FDUS 1696

FINAL DRAFT UGANDA

STANDARD First Edition
2017-mm-dd

Standard Test Method for Pour Point of Crude Oils

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Reference number
FDUS 1696: 2017

This Final Draft Uganda Standard, FDUS 1696: 2017, Standard Test Method for Pour
Point of Crude Oils, is based on ASTM D5853 − 11, Standard Test Method for Pour
Point of Crude Oils, Copyright ASTM International, 100 Barr Harbor Drive, West
Conshohocken, PA 19428, USA, pursuant to license with ASTM International © UNBS 2017
FDUS 1696: 2017

Compliance with this standard does not, of itself confer immunity from legal obligations

A Uganda Standard does not purport to include all necessary provisions of a contract. Users are
responsible for its correct application

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© UNBS 2017
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilised in any
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form or by any means, electronic or mechanical, including photocopying and microfilm, without prior written
permission from UNBS.

Requests for permission to reproduce this document should be addressed to

The Executive Director

Uganda National Bureau of Standards
P.O. Box 6329
Kampala
Uganda
Tel: +256 417 333 250/1/2/3
Fax:+ 256 414 286 123
E-mail: [email protected]
Web: www.unbs.go.ug

This Final Draft Uganda Standard, FDUS 1696: 2017, Standard Test Method for Pour Point of Crude Oils, is
based on ASTM D5853 − 11, Standard Test Method for Pour Point of Crude Oils, Copyright ASTM
International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA, pursuant to license with ASTM
International

ii © UNBS 2017 - All rights reserved

 FDUS 1696: 2017

National foreword

Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry of Trade, Industry and
Cooperatives established under Cap 327, of the Laws of Uganda, as amended. UNBS is mandated to co-
ordinate the elaboration of standards and is
(a) a member of International Organisation for Standardisation (ISO) and

(b) a contact point for the WHO/FAO Codex Alimentarius Commission on Food Standards, and

(c) the National Enquiry Point on TBT Agreement of the World Trade Organisation (WTO).

The work of preparing Uganda Standards is carried out through Technical Committees. A Technical

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Committee is established to deliberate on standards in a given field or area and consists of representatives of
consumers, traders, academicians, manufacturers, government and other stakeholders.

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Draft Uganda Standards adopted by the Technical Committee are widely circulated to stakeholders and the

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general public for comments. The committee reviews the comments before recommending the draft standards
for approval and declaration as Uganda Standards by the National Standards Council.
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This Final Draft Uganda Standard, FDUS 1696: 2017, Standard Test Method for Pour Point of Crude Oils, is
based on ASTM D5853 − 11, Standard Test Method for Pour Point of Crude Oils, Copyright ASTM
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International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, USA, pursuant to license with ASTM
International.
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This standard was developed by the Subcommittee on Petroleum and petrochemical products, SC 1, under
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the Petroleum Standards Technical Committee (UNBS/TC 16)

Wherever the words, “ASTM Standard" appear, they should be replaced by "Uganda Standard."
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© UNBS 2017 - All rights reserved iii

 Designation: D5853 − 11

Designation: 441/99

Standard Test Method for

Pour Point of Crude Oils1
This standard is issued under the fixed designation D5853; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents

1.1 This test method covers two procedures for the deter- 2.1 ASTM Standards:2
mination of the pour point temperatures of crude oils down to D97 Test Method for Pour Point of Petroleum Products
−36°C. Procedure A provides a measure of the maximum D130 Test Method for Corrosiveness to Copper from Petro-

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(upper) pour point temperature and is described in 9.1. Proce- leum Products by Copper Strip Test
D323 Test Method for Vapor Pressure of Petroleum Products

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dure B provides a measure of the minimum (lower) pour point
temperature and is described in 9.2. (Reid Method)

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D4057 Practice for Manual Sampling of Petroleum and
1.2 The use of this test method is limited to use for crude Petroleum Products
oils. Pour point temperatures of other petroleum products can D4177 Practice for Automatic Sampling of Petroleum and

