient or Ambient or
conditioning prior to analysis 9 °C to 21 °C above pour pointC
°F <50 <50 Ambient or Ambient or
48 °F to 70 °F above pour pointC
If sample is wet resample resample dry in accordance with 7.5.3
If resample is still wetD dry in accordance with 7.5.2
A
Under certain circumstances, samples can also be stored at temperatures below 20 °C (68 °F). See also 7.3.2 and 7.3.3.
B
If sample is to be immediately tested and is already at the temperature prescribed in Table 3, see 7.4.1.1.
C
If sample is (semi)-solid at ambient temperature, see also 10.3.1.1.
D
If sample is known to be wet, resampling may be omitted. Dry sample in accordance with 7.5.2 and 7.5.3.
TABLE 3 Preparation of Apparatus and Specimen

Flask, mL 125 125 125 125
ASTM distillation thermometer 7C (7F) 7C (7F) 7C (7F) 8C (8F)
IP distillation thermometer range low low low high
Flask support board B B C C
diameter of hole, mm 38 38 50 50
Temperature at start of test
Flask °C 13–18 13–18 13–18 not above
°F 55–65 55–65 55–65 ambient
Flask support and shield not above not above not above
ambient ambient ambient
Receiving cylinder and sample
°C 13–18 13–18 13–18A 13–ambientA
°F 55–65 55–65 55–65A 55–ambientA
A
See 10.3.1.1 for exceptions.
8.2 Make any necessary provisions so that the temperature forming this verification, no algorithms shall be used to correct
of the condenser bath and the receiving cylinder will be the temperature for lag and the emergent stem effect (see
maintained at the required temperatures. The receiving cylin- manufacturer’s instructions).
der shall be in a bath such that either the liquid level is at least 9.1.2 Verification of the calibration of temperature measur-
as high as the 100 mL mark or the entire receiving cylinder is ing devices shall be conducted by distilling toluene in accor-
surrounded by an air circulation chamber. dance with Group 1 of this test method and comparing the
8.2.1 Groups 1, 2, and 3—Suitable media for low tempera- 50 % recovered temperature with that shown in Table 4.7
ture baths include, but are not limited to, chopped ice and 9.1.2.1 If the temperature reading is not within the values
water, refrigerated brine, and refrigerated ethylene glycol. shown in Table 4 for the respective apparatus being used (see
8.2.2 Group 4—Suitable media for ambient and higher bath Note 11 and Table 4), the temperature measurement system
temperatures include, but are not limited to, cold water, hot shall be considered defective and shall not be used for the test.
water, and heated ethylene glycol. NOTE 10—Toluene is used as a verification fluid for calibration; it will
8.3 Remove any residual liquid in the condenser tube by yield almost no information on how well an electronic measurement
swabbing with a piece of soft, lint-free cloth attached to a cord system simulates the temperature lag of a liquid-in-glass thermometer.
or wire. 9.1.2.2 Reagent grade toluene and hexadecane (cetane),
conforming to the specifications of the Committee on Analyti-
9. Calibration and Standardization cal Reagents of the American Chemical Society,8 shall be used.
9.1 Temperature Measurement System—Temperature mea- However, other grades may also be used, provided it is first
surement systems using other than the specified mercury-in- ascertained that the reagent is of sufficient purity to permit its
glass thermometers shall exhibit the same temperature lag, use without lessening the accuracy of the determination.
emergent stem effect, and accuracy as the equivalent mercury-
in-glass thermometer. Confirmation of the calibration of these 7
temperature measuring systems shall be made at intervals of be obtained by requesting Research Report RR:D02-1580.
not more than six months, and after the system has been 8
Reagent Chemicals, American Chemical Society Specifications, American
replaced or repaired. Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
9.1.1 The accuracy and the calibration of the electronic
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
circuitry or computer algorithms, or both, shall be verified by and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the use of a standard precision resistance bench. When per- MD.
7
D86 − 16a
TABLE 4 True and Min and Max D86 50 % Recovered Boiling Points (°C)A
Manual Automated
Distillation con- Distillation Distillation condi- Distillation con-
ditions min D86 conditions tions min D86 ditions max
50 % boiling max D86 50 % boiling D86 50 % boil-
point 50 % boiling point ing point
point
ASTM/IP true boil- Group 1, 2, and Group 1, 2, Group 1, 2, and Group 1, 2,
Toluene ing point 3 and 3 3 and 3
110.6 105.9 111.8 108.5 109.7
ASTM/IP true boil- Group 4 Group 4 Group 4 Group 4

Hexadecane ing point
287.0 272.2 283.1 277.0 280.0
A
The manual and automated temperatures show in this table are the values for the 95 % tolerance interval for the 99 % population coverage. The proposed tolerance
is approximately 3× sigma. Information on the values in this table can be found in RR:D02-1580.
NOTE 11—At 101.3 kPa, toluene is shown in reference manuals as provided with a snug-fitting cork or stopper of silicone rubber,
boiling at 110.6 °C when measured using a partial immersion thermom- or equivalent polymeric material, tightly into the neck of the
eter. Because this test method uses thermometers calibrated for total
immersion, the results typically will be lower and, depending on the
sample container and bring the temperature of the sample to the
thermometer and the situation, may be different for each thermometer. At temperature indicated in Table 3.
101.3 kPa, hexadecane is shown in reference manuals as boiling at
10.3 Groups 1, 2, 3, and 4—Check that the temperature of
287.0 °C when measured using a partial immersion thermometer. Because
this test method uses thermometers calibrated for total immersion, the the sample is as shown in Table 3. Pour the specimen precisely
results typically will be lower, and, depending on the thermometer and the to the 100 mL mark of the receiving cylinder, and transfer the
situation, may be different for each thermometer. contents of the receiving cylinder as completely as practical
9.1.3 A procedure to determine the magnitude of the tem- into the distillation flask, ensuring that none of the liquid flows
perature lag is described in Annex A3. into the vapor tube.
9.1.4 A procedure to emulate the emergent stem effect is NOTE 14—It is important that the difference between the temperature of
described in Appendix X4. the specimen and the temperature of the bath around the receiving cylinder
9.1.5 To verify the calibration of the temperature measure- is as small as practically possible. A difference of 5 °C can make a
ment system at elevated temperatures, use hexadecane. The difference of 0.7 mL.
temperature measurement system shall indicate, at 50% 10.3.1 Groups 3 and 4—If the sample is not fluid at ambient
recovered, a temperature comparable to that shown in Table 4 temperature, it is to be heated to a temperature between 9 °C
for the respective apparatus under Group 4 distillation condi- and 21 °C above its pour point (Test Methods D97, D5949,
tions. D5950, or D5985) prior to analysis. If the sample has partially
NOTE 12—Because of the high melting point of hexadecane, Group 4 or completely solidified in the intervening period, it shall be
verification distillations will have to be carried out with condenser vigorously shaken after melting, and prior to sampling, to
temperatures >20 °C. ensure homogeneity.
9.2 Automated Method: 10.3.1.1 If the sample is not fluid at ambient temperatures,
9.2.1 Level Follower—For an automated distillation disregard the temperature range shown in Table 3 for the
apparatus, the level follower/recording mechanism of the receiving cylinder and sample. Prior to analysis, heat the
apparatus shall have a resolution of 0.1 % volume or better receiving cylinder to approximately the same temperature as
with a maximum error of 0.3 % volume between the 5 % and the sample. Pour the heated specimen precisely to the 100 mL
100 % volume points. The calibration of the assembly shall be mark of the receiving cylinder, and transfer the contents of the
verified in accordance with manufacturer’s instructions at receiving cylinder as completely as practical into the distilla-
intervals of not more than three months and after the system tion flask, ensuring that none of the liquid flows into the vapor
has been replaced or repaired. tube.
NOTE 13—The typical calibration procedure involves verifying the NOTE 15—Any material that evaporates during the transfer will
output with the receiver containing 5 % and 100 % volume of material contribute to the loss; any material that remains in the receiving cylinder
respectively. will contribute to the observed recovery volume at the time of the IBP.
9.2.2 Barometric Pressure—At intervals of not more than 10.4 If the sample can be expected to demonstrate irregular
six months, and after the system has been replaced or repaired, boiling behavior, that is, bumping, add a few boiling chips to
the barometric reading of the instrument shall be verified the specimen. The addition of a few boiling chips is acceptable
against a barometer, as described in 6.6. for any distillation.
10. Procedure 10.5 Fit the temperature sensor through a snug-fitting

device, as described in 6.4, to mechanically center the sensor in
10.1 Record the prevailing barometric pressure. the neck of the flask. In the case of a thermometer, the bulb is
10.2 Groups 1 and 2—Ensure that the sample is conditioned centered in the neck and the lower end of the capillary is level
in accordance with Table 2. Fit a low range thermometer with the highest point on the bottom of the inner wall of the
8
D86 − 16a
FIG. 6 Example of One Manufacturer’s Recommended Placement

