An American National Standard

Designation: D 86 – 05

Standard Test Method for

Distillation of Petroleum Products at Atmospheric Pressure 1
This standard is issued under the fixed designation D 86; the number immediately following the designation indicates the year of original
adoption
adopt ion or, in the case of revisio
revision,
n, the year of last revision.
revision. A numb
number
er in parentheses indicates
indicates the year of last reapproval.
reapproval. A supers
superscript
cript
epsilon (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope
Scope*
* D 97  Test Method for Pour Point of Petroleum Products
1.1 This test method covers the atmospheric
atmospheric distillati
distillation
on of  D 323   Test Method for Vapor Pressure of Petroleum Prod-
petroleum products using a laboratory batch distillation unit to ucts (Reid Method)
determine
deter mine quant
quantitat
itativel
ivelyy the boili
boiling
ng range charcharacte
acterist
ristics
ics of  D 2892   Test
Test Meth
Methodod for Dist
Distilla
illation
tion of Crude Petroleum
Petroleum
such products as natural gasolines, light and middle distillates, (15-Theoretical Plate Column)
automotive
autom otive spar
spark-ign
k-ignitio
ition
n engin
enginee fuel
fuels,
s, avia
aviation
tion gaso
gasolines
lines,, D 4057   Practic
Practicee for Man
Manual
ual Sam
Sampli
pling
ng of Pet
Petrol
roleum
eum and
aviati
avi ation
on tur
turbin
binee fue
fuels,
ls, 1-D and 2-D reg regula
ularr and low sul sulfur
fur Petroleum Products
diesel fuels, special petroleum spirits, naphthas, white spirits, D 4177   Practice for Automatic Sampling of Petroleum and
kerosines, and Grades 1 and 2 burner fuels. Petroleum Products
1.2 The test method is designed for the analysis analysis of distillate D 4953   Test
Test Meth
Methodod for Vapor
Vapor Pres
Pressure
sure of Gasol
Gasoline
ine and
fuels; it is not applicable to products containing appreciable Gasoline-Oxygenate Blends (Dry Method)
quantities of residual material. D 5190  Test Method for Vapor Pressure of Petroleum Prod-
1.3 Thi
Thiss tes
testt met
method
hod cov
covers
ers bot
both
h man
manualual and aut automa
omatedted ucts (Automatic Method)
instruments. D 5191  Test Method for Vapor Pressure of Petroleum Prod-
1.4 Unles
Unlesss otherwise
otherwise noted, the values statedstated in SI unit
unitss are ucts (Mini Method)
to be regarded as the standard. The values given in parentheses D 5482  Test Method for Vapor Pressure of Petroleum Prod-
are provided for information only. ucts (Mini Method-Atmospheric)
1.5   This sta
standa
ndard rd does not purport
purport to addaddreress
ss all of the D 5949  Test Method for Pour Point of Petroleum Products
safe
sa fety
ty co
conc
ncer
erns
ns,, if ananyy, as
asso
soci
ciat
ated
ed wi
with
th it
itss us
use.
e. It is ththee (Automatic Pressure Pulsing Method)
responsibility of the user of this standard to establish appro- D 5950  Test Method for Pour Point of Petroleum Products
 priate safety and health practices and determine the applica- (Automatic Tilt Method)
bility of regulatory limitations prior to use. D 5985  Test Method for Pour Point of Petroleum Products
(Rotational Method)
2. Referenced Documents E 1  Specification for ASTM Liquid-in-Glass Thermometers
2.1 All sta
standa
ndards
rds are sub
subjec
jectt to rev
revisi
ision,
on, and par
partie
tiess to E 77   Test Method for Inspection and Verification of Ther-
agreement on this test method are to apply the most recent mometers
editio
edition
n of the sta
standa
ndards
rds ind
indica
icated
ted bel
below
ow,, unl
unless
ess oth
otherw
erwise
ise E 1272  Specification for Laboratory Glass Graduated Cyl-
specified, such as in contractual agreements or regulatory rules inders
where
whe re ear
earlie
lierr ver
versio
sions
ns of the met
method
hod(s)
(s) ide
identi
ntified
fied may be E 1405   Spec
Specifica
ification
tion for Labor
Laborator
atory
y Glass Dist
Distilla
illation
tion
required. Flasks
2.2   ASTM Standards:   2 2.3   Energy Institute Standards:3
Institute Standards:
IP 69  Determination of Vapour Pressure—Reid Method
IP 123   Petroleum Products—Determination
Products—Determination of Distillation
1
Thiss test method
Thi method is und
under
er the jurisdicti
jurisdiction
on of ASTM Committee
Committee D02 on Characteristics
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
IP 394  Determination of Air Saturated Vapour Pressure
D02.08 on Volatility.
In the IP, the equivalent test method is published under the designation  IP 123.
123. IP Standard Methods for Analysis and Testing of Petroleum
It is under the jurisdiction of the Standardization Committee. and Related Products
Products 1996—Appendix
1996—Appendix A
Currentt edition approved July 1, 2005
Curren 2005.. Publis
Published
hed August 2005. Origin
Originally
ally
approved in 1921. Last previous edition approved in 2004 as D 86-04b.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@
service@astm.or
astm.org. For   Annual Book of ASTM 
g. For
3
Standards volume
Standards  volume information, refer to the standard’s Document Summary page on Availabl
vailablee from the Energ
Energy
y Institu
Institute,
te, 61 New Cavendish St., London, W1G
the ASTM website
website.. 7AR, UK.

*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
 

D 86 – 05
TABLE 1 Preparation of Apparatus
Apparatus
Group 0 Group 1 Group 2 Group 3 Group 4
Flask, mL 100 125 125 125 125
ASTM distillation thermometer 7C (7F) 7C (7F) 7C (7F) 7C (7F) 8C (8F)
IP distillation thermometer range low low low low high
Flask support board A B B C C
diameter of hole, mm
mm 32 38 38 50 50
Temperature at start of test
Flask °C 0–5 13–18 13–18 13–18 not above
°F 32–40 55–65 55–65 55–65 ambient
Flask support and shield not above not above not above not above

Receiving cylinder and 100 mL ambient ambient ambient ambient

charge
°C 0–5 13–18 13–18 13–18A 13–ambientA
°F 32–40 55–65 55–65 55–65A 55–ambientA
A
See   10.3.1.1 for
See 10.3.1.1  for exceptions.

3. Terminology 3.1.7   end point (EP) or final boiling point (FBP),   n—the
3.1   Definitions: maximum corrected thermometer reading obtained during the
3.1.1   charge volume,   n—the volume of the specimen, 100 test.
mL, charged to the distillation flask at the temperature speci- 3.1.7.1   Discussion—This usually occurs after the evapora-
fied in Table
in  Table 1.
1. tion
tion of al alll li
liqu
quid
id fr
from
om th thee bo
bott
ttom
om of th
thee fla
flask
sk.. Th
Thee te
term
rm
3.1.2   decomposition,  n —of a hydrocarbon, the pyrolysis or maximum temperature is a frequently used synonym.
cracking of a molecule yielding smaller molecules with lower 3.1.8   front losss,   n—lo
front end los —lossss due to eva
evapor
porati
ation
on dur
during
ing
boiling points than the original molecule. transfer from receiving cylinder to distillation flask, vapor loss
3.1.2.1   Discussion—Char
—Character
acteristi
isticc indi
indicati
cations
ons of ther
thermal
mal during the distillation, and uncondensed vapor in the flask at
decomposition are evolution of fumes and erratic temperature the end of the distillation.
readings
readi ngs that usual
usuallyly decr
decrease
ease after any atte attempt
mpt is made to 3.1.9  initial boiling point (IBP) ,  n —the corrected thermom-
adjust the heat. eterr rea
ete readin
ding
g tha
thatt is obs
observ
erved
ed at the instant
instant the firs
firstt dro
dropp of 
3.1.3   decomposition
decomposition point ,   n—the corre corrected
cted ther
thermome
mometerter condensate falls from the lower end of the condenser tube.
readin
rea dingg tha
thatt coi
coinci
ncides
des wit
withh the firs
firstt ind
indica
icatio
tions
ns of the
therm
rmal
al 3.1.10   percent evaporated ,   n—the sum of the percent re-
decomposition of the liquid in the flask. covered and the percent loss.
3.1.3.1   Discussion—Th —Thee decdecomp
omposi ositio
tion
n poi
point,
nt, as det
deter
er-- 3.1.11   per
percen
centt los
losss (or obs
observerved
ed los s), n—one hundr
loss), hundred
ed
mined
min ed und
under
er the concondit
dition
ionss of thi
thiss tes
testt met
method
hod,, doe
doess not minus the percent total recovery.
necessari
neces sarily
ly corre
correspond
spond to the decom
decomposiposition
tion temp
temperat
erature
ure in 3.1.11.1   corrected loss, n—percent loss corrected for baro-
other applications. metric pressure.
3.1.4   dry point ,   n—the corrected thermometer reading that 3.1.12   percent
percent recover ed ,   n—th
recovered  —thee vol
volum
umee of con
conden
densat
satee
is observed at the instant the last drop of liquid (exclusive of  observed in the receiving cylinder, expressed as a percentage of 
any drops or film of liquid on the side of the flask or on the the charge volume, associated with a simultaneous temperature
temperature sensor), evaporates from the lowest point in the reading.
distillation flask. 3.1.13   percent recovery,
recovery, n—the maxi maximum
mum perc
percent
ent recov
recov--
3.1.4.1   Discussion—Th
—Thee end poi point
nt (fin
(final
al boi
boilin
lingg poi
point)
nt),, ered, as observed in accordance with  10.18
 10.18..
rather than the dry point, is intended for general use. The dry 3.1.13.1   corrected percent recovery, n—the percent recov-
point
point can be repreport
orted
ed in con
connecnecti
tion
on wit
with
h spe
specia
ciall pur
purpos
posee ery, adjusted for the difference between the observed loss and
naphthas, such as those used in the paint industry. Also, it is the corrected loss, as described in Eq 8.
substituted for the end point (final boiling point) whenever the 3.1.13.2   percent
percent tota
totall recoveryy, n—the combi
recover combined
ned perce
percent
nt
sample is of such a nature that the precision of the end point recovery and residue in the flask, as determined in accordance
(final boiling point) cannot consistently meet the requirements with 11.1
with  11.1..
given in the precision section. 3.1.14   percent
percent residue,   n—th
—thee vol
volume
ume of res residu
iduee in the
3.1.5   dynamic holdup,  n —the amount of material present in flask, measured in accordance with  10.19 10.19,,  and expressed as a
the neck of the flask, in the sidearm of the flask, and in the percentage of the charge volume.
condenser tube during the distillation. 3.1.15  rate of change (or slope) ,  n —the change in tempera-
3.1.6   emergent
emergent stem ef fect ,   n—the of
effect  offset
fset in temp
temperatu
erature
re ture reading per percent evaporated or recovered, as described
reading caused by the use of total immersion mercury-in-glass in 13.2
in  13.2..
thermometers in the partial immersion mode. 3.1.16   temperature lag,  n —the offset between the tempera-
3.1.6.1   Discussion—In the partial immersion mode, a por- ture reading obtained by a temperature sensing device and the

tion of the mercury thread, that is, the emergent portion, is at true temperature at that time.
a lower temperature than the immersed portion, resulting in a 3.1.17  temperature measurement device,  n —a thermometer,
shrink
shrinkage
age of the mer
mercur
cury
y thr
thread
ead and a low
lower
er tem
temper
peratu
ature
re as described in 6.3.1
in  6.3.1,,   or a temperature sensor, as described in
reading. 6.3.2..
6.3.2

2
 

D 86 – 05
3.1.18  temperature reading, n—the temperature obtained by
a temperature measuring device or system that is equal to the
thermometer reading described in  3.1.19
 3.1.19..
3.1.18.1  corrected temperature reading, n—the temperature
readin
rea ding,
g, as des
descri
cribed
bed in   3.1.18,
3.1.18,   correct
corrected
ed for baro
barometr
metric
ic
pressure.
3.1.19  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.
3.1.19.1   corrected thermometer reading, n—the thermom-
eter reading, as described in   3.1.19,
3.1.19,   corrected for barometric
pressure.