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be determined by Test Method D97. IC Petroleum Products
1.3 The values stated in SI units are to be regarded as E1 Specification for ASTM Liquid-in-Glass Thermometers
standard. No other units of measurement are included in this E77 Test Method for Inspection and Verification of Ther-
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standard. mometers
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1.4 WARNING—Mercury has been designated by many 3. Terminology

regulatory agencies as a hazardous material that can cause
3.1 Definitions of Terms Specific to This Standard:
central nervous system, kidney and liver damage. Mercury, or
3.1.1 maximum (upper) pour point, n—the pour point ob-
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its vapor, may be hazardous to health and corrosive to

tained after the test specimen has been subjected to a pre-
materials. Caution should be taken when handling mercury and
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scribed treatment designed to enhance gelation of wax crystals

mercury containing products. See the applicable product Ma-
and solidification of the test specimen.
terial Safety Data Sheet (MSDS) for details and EPA’s
3.1.2 minimum (lower) pour point, n—the pour point ob-
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website—http://www.epa.gov/mercury/faq.htm—for addi-
tained after the test specimen has been subjected to a pre-
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tional information. Users should be aware that selling mercury

and/or mercury containing products into your state or country scribed treatment designed to delay gelation of wax crystals
may be prohibited by law. and solidification of the test specimen.
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3.1.3 pour point, n—the lowest temperature at which move-

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1.5 This standard does not purport to address all of the

ment of the test specimen is observed under the conditions of
safety concerns, if any, associated with its use. It is the
the test.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4. Summary of Test Method
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 7. 4.1 After preliminary heating, the test specimen is cooled at
a specified rate and examined at intervals of 3°C for flow
characteristics. The lowest temperature at which movement of
the test specimen is observed is recorded as the pour point.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.07 on Flow Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2011. Published July 2011. Originally approved contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
in 1995. Last previous edition approved in 2009 as D5853–09. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D5853-11. the ASTM website.

*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
Copyright by ASTM Int'l (all rights reserved); Wed Jun 8 01:06:17 EDT 2016
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 D5853 − 11

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NOTE 1—All dimensions are stated in millimetres.
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FIG. 1 Apparatus for Pour Point Test

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5. Significance and Use Thermometer

Number
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5.1 The pour point of a crude oil is an index of the lowest Thermometer Temperature Range
ASTM IP
temperature of handleability for certain applications.
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High cloud and pour −38 to +50°C 5C 1C

5.2 This is the only pour point method specifically designed Low cloud and pour −80 to +20°C 6C 2C
for crude oils. Melting point +32 to +127°C 61C 63C
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5.3 The maximum and minimum pour point temperatures 6.1.2.1 Since separation of liquid column thermometers
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provide a temperature window where a crude oil, depending on occasionally occurs and may escape detection, the ice point of
its thermal history, might appear in the liquid as well as the the thermometers shall be checked prior to the test and used
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solid state. only if they are accurate within 61°C (see Test Method E77).
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5.4 The test method can be used to supplement other 6.1.3 Cork, to fit the test jar, center bored for the test
measurements of cold flow behavior. It is especially useful for thermometer.
the screening of the effect of wax interaction modifiers on the 6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed,
flow behavior of crude oils. 115 6 3 mm depth, with inside diameter of 44.2 to 45.8 mm.
It shall be supported in a vertical position in the cooling bath
6. Apparatus (6.1.7) so that no more than 25 mm projects out of the cooling
medium. The jacket shall be capable of being cleaned.
6.1 Pour Point Test Apparatus Assembly (see Fig. 1):
6.1.1 Test Jar, cylindrical, of clear glass, flat bottomed, 6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
outside diameter 33.2 to 34.8 mm, and height 115 to 125 mm. jacket.
The inside diameter of the jar can range from 30.0 to 32.4 mm, 6.1.6 Gasket, to fit snugly around the outside of the test jar
within the constraint that the wall thickness shall be no greater and loosely inside the jacket. The gasket shall be made of
than 1.6 mm. The jar shall have a line to indicate a sample rubber, leather, or other material that is sufficiently elastic to
height 54 6 3 mm above the inside bottom. The inside of the cling to the test jar and hard enough to hold its shape. Its
test jar (up to the mark) shall be visibly clean and free of purpose is to prevent the test jar from touching the jacket.
scratches. 6.1.7 Cooling Bath or Baths, of a type suitable for obtaining
6.1.2 Thermometers, having ranges shown in the following the required temperatures. The size and shape of the bath are
table and conforming to the requirements prescribed in Speci- options, but a support to hold the jacket firmly in a vertical
fication E1 for thermometers: position is essential. The bath temperature shall be monitored

