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IP 143JOl
!{I/$
ASTM 06560-00
psg
BS 2000-143
: 2001
products
Scope
or relative
This
standard
specifies
determination
content
lubricating
260
procedure
of the heptane
of gas oil,
which
diesel
insoluble
fuel,
bitumen
oil,
has been
determination
Hydrometer
of density
method.
(= IS0 3675)
the
asphaltene
residual
and
topped
for
Laboratory
density
crude
fuel
oils,
petroleum
to an oil temperature
of
IP 365,
Crude
products
petroleum
and
Determination
U-tube
method.
(- IS0
Diefinitions
For the
purposes
liquid
of den&y
petroleum
- QsciIJating
12185)
C (see A.2.1).
The
prelcision
0,50
?h(M//;n)
this range
same
is applicable
and 30,O
to
precision
values
%(m/m).
between
Values
outside
definitions
of this
standard,
the
following
apply:
values.
31.
Oils
containing
additives
may
give
asphaltenes
erroneous
wax-free
results.
organic
but soluble
Normative
2
The
following
normative
which,
constitute
provisions
this
documents
through
of,
anty of
However,
standard
possibility
these
documents
the
latest
referenced
IS0 3 170,
PetroJeum liquids -
pipeline
IP 123,
not
3.2
crude petroleum
on
the
editions
residue
of
260
For undated
of the
liquids
products
sampling.
test
heptane
Automatic
the
Determination
of
atmospheric
at
(E IS0 3405)
Crude
petroleum
and
liquid
to an oil temperature
under
the
procedure
conditions
described
of
of the
in annex A.
Principle
portion
petroleum
precipitated
the
material
waxy
with
hot heptane
After
removal
mixed
and
substances
on a filter
are removed
with
reflux,
paper.
by washing
in an extractor.
of
are
is
under
waxy
collected
substances
by
sample
heated
asphaltenes,
The
material
143.1
of
asphaltenes
IP 160,
out
speciific plreparatory
and inorganic
characteristics
residue
distillation
C carried
4
Manual
from
normative
applies.
Petroleum
Petroleum
in hot toluene.
benzene.
samp,ling.
recent
indicated.
edition
document
3171,
do
based
to investigate
the most
text,
For dated
to,
or
publications
are encouraged
of applyiing
referelnces,
IS0
in this
p#arties to agreements
the normative
in heptane,
contain
reference
of this standard.
amendments
subsequent
revisions
apply.
insoluble
references
provisions
references,
material
the
waxy
separated
dissolution
substances,
from
in
hot
t,he
the
inorga~nic
toluene,
the
ASPHALTENES
is
extraction
solvent
asphaltenes
weighed.
Reagents
(HEPTANE
the
evaporated,,
INSOLUBLES),
6.2,
Condenser
With
a coil or double
or 34/35
and materials
IPI
surface,,
ground-glass
joinit
Methylbenzene
51.
(toluene)
reagent
grade,
or nitration
Reflux
Heptane
the
Analytical
reagent
top
Apparatus
61.
General
Ground-glass
bott:om
joints
from
diameter
for some
applications,
series
However,
parts
to avoid
shall
body,
and
the
match
0,5
mm
ground-glass
male
given
in Fiigure
1 mm on the height
The female
match
condenser,
purposes
and female
extractor
on all other
joint
at the
of the
ground-glass
the
1.
and OD of
female
of
joint
the
at the
conical
flask.
one of two.
to fit
300 mm.
extractor
are
dimensions.
grade.
length
to the dimensions
Tolerances
6l
[C,H,
Minimum
a 34/45
bottoim
grade.
Conforming
5.2
with
[C,H,CH,]
6.3
Analytical
fitted
at the
sources
to length
ratios.
For the
is suitable,
the diameter
itself
it is critical
joint
that
is from
the
Of borosilicate
and
10.2
can be
the
same
NOTE 2
suitalble.
flasks
glass
and Table
the bottom
male
or protuberance.
-5-7
Conical
6.4
may
, either
of each
recession
different
I),
of appropriate
with
ground-glass
Sizes 24/39,
24/29,
2!3/43
DIA
143.2
(see
joints
to fit
of the extractor.
HOLE
Figure 1 - Extractor
capacity
or 29/32
are
ASPHALTENES
(HEPTANE
6.16
Stopper
6.5
Of borosilicate
INSOLUBLES),
glass
conical
IP143
Mlixer
High-speeid,
non-aerating.
flask.
