EN ISO 9029:1995
(Main)Crude petroleum - Determination of water - Distillation method (ISO 9029:1990)
Crude petroleum - Determination of water - Distillation method (ISO 9029:1990)
The precision data of this procedure have only been determined for water contents up to 1 % (V/V). Includes principle, apparatus, solvent, calibration and recovery test, sampling, procedure, expression of results, precision and test report. The distillation apparatus is shown in figures 1 and 2. The precision of the method is shown in figure 3. The sample handling is described in annex A.
Rohöl - Bestimmung des Wassergehaltes - Destillationsverfahren (ISO 9029:1990)
Pétrole brut - Détermination de la teneur en eau - Méthode de distillation (ISO 9029:1990)
La présente Norme internationale prescrit une méthode de détermination de la teneur en eau des pétroles bruts par distillation. Les valeurs de fidélité n'ont été déterminées que pour des teneurs en eau allant jusqu'à 1 % (V/V).
Surova nafta - Določevanje vode - Destilacijska metoda (ISO 9029:1990)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-maj-1998
6XURYDQDIWD'RORþHYDQMHYRGH'HVWLODFLMVNDPHWRGD ,62
Crude petroleum - Determination of water - Distillation method (ISO 9029:1990)
Rohöl - Bestimmung des Wassergehaltes - Destillationsverfahren (ISO 9029:1990)
Pétrole brut - Détermination de la teneur en eau - Méthode de distillation (ISO
9029:1990)
Ta slovenski standard je istoveten z: EN ISO 9029:1995
ICS:
75.040 Surova nafta Crude petroleum
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL
STANDARD
First edition
1990-l 2-l 5
Crude petroleum - Determination of water -
Distillation method
- CWermination de ia feneur en eau - M6thode de
P&hole brut
dis tilla fion
Reference number
is0 9029: 1990(E)
IS0 90293 990(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work
of preparing International Standards is normally carried out through IS0
technical committees. Each member body interested in a subject for
which a technical committee has been established has the right to be
represented on that committee. International organizations, govern-
mental and non-governmental, in liaison with ISO, also take part in the
work. IS0 collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an lnter-
national Standard requires approval by at least 75 % of the member
bodies casting a vote.
International Standard IS0 9029 was prepared by Technical Committee
ISO/TC 28, Petroleum products and lubricants.
Annex A forms an integral part of this International Standard.
0 IS0 1990
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronic or mechanical, including photocopying and microfilm, without
permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l Cl-I-121 1 Genkve 20 l Switzerland
Printed in Switzerland
ii
_-- ~- -
INTERNATIONAL STANDARD IS0 9029:1990(E)
Determination of water - Distillation
Crude petroleum -
met hod
WARNlNG - The use of this International Standard may involve hazardous materials, operations and
equipment. This standard does not purport to address all of the safety problems 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.
3 Significance
1 Scope
A knowledge of the water content of crude oil is im-
This International Standard specifies a method for
portant in the refining, purchase, sale and transfer
determining water in crude oil by distillation. The
precision data have only been determined for water of products.
contents up to I % (V/v).
The amount of water as determined by this method
is used to correct the volume involved in the custody
transfer of oil.
2 Normative references
4 Principle
The following standards contain provisions which,
through reference in this text, constitute provisions A test portion is heated under reflux conditions with
of this International Standard. At the time of publi-
a water-immiscible solvent which co-distills with the
cation, the editions indicated were valid. All stan- water in the sample. Condensed solvent and water
dards are subject to revision, and parties to are continuously separated in a trap. The water set-
agreements based on this International Standard tles in the graduated section of the trap, and the
are encouraged to investigate the possibility of ap-
solvent returns to the distillation flask.
plying the most recent editions of the standards in-
dicated below. Members of IEC and IS0 maintain
registers of currently valid International Standards.
5 Apparatus
IS0 383:1976, Laboratory glassware - Interchange-
able conical ground joints. Usual laboratory apparatus, together with the fol-
lowing:
IS0 3170:1988, Petroleum liquids -- Manual
sampling.
5.1 General.
IS0 3171:1988, Petroleum liquids - Automatic pipe-
The recommended apparatus, shown in figure I,
line sampling.
consists of a glass distillation flask, a condenser, a
graduated glass trap and a heater. Other types of
IS0 4259:1979, Petroleum products - Determination
and application of precision data in relation to apparatus may be used for this International Stan-
dard, provided it can be demonstrated that they op-
methods of test.
erate within the precision established, in
accordance with IS0 4259, with the preferred appa-
IS0 5280:1979, Xylene for industrial use - Specifica-
ratus.
tion.