4. Summa
Summary
ry of Test Method
4.1 Based on its composition,
composition, vapor pressure, expected IBP
or expected EP, or combination thereof, the sample is placed in
one of five groups. Apparatus arrangement,
arrangement, condenser tempera-
ture, and other operational variables are defined by the group in
which the sample falls.
4.2 A 100100-mL
-mL specime
specimen n of the sample
sample is disdistil
tilled
led 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 FIG. 1 Apparatus Assembly Using Gas Burner
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 temperature or at high altitude, or both. The presence of high
data
da ta.. Th
Thee vo
volu
lume
me of th thee re
resi
sidu
duee anand
d th
thee lo
loss
sses
es araree al
also
so boiling point components in these and other fuels can signifi-
recorded. cantly
can tly af
affec
fectt the degdegree
ree of for
format
mation
ion of sol
solid
id com
combus
bustio
tion
n
4.3 At the conclusion of the distillation,
distillation, the observed vapor deposits.
temperatures can be corrected for barometric pressure and the 5.4 Volatility
olatility,, as it affects rate of evaporation, is an impor-
dataa are exa
dat examin
mineded for conconfor
forman
mance ce to proproced
cedura
urall req
requir
uire-
e- tant factor in the application
application of many solvents,
solvents, part
particula
icularly
rly
ments,
men ts, suc
such
h as dis
distil
tillat
lation
ion rat
rates.
es. The testestt is rep
repeat
eateded if any those used in paints.
specified condition has not been met. 5.5 Distillation limits
limits are often included in petroleum
petroleum prod-
4.4 Test results
results are commonly
commonly expressed
expressed as percent evapo- uct specifications, in commercial contract agreements, process
rated or percent recovered versus corresponding temperature, refinery/control applications, and for compliance to regulatory
either
either in a tabtable
le or gra
graphi
phical
cally
ly,, as a plo
plott of the distill
distillati
ation
on rules.
curve.
6. Appa
Apparatus
ratus
5. Signi
Significanc
ficancee and Use 6.1  Basic Components of the Apparatus:
5.1 The basic test method of determining
determining the boiling range 6.1.1 The basic components
components of the dist
distilla
illation
tion unit are the
of a petroleum product by performing a simple batch distilla- distillation flask, the condenser and associated cooling bath, a
tion has been in use as long as the petroleum industry has metal
met al shi
shield
eld or enc
enclos
losure
ure for the dis
distil
tillat
lation
ion flas
flask,
k, the hea
heatt
existed. It is one of the oldest test methods under the jurisdic- source, the flask support, the temperature measuring device,
tion of ASTM Committee D02, dating from the time when it and the receiving cylinder to collect the distillate.
was still referred to as the Engler distillation. Since the test 6.1.2   Figs. 1 and 2 and
2  and are examples of manual distillation
meth
me thod
od ha
hass be
been
en in ususee fo
forr su
such
ch an ex
exte
tend
nded
ed pe
peri
riod
od,, a units.
tremendous number of historical data bases exist for estimating 6.1.3 In addition to the basic components
components described in in  6.1.1
 6.1.1,,
end-use sensitivity on products and processes. automated units also are equipped with a system to measure
5.2 The dist
distilla
illation
tion (vol
(volatil
atility)
ity) chara
character
cteristi
istics
cs of hydro
hydrocar
car-- and automatically record the temperature and the associated
bons have an important effect on their safety and performance, recovered volume in the receiving cylinder.
especially in the case of fuels and solvents. The boiling range 6.2 A detailed description
description of the apparatus is given inin Annex
gives information on the composition, the properties, and the A2..
A2
behavior of the fuel during storage and use. Volatility is the 6.3  Temperature Measuring Device:
major determinant of the tendency of a hydrocarbon mixture to 6.3.1 Mercury-in-glas
Mercury-in-glasss thermometers, if used, shall
shall be filled
produce potentially explosive vapors. with an inert gas, graduated on the stem and enamel backed.
5.3 The dist
distilla
illation
tion chara
character
cteristi
istics
cs are crit
critical
ically
ly impo
importan
rtantt They
They sha
shall
ll con
confor
formm to Spe
Specifi
cificat
cation
ion   E 1   or IP St
Stan
anda
dard
rd
for both automotive and aviation gasolines, affecting starting, Methods for Analysis and Testing of Petroleum and Related
warm
wa rm-u
-up,
p, an
andd tetend
nden
ency
cy to va
vapo
porr lo
lock
ck at hihigh
gh op
oper
erat
atin
ing
g Products 1996, Appendix A, or both, for thermometers ASTM

3
 

D 86 – 05

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
 

D 86 – 05

FIG. 3 PTFE Centering

Centering Device for Groun
Ground
d Glass Joint

7C/IP 5C and ASTM 7F for the low range thermometers, and

ASTM 8C/IP 6C and ASTM 8F for the high range thermom-
eters.
6.3.1.1
6.3 .1.1 The
Therm
rmome
ometer
terss tha
thatt hav
havee bee
been
n exp
expose
osed
d 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   E 1  and Test Method 
Method   E 77.
77 .
NOTE  1—At an observed thermometer reading of 370°C, the tempera- FIG. 4 Example of Centering Device Designs for Straight-Bore
ture of th
ture thee bul
bulb
b is ap
appr
proa
oach
ching
ing a cr
criti
itica
call ra
range
nge in the glass
glass an
and
d the Neck Flasks
thermometer may lose its calibration.
6.3.2 Tempe
emperatu
rature
re meas
measurem
urement
ent syste
systems
ms other than those
described
descr ibed in   6.3.1   are satisfactory for this test method, pro-
vided that they exhibit the same temperaturetemperature lag, emer
emergent
gent
stem effect, and accuracy as the equivalent mercury-in-glass
thermometer.
6.3.2.1 The electronic
electronic circcircuitr
uitry
y or the algor
algorithm
ithms,
s, or both,
used shall include the capability to simulate the temperature lag
of a mercury-in-glass thermometer.
6.3.2.2
6.3.2.2 Alternat
Alternative
ivelyly,, the sen
sensor
sor can alsalso
o be pla
placed
ced in a
casing with the tip of the sensor covered so that the assembly,
because of its adjusted thermal mass and conductivity, has a
temper
tem peratu
ature
re lag tim
timee sim
simila
ilarr to tha
thatt of a mer
mercur
cury-i
y-in-g
n-glas
lasss
thermometer.
FIG. 5 Position of Thermometer in Distillation Flask 
NOTE   2—In a region where the temper
temperature
ature is changing rapidly during
the distillation, the temperature lag of a thermometer can be as much as 3
seconds.
a low IBP may have one or more readings obscured by the centering
6.3.3 In cas
6.3.3 casee of dis
disput
pute,
e, the referee
referee test method
method sha
shall
ll be device. See also 10.14.4.1
also  10.14.4.1..
carried out with the specified mercury-in-glass thermometer.
6.5 Autom
Automated
ated equipment
equipment manufactured
manufactured in 1999 and late
laterr
6.4  Temperature Sensor Centering Device:
shall be equipped with a device to automatically shut down
6.4.1 The temperature
temperature sensor shall be mounted through a
power to the unit and to spray an inert gas or vapor in the
snug-fitti
snug- fitting
ng devic
devicee desi
designed
gned for mech
mechanica
anically
lly cente
centering
ring the
chamber where the distillation flask is mounted in the event of 
sensor in the neck of the flask without vapor leakage. Examples
fire.
of acceptable centering devices are shown in   Figs. 3 and 4. 4.
(Warning
Warning—Th —Thee use of a pla plain
in stopper
stopper with a hol
holee dri
drille
lled
d NOTE  5—Some causes of fires are breakage of the distillation flask,
through the center is not acceptable for the purpose described electrical shorts, and foaming and spilling of liquid sample through the top
opening of the flask.
in 6.4.1
in  6.4.1.)
.)
6.6   Barometer —A
—A pressure
pressure meas
measuring
uring device capa
capable
ble of 
NOTE  3—Other centering devices are also acceptable, as long as they
position and hold the temperature sensing device in the proper position in
measuring local station pressure with an accuracy of 0.1 kPa (1
the neck of the distillation column, as shown in Fig.
in  Fig. 5 and
5  and described in mm Hg) or better, at the same elevation relative to sea level as

10.5
10.5..  4—When running the test by the manual method, products with
NOTE th
the
e ap
appa
para
readings ratu
tuss ordinary
from in th
thee aneroid
labo
labora
rato
tory
ry.. (Warning —Do
Warning—D
barometers, such asothose
nott used
no take
take

5
 

D 86 – 05
TABLE 2 Group Characteristics
Characteristics NOTE   6—If there are no, or ina
inadequ
dequate
ate,, fac
facilit
ilities
ies for storage
storage bel
below
ow
Grou
Group
p0 Grou
Group
p1 Grou
Group
p2 Grou
Group
p3 Grou
Group
p4 10°C, the sample may als
10°C, also
o be stor
stored
ed at a temtemper
peratu
ature
re bel
below
ow 20°
20°C,
C,
provided the operator ensures that the sample container is tightly closed
Sample
and leak-free.
characteristics
Distillate type natural 7.3.4   Group
Group 2—Stor
—Storee the sample at a temp
temperat
erature
ure below
gasoline
Vapor pressure at 10°C.
37.8°C, kPa   $ 65.5 <65.5 <65.5 <65.5
100°F, psi 9.5 <9.5 <9.5 <9.5
NOTE   7—If there are no, or ina
inadequ
dequate
ate,, fac
facilit
ilities
ies for storage
storage bel
below
ow
  $

(Test Methods 10°C, the sample may als

10°C, also
o be stor
stored
ed at a temtemper
peratu
ature
re bel
below
ow 20°
20°C,
C,
D 323,
323,   D 4953
4953,, provided the operator ensures that the sample container is tightly closed
D
D 5190,
5190
5482,,    D
5482, IP5191
5191,
69 or, and leak-free.
IP 394)
394) 7.3.5  Groups 3 and 4—Store the sample at ambient or lower
Distillation, IBP °C   #100 >100 temperature.
°F   #212 >212
EP °C   # 250   #250 >250 >250
7.4   Sample Conditioning Prior to Analysis:
°F   # 482   #482 >482 >482 7.4.1
7.4.1 Sample
Sampless sha shall
ll be con
condit
dition
ioned
ed to the tem temper
peratu
ature
re
shown in Table
in  Table 3 before
3  before opening the sample container.
7.4.1.1   Group 0—Samples shall be conditioned to a tem-
at weather stations and airports, since these are precorrected to perature of less than 5°C (40°F) before opening the sample
give sea level readings.) container.
7.4.1.2  Groups 1 and 2—Samples shall be conditioned to a
7. Sampl
Sampling,
ing, Storage,
Storage, and Sample Cond
Conditio
itioning
ning
temper
tem peratu
aturere of les
lesss tha
than
n 10°
10°C
C (50
(50°F)
°F) bef
before
ore ope
openin
ning
g the
7.1 Deter
Determine
mine the Group characteri
characteristic
sticss that correspond
correspond to sample container.
the sample to be tested (see  Table 2) 2). Where the procedure is 7.4.1.3   GrGrou
oups
ps 3 anandd 4—I
—Iff th
thee sa
samp
mple
le is nonott flu
fluid
id at
depend
dep endent
ent upon the group,
group, the section
section heaheadin
dingsgs wil
willl be so ambient temperature, it is to be heated to a temperature of 9 to
marked. 21°C
21°C abo
above ve its pou
pourr poi
point
nt (T
(Test
est Met
Method
hod   D 97,
97 ,   D 5949,   or
7.2   Sampling:
7.2.1 Sampl
Sampling
ing shall be done in accor
accordance
dance with Practice
Practice D 5985)
5985) pr prio
iorr to an
anal
alys
ysis
is.. If ththee sa
samp
mplele ha
hass papart
rtia
iall
lly
y or
complete
comp letely
ly solid
solidified
ified during storastorage,
ge, it shal
shalll be vigor
vigorously
ously
D 4057 
4057   or
or D
 D 4177 and
4177  and as described in Table
in  Table 3.3. shaken after melting prior to opening the sample container to
7.2.1.1   Group 0—Condition the sample container to below ensure homogeneity
homogeneity..
5°C, preferably by filling the bottle with the cold liquid sample 7.4.1.4
7.4.1. 4 If the sample is not fluid at room temperature,
temperature, the
and discarding the first sample. If this is not possible because, temperature ranges shown in Table
in  Table 3 for
3  for the flask and for the
for instance, the product to be sampled is at ambient tempera- sample do not apply.
ture,
tur e, the sample
sample sha
shall
ll be dra
drawn
wn int
intoo a bot
bottle
tle,, pre
prechi
chille
lled
d to 7.5   Wet Samples:
belo
be loww 5°5°C,
C, in su
such
ch a ma
mannnner
er th
that
at ag
agit
itat
atio
ionn is ke kept
pt at a 7.5.1 Samples of materials
materials that visibly contain
contain water are not
minimum.
mini mum. Close the bott bottle
le imme
immediate
diately
ly with a tighttight-fitti
-fitting
ng suitable for testing. If the sample is not dry, obtain another
closure and place the sample in an ice bath or refrigerator. sample that is free from suspended water.
7.2.1.2   Group 1—Collect the sample as described in 7.2.1.1in  7.2.1.1 7.5.2   Grou
Groupsps 0, 1, an
and d 2—I—Iff su such
ch a sasamp
mple le ca
cann
nnot
ot be
at a temperature below 10°C. If this is not possible because, for obtained, the suspended water can be removed by maintaining
instance, the product to be sampled is at ambient temperature, thee sa
th samp
mple
le at 0 to 10 10°C
°C,, adaddi
ding
ng ap appr
prox
oxim
imatatel
ely
y 10 g of 
the sample shall be drawn into a bottle prechilled to below anhydrous sodium sulfate per 100 mL of sample, shaking the
10°C, in such a manner that agitation is kept at a minimum. mixtu
mi xture
re for app
approx
roxima
imatel
tely
y 2 mi min,n, and the thenn all
allowi
owing
ng the
Close the bot
Close bottle
tle imm
immedi
ediate
ately
ly wit
with
h a tig tight-
ht-fitt
fitting
ing cloclosur
sure.
e. mixture to settle for approximately 15 min. Once the sample
(Warning
Warning—Do —Do not completely fill and tightly seal a cold bottle shows no visible signs of water, use a decanted portion of the
of sample because of the likelihood of breakage on warming.) sample, maintained between 1 and 10°C, for the analysis. Note
7.2.1.3   Groups 2, 3, and 4—Collect the sample at ambient in the report that the sample has been dried by the addition of 
temperature. After sampling, close the sample bottle immedi- a desiccant.
ately with a tight-fitting closure.
7.2.1.4 If the samp
sample
le received
received by the test testing
ing laboratory
laboratory has NOTE  8—Suspended water in hazy samples in Groups 1 and 2 can be
removed by the addition of anhydrous sodium sulfate and separating the
been sampled by others and it is not known whether sampling
liquid sample from the drying agent by decanting without statistically
has been performed as described in   7.2 7.2,,   the sample shall be affecting the results of the test.4
assumed to have been so sampled.
7.3   Sample Storage: 7.5.3   Grou
Groups
ps 3 an d 4—In cases in whi
and which
ch a wat
water
er-fr
-free
ee
7.3.1 If testing is not to star
startt imm
immediat
ediatelyely after collection,
collection, sample is not practical, the suspended water can be removed by
store the samples as indicated in 7.3.2
in  7.3.2,,  7.3.3
 7.3.3,,  7.3.4
 7.3.4,,  and  Table shaking
shak ing the sampl
samplee with anhydrous
anhydrous sodi
sodium
um sulfa
sulfate
te or othe
otherr
3. All samples shall be stored away from direct sunlight or suitable drying agent and separating it from the drying agent by
sources of direct heat. decanting. Note in the report that the sample has been dried by
the addition of a desiccant.
7.3.2   Group
Group 0—Sam
—Samples
ples shall be stored
stored in a refr
refriger
igerator
ator
below a temperature of 5°C.
7.3.3   Group 1—Stor
—Storee the sample at a temperat
temperature
ure below 4
Supporting
Supporting data have been filed at ASTM International
International Headquarters and may
10°C. be obtained by request
requesting
ing Research Repor
Reportt RR: D02-1455.
D02-1455.