Evaporating
6.6
Of borosilicate
of
90 mm
vessel
glass.
Sampling
Unless
otherwise
vessel
Either
a hemispherical
5 mm diameter,
used in conjunction
or another
with
dish
suitable
Filter funinel
Whatman
grade
Test portions
shall
be
fuels
100
mm
5 mm diameter.
Filter papers
6.8
81.
drawn
subdivision.
glass,
110
mm
or
125
mm
from
Heat
but
using
the laboratory
after
thorough
viscous
to a temperature
liquid,
be
or
samples
which
above
80
the mixer
(6.16)
as necessary.
Heat
bitumens
samples
of
to a temperature
before
of
renders
C,
samples
mixing
not
8.2
42,
shall
in IS0 3170
Of borosilicate
samples
described
a rotovapor.
6.7
specified,
the sample
anid
Ihomogenize
penetration
grade
not exceeding
taking
and
residual
120
C,
an aliquot.
diameter.
8.3
Analytical
6.9
Capable
balance
of weighing
with
Samples
to a powder
an accuracy
of 0,l
mg.
8.4
Samples
prepared
6.10
Forceps
6.1 I
steel,
Timing
Electronic
6.12
in
descriibed
crude
Stainless
spade
ended.
or manual,
accurate
to 1 ,O s.
of maintaining
to 110
C.
6.13
Graduated
a temperature
of 100
OC
that
followed
6.14
of glass
or polytetrafluorethylene
Coolhg
Consisting
desiccant,
of
use a strong
9.3
oven
vessel
either
or another
dletergent
cleanlliness
(PTFE),
mlm by 3 mm diameter.
6.15
by the
desiccator
suitable
vessel
without
tightly-stoppered
vessel.
143.3
After
(6.12)
(6.15)
that
thie
quantities
of
(6.:3)
oxidizing
soaking
water,
to
rinsing,
distilled
use
clean
no
based
water
a propriletary
the
described
cleaning
8 g/I,
12 h,
analysis,
rinses
for 30
agent
iin
for at least
using forceps
oxidizing
dishes
cleanliness
peroxydisulfate
in tap
required
and
the
acid at approximately
itself,
acetone,
followed
the
150
sulfuric
acid
For routine
9.2
laboratory
detergent
Stirring. rods
Made
ammonium
Iby rinses
and then
mil capacity.
flasks
matches
or sulfuric:
50 ml and 100
it is known
negligible
be
procedure
Preparation
glass
as
shall
the
80 C.
all
concentrated
cylinders
A, unless
below
Clean
obtained
petroleum
with
contains
by a means
such
Capable
in annex
shall be ground
is takern.
crude
Apparatus
91
(6.6)
Oven
of
boiling
an aliquot
accordance
petroleum
material
device
of hard bitumens
before
glassware,
in 10.1.
longer
on visual
When
matches
the
appearance,
agent.
place
min,
the
and
glassware
cool
in the
weighing.
in the
cooling
ASPHALTENES
Table
Estimated
10
asphaltene
(HEPTANIE
1 - Test portion
content
INSOLUBLES),
IP143
Test portion
% (m/m)
cl
sizer
Heptane
IO zt 2
300
~fr60
0.5 to 2.0
8 t
240
+ 60
4tl
120 I!z 30
2tl
60 t
Zi!
0.8 t 0.2
25 to 30
Over 25.0
0.5 + 0.2
25 + 1
10.1
Estimate
sample,
or residue
extraction
asphaltene
obtained
masses
the
the
period
heptane
fllask
at a ratio
iif the
below
25
to
of 30
10.6
Table
the test
asphaltene
content
is
with
an
samples
content
heptane
of
Boil the
rf: 5 min.
end
of
(6.5),
Remove
this
min,
under
the flask
period,
and store
150
mixture
cool,
of 25 ml
these
reflux
for 60
with
cupboard
from
the
min
and dry
(6X),
weighed
agaiinst
not
for 90 min to
of
Figure
2 ~(SOas to prevent
in
creeping),
Thereafter,
forceps.
the
paper
and then
transfer
completely
as
quantities
the
washing,
decant
of hot
hot heptane
filter.
