SIST EN ISO 13503-2:2007

SLOVENSKI STANDARD
SIST EN ISO 13503-2:2007
01-januar-2007
Industrija za predelavo nafte in zemeljskega plina - Tekočine in materiali za
zaključna dela - 2. del: Merjenje lastnosti podpornih materialov, ki se uporabljajo v
postopkih frakcioniranja in pri filtrskih zasipih s prodom (ISO 13503-2:2006)
Petroleum and natural gas industries - Completion fluids and materials - Part 2:
Measurement of properties of proppants used in hydraulic fracturing and gravel-packing
operations (ISO 13503-2:2006)
Erdöl- und Erdgasindustrie - Komplettierungsflüssigkeiten und -materialien - Teil 2:
Messung der Eigenschaften von Stützmaterialien zum Einsatz bei hydraulischen
Fraktionierungs- und in Kiespackungsvorgängen (ISO 13503-2:2006)
Industries du pétrole et du gaz naturel - Fluides de complétion et matériaux - Partie 2:
Mesurage des propriétés des matériaux de soutenement utilisés dans les opérations de
fracturation hydraulique et de remplissage de gravier (ISO 13503-2:2006)
Ta slovenski standard je istoveten z: EN ISO 13503-2:2006
ICS:
75.100 Maziva Lubricants, industrial oils and
related products
75.180.30 Oprema za merjenje Volumetric equipment and
prostornine in merjenje measurements
SIST EN ISO 13503-2:2007 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13503-2:2007

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SIST EN ISO 13503-2:2007
EUROPEAN STANDARD
EN ISO 13503-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2006
ICS 75.100

English Version
Petroleum and natural gas industries - Completion fluids and
materials - Part 2: Measurement of properties of proppants used
in hydraulic fracturing and gravel-packing operations (ISO
13503-2:2006)
Industries du pétrole et du gaz naturel - Fluides de Erdöl- und Erdgasindustrie - Komplettierungsflüssigkeiten
complétion et matériaux - Partie 2: Mesurage des und -materialien - Teil 2: Messung der Eigenschaften von
propriétés des matériaux de soutènement utilisés dans les Stützmaterialien zum Einsatz bei hydraulischen
opérations de fracturation hydraulique et de remplissage de Fraktionierungs- und in Kiespackungsvorgängen (ISO
gravier (ISO 13503-2:2006) 13503-2:2006)
This European Standard was approved by CEN on 22 September 2006.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13503-2:2006: E
worldwide for CEN national Members.

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SIST EN ISO 13503-2:2007

EN ISO 13503-2:2006 (E)





Foreword


This document (EN ISO 13503-2:2006) has been prepared by Technical Committee ISO/TC 67
"Materials, equipment and offshore structures for petroleum and natural gas industries" in
collaboration with Technical Committee CEN/TC 12 "Materials, equipment and offshore
structures for petroleum, petrochemical and natural gas industries", the secretariat of which is
held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by May 2007, and conflicting national standards
shall be withdrawn at the latest by May 2007.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.


Endorsement notice

The text of ISO 13503-2:2006 has been approved by CEN as EN ISO 13503-2:2006 without any
modifications.

2

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SIST EN ISO 13503-2:2007


INTERNATIONAL ISO
STANDARD 13503-2
First edition
2006-11-01
Petroleum and natural gas industries —
Completion fluids and materials —
Part 2:
Measurement of properties of proppants
used in hydraulic fracturing and
gravel-packing operations
Industries du pétrole et du gaz naturel — Fluides de complétion et
matériaux —
Partie 2: Mesurage des propriétés des matériaux de soutènement
utilisés dans les opérations de fracturation hydraulique et de
remplissage de gravier




Reference number
ISO 13503-2:2006(E)
©
ISO 2006

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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
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ii © ISO 2006 – All rights reserved