of Pt-100 Probe Relative to Distillation Flask Sidearm for Auto-
mated D86 Distillation Instrument
vapor tube (see Fig. 5). In the case of a thermocouple or being used, immediately move the receiving cylinder so that
resistance thermometer, follow the manufacturer’s instructions the tip of the condenser touches its inner wall.
as to placement (see Fig. 6). 10.8.2 Automated Method—To reduce evaporation loss of
NOTE 16—If vacuum grease is used on the mating surface of the
the distillate, use the device provided by the instrument
centering device, use the minimum amount of grease that is practical. manufacturer for this purpose. Apply heat to the distillation
flask and contents with the tip of the receiver deflector just
10.6 Fit the flask vapor tube, provided with a snug-fitting
touching the wall of the receiving cylinder. Note the start time.
cork or rubber stopper of silicone, or equivalent polymeric
Record the IBP to the nearest 0.1 °C (0.2 °F).
material, tightly into the condenser tube. Adjust the flask in a
vertical position so that the vapor tube extends into the 10.9 Regulate the heating so that the time interval between
condenser tube for a distance from 25 mm to 50 mm. Raise and the first application of heat and the IBP is as specified in Table
adjust the flask support board to fit it snugly against the bottom 5.
of the flask. 10.10 Regulate the heating so that the time from IBP to 5 %
10.7 Place the receiving cylinder that was used to measure recovered is as indicated in Table 5.
the specimen, without drying the inside of the cylinder, into its 10.11 Continue to regulate the heating so that the uniform
temperature-controlled bath under the lower end of the con- average rate of condensation from 5 % recovered to 5 mL
denser tube. The end of the condenser tube shall be centered in residue in the flask is 4 mL to 5 mL per minute. (Warning—
the receiving cylinder and shall extend therein for a distance of Due to the configuration of the boiling flask and the conditions
at least 25 mm, but not below the 100 mL mark. of the test, the vapor and liquid around the temperature sensor
10.8 Initial Boiling Point: are not in thermodynamic equilibrium. The distillation rate will
10.8.1 Manual Method—To reduce evaporation loss of the consequently have an effect on the measured vapor tempera-
distillate, cover the receiving cylinder with a piece of blotting ture. The distillation rate shall, therefore, be kept as constant as
paper, or similar material, that has been cut to fit the condenser possible throughout the test.)
tube snugly. If a receiver deflector is being used, start the 10.11.1 In the context of this test method, “uniform average
distillation with the tip of the deflector just touching the wall of rate of condensation” has the following intention. Heating of
the receiving cylinder. If a receiver deflector is not used, keep the boiling flask shall be regulated to maintain as best as
the drip tip of the condenser away from the wall of the possible a uniform flow of condensation, which will then
receiving cylinder. Note the start time. Observe and record the provide the most desired precision for the test. However, some
IBP to the nearest 0.5 °C (1.0 °F). If a receiver deflector is not distillation tests can have one or more short-term rates of
9
D86 − 16a
TABLE 5 Conditions During Test Procedure
Temperature of cooling bathA °C 0–1 0–5 0–5 0–60
°F 32–34 32–40 32–40 32–140
Temperature of bath around °C 13–18 13–18 13–18 ±3
receiving cylinder °F 55–65 55–65 55–65 ±5
of charge
temperature
Time from first application of heat to
initial boiling point, min 5–10 5–10 5–10 5–15
Time from initial boiling point
to 5 % recovered, s 60–100 60–100
Uniform average rate of condensation
from 5 % recovered to 5 mL
in flask, mL/min 4–5 4–5 4–5 4–5
Time recorded from 5 mL residue to
end point, min 5 max 5 max 5 max 5 max
A
The proper condenser bath temperature will depend upon the wax content of the sample and of its distillation fractions. The test is generally performed using one single
condenser temperature. Wax formation in the condenser can be deduced from (a) the presence of wax particles in the distillate coming off the drip tip, (b) a higher distillation
loss than what would be expected based on the initial boiling point of the specimen, (c) an erratic recovery rate and (d) the presence of wax particles during the removal
of residual liquid by swabbing with a lint-free cloth (see 8.3). The minimum temperature that permits satisfactory operation shall be used. In general, a bath temperature
in the 0 °C to 4 °C range is suitable for kerosine, Grade No. 1 fuel oil and Grade No. 1-D diesel fuel oil. In some cases involving Grade No. 2 fuel oil, Grade No. 2-D diesel
fuel oil, gas oils and similar distillates, it may be necessary to hold the condenser bath temperature in the 38 °C to 60 °C range.
condensation which deviate from the 4 mL ⁄min to 5 mL ⁄min tion and reporting of the results of the test as required by the
indicated in 10.11 and Table 5, this is a common occurrence for specification involved, or as previously established for the
some sample types. The periods of these short-term deviations sample under test. These observed data can include tempera-
may last for several percent of material condensed until the ture readings at prescribed percentages recovered or percent-
temperature slope becomes constant again, and may occur at ages recovered at prescribed temperature readings, or both.
several periods along the entire condensation range. These 10.14.1 Manual Method—Record all volumes in the gradu-
deviations will typically correct after the temperature slope ated cylinder to the nearest 0.5 mL, and all temperature
again becomes constant. These short-term deviations shall not readings to the nearest 0.5 °C (1.0 °F).
occur over the entire range of condensation. Typically, these 10.14.2 Automated Method—Record all volumes in the
short-term deviations should not occur for more than ten receiving cylinder to the nearest 0.1 mL, and all temperature
contiguous percent volume. The precision of the temperature readings to the nearest 0.1 °C (0.2 °F).
readings will be significantly affected during these periods.
When the overall calculated average rate of condensation 10.14.3 Group 1, 2, 3, and 4—In cases in which no specific
between 5 % recovered and 5 mL residue is within the pre- data requirements have been indicated, record the IBP and the
scribed rate, the requirement of 10.11 and Table 5 is satisfied. EP (FBP) or the dry point, or both, and temperature readings at
As example, those samples containing a 10 % ethanol-fuel 5 %, 15 %, 85 %, and 95 % recovered, and at each 10 %
blend or those that exhibit a significant change of temperature multiple of volume recovered from 10 to 90, inclusive.
slope at points during the distillation can have a short-term rate 10.14.3.1 Group 4—When a high range thermometer is used
of condensation which deviates from the 4 mL ⁄min to in testing aviation turbine fuels and similar products, pertinent
5 mL ⁄min indicated in 10.11 and Table 5. thermometer readings can be obscured by the centering device.
If these readings are required, perform a second distillation in
NOTE 17—When testing gasoline samples, it is not uncommon to see accordance with Group 3. In such cases, reading from a low
the condensate suddenly form non-miscible liquid phases and bead up on
the temperature measuring device and in the neck of the boiling flask at a range thermometer can be reported in place of the obscured
vapor temperature of around 160 °C. This may be accompanied by a sharp high range thermometer readings, and the test report shall so
(about 3 °C) dip in the vapor temperature and a drop in the recovery rate. indicate. If, by agreement, the obscured readings are waived,
The phenomenon, which may be due to the presence of trace water in the the test report shall so indicate.
sample, may last for 10 s to 30 s before the temperature recovers and the
condensate starts flowing smoothly again. This point is sometimes 10.14.4 When it is required to report the temperature
colloquially referred to as the Hesitation Point. reading at a prescribed percent evaporated or recovered for a
10.12 Repeat any distillation that did not meet the require- sample that has a rapidly changing slope of the distillation
ments described in 10.9, 10.10, and 10.11. curve in the region of the prescribed percent evaporated or
recovered reading, record temperature readings at every 1 %
10.13 If a decomposition point is observed, discontinue the recovered. The slope is considered rapidly changing if the
heating and proceed as directed in 10.17. change in slope ( C) of the data points described in 10.14.2 in
NOTE 18—Characteristic indications of thermal decomposition are that particular area is greater than 0.6 (change of slope (F ) is
evolution of fumes and erratic, typically decreasing, temperature readings greater than 1.0) as calculated by Eq 1 (Eq 2).
that occur during the final stages of the distillation.
Change of Slope ~ C ! 5 (1)
10.14 In the interval between the IBP and the end of the
distillation, observe and record data necessary for the calcula- ~ C 2 2 C 1! / ~ V 2 2 V 1! 2 ~ C 3 2 C 2! / ~ V 3 2 V 2!
10
D86 − 16a
Change of Slope ~ F ! 5 (2) temperature will start and continue to decrease. If the vapor temperature
starts to decrease but then increases and repeats this cycle while the vapor
~ F 2 2 F 1! / ~ V 2 2 V 1! 2 ~ F 3 2 F 2! / ~ V 3 2 V 2! temperature continues to increase you have added too much heat to the
final heat adjustment. If this is the case, it would be advisable to repeat the
where: test lowering final heat setting.
C1 = temperature at the volume % recorded one reading Groups 3 and 4, many Group 3 and 4 samples will have the same
distillation characteristics in regards to dry point and endpoint as Groups
prior to the volume % in question, °C, 1 and 2. With samples that contain higher temperature boiling materials it
C2 = temperature at the volume % recorded in question, °C, may not be possible to detect a dry point or an end point before the
decomposition point occurs.
C3 = temperature at the volume % recorded following the 10.17 Allow the distillate to drain into the receiving
volume % in question, °C, cylinder, after heating has been discontinued.
F1 = temperature at the volume % recorded one reading 10.17.1 Manual Method—While the condenser tube contin-
prior to the volume % in question, °F, ues to drain into the graduated cylinder, observe and note the
F2 = temperature at the volume % recorded in question, °F,
volume of condensate to the nearest 0.5 mL at 2 min intervals
until two successive observations agree. Measure the volume
F3 = temperature at the volume % recorded following the
in the receiving cylinder accurately, and record it to the nearest
volume % in question, °F,
V1 = volume % recorded one reading prior to the volume % 0.5 mL.
in question, 10.17.2 Automated Method—The apparatus shall continu-
V2 = volume % recorded at the volume % in question, and ally monitor the recovered volume until this volume changes
by no more than 0.1 mL in 2 min. Record the volume in the
V3 = volume % recorded following the volume % in ques- receiving cylinder accurately to the nearest 0.1 mL.
tion. 10.18 Record the volume in the receiving cylinder as
10.15 When the residual liquid in the flask is approximately percent recovery. If the distillation was previously discontin-
5 mL, make a final adjustment of the heat. The time from the ued under the conditions of a decomposition point, deduct the
5 mL of liquid residue in the flask to the EP (FBP) shall be percent recovered from 100, report this difference as the sum of
within the limits prescribed in Table 5. If this condition is not percent residue and percent loss, and omit the procedure given
satisfied, repeat the test with appropriate modification of the in 10.19.
final heat adjustment. 10.19 After the flask has cooled and no more vapor is
NOTE 19—Since it is difficult to determine when there is 5 mL of
observed, disconnect the flask from the condenser, pour its
boiling liquid left in the flask, this time is determined by observing the contents into a 5 mL graduated cylinder, and with the flask
amount of liquid recovered in the receiving cylinder. The dynamic holdup suspended over the cylinder, allow the flask to drain until no
has been determined to be approximately 1.5 mL at this point. If there are appreciable increase in the volume of liquid in the cylinder is
no front end losses, the amount of 5 mL in the flask can be assumed to observed. Measure the volume in the graduated cylinder to the
correspond with an amount of 93.5 mL in the receiving cylinder. This
amount has to be adjusted for the estimated amount of front end loss. nearest 0.1 mL, and record as percent residue.
10.19.1 If the 5 mL graduated cylinder does not have
10.15.1 If the actual front end loss differs more than 2 mL graduations below 1 mL and the volume of liquid is less than
from the estimated value, the test shall be rerun. 1 mL, prefill the cylinder with 1 mL of a heavy oil to allow a
10.16 Observe and record the EP (FBP) or the dry point, or better estimate of the volume of the material recovered.
both, as required, and discontinue the heating. 10.19.1.1 If a residue greater than expected is obtained, and
NOTE 20—The end point (final boiling point), rather than the dry point,
the distillation was not purposely terminated before the EP,
is intended for general use. The dry point can be reported in connection check whether adequate heat was applied towards the end of
with special purpose naphthas, such as those used in the paint industry. the distillation and whether conditions during the test con-
Also, it is substituted for the end point (final boiling point) whenever the formed to those specified in Table 5. If not, repeat test.
sample is of such a nature that the precision of the end point (final boiling
point) cannot consistently meet the requirements given in the precision NOTE 22—The distillation residues of this test method for gasoline,
section. kerosine, and distillate diesel are typically 0.9 % to 1.2 %, 0.9 % to 1.3 %,
NOTE 21—Groups 1 and 2, once the final heat adjustment is made, the and 1.0 % to 1.4 % volume, respectively.
vapor temperature/thermometer reading will continue to increase. As the NOTE 23—The test method is not designed for the analysis of distillate
distillation nears the end point (final boiling point) the distillation typically fuels containing appreciable quantities of residual material (see 1.2).
achieves dry point first. After the dry point has been achieved the vapor 10.19.2 Groups 1, 2, 3, and 4—Record the volume in the
temperature/thermometer reading should continue to increase. The bottom
of the flask will be dry but the sides and neck of the flask and the
5 mL graduated cylinder, to the nearest 0.1 mL, as percent
temperature sensor will still have vapor condensate present. The vapor residue.
condensate may have the appearance of a white cloud of fumes. This 10.20 If the intent of the distillation is to determine the
vapor condensate/cloud of fumes should totally engulf the temperature-
measuring sensor before the vapor temperature starts to decrease. If these percent evaporated or percent recovered at a predetermined
observations do not occur, the end point may not have been reached. It corrected temperature reading, modify the procedure to con-
would be advisable to repeat the test adding additional heat to the final form to the instructions described in Annex A4.
heat adjustment. Typically the vapor temperature will continue to rise as
the dry point is reached and the vapor cloud engulfs the temperature- 10.21 Examine the condenser tube and the side arm of the
measuring sensor. When the end point is near, the rate of temperature flask for waxy or solid deposits. If found, repeat the test after
increase will slow and level off. Once the endpoint is reached the vapor making adjustments described in Footnote A of Table 5.
11
D86 − 16a
TABLE 6 Approximate Thermometer Reading Correction After applying the corrections and rounding each result to
Temperature Range CorrectionA per 1.3 kPa (10 mm Hg) the nearest 0.5 °C (1.0 °F) or 0.1 °C (0.2 °F), as appropriate to
Difference in Pressure
the apparatus being used, use the corrected temperature read-
°C °F °C °F
ings in all further calculations and reporting.
10–30 50–86 0.35 0.63
30–50 86–122 0.38 0.68 NOTE 25—Temperature readings are not corrected to 101.3 kPa
50–70 122–158 0.40 0.72 (760 mm Hg) when product definitions, specifications, or agreements
70–90 158–194 0.42 0.76 between the parties involved indicate, specifically, that such correction is
90–110 194–230 0.45 0.81 not required or that correction shall be made to some other base pressure.
110–130 230–266 0.47 0.85
130–150 266–302 0.50 0.89 11.4 Correct the actual loss to 101.3 kPa (760 mm Hg)
150–170 302–338 0.52 0.94 pressure when temperature readings are corrected to 101.3 kPa
170–190 338–374 0.54 0.98
190–210 374–410 0.57 1.02 pressure. The corrected loss, Lc, is calculated from Eq 6 or Eq
210–230 410–446 0.59 1.07 7, as appropriate, or can be read from the tables presented as
230–250 446–482 0.62 1.11
250–270 482–518 0.64 1.15
Fig. X3.1 or Fig. X3.2.
270–290 518–554 0.66 1.20 L c 5 0.51 ~ L 2 0.5! / $ 11 ~ 101.3 2 P k ! /8.00% (6)
290–310 554–590 0.69 1.24
310–330 590–626 0.71 1.28 L c 5 0.51 ~ L 2 0.5! / $ 11 ~ 760 2 P ! /60.0% (7)
330–350 626–662 0.74 1.33
350–370 662–698 0.76 1.37 where:
370–390 698–734 0.78 1.41
390–410 734–770 0.81 1.46
L = observed loss,
A
Lc = corrected loss,
Values to be added when barometric pressure is below 101.3 kPa (760 mm Hg)
and to be subtracted when barometric pressure is above 101.3 kPa.
Pk = pressure, kPa, and
P = pressure, mm Hg.
NOTE 26—Eq 6 and 7 above have been derived from the data in Table
A4.3 and Eqs 5 and 6 in Test Method D86 – 95 and earlier versions. It is
probable that Eq 6 and 7 shown were the original empirical equations from
11. Calculations which the table and equations in the Test Method D86 – 95 and earlier
11.1 The percent total recovery is the sum of the percent versions were derived.
recovery (see 10.18) and the percent residue (see 10.19). 11.4.1 Calculate the corresponding corrected percent recov-
Deduct the percent total recovery from 100 to obtain the ery in accordance with the following equation:
percent loss. R c 5 R1 ~ L 2 L c ! (8)
11.2 Do not correct the barometric pressure for meniscus
depression, and do not adjust the pressure to what it would be where:
at sea level. L = percent loss or observed loss,
Lc = corrected loss,
NOTE 24—The observed barometric reading does not have to be R = percent recovery, and
corrected to a standard temperature and to standard gravity. Even without Rc = corrected percent recovery.
performing these corrections, the corrected temperature readings for the
same sample between laboratories at two different locations in the world 11.5 To obtain the percent evaporated at a prescribed
will, in general, differ less than 0.1 °C at 100 °C. Almost all data obtained temperature reading, add the percent loss to each of the
earlier have been reported at barometric pressures that have not been observed percent recovered at the prescribed temperature
corrected to standard temperature and to standard gravity.
readings, and report these results as the respective percent
11.3 Correct temperature readings to 101.3 kPa (760 mm evaporated, that is:
Hg) pressure. Obtain the correction to be applied to each
P e 5 P r 1L (9)
temperature reading by means of the Sydney Young equation
as given in Eq 3, Eq 4, or Eq 5, as appropriate, or by the use where:
of Table 6. For Celsius temperatures: L = observed loss,
C c 5 0.0009 ~ 101.3 2 P k ! ~ 2731t c ! (3) Pe = percent evaporated, and
Pr = percent recovered.
C c 5 0.00012 ~ 760 2 P ! ~ 2731t c ! (4)
11.6 To obtain temperature readings at prescribed percent
For Fahrenheit temperatures: evaporated, and if no recorded temperature data is available
C f 5 0.00012 ~ 760 2 P ! ~ 4601t f ! (5) within 0.1 volume % of the prescribed percent evaporated, use
either of the two following procedures, and indicate on the
where:
report whether the arithmetical procedure or the graphical
tc = the observed temperature reading in °C, procedure has been used.
tf = the observed temperature reading in °F,
11.6.1 Arithmetical Procedure—Deduct the observed loss
Cc and Cf = corrections to be added algebraically to the
from each prescribed percent evaporated to obtain the corre-
observed temperature readings,
Pk = barometric pressure, prevailing at the time and sponding percent recovered. Calculate each required tempera-
location of the test, kPa, and ture reading as follows:
P = barometric pressure, prevailing at the time and T 5 T L 1 ~ T H 2 T L ! ~ P r 2 P rL! / ~ P rH 2 P rL! (10)
location of the test, mm Hg.
where:
12
D86 − 16a
Pr = percent recovered corresponding to the prescribed 12.6 Do not use the corrected loss in the calculation of
percent evaporated, percent evaporated.
PrH = percent recovered adjacent to, and higher than Pr, 12.7 It is advisable to base the report on relationships
PrL = percent recovered adjacent to, and lower than Pr, between temperature readings and percent evaporated when the
T = temperature reading at the prescribed percent sample is a gasoline, or any other product classified under
evaporated, Group 1, or in which the percent loss is greater than 2.0.
TH = temperature reading recorded at PrH, and Otherwise, the report can be based on relationships between
TL = temperature reading recorded at PrL.
temperature readings and percent evaporated or percent recov-
Values obtained by the arithmetical procedure are affected by ered. Every report must indicate clearly which basis has been
the extent to which the distillation graphs are nonlinear. used.
Intervals between successive data points can, at any stage of 12.7.1 In the manual method, if results are given in percent
the test, be no wider than the intervals indicated in 10.18. In no evaporated versus temperature readings, report if the arithmeti-
case shall a calculation be made that involves extrapolation. cal or the graphical procedure was used (see 11.6).
11.6.2 Graphical Procedure—Using graph paper with uni-
12.8 Report if a drying agent, as described in 7.5.2 or 7.5.3,
form subdivisions, plot each temperature reading corrected for
was used.
barometric pressure, if required (see 11.3), against its corre-
sponding percent recovered. Plot the IBP at 0 % recovered. 12.9 Fig. X1.1 is an example of a tabular report. It shows the
Draw a smooth curve connecting the points. For each pre- percent recovered versus the corresponding temperature read-
scribed percent evaporated, deduct the distillation loss to ing and versus the corrected temperature reading. It also shows
obtain the corresponding percent recovered and take from the the percent loss, the corrected loss, and the percent evaporated
graph the temperature reading that this percent recovered versus the corrected temperature reading.
indicates. Values obtained by graphical interpolation proce-
13. Precision and Bias
dures are affected by the care with which the plot is made.
13.1 Precision (Group 1, 2, 3 automated)—The precision of
NOTE 27—See Appendix X1 for numerical examples illustrating the this test method, as determined by the statistical examination of
arithmetical procedure.
the interlaboratory test results,9 is as follows:
11.6.3 In most automated instruments, temperature-volume
data are collected at 0.1 volume % intervals or less and stored NOTE 28—The precision was derived from data produced by automated
D86 apparatus. Typical examples of precision for manual apparatus can be
in memory. To report a temperature reading at a prescribed calculated from the information contained in Annex A4 (see A4.10).
percent evaporated, neither of the procedures described in NOTE 29—Information on the precision of percent evaporated or
11.6.1 and 11.6.2 have to be used. Obtain the desired tempera- percent recovered at a prescribed temperature can be found in Annex A4.
ture directly from the database as the temperature closest to and NOTE 30—For naphthas, solvents, and other similar materials where
percent recovered are reported and the percent loss is typically less than
within 0.1 % volume of the prescribed percent evaporated. one percent, the percent recovered temperatures can be considered
identical to the percent evaporated temperatures and precision can be
12. Report calculated as shown for Group 1, 2, 3.
12.1 Report the following information (see Appendix X5 13.1.1 Repeatability—The difference between successive
for examples of reports): test results, obtained by the same operator using the same
apparatus under constant operating conditions on identical test
12.2 Report the barometric pressure to the nearest 0.1 kPa
material, would in the long run, in the normal and correct
(1 mm Hg).
operation of this test method, exceed the values in Table 7 only
12.3 Report all volumetric readings in percentages. in one case in twenty.
12.3.1 Manual Method—Report volumetric readings to the 13.1.2 Reproducibility—The difference between two single
nearest 0.5, and all temperature readings to the nearest 0.5° C and independent test results, obtained by different operators
(1.0 °F). working in different laboratories on identical test material,
12.3.2 Automated Method—Report volumetric readings to would in the long run, in normal and correct operation of this
the nearest 0.1, and all temperature readings to the nearest one test method, exceed the values in Table 7 only in one case in
tenth degree. twenty.
12.4 After barometric corrections of the temperature read- 13.1.3 The precision statements were derived from a 2010
ings have been made, the following data require no further interlaboratory cooperative test program.9 Twenty six labora-
calculation prior to reporting: IBP, dry point, EP (FBP), tories participated and analyzed twenty one sample sets com-
decomposition point, and all pairs of corresponding values prised of; specification grade gasoline, both conventional and
involving percent recovered and temperature readings. oxygenated, some containing up to 20 % ethanol. The tem-
12.4.1 The report shall state if the temperature readings perature range covered was 20 °C to 220 °C. Information on
have not been corrected for barometric pressure. the type of samples and their average boiling points are in the
research report.
12.5 When the temperature readings have not been cor-
rected to 101.3 kPa (760 mm Hg) pressure, report the percent 9
residue and percent loss as observed in accordance with 10.19 be obtained by requesting Research Report RR:D02-1807. Contact ASTM Customer
and 11.1, respectively. Service at [email protected].
13
D86 − 16a
TABLE 7 Repeatability and Reproducibility for Group 1, 2, 3 TABLE 8 Repeatability and Reproducibility for Group 4
(Automated) (Automated)A
(Valid Range 20 °C to 260 °C) Percent Repeatability °C Reproducibility °C Valid Range °C
Percent Repeatability °C Reproducibility °C Recovered
Evaporated IBP 0.02T 0.055T 145 to 220
IBP 2.7 4.7 10 % 0.009T 0.022T 160 to 265
5 1.4 + 2.8(0.43Sc + 0.24) 2.5 + 2.8(0.43Sc + 0.24) 50 % 1.0 3.0 170 to 295
10 0.9 + 2.8(0.43Sc + 0.24) 1.9 + 2.8(0.43Sc + 0.24) 90 % 0.004T 0.015T 180 to 340
20 0.9 + 2.8(0.43Sc + 0.24) 2.0 + 2.8(0.43Sc + 0.24) 95 % 0.013(T-140) 0.041(T-140) 260 to 360
30 0.8 + 2.8(0.43Sc + 0.24) 1.8 + 2.8(0.43Sc + 0.24) FBP 2.2 7.1 195 to 365
40 0.9 + 2.8(0.43Sc + 0.24) 2.0 + 2.8(0.43Sc + 0.24)
where:
50 1.0 + 2.8(0.43Sc + 0.24) 1.9 + 2.8(0.43Sc + 0.24)
60 1.1 + 2.8(0.43Sc + 0.24) 2.0 + 2.8(0.43Sc + 0.24) T = percent recovered temperature within valid range prescribed.
70 1.5 + 2.8(0.43Sc + 0.24) 2.1 + 2.8(0.43Sc + 0.24) A
Refer to Annex A1 for tables of calculated repeatability and reproducibility.
80 1.1 + 2.8(0.43Sc + 0.24) 2.0 + 2.8(0.43Sc + 0.24)
90 1.8 + 2.8(0.43Sc + 0.24) 2.8 + 2.8(0.43Sc + 0.24)
95 2.0 + 2.8(0.43Sc + 0.24) 3.6 + 2.8(0.43Sc + 0.24)
FBP 3.3 7.1
where:
Sc = slope or rate of change of temperature in degrees Celcius calculated 13.2.3 The precision statements were derived from a 2005
using A4.10.1. interlaboratory cooperative test program.10 Sixteen laborato-
ries participated and analyzed sample sets comprised of;
specification grade diesel, with a B5 and B20 biodiesel,
13.2 Precision (Group 4)—The precision of this test specification grade heating oil, aviation turbine fuels, marine
method, as determined by the statistical examination of the fuels, mineral spirits and toluene. The temperature range
interlaboratory test results,10 is as follows: covered was 145 °C to 365 °C. Information on the type of
NOTE 31—Information on the precision of percent evaporated or samples and their average boiling points are in the research
percent recovered at a prescribed temperature can be found in Annex A4. report.
13.2.1 Repeatability—The difference between successive 13.3 Bias:
test results, obtained by the same operator using the same 13.3.1 Bias—Since there is no accepted reference material
apparatus under constant operating conditions on identical test suitable for determining the bias for the procedure in these test
material, would in the long run, in the normal and correct methods, bias has not been determined.
operation of this test method, exceed the following values in 13.3.2 Relative Bias between Manual and Automated
Table 8 only in one case in twenty. Apparatus—An interlaboratory study7 conducted in 2003 using
13.2.2 Reproducibility—The difference between two single manual and automated apparatus has concluded that there is no
and independent test results, obtained by different operators statistical evidence to suggest that there is a bias between
working in different laboratories on identical test material, manual and automated results.
would in the long run, in normal and correct operation of this
test method, exceed the following values in Table 8 only in one NOTE 32—See A2.1 for information on the application and use of
borosilicate and quartz distillation flasks.
case in twenty.
14. Keywords
10
Supporting data (results of the 2005 Interlaboratory Cooperative Test Pro-
gram) have been filed at ASTM International Headquarters and may be obtained by 14.1 batch distillation; distillates; distillation; laboratory
requesting Research Report RR:D02-1621. distillation; petroleum products
14
D86 − 16a
ANNEXES
(Mandatory Information)
A1. PRECISION TABLES FOR REPEATABILITY (r) AND REPRODUCIBILITY (R)
A1.1 Tables: 210 0.86 3.15

