ISO 9697:2008
(Main)Water quality — Measurement of gross beta activity in non-saline water — Thick source method
Water quality — Measurement of gross beta activity in non-saline water — Thick source method
ISO 9697:2008 specifies a method for the determination of gross beta activity in non-saline waters. The method covers non-volatile radionuclides with maximum beta energies > 0,3 MeV. Measurement of very low energy beta emitters, such as 3H; 14C, 35S and 241Pu, is not included in ISO 9697:2008. The method is applicable to the analysis of raw and potable waters.
Qualité de l'eau — Mesurage de l'activité bêta globale des eaux non salines — Méthode par source concentrée
L'ISO 9697:2008 spécifie une méthode de détermination de l'activité bêta globale des eaux non salines. La méthode couvre les radionucléides non volatiles émetteurs bêta avec des énergies maximales > 0,3 MeV. Le mesurage des émetteurs bêta de très faible énergie tels que 3H, 14C, 35S et 241Pu n'est pas inclus dans l'ISO 9697:2008. La méthode est applicable à l'analyse des eaux brutes et potables.
Kakovost vode - Merjenje skupne beta aktivnosti v neslanih vodah - Metoda robustnega vira
Ta mednarodni standard določa metodo določevanja skupne beta aktivnosti v neslanih vodah. Metoda zajema nehlapne radionuklide z največjimi energijami beta > 0,3 MeV. Meritev zelo nizkih beta energijskih oddajnikov, kot so 3H, 14C, 35S in 241Pu ni vključena v ta standard. Metoda se uporablja za analizo neobdelane in pitne vode.
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INTERNATIONAL ISO
STANDARD 9697
Second edition
2008-11-01
Water quality — Measurement of gross
beta activity in non-saline water — Thick
source method
Qualité de l'eau — Mesurage de l'activité bêta globale des eaux non
salines — Méthode par source concentrée
Reference number
ISO 9697:2008(E)
©
ISO 2008
---------------------- Page: 1 ----------------------
ISO 9697:2008(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
COPYRIGHT PROTECTED DOCUMENT
© ISO 2008
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 either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2008 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 9697:2008(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Symbols, definitions, and units. 2
4 Principle. 2
5 Reagents and equipment . 3
6 Procedure . 4
7 Source control. 7
8 Expression of results . 7
9 Test report . 9
Bibliography . 11
© ISO 2008 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 9697:2008(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 9697 was prepared by Technical Committee ISO/TC 147, Water quality.
This second edition cancels and replaces the first edition (ISO 9697:1992), which has been technically revised.
iv © ISO 2008 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 9697:2008(E)
Water quality — Measurement of gross beta activity in non-
saline water — Thick source method
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this International Standard
be carried out by suitably trained staff.
1 Scope
This International Standard specifies a method for the determination of gross beta activity in non-saline waters.
The method covers non-volatile radionuclides with maximum beta energies > 0,3 MeV. Measurement of very
3 14 35 241
low energy beta emitters, such as H, C, S and Pu, is not included in this International Standard.
The method is applicable to the analysis of raw and potable waters.
2 Normative references
The following referenced documents are indispensable for the application of this documents. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
ISO 5667-14, Water quality — Sampling — Part 14: Guidance on quality assurance of environmental water
sampling and handling
ISO 9696, Water quality — Measurement of gross alpha activity in non-saline water — Thick source method
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
1)
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
1) To be published. (Revision of ISO 31-9:1992)
© ISO 2008 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 9697:2008(E)
3 Symbols, definitions, and units
For the purposes of this document, the symbols, definitions, and units given in ISO 80000-10, and the
following, apply.
A beta activity, in becquerels, of the calibration source
c beta activity concentration, in becquerels per litre
A
∗
c decision threshold, in becquerels per litre
A
#
c detection limit, in becquerels per litre
A
cc, lower and upper limits of the confidence interval, in becquerels per litre
AA
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the residue deposited on the planchet sample
r
r background count rate, in reciprocal seconds
0
r background count rate, in reciprocal seconds, from the alpha window
0α
r sample gross count rate, in reciprocal seconds
g
r gross count rate, in reciprocal seconds, from the alpha calibration source
gα
r calibration count rate, in reciprocal seconds
s
r calibration count rate, in reciprocal seconds, from the alpha calibration source
sα
S area, in square millimetres, of the planchet
t background counting time, in seconds
0
t sample counting time, in seconds
g
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
A
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
A
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample
t
ε counting efficiency for the specified radioactive standard
alpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
χ
calibration source
4 Principle
Gross beta activity determination is not an absolute determination of the radioactivity of all beta-emitting
radionuclides in a sample, but a relative determination referred to a specific beta emitter that constitutes the
standard calibration source. This type of determination is also known as beta index.
The sample, taken, handled and preserved as specified in ISO 5667-1 and ISO 5667-3, is evaporated almost
to dryness, converted to the sulfate form and then ignited at 350 °C. A portion of the residue is transferred to a
planchet and the beta activity measured by counting in an appropriate counting assembly calibrated against a
40 90 90
suitable beta calibration standard, such as potassium-40 ( K) or strontium-90-yttrium-90 ( Sr + Y).
