EN ISO 13500:1998

SLOVENSKI STANDARD
01-december-2000
Petroleum and natural gas industries - Drilling fluid materials - Specifications and
tests (ISO 13500:1998)
Petroleum and natural gas industries - Drilling fluid materials - Specifications and tests
(ISO 13500:1998)
Erdöl- und Erdgasindustrien - Bohrspülungen - Spezifikationen und Prüfungen (ISO
13500:1998)
Industries du pétrole et du gaz naturel - Fluides de forage - Spécifications et essais (ISO
13500:1998)
Ta slovenski standard je istoveten z: EN ISO 13500:1998
ICS:
75.180.10 Oprema za raziskovanje in Exploratory and extraction
odkopavanje equipment
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 13500
First edition
1998-07-01
Petroleum and natural gas industries —
Drilling fluid materials — Specifications and
tests
Industries du pétrole et du gaz naturel — Fluides de forage —
Spécifications et essais
A
Reference number
ISO 13500:1998(E)
ISO 13500:1998(E)
Contents
Page
Scope.
1  1
2  Normative references. 1
3  Definitions and abbreviations. 2
4  Requirements. 2
5  Calibration. 3
6  Packaged materials . 13
7  Barite. 15
8  Haematite. 24
9  Bentonite. 34
10  Nontreated bentonite . 36
11  OCMA grade bentonite . 39
12  Attapulgite . 42
13  Sepiolite . 45
14  Technical grade low-viscosity CMC (CMC-LVT) . 48
15  Technical grade high-viscosity CMC (CMC-HVT) . 51
16  Starch. 54
Annex A (informative) Mineral impurities in barite . 58
Annex B (informative) Test precision. 59
Annex C (informative) Examples of calculations. 64
©  ISO 1998
All rights reserved. Unless otherwise specified, 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 • CH-1211 Genève 20 • Switzerland
Internet iso@iso.ch
Printed in Switzerland
ii
©
ISO ISO 13500:1998(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 collab-
orates 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 International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 13500 was prepared by Technical Committee
ISO/TC 67, Materials, equipment and offshore structures for petroleum and
natural gas industries, Subcommittee SC 3, Drilling and completion fluids,
and well cement.
Annexes A, B and C of this International Standard are for information only.
iii
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ISO 13500:1998(E) ISO
Introduction
This International Standard covers materials which are in common usage in
petroleum and natural gas drilling fluids. These materials are used in bulk
quantities, can be purchased from multiple sources, and are available as
commodity products. No single-source or limited-source products are
included, nor are speciality products.
International Standards are published to facilitate communication between
purchasers and manufacturers, to provide interchangeability between
similar equipment and materials purchased from different manufacturers
and/or at different times, and to provide an adequate level of safety when
the equipment or materials are utilised in the manner and for the purposes
intended. This International Standard provides minimum requirements and
is not intended to inhibit anyone from purchasing or producing materials to
other standards.
This International Standard is substantially based on API Spec 13A,
th
15 Edition, May 1, 1993. The purpose of this International Standard is to
provide product specifications for barite, haematite, bentonite, nontreated
bentonite, Oil Companies Materials Association (OCMA) grade bentonite,
attapulgite, sepiolite, technical-grade low viscosity carboxymethylcellulose
(CMC-LVT), technical-grade high viscosity carboxymethylcellulose (CMC-
HVT), and starch.
The intent of the document was to incorporate all International Standards
for drilling fluid materials into an ISO formatted document. A survey of the
industry found that only the American Petroleum Institute (API) issued
testing procedures and specification standards for these materials.
Reference to OCMA materials has been included in API work, as the
OCMA and subsequent holding committees were declared defunct, and all
specifications were submitted to API in 1983.
iv
©
INTERNATIONAL STANDARD  ISO ISO 13500:1998(E)
Petroleum and natural gas industries — Drilling fluid
materials — Specifications and tests
1  Scope
This International Standard covers physical properties and test procedures for materials manufactured for use in oil-
and gas-well drilling fluids. The materials covered are barite, haematite, bentonite, nontreated bentonite, OCMA
grade bentonite, attapulgite, sepiolite, technical grade low-viscosity carboxymethylcellulose (CMC-LVT), technical
grade high-viscosity carboxymethylcellulose (CMC-HVT), and starch. This International Standard is intended for the
use of manufacturers of named products.
2  Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 6780:1988, General-purpose flat pallets for through transit of goods — Principal dimensions and tolerances
API RP 13B-1, Recommended Practice Standard Procedure for Field Testing Water-Based Drilling Fluids (second
1)
edition, 1997)
API RP 13K, Recommended Practice for Chemical Analysis of Barite (second edition, 1996)
APME 1993 (Association of Plastic Manufacturers in Europe)
ASTM D422, Standard Test Method for Particle-Size Analysis of Soils (1963)
ASTM E11, Standard Specification for Wire-Cloth Sieves for Testing Purposes (1995)
ASTM E77, Standard Test Method for Inspection and Verification of Liquid-in-Glass Thermometers (1992)
ASTM E691, Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test
Method. (1992)
ASTM E177, Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods (1990)
NIST (NBS) Monograph 150
1)
ISO 10414-1 under preparation.