215 0.88 3.23
Recovered IBP IBP_GRP4
220 0.90 3.30
Temperature (°C) r_D86auto R_D86auto
225 0.92 3.38
145 2.61 7.98
230 0.94 3.45
150 2.70 8.25
235 0.96 3.53
155 2.79 8.53
240 0.98 3.60
160 2.88 8.80
245 1.00 3.68
165 2.97 9.08
250 1.03 3.75
170 3.06 9.35
255 1.05 3.83
175 3.15 9.63
260 1.07 3.90
180 3.24 9.90
265 1.09 3.98
185 3.33 10.18
270 1.11 4.05
190 3.42 10.45
275 1.13 4.13
195 3.51 10.73
280 1.15 4.20
200 3.60 11.00
285 1.17 4.28
205 3.69 11.28
290 1.19 4.35
210 3.78 11.55
295 1.21 4.43
215 3.87 11.83
300 1.23 4.50
220 3.96 12.10
305 1.25 4.58
Recovered 10 % T10_GRP4 310 1.27 4.65
Temperature (°C) r_D86auto R_D86auto 315 1.29 4.73
160 1.50 3.52 320 1.31 4.80
165 1.55 3.63 325 1.33 4.88
170 1.60 3.74 330 1.35 4.95
175 1.65 3.85 335 1.37 5.03
180 1.69 3.96 340 1.39 5.10
185 1.74 4.07
190 1.79 4.18
Recovered 95 % T95_GRP4
195 1.83 4.29
Temperature (°C) r_D86auto R_D86auto
200 1.88 4.40
260 1.58 4.93
205 1.93 4.51
265 1.65 5.13
210 1.97 4.62
270 1.71 5.34
215 2.02 4.73
275 1.78 5.54
220 2.07 4.84
280 1.85 5.75
225 2.12 4.95
285 1.91 5.95
230 2.16 5.06
290 1.98 6.16
235 2.21 5.17
295 2.04 6.36
240 2.26 5.28
300 2.11 6.57
245 2.30 5.39
305 2.17 6.77
250 2.35 5.50
310 2.24 6.98
255 2.40 5.61
315 2.31 7.18
260 2.44 5.72
320 2.37 7.39
265 2.49 5.83
325 2.44 7.59
Recovered 50 % T50_GRP4 330 2.50 7.80
170–295 0.94 2.97 340 2.64 8.21
Recovered 90 % T90_GRP4 345 2.70 8.42
180 0.74 2.70 355 2.83 8.83
185 0.76 2.78 360 2.90 9.03
190 0.78 2.85 Recovered FBP FBP_GRP4
195 0.80 2.93 Temperature (°C) r_D86auto R_D86auto
200 0.82 3.00 195–365 2.2 7.1
205 0.84 3.08
15
D86 − 16a
FIG. A2.1 125 mL Flask and 125 mL Flask with Ground Glass Joint
A2. DETAILED DESCRIPTION OF APPARATUS
A2.1 Distillation Flasks—Flasks shall be of heat resistant Borosilicate = Quartz + 0.40