If simultaneous gross alpha and beta measurements are required on the same water sample, the procedure
specified in this International Standard is common to that of ISO 9696, and sample sources can be measured
2
up to 10 mg/cm .
2 © ISO 2008 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 9697:2008(E)
5 Reagents and equipment
5.1 Reagents
Except for the certified reference solution, all reagents shall be of recognised analytical grade and shall not
contain any detectable beta activity.
NOTE A method for preparing reagent blanks to check for the absence of any endemic radioactivity or contamination
is given in Clause 7.
5.1.1 Water, complying with ISO 3696:1987, grade 3.
5.1.2 Certified reference solution. A calibration laboratory establishes traceability of its own measurement
standards and measuring instruments to the International System of Units (SI) by means of an unbroken chain
of calibrations or comparisons linking them to relevant primary standards of the SI units of measurement. The
link to SI units may be achieved by reference to national measurement standards. National measurement
standards may be primary standards, which are primary realisations of the SI units or agreed representations
of SI units based on fundamental physical constants, or they may be secondary standards which are
standards calibrated by another national metrology institute. When using external calibration services,
traceability of measurement shall be assured by the use of calibration services from laboratories that can
demonstrate competence, measurement capability and traceability. The calibration certificates issued by
these laboratories shall contain the measurement results, including the measurement uncertainty and/or a
statement of compliance with an identified metrological specification.
The choice of beta standards will depend on the knowledge of the type of radioactive contaminant likely to be
90 40
present in the waters being tested. Among standard solutions of beta-emitting radionuclides, Sr and K are
commonly used.
40
NOTE The beta activity of K in natural potassium is 27,4 Bq/g and hence in potassium chloride, it is
14,4/1 000 Bq/mg.
5.1.3 Nitric acid, c(HNO ) = 8 mol/l.
3
5.1.4 Sulfuric acid, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, mass fraction w(H SO ) = 95 %.
2 4 2 4
5.1.5 Volatile organic solvents: methanol and acetone.
5.1.6 Calcium sulfate, CaSO .
4
226 210
CAUTION — As calcium salts may contain trace amounts of Ra and/or Pb, checks for the
presence of these nuclides shall be made.
5.2 Equipment
Usual laboratory equipment and, in particular, the following.
5.2.1 Beta counter, preferably of the gas-flow proportional type, incorporating a plastic scintillation detector
or a silicon-charged particle detector [passivated implanted planar silicon (PIPS)].
When using a gas-flow proportional counter, it is advisable to choose the beta window to have the beta-alpha
cross-talk close to zero and take into account the alpha-beta cross-talk. If equipment other than gas-flow
proportional counters is used, then cross-talk may be ignored.
If a windowless gas-flow proportional counter is used, carry out regular checks for possible contamination of
the counting system by counting blank samples.
NOTE The particulate nature of the source to be counted can give rise to contamination if operated in a vacuum (as
in the case of a PIPS) or gas-flow systems (as used in a proportional counter).
© ISO 2008 – All rights reserved 3
---------------------- Page: 7 ----------------------
ISO 9697:2008(E)
2 2
5.2.2 Planchet, counting tray, of surface density at least 2,5 mg/mm (250 mg/cm ), having a lipped edge
and made of stainless steel.
The diameter of the planchet to be used is determined by the counter requirements, i.e. the detector diameter
and source holder dimensions.
NOTE An evenly spread source is required and some workers find it easier to produce this on a polished metal
surface, whereas others prefer to use an etched or roughened planchet (sand blasting and chemical etching has been
applied for this purpose).
5.2.3 Muffle furnace, capable of being maintained at (350 ± 10) °C.
6 Procedure
6.1 Sampling
The taking, handling, and storage of water samples shall be performed as specified in ISO 5667-1, ISO 5667-3
and ISO 5667-14.
Carry out filtration immediately on collection and before acidification, if any, if the measurement of the activity
must be done on the filtered sample of water.
NOTE Acidification of the water sample will minimise the loss of radioactive material from solution by adsorption. If
carried out before filtration, acidification will desorb radioactive material initially adsorbed on the particulate material.
6.2 Pretreatment
The determination of the total solids content of the water may be performed to determine the smallest volume
of water needed for the measurement. Making due allowance for changes in composition due to ignition at
350 °C and sulfation of the residue, calculate the volume of sample required to produce a mass per unit area
of solid residue slightly in excess of ρ given by:
S
m
r
ρ = W 0,1 (1)
S
S
where
...