©
ISO
ISO 13500:1998(E)
3  Definitions and abbreviations
3.1  Definitions
For the purposes of this International Standard, the following definitions apply.
3.1.1
ACS reagent grade
chemicals which meet purity standards as specified by the American Chemical Society (ACS)
3.1.2
flash side
side containing residue ("flash") from stamping; also, the side with concave indentations
3.2  Abbreviations
ACS American Chemical Society
API American Petroleum Institute
ASTM American Society for Testing and Materials
EDTA Ethylenediaminetetraacetic acid
CAS Chemical Abstracts Service
CMC-HVT Carboxymethylcellulose — High viscosity technical grade
CMC-LVT Carboxymethylcellulose — Low viscosity technical grade
OCMA Oil Companies Materials Association
NBS National Bureau of Standards
NIST National Institute of Standards and Technology
TC To contain
TD To deliver
4  Requirements
4.1  Quality control instructions
All quality control work shall be controlled by manufacturer's documented instructions, which include appropriate
methodology and quantitative or qualitative acceptance criteria.
4.2  Use of test calibration materials in checking testing procedures
4.2.1  Test Calibration Barite Lot 001 and Lot 002, and Test Calibration Bentonite can be obtained by contacting the
2)
API . The calibration test materials are shipped in a 7,6 litre (2 gallon) plastic container.
NOTE  Test Calibration Barite 001 will be routinely supplied until quantities are exhausted, at which time Test Calibration
Barite 002 will take its place.

2)
American Petroleum Institute, 1220 L Street NW, Washington, D.C. 20005-4070, USA.
©
ISO
ISO 13500:1998(E)
4.2.2  The API office will forward the request to the designated custodian for further handling. The test calibration
products will be furnished with a certificate of calibration giving the established values for each property and the
confidence limits within which a laboratory's results shall fall.
4.2.3  The custodian shall furnish a certificate of analysis for each sample.
4.2.4  For calibration requirements of API Test Calibration Materials, refer to 5.2.11 and 5.3.10.
4.2.5  API Standard Evaluation Base Clay (formerly OCMA Base Clay - Not OCMA Grade Bentonite): Stocks of API
Standard Evaluation Base Clay have been set aside and can be ordered through the API.
4.3  Records retention
All records specified in this International Standard shall be maintained for a minimum of five years from the date of
preparation.
5  Calibration
5.1  Coverage
5.1.1  This clause covers calibration procedures and calibration intervals for laboratory equipment and reagents
specified. For laboratory items not listed, the manufacturer shall develop procedures where deemed appropriate.
5.1.2  The manufacturer shall control, calibrate, verify, and maintain the laboratory equipment and reagents used in
this standard for measuring product conformance to standard requirements.
5.1.3  The manufacturer shall maintain and use laboratory equipment and reagents in a manner such that
measurement uncertainty is known and meets required measurement capability.
5.1.4  The manufacturer shall document and maintain calibration procedures, including details of laboratory
equipment and reagent type, identification number, frequency of checks, acceptance criteria, and corrective action
to be taken when results are unsatisfactory.
5.1.5  The manufacturer shall establish and document responsibility for administration of the calibration program,
and responsibility for corrective action.
5.1.6  The manufacturer shall document and maintain calibration records for laboratory equipment and reagents;
shall periodically review these records for trends, sudden shifts or other signals of approaching malfunction; and
shall identify each item with a suitable indicator or approved identification record to show calibration status.
5.2  Apparatus and reagents
5.2.1  Volumetric glassware
Laboratory volumetric glassware used for final acceptance, including Le Chatelier flasks, pipettes, and burettes, are
usually calibrated by the supplier. Manufacturers of products to this International Standard shall document evidence
of glassware calibration prior to use. Supplier certification is acceptable. Calibration may be checked gravimetrically.
Periodic recalibration is not required.
5.2.2  Laboratory thermometers
The manufacturer shall calibrate all laboratory thermometers used in measuring product conformance to standards
against a secondary reference thermometer. The secondary reference thermometer shall show evidence of
calibration as performed against NIST certified master instruments in accordance with the procedures outlined by
ASTM E77-92 and NBS (NIST) Monograph 150.
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ISO
ISO 13500:1998(E)
5.2.3  Laboratory balances
The manufacturer shall calibrate laboratory balances periodically in the range of use with NIST Class P, Grade 3, or
better weights; and shall service and adjust balances whenever calibration indicates a problem.