glass, constructed to the dimensions and tolerances shown in
Fig. A2.1 and Fig. A2.2. Flasks made of borosilicate glass shall A2.2 Condenser and Condenser Bath—Typical types of
comply with the requirements of Specification E1405. Flasks condenser and condenser baths are illustrated in Figs. 1 and 2.
made of quartz shall be composed of 99.9+ % SiO2. Flasks A2.2.1 The condenser shall be made of seamless noncorro-
may also be constructed with a ground glass joint. sive metal tubing, 560 6 5 mm in length, with an outside
NOTE A2.1—Since the thermal response of borosilicate glass and quartz
can be different, consider appropriate adjustments for the initial and final diameter of 14 mm and a wall thickness of 0.8 mm to 0.9 mm.
heat regulation to attain the time limits stated in the procedure.
NOTE A2.2—For tests specifying dry point, specially selected flasks NOTE A2.3—Brass or stainless steel has been found to be a suitable
with bottoms and walls of uniform thickness are desirable. material for this purpose.
A2.1.1 Intralaboratory and interlaboratory data11 for motor A2.2.2 The condenser shall be set so that 393 mm 6 3 mm
gasoline, kerosene, aviation turbine fuel, fuel oil, and diesel of the tube is in contact with the cooling medium, with 50 mm
fuel were assessed by Practice D6708 indicating that some 6 3 mm outside the cooling bath at the upper end, and with
correction could improve the degree of agreement between 114 mm 6 3 mm outside at the lower end. The portion of the
quartz and borosilicate flask results. The level of correction tube projecting at the upper end shall be set at an angle of 75°
could be considered practically not significant. Correction is 6 3° with the vertical. The portion of the tube inside the
more probable at the IBP and FBP of both motor gasoline and condenser bath shall be either straight or bent in any suitable
distillate fuels. Optimizing D86 parameters for motor gasoline continuous smooth curve. The average gradient shall be 15° 6
and distillate fuels may further minimize the differences in D86 1° with respect to the horizontal, with no 10 cm section having
IBP and FBP when using borosilicate versus quartz flask. Bias a gradient outside of the 15° 6 3° range. The projecting lower
can conceivably occur for materials and temperatures not portion of the condenser tube shall be curved downward for a
studied in this limited program. length of 76 mm and the lower end shall be cut off at an acute
A2.1.1.1 For motor gasoline in the temperature range of
angle. Provisions shall be made to enable the flow of the
25 °C to 220 °C:
distillate to run down the side of the receiving cylinder. This
Borosilicate = 1.0054 Quartz – 0.73
can be accomplished by using a drip-deflector, which is
A2.1.1.2 For kerosene, aviation turbine fuel, fuel oil, and
diesel fuel in the temperature range of 140 °C to 350 °C: attached to the outlet of the tube. Alternatively, the lower
portion of the condenser tube can be curved slightly backward
to ensure contact with the wall of the receiving cylinder at a
11
point 25 mm to 32 mm below the top of the receiving cylinder.
be obtained by requesting Research Report RR:D02-1753. Contact ASTM Customer Fig. A2.3 is a drawing of an acceptable configuration of the
Service at [email protected]. lower end of the condenser tube.
16
D86 − 16a
FIG. A2.2 Detail of Upper Neck Section
A2.2.3 The volume and the design of the bath will depend during operation. A typical shield would be 480 mm high,
on the cooling medium employed. The cooling capacity of the 280 mm long, and 200 mm wide, made of sheet metal of
bath shall be adequate to maintain the required temperature for 0.8 mm thickness (22 gauge). The shield shall be provided with
the desired condenser performance. A single condenser bath at least one window to observe the dry point at the end of the
may be used for several condenser tubes. distillation.
A2.3 Metal Shield or Enclosure for Flask. (Manual units A2.3.2 Shield for Electric Heater (see Fig. 2)—A typical
only). shield would be 440 mm high, 200 mm long, and 200 mm
A2.3.1 Shield for Gas Burner (see Fig. 1)—The purpose of wide, made of sheet metal of approximately 0.8 mm thickness
this shield is to provide protection for the operator and yet (22 gauge) and with a window in the front side. The shield shall
allow easy access to the burner and to the distillation flask
17
D86 − 16a
board (see A2.6) above the electric heater. The whole assembly
is adjustable from the outside of the shield.
A2.6 Flask Support Board—The flask support board shall
be constructed of ceramic or other heat-resistant material,
3 mm to 6 mm in thickness. Flask support boards are classified
as A, B, or C, based on the size of the centrally located
opening, the dimension of which is shown in Table 3. 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 —Asbestos-
containing materials shall not be used in the construction of the
flask support board.)
A2.7 The flask support board can be moved slightly in
different directions on the horizontal plane to position the
distillation flask so that direct heat is applied to the flask only
through the opening in this board. Usually, the position of the
flask is set by adjusting the length of the side-arm inserted into
the condenser.
A2.8 Provision shall be made for moving the flask support
assembly vertically so that the flask support board is in direct
contact with the bottom of the distillation flask during the
FIG. A2.3 Lower End of Condenser Tube
distillation. The assembly is moved down to allow for easy
mounting and removal of the distillation flask from the unit.
be provided with at least one window to observe the dry point A2.9 Receiving Cylinders—The receiving cylinder shall
at the end of the distillation. have a capacity to measure and collect 100 mL 6 1.0 mL. The
shape of the base shall be such that the receiver does not topple
A2.4 Heat Source when placed empty on a surface inclined at an angle of 13°
A2.4.1 Gas Burner (see Fig. 1), capable of bringing over the from the horizontal.
first drop from a cold start within the time specified and of A2.9.1 Manual Method—The cylinder shall be graduated at
continuing the distillation at the specified rate. A sensitive intervals of 1 mL beginning at least at 5 mL and have a
manual control valve and gas pressure regulator to give graduation at the 100 mL mark. Construction details and
complete control of heating shall be provided. tolerances for the graduated cylinder are shown in Fig. A2.4.
A2.4.2 Electric Heater (see Fig. 2), of low heat retention.
A2.9.2 Automated Method—The cylinder shall conform to
NOTE A2.4—Heaters, adjustable from 0 W to 1000 W, have been found the physical specifications described in Fig. A2.4, except that
to be suitable for this purpose. graduations below the 100 mL mark are permitted, as long as
A2.5 Flask Support they do not interfere with the operation of the level follower.
Receiving cylinders for use in automated units may also have
A2.5.1 Type 1—Use a Type 1 flask support with a gas burner a metal base.
(see Fig. 1). This support consists of either a ring support of the
ordinary laboratory type, 100 mm or larger in diameter, sup- A2.9.3 If required, the receiving cylinder shall be immersed
ported on a stand inside the shield, or a platform adjustable during the distillation to above the 100 mL graduation line in a
from the outside of the shield. On this ring or platform is cooling liquid contained in a cooling bath, such as a tall-form
mounted a hard board made of ceramic or other heat-resistant beaker of clear glass or transparent plastic. Alternatively, the
material, 3 mm to 6 mm in thickness, with a central opening receiving cylinder may be placed in a thermostated bath air
76 mm to 100 mm in diameter, and outside line dimensions circulation chamber.
slightly smaller than the inside boundaries of the shield. A2.10 Residue Cylinder—The graduated cylinder shall
A2.5.2 Type 2—Use a Type 2 flask support assembly with have a capacity of 5 mL or 10 mL, with graduations into
electric heating (see Fig. 2 as one example). The assembly 0.1 mL subdivisions, beginning at 0.1 mL. The top of the
consists of an adjustable system onto which the electric heater cylinder may be flared, the other properties shall conform to
is mounted with provision for placement of a flask support Specification E1272.
18
D86 − 16a
NOTE 1—1 mL graduations – minimum 5 mL to 100 mL

