Petroleum products -- Determination of pour point

Cancels and replaces the first edition (1974). Gives a method for the determination of the pour point of petroleum products. Also describes a separate procedure suitable for the determination of the lower pour point of fuel oils, heavy lubricant base stock, and products containing residual fuel components.

Produits pétroliers -- Détermination du point d'écoulement

Naftni proizvodi - Določanje točke tečenja

General Information

Status
Withdrawn
Publication Date
30-Nov-1996
Withdrawal Date
04-Jun-2019
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
05-Jun-2019
Due Date
28-Jun-2019
Completion Date
05-Jun-2019

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ISO
INTERNATIONAL
3016
STANDARD
Second edition
1994-08-01
Corrected and reprinted
1995-03-15
Petroleum products - Determination of
pour Point
Produits petroliers - Dhermination du Point d ’koulement
Reference number
ISO 3016:1994(E)

---------------------- Page: 1 ----------------------
ISO 3016:1994(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be re-
presented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take patt in the work. ISO
collaborates closely with the International Electrotechnical Commission
(1 EC) 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 International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 3016 was prepared by Technical Committee
ISOnC 28, Petroleum products and lubricants.
This second edition cancels and replaces the first edition
(ISO 3016:1974), which has been technically revised.
Annex A forms an integral part of this International Standard.
0 ISO 1994
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopying and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland

---------------------- Page: 2 ----------------------
INTERNATIONAL STANDARD 0 ISO ISO 3016:1994(E)
Petroleum products - Determination of pour Point
WARNING - 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. lt 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.
4 Reagents and materials
1 Scope
This International Standard specifies a method for the
4.1 Sodium chloride (NaCI), crystals.
determination of the pour Point of Petroleum prod-
ucts. A separate procedure suitable for the determi-
nation of the lower pour Point of fuel oils, heavy
4.2 Calcium chloride (CaCI,), crystals.
lubricant base stock, and products containing residual
fuel components is also described.
4.3 Carbon dioxide (CO,), solid.
NOTE 1 A method for the pour Point of crude oils is
under development. The pour Point of crude oils may be
determined by the general procedure described in this
4.4 Coolant liquid: acetone, methanol or Petroleum
International Standard, but some crude oils may need a
naphtha.
modified pretreatment to avoid the loss of volatile material.
The precision in this International Standard was derived on
a Sample matrix that did not include crude oils (see note 5).
4.5 Wiping fluid: acetone, methanol or ethanol.
2 Definition
5 Apparatus (see figure 1)
For the purposes of this International Standard, the
following definition applies. 5.1 Test jar, cylindrical, of clear glass, flat-bottomed,
33,2 mm to 34,8 mm outside diameter and 115 mm
to 125 mm in height. The test jar shall have an inside
2.1 pour Point: Lowest temperature at which a
Sample of Petroleum product will continue to flow diameter of 30,O mm to 32,4 mm, with the constraint
when it is cooled under specified Standard conditions. that the wall thickness be no greater than 1,6 mm.
The jar shall be marked with a line to indicate a con-
tents level 54 mm + 3 mm above the inside bottom.
-
3 Principle
5.2 Thermometers, partial immersion type con-
After preliminary heating, the Sample is cooled at a
forming to the specifications given in annex A.
specified rate and examined at intervals of 3 “C for
flow characteristics. The lowest temperature at which
movement of the Sample is observed is recorded as 5.3 Cork, to fit the test jar, bored centrally to take
the pour Point. the test thermometer.