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 D5853 − 11
TABLE 1 Cooling Mixtures and Bath Temperatures
Bath Temperature
Ice and water 0 ± 1.5°C

Crushed ice and sodium chloride crystals or −18 ± 1.5°C

Acetone or petroleum naphtha or methanol or ethanol
(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –33 ± 1.5°C

(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –51 ± 1.5°C

(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –69 ± 1.5°C

(see Section 7) with solid carbon dioxide added to
give the desired temperature

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by means of the appropriate thermometer (6.1.2) or any other 7.4 Sodium Chloride Crystals—Commercial or technical

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temperature measuring device capable of measuring and dis- grade sodium chloride is suitable.
playing the designated temperature with the required precision

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7.5 Ethanol or Ethyl Alcohol—A commercial or technical
and accuracy. The required bath temperatures shall either be grade of dry ethanol is suitable for the cooling bath.
obtained by refrigeration or by suitable cooling mixtures and (Warning—Flammable. Denatured. Cannot be made non-

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shall maintain the designated temperatures to within 61.5°C. toxic.)
Cooling mixtures commonly used for bath temperatures are
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shown in Table 1. 7.6 Methanol or Methyl Alcohol—A commercial or techni-
cal grade of dry methanol is suitable for the cooling bath.
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6.2 Water Bath—The size and shape of the bath are optional, (Warning—Flammable. Vapor harmful.)
but a support to hold the test jar immersed in the bath to above
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the sample height in the test jar and in a firm vertical position 8. Sampling, Test Samples, and Test Specimens
is required. The required bath temperature may be maintained NOTE 3—Sampling is defined as all steps required to obtain a portion of
by any suitable means, provided the temperature can be the contents of any pipe, tank, or other system and to place the sample into
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monitored and controlled to the designated temperature (61°C the laboratory test container.
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(9.1.4; 9.2.4)). 8.1 Laboratory Sample—It is essential that the sample

6.3 Pressure Vessel, constructed of stainless steel according received by the laboratory is representative of the batch or lot
to the dimensions given in Fig. 2, and capable of withstanding of crude oil from which it was taken. Practices D4057 and
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a test pressure of 700 kPa. Alternative designs for the pressure D4177 provide guidance for obtaining such representative
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vessel cap and synthetic rubber gasket may be used provided samples.
that the internal dimensions of the pressure vessel are the same 8.2 Preparation of Test Samples—The pour point of crude
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as those shown in Fig. 2. oils is very sensitive to trace amounts of high melting waxes.
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NOTE 1—This pressure vessel is identical to the pressure vessel Exercise meticulous care to ensure such waxes, if present, are
described in Test Method D130. either completely melted or, if volatility constraints prevent
6.4 Timing Device, capable of measuring up to 30 s with a heating to complete melting, homogeneously suspended in the
resolution of at least 0.1 s and an accuracy of 60.2 s or better. sample (Appendix X1). Inspect the walls of the original
container to ensure that no high melting point material is left
7. Reagents and Materials sticking to the wall.
7.1 The following solvents of technical grade are appropri- NOTE 4—It is not possible to define universal mandatory rules for the
ate for low-temperature bath media. preparation of crude oil test samples. Guidelines for sample handling for
the most common situations are given in Appendix X1.
7.1.1 Acetone, (Warning—Extremely flammable.)
7.1.2 Petroleum Naphtha, (Warning—Combustible. Vapor
9. Procedure
harmful.)
9.1 Procedure A for Maximum (Upper) Pour Point:
NOTE 2—Typical petroleum naphtha used for cleaning purposes are VM
and P naphthas.
9.1.1 Pour the test sample into the test jar to the level mark.
If necessary, reheat the test sample to a temperature at least
7.2 Toluene, technical grade (Warning—Flammable. Vapor 20°C above the expected pour point (8.2 and Appendix X1) but
harmful.). not higher than a temperature of 60°C (Warning—The vapor
7.3 Solid Carbon Dioxide, (Warning—Extremely cold pressure of crude oils at temperatures higher than 60°C will
(−78.5°C).) usually exceed 100 kPa. Under these circumstances the sample