FIG. A2.4 100 mL Graduated Cylinder
A3. DETERMINATION OF THE DIFFERENCE IN LAG TIME BETWEEN AN ELECTRONIC TEMPERATURE MEASURE-
MENT SYSTEM AND A MERCURY-IN-GLASS THERMOMETER
A3.1 The response time of an electronic temperature mea- A3.3 Replace the electronic temperature measuring device
suring device is inherently more rapid than that of a mercury- with a low range or a high range mercury-in-glass
in-glass thermometer. The temperature measuring device as- thermometer, depending on the boiling range of the sample.
sembly in general use, consisting of the sensor and its casing,
or an electronic system and its associated software, or both, is A3.4 Repeat the distillation with this thermometer, and
so designed that the temperature measuring system will simu- manually record the temperature at the various percent recov-
late the temperature lag of the mercury-in-glass thermometer. ered as described in 10.14.
A3.2 To determine the difference in lag time between such A3.5 Calculate the values for the repeatability for the
a temperature measuring system and a mercury-in-glass observed slope (∆T/∆V) for the different readings in the test.
thermometer, analyze a sample such as gasoline, kerosine, jet
fuel, or light diesel fuel with the electronic temperature A3.6 Compare the test data obtained using these two tem-
measurement system in place and in accordance with the perature measuring devices. The difference at any point shall
procedures described in this test method. In most cases this is be equal to, or less than, the repeatability of the method at that
the standard distillation step performed with an automated unit. point. If this difference is larger, replace the electronic tem-
A3.2.1 Do not use a single pure compound, a very narrow perature measuring device or adjust the electronics involved, or
boiling range product, or a synthetic blend of less than six both.
compounds for this test.
A3.2.2 Best results are obtained with a sample that is typical
of the sample load of the laboratory. Alternatively, use a
full-range mixture with a 5 % to 95 % boiling range of at least
100 °C.
19
D86 − 16a
TABLE A4.1 Precision for Percent Evaporated at a Prescribed Temperature—Gasoline (Consolidated Equation)
Valid Range E70 – E180°C (Automated Apparatus)
D86 Auto r R
0.00836 (150 – X) 0.0200 (150 – X)
where: X = percent evaporated at the prescribed temperature
A4. PROCEDURE TO DETERMINE THE PERCENT EVAPORATED OR PERCENT RECOVERED AT A PRESCRIBED TEM-
PERATURE READING
A4.1 Many specifications require specific percentages temperature, allow the distillate to drain into the receiving
evaporated or recovered at prescribed temperature readings, graduate. Allow the contents of the flask to cool to below
either as maxima, minima, or ranges. The procedures to approximately 40 °C and then drain its contents into the
determine these values are frequently designated by the terms receiving graduate. Note the volume of product in the receiving
Exxx or Rxxx, where xxx is the desired temperature. graduate to the nearest 0.5 mL at 2 min intervals until two
NOTE A4.1—Regulatory standards on the certification of reformulated successive observations agree.
gasoline under the complex model procedure require the determination of A4.5.2.2 The amount recovered in the receiving graduate is
E200 and E300, defined as the percent evaporated fuel at 93.3 °C (200 °F)
and 148.9 °C (300 °F), respectively. E158, the percent evaporated at a
the percent recovery. Determine the amount of observed loss
distillation temperature of 70 °C (158 °F), is also used in describing fuel by subtracting the percent recovery from 100.0.
volatility characteristics. Other typical temperatures are R 200 for kero-
sines and R 250 and R 350 for gas oils, where R 200, R 250, and R 350 A4.6 Automated Distillation
are the percent recovered fuel at 200 °C, 250 °C, and 350 °C, respectively. A4.6.1 In the region between about 10 °C below and 10 °C
A4.2 Determine the barometric pressure, and calculate the above the desired expected temperature reading determined in
correction to the desired temperature reading using Eq 3, Eq 4, A4.3, collect temperature-volume data at 0.1 % volume inter-
or Eq 5 for t = xxx°C (or tf = xxx°F). vals or less.
A4.2.1 Manual Method—Determine this correction to A4.6.2 Continue the distillation, as described in Section 10,
0.5 °C (1 °F). and determine the percent loss, as described in 11.1.
A4.2.2 Automated Method—Determine this correction to A4.7 Calculations
0.1 °C (0.2 °F). A4.7.1 Manual Method—If a volume percent recovered
A4.3 Determine the expected temperature reading to yield reading is not available at the exact temperature calculated in
xxx °C (or xxx °F) after the barometric correction. To obtain A4.3, determine the percent recovered by interpolation be-
the expected value, add the absolute value of the calculated tween the two adjacent readings. Either the linear, as described
correction to the desired temperature if the barometric pressure in 11.6.1, or the graphical procedure, as described in 11.6.2, is
is above 101.3 kPa. If the barometric pressure is below permitted. The percent recovered is equal to Rxxx.
101.3 kPa, subtract the absolute value of the calculated correc- A4.7.2 Automated Method—Report the observed volume to
tion from the desired temperature. 0.1 % volume corresponding to the temperature closest to the
expected temperature reading. This is the percent recovered, or
A4.4 Perform the distillation, as described in Section 10, Rxxx.
while taking into account A4.5 and A4.6.
A4.7.3 Manual and Automated Methods—To determine the
A4.5 Manual Distillation value of Exxx, add the observed loss to the percent recovered,
A4.5.1 In the region between about 10 °C below and 10 °C Rxxx, as determined in A4.7.1 or A4.7.2 and as described in
above the desired expected temperature reading determined in Eq 9.
A4.3 record the temperature reading in intervals of 1 volume A4.7.3.1 As prescribed in 12.6, do not use the corrected
%. loss.
A4.5.2 If the intent of the distillation is to solely determine A4.8 Precision—The statistical determination of the preci-
the value of Exxx or Rxxx, discontinue the distillation after at sion of the volume % evaporated or recovered at a prescribed
least another 2 mL of distillate have been collected. Otherwise, temperature for automated apparatus were derived according to
continue the distillation, as described in Section 10, and Practice D6300 from a 2005 interlaboratory program.10Table
determine the observed loss, as described in 11.1. A4.1 shows the consolidated equations for volume percent
A4.5.2.1 If the intent of the distillation is to determine the evaporated for gasoline, Table A4.2 shows the precision for
value of Exxx and the distillation was terminated after about volume percent recovered for diesel. The precision is valid
2 mL of distillate was collected beyond the desired only for the range of temperatures stated. The estimation of
20
D86 − 16a
TABLE A4.2 Precision for Percent Recovered at a Prescribed Temperature—Diesel (Rxxx)
Valid Range R200 – R300°C (Automated Apparatus)
R200C, R250C, R300C
D86 Auto
r R
1.07 2.66
precision for temperature points outside the stated range can be VEP = the volume % recovered or evaporated corresponding
calculated from the procedures in A4.10 and the precision to the end point.
tables in Annex A1.
A4.10.1.4 In the event that the distillation end point occurs
A4.9 The statistical determination of the precision of the prior to the 95 % point, the slope at the end point is calculated
volume percent evaporated or recovered at a prescribed tem- as follows:
perature for manual apparatus has not been directly measured S C ~ or S F ! 5 ~ T EP 2 T HR! / ~ V EP 2 V HR! (A4.2)
in an interlaboratory program. It can be shown that the
precision of the volume percent evaporated or recovered at a where:
prescribed temperature is equivalent to the precision of the TEP or THR = the temperature, in °C or °F, at the percent
temperature measurement at that point divided by the rate of volume recovered indicated by the
change of temperature versus volume percent evaporated or subscript, and
recovered. The estimation of precision becomes less precise at VEP or VHR = the volume % recovered.
high slope values. Subscript EP = end point, and
Subscript HR = highest reading, either 80 % or 90 %, prior
A4.10 Calculate the slope or rate of change in temperature to the end point.
reading, SC (or SF), as described in A4.10.1 and Eq A4.1 and
using temperature values bracketing the desired temperature. A4.10.1.5 For points between 10 % to 85 % recovered that
are not shown in Table A4.3, the slope is calculated as follows:
A4.10.1 Slope or Rate of Change of Temperature:
S C ~ or S F ! 5 0.05 ~ T ~ V110! 2 T ~ V210! ! (A4.3)
NOTE A4.2—The slope can have a dramatic influence on precision for
some samples, typically those containing oxygenates, and the calculated A4.10.2 Calculate the repeatability, r, or the reproducibility,
precision obtained using the values in Table A4.3 may not reflect this in R, from the slope, SC (or SF) and the data in Tables A4.4 and
all cases. This can be due to the changing composition of the sample,
causing the slope to change rapidly over a short interval. This change may
A4.5.
occur either during the data increments prior to, or subsequent to, the data A4.10.3 Determine the repeatability or reproducibility, or
point under calculation.
both, of the volume % evaporated or recovered at a prescribed
A4.10.1.1 To determine the precision of a result, it is temperature from the following formulas:
generally necessary to determine the slope or rate of change of
r volume % 5 r/S C ~ S F ! (A4.4)
the temperature at that particular point. This variable, denoted
as SC or SF, is equal to the change in temperature, either in °C R volume % 5 R/S C ~ S F ! (A4.5)
or in °F, respectively, per percent recovered or evaporated.
A4.10.1.2 The precision of the IBP and EP does not require where:
any slope calculation. rvolume % = repeatability of the volume percent evaporated
A4.10.1.3 With the exception stated in A4.10.1.2, the slope or recovered,
at any point during the distillation is calculated from the Rvolume % = reproducibility of the volume percent evapo-
following equations, using the values shown in Table A4.3: rated or recovered,
r = repeatability of the temperature at the pre-
S C ~ or S F ! 5 ~ T U 2 T L ! / ~ V U 2 V L ! (A4.1) scribed temperature at the observed percent
where: distilled,
SC = the slope, °C/volume %, R = reproducibility of the temperature at the pre-
SF = the slope, °F/volume %, scribed temperature at the observed percent
TU = the upper temperature, °C (or °F), distilled, and
TL = the lower temperature, °C (or °F), SC (SF) = rate of change in temperature reading in °C (°F)
VU = the volume % recovered or evaporated corresponding per the volume percent evaporated or
to TU, recovered.
VL = the volume % recovered or evaporated corresponding A4.10.4 Examples on how to calculate the repeatability and
to TL, and
the reproducibility are shown in Appendix X2.
21
D86 − 16a
TABLE A4.3 Data Points for Determining Slope, SC or SF
Slope at % IBP 5 10 20 30 40 50 60 70 80 90 95 EP
TL at % 0 0 0 10 20 30 40 50 60 70 80 90 95
TU at % 5 10 20 30 40 50 60 70 80 90 90 95 VEP
VU - V L 5 10 20 20 20 20 20 20 20 20 10 5 VEP −95
TABLE A4.4 Repeatability and Reproducibility for Group 1