---------------------- Page: 3 ----------------------
0 ISO
ISO 3016:1994(E)
Position in the cooling bath (5.7) so that no more than
5.4 Jacket, watertight, cylindrical, metal, flat-
25 mm projects out of the cooling medium, and shall
bottomed, 115 mm + 3 mm in depth with inside di-
-
be capable of being cleaned.
ameter 44,2 mm to 45,8 mm, and a wall thickness of
approximately 1 mm. lt shall be supported in a vertical
Dimensions in millimetres
Q> int. 45,8
@ int. 44.2
Q, ext. 34,8
_Q, ext. 332
.
@ int. 32,4
@ int. 30,O
Thermometer
Cork
Coolant Level
‘L-.Y.Y:-:
----------
-m-m-s-s-m-s-
::::::
1:::::
_-----
: : 5 : z I
.:::-L:
L
Test jar-
%
Fill Level -
.
Jacket -
I
- .
4
i
Ln
7
Ki
Gasket -
I
- .
- .
: .
z
Disc
Cooling bath
Figure 1 - Apparatus for pour Point test

---------------------- Page: 4 ----------------------
Q ISO
ISO 3016:1994(E)
If it is necessary to heat the Sample to a temperature
5.5 Disc, of cork or felt approximately 6 mm in
greater than 45 “C to effect the transfer to the test jar,
thickness, to fit inside the jacket.
or when it is known that a Sample has been heated
to a temperature higher than 45 “C during the pre-
5.6 Gasket, ring form, approximately 5 mm in
ceding 24 h, or when the thermal history of the sam-
thickness, to fit snugly on the outside of the test jar
ple is not known, keep the Sample at room
and loosely inside the jacket. This gasket shall be
temperature for 24 h before testing it.
made of rubber, leather or other suitable material,
elastic enough to cling to the test jar and hard enough
6.2 Close the test jar (5.1) with the cork (5.3) carry-
to hold its shape.
ing the high-cloud-and-pour thermometer or, if the
expected pour Point is above 36 OC, the melting Point
NOTE 2 The purpose of the ring gasket is to prevent the
thermometer (annex A). Adjust the Position of the
test jar from touching the jacket.
cork and thermometer so that the cork fits tightly, the
thermometer and the test jar are coaxial, and the
5.7 Cooling bath, of a type suitable for obtaining
thermometer bulb is immersed to a depth which
the required temperatures. The size and shape of the
places the beginning of the capillary 3 mm below the
bath are optional, but a support to hold the jacket
surface of the Sample.
firmly in a vertical Position is essential. The bath
temperature shall be monitored by means of the ap-
6.3 Subject the Sample in the test jar to a prelimi-
propriate thermometer (specified in annex A) im-
nary treatment, appropriate to its pour Point, in ac-
mersed to the correct immersion depth. For the
cordante with 6.4 or 6.5.
determination of pour Points below 9 “C, two or more
baths are required. The required bath temperatures
6.4 Samples having pour Points above - 33 “C shall
shall be obtained either by refrigeration or by suitable
be treated as follows.
freezing mixtures, and shall be maintained at the de-
sired temperatures + 1,5 “C.
-
6.4.1 Heat the Sample without stirring to 9 “C above
NOTE 3 The freezing mixtures commonly used are as
the expected pour Point, or to 45 “C, whichever is
follows:
greater, in a bath maintained at 12 “C above the ex-
pected pour Point, but at least 48 “C.
pour-Point temperatures down to:
For
6.4.2 Transfer the test jar to a bath maintained at
9 “C: ice and water (tan be used to prepare the 0 “C
a)
24 “C + 1,5 “C.
bath in 6.8); -
-
12 “C: crushed ice and sodium chloride (4.1) (tan be
b)
6.4.3 When the Sample temperature reaches 9 “C
used to prepare the - 18 “C bath in 6.8);
above the expected pour Point (estimated as a multi-
ple of 3 “C), commence observations for flow in ac-
- 27 “C: crushed ice and Calcium chloride (4.2) (tan be
Cl
cordante with 6.7.
used to prepare the - 33 “C bath in 6.8);
6.4.4 If the Sample has not ceased to flow when the
-
57 “C: carbon dioxide (4.3) and coolant liquid (4.4) ‘)
d)
temperature has reached 27 OC, carefully remove the
(tan be used to prepare the - 51 “C and - 69 “C baths
in 6.8). test jar from the bath, wipe the outside surface with
a clean cloth moistened with wiping fluid (4.5), and
place it in the 0 “C bath (5.7) in accordance with 6.6.
5.8 Timing device, capable of measuring up to
Make observations for flow in accordance with 6.7
30 s with an accuracy of 0,2 s.
and cool as specified in the schedule given in 6.8.
6.5 Samples having pour Points of - 33 “C and be-
6 Procedure
low shall be treated as follows.
6.5.1 Heat the Sample without stirring to 45 “C in a
6.1 Pour the Sample into the test jar to
...