SLOVENSKI STANDARD
SIST ISO 9697:2010
01-september-2010
Kakovost vode - Merjenje skupne beta aktivnosti v neslanih vodah - Metoda
robustnega vira
Water quality - Measurement of gross beta activity in non-saline water - Thick source
method
Qualité de l'eau - Mesurage de l'activité bêta globale des eaux non salines - Méthode par
source concentrée
Ta slovenski standard je istoveten z: ISO 9697:2008
ICS:
13.060.60 Preiskava fizikalnih lastnosti Examination of physical
vode properties of water
17.240 Merjenje sevanja Radiation measurements
SIST ISO 9697:2010 en,fr
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 9697:2010
---------------------- Page: 2 ----------------------
SIST ISO 9697:2010
INTERNATIONAL ISO
STANDARD 9697
Second edition
2008-11-01
Water quality — Measurement of gross
beta activity in non-saline water — Thick
source method
Qualité de l'eau — Mesurage de l'activité bêta globale des eaux non
salines — Méthode par source concentrée
Reference number
ISO 9697:2008(E)
©
ISO 2008
---------------------- Page: 3 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
COPYRIGHT PROTECTED DOCUMENT
© ISO 2008
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 either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2008 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Symbols, definitions, and units. 2
4 Principle. 2
5 Reagents and equipment . 3
6 Procedure . 4
7 Source control. 7
8 Expression of results . 7
9 Test report . 9
Bibliography . 11
© ISO 2008 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(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 9697 was prepared by Technical Committee ISO/TC 147, Water quality.
This second edition cancels and replaces the first edition (ISO 9697:1992), which has been technically revised.
iv © ISO 2008 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 9697:2010
INTERNATIONAL STANDARD ISO 9697:2008(E)
Water quality — Measurement of gross beta activity in non-
saline water — Thick source method
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this International Standard
be carried out by suitably trained staff.
1 Scope
This International Standard specifies a method for the determination of gross beta activity in non-saline waters.
The method covers non-volatile radionuclides with maximum beta energies > 0,3 MeV. Measurement of very
3 14 35 241
low energy beta emitters, such as H, C, S and Pu, is not included in this International Standard.
The method is applicable to the analysis of raw and potable waters.
2 Normative references
The following referenced documents are indispensable for the application of this documents. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
ISO 5667-14, Water quality — Sampling — Part 14: Guidance on quality assurance of environmental water
sampling and handling
ISO 9696, Water quality — Measurement of gross alpha activity in non-saline water — Thick source method
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
1)
ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics
1) To be published. (Revision of ISO 31-9:1992)
© ISO 2008 – All rights reserved 1
---------------------- Page: 7 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(E)
3 Symbols, definitions, and units
For the purposes of this document, the symbols, definitions, and units given in ISO 80000-10, and the
following, apply.
A beta activity, in becquerels, of the calibration source
c beta activity concentration, in becquerels per litre
A
∗
c decision threshold, in becquerels per litre
A
#
c detection limit, in becquerels per litre
A
cc, lower and upper limits of the confidence interval, in becquerels per litre
AA
m mass, in milligrams, of ignited residue from volume, V
m mass, in milligrams, of the residue deposited on the planchet sample
r
r background count rate, in reciprocal seconds
0
r background count rate, in reciprocal seconds, from the alpha window
0α
r sample gross count rate, in reciprocal seconds
g
r gross count rate, in reciprocal seconds, from the alpha calibration source
gα
r calibration count rate, in reciprocal seconds
s
r calibration count rate, in reciprocal seconds, from the alpha calibration source
sα
S area, in square millimetres, of the planchet
t background counting time, in seconds
0
t sample counting time, in seconds
g
u(c ) standard uncertainty, in becquerels per litre, associated with the measurement result
A
U expanded uncertainty, in becquerels per litre, calculated from U = ku(c ), with k = 1, 2 …
A
V volume, in litres, of test sample equivalent to the mass of solid on the planchet
V volume, in litres, of the water sample
t
ε counting efficiency for the specified radioactive standard
alpha-beta cross-talk, percentage of alpha count going into the beta window from the alpha
χ
calibration source
4 Principle
Gross beta activity determination is not an absolute determination of the radioactivity of all beta-emitting
radionuclides in a sample, but a relative determination referred to a specific beta emitter that constitutes the
standard calibration source. This type of determination is also known as beta index.
The sample, taken, handled and preserved as specified in ISO 5667-1 and ISO 5667-3, is evaporated almost
to dryness, converted to the sulfate form and then ignited at 350 °C. A portion of the residue is transferred to a
planchet and the beta activity measured by counting in an appropriate counting assembly calibrated against a
40 90 90
suitable beta calibration standard, such as potassium-40 ( K) or strontium-90-yttrium-90 ( Sr + Y).
If simultaneous gross alpha and beta measurements are required on the same water sample, the procedure
specified in this International Standard is common to that of ISO 9696, and sample sources can be measured
2
up to 10 mg/cm .
2 © ISO 2008 – All rights reserved
---------------------- Page: 8 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(E)
5 Reagents and equipment
5.1 Reagents
Except for the certified reference solution, all reagents shall be of recognised analytical grade and shall not
contain any detectable beta activity.
NOTE A method for preparing reagent blanks to check for the absence of any endemic radioactivity or contamination
is given in Clause 7.