5.2.4  Sieves conforming to ASTM E11
Approximate dimensions are 76 mm diameter and 69 mm from top of frame to wire cloth. Barite (clause 7) and
haematite (clause 8) manufacturers shall calibrate 75 μm sieves using API Test Calibration Barite with established
values for residue retained. Haematite (clause 8) manufacturers shall calibrate 45 μm sieves using a suitable
quantity of uniform haematite. Bentonite (clause 9), OCMA grade bentonite (clause 11), attapulgite (clause 12) and
sepiolite (clause 13) manufacturers shall calibrate 75 μm sieves using API Test Calibration Bentonite. No sieve
calibration is available for CMC-Low Viscosity Technical Grade, CMC-High Viscosity Technical Grade and starch,
as no reference material and sieve calibration has been established.
5.2.5  Hydrometer
The manufacturer shall calibrate each hydrometer with the dispersant solution used in the sedimentation procedure.
5.2.6  Motor-driven direct-indicating viscometer
The manufacturer shall calibrate each meter with 20 mPa·s and 50 mPa·s, certified standard silicone fluids.
5.2.7  Laboratory pressure-measuring device
The manufacturer shall document evidence of laboratory pressure-measuring device calibration prior to use.
5.2.8  Mixer
3)
(e.g. Multimixer® Model 9B with 9B29X impeller blades or equivalent, mounted flash side up): The manufacturer
shall verify that all spindles rotate at 11 500 r/min ± 300 r/min under no load with one spindle operating. Each
spindle will be fitted with a single sine-wave impeller approximately 25 mm in diameter mounted flash side up. New
impellers shall be weighed prior to installation, with mass and date recorded.
5.2.9  Chemicals and solutions
Shall meet ACS or international equivalent reagent grade if available.
5.2.10  Deionized (or distilled) water
Manufacturer shall develop, document, and implement a method to determine hardness of water. The water shall
not be used if hardness is indicated.
5.2.11  API Test Calibration Materials
Manufacturer shall perform in-house verification of API Test Calibration Barite and/or (where applicable) API Test
Calibration Bentonite for properties listed with their Certificates of Analysis.
5.3  Calibration intervals
5.3.1  General
Any instrument subjected to movement which can affect its calibration shall be recalibrated prior to use.

3)
Multimixer® Model 9B is an example of a suitable product available commercially. This information is given for the
convenience of users of this International Standard and does not constitute an endorsement by ISO of this product.
©
ISO
ISO 13500:1998(E)
5.3.2  Thermometers
Calibrate each thermometer before being put into service. After calibration, mark each thermometer with an
identifying number that ties it to its corresponding correction chart. Check calibration annually against the secondary
reference thermometer.
5.3.3  Laboratory balances
Calibrate each balance prior to being put into service. Check calibration at least once per month for six months, then
at least once per six months if required measurements capability is being maintained. If not, service and recalibrate,
then check at least once per month until required measurement capability is maintained for six months, then once
per six months.
5.3.4  Sieves
Calibrate each sieve (where required: see 5.2.4) prior to being put into service. Check calibration at least once per
40 tests. After calibration, mark each sieve with an identifying number that ties it to its correction record. Since sieve
calibration will change with use, maintain an up-to-date correction record.
5.3.5  Hydrometer
Calibrate each hydrometer prior to its being put into service. After calibration, note and record each hydrometer
identifying number that ties it to its correction chart. Periodic recalibration is not required.
5.3.6  Motor-driven direct-indicating viscometers
Calibrate each viscometer prior to its being put into service. Check calibration at least once per week for three
months, then at least once per month if required measurement capability is being maintained.
5.3.7  Mixer
(e.g. Multimixer® Model 9B with 9B29X impellers or equivalent): Check and record mixer spindle speed at least
once every 90 days to ensure operation within the prescribed r/min range, using a phototachometer or similar
device. Remove, clean, dry, and weigh each impeller blade in service at least once every 90 days. Record masses,
and replace blades when mass drops below 90 % of its original value.
5.3.8  Deionized (or distilled) water
Manufacturer shall determine hardness of water whenever a new batch of water is prepared or purchased, or
whenever deionizing cartridges are replaced.
5.3.9  Laboratory pressure-measuring devices
Manufacturer shall document evidence of laboratory pressure-measuring device calibration prior to placing into
service and annually thereafter.
5.3.10  API Test Calibration Materials
Manufacturer shall test the applicable API Test Calibration Material(s) at least once per three months.
5.4  Calibration procedure — Thermometers
5.4.1  Place thermometer to be calibrated side by side with secondary reference thermometer into a constant-
temperature water bath (or suitable container of 4 litres or more, filled with water, on a counter in a constant-
temperature room) and allow to equilibrate for at least 1 h.