SLOVENSKI STANDARD
SIST ISO 3016:1996
01-december-1996
1DIWQLSURL]YRGL'RORþDQMHWRþNHWHþHQMD
Petroleum products -- Determination of pour point
Produits pétroliers -- Détermination du point d'écoulement
Ta slovenski standard je istoveten z: ISO 3016:1994
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST ISO 3016:1996 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

ISO
INTERNATIONAL
3016
STANDARD
Second edition
1994-08-01
Corrected and reprinted
1995-03-15
Petroleum products - Determination of
pour Point
Produits petroliers - Dhermination du Point d ’koulement
Reference number
ISO 3016:1994(E)

---------------------- Page: 2 ----------------------

ISO 3016:1994(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be re-
presented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take patt in the work. ISO
collaborates closely with the International Electrotechnical Commission
(1 EC) 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 International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 3016 was prepared by Technical Committee
ISOnC 28, Petroleum products and lubricants.
This second edition cancels and replaces the first edition
(ISO 3016:1974), which has been technically revised.
Annex A forms an integral part of this International Standard.
0 ISO 1994
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopying and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland

---------------------- Page: 3 ----------------------

INTERNATIONAL STANDARD 0 ISO ISO 3016:1994(E)
Petroleum products - Determination of pour Point
WARNING - 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. lt 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.
4 Reagents and materials
1 Scope
This International Standard specifies a method for the
4.1 Sodium chloride (NaCI), crystals.
determination of the pour Point of Petroleum prod-
ucts. A separate procedure suitable for the determi-
nation of the lower pour Point of fuel oils, heavy
4.2 Calcium chloride (CaCI,), crystals.
lubricant base stock, and products containing residual
fuel components is also described.
4.3 Carbon dioxide (CO,), solid.
NOTE 1 A method for the pour Point of crude oils is
under development. The pour Point of crude oils may be
determined by the general procedure described in this
4.4 Coolant liquid: acetone, methanol or Petroleum
International Standard, but some crude oils may need a
naphtha.
modified pretreatment to avoid the loss of volatile material.
The precision in this International Standard was derived on
a Sample matrix that did not include crude oils (see note 5).
4.5 Wiping fluid: acetone, methanol or ethanol.
2 Definition
5 Apparatus (see figure 1)
For the purposes of this International Standard, the
following definition applies. 5.1 Test jar, cylindrical, of clear glass, flat-bottomed,
33,2 mm to 34,8 mm outside diameter and 115 mm
to 125 mm in height. The test jar shall have an inside
2.1 pour Point: Lowest temperature at which a
Sample of Petroleum product will continue to flow diameter of 30,O mm to 32,4 mm, with the constraint
when it is cooled under specified Standard conditions. that the wall thickness be no greater than 1,6 mm.
The jar shall be marked with a line to indicate a con-
tents level 54 mm + 3 mm above the inside bottom.
-
3 Principle
5.2 Thermometers, partial immersion type con-
After preliminary heating, the Sample is cooled at a
forming to the specifications given in annex A.
specified rate and examined at intervals of 3 “C for
flow characteristics. The lowest temperature at which
movement of the Sample is observed is recorded as 5.3 Cork, to fit the test jar, bored centrally to take
the pour Point. the test thermometer.