5.1.1 Water, complying with ISO 3696:1987, grade 3.
5.1.2 Certified reference solution. A calibration laboratory establishes traceability of its own measurement
standards and measuring instruments to the International System of Units (SI) by means of an unbroken chain
of calibrations or comparisons linking them to relevant primary standards of the SI units of measurement. The
link to SI units may be achieved by reference to national measurement standards. National measurement
standards may be primary standards, which are primary realisations of the SI units or agreed representations
of SI units based on fundamental physical constants, or they may be secondary standards which are
standards calibrated by another national metrology institute. When using external calibration services,
traceability of measurement shall be assured by the use of calibration services from laboratories that can
demonstrate competence, measurement capability and traceability. The calibration certificates issued by
these laboratories shall contain the measurement results, including the measurement uncertainty and/or a
statement of compliance with an identified metrological specification.
The choice of beta standards will depend on the knowledge of the type of radioactive contaminant likely to be
90 40
present in the waters being tested. Among standard solutions of beta-emitting radionuclides, Sr and K are
commonly used.
40
NOTE The beta activity of K in natural potassium is 27,4 Bq/g and hence in potassium chloride, it is
14,4/1 000 Bq/mg.
5.1.3 Nitric acid, c(HNO ) = 8 mol/l.
3
5.1.4 Sulfuric acid, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, mass fraction w(H SO ) = 95 %.
2 4 2 4
5.1.5 Volatile organic solvents: methanol and acetone.
5.1.6 Calcium sulfate, CaSO .
4
226 210
CAUTION — As calcium salts may contain trace amounts of Ra and/or Pb, checks for the
presence of these nuclides shall be made.
5.2 Equipment
Usual laboratory equipment and, in particular, the following.
5.2.1 Beta counter, preferably of the gas-flow proportional type, incorporating a plastic scintillation detector
or a silicon-charged particle detector [passivated implanted planar silicon (PIPS)].
When using a gas-flow proportional counter, it is advisable to choose the beta window to have the beta-alpha
cross-talk close to zero and take into account the alpha-beta cross-talk. If equipment other than gas-flow
proportional counters is used, then cross-talk may be ignored.
If a windowless gas-flow proportional counter is used, carry out regular checks for possible contamination of
the counting system by counting blank samples.
NOTE The particulate nature of the source to be counted can give rise to contamination if operated in a vacuum (as
in the case of a PIPS) or gas-flow systems (as used in a proportional counter).
© ISO 2008 – All rights reserved 3
---------------------- Page: 9 ----------------------
SIST ISO 9697:2010
ISO 9697:2008(E)
2 2
5.2.2 Planchet, counting tray, of surface density at least 2,5 mg/mm (250 mg/cm ), having a lipped edge
and made of stainless steel.
The diameter of the planchet to be used is determined by the counter requirements, i.e. the detector diameter
and source holder dimensions.
NOTE An evenly spread source is required and some workers find it easier to produce this on a polished metal
surface, whereas others prefer to use an etched or roughened planchet (sand blasting and chemical etching has been
applied for this purpose).
5.2.3 Muffle furnace, capable of being maintained at (350 ± 10) °C.
6 Procedure
6.1 Sampling
The taking, handling, and storage of water samples shall be performed as specified in ISO 5667-1, ISO 5667-3
and ISO 5667-14.
Carry out filtration immediately on collection and before acidification, if any, if the measurement of the activity
must be done on the filtered sample of water.
NOTE Acidification of the water sample will minimise the loss of radioactive material from solution by adsorption. If
carried out before filtration, acidification will desor
...
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kakovost vode - Merjenje celotne beta aktivnosti v neslanih vodah - Metoda robustnega viraQualité de l'eau - Mesurage de l'activité bêta globale des eaux non salines - Méthode par source concentréeWater quality - Measurement of gross beta activity in non-saline water - Thick source method13.280Varstvo pred sevanjemRadiation protection13.060.60Preiskava fizikalnih lastnosti vodeExamination of physical properties of waterICS:Ta slovenski standard je istoveten z:ISO 9697:2008oSIST ISO 9697:2009en,fr01-junij-2009oSIST ISO 9697:2009SLOVENSKI
STANDARD
oSIST ISO 9697:2009
Reference numberISO 9697:2008(E)© ISO 2008
INTERNATIONAL STANDARD ISO9697Second edition2008-11-01Water quality — Measurement of gross beta activity in non-saline water — Thick source method Qualité de l'eau — Mesurage de l'activité bêta globale des eaux non salines — Méthode par source concentrée
oSIST ISO 9697:2009
ISO 9697:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
COPYRIGHT PROTECTED DOCUMENT
©
ISO 2008 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 either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.
