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Ip

IP 143JOl

!{I/$

ASTM 06560-00

psg

BS 2000-143

: 2001

Determination of asphaltenes (heptane insolublesl) in


crude petroleum and petroleum products
.___-_-----_~--------~------- ----- -This standard does not purport to address all of the safety problerns associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability
of regulatory limitations prior to use.
- --.

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

may stlill be valid,

precision

values

%(m/m).

between

Values

outside

definitions

but may not give the

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

and the mixture

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.

dis tilla tiion


pressure.

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,

NOTE. 1 l-lot benzene appeared in the original definition


asphaltenes, but for health reasons, this material is no
longer used. The precision of this method, when using
toluene, has been found to be the same as when using

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

the top of the extractor.

Methylbenzene

51.

(toluene)

reagent

grade,

or nitration

Reflux

Heptane

the
Analytical

reagent

top

Apparatus

61.

General

Ground-glass

bott:om

joints

from

diameter

off this standard

for some

applications,

series

However,
parts

to avoid

shall

body,

and

the

match

0,5

mm

ground-glass

male

and the male


shall

given

in Fiigure

1 mm on the height

The female
match

condenser,

purposes

and female

extractor

on all other
joint

at the

ai: tlhe bottom1

of the

ground-glass

the

1.

and OD of

female

of

joint
the

at the
conical

flask.

have one of two

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

Figure 2 - Filter paper

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

of a size to fit the

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

and stir well

before

of

renders
C,

samples

mixing

not

8.2

42,

shall

in IS0 3170

Test Portion Preparation

Of borosilicate

samples

described

a rotovapor.

NOTE 3 A rotovapor in conjunction


with a nitrogen
atmosphere reduces the hazard of toluene evaporation
(see 10.7)L

6.7

specified,

taken by the procedures


is0 3171 .

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,

only for handling.

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

by the use of a strongly

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

for 30 min before

in the

weighing.

in the
cooling

ASPHALTENES

Table

Estimated

10

asphaltene

(HEPTANIE

1 - Test portion

content

INSOLUBLES),

IP143

size, flask and heptane

Test portion

% (m/m)

cl

Less than 0.5

sizer

Heptane

IO zt 2

300

~fr60

0.5 to 2.0

8 t

240

+ 60

Over 2.0 to 5.0

4tl

120 I!z 30

Over 5.0 to 10.0

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

Place the filter

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

the dish used previously

which

has

and

containing

been

cooling

for this

subject,ed

procedure

to
as was

oven
vessel

for 30 min to 60 min and re-weigh

by tare
purpose,

the

same

the

dish

asphaltenes.

NOTE 6 Asphaltenes are very susceptible to o:xidation,


and it is important. that the procedure specified in the
final drying stage is adhered to exactly as regards to
temperature and time.

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

Give the flask

flask

from

on a

by the one used initially,


added

(see clause

exceeding

and

with

residue

heptane,

paper

by

the liquid

and pour

in the

different

in

forceps,,

possible

as necessary.

for use as specified

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

f rolm ref Iux.


IO,.4

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 not less than

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

Over 10.0 to 25.0

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

no bias can be asisigned.

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.

valules less than I,00

content

and

the

of

between
results

operaltors
normal

mass

sample

difference

independent

in grams;

is the mass of the residue

Reproducibility,

in

test report

shall contain

at least the following

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;

France on four samples

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

and of lbeing heated

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),

dry the sample

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

200 ml1 separating

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

iand then decant

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

NOTE 9 The position of the temperature sensor in the


holder may be pre-marked before addition of the test
portion to the flask.
A.5.3

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

keep the rate of distillation


to 3 5 ml/min

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

flask and residue.

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

Place the liquid-in-glass


bottom

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

add t,he oily distilllate


by the method

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

the loss of volatile

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

1 I) for the determination

of

( R).
AS.7

Use

proIcedwe
asphaltene

this

residue

(see clause
content.

carry

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