5.4.2  Read both thermometers and record readings.
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ISO
ISO 13500:1998(E)
5.4.3  Repeat readings throughout at least a 1-h interval to obtain a minimum of four readings.
5.4.4  Calculate the average and the range of readings for each thermometer. The difference between the range of
readings for each thermometer shall not exceed 0,1 °C, or the smallest scale division on the thermometer being
calibrated.
5.4.5  Calculate average deviation of thermometer reading from secondary reference thermometer reading.
Calculate and document correction for each thermometer.
5.5  Calibration procedure — Sieve 75 μm (5.2.4) for barite, haematite, bentonite, attapulgite and
sepiolite
NOTE  Bentonite is tested by this calibration procedure with the following changes noted:
a) Take at least three samples of approximately 10 g Test Calibration Bentonite per 9.8.
b) Test each sample per 9.8 using the certified sieve described in 5.5.1.
c) Continue procedure outlined in 5.5.4 through 5.5.10.
5.5.1  Obtain a 75-μm sieve with a certified centreline value.
5.5.2  Take at least three samples of approximately 50 g dry API Test Calibration Barite (TCB).
5.5.3  Test each of the samples per 7.9 using the certified sieve described in 5.5.1.
5.5.4  Calculate % residue, R, for each sample by:
(mass of residue, g)
% Residue,R = 100 (1)
(mass of sample, g)
5.5.5  Calculate average % residue, S, of test calibration material on certified sieve by:
RR++R +K12 3
S = (2)
N
where
R + R + R is the sum of each individual test result
1 2 3
N is the number of samples tested
Individual sample values shall agree within ± 0,2 of their average. If not, review test procedure technique and
equipment operation for sources of error. Make corrections where needed and repeat.
5.5.6  From the intersection of % residue and certified sieve opening size on the Sieve Calibration Graph, Figure 1,
determine the calibration line (A, B, C, etc.) for use with the specific container of test calibration material. Record
this and identify the container with this value.
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ISO
ISO 13500:1998(E)
Figure 1 — Sieve calibration graph, 75 μm sieve
5.5.7  Repeat 5.5.2 through 5.5.4 except substitute the working sieve to be calibrated from the certified sieve.
5.5.8  Calculate average % residue, R , of test calibration material on working sieve by:
a
RR+++RK12 3
R
= (3)
a
N
Individual sample values shall agree within ± 0,2 of their average. If not, review test procedure technique and
equipment operation for sources of error. Make corrections where needed and repeat, beginning at 5.5.7.
5.5.9  From Sieve Calibration Graph, Figure 1, determine the working sieve opening size to the nearest whole
value from intersection of % residue and the calibration line from 5.5.6 above. Record the working sieve opening
size and identify the calibrated sieve and test calibration material container.
5.5.10  Determine correction value (C) for working sieve from Table 1. Record this value and identify it with the
calibrated sieve and specified test calibration material container.
NOTE  The sieve correction value obtained from Table 1 as specified is a number to be added to the residue value obtained
on a test sample. (Negative values are subtracted.)
5.5.10.1  Example of barite sieve correction value determination:
Certified sieve size = 73 μm
Test calibration barite average % residue on certified sieve, S = 2,0 %
Calibration line = F
Test calibration barite average % residue on working sieve, R = 1,3 %
a
Working sieve size average opening (determined from sieve calibration graph, Figure 1) = 78 μm
Correction value (from Table 1), C = + 0,4 %
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ISO
ISO 13500:1998(E)
5.5.10.2  Example of sieve correction application:
Sieve correction value, C = + 0,4 %
Test sample % residue, R = 2,8 %
s
Corrected test sample % residue, R = 2,8 % + 0,4 % = 3,2 %
c
These correction values are valid from 0 % to 4 % residue retained on sieve.
NOTE  Correction values are rounded to the nearest 0,1.
4)
Table 1 — Correction values (C) for 75 μm sieves
b
Working sieve size Correction size :
a
Average opening ,
μm
Barite/Haematite Bentonite
70 20,7 20,3
71 20,6 20,2
72 20,4 0
73 20,3 0
74 20,1 0
75 0 0
76 + 0,1 0
77 + 0,3 0
78 + 0,4 0
79 + 0,6 + 0,2
80 + 0,7 + 0,3
a
Determined from sieve calibration graph, Figure 1.
b
Value to be added to test result of sample tested on sieve to convert
results to equivalent 75 μm (NOTE Negative values are subtracted).
5.6  Calibration procedure — Sieve 45 μm (5.2.4) for haematite
5.6.1  Obtain a 45-μm sieve with a certified centreline value.
5.6.2  Obtain a suitable quantity of uniform haematite sufficient to last six months or longer. Mix thoroughly and
store in a closed container. Identify this as "uniform haematite for 45-μm sieve calibration." Take at least three
samples of approximately 50 g dry haematite.