6
 

D 86 – 05
TABLE
TABLE 3 Sampling, Storage, and Sample Conditioning
Conditioning
Group 0 Group 1 Group 2 Group 3 Group 4
Temperature of sample bottle °C <5 <10
°F <40 <50
Temperature of stored sample °C <5 <10A <10 ambient ambient
°F <40 <50A <50 ambient ambient
Temperature of sample after °C <5 <10 <10 Ambient or Ambient or
conditioning prior to analysis 9 to 21°C above pour pointB 
°F <40 <50 <50 Ambient or Ambient or
48 to 70°F above pour point B 
If sample is wet resample resample resample dry in accordance with  7.5.3
C 

If resample is still wet dry in accordance with 7.5.2

with  7.5.2
A
Under certain circumstances, samples can also be stored at temperatures below 20°C (68°F). See also  7.3.3
 7.3.3 and
 and  7.3.4
 7.3.4..
B 
If sample is (semi)-solid at ambient temperature, see also  10.3.1.1
 10.3.1.1..
C 
If sample is known to be wet, resampling may be omitted. Dry sample in accordance with  7.5.2
 7.5.2 and
 and  7.5.3
 7.5.3..

8. Prep
Preparati
aration
on of Apparatus
Apparatus 9.1.2.1
9.1.2. 1 If the temp
temperat
erature
ure reading is not withi
within
n the values
8.1 Ref
Refer
er to Table
to Table 1 and
1  and prepare the apparatus by choosing shown in Table
in  Table 4 for
4  for the respective apparatus being used (see
the appro
appropria
priate
te disti
distillat
llation
ion flask, temp
temperat
erature
ure meas
measuring
uring de- Note 10   and   Table
Table 4), the temp
temperat
erature
ure meas
measurem
urement
ent syst
system
em
vice,
vice, and flas
flaskk sup
suppor
portt boa
board,
rd, as dir
direct
ected
ed for the ind
indica
icated
ted shall be considered defective and shall not be used for the test.
group.. Bring the temp
group temperat
erature
ure of the rece
receivin
iving
g cyli
cylinder
nder,, the NOTE  9—Toluene is used as a verification fluid for calibration; it will
flask, and the condenser bath to the indicated temperature. yield alm
yield almost
ost no inf
inform
ormati
ation
on on how wel
welll an ele
electr
ctronic
onic measurem
measurement
ent
8.2 Make any necessary
necessary provisions
provisions so that the temperature
temperature system simulates the temperature lag of a liquid-in-glass thermometer.
of th
thee co
cond
nden
ense
serr ba
bath
th an
andd th
thee re
rece
ceiv
ivin
ing
g cy
cyli
lind
nder
er wi
will
ll be 9.1.2.2 Rea
9.1.2.2 Reagen
gentt gra
grade
de tol
toluen
uenee and hex
hexade
adecan
canee (ce
(cetan
tane),
e),
maintained at the required temperatures. The receiving cylin- conforming to the specifications of the Committee on Analyti-
der shall be in a bath such that either the liquid level is at least Society,6 shall be used.
cal Reagents of the American Chemical Society,
as high as the
surrounded by100-mL mark or the
an air circulation entire receiving cylinder is
chamber. However, other grades may also be used, provided it is first
ascertained that the reagent is of sufficient purity to permit its
8.2.1   Gr
Grou
oupps 0, 1, 2, and 3—Su —Suitaitable
ble med
media
ia for low use without lessening the accuracy of the determination.
temperature baths include, but are not limited to, chopped ice
NOTE   10—At
10—At 101.101.33 kPa
kPa,, tolu
toluene
ene is show
shownn in ref
refere
erence
nce manuals
manuals as
and water, refrigerated brine, and refrigerated ethylene glycol.
boiling at 110.6°C when measured using a partial immersion thermometer.
8.2.2   Group 4—Suitable media for ambient and higher bath Because this test method uses thermometers calibrated for total immer-
temperatures include, but are not limited to, cold water, hot sion, the results typically will be lower and, depending on the thermometer
water, and heated ethylene glycol. and the situation, may be different for each thermometer. At 101.3 kPa,
8.3 Rem
Removeove any res
residu
idual
al liq
liquid
uid in the condense
condenserr tub
tubee by hexadecane is shown in reference manuals as boiling at 287.0°C when
swabbing with a piece of soft, lint-free cloth attached to a cord measur
mea sured
ed usin
usingg a par
partial
tial imm
immers
ersion
ion the
thermo
rmomet
meter er.. Bec
Becaus
ausee this tes
testt
or wire. method uses thermo
thermometers
meters calibrated
calibrated for total immer
immersion,
sion, the result
resultss
typical
typically
ly wil
willl be lowe
lower,r, and, dep
depend
ending
ing on the thermomet
thermometer er and the
9. Cali
Calibrati
bration
on and Stand
Standardiz
ardizatio
ation
n situation,
situatio n, may be dif
differen
ferentt for each therm
thermometer
ometer..

9.1   Temperature
Temperature Measure
Measurementment System—T —Temperature
emperature mea- 9.1.3 A procedure
procedure to dete
determin
rminee the magni
magnitude
tude of the tem-
surement systems using other than the specified mercury-in- perature lag is described in Annex
in  Annex A3.
A3.
glass thermometer
thermometerss shal
shalll exhib
exhibitit the same temperature
temperature lag, 9.1.4 A procedure
procedure to emul
emulate
ate the emer
emergent
gent stem effect
effect is
emergent stem effect, and accuracy as the equivalent mercury- described in Appendix
in  Appendix X4.
X4.
in-glass thermometer. Confirmation of the calibration of these 9.1.5 To verif
verify
y the calibration
calibration of the temperature
temperature measure-
measure-
temperature measuring systems shall be made at intervals of  ment system at eleva
elevated
ted temp
temperatu
eratures,
res, use hexad
hexadecan
ecane.e. The
nott mo
no more re th
than
an si
six
x mo
mont
nthshs,, an
and
d afafte
terr th
thee sy
syst
stem
em ha
hass be
been
en temperature measurement system shall indicate, at 50% recov-
replaced or repaired. ered, a temperature comparable to that shown in Table
in  Table 4 for
4  for the
9.1.1
9.1.1 The accaccura
uracy
cy and the cal calibr
ibrati
ation
on of the ele
electr
ctroni
onicc respective apparatus under Group 4 distillation conditions.
circuitry or computer algorithms, or both, shall be verified by NOTE  11—Because of the high melting point of hexadecane, Group 4
the use of a standard precision resistance bench. When per- verificatio
verification
n dist
distilla
illation
tionss will have to be car
carrie
ried
d out with condenser
condenser
forming this verification, no algorithms shall be used to correct temperatures >20°C.
the tem
temper
peratu
ature
re for lag and the eme emerg rgent
ent ste
stem
m ef
effec
fectt (se
(seee 9.2   Automated Method :
manufacturer’s instructions). 9.2.1   Level Follower —For
—For an automated distillation appa-
9.1.2 Verification of the calibration of temperature measur- ratus, the level follower/recording mechanism of the apparatus
ing devices shall be conducted by distilling toluene in accor-
dance with Group 1 of this test method and comparing the
4.5
6
50 % recovered temperature with that shown in  Table 4. Specificationss, Amer
 Reagent Chemicals, American Chemical Society Specification American
ican

Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see   Analar Standards for Laboratory
Chemicals,   BDH Ltd., Poole, Dorset, U.K., and the  United States Pharmacopeia
5
Supporting
Supporting data have been filed at ASTM International
International Headquarters
Headquarters and may and National Formulary, 
Formulary,  U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
be obtained
obtained by request
requesting
ing Research Report RR: D02–1580.
D02–1580. MD.

7
 

D 86 – 05
TABLE 4 Tru
True
e and Min and Max D 86 50 % Recovered Points (°C)A
Recovered Boiling Points
Manual Automated
Distillation Distillation Distillation Distillation
conditions min conditions conditions min conditions max
D 86 50 % max D 86 D 86 50 % D 86 50 %
boiling point 50 % boiling boiling point boiling point
point
ASTM/IP true Group 1, 2, and Group 1, 2, Group 1, 2, and Group 1, 2,
Toluene boiling point 3 and 3 3 and 3
110.6 105.9 111.8 108.5 109.7

ASTM/IP true Group 4 Group 4 Group 4 Group 4

Hexadecane boiling 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  3  sigma. Information on the values in this table can be found in RR:D02–1580.

shall have a resolution of 0.1 mL or better with a maximum receiving cylinder as completely as practical into the distilla-
erro
errorr of 0.
0.3
3 mL betwe
between
en th
thee 5 an
and
d 10
100
0 mL po poin
ints
ts.. Th
Thee tion flask, ensuring that none of the liquid flows into the vapor
calibration of the assembly shall be verified in accordance with tube.
manufacturer’s instructions at intervals of not more than three
NOTE   14—Any material that evaporates during the transfer will con-
months and after the system has been replaced or repaired. tribute to the loss; any material that remains in the receiving cylinder will
NOTE   12—The
12—The typical calibr
calibration
ation procedure involves verify
verifying
ing the contribute to the observed recovery volume at the time of the IBP.
output with the receiver containing 5 and 100 mL of material respectively. 10.4 If the sample can be expected to demonstrate
demonstrate irregular
9.2.2   Barometric Pressur
Pressuree—At intervals of not more than boiling behavior, that is, bumping, add a few boiling chips to
six months, and after the system has been replaced or repaired, the specimen. The addition of a few boiling chips is acceptable
the bar
barome
ometri
tricc rea
readin
ding
g of the ins
instru
trumen
mentt sha
shall
ll be ver
verifie
ified
d for any distillation.
against a barometer, as described in   6.6
6.6.. 10.5 Fit the temp
temperatu
erature re sensor through a snug-
snug-fitti
fitting
ng de-
vice, as described in in   6.4
6.4,,   to mechanically center the sensor in
10. Proc
Procedur
eduree the neck of the flask. In the case of a thermometer, the bulb is
10.1 Recor
Record
d the prevailing
prevailing barometric
barometric pressure.
pressure. centered in the neck and the lower end of the capillary is level
10.2   Grou
Groups
ps 0, 1, anandd 2—Fi
—Fitt a low ranrange
ge the
therm
rmome
ometer
ter with the highest point on the bottom of the inner wall of the
provided with a snug-fitting cork or stopper of silicone rubber, vapor
vap or tub
tubee (se
(seee   Fig.
Fig. 5). In th thee ca
case
se of a th
ther
ermo
moco
coup
uple
le or
or equivalent polymeric material, tightly into the neck of the resistance thermometer, follow the manufacturer’s instructions
sample container and bring the temperature of the sample to the as to placement.
temperature indicated in Table
in  Table 3.
3. NOTE   15—If
15—If va
vacu
cuum
um grgrea
ease
se is us
used
ed on the mating
mating sur
surfa
face
ce of the
10.3  Groups 0, 1, 2, 3, and 4—Check that the temperature centering device, use the minimum amount of grease that is practical.
of th
thee sa
samp
mple
le is as sh
show
own n in   Table
Table 3. Pou
Pourr the specimen
specimen 10.6 Fit the flask vapor tube, provided
provided with a snug-
snug-fitti
fitting
ng
precisely to the 100-mL mark of the receiving cylinder, and cork or rubbe
rubberr stopp
stopper
er of sili
silicone,
cone, or equiv
equivalen
alentt poly
polymeri
mericc
transfer the contents of the receiving cylinder as completely as material, tightly into the condenser tube. Adjust the flask in a
practical into the distillation flask, ensuring that none of the vert
ve rtic
ical
al po
posi
siti
tion
on so ththat
at th
thee va
vapo
porr tu
tube
be ex
exte
tend
ndss in
into
to th
thee
liquid flows into the vapor tube. condenser tube for a distance from 25 to 50 mm. Raise and
NOTE   13—It is important that the difference between the temperature of  adjust the flask support board to fit it snugly against the bottom
the specimen and the temperature of the bath around the receiving cylinder of the flask.
is as sma
small
ll as pra
practi
ctical
cally
ly poss
possible
ible.. A dif
differ
ferenc
encee of 5°C can mak
makee a 10.7 Place the receiving
receiving cylinder
cylinder that was used to measure
measure
difference of 0.7 mL. the specimen, without drying the inside of the cylinder, into its
10.3.1  Groups 3 and 4—If the sample is not fluid at ambient temperature-controlled bath under the lower end of the con-
temperature, it is to be heated to a temperature between 9 and denser tube. The end of the condenser tube shall be centered in
21°C above its pour point (Test Method D
Method  D 97, D 5949, D 5950, the receiving cylinder and shall extend therein for a distance of 
or D 5985)
5985) pri
prior
or to ana
analys
lysis.
is. If the sample
sample has partial
partially
ly or at least 25 mm, but not below the 100-mL mark.
comple
com pletel
tely
y sol
solidi
idified
fied in the int interv
erveni
ening
ng per
period
iod,, it sha
shall
ll be 10.8   Initial Boiling Point :
vigoro
vig orousl
usly
y sha
shaken
ken aft
after
er mel
melti
ting,
ng, and pri
prior
or to sam
sampli
pling,
ng, to 10.8.1   Manual Method —To —To reduce evaporation loss of the
ensure homogeneity. distillate, cover the receiving cylinder with a piece of blotting
10.3.1.1
10.3.1 .1 If the sample is not fluid at ambiambient
ent temperatur
temperatures,es, paper, or similar material, that has been cut to fit the condenser
disreg
disregard
ard the tem
temper
peratu
ature
re ran
rangege sho
shown
wn in   Table
Table 1   for the tubee snu
tub snugly
gly.. If a rec
receiv
eiver
er defl
deflect
ector
or is bei
being
ng use
used,
d, sta
start
rt the
receiving
receiving cyl
cylind
inder
er and sam
sample
ple.. Pri
Prior
or to ana
analys
lysis,
is, hea
heatt the distillation with the tip of the deflector just touching the wall of 
receiving cylinder to approximately the same temperature as the receiving cylinder. If a receiver deflector is not used, keep
the sample. Pour the heated specimen precisely to the 100-mL thee dr
th drip
ip ti
tip
p of th
thee co
cond
nden
ense
serr aw
away
ay fr
from
om ththee wa
wall
ll of th
thee
mark of the receiving cylinder, and transfer the contents of the receiving cylinder. Note the start time. Observe and record the

8
 

D 86 – 05
TABLE
TABLE 5 Conditions During Test
Test Procedure
Group 0 Group 1 Group 2 Group 3 Group 4
A
Temperature of cooling bath °C 0–1 0–1 0–5 0–5 0–60
°F 32–34 32–34 32–40 32–40 32–140
Temperature of bath around °C 0–4 13–18 13–18 13–18   63
receiving cylinder °F 32–40 55–65 55–65 55–65   65
of charge
temperature
Time from first application of heat to
initial boiling point, min 2–5 5–10 5–10 5–10 5–15
Time from initial boiling point
to 5 % recovered, s 60–100 60–100
to 10 % recovered, min 3–4
Uniform average rate of condensation
from 5 % recovered to 5 mL
in flask, mL/min 4–5 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 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
formation in the condenser can be deduced from (a 
(a ) the presence of wax particles in the distillate coming off the drip tip, (b 
(b ) a higher distillation
loss than what would be expected based on the initial boiling point of the specimen, (c  ( c ) an erratic recovery rate and (d 
(d ) the presence of wax particles during the removal
of residual liquid by swabbing with a lint-free cloth (see  8.3
 8.3)). The minimum temperature that permits satisfactory operation shall be used. In general, a bath temperature
in the 0 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 to 60°C range.