Set
Remove
and place
a flask
refllux with
4 drops/s;
the filter
the
heptane
from
the
(7.2)
only
the
using
the
aside,
without
contents
the
ml.
on a boiling
evaporation
of the
Wash
quantities
30
flask
0,2
out
water
a
bath
by
tare
fla:sk
of ,toluene
the
to
vessel
mg
the
Remove
in
all the
the paper.
9,) evaporating
nearest:
dish.
until
from
with
to a total
toluene
by
(see note
5),
unider
an
rotovapor
of nitrogen
- Perform
the evaporation
in a fume
cupboard.
10.8
Dry
(6.12)
for
(6.15)
the
30
dish
min.
and
Cool
contents
in the
in the
cooling
against
which
has
and
containing
been
cooling
for this
subject,ed
procedure
to
as was
oven
vessel
by tare
purpose,
the
same
the
dish
asphaltenes.
11
extractor
used
from
(6.3).
initially,
at a rate of 2 drops/s
end of the
by
dissolved
the rinsings
and contents
that
to
30 ml to 6;O ml of
refluxing
in
with
in 11.6.
reflux
the
small
atmosphere
heating
into
flask
from
on a
(see clause
exceeding
and
with
residue
heptane,
paper
by
the liquid
and pour
in the
different
in
forceps,,
possible
as necessary.
the funnel
Usiing
filter
as
rod ( 6.14)
as shown
using
paper,
rinse with
10.5
funnel
the
of the
removal
loss of asphaltenes
filter
agitation,
successive
through
folded
Without
flask
stirring
the
handle
the filter
final
paper,
been
a similar
CAIJTION
or until
bottom
at the
a stopper
time
Transfer
clealn
evaporation
values.
and contents
close
in a dark
calculated
60 min,
the
on evaporation
and continue
have
successive
above
volume
1 also gives
1 g of
the flask
has been
( 7.1),
10.7
portion
or
IO,.3
no residue
Replace
toluene
capacity,,
ml to each
For
asphaltene
be used.
in
and to which
nearest
indicated
of appropriate
expected
a minimum
shall
glasIs slide.
asphaltenes
%(m/m).
25 %(Mm),
leave
frorn
to the nearest
1 g, and to the
(7.2)
expected
extractor
of heptane
in
I.
Add
sample
quantity,
(6.4)
in Table
of the
the procedure
of 1 g and below,
1 into a flask
10.2
content
from
above
mg for masses
also shown
in
the
A, and weigh
1 mg for
Table
15
a fe!w drops
0,l
volume
ml
Procedure
annex
Volumes
condenser
to
for an
11.1
(m/,m),
Calculation
Calculate
of petroleum
A=
100
the asphaltene
products
content,
using
A, in %
the equation:
(M/G)
(1)
ASPHALTENES
(HEPTANE
where:
INSOLUBLES),
13.2
M
is the
mass
of
asphaltenes,
in
mass
of
test
in
grams;
G
Repeatability,
The
is the
portion,
grams.
difference
Calculate
%(m/xn),
manner
of
the
crude
described
asphaltene
content,
petroleum
in annex
C, in
obtained
same
apbparatus
prepared
A, using
in
normal
the
operat,lor
test
would,
of the test
only
the
operating
material
below
test
with
constant
operation
value
successive
same
under
on identical
the
two
by the
and correct
exceed
the equation:
between
results
conditions
11.2
IP143
in
in the
method,
one
case
in
twenty.
c = 100 (MRIGD)
r := 0,l
(2)
where
A is the average
result,
in %(m/m).
where:
13.3
M
is the
mass
of
asphaltenes,
grams;
R
The
is the
mass
distillation,
G
of the
residue
from
aliquot,
in grams;
5
is the
12
Expression
12.1
Report
crude
distilled,
of
nearest
0,05
12.2
Report
asphaltene
heptane
the
R=
insoluble
% (m/m),
heptane
of
the
values
nearest
of I,0
0,l
solvent
1956.
in
programme,
out
the
using toluene
in 1975
from
were
programme
to
1956
confirm
evaluation
the
precision.
in
in ?~(m/lm).
heptane
term
may
by
in
insoluble
asphaltenes
procedures
asphalten!es
using
alkanes
other
than
heptane.
alkanes
will
give
higher
will
give
lower
ratio
are defined
be associateld
agents
14
an
with
as precipitating
In genieral,
results,
results
The
other
and
light,er
heavier
than1 heptane,
but
can be assigned.