5.6.3  Test each of the samples per 8.9 using the certified sieve described in 5.6.1.
5.6.4  Calculate % residue, R, for each sample by:
mass of residue, g
()
% Residue, R = 100 (1)
()mass of sample, g
4)
ASTM sieve specifications allow ± 5 μm variation.
©
ISO
ISO 13500:1998(E)
5.6.5  Calculate average % residue, S, of test calibration material on certified sieve by:
RR++R+K12 3
S= (2)
N
where
R + R + R is the sum of each individual test result
1 2 3
N is the number of samples tested
Individual sample values shall agree within ± 0,5 of their average. If not, review test procedure technique and
equipment operation for sources of error. Make corrections where needed and repeat.
5.6.6  From the intersection of % residue and certified sieve opening size on the Sieve Calibration Graph, Figure 2,
determine the calibration line (A, B, C, etc.) for use with the specific container of test calibration material. Record
this and identify the container with this value.
Figure 2 — Sieve calibration graph, 45 μm sieve
5.6.7  Repeat 5.6.2 through 5.6.4 except substitute the working sieve to be calibrated from the certified sieve.
5.6.8  Calculate average % residue, R , of test calibration material on working sieve by:
a
RR+++RK12 3
R = (3)
a
N
Individual sample values shall agree within ± 0,5 of their average. If not, review test procedure technique and
equipment operation for sources of error. Make corrections where needed and repeat, beginning at 5.6.7.
5.6.9  From Sieve Calibration Graph, Figure 2, determine the working sieve opening size to the nearest whole
value from intersection of % residue and the calibration line from 5.6.6 above. Record the working sieve opening
size and identify the calibrated sieve and test calibration material container.
5.6.10  Determine correction value (C) for working sieve from Table 2. Record this value and identify it with the
calibrated sieve and specified test calibration material container.
NOTE  The sieve correction value obtained from Table 2 as specified is a number to be added to the residue value obtained
on a test sample. (Negative values are subtracted).
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ISO
ISO 13500:1998(E)
5.6.10.1  Example of haematite sieve correction value determination:
Certified sieve size = 46,5 μm
Haematite average % residue on certified sieve, S = 7,0 %
Calibration line = C
Haematite average % residue on working sieve, R = 9,7 %
a
Working sieve size average opening (determined from sieve calibration graph, Figure 2) = 42,5 μm
Correction value (from Table 2), C = 21,7 %
5.6.10.2  Example of sieve correction application:
Sieve correction value, C = 21,7 %
Test sample residue, R = 8,8 %
Corrected test sample residue, R = 8,8 % + (21,7 %) = 7,1 %
c
)
Table 2 — Correction value (C) for 45 μm sieves
b
Working sieve size Correction size
a
Average opening Haematite
m
μ
42,0 22,0
42,5 21,7
43,0 21,3
43,5 1,0
44,0 20,7
44,5 20,3
45,0 0,0
45,5 + 0,3
46,0 + 0,7
46,5 + 1,0
47,0 + 1,3
47,5 + 1,7
48,0 + 2,0
NOTE  Correction values are rounded to the nearest 0,1.
a
Determined from sieve calibration graph, Figure 2.
b
Value to be added to test result of sample tested on sieve to convert
results to equivalent 45 μm. (NOTE Negative values are subtracted).

5)
ASTM sieve specifications allow ± 3 μm variation.
©
ISO
ISO 13500:1998(E)
5.7  Calibration procedure — Hydrometers
5.7.1  Calibrate each hydrometer to be used using the same concentration dispersant solution as is used in the
test, at temperatures spanning the anticipated test temperatures, and by reading the top rather than the bottom of
the meniscus. Calibrate each hydrometer using the procedure below.
5.7.2  Prepare one litre of dispersant solution as follows:
3 3
5.7.2.1  Place 125 cm ± 2 cm (125 g ± 2 g) of dispersant solution from test procedure (7.11.1) into a 1-litre
volumetric flask.
5.7.2.2  Dilute to the 1 000-cm mark with deionized water. Mix thoroughly.
5.7.3  Place the dispersant solution in a sedimentation cylinder. Then place the cylinder in a constant-temperature
bath. Set bath temperature to the lowest expected temperature for any actual test. Allow to reach equilibrium
± 0,2 °C. Insert the hydrometer to be calibrated and wait at least 5 min for the hydrometer and solution to reach bath
temperature.
5.7.4  Take a hydrometer reading at the top of the meniscus formed by the stem, and take a thermometer reading.
Repeat readings at least 5 min apart so as to obtain a minimum of four readings each.
5.7.5  Calculate the average hydrometer reading and designate as R1. Calculate the average temperature reading
and designate as T1.
5.7.6  Repeat 5.7.3 through 5.7.4 except set bath temperature to highest expected test temperature, calculate
average hydrometer and temperature readings, and designate these readings as R2 and T2.