Manual Manual
Evaporated RepeatabilityA ReproducibilityA
Point, %
°C °F °C °F
IBP 3.3 6 5.6 10
5 1.9+0.86SC 3.4+0.86SF 3.1+1.74SC 5.6+1.74SF
10 1.2+0.86SC 2.2+0.86SF 2.0+1.74SC 3.6+1.74SF
20 1.2+0.86SC 2.2+0.86SF 2.0+1.74SC 3.6+1.74SF
30–70 1.2+0.86SC 2.2+0.86SF 2.0+1.74SC 3.6+1.74SF
80 1.2+0.86SC 2.2+0.86SF 2.0+1.74SC 3.6+1.74SF
90 1.2+0.86SC 2.2+0.86SF 0.8+1.74SC 1.4+1.74SF
95 1.2+0.86SC 2.2+0.86SF 1.1+1.74SC 1.9+1.74SF
FBP 3.9 7 7.2 13
A
SC or SF is the average slope (or rate of change) calculated in accordance with A4.10.1. Table A4.4 precision data obtained from RR study on both manual and automated
D86 units by North American and IP laboratories.
TABLE A4.5 Repeatability and Reproducibility for Groups 2, 3 and 4 (Manual Method)
RepeatabilityA ReproducibilityA
°C °F °C °F
IBP 1.0+0.35SC 1.9+0.35SF 2.8+0.93SC 5.0+0.93SF
5—95 % 1.0+0.41SC 1.8+0.41SF 1.8+1.33SC 3.3+1.33SF
FBP 0.7+0.36SC 1.3+0.36SF 3.1+0.42SC 5.7+0.42SF
% volume at 0.7+0.92/SC 0.7+1.66/SF 1.5+1.78/SC 1.53+3.20/SF