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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
Contents Page
Foreword. v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Abbreviations . 1
4 Standard proppant sampling procedure .2
4.1 General. 2
4.2 Particle segregation. 2
4.3 Equipment . 2
4.4 Number of required samples — Bulk. 4
4.5 Sampling —Bulk material . 5
4.6 Sampling — Bagged material . 5
5 Sample handling and storage. 5
5.1 Sample reduction. 5
5.2 Sample splitting . 5
5.3 Sample and record retention and storage .5
6 Sieve analysis . 6
6.1 Purpose. 6
6.2 Description . 6
6.3 Equipment and materials . 6
6.4 Procedure . 6
6.5 Calculation of the mean diameter, median diameter and standard deviation. 7
6.6 Sieve calibration . 9
7 Proppant sphericity and roundness . 11
7.1 Purpose. 11
7.2 Description . 12
7.3 Apparatus capability. 12
7.4 Procedure . 12
7.5 Alternate method for determining average sphericity and roundness . 13
8 Acid solubility . 13
8.1 Purpose. 13
8.2 Description . 13
8.3 Equipment and materials . 14
8.4 Procedure . 14
9 Turbidity test . 15
9.1 Purpose. 15
9.2 Description . 16
9.3 Equipment and materials . 16
9.4 Equipment calibration . 16
9.5 Procedure . 16
10 Procedures for determining proppant bulk density, apparent density and absolute density. 17
10.1 Purpose. 17
10.2 Description . 17
10.3 Bulk density. 17
10.4 Apparent density. 19
10.5 Absolute density. 21
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
11 Proppant crush-resistance test . 21
11.1 Purpose . 21
11.2 Description. 21
11.3 Equipment and materials . 22
11.4 Sample preparation. 22
11.5 Crush-resistance procedure . 23
12 Loss on ignition of resin-coated proppant.25
12.1 Objective . 25
12.2 Apparatus and materials . 25
12.3 Loss-on-ignition procedure for whole-grain proppant . 25
Annex A (informative) Formazin solution preparation. 27
Bibliography . 28

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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(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. 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, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. 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.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 13503-2 was prepared by Technical Committee ISO/TC 67, Materials, equipment and offshore structures
for petroleum, petrochemical and natural gas industries, Subcommittee SC 3, Drilling and completion fluids,
and well cements.
ISO 13503 consists of the following parts, under the general title Petroleum and natural gas industries —
Completion fluids and materials:
⎯ Part 1: Measurement of viscous properties of completion fluids
⎯ Part 2: Measurement of properties of proppants used in hydraulic fracturing and gravel-packing
operations
⎯ Part 3: Testing of heavy brines
⎯ Part 4: Procedure for measuring stimulation and gravel-pack fluid leakoff under static conditions
⎯ Part 5: Procedures for measuring the long-term conductivity of proppants
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
Introduction
[1] [2] [3]
This part of ISO 13503 is a compilation and modification of API RP 56 , API RP 58 and API RP 60 .
The procedures have been developed to improve the quality of proppants delivered to the well site. They are
for use in evaluating certain physical properties used in hydraulic fracturing and gravel-packing operations.
These tests should enable users to compare the physical characteristics of various proppants tested under the
described conditions and to select materials useful for hydraulic fracturing and gravel-packing operations.
The procedures presented in this part of ISO 13503 are not intended to inhibit the development of new
technology, material improvements or improved operational procedures. Qualified engineering analysis and
judgment are required for their application to a specific situation.
In this part of ISO 13503, where practical, US Customary (USC) units are included in brackets for information.
Annex A of this part of ISO 13503 is for information only.

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SIST EN ISO 13503-2:2007
INTERNATIONAL STANDARD ISO 13503-2:2006(E)