5.7.7  Calculate the hydrometer correction curve slope (Mc) as follows:
RR12−
()
Mc= 1000 (4)
TT21−
()
where
R1 is the average hydrometer reading at lower temperature;
R2 is the average hydrometer reading at higher temperature;
T1 is the average temperature reading at lower temperature;
T2 is the average temperature reading at higher temperature.
NOTE  Temperature may be measured in either °C or °F so long as all measurements and calculations are consistent in units
(including subsequent use of hydrometer in routine test situations).
5.7.8  Calculate the hydrometer correction curve intercept (Bc) as follows:
BMcc=×T1+−R1 1× 1000 (5)
()( )
[]
where
Mc is the hydrometer correction curve slope;
T1 is the average thermometer reading at lower temperature;
R1 is the average hydrometer reading at lower temperature.
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ISO
ISO 13500:1998(E)
5.7.9  Record Mc, Bc and hydrometer serial number in permanent calibration record and on test data sheet used in
test 7.13 and 8.13.
For “Hydrometer calibration. Example data sheet and calculation”, see C.1.
5.8  Calibration — Motor-driven direct-indicating viscometers
5.8.1  Apparatus and materials.
5.8.1.1  Standard thermometer, with an accuracy of ± 0,1°C, e.g., ASTM 90c or 91c.
5.8.1.2  Certified calibration fluid, of viscosity 20 mPa{s, with chart (viscosity vs. temperature).
5.8.1.3  Certified calibration fluid, of viscosity 50 mPa{s, with chart (viscosity vs. temperature).
5.8.1.4  Magnifying glass, approximately 3· magnification.
5.8.2  Procedure
5.8.2.1  Allow the viscometer and the calibration fluids to stand on counter-top a minimum of 2 h to approach
temperature equilibrium.
5.8.2.2  Operate viscometer without fluid a minimum of 2 min to loosen bearing and gears.
5.8.2.3  Clean and dry viscometer cup. Fill the viscometer cup to scribed line with 20 mPa{s calibration fluid and
place on meter stage. Raise stage until fluid level is to inscribed line on rotor sleeve.
5.8.2.4  Place thermometer into the fluid and hold or tape to the side of viscometer to prevent breakage.
5.8.2.5  Operate viscometer at 100 r/min setting until thermometer reading is stable to within ± 0,1 °C. Record
temperature reading.
5.8.2.6  Using magnifying glass, take dial readings at 300 r/min and 600 r/min settings. Estimate readings to
nearest 0,5 dial unit and record.
5.8.2.7  Compare 300 r/min dial reading to certified viscosity at test temperature from fluid calibration chart. Record
readings and deviation from certified calibration fluid viscosity as furnished by supplier. Divide 600 r/min reading by
1,98 to obtain viscosity value at 600 r/min. Compare this value to certified fluid.
5.8.2.8  Repeat 5.8.2, 5.8.2.3 through 5.8.2.7 using 50 mPa{s fluid.
5.8.2.9  Compare deviations to values in Table 3. Tolerances shall not exceed values in Table 3.
Table 3 — Dial reading tolerances with various calibration fluids, F-1 spring (or equivalent)
in motor-driven viscometer
Calibration fluid Acceptable tolerance
300 r/min 600 r/min/1,98
20 mPa·s ± 1,5 ± 2
50 mPa·s ± 1,5 ± 2
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5.9  Calibration — Laboratory pressure-measuring devices
5.9.1  Type and accuracy: Pressure-measuring devices shall be readable to at least 2,5 % of full-scale range.
5.9.2  Pressure-measuring devices shall be calibrated to maintain ± 2,5 % accuracy of full-scale range.
5.9.3  Usable range: Pressure measurements shall be made at not less than 25 % nor more than 75 % of the full-
pressure span of pressure gauges.
5.9.4  Pressure-measuring devices shall be recalibrated with a master pressure-measuring device or a dead-weight
tester at 25 %, 50 , and 75 % of full scale.
5.10  Calibration — Standardization of EDTA solution
5.10.1  Reagent
5.10.1.1  Standard calcium chloride solution, c(CaCl ) = (0,010 0 ± 0,000 1) mol/l.
5.10.2  Procedure
3 3 3 3
5.10.2.1  To a suitable flask, add 50 cm ± 0,05 cm deionized water and 50 cm ± 0,05 cm of standard CaCl
solution.
5.10.2.2  Proceed as in 7.6.1 through 7.6.5, but without adding barite or additional water. (Use the 100 cm solution
prepared above in place of the 100 cm deionized water specified in 7.6.1.)