Test report
as
The
interlaboratory
programme
result,
by thlis procedure,
benzene
as solvent,
case
Since
determined
second
method,
% (m/m)
% (m/m),
using
one
0,2 A
no consistent
values
in
insoluble
General
precision
of the test
only
on
in the
Bias
similar
interlaboratory
below
would,
13.4#
alkanes
The
laboratories
material
operation
value
and
different
to the
Precision
13.1
different
A is the average
wherle
asphaltene
IP 143.
13
in
test
and correct
single
by
twenty.
by IP 143.
the
content
to
working
identical
exceed
two
obtained
nominally
of results
SJa(m/m),
greater,
petroleum
in grams.
content
and
the
of
between
results
operaltors
normal
mass
sample
difference
independent
in grams;
Reproducibility,
in
test report
shall contain
infor~mation:
was carried
No data
can
be
a)
a reference
to this
b)
all
details
identification
standard;
found.
NOTE 7 A recent
(1998) interlaboratory
programme in
with asphaltene contents in the
range of 0,50 %(~-&m) to 22,0 %(m/m) resulted in
estimated precision values very similar to those given in
13.2 and 13.3,, except for the reproducibility
at very
low levels [C ,T,O 9-6 (m/m)] which was significantly
worse.
for
necessary
of the
product
complete
testedl;
cl
the result
d)
any deviation,
from
e)
143.5
of the test
by
12);
agreemeint or otherwise,
the procedure
the date
(see clause
of the test.
specified;
ASPHALTENES
(HEPTANE
INSOLUBLES),
IP143
Annex A,
(normative)
Preparation
A.1
Scope
A.1 .I
This annex
preparation
describes
to an oil temperature
A.2
residue by distillation
A.3.3
of a crude
determination
of crude petroleum
a procedure
petroleum
of 260
of asphaltene
for the
residue
(topped
C) suitable
content
Drying
The drying
following:
apparatus
apparatus
shall
conisist
of one of the
for the
A3.3.
(see 9.4).
I Centrifuge
A.3.3.2
Principle
Filter apparatus,
operating
alt inicreased
pressure.
A Iweighed
sample
test
portion
i:s distilled
under
specified
conditions
of distillation
of
crude
petroleum
glass
apparatus
of heat
The distillation
temperature
residue
of the
in specified
260
input
and rate
is stopped
and
the
A.3#.3.3
1000
Steel container,
kPa pressure,
capable
of withstanding
to 200
C.
at an oil
mass
of
the
A.3(.3.4
Cottrell-type
electro:static
separator
determined.
A.4
A.3
Sample
Preparation
Apparatus
A.4,,1
A.3.1
Residue
The apparatus
of IP 123,
distillation
shall
with
apparatus
conform
to the
the exception
If the crude
water
requirements;
to cause
c:ontains
in distillation
foaming),
by a method
the
of
loss
given
of the temperature
petroleum
difficulties
volatile
in A.4.1.1
components.
to A.4.1
sufficient
(ex.cessive
that
The
avoids
methods
.5 are suitable.
sensor.
A.4,,1 .I
The temperature
tlhermometer
length
range
error
sensor
of
300
total
m/m to 320
of -4 C to 360
of
C,
meiasurement
or
be a liquid-in-glass
mm,
with
type
of
alternative
or
scale
of
at
least
transparent
bath,
at 15 C zt 3 C is mandatory
for the
receiver.
NOTE 8 A witable
A.3.2
The
Drying
apparatus
exception
the flask
by a
ice.
thermometer
distillation
shall
of a 500
specified,
is an IP 4C.
to
ml distillation
and the receiver
funnel
water
by
gravity
container
or
by
at the
lowest
the
lowest
temperature.
.2
Filter
through
flask
instead
the
of
is substituted
in broken
sample
anhydrous
sulfate,
or other
at
and
applied
calcium
suitable
pressure,
chloride,
drying
agent,
sodium
in a closed
vessel.