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 D5853 − 11

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FIG. 2 Pressure Vessel

container may rupture. Opening of the container may induce 9.1.3 Keep the test jar with the test specimen at room
foaming with resultant loss of sample and possible injury to temperature (between 18 and 24°C) for at least 24 h.
personnel.) NOTE 5—The pour point of a crude oil is dependent on the state of
9.1.2 Immediately close the test jar with the cork carrying crystallization of the wax in the test specimen. In crude oils, achieving
the high cloud and pour thermometer, or, if the expected pour equilibrium between crystallized wax and dissolved wax is a rather slow
point is above 36°C, the melting point thermometer. Adjust the process. However, experience has shown that in a majority of cases, such
position of the cork and thermometer so the cork fits tightly, the an equilibrium is reached within 24 h.
thermometer and the jar are coaxial, and the thermometer bulb 9.1.4 If the expected pour point is greater than 36°C, heat
is immersed to a depth that places the beginning of the the sample to 9°C above the expected pour point. If the
capillary 3 mm below the surface of the test specimen. expected pour point is less than 36°C, heat the sample to a

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 D5853 − 11
temperature of 45 6 1°C. Maintain the water bath (6.2) to heat ment before 5 s has passed, replace the test jar immediately in
the sample at 48 6 1°C or at a temperature 12°C higher than the jacket, and repeat a test for flow at the next temperature,
the expected pour point, whichever is higher. 3°C lower.
9.1.4.1 As soon as the test specimen has reached the 9.1.8 Continue in this manner until a point is reached at
required temperature, remove the cork carrying the thermom- which the test specimen shows no movement when the test jar
eter and stir the test specimen gently with a spatula or similar is held in a horizontal position for 5 s. Record the observed
device. Put the cork carrying the thermometer back in place reading of the test temperature.
(see 9.1.2). 9.1.8.1 If the test specimen has reached −36°C and still
9.1.5 Ensure that the disk, gasket, and the inside of the shows movement, discontinue the test.
jacket are clean and dry. Place the disk in the bottom of the
jacket. Place the disk and jacket in the cooling medium a NOTE 7—To determine compliance with existing specifications having
pour point limits at temperatures not divisible by 3°C, it is acceptable
minimum of 10 min before the test jar is inserted. The use of practice to conduct the pour point measurement according to the following
a jacket cover, while the empty jacket is cooling, is permitted. schedule. Begin to examine the appearance of the test specimen when the
Remove the test jar from the water bath and dry with a tissue. temperature of the test specimen is 9°C above the specification pour point.
Place the gasket around the test jar, 25 mm from the bottom. Continue observations at 3°C intervals as described in 9.1.6 and 9.1.7 until
Insert the test jar into the jacket in the first bath maintained at the specification temperature is reached. Report the sample as passing or
failing the specification limit.
21°C and commence observations for pour point. Never place

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a test jar directly into the cooling medium. 9.2 Procedure B for Minimum (Lower) Pour Point:
9.1.6 Exercise care not to disturb the mass of test specimen 9.2.1 Pour 50 g of the test sample into a clean pressure

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nor permit the thermometer to shift in the test specimen; any vessel (6.3 and Note 8). When necessary, reheat the test sample

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disturbance of the spongy network of wax crystals will lead to to a temperature of at least 20°C above the expected pour point
a lower pour point and erroneous results (Note 5). (8.2 and Appendix X1) but not higher than 60°C (Warning—
The vapor pressure of crude oils at temperatures higher than