---------------------- Page: 4 ----------------------

0 ISO
ISO 3016:1994(E)
Position in the cooling bath (5.7) so that no more than
5.4 Jacket, watertight, cylindrical, metal, flat-
25 mm projects out of the cooling medium, and shall
bottomed, 115 mm + 3 mm in depth with inside di-
-
be capable of being cleaned.
ameter 44,2 mm to 45,8 mm, and a wall thickness of
approximately 1 mm. lt shall be supported in a vertical
Dimensions in millimetres
Q> int. 45,8
@ int. 44.2
Q, ext. 34,8
_Q, ext. 332
.
@ int. 32,4
@ int. 30,O
Thermometer
Cork
Coolant Level
‘L-.Y.Y:-:
----------
-m-m-s-s-m-s-
::::::
1:::::
_-----
: : 5 : z I
.:::-L:
L
Test jar-
%
Fill Level -
.
Jacket -
I
- .
4
i
Ln
7
Ki
Gasket -
I
- .
- .
: .
z
Disc
Cooling bath
Figure 1 - Apparatus for pour Point test

---------------------- Page: 5 ----------------------

Q ISO
ISO 3016:1994(E)
If it is necessary to heat the Sample to a temperature
5.5 Disc, of cork or felt approximately 6 mm in
greater than 45 “C to effect the transfer to the test jar,
thickness, to fit inside the jacket.
or when it is known that a Sample has been heated
to a temperature higher than 45 “C during the pre-
5.6 Gasket, ring form, approximately 5 mm in
ceding 24 h, or when the thermal history of the sam-
thickness, to fit snugly on the outside of the test jar
ple is not known, keep the Sample at room
and loosely inside the jacket. This gasket shall be
temperature for 24 h before testing it.
made of rubber, leather or other suitable material,
elastic enough to cling to the test jar and hard enough
6.2 Close the test jar (5.1) with the cork (5.3) carry-
to hold its shape.
ing the high-cloud-and-pour thermometer or, if the
expected pour Point is above 36 OC, the melting Point
NOTE 2 The purpose of the ring gasket is to prevent the
thermometer (annex A). Adjust the Position of the
test jar from touching the jacket.
cork and thermometer so that the cork fits tightly, the
thermometer and the test jar are coaxial, and the
5.7 Cooling bath, of a type suitable for obtaining
thermometer bulb is immersed to a depth which
the required temperatures. The size and shape of the
places the beginning of the capillary 3 mm below the
bath are optional, but a support to hold the jacket
surface of the Sample.
firmly in a vertical Position is essential. The bath
temperature shall be monitored by means of the ap-
6.3 Subject the Sample in the test jar to a prelimi-
propriate thermometer (specified in annex A) im-
nary treatment, appropriate to its pour Point, in ac-
mersed to the correct immersion depth. For the
cordante with 6.4 or 6.5.
determination of pour Points below 9 “C, two or more
baths are required. The required bath temperatures
6.4 Samples having pour Points above - 33 “C shall
shall be obtained either by refrigeration or by suitable
be treated as follows.
freezing mixtures, and shall be maintained at the de-
sired temperatures + 1,5 “C.
-
6.4.1 Heat the Sample without stirring to 9 “C above
NOTE 3 The freezing mixtures commonly used are as
the expected pour Point, or to 45 “C, whichever is
follows:
greater, in a bath maintained at 12 “C above the ex-
pected pour Point, but at least 48 “C.
pour-Point temperatures down to:
For
6.4.2 Transfer the test jar to a bath maintained at
9 “C: ice and water (tan be used to prepare the 0 “C
a)
24 “C + 1,5 “C.
bath in 6.8); -
-
12 “C: crushed ice and sodium chloride (4.1) (tan be
b)
6.4.3 When the Sample temperature reaches 9 “C
used to prepare the - 18 “C bath in 6.8);
above the expected pour Point (estimated as a multi-
ple of 3 “C), commence observations for flow in ac-
- 27 “C: crushed ice and Calcium chloride (4.2) (tan be
Cl
cordante with 6.7.
used to prepare the - 33 “C bath in 6.8);
6.4.4 If the Sample has not ceased to flow when the
-
57 “C: carbon dioxide (4.3) and coolant liquid (4.4) ‘)
d)
temperature has reached 27 OC, carefully remove the
(tan be used to prepare the - 51 “C and - 69 “C baths
in 6.8). test jar from the bath, wi
...

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