A.4.1.3
Heat
container
(A.3.3)
the
pressure
oil reaches
with
the
temperature
approximately
A.3.1
immersed
A.4.J
and
apparatus
conform
practicable
practicable
temperature
system
A
accuracy.
total
the
in a closed
a temperature
C, and a maximum
an
device
equivalenit
maintained
shall
immersion
Separate
centrifuging
pressure
with
Fill
sensor.
a temperature
reaches
700
closed
the
Iof 200
water.
steel
sensor
container
and heat
kPa. Allow
temperature
the separated
int a
a temperature
70 % capacity
cool to ambient
oil from
sample
fitted
to
it until the
C, or until
the container
the
to
the
ASPHALTENES
A.4. II .4 Constwct
a tall
glass
lined
with
and then
fitted
tightly
mounted
stirrer
glass
apply
has
saturated
30 rev/min
sample
to
the
precipitation
coalesced
the
run
to
and allow
oil from
the
down
Swab
assemble
the
flask
extending
hydrocarbons
Charge
the
in the apparatus
the flask
temperature
point
(bulb)
flask
gently
slowlly
by
with
flannel
so
means
that
the
oil
Allow
sensing
back
flame,
rises
any
drops
of the flask.
water
by means
vapour
tube
A.5.4
Place a clean
Procedure
A.5.l
Determine
below
to
the
the
of
Cover
crude
petroleum
A.52
Weigh
0,l
lg and
100
ml
durilng
the
during
it with
sample
that
at
no oil flows
this operation.
the
of the
bottom
temperature
give
dentical
bulb
of
the
overcome
the
down
Record
bath.
through
and
and mix
filter
is 2,0
flask,
mm
or
seinsor to a position
temperature
C of the
readings
the
to
0,l
g,
tube
of oil (D).
so that
0,5
of
the receiver
receiver
a piece
of the
up
biath
closely
of
and
paper
also
receiver
(below
or
lbut not
transparent
losses,
ice-cold
of
tube
.25 mm,
the
with
23
mllmin
heat
mm
the
from
alternative
established
to
to
the
at
a
it ceases
until
to
in the
4 C) water
A.56
without
the
heat
and
constant
the
at 2,0 ml/min
1 drop/s).
interruption
and
distil
allow
to
thie
Continue
260
C.
condenser
to
the receiver.
Allow
remove
flask
rate
not
exceeding
to foami, after which
(approximately
the
the
residue
temperature
within
mass
the
at the outlet
condlenser
the
volatile
Circulate
run off
the vapour
the
which
the condenser.
the-bist:illation
thermometer
tight
Immerse
in
buoyancy
petroleum
equivalent
to
and condenser
the
top
to restrict
Apply
to the nearest
a mass
15
flask
mark
distillation
weighted
crude
or IP 365.
the distillation
charge
of
ensuring
by IP 160
Make
it at least
the
A.5.5
funnel,
15
tube
50 mm.
dry receiver
that
ml mark.
ml
over
present,
at
flask
into
100
100
(A.3.1).
water
in A.4.1.2.
density
condlenser
and
or bung through
such
extends
drailn into
the
of
passes.
conldenser
Remove
A. 5
between
of a stopper
iand
tube
the
25 mm
tub/e
the vapour
Stop
passes
to cool,
is still
the
condenser
to the residue
water
described
Heat
the
the residue
If visible
in A.3.2.
and place
the
in the separating
into
gas
volatile
temperature
no more
colllected
thoroughly.
that
on the walls
when
in the distillatle.
the water
such
C, vaporizing
collect
the distillation
described
in the sample.
off a small
that
the more
ml of sample
sensor
is immersed
to l5Q
water
300
condenser
with
into
of between
adaptor
with
the
water
the
lining.
Distil off the water
out
the apparatus,
distance
the
A.4.1.5
IP143
the connection
electrodes.
at intervals
the
and
forms
into
components
Separate
with
INSOLUBLES),
it damp,
gauze
cylinder
of a laboratory
the
a voltage
from
cylinder,
to leave
brass
spindle
Pour
water
oil to cool.
that
gauze
been
out
at approximately
the
prevent
has
electrode.
and
Interrupt
the
the
rotated
central
that
separator
a brass
squeezed
inside.
on
beaker
with
flannel
water,
the
a Cottrell-type
beaker
(HEPTANE
in the
,flask
Record
to
and weigh
sensor,
cool,
the
the mass
of the residue
to
out
the
of
( R).
AS.7
Use
proIcedwe
asphaltene
this
residue
(see clause
content.
carry