5.10.2.3  Calculate calibration correction (C ) as follows:
c
CC=- 200 (6)
cm
where C is the 40 · (EDTA volume, cm )
m
NOTE  The calibration correction as determined by this procedure results in a number to be subtracted from the sample test
value, Ss.
a) Example of calibration correction determination:
EDTA volume for CaCl solution = 4,8 cm
C = 40 · 4,8 = 192
m
C = 192 2 200
c
C = 2 8
c
a) Example of calibration correction use:
EDTA for sample = 6,1 cm
Test value for sample, s = 244 mg/kg
S
Corrected test value, S = Ss 2 C = 244 2 (28) = 252 mg/kg
c c
6  Packaged materials
6.1  Description
6.1.1  Packaging of palletized goods should safeguard the means of safe handling, transport, storage, and
identification, and minimize damage and spillage. Packed material should be inside the dimensions of the pallet
although some overhang is allowed.
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6.1.2  This procedure applies to products covered by this International Standard. The main intention is to improve
the possible recycling of all packaging materials, including dry powdered or granular materials, not covered under
this International Standard, used in drilling fluids, completion fluids and oil well cements.
6.2  Apparatus — Pallets
6.2.1  The preferred pallet design and construction should be in accordance with ISO 6780 or APME 1993.
6.2.2  Preferred sizes for wooden pallets include:
a) 1200 mm · 1000 mm (47 in · 39 in) CP6;
b) 1140 mm · 1140 mm (45 in · 45 in) CP8/CP9/CP3;
c) 1219 mm 1219 mm (48 in 48 in);
· ·
d) 1118 mm · 1321 mm (44 in · 52 in);
e) 1067 mm · 1321 mm (42 in · 52 in) equivalent to CP4/CP7;
f) 1016 mm · 1219 mm (40 in · 48 in).
NOTE  CP is the size in accordance with ISO 6780.
6.2.3  Other pallet sizes and details concerning design and construction shall be agreed upon by the manufacturer
and the customer.
6.2.4  The maximum outside dimensions of the total package shall be in accordance with the applicable pallet size
plus a maximum overhang of 3 cm (1,2 in). The overall height shall not exceed 203,2 cm (80 in).
6.2.5  The maximum net mass should not exceed 2 000 kg (4 409 lb).
6.3  Apparatus — Bags
6.3.1  The manufacturer filling the bag shall take reasonable steps to ensure bag construction capable of safe
handling, transport and storage.
6.3.2  The manufacturer shall take reasonable steps to select bags that will minimize waste and provide recycling
possibilities of the packaging material.
6.3.3  The manufacturer shall consider humidity-barrier capabilities of the bags against the needs of the particular
product when selecting bags.
6.4  Marking — Pallets
Markings shall include the following where applicable and as specified by individual contracts:
a) product name;
b) gross/net mass, in kilograms or pounds.
6.5  Marking — Bags
Markings shall include the following where applicable and as specified by individual contracts:
a) name of the material in print script at least 13 mm in height;
b) mass of the material in letters, or numbers and letters, at least 6 mm in height. The mass shall be listed in
kilograms;
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c) lot/batch number in print script and/or numbers at least 3 mm in height, traceable to manufacturer’s country of
origin;
d) identification as recyclable;
e) safety information.
6.6  Pallet covers
6.6.1  Each pallet may have a cover made of at least one of the following:
a) Polyethylene (PE) shrink or wrapped film.
b) PE bonnet type.
c) Polypropylene (PP) bonnet type.
6.6.2  All plastics shall be UV-stabilized, unless otherwise requested. Cardboard, carton, or wood covers may be
used in place of the above. If appropriate, a bottom layer of cardboard, PE sheet or plywood may be connected to
the cover to unitize the overall package.
6.7  Storage
The manufacturer shall advise on storage upon request.
6.8  Recycling
6.8.1  General
If appropriate, recycling of the remaining materials after using the contents may be done in accordance with the
guidelines given below. All recycling should be done in accordance with local instructions as well as with the
administration concerned
6.8.2  Pallets
General recovery and recycling, provided that pallet description is in accordance with ISO 6780 or APME 1993.
6.8.3  Cover
Selection for PE, PP or carton and recycle accordingly.
6.8.4  Bags
Use of high performance paper quality results in less packaging materials and less waste for recycling. After
separation of the various components, recycle accordingly.
NOTE  When handling chemicals, reduction in the volume of packaging materials can be obtained by application of containers
in a dedicated container scheme.
7  Barite
7.1  Description
7.1.1  Drilling grade barite is produced from commercial barium sulfate-containing ores. The manufacturer shall
retain certificates of analysis or similar documentation on these commercial barium sulfate ores. It may be produced
from a single ore or a blend of ores and may be a straight-mined product or processed by beneficiation methods,
i.e., washing, tabling, jigging, or flotation. It may contain accessory minerals other than the barium sulfate (BaSO )
mineral. Because of mineral impurities, commercial barite may vary in colour from off-white to grey to red or brown.