IS0 9029:1990(E)
5.2 Distillation flask.
7 Calibration and recovery test
A 1000 ml round-bottom glass distillation flask with
a 24/39 conical ground-glass socket shall be used.
7.1 General
5.3 Trap.
Before initial use, calibrate the trap in accordance
with 7.2. Before a series of tests, check the entire
A 5 ml graduated glass trap with 0,05 ml gradu-
apparatus in accordance with 7.3.
ations and 24/39 ground-glass cone and socket shall
be used.
7.2 Calibration
5.4 Condenser.
Before initial use, verify the accuracy of the gradu-
The trap (5.3) shall be fitted with a 400 mm Liebig
ation marks on the trap by adding 0,05 ml incre-
condenser.
ments of distilled water, from a 5 ml microburette
or a precision micro-pipette readable to the nearest
5.5 Drying tube.
0,Ol ml. If there is a deviation of more than 0,05 ml
between the water added and water observed, reject
A drying tube filled with a self-indicating dessicant
the trap or recalibrate.
shall be placed at the top of the condenser (5.4).
NOTE 1 This tube is to prevent entry of atmospheric
7.3 Recovery test
moisture.
Test the overall recovery of water in the entire ap-
5.6 Heater.
paratus by introducing 400 ml of dry (0,02 % water
maximum) xylene into the apparatus and proceed-
Any suitable gas or electric heater that can uni-
ing as described in clause 9. When this initial run is
formly distribute heat to the entire lower half of the
complete, discard the contents of the trap and add
flask may be used. An electric heating mantle is
I,00 ml + 0,01 ml of distilled water, from a burette
preferred for safety reasons.
or micro-pipette, directly to the distillation flask and
proceed again in accordance with clause 9. Repeat
5.7 Jet-spray tube, for washing down the con-
this procedure again, but adding 4,50 ml + 0,Ol ml
-
denser inner tube, as shown in figure 2.
of distilled water to the xylene in the distillation
flask.
5.8 Pick, made of brass or bronze, or scraper,
made of steel, with a PTFE tip, as shown in figure2.
The assembly of the apparatus is satisfactory only
if trap readings are within the tolerances specified
5.9 Calibration of the apparatus.
in table I.
The assembled apparatus shall be calibrated and
tested as described in clause 7 and the readings
7.4 Malfunctions
obtained shalt be within the tolerances specified.
A reading outside the limits suggests malfunctioning
due to vapour leaks, too rapid boiling, inaccuracies
6 Solvent
in the graduations of the trap, or ingress of extrane-
Use xylene meeting the requirements of IS0 5280. ous moisture. If such a malfunction can be identified,
The water content of the xylene is determined by eliminate the malfunction and repeat the recovery
carrying out a blank test (see 9.6). test described in 7.3.
Table 1 - Tolerances on water recovery
Permissible limits for recovered water
Volume of water added at 20 “C
Maximum capacity of trap at 20 T
at 20 “C
ml ml ml
5,OO 1 ,oo l,oo + 0,025
5,00 430 4,50 T 0,025
-
I
IS0 9029:1990(E)
portions, and add the rinsings to the flask. Drain the
8 Sampling (see annex A)
cylinder thoroughly to ensure complete test portion
transfer,
8.1 General
8.3.3 To determine water on a mass basis, weigh
Sampling is defined as all steps required to obtain
out a test portion (see 8.3.1), pouring the test portion
a representative sample of the contents of any pipe,
directly into the distillation flask. If it is necessary to
tank or other system and to place the sample into
use a transfer vessel (e.g. a beaker or a cylinder),
the laboratory test container.
rinse this vessel with five portions of xylene in the
same way as described in 8.3.2 and add the rinsings
8.2 Laboratory sample
to the flask, then calculate the mass of the test por-
tion.
Only representative samples obtained as specified
in IS0 3170 or IS0 3171 shall be used for this lnter-
9 Procedure (see also annex A)
national Standard.
9.1 The precision of this International Standard can
8.3 Preparation of test portions
be affected by water droplets adhering to surfaces
in the apparatus and therefore not settling into the
The following sample-handling procedure shall ap-
water trap to be measured. To minimize the prob-
ply in addition to those covered in 8.2.
lem, chemically clean all apparatus, at least daily,
to remove surface films and debris which hinder free
8.3.1 The size of the test portion shall be selected
drainage of water in the test apparatus. More fre-
as indicated in table2, based on the expected water
quent cleaning is recommended if the nature of the
content of the sample.
samples being run causes persistent contamination.