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NOTE 6—With dark colored materials, such as crude oils, it is
impractical to observe, in the test jar, the onset of crystallization and
IC 60°C will usually exceed 100 kPa. Under these circumstances
network formation in the test specimen. Hence, it is presumed that the sample container may rupture. Opening of the container
network formation will begin at the very early stages of the cooling may induce foaming with resultant loss of sample and possible
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sequence. injury to personnel.) Check that the rubber ring is in place and
9.1.7 Pour points are expressed in temperatures which are screw the lid on tightly.
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positive or negative multiples of 3°C. Begin to examine the NOTE 8—The pressure vessel may be cleaned by any appropriate
appearance of the test specimen when the temperature of the solvent, provided the solvent is capable of dissolving remnants of high
test specimen is 9°C above the expected pour point (estimated
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melting wax and asphaltenes. Hot toluene (100°C) has been found to be an
as a multiple of 3°C). At each test thermometer reading which appropriate solvent for this purpose.
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is a multiple of 3°C below the starting temperature, remove the 9.2.2 Heat the pressure vessel in an oil bath or by any other
test jar from the jacket. When necessary, remove moisture that suitable means to a temperature of 105 6 2°C and leave at that
limits visibility of the test specimen by wiping the surface of
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temperature for at least 30 min.

the test jar with a clean cloth moistened in alcohol at
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approximately the temperature of the test specimen in the jar. 9.2.3 Take the pressure vessel from the oil bath, wipe and
Then tilt the jar just enough to ascertain whether there is dry the surface of the pressure vessel, swirl gently to homog-
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movement of the test specimen in the jar. When movement is enize the contents, and leave the pressure vessel to cool at
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observed, immediately return the test jar into the jacket. If room temperature for exactly 20 min.
movement of the specimen in the test jar is noted, then replace 9.2.4 Carefully open the pressure vessel and transfer the
the test jar immediately in the jacket, and repeat a test for flow sample into the test jar filling to the level mark of the test jar,
at the next temperature, 3°C lower. Typically the complete preheated in a water bath (6.2) kept at a temperature of 48 6
operation of removal, wiping, and replacement shall require 1°C (Warning—After 20 min at ambient temperature, the
not more than 3 s. temperature of the test specimen will be approximately 50°C.
9.1.7.1 If the test specimen has not ceased to flow when its The vapor pressure at that temperature may still exceed 100
temperature has reached 30°C, transfer the test jar to the next kPa. Under these circumstances, inattentive opening of the
lower temperature bath per the following schedule: pressure vessel may induce foaming with resultant loss of
(1) If the test specimen is at +30°C, move to 0°C bath; sample and possible injury to personnel.)
(2) If the test specimen is at +9°C, move to −18°C bath; 9.2.5 Immediately close the test jar with the cork carrying
(3) If the test specimen is at −9°C, move to −33°C bath; the high cloud and pour thermometer, or, if the expected pour
and point is above 36°C, the melting point thermometer. Adjust the
(4) If the test specimen is at −24°C, move to −51°C bath. position of the cork and thermometer so the cork fits tightly, the
9.1.7.2 If the test specimen in the jar does not show thermometer and the jar are coaxial, and the thermometer bulb
movement when tilted, hold the jar in a horizontal position for is immersed to a depth which places the beginning of the
5 s, as shown by an accurate timing device (6.4), and observe capillary 3 mm below the surface of the test specimen.
the specimen carefully. If the test specimen shows any move- 9.2.6 Proceed as described in 9.1.5 – 9.1.8.

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 D5853 − 11
10. Calculation and Report 11.1.2 Reproducibility—The difference between two, single
10.1 Add 3°C to the temperature recorded in 9.1.8 and and independent results, obtained by different operators work-
report as Maximum Pour Point, ASTM D5853, Procedure A, or ing in different laboratories on identical test material would, in
Minimum Pour Point, ASTM D5853, Procedure B, if the the long run, in the normal and correct operation of the test
procedure in 9.2 has been followed. method, exceed the following value only in 1 case in 20.
Reproducibility
10.2 If the test was discontinued (9.1.8.1), report the pour Procedure °C (rounded)
point as ≤ − 36°C.
A (max) 18.0 (18) (Note 9)
B (min) 22.0 (21) (Note 9)
11. Precision and Bias
NOTE 9—These precision values are derived from a 1994 cooperative
11.1 The following criteria are to be used for judging the program3 and the current Committee D02 Statistical Method, RR:D02-
acceptability of results (95 % confidence): 1007.4
11.1.1 Repeatability—The difference between successive 11.2 Bias—The procedure in this test method has no bias
test results obtained by the same operator with the same because the value of pour point is defined only in terms of this
apparatus under constant operating conditions on identical test test method.
material would, in the long run, in the normal and correct
operation of the test method, exceed the following value only 12. Keywords
in 1 case in 20. 12.1 cold flow; crude oil; pour point

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Repeatability

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Procedure °C (rounded) 3
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1371.