IBP to the nearest 0.5°C (1.0°F). If a receiver deflector is not tion and reporting of the results of the test as required by the
being used, immediately move the receiving cylinder so that specificat
spec ification
ion invol
involved,
ved, or as previ
previously
ously established
established for the
the tip of the condenser touches its inner wall. sample under test. These observed data can include tempera-
10.8.2   Automated Method —To
—To reduce evaporation loss of  ture readings at prescribed percentages recovered or percent-
the dis
distil
tillat
late,
e, use the dev device
ice pro
provid
vided
ed by the insinstru
trumen
mentt ages recovered at prescribed temperature readings, or both.
manufacturer for this purpose. Apply heat to the distillation 10.14.1   Manual Method —Record
—Record all volumes in the gradu-
flask and contents with the tip of the receiver deflector just ated
ated cy
cyli
lind
nder
er to th
thee ne
near
ares
estt 0.
0.5
5 mL
mL,, an
andd al
alll te
temp
mper
erat
atur
uree
touching the wall of the receiving cylinder. Note the start time. readings to the nearest 0.5°C (1.0°F).
Record the IBP to the nearest 0.1°C (0.2°F). 10.14.2   Automated
Automated Meth od —Rec
Method  — Recor
ord
d al
alll vo
volulume
mess in ththee
10.9 Regul
Regulateate the heating so that the time interval
interval between
between receiving cylinder to the nearest 0.1 mL, and all temperature
the first application of heat and the IBP is as specified in Table
in  Table readings to the nearest 0.1°C (0.2°F).
5. 10.14.3   Group
Group 0—In cases in which no specific data re-
10.10 Regul
Regulateate the heating
heating so that the time from IBP to 5 or quirements have been indicated, record the IBP, the EP (FBP),
10 % recovered is as indicated in  Table 5. 5. and tem
temper
peratu
ature
re rea
readin
dings
gs at eac
eachh 10 % mul
multip
tiple
le of vol
volume
ume
10.11
10.1 1 Conti
Continuenue to regul
regulate
ate the heating so that the uniform
uniform recovered from 10 to 90, inclusive.
average rate of condensation from 5 or 10 % recovered to 5 mL
10.14.4  Group 1, 2, 3, and 4—In cases in which no specific
( Warning—Due
residue in the flask is 4 to 5 mL per min. (Warning —Due to
data requirements have been indicated, record the IBP and the
the configuration of the boiling flask and the conditions of the
EP (FBP) or the dry point, or both, and temperature readings at
test, the vapor and liquid around the temperature sensor are not
5, 15, 85, and 95 % recovered, and at each 10 % multiple of 
in thermodynamic equilibrium. The distillation rate will con-
sequently have an effect on the measured vapor temperature. volume recovered from 10 to 90, inclusive.
10.14.4.1   Group
Group 4—Wh
—When en a hig
highh ran
range
ge the
thermo
rmome
meter
ter is
The distillation
distillation rate shal
shall,
l, there
therefore,
fore, be kept as const
constant
ant as
used in testi
testing
ng aviat
aviation
ion turbi
turbine
ne fuels and simi
similar
lar products,
products,
possible throughout the test.)
pertinent thermometer readings can be obscured by the center-
NOTE   16—When testing gasoline samples, it is not uncommon to see ing device. If these readings are required, perform a second
the condensate suddenly form non-miscible liquid phases and bead up on distillation in accordance with Group 3. In such cases, reading
the temperature measuring device and in the neck of the boiling flask at a
from a low range thermometer can be reported in place of the
vapor temperature
temperature of around 160°C. This may be accompanied
accompanied by a sharp
(about 3°C) dip in the vapor temperature and a drop in the recovery rate. obscured high range thermometer readings, and the test report
The phenomenon, which may be due to the presence of trace water in the shall so indicate. If, by agreement, the obscured readings are
sample, may last for 10 to 30 s before the temperature recovers and the waived, the test report shall so indicate.
condens
cond ensate
ate star
starts
ts flow
flowing
ing smoo
smoothly
thly aga
again.
in. This poin
pointt is som
sometim
etimes
es 10.1
10 .14.
4.5
5 Wh
When en it is rerequ
quir
ired
ed to rerepo
port
rt th
thee te
temp
mper
erat
atur
uree
colloquially referred to as the Hesitation Point. reading at a prescribed percent evaporated or recovered for a
10.12 Repea
Repeatt any distillati
distillation
on that did not meet the require-
require- sample
samp le that has a rapi
rapidly
dly changing slope of the distillati
distillation
on
ments described in  10.9
 10.9,,  10.10
 10.10,,   and
and 10.11
 10.11.. curvee in the regi
curv region
on of the presc
prescribed
ribed percent
percent evapo
evaporated
rated or
10.13
10.13 If a dec
decomp
omposi
ositio
tion
n poi
point,nt, as des
descri
cribed
bed in   3.1.3,
3.1.3, is recovered reading, record temperature readings at every 1 %
observed, discontinue the heating and proceed as directed in recovered
recove red.. The slo
slope
pe is con
consid
sidere
ered
d rap
rapidl
idly
y cha
changi
ngingng if the
10.17..
10.17 change in slope (C ) of the data points described in 10.14.2
in  10.14.2   in
10.14
10. 14 In the int
interv
erval
al between
between the IBP and the end of the that particular area is greater than 0.6 (change of slope ( F ) is
distillation, observe and record data necessary for the calcula- greater than 1.0) as calculated by Eq 1 (Eq 2).

9
 

D 86 – 05
Change of Slope ~C ! 5 10.1
10 .19
9 Af
Afte
terr th
thee fla
flask
sk ha
hass co
cool
oled
ed an
andd no mo
more
re vavapo
porr is
~C 2 2 C 1! / ~V 2 2 V 1! 2 ~C 3 2 C 2! / ~V 3 2 V 2! observed, disconnect
observed, disconnect the flask from the conde condenser
nser,, pour its
(1) contents
contents into a 5-mL graduated
graduated cylinder,
cylinder, and with the flask 
suspended over the cylinder, allow the flask to drain until no
Change of Slope ~F ! 5 appreciable increase in the volume of liquid in the cylinder is
~F 2 2 F 1! / ~V 2 2 V 1! 2 ~F 3 2 F 2! / ~V 3 2 V 2! observed. Measure the volume in the graduated cylinder to the
(2)
nearest 0.1 mL, and record as percent residue.
where: 10.1
10 .19.
9.1
1 If ththee 5-
5-mL
mL grgrad
adua
uate
ted
d cy
cyli
lind
nder
er do
does
es nonott ha
have
ve
C 1   = tem
temper
peratu
ature
re at the volume
volume % rec
record
orded
ed one rea
readin
ding
g graduations below 1 mL and the volume of liquid is less than
prior to the volume % in question, °C, 1 mL, prefill the cylinder with 1 mL of a heavy oil to allow a
C 2   = temper
temperatu
ature
re at the volume
volume % rec record
orded
ed in que
questi
stion,
on, better estimate of the volume of the material recovered.
°C, 10.19.1.1 If a residue greater than expected
expected is obtained, and
C 3   = temp
temperat
erature
ure at the volume
volume % recorded
recorded followin
following
g the the distillation
distillation was not purp
purposely
osely terminated
terminated before the EP EP,,
volume % in question, °C, check whether adequate heat was applied towards the end of 
F 1   = tem
temper
peratu
ature
re at the volume
volume % rec record
orded
ed one rea
readin
dingg the distillation
distillation and wheth
whether
er cond
condition
itionss durin
duringg the test con-
prior to the volume % in question, °F, formed to those specified in  Table 5.
5. If not, repeat test.
F 2   = temperature at the volume % recorded in question, °F, °F,
F 3   = temp
temperat
erature
ure at the volume
volume % recorded
recorded followin
following
g the NOTE   18—Test Method D 86 distillation residues for gasoline, kero-
volume % in question, °F, sine, and dist
sine, distilla
illate
te die
diesel
sel are   typically   0.9–1.3,
0.9–1.3, 0.9–1.3, and 1.0–1.
1.0–1.4
4
volume %, respectively.
V 1   = volume % recorded one one reading prior to to the volume %
NOTE   19—The test method is not designe
designedd for the analys
analysis
is of distillat
distillatee
in question,
fuels containing appreciable quantities of residual material (see  1.2
 1.2)).
V 2   = volum
volumee % recorded
recorded at the
the volume
volume % in question,
question, and
and
V 3   = vo
volu
lume
me % re reco
cord
rded
ed fofoll
llow
owin
ing g th
thee vo
volu
lume
me % in 10.19.2   Group
Group 0—Co
—Coolol the 5-m
5-mL L gra
gradua
duated
ted cyl
cylind
inder
er to
question. below 5°C. Record the volume in the graduated cylinder, to the
10.15 When the residual liquid in the flask is is approximately nearest 0.1 mL, as percent residue.
5 mL, make a final adjustment of the heat. The time from the 10.19.3   Groups 1, 2, 3, and 4—Record the volume in the
5 mL of liquid residue in the flask to the EP (FBP) shall be 5-mL graduated
graduated cylinder
cylinder,, to the nearest 0.1 mL, as perce
percent
nt
within the limits prescribed in Table
in  Table 5.
5.  If this condition is not residue.
satisfied, repeat the test with appropriate modification of the 10.20
10.20 If the intent
intent of the distilla
distillati
tion
on is to det
determ
ermine
ine the
final heat adjustment. percent
percent evapo
evaporated
rated or perce
percentnt recov
recovered
ered at a prede
predeterm
termined
ined
NOTE   17—Sinc
17—Sincee it is dif
diffficul
icultt to det
determ
ermine
ine when thethere
re is 5 mL of  corrected temperature reading, modify the procedure to con-
boiling liquid left in the flask, this time is determined by observing the form to the instructions described in  Annex A4.A4.
amount of liquid recovered in the receiving cylinder. The dynamic holdup 10.21 Exam
Examine
ine the condenser
condenser tube and the side arm of the
has been determined to be approximately 1.5
approximately  1.5 mL mL at this point. If there are flask for waxy or solid deposits. If found, repeat the test after
no front end losses, the amount of 5 mL in the flask can be assumed to
making adjustments described in Footnote A of  Table
of  Table 5.
5.
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.
11. Calculations
10.15.1 If the actual front end loss differs
10.15.1 differs more than 2 mL
11.1 The percent total
11.1 total recovery is the sum of the perce
percent
nt
from the estimated value, the test shall be rerun.
recovery
recovery (see   10.18)
10.18)   and the per
percen
centt res
residu
iduee (se
(seee   10.19).
10.19).
10.16 Obser
Observe
ve and record the EP (FBP) or the dry point, or
both, as required, and discontinue the heating. Ded
Deduct
uct loss.
percent the per
percen
centt tot
total
al rec
recove
overy
ry fr
from
om 100 to obtobtain
ain the
10.17 Allow the distillate
distillate to drain into the rece
receiving
iving cylin-
cylin-
der, after heating has been discontinued. 11.2
11.2 Do not correct the barobarometr
metric
ic pres
pressure
sure for meni
meniscus
scus
10.17.1  Manual Method —While
—While the condenser tube contin- depression, and do not adjust the pressure to what it would be
ues to drain into the graduated cylinder, observe and note the at sea level.
volume of condensate to the nearest 0.5 mL at 2 min intervals NOTE   20—T
20—Thehe obobser
serve
ved
d ba
baro
rome
metr
tric
ic re read
ading
ing do
does
es not hahave
ve to be
until two successive observations agree. Measure the volume corrected to a standard temperature and to standard gravity. Even without
in the receiving cylinder accurately, and record it to the nearest performing these corrections, the corrected temperature readings for the
0.5 mL. same sample between laboratories at two different locations in the world
will, in general, differ less than 0.1°C at 100°C. Almost all data obtained
10.17.2   Automated Method —The—The appar
apparatus
atus shall continu-
earlier
earlier have bee
beenn rep
report
orted
ed at bar
barome
ometri
tricc pre
pressur
ssures
es tha
thatt hav
havee not bee
been
n
ally monitor the recovered volume until this volume changes corrected to standard temperature and to standard gravity.
by no more than 0.1 mL in 2 min. Record the volume in the
receiving cylinder accurately to the nearest 0.1 mL. 11.3 Corre
11.3 Correct
ct temperature
temperature readings
readings to 101.3 kPa (760 mm
10.1
10.188 Record
Record ththee vo
volu
lume
me in th thee re
rece
ceiv
ivin
ing
g cy
cyli
lind
nder
er as Hg) pre
pressu
ssure.
re. Obt
Obtain
ain the cor
correc
rectio
tion
n to be app
applie
lied
d to eac
each
h
percent recovery. If the distillation was previously discontin- temperature reading by means of the Sydney Young equation

ued under the conditions of a decomposition point, deduct the as   given

of  Table in.  For
Table 6.
6 Eq 3, Eq 4, temperatures:
Celsius or Eq 5, as appropriate, or by the use
percent recovered from 100, report this difference as the sum of 
percent residue and percent loss, and omit the procedure given C c 5 0.0009 ~101.3 2 Pk ! ~273 1 t c!   (3)
in 10.19
in  10.19..