If there is any doubt about the homogeneity of the
9.2 To determine water on a volume basis, pro-
mixed sample, determinations shall be made on the
ceed as indicated in 8.3.2. Add sufficient xylene to
total volume of the sample if the sample size is
the flask to make the total volume 400 ml.
compatible with the expected water content (see ta-
ble 2). If this is not possible, a determination shall
92.1 To determine water on a mass basis, proceed
be made on at least three test portions. Include all
as indicated in 8.3.3. Add sufficient xylene to the
these results in the test report and record their av-
flask to make the total volume 400 ml.
erage as the water content of the sample.
9.2.2 A magnetic stirrer is the most effective device
8.3.2 To determine water on a volume basis,
to reduce bumping. Glass beads or other boiling
measure out mobile liquids in a cylinder of capacity
aids, although less effective, have been found to be
equal to the test portion size selected in 8.3.1. Take
llseful.
care to pour the sample slowly into the graduated
cylinder to avoid entrapment of air, and adjust the
level as closely as possible to the appropriate 9.3 Assemble the apparatus as shown in figure 1,
graduation. Carefully pour the contents of the cylin- making sure all connections are vapour- and liquid-
der into the distillation flask and rinse the cylinder tight. It is recommended that glass joints are not
greased. Circulate water, between 20 ‘C and 25 ‘C,
with a measured volume, consistent with the size of
the cylinder, through the condenser jacket.
of xylene (see clause 6), in five
Table 2 - Size of test portion
Expected water content Approximate test portion size
% (m/m) or O/o ( V/ v) g or ml
50,l to 100,o 5
25,l to 50,O 10
10,l to 25,O
5,l to 10,o 50
1,l to 5,0 100
0,5 to 1,o 200
Less than 0,5 200
IS0 9029:1990(E)
9.4 Apply heat to the flask. The type of crude oil v
- vo
c) O/O (m/m) = 2 112 x 100
being evaluated can significantly alter the boiling
characteristics of the crude/solvent mixture. Apply
where
heat slowly during the initial stages of the distillation
(approximately half an hour to one hour) to prevent
is the volume, expressed in millilitres, of
vo
bumping and possible loss of water from the system
water in the trap (rounded to the nearest
(condensate shall not proceed higher than three-
0,025 ml) when measurement is made on
quarters of the distance up the condenser inner tube
the solvent blank;
- point A in figure 1; to facilitate condenser wash-
down, the condensate should be held as close as is the volume, expressed in millilitres, of
VI
possible to the condenser outlet). After the initial the test portion;
heating, adjust the rate of boiling so that the
is the volume, expressed in millilitres, of
condensate proceeds no more than three-quarters
water in the trap (rounded to the nearest
of the distance up the condenser inner tube. Collect
0,025 ml);
the distillate in the trap at a rate of approximately 2
to 5 drops per second. Continue distillation until no
m is the mass, expressed in grams, of the
water is visible in any part of the apparatus, except
test portion;
in the trap, and the volume of water in the trap re-
mains constant for at least 5 min.
is the density, expressed in grams per
P
millilitre, of the sample.
If there is a persistent accumulation of water drop-
lets in the condenser inner tube, flush with xylene
It is assumed that the density of water is 1 g/ml.
[a jet-spray washing tube (5.7) or equivalent device
is recommended]. It is essential to shut off the heat Volatile water-soluble material, if present, may be
at least 15 min prior to wash-down to prevent measured as water.
bumping. The addition to the xylene wash of an oil-
Report the result as the water content rounded to
soluble emulsion breaker at a concentration of
the nearest 0,025 %.
1000 ppm helps dislodge the clinging water drops.
After flushing, redistill for at least 5 min, applying
the heat slowly to prevent bumping.
11 Precision
Repeat this procedure until no water is visible in the
The precision of the method as obtained by statis-
condenser and the volume of water in the trap re-
tical examination of inter-laboratory test results in
mains constant for at least 5 min. If this procedure
the range from 0,Ol % to I,0 % is as follows:
does not dislodge the water, use the pick or PTFE
scraper (5.8), or an equivalent device, to cause the
water to run into the trap.
11.1 Repeatability
The difference between successive test results ob-
9.5 When the car
...
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