Common accessory minerals are silicates such as quartz and chert, carbonate compounds such as siderite and
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dolomite, and metallic oxide and sulfide compounds. Although these minerals are normally insoluble, they can,
under certain conditions, react with other components in some types of drilling fluids and cause adverse changes in
the drilling fluid properties. (See Annex A for more details.)
7.1.2  Drilling-grade barite shall be deemed to meet the requirements of this International Standard if a composite
sample representing no more than one day's production conforms to the chemical and physical requirements of
Table 4, represents the product produced, and is controlled by the manufacturer.
Table 4 — Barite physical and chemical requirements
Requirement Standard
Density 4,20 g/cm , minimum
Water-soluble alkaline earth metals, as calcium 250 mg/kg, maximum
Residue greater than 75 μm maximum mass fraction 3,0 %
Particles less than 6 μm in equivalent spherical diameter maximum mass fraction 30 %
7.2  Density — Reagent and apparatus for Le Chatelier flask method
.
7.2.1 Kerosene or mineral spirits
, regulated to 105 °C ± 3 °C.
7.2.2 Oven
with calcium sulfate (CAS No.7778-18-9) desiccant, or equivalent.
7.2.3 Desiccator
, clamped or weighted to prevent flotation in water bath.
7.2.4 Le Chatelier flask
at 32 °C ± 0,5 °C regulated to ± 0,1 °C (e.g. approximately 40 litre
7.2.5 Transparent constant-temperature bath
aquarium with heater/circulator attachment, or functional equivalent).
, with accuracy of 0,01 g.
7.2.6 Balance
7.2.7  Volumetric pipette, of capacity 10 cm .
.
7.2.8 Magnifying glass
, approximately 8 mm in diameter and 30 cm in length, or a functional equivalent.
7.2.9 Wooden dowel
, absorbent.
7.2.10 Tissue paper
NOTE  Laboratory grade tissues are non-absorbent and thus unsuitable for use in this test procedure.
7.2.11  Low-form weighing dish with spout, of approximately 100 cm capacity, or a functional equivalent.
7.2.12  Fine-bristle brush.
7.3  Density — Procedure
7.3.1  If required, equilibrate approximately 100 g dried barite to room temperature in the desiccator.
7.3.2  Fill a clean Le Chatelier flask to approximately 22 mm below the zero mark with kerosene.
Place the flask upright in the constant-temperature bath. The level of water in the bath shall be higher than
7.3.3
the 24 cm graduation of the flask, but below the stopper level. Assure flask is stabilized by use of clamps or
weights.
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7.3.4  Allow the flask and contents to equilibrate for a minimum of 1 h. Using the magnifying glass with care to keep
eyes at meniscus level, record the initial volume to the nearest 0,05 cm (doubtful digit) without removing the flask
from the constant-temperature bath.
3 3 3
NOTE  If kerosene level is above or below the 2 0,2 cm to + 1,2 cm volume range after equilibrating, use the 10 cm pipette
to add or remove kerosene in order for it to come within this range. Allow the flask to equilibrate at least 1 h and record initial
volume as in 7.3.4.
7.3.5  Remove the Le Chatelier flask from the bath, wipe dry, and remove the stopper. Roll several lengths of tissue
paper diagonally along the length of the dowel, and use this assembly as a swab to dry the inside neck of the flask.
Do not allow the swab to come into contact with the kerosene in the flask.
7.3.6  Weigh 80 g ± 0,05 g dried barite into the weighing dish and carefully transfer to the Le Chatelier flask. Take
care to avoid splashing of the kerosene or plugging of the flask with barite at the bulb. This is a slow process,
requiring repeated transfers of small amounts of barite. Use a brush to transfer any residual barite into the flask,
then replace the stopper.
7.3.7  If necessary, carefully tap the neck of the flask with the wooden dowel, or agitate carefully side to side, to
dislodge any barite clinging to the walls. Do not allow kerosene to come into contact with the ground glass stopper
joint of the flask.
7.3.8  Gently roll the flask along a smooth surface at no more than 45° from vertical, or twirl the upright flask at the
neck vigorously between the palms of both hands, to remove entrained air from the barite sample. Repeat this
procedure until no more bubbles can be seen rising from the barite.
7.3.9  Return the flask to the bath and let stand for at least 0,5 h.
7.3.10  Remove the flask from the bath and repeat 7.3.8 to remove any remaining air from the barite sample.
7.3.11  Immerse the flask in the bath again for at least 1 h.
7.3.12  Record the final volume in the same manner as described in 7.3.4.
7.4  Density — Calculation
Sample mass, g
Density, g / cm = (7)
Final volume, cm− Initial volume, cm
()( )
Record calculated density.
7.5  Water-soluble alkaline earth metals as calcium — Reagents and apparatus
7.5.1  A
...