10
 

D 86 – 05
TABLE
TABLE 6 Approximate Thermometer Reading
Reading Correction Pk    = press
pressure,
ure, kPa, and
  CorrectionA per 1.3 kPa (10 mm Hg) P   = pressu
pressure,
re, mm Hg.
Temperature Range
Difference in Pressure
NOTE   22—Eq 6
22—Eq  6 and 7 above
7  above have been derived from the data in  Table
°C °F °C °F
7  and Eqs 5 and 6 in Test Method D 86 – 95 and earlier versions. It is
10–30 50–86 0.35 0.63 probable that Eq 6
Eq  6 and 7 shown
7 shown were the original empirical equations from
30–50 86–122 0.38 0.68
which the table and equations in the Test Method D 86 – 95 and earlier
50–70 122–158 0.40 0.72
70–90 158–194 0.42 0.76 versions
versions were derived.
90–110 194–230 0.45 0.81 11.4.1 Calculate the corresponding
corresponding corrected percent recov-
recov-
110–130 230–266 0.47 0.85
130–150 266–302 0.50 0.89 ery in accordance with the following equation:
150–170 302–338 0.52 0.94  Rc   5  R   1 ~ L 2  Lc!   (8)
170–190 338–374 0.54 0.98
190–210 374–410 0.57 1.02
210–230 410–446 0.59 1.07
230–250 446–482 0.62 1.11 where:
250–270 482–518 0.64 1.15  L   = perce
percent
nt loss
loss or
or observe
observed d loss,
loss,
270–290 518–554 0.66 1.20  Lc   = corr
corrected
ected loss
loss,,
290–310 554–590 0.69 1.24
310–330 590–626 0.71 1.28
 R   = perce
percent
nt reco
recovery
very,, and
and
330–350 626–662 0.74 1.33  Rc   = corr
corrected
ected perce
percent nt recovery
recovery..
350–370 662–698 0.76 1.37 11.
1.5
5 To ob obta
tain
in ththee peperc
rcen
entt ev
evap
apor
orat
ated
ed at a pr pres
escr
crib
ibed
ed
370–390 698–734 0.78 1.41
390–410 734–770 0.81 1.46
temp
tempererat
atur
uree re
read
adin
ing,
g, ad addd th
thee pe
percrcen
entt lo
loss
ss to ea
each
ch of th
thee
A
observ
obs erved
ed per
percen
centt rec
recove
overed
red at the pre prescr
scribe
ibed
d tem
temper
peratu
ature
re
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. readings,
read ings, and repor
reportt thes
thesee resu
results
lts as the respective
respective perce
percent
nt
evaporated, that is:
Pe 5 Pr 1  L   (9)
C c 5 0.00012 ~760 2 P! ~273 1 t c !   (4)

For Fahrenheit temperatures: where:

 L   = obser
observed
ved loss,
C  f  5 0.00012 ~760 2 P! ~460 1 t  f !   (5)
Pe   = perce
percent
nt evaporat
evaporated,
ed, and
Pr   = perce
percent
nt recov
recovered.
ered.
where: 11.6
11 .6 To obtai
obtain n temp
temperat
erature
ure read
readings
ings at presc
prescribe
ribed
d perce
percent
nt
t c   = the obser
observed
ved temp
temperat
erature
ure readi
reading
ng in °C, evaporated, and if no recorded temperature data is available
t  f    = the obser
observed
ved temp
temperat
erature
ure readi
reading
ng in °F
°F,, within 0.1 volume % of the prescribed percent evaporated, use
C c  and   C  f    = cor
correc
rectio
tions
ns to be added algebra
algebraica
ically
lly to the either
either of the two follfollowing
owing procedures,
procedures, and indi
indicate
cate on the
observed temperature readings, report
rep ort whe
whethe
therr the ari
arithm
thmeti
etical
cal pro
proced
cedure
ure or the gragraphi
phical
cal
Pk    = barometric pressure, prevailing at the time and procedure has been used.
location of the test, kPa, and 11.6.1   Arithmetical Procedur
Proceduree—Dedu
—Deductct the observed loss
P   = barometric pressure, prevailing at the time and from each prescribed percent evaporated to obtain the corre-
location of the test, mm Hg. sponding percent recovered. Calculate each required tempera-
After applying the corrections and rounding each result to ture reading as follows:
the nearest 0.5°C (1.0°F) or 0.1°C (0.2°F), as appropriate to the
T   5 T  L   1 ~T  H  2 T  L! ~ R 2  R L! / ~ R H  2  R L!   (10)
apparatus being used, use the corrected temperature readings in
all further calculations and reporting.
where:
NOTE   21—Temperature readings are not corrected to 101.3 kPa (760
mm Hg) when product definitions, specifications,
specifications, or agree
agreements
ments between
 R   = percent
percent recovered
recovered correspo
correspondin
nding g to the prescribed
prescribed
the par
partie
tiess invo
involve
lved
d ind
indica
icate,
te, spec
specific
ifically
ally,, tha
thatt suc
such
h cor
correc
rection
tion is not percent evaporated,
required or that correction shall be made to some other base pressure.  R H    = perc
percent
ent recovere
recoveredd adjacent
adjacent to, and higher
higher than
than  R ,
 R L   = perc
percent
ent recovere
recoveredd adjacent
adjacent to,
to, and lower
lower than  R,
11.4 Cor
11.4 Correc
rectt the actual
actual loss to 101
101.3
.3 kPa (760 mm Hg)
T    = temperature reading at the prescribed percent evapo-
pressure when temperature readings are corrected to 101.3 kPa
rated,
pressure. The corrected loss,  L c, is calculated from Eq 6 or Eq T  H    = temp
temperat
erature
ure reading
reading recor
recorded
ded at R H , and
7, as appropriate, or can be read from the tables presented as T  L   = temp
temperat
erature
ure readi
reading
ng recorde
recorded d at  R L.
Fig. X3.1 
X3.1   or
or Fig.
 Fig. X3.2.
X3.2. Values obtained by the arithmetical procedure are af affected
fected by
 Lc   5 0.5 1 ~ L 2 0.5! / $1 1 ~101.3 2 Pk ! /8.00%   (6) the extextent
ent to whi
which
ch the dis
disti
tilla
llatio
tion
n gra
graphs
phs are nonnonlin
linear
ear..
Intervals between successive data points can, at any stage of 
 Lc   5 0.5 1 ~ L 2 0.5! / $1 1 ~760 2 P! /60.0%   (7) the test, be no wider than the intervals indicated in 10.18
in  10.18.. In no
case shall a calculation be made that involves extrapolation.

where: 11.6.2   Graphical Procedure—Using graph paper with uni-

form subdivisions, plot each temperature reading corrected for
 L   = obser
observed
ved loss
loss,, barometric pressure, if required (see   11.3)
11.3), against its corre-
 Lc   = corr
corrected
ected loss
loss,,
sponding
sponding perce
percent
nt recov
recovered.
ered. Plot the IBP at 0 % recorecovered
vered..

11
 

D 86 – 05
TABLE
TABLE 7 Data Points
Points for Deter
Determini
mining
ng Slope, S C  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- VL   5 10 20 20 20 20 20 20 20 20 10 5 VEP−95

Dra
Draww a sm
smoot
oothh cur
curve
ve con
connec
nectin
ting
g the points.
points. For eac each
h pre
pre-- 12.8 Repor
Reportt if a dryi
drying
ng agent, as described
described in 7.5.2
in  7.5.2 or
 or 7.5.3
 7.5.3,,
scribe
scribed
d per
percen
centt eva
evapor
porate
ated,
d, ded
deduct
uct the disdistil
tillat
lation
ion los
losss to was used.
obtain the corresponding percent recovered and take from the 12.9  Fig. X1.1 is
X1.1  is an example of a tabular report. It shows the
graph
gra ph the tem
temper
peratu
ature
re rea
readin
ding
g tha
thatt thi
thiss per
percen
centt rec
recove
overed
red percent recovered versus the corresponding temperature read-
indicates.
indicates. Value
aluess obtai
obtained
ned by grap
graphical
hical inte
interpola
rpolation
tion proc
proce-
e- ing and versus the corrected temperature reading. It also shows
dures are affected by the care with which the plot is made. the percent loss, the corrected loss, and the percent evaporated
versus the corrected temperature reading.
NOTE   23—See   Appendix X1   for numerical examples illustrating the
arithmetical procedure.
13. Prec
Precisio
ision
n and Bias
11.6.3 In most automated instruments, temperature-volume
temperature-volume
data are collected at 0.1 volume % intervals or less and stored 13.1   Precision:
in memory. To report a temperature reading at a prescribed 13.1.1
13.1.1 The pre precis
cision
ion of thi
thiss tes
testt met
method
hod has bee been n det
deterer--
percen
percentt eva
evapor
porate
ated,
d, nei
neithe
therr of the pro
proced
cedure
uress des
descri
cribed
bed in mined
mine d by the statstatisti
istical
cal exam
examinat
ination
ion of inteinterlabo
rlaborator
ratory
y test
11.6.1 and
11.6.1  and 11.6.2
 11.6.2 have
 have to be used. Obtain the desired tempera- result
resultss obt
obtain
ained
ed by 26 lab labora
orator
tories
ies on 14 gas gasoli
olines
nes,, by 4
ture directly from the database as the temperature closest to and laboratories on 8 samples of kerosine by the manual procedure,
within 0.1 volume % of the prescribed percent evaporated. 3 lab
labora
orator
tories
ies on 6 sam sample
pless of ker
kerosi
osine
ne by the aut automa
omatedted
procedure, and 5 laboratories on 10 samples of diesel fuel by
12. Repo
Report
rt both the manual and automated procedures.  Table A1.1  lists
12.1 Report the following information
information (see(see Appendix X5 for
X5 for which tables and figures are to be used for the different fuel
examples of reports): groups, distillation methods, and temperature scales.
12.2 Report the barometric
barometric pressure to the the nearest 0.1 kPa (1 13.1.2 The following
following terms are used in this section: (1)  r  =
mm Hg). repeatability and (2)   R  = reproducibility. The value of any of 
12.3 Repor
Reportt all volumetric
volumetric readings in perc percentag
entages.es. these terms will depend upon whether the calculations were
12.3.1   Manual Method —Report —Report volumetric readings to the carried out in °C or °F.
nearest 0.5, and all temperature readings to the nearest 0.5°C 13.2   Slope or Rate of Change of Temperature :
(1.0°F). 13.2.1 To determine
determine the preci
precision
sion of a resul
result,
t, it is generally
generally
12.3.2   Automated Method —Report —Report volum volumetri
etricc read
readings
ings to necess
nec essary
ary to det
determ
ermine
ine the sloslope
pe or ratratee of cha
change
nge of the
the nea
neares
restt 0.1
0.1,, and all temtemper
peratu
ature
re reareadin
dings
gs to the nea neares
restt temperature at that particular point. This variable, denoted as
0.1°C (0.2°F) or less. SC  or SF, is equal to the change in temperature, either in °C or
12.4 Afte
Afterr barom
barometri
etricc corr
correctio
ections
ns of the temperature
temperature read- in °F, respectively, per percent recovered or evaporated.
ingss hav
ing havee beebeenn mad
made,e, the fol
follow
lowing
ing datdataa req
requir
uiree no furfurthe
therr 13.2.2 For Group 1 in the manual method method and for all groups
calcul
calculati
ation
on priprior
or to repreport
orting
ing:: IBP
IBP,, dry poi point,
nt, EP (FB (FBP),
P), in the automated method, the precision of the IBP and EP does
decomposit
decom position
ion point
point,, and all pairs of corr correspon
esponding
ding values not require any slope calculation.
involving percent recovered and temperature readings. 13.2.3 With thethe exception stated
stated in 13.2.2
in 13.2.2 and
 and in 13.2.4
in  13.2.4,,  the
12.4.1
12. 4.1 The rep report
ort sha
shallll sta
state
te if the temtemper
peratu
ature
re rea
readin
dings
gs slope at any point during the distillation is calculated from the
have not been corrected for barometric pressure. following equations, using the values shown in  Table 7: 7:
12.5
12. 5 Whe
When n the tem
temper
peratu
ature
re rea
readin
dings gs hav
havee not bee beenn cor
cor--
S C ~or  S F! 5 ~T U  2 T  L!  /  ~V U  2 V  L!   (11)
rected to 101.3 kPa (760 mm Hg) pressure, report the percent
residue and percent loss as  observed  in   in accordance with 10.19
with  10.19 where:
and 11.1
and  11.1,,   respectively. S C    = is the slope
slope,, °C/vol
°C/volume ume %,
12.6
12. 6 Do not use the correct correcteded los
losss in the calculat
calculationion of  S F    = is the slope
slope,, °F/vo
°F/volume lume %,
percent evaporated. T U    = is the
the upper
upper temp
temperat erature,
ure, °C (or
(or °F),,
°F)
12.7
12. 7 It is adv advisa
isable
ble to basbasee the rep report
ort on rel relati
ations
onship
hipss T  L   = is the
the lower
lower temp
temperat erature,
ure, °C (or
(or °F),
between temperature readings and percent evaporated when the V U    = is the volume
volume % rec recove
overed
red or evaporated
evaporated corre-
corre-
sample
sam ple is a gas gasoli
oline,
ne, or any oth other
er proproduc
ductt cla
classi
ssified
fied und
under
er sponding to   T U ,
Group 0 or 1, or in which the percent loss is greater than 2.0. V  L   = is the volume
volume % rec recove
overed
red or evaporated
evaporated corre-
corre-
Otherwise, the report can be based on relationships between sponding to   T  L ,   and
temperature readings and percent evaporated or percent recov- V  EP   = is the vol
volume
ume % rec recove
overed
red or evapor
evaporate
ated
d cor
corre-
re-
ered. Every report must indicate clearly which basis has been sponding to the end point.

used. to 13.2.4
the 95 In
% the event
point, thethat the at
slope distillation end point
the end point point occurs prior
is calculated as
12.7.1 In the manual method,
method, if resul
results
ts are given in percent
evaporated versus temperature readings, report if the arithmeti- follows:
cal or the graphical procedure was used (see  11.6
 11.6).
). S C ~or  S F! 5 ~T  EP 2 T  HR!  /  ~V  EP 2 V  HR!   (12)

12
 

D 86 – 05
TABLE 8 Repeatability and Reproducibility
Reproducibility for Group 1
Manual Manual Automated Automated
Evaporated RepeatabilityA ReproducibilityA RepeatabilityA ReproducibilityA
Point, %
°C °F °C °F °C °F °C °F
IBP 3.3 6 5.6 10 3.9 7 7.2 13
5 1.9+0.86SC   3.4+0.86SF   3.1+1.74SC   5.6+1.74SF   2.1+0.67SC   3.8+0.67SF   4.4+2.0SC   7.9+2.0SF
10 1.2+0.86SC   2.2+0.86SF   2.0+1.74SC   3.6+1.74SF   1.7+0.67SC   3.0+0.67SF   3.3+2.0SC   6.0+2.0SF
20 1.2+0.86SC   2.2+0.86SF   2.0+1.74SC   3.6+1.74SF   1.1+0.67SC   2.0+0.67SF   3.3+2.0SC   6.0+2.0SF
30–70 1.2+0.86SC   2.2+0.86SF   2.0+1.74SC   3.6+1.74SF   1.1+0.67SC   2.0+0.67SF   2.6+2.0SC   4.7+2.0SF
80 1.2+0.86SC   2.2+0.86SF   2.0+1.74SC   3.6+1.74SF   1.1+0.67SC   2.0+0.67SF   1.7+2.0SC   3.0+2.0SF
90 1.2+0.86SC   2.2+0.86SF   0.8+1.74SC   1.4+1.74SF   1.1+0.67SC   2.0+0.67SF   0.7+2.0SC   1.2+2.0SF
95 1.2+0.86SC   2.2+0.86SF   1.1+1.74SC   1.9+1.74SF   2.5+0.67SC   4.5+0.67SF   2.6+2.0SC   4.7+2.0SF
FBP 3.9 7 7.2 13 4.4 8 8.9 16
A
SC  or SF   is the average slope (or rate of change) calculated in accordance with 13.2
with  13.2..