temperature reading
A
SC or SF is the average slope (or rate of change) calculated in accordance with A4.10.1. Table A4.5 has been derived from the monographs in Figs. 6 and 7 in D86–97.
APPENDIXES
(Nonmandatory Information)
X1. EXAMPLES ILLUSTRATING CALCULATIONS FOR REPORTING OF DATA
X1.1 The observed distillation data used for the calculation

of the examples below are shown in the first three columns of
Fig. X1.1.
X1.1.1 Temperature readings corrected to 101.3 kPa
(760 mm Hg) pressure (see 11.3) are as follows:
correction ~ °C ! 5 0.0009 ~ 101.3 2 98.6! ~ 2731t c ! (X1.1)
correction ~ °F ! 5 0.00012 ~ 760 2 740! ~ 4601t f ! (X1.2)
X1.1.2 Loss correction to 101.3 kPa (see 11.4) are as

follows. The data for the examples are taken from Fig. X1.1.
corrected loss 5 ~ 0.5 1 ~ 4.7 2 0.5!! / (X1.3)
$ 11 ~ 101.3 2 98.6! /8.0% 5 3.6

X1.1.3 Recovery correction to 101.3 kPa (see 11.4.1) are as
follows:
corrected recovery 5 94.21 ~ 4.7 2 3.6! 5 95.3 (X1.4)
FIG. X1.1 Example of Test Report
22
D86 − 16a
X1.2 Temperature Readings at Prescribed Percent X1.2.3 Temperature reading at 90 % evaporated (85.3 %
Evaporated recovered) (see 11.6.1) are as follows:
X1.2.1 Temperature reading at 10 % evaporated (4.7 % T 90E ~ °C ! 5 181.61 @ ~ 201.6 2 181.6! (X1.9)
observed loss = 5.3 % recovered) (see 11.6.1) are as follows:
~ 85.3 2 85! / ~ 90 2 85! # 5 182.8°C
T 10E ~ °C ! 5 33.71 @ ~ 40.3 2 33.7! (X1.5)
T 90E ~ °F ! 5 358.91 @ ~ 394.8 2 358.9! (X1.10)
~ 5.3 2 5 ! / ~ 10 2 5 ! # 5 34.1°C
~ 85.3 2 85! / ~ 90 2 85! # 5 361.0°F
T 10E ~ °F ! 5 92.71 @ ~ 104.5 2 92.7! (X1.6)
X1.2.4 Temperature reading at 90 % evaporated (85.3 %
~ 5.3 2 5 ! / ~ 10 2 5 ! # 5 93.1°F recovered) not corrected to 101.3 kPa pressure (see 11.6.1) are
as follows:
X1.2.2 Temperature reading at 50 % evaporated (45.3 %
T 90E ~ °C ! 5 180.51 @ ~ 200.4 2 180.5! (X1.11)
recovered) (see 11.6.1) are as follows:
T 50E ~ °C ! 5 93.91 @ ~ 108.9 2 93.9! (X1.7) ~ 85.3 2 85! / ~ 90 2 85! # 5 181.7°C
T 90E ~ °F ! 5 3571 @ ~ 392 2 357! (X1.12)
~ 45.3 2 40! / ~ 50 2 40! # 5 101.9°C
T 50E ~ °F ! 5 2011 @ ~ 228 2 201! (X1.8) ~ 85.3 2 85! / ~ 90 2 85! # 5 359.1°F
NOTE X1.1—Results calculated from °C data may not correspond
~ 45.3 2 40! / ~ 50 2 40! # 5 215.3°F exactly to results calculated from °F data because of errors in rounding.
X2. EXAMPLES OF CALCULATION OF REPEATABILITY AND REPRODUCIBILITY OF VOLUME % (RECOVERED OR