+ 41 22 749 01 11 Fax
+ 41 22 749 09 47 E-mail
copyright@iso.org Web
www.iso.org Published in Switzerland
ii © ISO 2008 – All rights reserved
oSIST ISO 9697:2009
ISO 9697:2008(E) © ISO 2008 – All rights reserved iiiContents Page Foreword.iv 1 Scope.1 2 Normative references.1 3 Symbols, definitions, and units.2 4 Principle.2 5 Reagents and equipment.3 6 Procedure.4 7 Source control.7 8 Expression of results.7 9 Test report.9 Bibliography.11
oSIST ISO 9697:2009
ISO 9697:2008(E) iv © ISO 2008 – All rights reserved 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 9697 was prepared by Technical Committee ISO/TC 147, Water quality. This second edition cancels and replaces the first edition (ISO 9697:1992), which has been technically revised. oSIST ISO 9697:2009
INTERNATIONAL STANDARD ISO 9697:2008(E) © ISO 2008 – All rights reserved 1Water quality — Measurement of gross beta activity in non-saline water — Thick source method WARNING — Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT — It is absolutely essential that tests conducted according to this International Standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for the determination of gross beta activity in non-saline waters. The method covers non-volatile radionuclides with maximum beta energies > 0,3 MeV. Measurement of very low energy beta emitters, such as 3H, 14C, 35S and 241Pu, is not included in this International Standard. The method is applicable to the analysis of raw and potable waters. 2 Normative references The following referenced documents are indispensable for the application of this documents. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use — Specification and test methods ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and sampling techniques ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water samples ISO 5667-14, Water quality — Sampling — Part 14: Guidance on quality assurance of environmental water sampling and handling ISO 9696, Water quality — Measurement of gross alpha activity in non-saline water — Thick source method ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories ISO 80000-10, Quantities and units — Part 10: Atomic and nuclear physics 1)
1) To be published. (Revision of ISO 31-9:1992) oSIST ISO 9697:2009
ISO 9697:2008(E) 2 © ISO 2008 – All rights reserved 3 Symbols, definitions, and units For the purposes of this document, the symbols, definitions, and units given in ISO 80000-10, and the following, apply. A beta activity, in becquerels, of the calibration source cA beta activity concentration, in becquerels per litre Ac∗ decision threshold, in becquerels per litre #Ac detection limit, in becquerels per litre ,AAcc lower and upper limits of the confidence interval, in becquerels per litre m mass, in milligrams, of ignited residue from volume, V mr mass, in milligrams, of the residue deposited on the planchet sample r0 background count rate, in reciprocal seconds r0α background count rate, in reciprocal seconds, from the alpha window rg sample gross count rate, in reciprocal seconds rgα gross count rate, in reciprocal seconds, from the alpha calibration source rs calibration count rate, in reciprocal seconds rsα calibration count rate, in reciprocal seconds, from the alpha calibration source S area, in square millimetres, of the planchet t0 background counting time, in seconds tg sample counting time, in seconds u(cA) standard uncertainty, in becquerels per litre, associated with the measurement result U expanded uncertainty, in becquerels per litre, calculated from U = ku(cA), with k
= 1, 2 … V volume, in litres, of test sample equivalent to the mass of solid on the planchet Vt volume, in litres, of the water sample ε=counting efficiency for the specified radioactive standard
alpha-beta cross-talk, percentage of alpha count going into the beta window from the alphacalibration source 4 Principle Gross beta activity determination is not an absolute determination of the radioactivity of all beta-emitting radionuclides in a sample, but a relative determination referred to a specific beta emitter that constitutes the standard calibration source. This type of determination is also known as beta index. The sample, taken, handled and preserved as specified in ISO 5667-1 and ISO 5667-3, is evaporated almost to dryness, converted to the sulfate form and then ignited at 350 °C. A portion of the residue is transferred to a planchet and the beta activity measured by counting in an appropriate counting assembly calibrated against a suitable beta calibration standard, such as potassium-40 (40K) or strontium-90-yttrium-90 (90Sr + 90Y). If simultaneous gross alpha and beta measurements are required on the same water sample, the procedure specified in this International Standard is common to that of ISO 9696, and sample sources can be measured up to 10 mg/cm2. oSIST ISO 9697:2009
ISO 9697:2008(E) © ISO 2008 – All rights reserved 35 Reagents and equipment 5.1 Reagents Except for the certified reference solution, all reagents shall be of recognised analytical grade and shall not contain any detectable beta activity. NOTE A method for preparing reagent blanks to check for the absence of any endemic radioactivity or contamination is given in Clause 7. 5.1.1 Water, complying with ISO 3696:1987, grade 3. 5.1.2 Certified reference solution. A calibration laboratory establishes traceability of its own measurement standards and measuring instruments to the International System of Units (SI) by means of an unbroken chain of calibrations or comparisons linking them to relevant primary standards of the SI units of measurement. The link to SI units may be achieved by reference to national measurement standards. National measurement standards may be primary standards, which are primary realisations of the SI units or agreed representations of SI units based on fundamental physical constants, or they may be secondary standards which are standards calibrated by another national metrology institute. When using external calibration services, traceability of measurement shall be assured by the use of calibration services from laboratories that can demonstrate competence, measurement capability and traceability. The calibration certificates issued by these laboratories shall contain the measurement results, including the measurement uncertainty and/or a statement of compliance with an identified metrological specification. The choice of beta standards will depend on the knowledge of the type of radioactive contaminant likely to be present in the waters being tested. Among standard solutions of beta-emitting radionuclides, 90Sr and 40K are commonly used. NOTE The beta activity of 40K in natural potassium is 27,4 Bq/g and hence in potassium chloride, it is 14,4/1 000 Bq/mg. 5.1.3 Nitric acid, c(HNO3) = 8 mol/l. 5.1.4 Sulfuric acid, c(H2SO4) = 18 mol/l,