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A (max) 3.1 (3) (Note 9) 4
Supporting data have been filed at ASTM International Headquarters and may
B (min) 5.8 (6) (Note 9) be obtained by requesting Research Report RR:D02-1007.

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APPENDIX
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(Nonmandatory Information)
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X1. GUIDELINE FOR SAMPLE HANDLING

X1.1 Introduction X1.1.4.2 They contain water or sediment, or both, which

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tends to separate in the sample container.

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X1.1.1 Sampling of crude oils from pipelines, tankers,

X1.1.4.3 If not maintained at a sufficiently high
barges, or trucks is usually beyond control of the laboratory
temperature, wax deposition at the walls of the container or
and adequately covered by the appropriate sampling protocols
wax precipitation can occur.
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as specified in Practices D4057 and D4177.

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X1.1.5 When making up composite samples, exercise care

X1.1.2 This guideline covers the sampling from containers not to lose light ends and to ensure homogeneity of the
submitted to the analytical laboratory for analysis. It covers the composing samples.
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handling of samples between the point at which they were

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extracted or drawn, and the laboratory test bench or sample X1.1.6 If crude oil samples are to be tested for vapor
storage. It is meant to ensure that the nature and integrity of the pressure, density, or any other test in which retention of light
samples are maintained as far as possible. ends is essential, subsamples for these test methods shall be
taken first before any other sample handling procedures are
X1.1.3 The method of handling a sample will depend on the invoked for performing sampling for other tests such as pour
purpose for which it was taken. The laboratory analytical point.
procedure to be used will often require a special handling
X1.1.7 Never subsample crude oils in plastic containers or
procedure to be associated with it. For this reason, consult the any other container that will not retain gases or light materials
appropriate methods of test so that any necessary instructions and cannot be heated without deformation.
as to sample handling can be given to the person drawing the
sample. If the analytical procedures to be applied have con- X1.2 Heating of Samples
flicting requirements, as is often the case for crude oils, then
draw separate samples and apply the appropriate procedure to X1.2.1 Crude oils stored at temperatures below their cloud
each sample. point will show wax deposition on the walls of the (sample)
containers. The wax coming out of the solution will be
X1.1.4 For crude oils, care in sampling is particularly preferentially the high melting wax. It is this type of wax that
necessary because: has the most pronounced influence on the crude oil pour point
X1.1.4.1 They contain volatile material, hence loss by and, at the same time, is the most difficult to redissolve or
evaporation can occur. disperse in the crude oil. Proper treatment of the samples

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 D5853 − 11
before subsampling for pour point, therefore, is crucial for of the container. For a 1 L tin, 2 h has been found to be
obtaining reliable crude oil pour point results. adequate. For larger tins, longer times will be required.
X1.2.2 In order to achieve complete solubility of the wax, Although it is strongly recommended that the containers be
heat crude oil samples to a temperature above the wax cloud closed when heated, it is advised that after approximately 30
point. This value is seldom known however. As a rule of min, the excess pressure is slowly released before continuing
thumb, a temperature of 20°C above the expected pour point the heating. (Warning—Exercise care when opening the
will usually satisfy the cloud point requirement, although container as significant vapor pressure will have built up
exceptions do occur. (X1.2.3). Opening the container may induce foaming with
resultant spillage of sample and possible injury to personnel.)
X1.2.3 The vast majority of crude oils show a significant
Mixing can be accomplished by a mechanical shaker or by
vapor pressure even at ambient temperatures. Dead crude is
vigorous manual shaking. Although the use of (high speed)
usually stabilized at a vapor pressure of 50 kPa (Test Method
mixers or similar devices might be effective, it will require that
D323, RVP at 37.8°C) or below. However, occasionally, high
the container be open for some time, during which the escape
RVP crudes (80 kPa) are produced and marketed. Before
of light ends can be excessive, and hence, this procedure is not
testing, never subject a crude oil sample to a temperature
recommended (Warning—During this operation significant
higher than 60°C or to a temperature above the bubble point
amounts of highly flammable vapors might escape. Vent in a
(vapor pressure ≥100 kPa). As a rule of thumb, the vapor
pressure doubles for every 20°C increase in temperature. safe area.)