TABLE 9 Repeatability and Reproducibility

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
Calculate SC  or SF  from 13.2.

where: under constant operating conditions on identical test material

T  EP   or   T  HR   is the temperature, in °C or °F at the percent would, in the long run, in the normal and correct operation of 
volume recovered indicated by the subscript, this test method, exceed the values calculated from  Table 9 in9  in
V  EP   or   V  HR  is the volume % recovered. only one case in twenty.
13.2.4.1
13.2.4 .1 The subscript
subscriptss in Eq 12 refer to: 13.3.1.3   GROU
GROUPSPS 2, 3, and 4—The dif differe
ference
nce betwe
between
en
successive results obtained by the same operator with the same
apparatus under constant operating conditions on identical test
 EP   = en
end
d po
poin
intt materi
mat erial
al wou
would,
ld, in the long runrun,, in the normal
normal and correct
correct
 HR   = highest
highest reading,
reading, eithe
eitherr 80 % of 90 %, prior
prior to the
the end
operation
oper ation of this test metho
method, d, excee
exceed d the values calc
calculat
ulated
ed
point.
from the values in  Table 9 in
9  in only one case in twenty.
13.2.5 For points
points between 10 to 85 % recovered
recovered which are
13.3.2   Reproducibility:
not shown in Table
in  Table 7,
7,  the slope is calculated as follows:
13.3.2.1   GROUP 0—The reproducibility of the test method
S C ~or  S F! 5 0.05 ~T  ~V 110! 2 T  ~V 210!!   (13) for this group has not been determined.
13.2.6 For samples
samples in Group 1, the precision
precision data reported
reported 13.3.2.2   GROUP 1—The difference between two single and
are based on slope values calculated from percent evaporated independent results obtained by different operators working in
data. different laboratories on identical test material would, in the
13.2.7 For samples
samples in Group 2, 3, and 4, the precision
precision data normal and correct operation of this method, exceed 7the values
reported (Table
(Table 8)
8) are based on slope values calculated from calculated from Table
from  Table 9 in
9  in only one case in twenty.
percent recovered data. 13.3.2.3  GROUPS 2, 3, and 4—The difference between two
13.2.8 When results
results are repo
reported
rted as volu
volume
me % recov
recovered
ered,, single and independent results obtained by different operators
slope values for the calculation of precision are to be deter- working
worki ng in difdifferen
ferentt labo
laborator
ratories
ies on ident
identical
ical test mate
material
rial
mined from percent recovered data; when results are reported would, in the normal and correct operation of this test method,
as vol
volume
ume % evaevapor
porate
ated
d slo
slope
pe val
values
ues are to be det
determ
ermine
ined
d exceed the values calculated from the data in  Table 9 in 9  in only
8
from % evaporated data. one case in twenty.
13.3   Manual Method : 13.4   Automated Method :
13.3.1   Repeatability: 13.4.1   Repeatability:
13.3.1.1   GROUP 0—Duplicate results obtained for the EP 13.4.1.1   GRO
GROUPUP 0—Du—Dupli plicat
catee res
result
ultss obt
obtain
ained
ed for the
shall not differ from each other by more than 3.5°C (6°F) in endpoint shall not differ from each other by more than 3.5°C
one cas
casee in twe
twenty
nty.. Dif
Differ
ferenc
ences
es in dup
duplic
licate
ate tem
temper
peratu
ature
re (6°F) in one case in twenty. Differences in duplicate tempera-
readings for each prescribed percentage point shall not exceed ture readings
readings for each prescribed
prescribed perc
percentag
entagee poin
pointt shall not
the amounts equivalent to 2 mL of distillate at each point in
question.
question. The calcalcul
culati
ation
on of thi
thiss max
maximu
imum
m dif
differ
ferenc
encee is 7
Precision data obtained from RR study on both manual and automated D 86
described in Annex
in  Annex A5.
A5.
units by North American
American and IP Labora
Laboratories.
tories.
13.3.1.2   GROU
GROUP P 1—The dif differe
ference
nce betwe
between
en succe
successive
ssive 8
Table 9   has been derived from the nomographs in Figs. 6 and 7 in ASTM
results obtained by the same operator with the same apparatus D 86–97.

13
 

D 86 – 05
TABLE 10 Repeatability and Reproducibility
Reproducibility for Groups 2, 3 and 4 (Automated)
RepeatabilityA ReproducibilityA
Collected, %
°C °F °C °F
IBP 3.5 6.3 8.5 15.3
2% 3.5 6.3 2.6 + 1.92SC   4.7 + 1.92SF
5% 1.1 + 1.08SC   2.0 + 1.08SF   2.0 + 2.53SC   3.6 + 2.53SF
10 % 1.2 + 1.42SC   2.2 + 1.42SF   3.0 + 2.64SC   5.4 + 2.64SF
20–70 % 1.2 + 1.42SC   2.2 + 1.42SF   2.9 + 3.97SC   5.2 + 3.97SF
80 % 1.2 + 1.42SC   2.2 + 1.42SF   3.0 + 2.64SC   5.4 + 2.64SF
90–95 % 1.1 + 1.08SC   2.0 + 1.08SF   2.0 + 2.53SC   3.6 + 2.53SF
FBP 3.5 6.3 10.5 18.9
A
S C  or SF   is the average slope (or rate of change) calculated in accordance with 13.5
with  13.5..

exceed the amounts equivalent to 2 mL of distillate at each working in dif

working differen
ferentt labo
laborator
ratories
ies on ident
identical
ical test mate
material
rial
point in question. The calculation of this maximum difference would, in the normal and correct operation of this test method,
is described in Annex
in  Annex A5.
A5. exceed the values calculated from Table
from  Table 10 in
10  in only one case in
13.4.1.2   GROU
GROUP P 1—The difdiffere
ference
nce betwe
betweenen succe
successive
ssive twenty.
results obtained by the same operator with the same apparatus 13.5   Bias:
under constant operating conditions on identical test material 13.5.1   Bias—Due to the use of total immersion thermom-
would, in the long run, in the normal and correct operation of  eters,
eters, or temp
temperat
erature
ure sens
sensing
ing syste
systems
ms desi
designed
gned to emul
emulate
ate
this test method, exceed the values calculated from  Table 8 in
8  in them,
the m, the dis
distil
tillat
lation
ion tem
temper
peratu
atures
res in thi
thiss tes
testt me
metho
thod
d are
only one case in twenty. somewhat
some what lower than the true temperatur
temperatures.
es. The amou
amountnt of 
13.4.1.3   GROU
GROUPS PS 2, 3, an
andd 4—The difdifferen
ference
ce betwe
between
en bias depends on the product being distilled and the thermom-
successive results obtained by the same operator with the same eter used.
apparatus under constant operating conditions on identical test
13.5.2   Relative Bias—T
Relative —The here
re ex
exis
ists
ts a bibias
as bebetw
twee
een
n th
thee
materi
mat erial
al wou
would,ld, in the long run, in the normal
normal and correct
correct
empirical results of distillation properties obtained by this test
operation of this test meth
operation method,
od, excee
exceed
d the values calculated
calculated method and the true boiling point distillation curve obtained by
from Table
from  Table 10 in
10  in only one case in twenty.
Test Method D
Method  D 2892.
2892.  The magnitude of this bias, and how it
13.4.2   Reproducibility:
relates to test precision, has not been rigorously studied.
13.4.2.1  GROUP 0—The reproducibility of the test method
13.5.3   Relative Bias—An interlaboratory study5 conducted
for this group has not been determined.
in 2003 using manual and automated apparatus has concluded
13.4.2.2   GROUP 1—The difference between two single and
that there is no statistical evidence to suggest that there is a bias
independent results obtained by different operators working in
between manual and automated results.
different laboratories on identical test material would, in the
normal and correct operation of this test method, exceed the
14. Keyw
Keywords
ords
values calculated from Table 8  in only one case in twenty.7
from  Table 8 in
13.4.2.3  GROUPS 2, 3, and 4—The difference between two 14.1 batch disti
distillat
llation;
ion; disti
distillat
llates;
es; dist
distilla
illation
tion;; labo
laborator
ratory
y
single and independent results obtained by different operators distillation; petroleum products

ANNEXES

(Mandatory Information)

A1. REPEA
REPEATABILITY
TABILITY AND REPRODUCIBILITY DEFINITION AIDS

A1.1   Tab
Table
le A1.1 
A1.1   is an aid for determining which repeat-
ability and reproducibility table or section, is to be used.

14
 

D 86 – 05
TABLE A1.1 Summary of Aids for Definition of Repeatability and Reproducibility
Table or Section to Use
Group Method Temperature Scale
Repeatability Reproducibility
0 Manual °C or °F   13.3.1.1 13.3.2.1
Automated °C or °F   13.4.1.1   13.4.2.1
1 Manual °C   Table 8 Table 8
°F   Table 8 Table 8
1 Automated °C   Table 8 Table 8
°F   Table 8 Table 8
2,3,4 Manual °C   Table 9 Table 9
°F   Table 9 Table 9
2,3,4 Automated °C   Table 10 Table 10
°F   Table 10 Table 10

A2. DETAILED DESCRIPTION OF APPARATUS

APPARATUS

A2.1   Distillation Flasks—Flasks shall be of heat resistant A2.3   Meta Enclosure for Flask . (Manual units
Metall Shield or Enclosure
glass, constructed to the dimensions and tolerances shown in only).
Fig. A2.1 and
A2.1  and shall otherwise comply with the requirements of  A2.3.1  Shield for Gas Burner (see  Fig. 1)—The purpose of 
Specification  E 1405.
1405.   Flask
Flask A (1
(100
00 mL
mL)) ma
mayy al
also
so be co
con-
n- thiss shi
thi shield
eld is to pro
provid
videe pro
protec
tectio
tion
n for the ope
operat
rator
or and yet
structed with a ground glass joint, in which case the diameter allow
allow easeasy
y acc
access
ess to the burner
burner and to the disdistil
tillat
lation
ion flask 
of the neck shall be the same as the 125-mL flask. during
dur ing ope
operat
ration
ion.. A typ
typica
icall shi
shield
eld wou
would
ld be 480
480-mm
-mm hig
high,
h,
NOTE   A2.1—For
A2.1—For tests specifying dry point, specially selected flasks 280-mm
280 -mm long and 200 200-mm
-mm wide,
wide, mad
madee of she
sheet
et met
metal
al of 
with bottoms and walls of uniform thickness are desirable. 0.8-mm thickness (22 gage). The shield shall be provided with
A2.2   Conde
Condenser Condenser Bath—T
nser and Condenser —Typic
ypical
al type
typess of  at least one window to observe the dry point at the end of the
distillation.
condenser and condenser baths are illustrated in  Figs. 1 and 2.
2.
A2.3.2   Shield for Electric Heater (see   Fig. 2)—A typical
A2.2.1 The condenser
condenser shall be made of seamless
seamless noncorro-
noncorro- shield
shi eld would be 440440-mm
-mm high, 200
200-mm
-mm long, and 200200-mm
-mm
sive metal tubing, 560   6   5 mm in len
length
gth,, wit
with
h an outside
outside wide, made of sheet metal of approximately 0.8-mm thickness
diameter of 14 mm and a wall thickness of 0.8 to 0.9 mm. (22 gage) and with a window in the front side. The shield shall
NOTE  A2.2—Brass or stainless steel has been found to be a suitable be provided with at least one window to observe the dry point
material for this purpose. at the end of the distillation.
A2.2.2 The condenser shallshall be set soso that 393 6 3 mm of the
tube is in contact with the cooling medium, with 50  6   3 mm A2.4   Heat Source:
Source:
outside the cooling bath at the upper end, and with 114 6 3 mm A2.4.1   Gas Burner   (see   Fig. 1),
1), capable of bringing over
outside at the lower end. The portion of the tube projecting at the first drop from a cold start within the time specified and of 
the upper end shall be set at an angle of 75   6   3° with the continuin
continuingg the dist
distilla
illation
tion at the speci
specified
fied rate
rate.. A sens
sensitiv
itivee
vertical. The portion of the tube inside the condenser bath shall manu
ma nual
al co
cont
ntro
roll va
valv
lvee an
and
d gagass pr
pres
essu
sure
re re
regu
gula
latotorr to gi
give
ve
be either straight or bent in any suitable continuous smooth complete control of heating shall be provided.
curve. The average gradient shall be 15   6  1° with respect to A2.4.2   Electric Heater   (see Fig.
(see  Fig. 2)
2), of low heat retention.
the horizontal, with no 10-cm section having a gradient outside
of the 15   6   3° ran
range.
ge. The pro projec
jectin
ting
g low
lower er por
portio
tion
n of the NOTE  A2.3—Heaters, adjustable from 0 to 1000 W, have been found to
be suitable for this purpose.
condenser tube shall be curved downward for a length of 76
mm anandd th
thee lo
lowe
werr en
end
d shshal
alll be cu
cutt of
offf at an ac acut
utee an
angl
gle.
e.
A2.5   Flask Support:
Provisions shall be made to enable the flow of the distillate to
run
run do
down
wn ththee si
side
de of th
thee re
rece
ceiv
ivin
ingg cy
cylilind
nder
er.. Th
Thisis ca
can
n be A2.5.1   Type
Type 1—U—Usese a Typ
ypee 1 flaflask
sk su
supp
ppor
ortt wi
withth a gagass
accomplished by using a drip-deflector, which is attached to the burner
burn er (see   Fig.
Fig. 1). Thi
Thiss sup
suppor
portt con
consis
sists
ts of eit
either
her a rin
ringg
outlet
outlet of the tub tube.
e. Alt
Altern
ernati
ativel
vely
y, the low
lower er por
portition
on of the support of the ordinary laboratory type, 100 mm or larger in
conden
con denser
ser tub
tubee can be curcurved
ved sli
slight
ghtly
ly bac
backwa
kward rd to ensensure
ure diameter, supported on a stand inside the shield, or a platform
contact with the wall of the receiving cylinder at a point 25 to adjust
adj ustabl
ablee fro
from
m the outside
outside of the shield.
shield. On thi
thiss rin
ring
g or
32 mm below the top of the receiving cylinder.  Fig. A2.3 is A2.3  is a platform is mounted a hard board made of ceramic or other
drawing of an acceptable configuration of the lower end of the heat-resistant material, 3 to 6 mm in thickness, with a central
condenser tube. opening 76 to 100 mm in diameter, and outside line dimensions
A2.2.3 The volume and the design of the bath will depend slightly smaller than the inside boundaries of the shield.
on the cooling medium employed. The cooling capacity of the A2.5.2   Type 2—Use a Type 2 flask support assembly with
bath shall be adequate to maintain the required temperature for electric heat
electric heating
ing (see
(see   Fig. 2   as one exam
example)
ple).. The assem
assembly
bly
the desir
desired
ed conde
condenser
nser perf
performa
ormance.
nce. A singl
singlee conde
condenser
nser bath consists of an adjustable system onto which the electric heater
may be used for several condenser tubes. is mounted with provi
provision
sion for place
placement
ment of a flask support