Petroleum and natural gas industries — Completion fluids and
materials —
Part 2:
Measurement of properties of proppants used in hydraulic
fracturing and gravel-packing operations
1 Scope
This part of ISO 13503 provides standard testing procedures for evaluating proppants used in hydraulic
fracturing and gravel-packing operations.
NOTE “Proppants” mentioned henceforth in this part of ISO 13503 refer to sand, ceramic media, resin-coated
proppants, gravel-packing media and other materials used for hydraulic fracturing and gravel-packing operations.
The objective of this part of ISO 13503 is to provide a consistent methodology for testing performed on
hydraulic fracturing and/or gravel-packing proppants.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ASTM E11, Standard Specification for Wire Cloth and Sieves for Testing Purposes
3 Abbreviations
API American Petroleum Institute
ASTM American Society for Testing and Materials
ASG apparent specific gravity
FTU formazin turbidity unit
HCI hydrochloric acid
HF hydrofluoric acid
LOI loss on ignition
NTU nephelometric turbidity unit
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
4 Standard proppant sampling procedure
4.1 General
Before any sample is taken, consider what tests will be performed, as each test requires a different volume. It
is very important that both the supplier and customer obtain the best representative sample possible. Unless
the sample is truly representative of a total shipment or container, testing and correlation with
specifications/standards is very difficult. It is unlikely that sampling/testing methods in the field duplicate the
producer’s system. The standard procedures included within this part of ISO 13503 are to assist in obtaining
representative samples. However, there are inherent variations associated with sampling, testing equipment
and the procedures that can lead to inconsistent results. A sample that is representative of a truckload
[23 000 kg (50 700 lb)] or a railcar load [90 000 kg (198 000 lb)] can be an initial source of wide variation when
making comparisons. All parties shall take care to insure uniform sampling. The customer and the supplier
shall agree on sampling and testing methods/techniques.
For the best representation, continuous sampling is ideal. Although many proppant suppliers utilize automatic
sampling, it is usually impractical at the job site. If sampling is conducted while unloading a container or at the
site, consideration should be given to the number or frequency of samples.
If bulk containers are filled from a flowing stream of proppant material, sampling procedures in accordance
with 4.5 shall be applied. If bulk containers are filled using sacked proppant material, sampling procedures in
accordance with 4.6 shall be applied.
4.2 Particle segregation
It is important to have a basic understanding of segregation when sampling proppant. Depending on the size,
shape, distribution and mechanisms involved, there is usually a certain amount of error or variability involved
in sampling due to segregation. The sampling procedures described here are the result of much experience
and are designed to minimize the effects of segregation of particles by size.
Particles, such as proppants, naturally find the path of least resistance when moved or when force is applied.
During transfer or movement, particles of differing size and mass naturally separate or segregate. The degree
of segregation depends on the mechanisms involved in the transfer or movement.
There are several forces, such as gravity, acting on a stream of particles as it flows. Within a moving stream,
fine particles drop through the voids or gaps and coarser particles move to the outside. The fine particles
migrate and usually rest close to the area where they land. The heavier, coarser particles bounce or roll much
further, stratifying the material by size.
4.3 Equipment
The following equipment shall be used to compile representative proppant material samples.
4.3.1 Box sampling device, with a 13 mm (0,50 in) slot opening.
The length of the 13 mm (0,50 in) slot shall be longer than the thickness of the stream being sampled. The
volume of the sampler shall be large enough so as to not overflow while cutting through the entire stream. A
box sampling device meeting these criteria is shown in Figure 1.
4.3.2 Sample reducer, of appropriate size for handling sack-size samples and reducing the material to 1/16
of the original mass; see Figure 2.
4.3.3 Sample splitter, of appropriate size; see Figure 3.
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
Dimensions in centimetres (inches)

Key
1 sampler body, 15,9 × 20,9 × 6,35 (6,25 × 8,25 × 2,5) 3 pipe coupling
2 handle 4 sample opening, 1,27 (0,50)
Figure 1 — Box sampling device
Dimensions in centimetres (inches)

Key
1 main body, 36,8 × 48,3 × 11,4 (14,5 × 19,0 × 4,5) 5 hopper, 36,8 × 24,1 × 15,2 (14,5 × 9,5 × 6,0)
2 splitter plate, 5,1 × 5,1 × 5,1 (2 × 2 × 2) 6 gate, 36,8 × 19,1 × 0,32 (14,5 × 7,5 × 0,125)
3 discharge plate, 36,8 × 30,5 × 0,32 (14,5 × 12 × 0,125) 7 hand knob, 3,8 (1,5) diameter
4 discharge chute, 5,7 × 5,7 × 7,6 (2,25 × 2,25 × 3,0) 8 support stand assembly,
71,1 × 38,1 × 68,6 (28 × 15 × 27)
Figure 2 — Sample reducer
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
Dimensions in centimetres (inches)