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X1.3.4 Bottles—Follow as described in X1.3.3. Exercise
X1.3 Homogenization of Samples
special care when heating bottles that are closed with a cork or

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X1.3.1 The proper means and effectiveness of mixing in rubber stopper. The pressure buildup due to the heating will

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order to achieve homogeneity depend, in addition to the inevitably blow out the stopper. Take proper measures to
physical properties (for example, viscosity) of the crude oil, on safeguard against such an event (Warning—Before embarking
the capacity and shape of the container in which the crude oil on any heating or mixing procedure, or both, ensure that the

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arrives at the laboratory. It is virtually impossible to cater to IC drum and plugs can withstand the expected pressure buildup
every possibility and achieve optimum results under all cir- and can be handled safely without leakage.)(Warning—
cumstances. Guidelines are provided which in actual practice Exercise care when opening the container as significant vapor
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have proven to achieve the best possible results for the most pressure will have built up (X1.2.3). Opening the container
common situations. may induce foaming with resultant spillage of sample and
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X1.3.2 Drums, 15 to 200 L—The most effective way of possible injury to personnel.)
achieving homogenization is mixing the contents of the drum
X1.3.5 Plastic Containers—The use of plastic containers
on a roller bank in a hot room kept at a temperature between 40
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for crude oil samples is strongly discouraged for a number of

and 60°C for 48 h (X1.2.3). Alternatively, keep the drum at a
reasons (X1.1.7). If such a container is offered to the
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temperature of 20°C above the expected pour point for 48 h

laboratory, however, the only way to handle these containers is
(X1.2.3) and roll the drum for at least 15 min before taking a
by heating to a temperature 20°C above the expected pour
sample. If heating of the drum is not feasible, the only
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point (X1.2.1 – X1.2.3) in a water bath kept at the appropriate

alternative is extensive rolling for at least 30 min to disperse
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temperature. The water bath prevents localized high tempera-

the wax and wax particles as effectively as possible. In order to
avoid the cumbersome procedure of (re)mixing the contents of tures in the container, which can create weak sections increas-
ing the possibility of rupture. In any case, rupture of these
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large sample containers, it is recommended to draw an ad-

containers due to pressure buildup is a distinct possibility and
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equate number of subsamples in smaller containers, using

Practice D4057 as a guide (X1.1.3 – X1.1.7) (Warning— adequate measures must be taken to ensure safety (Warning—
Before embarking on any heating or mixing procedure, or both, Exercise care when opening the container as significant vapor
ensure that the drum and plugs can withstand the expected pressure will have built up (X1.2.3). Opening the container
pressure build-up and can be handled safely without may induce foaming with resultant spillage of sample and
leakage.)(Warning—Exercise care when opening the con- possible injury to personnel.)
tainer as significant vapor pressure will have built up (X1.2.3). X1.3.6 Sample Receivers (Practice D4177)—Follow the
Opening the container may induce foaming with resultant prescribed sample mixing and handling procedure as described
spillage of sample and possible injury to personnel.) in Practice D4177. It is recommended that a 1 L (tin)
X1.3.3 Tins, 1 to 15 L—Store the container at a temperature subsample be taken concurrently with subsampling for density
20°C above the expected pour point (X1.2.1) preferably in a and water and sediment, provided that the sample receiver has
water bath kept at the appropriate temperature. Alternatively, not been below the crude oil cloud point for more than 6 h. If
store the container in an explosion-proof oven, bearing in mind the container has been kept at a temperature below the cloud
that local surface temperatures might be much higher than the point for more then 6 h, reheat the container to a temperature
oven temperature reading indicates. The time required to 20°C above the expected pour point (X1.2.1 – X1.2.3) before
dissolve the wax will depend on the type of wax and the size mixing and subsampling.

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 D5853 − 11
SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D5853–09) that may impact the use of this standard.

(1) Revised Table 1. (2) Revised Section 7.

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Copyright by ASTM Int'l (all rights reserved); Wed Jun 8 01:06:17 EDT 2016
8
Downloaded/printed by
Uganda MOU - Online Access (Uganda MOU - Online Access) pursuant to License Agreement. No further reproductions authorized.