= 1,84 g/ml, mass fraction w(H2SO4) = 95 %. 5.1.5 Volatile organic solvents: methanol and acetone. 5.1.6 Calcium sulfate, CaSO4. CAUTION — As calcium salts may contain trace amounts of 226Ra and/or 210Pb, checks for the presence of these nuclides shall be made. 5.2 Equipment Usual laboratory equipment and, in particular, the following. 5.2.1 Beta counter, preferably of the gas-flow proportional type, incorporating a plastic scintillation detector or a silicon-charged particle detector [passivated implanted planar silicon (PIPS)]. When using a gas-flow proportional counter, it is advisable to choose the beta window to have the beta-alpha cross-talk close to zero and take into account the alpha-beta cross-talk. If equipment other than gas-flow proportional counters is used, then cross-talk may be ignored. If a windowless gas-flow proportional counter is used, carry out regular checks for possible contamination of the counting system by counting blank samples. NOTE The particulate nature of the source to be counted can give rise to contamination if operated in a vacuum (as in the case of a PIPS) or gas-flow systems (as used in a proportional counter). oSIST ISO 9697:2009
ISO 9697:2008(E) 4 © ISO 2008 – All rights reserved 5.2.2 Planchet, counting tray, of surface density at least 2,5 mg/mm2 (250 mg/cm2), having a lipped edge and made of stainless steel. The diameter of the planchet to be used is determined by the counter requirements, i.e. the detector diameter and source holder dimensions. NOTE An evenly spread source is required and some workers find it easier to produce this on a polished metal surface, whereas others prefer to use an etched or roughened planchet (sand blasting and chemical etching has been applied for this purpose). 5.2.3 Muffle furnace, capable of being maintained at (350 ± 10) °C. 6 Procedure 6.1 Sampling The taking, handling, and storage of water samples shall be performed as specified in ISO 5667-1, ISO 5667-3 and ISO 5667-14. Carry out filtration immediately on collection and before acidification, if any, if the measurement of the activity must be done on the filtered sample of water. NOTE Acidification of the water sample will minimise the loss
...
NORME ISO
INTERNATIONALE 9697
Deuxième édition
2008-11-01
Qualité de l'eau — Mesurage de l'activité
bêta globale des eaux non salines —
Méthode par source concentrée
Water quality — Measurement of gross beta activity in non-saline
water — Thick source method
Numéro de référence
ISO 9697:2008(F)
©
ISO 2008
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ISO 9697:2008(F)
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ISO 9697:2008(F)
Sommaire Page
Avant-propos. iv
1 Domaine d'application. 1
2 Références normatives . 1
3 Symboles, définitions et unités. 2
4 Principe. 2
5 Réactifs et matériel. 3
6 Mode opératoire . 4
7 Contrôle de source . 7
8 Expression des résultats . 8
9 Rapport d'essai . 10
Bibliographie . 12
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ISO 9697:2008(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de
normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée
aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du
comité technique créé à cet effet. Les organisations internationales, gouvernementales et non
gouvernementales, en liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec
la Commission électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,
Partie 2.
La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes
internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur
publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres
votants.
L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable de ne
pas avoir identifié de tels droits de propriété et averti de leur existence.
L'ISO 9697 a été élaborée par le comité technique ISO/TC 147, Qualité de l'eau.
Cette deuxième édition annule et remplace la première édition (ISO 9697:1992), qui a fait l'objet d'une
révision technique.
iv © ISO 2008 – Tous droits réservés
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NORME INTERNATIONALE ISO 9697:2008(F)
Qualité de l'eau — Mesurage de l'activité bêta globale des eaux
non salines — Méthode par source concentrée
AVERTISSEMENT — Il convient que l'utilisateur de la présente Norme internationale soit familiarisé
avec les pratiques courantes de laboratoire. La présente Norme internationale n'a pas pour but de
traiter tous les problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe à
l'utilisateur d'établir des pratiques appropriées en matière d'hygiène et de sécurité, et de s'assurer de
la conformité à la réglementation nationale en vigueur.
IMPORTANT — Il est absolument essentiel que les essais conduits conformément à la présente
Norme internationale soient effectués par du personnel ayant reçu une formation adéquate.
1 Domaine d'application
La présente Norme internationale spécifie une méthode de détermination de l'activité bêta globale des eaux
non salines. La méthode couvre les radionucléides non volatils émetteurs bêta avec des énergies maximales
3 14 35 241
> 0,3 MeV. Le mesurage des émetteurs bêta de très faible énergie tels que H, C, S et Pu n'est pas
inclus dans la présente Norme internationale.
La méthode est applicable à l'analyse des eaux brutes et potables.