Key
1 main body, 29,2 × 27,9 × 16,5 (11,5 × 11,0 × 6,5)
2 handle
3 gate plate
4 hopper
5 pan
6 splitter vanes, 1,25 (0,5)
Figure 3 — Sample splitter
4.4 Number of required samples — Bulk
4.4.1 Proppants for hydraulic fracturing
A minimum of one sample per 9 000 kg (20 000 lb) or fraction thereof, shall be obtained. A maximum of
10 samples per bulk container shall be obtained, combined and tested.
4.4.2 Gravel-packing media
A minimum of one sample per 4 500 kg (10 000 lb) but no fewer than two samples per job shall be obtained,
combined and tested.
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
4.5 Sampling —Bulk material
All samples shall be obtained from a flowing stream of proppant by a manual or automatic sampler. Samples
shall not be taken from a static pile. The sampling device shall be used with its length perpendicular to the
flowing proppant stream. The sampler shall be passed at a uniform rate from side to side through the full
stream width of moving proppant. This shall be done as the material is moving to or from a conveyor belt into
a blender, truck, railcar or bulk container. Two metric tons of proppant material shall be allowed to flow prior to
taking the first sample. The number of samples taken shall comply with 4.4. During sampling, the sampling
receptacle shall be passed completely across the moving proppant stream in a brief interval of time so as to
take the entire stream with each pass. Under no circumstances shall the sampling receptacle be allowed to
overflow.
4.6 Sampling — Bagged material
4.6.1 Bags up to 50 kg (110 lb)
Only whole bags shall be used for sampling bagged proppant materials.
4.6.2 Totes/bulk bags/super sacks weighing up to 2 000 kg (4 400 lb)
Unless the product can be sampled in a free-flowing state, the sampling of large bags presents the same
problems as for a static pile. Follow the same sample frequency as described in 4.4, using the sampling
method described in 4.5, except for allowing approximately 50 kg (110 lb) to be discharged from the bulk bag
before sampling.
5 Sample handling and storage
5.1 Sample reduction
Place the contents of the combined bulk sample of proppant, or an entire sack up to 50 kg (110 lb), in the 16:1
sample reducer (see Figure 2) or equivalent. Obtain a reduced sample of approximately 1/16 of the original
mass of the total sack’s contents, typically 3 kg (6,6 lb).
5.2 Sample splitting
An appropriately-sized sample reducer and sample splitter shall be used to permit samples to be prepared for
testing. Place the reduced sample, obtained according to 5.1, or the sample obtained during bulk material
loading operations (refer to 4.5), in the sample splitter (refer to Figure 3) and split the sample to a
testing-aliquot size of approximately 1 kg (2,2 lb). Sufficient proppant material shall be split to permit
performance of recommended tests as specified in this part of ISO 13503.
5.3 Sample and record retention and storage
The proppant supplier shall maintain records of all tests conducted on each shipment for a minimum of one
year. Physical samples of an amount sufficient to conduct all tests recommended herein, but in no cases less
than 0,25 kg (0,5 lb), shall be retained in storage for a minimum of six months. Any material subsequently
taken for testing shall be split from the retained sample. Samples shall be sealed in a type of container that is
sufficient to protect the sample from contamination and moisture. Samples shall be stored in a cool dry place.
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SIST EN ISO 13503-2:2007
ISO 13503-2:2006(E)
6 Sieve analysis
6.1 Purpose
The purpose of the procedure in Clause 6 is to ensure a consistent methodology for sieve analysis and to
provide a consistent procedure for sieve evaluation.
6.2 Description
The procedure and equipment described in 6.3 to 6.6 are the most widely utilized in the gas and oil industry.
Alternate methods may be used but shall be correlated with these standard methods.
6.3 Equipment and materials
6.3.1 Sieve sets, two, complying with the requirements of the ASTM Series, 200 mm (8 in) diameter or
equivalent.
One set is a working set of sieves, and the other a master set to be used for standardizati
...