15
 

D 86 – 05

FIG. A2.1 Flask A, 100 mL, Flask B, 125 mL, and Flask B with Ground Glass Joint, 125 mL

board (see A2.6

A2.6)) above the electric heater. The whole assembly A2.9   Receiving Cylinders
Cylinders—The rece
receivin
iving
g cyli
cylinder
nder shal
shalll
is adjustable from the outside of the shield. have a capacity to measure and collect 100 mL. The shape of 
the base shall be such that the receiver does not topple when
A2.6   Flask Support Board —The
—The flask support board shall placed empty on a surface inclined at an angle of 13° from the
be constructed of ceramic or other heat-resistant material, 3 to horizontal.
6 mm in thickness. Flask support boards are classified as A, B, A2.9.1  Manual Method —The
—The cylinder shall be graduated at
or C, based on the size of the centrally located opening, the intervals of 1 mL and have a graduation at the 100-mL mark.
dimension of which is shown in   Table
Table 1. The flask support Construction details and tolerances for the graduated cylinder
board shall be of sufficient dimension to ensure that thermal are shown in Fig.
in  Fig. A2.4.
A2.4.
heat to the flask only comes from the central opening and that A2.9.2   Automated Method —The
—The cylinder shall conform to
extran
extraneou
eouss hea
heatt to the flas
flaskk oth
other
er tha
than
n thr
throug
oughh the central
central the physical specifications described in Fig.
in  Fig. A2.4,
A2.4,  except that
opening is minimized. (Warning
(Warning—Asbestos-conta
—Asbestos-containing
ining mate- graduations below the 100-mL mark are permitted, as long as
rials shall not be used in the construction of the flask support they do not interfere with the operation of the level follower.
board.) Receiving cylinders for use in automated units may also have
a metal base.
A2.7
A2. 7 The flask suppor
supportt board can be moved slight
slightly
ly in A2.9.3 If required, the receiving cylinder
cylinder shall be immersed
immersed
differentt dire
differen directio
ctions
ns on the horizontal
horizontal plane to posi
position
tion the during the distillation to above the 100-mL graduation line in
distillation flask so that direct heat is applied to the flask only
a cooling liquid contained in a cooling bath, such as a tall-form
through the opening in this board. Usually, the position of the beaker of clear glass or transparent plastic. Alternatively, the
flask is set by adjusting the length of the side-arm inserted into
receiving cylinder may be placed in a thermostated bath air
the condenser. circulation chamber
chamber..
A2.8 Provi
Provision
sion shall
shall be made for moving
moving the flask
flask support
support A2.10   Resid
Residue
ue Cylinder —The
Cylinder  —The gradu
graduated
ated cyli
cylinder
nder shal
shalll
assembly vertically so that the flask support board is in direct have a capacity of 5 or 10 mL, with graduations into 0.1 mL
contac
con tactt wit
with
h the bot
bottom
tom of the dis
disti
tilla
llatio
tion
n flas
flask
k dur
during
ing the subdivisions, beginning at 0.1 mL. The top of the cylinder may
distillation. The assembly is moved down to allow for easy be flared, the other properties shall conform to Specification
mounting and removal of the distillation flask from the unit. E 1272.
1272.

16
 

D 86 – 05

FIG. A2.2 Detail of Upper Neck Section

17
 

D 86 – 05

FIG. A2.3 Lower End of Condenser Tube

NOTE—1 to 100 mL in 1 mL graduations; tolerance  6  1.0 mL.

FIG. A2.4 100 mL Graduated Cylinder

18
 

D 86 – 05

A3. DETERM
DETERMINA
INATION
TION OF THE DIFF
DIFFERENCE
ERENCE IN LAG TIME BETWEE
BETWEEN
N AN ELECTR
ELECTRONIC
ONIC TEMPERATURE
TEMPERATURE
MEASUREMENT SYSTEM AND A MERCURY-IN-GLASS THERMOMETER

A3.1
A3 .1 ThThee re
resp
spon
onse
se ti
time
me of an el elec
ectr
tron
onic
ic te
temp
mper
erat
atur
uree A3.2.2 Best results are obtained
obtained with a sample that is typical
typical
measuring
measur ing device
device is inh
inhere
erentl
ntlyy mor
moree rap
rapid
id tha
thann tha
thatt of a of the sam
sample
ple loa
load
d of the lablabora
orator
tory
y. Alt
Altern
ernati
ativel
vely
y, use a
mercury-i
merc ury-in-gla
n-glass
ss therm
thermomet
ometer
er.. The tempe
temperatu
rature
re meas
measuring
uring full-range mixture with a 5 to 95 % boiling range of at least
device assembly in general use, consisting of the sensor and its 100°C.
casing, or an electronic system and its associated software, or
both, is so designed that the temperature measuring system will A3.3
with Replace
Repla
a low ce the
range or aelectronic
electronic temperature
high rangetemperature measurin
measuring
mercury-in-glass g device
thermom-
simulate the temperature lag of the mercury-in-glass thermom- eter, depending on the boiling range of the sample.
eter.
A3.4
A3. 4 Rep
Repeat
eat the dis
distil
tillat
lation
ion with thi
thiss the
thermo
rmomet
meter
er,, and
A3.2 To determine
determine the differe
difference
nce in lag time between
between such manually record the temperature at the various percent recov-
a temperature measuring system and a mercury-in-glass ther- ered as described in 10.14
in  10.14..
mometer, analyze a sample such as gasoline, kerosine, jet fuel, A3.5 Cal
A3.5 Calcul
culate
ate the valvalues
ues for the repeata
repeatabil
bility
ity for the
or light diesel fuel with the electronic temperature measure- observed slope (DT  / DV ) for the different readings in the test.
ment system in place and in accordance with the procedures
A3.6 Co
A3.6 Comp
mpararee th
thee te
test
st da
data
ta ob
obta
tain
ined
ed ususin
ing
g th
thes
esee tw
twoo
described in this test method. In most cases this is the standard
temperat
temp erature
ure meas
measuring
uring devices. The difdiffere
ference
nce at any poin
pointt
distillation step performed with an automated unit.
shall be equal to, or less than, the repeatability of the method
A3.2.1 Do not use a sing
single
le pure compound,
compound, a very narrow at that point. If this difference is larger, replace the electronic
boilin
boiling
g ran
range
ge pro
produc
duct,
t, or a syn
synthe
thetic
tic blend of les
lesss tha
than
n six temperat
temp erature
ure measu
measuring
ring device or adjus
adjustt the elec
electroni
tronics
cs in-
compounds for this test. volved, or both.

A4. PROCEDURE TO DETERMINE THE PERCENT EV

EVAPORA
APORATED
TED OR PERCENT RECOVERED AT
AT A PRESCRIBED
TEMPERATURE READING

A4.1 ManMany y spe

specifi
cificat
cation
ionss req
requir
uiree spe
specifi
cificc per
percen
centag
tages
es while taking into account A4.5
account  A4.5   and
and A4.6
 A4.6..
evaporate
evapo rated
d or recov
recovered
ered at presc
prescribed
ribed temp
temperat
erature
ure read
readings,
ings,
either
either as max
maxima
ima,, min
minima
ima,, or ran
ranges
ges.. The pro
proced
cedure
uress to A4.5   Manual Distillation:
Distillation:
determine these values are frequently designated by the terms A4.5.1 In the region between
between about 10°C below and 10°C
Exxx or Rxxx, where xxx is the desired temperature. above the desired expected temperature reading determined in
NOTE   A4.1—R
A4.1—Regulato
egulatoryry standar
standards
ds on the certification
certification of refor
reformulate
mulated
d A4.3 record
A4.3  record the temperature reading in intervals of 1 volume
gasoline under the complex model procedure require the determination of  %.
E 200 and E 300, defined as the percent evaporated
evaporated fuel at 93.3°C (200°F) A4.5.2 If the intent of the distillati
distillation
on is to solely determine
determine
and 148.9°C (300°F), respectively
respectively.. E 158, the perce
percent
nt evaporated at a the value of Exxx or Rxxx, discontinue the distillation after at
distillation temperature of 70°C (158°F), is also used in describing fuel
least another 2 mL of distillate have been collected. Otherwise,
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 continue
continue the dis
distil
tillat
lation
ion,, as des
descri
cribed
bed in Sec Sectio
tionn 10, and
are the percent recovered fuel at 200°C, 250°C, and 350°C, respectively. determine the observed loss, as described in 11.1
in  11.1..
A4.5.2.1
A4.5.2.1 If the intent of the distillati
distillation
on is to determine
determine the
A4.2 Deter
Determine
mine the barometr
barometric ic pressure,
pressure, and calculate
calculate the value of Exxx and the distillation was terminated after about 2
correction to the desired temperature reading using Eq 3, Eq 4, mL of distillate was collected beyond the desired temperature,
or Eq 5 for   t  = xxx°C (or  t  f  = xxx°F). allow the distillate to drain into the receiving graduate. Allow
A4.2.1   Manual
Manual Meth od —Deter
Method — Determin
minee thi
thiss cor
correc
rectio
tionn to the contents of the flask to cool to below approximately 40°C
0.5°C (1°F). and then drain its contents into the receiving graduate. Note the
A4.2.2   Automated
Automated Method —Determi
—Determine
Method  ne this corr
correcti
ection
on to volume of product in the receiving graduate to the nearest 0.5
0.1°C (0.2°F). mL at 2 min intervals until two successive observations agree.
A4.5.2.2 The amount recovered in in the receiving graduate isis
A4.3 Deter
Determine
mine the expected
expected temperatu
temperaturere reading
reading to yield the percent recovery. Determine the amount of observed loss
xxx°C (or xxx°F) after the barometric correction. To obtain the by subtracting the percent recovery from 100.0.
expect
exp ected
ed val
value,
ue, add the absabsolu
olute
te val
value
ue of the cal
calcul
culate
ated
d
correction to the desired temperature if the barometric pressure A4.6   Automated Distillation:
Distillation:
is above 101.3 kPa. If the barometric pressure is below 101.3
kPa, subtract the absolute value of the calculated correction A4.6.1 In the region between
between about 10°C below and 10°C
above the desired expected temperature reading determined in
from the desired temperature.
A4.3,, collect temperature-volume data at 0.1 volume % inter-
A4.3
A4.4 Perfo
Perform
rm the distillat
distillation,
ion, as described
described in Section
Section 10, vals or less.

19
 

D 86 – 05
A4.6.2 Continue the distillation,
distillation, as described in Section 10
Section 10,, A4.8.2 Calcu
Calculate
late the slope or rate of chan
change
ge in temp
temperat
erature
ure
and determine the percent loss, as described in  11.1
 11.1.. reading, SC(or SF), as described in  13.2
 13.2 and
 and Eq 11 and using
temperature values bracketing the desired temperature.
A4.7   Calculations:
A4.8.3 Calculate the repeatability,
repeatability,  r , or the reproducibility,
A4.7.1   Manual Method —If
—If a volume % recovered reading
 R, from the slope, SC  (or SF), and the data in Table
in  Table 8,
8,  Table 9,
9,
is not available at the exact temperature calculated in  A4.3  A4.3,,
or Table
or  Table 10.
10.
determine the percent recovered by interpolation between the
two adjacent readings. Either the linear, as described in 11.6.1
in  11.6.1,, A4.8.4 Determine
Determine the repe
repeatabi
atability
lity or repr
reproduci
oducibili
bility
ty,, or
or the graphical procedure, as described in 11.6.2
in  11.6.2,,  is permitted. both, of the volume % evaporated or recovered at a prescribed

The percent recovered is equal to Rxxx. temperature from ther following formulas:

A4.7.2   Automated Method —Report
—Report the observed volume to volume % 5 r  / S 
  ~S F !
SC    (A4.1)
0.1 volume % corresponding to the temperature closest to the
expected temperature reading. This is the percent recovered, or  R
volume % 5  R / S 
S C  ~S F !   (A4.2)
Rxxx.
A4.7.3  Manual and Automated Methods—To determine the
value of Exxx, add the observed loss to the percent recovered, where:
r 
Rxxx, as determined in A4.7.1
A4.7.1 or
 or A4.7.2
A4.7.2 and
 and as described in Eq volumee %
volum = repeatabil
repeatability
ity of the volum
volumee % evapo
evaporate
rated
d or
9. recovered,
 R
A4.7.3.1
A4.7.3.1 As pres
prescribe
cribed
d in   12.6,
12.6,   do not use the correcte
corrected
d volumee %
volum = repro
reproducib
ducibilit
ility
y of the volu
volume
me % evapo
evaporate
rated
d
loss. or recovered,
r    = repeatabil
repeatability
ity of the temp
temperat
erature
ure at the pre-
A4.8   Precision: scribed temperature at the observed percent
A4.8.1 The statistical
statistical determinat
determination
ion of the precision
precision of the distilled,
volume % evaporated or recovered at a prescribed temperature  R   = rep
reprod
roduci
ucibil
bility
ity of the tem
temper
peratu
ature
re at the
has not been directly measured in an interlaboratory program. prescribed temperature at the observed per-
It can be shown that the precision of the volume % evaporated cent distilled, and
or recovered at a prescribed temperature is equivalent to the S C (S F )   = rate of chang
changee in temp
temperat
erature
ure readi
reading
ng in °C
precision of the temperature measurement at that point divided (°F) per the volume % evaporated or recov-
by ththee ra
rate
te of ch
chan
ange
ge of tetemp
mper
erat
atur
uree ve
vers
rsus
us vo
volu
lume
me % ered.
evaporated or recovered. The estimation of precision becomes A4.8.5 Examp
Examplesles on how to calcu
calculate
late the repeatabilit
repeatability
y and
less precise at high slope values. the reproducibility are shown in Appendix
in  Appendix X2.
X2.