EVAPORATED) AT A PRESCRIBED TEMPERATURE READING
TABLE X2.1 Distillation Data from a Group 1 Sample Manual 51.1

Distillation
Volume (mL) S F % 5 0.1 ~ T ~ 20! 2 T ~ 10! !
Distillation Point
Temperature °C Temperature °F Recovered at
Recovered, mL
93.3 °C (200 °F) 50.1 ~ 201 2 182!
18.0
10 84 183 51.9
20 94 202
30 103 217 X2.2.2 From Table A4.4, determine the value of R, the
40 112 233 reproducibility at the observed percentage distilled. In this
Volume (mL)
Distillation Point
Temperature° C Temperature° F Evaporated at
case, the observed percentage distilled is 18 % and
Evaporated, mL
93.3 °C (200 °F) R 5 2.011.74 ~ S C ! (X2.2)
18.4
10 83 182
20 94 201 52.011.74 3 1.1
30 103 217
40 111 232 53.9
R 5 3.611.74 ~ S F !
X2.1 Some specifications require the reporting of the vol- 53.611.74 3 1.9
ume % evaporated or recovered at a prescribed temperature.
Table X2.1 shows the distillation data of a Group 1 sample as 56.9
obtained by a manual unit. X2.2.3 From the calculated value of R, determine the value
X2.2 Example Calculation of volume, as described in A4.10.
R volume % 5 R/ ~ S C ! (X2.3)
X2.2.1 For a Group 1 sample exhibiting distillation charac-
teristics as per Table X2.1, as determined by a manual unit, the 53.9/1.1
reproducibility of the volume evaporated, Rvolume %, at
93.3 °C (200 °F) is determined as follows: 53.5
X2.2.1.1 Determine first the slope at the desired tempera-
ture: R volume % 5 R/ ~ S F !
S C % 5 0.1 ~ T ~ 20! 2 T ~ 10! ! (X2.1) 56.9/1.9
50.1 ~ 94 2 83! 53.6
23
D86 − 16a
FIG. X3.1 Corrected Loss from Observed Loss and Barometric Pressure kPa
X3. TABLES OF CORRECTED LOSS FROM MEASURED LOSS AND BAROMETRIC PRESSURE
X3.1 The table presented as Fig. X3.1 can be used to X3.2 The table presented as Fig. X3.2 can be used to
determine the corrected loss from the measured loss and the determine the corrected loss from the measured loss and the
barometric pressure in kPa. barometric pressure in mm Hg.
24
D86 − 16a
FIG. X3.2 Corrected Loss from Observed Loss and Barometric Pressure mm Hg
X4. PROCEDURE TO EMULATE THE EMERGENT STEM ERROR OF A

MERCURY-IN-GLASS THERMOMETER
X4.1 When an electronic or other sensor without an emer- ASTM 7C T elr 5 T t 2 0.000162 3 ~ T t 2 20°C ! 2
(X4.1)
gent stem error is used, the output of this sensor or the
associated data system should emulate the output of a mercury- X4.3 When a high range thermometer would have been
in-glass thermometer. Based on information supplied by four used, no stem correction is to be applied below 35°C. Above
manufacturers of automated Test Method D86 equipment, the this temperature the correction is calculated using the follow-
averaged equations shown in X4.2 and X4.3 have been ing formula:
reported to be in use. 2
ASTM 8C T ehr 5 T t 2 0.000131 3 ~ T t 2 35°C ! (X4.2)
X4.1.1 The equations shown in X4.2 have limited applica-
bility and are shown for information purposes only. In addition where:
to the correction for the emergent stem, the electronic sensor Telr = emulated temperature in °C for low range
and associated data system will also have to emulate the lag in thermometers,
response time observed for mercury-in-glass thermometers. Tehr = emulated temperature in °C for high range
thermometers, and
X4.2 When a low range thermometer would have been used, Tt = true temperature in °C.
no stem correction is to be applied below 20°C. Above this
temperature, the correction is calculated using the following
formula:
25
D86 − 16a
FIG. X5.1 Percent Recovered Report Form
X5. EXPLANATORY REPORT FORMS
X5.1 Fig. X5.1 and Fig. X5.2 show report forms.
26
D86 − 16a
FIG. X5.2 Percent Evaporated Report Form
27
D86 − 16a
SUMMARY OF CHANGES
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D86 – 16) that may impact the use of this standard. (Approved Aug. 1, 2016.)
(1) Added new subsection 10.11.1.
(D86 – 15) that may impact the use of this standard. (Approved July 1, 2016.)
(1) Updated Table 8 to revise precision for GROUP 4 T95 (4) Revised Research Report RR:D02-1621 to include descrip-
including additional sample data from original ILS. tion and D6300 outputs of revised T95 precision and tempera-
(2) Updated Table 8 to revise temperature range for GROUP 4 ture range.
T95 to include 360 °C.
(3) Updated Annex A1 to revise precision and temperature
range.
(D86 – 12) that may impact the use of this standard. (Approved Oct. 1, 2015.)
(1) Revised title and scope to include liquid fuels. (4) Added Note A4.2 to A4.10.1 for information on slope effect
(2) Updated Section 13 to include revised precision. on R.
(3) Updated Annex A1 to remove tables of NOT4 evaporated
precision, as they no longer apply.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/
28

D86-16a Distillation of Petroleum Products at Atmospheric Pressure

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SAI GLOBAL, Index House, Ascot, Berks, SL5 7EU, UK

SAI GLOBAL, 286 Sussex Street, Sydney NSW 2000, Australia

Designation: D86 − 16a

Standard Test Method for

1. Scope* its vapor, may be hazardous to health and corrosive to

*A Summary of Changes section appears at the end of this standard

1–Condenser bath 11–Distillation flask

FIG. 2 Apparatus Assembly Using Electric Heater

FIG. 3 PTFE Centering Device for Ground Glass Joint

6.3.1.1 Thermometers that have been exposed for an ex-

TABLE 3 Preparation of Apparatus and Specimen

ASTM/IP true boil- Group 4 Group 4 Group 4 Group 4

10. Procedure 10.5 Fit the temperature sensor through a snug-fitting

FIG. 6 Example of One Manufacturer’s Recommended Placement

A1. PRECISION TABLES FOR REPEATABILITY (r) AND REPRODUCIBILITY (R)

A1.1 Tables: 210 0.86 3.15

A2. DETAILED DESCRIPTION OF APPARATUS

A2.1 Distillation Flasks—Flasks shall be of heat resistant Borosilicate = Quartz + 0.40

FIG. A2.2 Detail of Upper Neck Section

NOTE 1—1 mL graduations – minimum 5 mL to 100 mL

TABLE A4.4 Repeatability and Reproducibility for Group 1

% volume at 0.7+0.92/SC 0.7+1.66/SF 1.5+1.78/SC 1.53+3.20/SF

X1. EXAMPLES ILLUSTRATING CALCULATIONS FOR REPORTING OF DATA

X1.1 The observed distillation data used for the calculation

X1.1.2 Loss correction to 101.3 kPa (see 11.4) are as

$ 11 ~ 101.3 2 98.6! /8.0% 5 3.6

X2. EXAMPLES OF CALCULATION OF REPEATABILITY AND REPRODUCIBILITY OF VOLUME % (RECOVERED OR

TABLE X2.1 Distillation Data from a Group 1 Sample Manual 51.1

S C % 5 0.1 ~ T ~ 20! 2 T ~ 10! ! (X2.1) 56.9/1.9

50.1 ~ 94 2 83! 53.6

X4. PROCEDURE TO EMULATE THE EMERGENT STEM ERROR OF A

FIG. X5.1 Percent Recovered Report Form

X5. EXPLANATORY REPORT FORMS

X5.1 Fig. X5.1 and Fig. X5.2 show report forms.

FIG. X5.2 Percent Evaporated Report Form

(1) Added new subsection 10.11.1.

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