2 Références normatives
Les documents de référence suivants sont indispensables pour l'application du présent document. Pour les
références datées, seule l'édition citée s'applique. Pour les références non datées, la dernière édition du
document de référence s'applique (y compris les éventuels amendements).
ISO 3696:1987, Eau pour laboratoire à usage analytique — Spécification et méthodes d'essai
ISO 5667-1, Qualité de l'eau — Échantillonnage — Partie 1: Lignes directrices pour la conception des
programmes et des techniques d'échantillonnage
ISO 5667-3, Qualité de l'eau — Échantillonnage — Partie 3: Lignes directrices pour la conservation et la
manipulation des échantillons d'eau
ISO 5667-14, Qualité de l'eau — Échantillonnage — Partie 14: Lignes directrices pour le contrôle de la qualité
dans l'échantillonnage et la manutention des eaux environnementales
ISO 9696, Qualité de l'eau — Mesurage de l'activité alpha globale des eaux non salines — Méthode par
source concentrée
ISO/CEI 17025, Exigences générales concernant la compétence des laboratoires d'étalonnages et d'essais
1)
ISO 80000-10, Grandeurs et unités — Partie 10: Physique atomique et nucléaire
1) À publier. (Révision de l'ISO 31-9:1992)
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ISO 9697:2008(F)
3 Symboles, définitions et unités
Pour les besoins du présent document, les symboles, définitions et unités donnés dans l'ISO 80000-10 ainsi
que les suivants s'appliquent.
A activité bêta, en becquerels, de la source d'étalonnage
c concentration en activité bêta, en becquerels par litre
A
∗
c seuil de décision, en becquerels par litre
A
#
c limite de détection, en becquerel par litre
A
cc, limites supérieure et inférieure de l'intervalle de confiance, en becquerels par litre
AA
m masse, en milligrammes, de résidu calciné du volume, V
m masse, en milligrammes, du résidu de l'échantillon déposé sur la coupelle
r
r taux de comptage du bruit de fond, par seconde
0
r taux de comptage du bruit de fond, par seconde, de la fenêtre alpha
0α
r taux de comptage global d'échantillon, par seconde
g
r taux de comptage global, par seconde, de la source d'étalonnage alpha
gα
r taux de comptage de l'étalonnage, par seconde
s
r taux de comptage d'étalonnage, par seconde, de la source d'étalonnage alpha
sα
S surface, en millimètres carrés, de la coupelle
t temps de comptage du bruit de fond, en secondes
0
t temps de comptage de l'échantillon, en secondes
g
u(c ) incertitude type, en becquerels par litre, associée au résultat de mesure
A
U incertitude étendue, en becquerels par litre, calculée par U = ku(c ) avec k = 1, 2, …
A
V volume, en litres, de l'échantillon soumis à essai équivalent à la masse de solide sur la coupelle
V volume, en litres, de l'échantillon d'eau
t
ε efficacité de comptage pour l'étalon radioactif spécifié
taux de rejet alpha-bêta, pourcentage de comptage alpha passant dans la fenêtre bêta depuis la
χ
source d'étalonnage alpha
4 Principe
La détermination de l’activité bêta globale n'est pas une détermination absolue de la radioactivité de
l’ensemble des radionucléides émetteurs bêta d'un échantillon, mais une détermination relative par rapport à
un émetteur bêta spécifique qui constitue la source d'étalonnage de référence. Ce type de détermination est
également appelé indice bêta.
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ISO 9697:2008(F)
L'échantillon, prélevé, manipulé et conservé comme spécifié dans l'ISO 5667-1 et dans l'ISO 5667-3, est
évaporé pratiquement à sec, converti sous forme de sulfate puis calciné à 350 °C. Une partie du résidu est
transférée sur une coupelle et l'activité bêta est mesurée par comptage dans un dispositif de comptage
40
approprié étalonné par rapport à un étalon bêta approprié, tel que le potassium-40 ( K) ou le strontium-90-
90 90
yttrium-90 ( Sr + Y).
Si des mesurages alpha et bêta globaux sont nécessaires simultanément sur le même échantillon d'eau, le
mode opératoire spécifié dans la présente Norme internationale est identique à celui spécifié dans l'ISO 9696
2
et les sources d'échantillon peuvent être mesurées jusqu'à 10 mg/cm .
5 Réactifs et matériel
5.1 Réactifs
À l'exception de la solution de référence certifiée, tous les réactifs doivent être de qualité analytique reconnue
et ne doivent contenir aucune activité bêta détectable.
NOTE Une méthode permettant de préparer des blancs de réactif afin de contrôler l'absence de toute radioactivité
endémique ou de contamination est présentée à l'Article 7.