A5. REPEA
REPEATABILITY
TABILITY FOR
FOR GROUP 0 SAMPLES

A5.1 Dif
Differences
ferences in duplicate temperature
temperature readings
readings for each where:
prescribed
prescribed perce
percentag
ntagee point should not exce
exceeded the amounts T  x  (V)  
= temperat
temperatureure read
reading
ing of samp
sample
le x at volum
volumee
equivalent to 2 mL of distillate at each point in question. V ,
T  x  (V + 2 )   = temp
temperat
erature
ure reading
reading of sampl
samplee x at volume
volume
V  +
  + 2 mL, and
A5.2
ings 2 mLThe differe
dif
apart ference,
for nce,   d , in temperature
Determination between
1 at Volume   istwo
  V  is read-
either: T  x  (V − 2 )   = temp
temperat
erature
ure reading
reading of sampl
samplee x at volume
volume
V  −
  − 2 mL.
d 1 5 | T 1 ~V  2 2! 2 T 1~V ! | or (A5.1)
A5.2.2 To be conse
conservati
rvative,
ve, we now choose the smallest of 
smallest
d 2 5 | T 1 ~V   1 2! 2 T 1~V ! | (A5.2) these four values, that is,
A5.2.1 For Determinati
Determination
on 2, the two values of   d   are d min 5 lowest value of  d 
 d 1,  d 2,  d 3, or  d 4   (A5.5)

d 3 5 | T 2 ~V  2 2! 2 T 2~V ! | or (A5.3) A5.2.3 Duplicate

Duplicate temp
temperat
erature
ure readings are deem
deemed
ed to be
within the repeatability criterion if 
d 4 5 |  T 2 ~V   1 2! 2 T 2~V ! | (A5.4) |  T 1 ~V ! 2 T 2 ~V ! | # d min   (A5.6)

20
 

D 86 – 05
APPENDIXES

(Nonmandatory Information)

X1. EXAMPLES ILLUSTRATING CALCULATIONS

CALCULATIONS FOR REPORTING OF DATA
DATA

X1.2   Temperature Readings at Prescribed

Prescribed Percent Evapo-
rated:

X1.2.1
X1.2.1 loss
observed Temp
emperaeratur
ture
 %erecovered)
=  5.3 %
= 5.3 readin
reading
g at(see
10  11.6.1)
% eva
evapor
11.6.1 porate
)  are ated
as dfollows:
(4.7
(4.7%

T 10 E  ~°C ! 5 33.7 1 [~40.3 2 33.7!   (X1.5)

~5.3 2 5! / ~10 2 5!# 5 34.1°C 
T 10 E  ~°F ! 5 92.7 1 [~104.5 2 92.7!   (X1.6)
~5.3 2 5! / ~10 2 5!# 5 93.1°F 

X1.2.2 Temperatu
Temperature re read
reading
ing at 50 % evap
evaporate
orated
d (45.3 %
recovered) (see 11.6.1
(see  11.6.1))  are as follows:
T 50 E ~°C ! 5 93.9 1 [~108.9 2 93.9!   (X1.7)
~45.3 2 40! / ~50 2 40!# 5 101.9°C 
T 50 E  ~°F ! 5 201 1 [~228 2 201!   (X1.8)
~45.3 2 40! / ~50 2 40!# 5 215.3°F 
FIG. X1.1 Example of Test Report
X1.2.3 Temperatu
Tempe
recovered) rature
re)  are
(see  11.6.1)
(see 11.6.1 reading
read ing
as at 90 % evap
follows: evaporate
orated
d (85.3 %
X1.1 The observed distillation data used for the calculation
T 90 E  ~°C ! 5 181.6 1 [~201.6 2 181.6!   (X1.9)
of the examples below are shown in the first three columns of 
Fig. X1.1.
X1.1. ~85.3 2 85! / ~90 2 85! ] 5 182.8°C 

X1.1.1 Tempe
emperatur
raturee read
readings
ings corrected
corrected to 101.3 kPa (760 T 90 E  ~°F ! 5 358.9 1 [~394.8 2 358.9!   (X1.10)
mm Hg) pressure (see 11.3
(see  11.3)) are as follows: ~85.3 2 85! / ~90 2 85!# 5 361.0°F 
correction   ~°C ! 5 0.0009 ~101.3 2 98.6! ~273 1 t c!   (X1.1) X1.2.4 Temperatu
Temperaturere read
reading
ing at 90 % evap
evaporate
oratedd (85.3 %
correction ~°F ! 5 0.00012 ~760 2 740! ~460 1 t  f !   (X1.2) recovered) not corrected to 101.3 kPa pressure (see  11.6.1
 11.6.1)) are
X1.1.2
X1. 1.2 Loss
Loss cor
correc
rectio
tion
n to 101
101.3
.3 kPa (se
(seee   11.4)
11.4) are as as follows:
follows. The data for the examples are taken from  Fig. X1.1.
X1.1. T 90 E  ~°C ! 5 180.5 1 [~200.4 2 180.5!   (X1.11)

corrected loss 5 ~0.5 1 ~4.7 2 0.5! / (X1.3) ~85.3 2 85! / ~90 2 85!# 5 181.7°C 

$1 1 ~101.3 2 98.6! /8.0% 5 3.6 T 90 E  ~°F ! 5 357 1 [~392 2 357!   (X1.12)

X1.1.3 Recovery correction

correction to 101.3 kPa (see 11.4.1
(see 11.4.1))  are as ~85.3 2 85! / ~90 2 85!# 5 359.1°F 
follows: NOTE   X1.1—
X1.1—ResResults
ults cal
calcula
culated
ted fro
from
m °C data may not cor corres
respond
pond
corrected recovery 5 94.2 1 ~4.7 2 3.6! 5 95.3 (X1.4) exactly to results calculated from °F data because of errors in rounding.

X2. EXAMPLES OF CALCULATION OF REPEATABILITY

REPEATABILITY AND REPRODUCIBILITY OF VOLUME % (RECOVERED OR
EVAPORATED) AT A PRESCRIBED TEMPERATURE READING

X2.1
X2 .1 So
Someme sp
spec
ecifi
ifica
cati
tion
onss re
requ
quir
iree th
thee re
repo
port
rtin
ing
g of th
thee X2.2.1.1
X2.2.1.1 Dete
Determin
rminee first the slope at the desired
desired tempe
tempera-
ra-
volume % evaporated or recovered at a prescribed temperature. ture:
Table X2.1 shows
X2.1  shows the distillation data of a Group 1 sample as S C  % 5 0.1 ~T  ~20! 2 T  ~10!!   (X2.1)
obtained by an automated unit.
5 0.1 ~94 2 83!
X2.2   Example Calculation:
Calculation: 5 1.1
X2.2.1 For a Group 1 sample exhibiting
exhibiting distillation
distillation charac- S F  % 5 0.1 ~T  ~20! 2 T  ~10!!
teristics as per Table
per  Table X2.1,
X2.1, as determined by an automated unit,
the repro
reproducib
ducibilit
ility
y of the volum
volumee evap
evaporate d,Rvolume %, at
orated, 5 0.1 ~201 2 182 !
93.3°C (200°F) is determined as follows: 5 1.9

21
 

D 86 – 05
TABLE
TABLE X2.1 Distillati
Distillation
on Data from a Group 1 Sample Automated
Automated  R 5 3.3 1 2.0 ~S C !   (X2.2)
Distillation
5 3.3 1 2.0 3 1.1
Volume (mL)
Distillation Point
Distillation 5 5.5
  Tempe
emperatur
rature°
e° C Tempe
emperatur
rature
e °F Recovered at
Recovered, mL
93.3°C (200°F)
 R 5 6.0 1 2.0 ~S F !
18.0
10 84 183 5 6.0 1 2.0 3 1.9
20 94 202
5 9.8
30 103 217
40 112 233
X2.2.3 From the calculat
calculated
ed value of  R
 R , determine the value
Distillation Point   Tempe
Distillation emperatur
rature°
e° C Tempe
emperatur
rature°
e° F Volume (mL0
Evaporated at of volume, as described in A4.8.4
in  A4.8.4..
Evaporated, mL
93.3°C (200°F)  R volume % 5  R / ~S C !   (X2.3)
18.4 5 5.5/1.1
10 83 182
20 94 201 5 5.0
30 103 217
40 111 232  R volume % 5  R / ~S F !
5 9.8/1.9

X2.2.2 From Table
From  Table 9,
9,  determine the value of   R, the repro- 5 5.1
ducibility at the observed percentage distilled. In this case, the
observed percentage distilled is 18 % and

X3. TABLES OF CORRECTED LOSS FROM MEASURED

MEASURED LOSS AND BAROMETRIC
BAROMETRIC PRESS
PRESSURE
URE

X3.1
X3 .1 Th
Thee ta
tabl
blee pr
pres
esen
ente
ted
d as   Fig. X3.
X3.1
1   can
can be used
used to X3.2
X3 .2 Th
Thee ta
tabl
blee pr
pres
esen
ente
ted
d as   Fig. X3.
X3.2
2   can
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.

22
 

D 86 – 05

FIG. X3.1 Corrected Loss from Observed Loss and Barometric Pressure kPa

FIG. X3.2 Corrected Loss from Observed Loss and Barometric Pressure mm Hg

23
 

D 86 – 05

X4. PROC
PROCEDURE
EDURE TO EMULATE
EMULATE THE EMERG
EMERGENT
ENT STEM ERROR OF A
MERCURY-IN-GLASS
MERCURY -IN-GLASS THERMOMETER

X4.1 Wh
X4.1 When
en an elelec
ectr
tron
onic
ic or ot
othe
herr se
sens
nsor
or wi
with
thou
outt an  7 C T elr   5 T t  2 0.000162 3 ~T t  2 20°C! 2
 ASTM  7 (X4.1)
emergent stem error is used, the output of this sensor or the
associated data system should emulate the output of a mercury-
in-glass thermometer. Based on information supplied by four X4.3 Whe
X4.3 When n a hig
high
h ran
range
ge thermom
thermometeeterr would have been
been
manufacturers of automated Test Method D 86 equipment, the used, no stem correction is to be applied below 35°C. Above
averaged
averaged equ
equati
ations
ons sho
shown
wn in   X4.2   and   X4.3   have
have bee
been
n this temperature the correction is calculated using the follow-
reported to be in use. ing formula:
X4.1.1 The equations
equations shown in X4.2
in  X4.2 have
 have limited applica-  8C T ehr    5 T t  2 0.000131 3 ~T t  2 35°C ! 2
 ASTM  8 (X4.2)
bility and are shown for information purposes only. In addition
to the correction for the emergent stem, the electronic sensor
and associated data system will also have to emulate the lag in where:
response time observed for mercury-in-glass thermometers. T elr    = emulated temperature in °C °C for low range
range thermom-
thermom-
eters,
X4.2
X4. 2 Whe
When n a low range
range thermom
thermometeeterr would have
have bee
been
n T ehr    = emu
emulat
lated
ed temperat
temperature
ure in °C for hig
high
h ran
range
ge ther-
ther-
used, no stem correction is to be applied below 20°C. Above mometers, and
this temperature, the correction is calculated using the follow- T t    = true temp
temperat
erature
ure in °C.
ing formula:

X5. EXPLANA
EXPLANATORY
TORY REPORT
REPORT FORMS

X5.1   Fig. X5.1 

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

24
 

D 86 – 05

FIG. X5.1 Percent Recovered Report Form

25
 

D 86 – 05

FIG. X5.2 Percent Evaporated Report Form

26
 

D 86 – 05
SUMMARY OF CHANGES

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue,
(D 86–04b), that may impact the use of this standard. (Approved July 1, 2005.)

(1) Re
Repl
plac
aced
ed Table
 Table 4 with
4  with new values. (4) Ad
Adde
ded
d Appendix X5,
X5,  and cross-reference in Section 12.1
Section  12.1..
(2) Re
Revi
vise
sed
d  9.1.2-9.1.2.2
 9.1.2-9.1.2.2,,  9.1.5
 9.1.5,, and Notes 9-11
Notes  9-11..
(3) Added   13.5.3   and foofootno
tnote
te ref
refere
erence
nce to the res
resear
earch
ch
report.

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue,
(D 86–04a), that may impact the use of this standard. (Approved May 1, 2004.)

(1) Repla
Replaced
ced dimensions
dimensions in Fig.
in  Fig. A2.1  and added Fig.
added  Fig. A2.2.
A2.2.

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue,
(D 86–04), that may impact the use of this standard. (Approved April 1, 2004.)

(1) Revis
Revised
ed 10.19.1.1
 10.19.1.1 and
 and added Note
added  Note 18.
18.

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue,
(D 86–03), that may impact the use of this standard. (Approved Feb. 1, 2004.)

(1) Corrected section cross-reference

cross-reference in 3.1.13
in 3.1.13.. (2) Corre
Corrected
cted table reference
referencess in  10.2
 10.2   and
and 10.3
 10.3..
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27