5.1.1 Eau, conforme à l'ISO 3696:1987, qualité 3.
5.1.2 Solution de référence certifiée. Un laboratoire d'étalonnage établit la traçabilité de ses propres
étalons de mesure et instruments de mesure conformément au Système international d'unités (système SI) au
moyen d'une chaîne continue d'étalonnages ou de comparaisons reliant ceux-ci à des étalons primaires
appropriés du système d'unités SI. Le lien avec les unités SI peut être établi en référence à des étalons de
mesure nationaux. Les étalons de mesure nationaux peuvent être des étalons primaires, qui sont des
réalisations primaires des unités SI ou des représentations reconnues d'unités SI basées sur des constantes
physiques fondamentales, ou peuvent être des étalons secondaires qui sont des étalons étalonnés par un
autre institut de métrologie national. Lors de l'utilisation de services d'étalonnage externes, la traçabilité de
mesure doit être assurée par l'utilisation de services d'étalonnage de laboratoires qui peuvent démontrer leur
compétence, leur capacité de mesure et leur traçabilité. Les certificats d'étalonnage émis par ces laboratoires
doivent contenir les résultats de mesure, comprenant l'incertitude de mesure et/ou une déclaration de
conformité à une spécification métrologique identifiée.
Le choix d'étalons bêta dépendra de la connaissance du type de contaminant radioactif susceptible d'être
présent dans les eaux soumises à essai. Parmi les solutions étalons de radionucléides émetteurs bêta, celles
90 40
avec du Sr et du K sont couramment utilisées.
40
NOTE L'activité bêta du K dans le potassium naturel est de 27,4 Bq/g et donc dans le chlorure de potassium, elle
est de 14,4/1 000 Bq/mg.
5.1.3 Acide nitrique, c(HNO ) = 8 mol/l.
3
5.1.4 Acide sulfurique, c(H SO ) = 18 mol/l, ρ = 1,84 g/ml, de fraction massique w(H SO ) = 95 %.
2 4 2 4
5.1.5 Solvants organiques volatils: méthanol et acétone.
5.1.6 Sulfate de calcium, CaSO .
4
226
ATTENTION — Étant donné que les sels de calcium peuvent contenir des traces de Ra et/ou de
210
Pb, le contrôle de la présence de ces nucléides doit être effectué.
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ISO 9697:2008(F)
5.2 Matériel
Matériel courant de laboratoire et en particulier ce qui suit.
5.2.1 Compteur bêta, de préférence du type utilisant un compteur proportionnel à circulation de gaz,
comportant un détecteur de scintillation plastique ou un détecteur de particules chargées de silicium [silicium
plan implanté passivé (PIPS)].
Si un compteur proportionnel à circulation de gaz est utilisé, il est recommandé de choisir la fenêtre bêta de
manière à obtenir un taux de rejet bêta-alpha proche de zéro et de prendre en compte le taux de rejet alpha-
bêta. Si un matériel autre qu'un compteur proportionnel à circulation de gaz est utilisé, le taux de rejet peut
être ignoré.
Si un compteur proportionnel à circulation de gaz sans fenêtre est utilisé, effectuer des contrôles réguliers à
l'aide de comptage d'échantillons de blanc pour détecter une contamination éventuelle du système de
comptage.
NOTE La nature particulaire de la source à compter peut conduire à des contaminations si elle est utilisée sous vide
(comme dans le cas du PIPS) ou dans des systèmes à circulation de gaz (comme dans le cas d'un compteur
proportionnel).
2
5.2.2 Coupelle, plateau de comptage, ayant une masse superficielle d'au moins 2,5 mg/mm
2
(250 mg/cm ), avec rebord et en acier inoxydable.
Le diamètre de la coupelle à utiliser est déterminé par les exigences du compteur, c'est-à-dire le diamètre du
détecteur et les dimensions du porte-source.
NOTE Une source uniformément répartie est requise et certains opérateurs trouvent plus commode de préparer
celle-ci sur une surface métallique polie, tandis que d'autres préfèrent utiliser une coupelle gravée ou rugueuse (le
décapage au sable et l'attaque chimique ont été utilisés à cette fin).
5.2.3 Four à moufle, pouvant être maintenu à une température de (350 ± 10) °C.
6 Mode opératoire
6.1 Échantillonnage
L'échantillonnage, la manipulation et la conservation des échantillons d'eau doivent être effectués comme
spécifié dans l'ISO 5667-1, l'ISO 5667-3 et l'ISO 5667-14.
Effectuer la filtration immédiatement après la collecte et avant acidification, le cas échéant, si le mesurage de
l'activité est à réaliser sur l'échantillon d'eau filtré.
NOTE L'acidification de l'échantillon d'eau réduit au minimum la perte de matériau radioactif de la solution par
adsorption. Si elle est effectuée avant la filtration, l'acidification désorbe le matériau radioactif initialement adsorbé sur le
matériau particulaire.
6.2 Prétraitement
La détermination des matières solides totales dans l'eau peut être effectuée pour déterminer le plus faible
volume d'eau nécessaire au mesurage. En tenant compte de manière appropriée des changements de
composition dus à la calcination à 350 °C et à la sulfatation du résidu, calculer le volume d'échantillon requis
pour produire une masse par unité de surface de résidu solide légèrement en excès, ρ , donnée par:
S
m
r
ρ = W 0,1 (1)
S
S
4 © ISO 2008 – Tous droits ré
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