SIST EN ISO 10111:2003
(Main)Metallic and other inorganic coatings - Measurement of mass per unit area - Review of gravimetric and chemical analysis methods (ISO 10111:2000)
Metallic and other inorganic coatings - Measurement of mass per unit area - Review of gravimetric and chemical analysis methods (ISO 10111:2000)
Migrated from Progress Sheet (TC Comment) (2000-07-10): N 201: New TD (980917)
Metallische und andere anorganische Überzüge - Messung der flächenbezogenen Masse - Übersicht über gravimetrische und chemische Analyseverfahren (ISO 10111:2000)
1.1 Allgemeines
Diese Internationale Norm erfasst allgemeine Verfahren zur Bestimmung der mittleren flächenbezogenen Masse von anodischen Oxidüberzügen, autokatalytisch, mechanisch, durch chemische Umwandlung, durch elektrolytische Abscheidung, durch Schmelztauchverfahren und durch Vakuum abgeschiedenen Überzügen durch gravimetrische und andere chemische Analysenverfahren die eine gewisse Bedeutung in der Nationalen und Internationalen Normung erreicht haben.
Eine Vielzahl von Verfahren werden beschrieben und sind eingeschlossen:
- Gravimetrische Verfahren für die chemische oder elektrochemische Auflösung des Überzugs oder des Substrats zur Bestimmung der flächenbezogenen Masse;
- Analytische Verfahren die die Auflösung des Überzugs für eine photometrische oder volumetrische Bestimmung der flächenbezogenen Masse nutzen;
- Zerstörungsfreie physikalische Instrumentenanalyse des Überzugs zur Bestimmung der flächenbezogenen Masse.
Außer für das gravimetrische Verfahren (ISO 3892:1980) werden in dieser Internationalen Norm keine Messunsicherheiten angegeben.
1.2 Quellen
Die im Anhang A zitierten Entmetallisierungsverfahren werden in der allgemein zugänglichen Fachliteratur beschrieben, oder sie sind zumindest von einem Laboratorium regelmäßig angewendet worden.
1.3 Einschränkungen
Die beschriebene Verfahren können für viele Kombinationen Überzug - Substrat angewandt werden. Sie sind nicht anwendbar, wenn weder der Überzug noch das Substrat chemisch oder physikalisch vollständig voneinander getrennt werden können, und ein Bestandteil, der beiden gemeinsam ist, kann nicht ohne weiteres abgetrennt werden kann (z.B. Nickel-Phosphor-Legierung von Nickel).
Revetements métalliques et autres revetements inorganiques - Mesurage de la masse surfacique - Présentation des méthodes d'analyse gravimétrique et chimique (ISO 10111:2000)
La présente Norme internationale présente un aperçu des méthodes générales d'analyse gravimétrique ou chimique de diverses sortes ayant atteint un degré de normalisation à l'échelon national ou international, utilisées pour la détermination de la masse surfacique moyenne de revêtements obtenus par dépôt électrolytique, dépôt par immersion, dépôt autocatalytique, matoplastie, dépôt sous vide, anodisation ou conversion chimique. Elle décrit un certain nombre de ces procédés de détermination de la masse surfacique, parmi lesquels : - des méthodes gravimétriques pour la mise en solution chimique ou électrochimique du dépôt ou du métal de base permettant la détermination de la masse surfacique du dépôt ; - des méthodes analytiques qui utilisent la mise en solution du dépôt en vue d'une détermination photométrique ou gravimétrique de la masse surfacique du dépôt ; - une méthode volumétrique ou une analyse physique du dépôt par des moyens non destructifs afin de déterminer sa masse surfacique. Sauf pour la méthode gravimétrique décrite dans l'ISO 3892:-, la présente Norme internationale n'indique pas les incertitudes de mesurage liées aux méthodes citées.
Kovinske in druge anorganske prevleke - Merjenje mase na enoto površine - Pregled gravimetrijskih in kemijskih analiznih metod (ISO 10111:2000)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 10111:2003
01-december-2003
Kovinske in druge anorganske prevleke - Merjenje mase na enoto površine -
Pregled gravimetrijskih in kemijskih analiznih metod (ISO 10111:2000)
Metallic and other inorganic coatings - Measurement of mass per unit area - Review of
gravimetric and chemical analysis methods (ISO 10111:2000)
Metallische und andere anorganische Überzüge - Messung der flächenbezogenen
Masse - Übersicht über gravimetrische und chemische Analyseverfahren (ISO
10111:2000)
Revetements métalliques et autres revetements inorganiques - Mesurage de la masse
surfacique - Présentation des méthodes d'analyse gravimétrique et chimique (ISO
10111:2000)
Ta slovenski standard je istoveten z: EN ISO 10111:2001
ICS:
25.220.40 Kovinske prevleke Metallic coatings
71.040.40 Kemijska analiza Chemical analysis
SIST EN ISO 10111:2003 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 10111:2003
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SIST EN ISO 10111:2003
EUROPEAN STANDARD
EN ISO 10111
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2001
ICS 25.220.20; 25.220.40
English version
Metallic and other inorganic coatings - Measurement of mass
per unit area - Review of gravimetric and chemical analysis
methods (ISO 10111:2000)
Revêtements métalliques et autres revêtements Metallische und andere anorganische Überzüge - Messung
inorganiques - Mesurage de la masse surfacique - der flächenbezogenen Masse - Übersicht über
Présentation des méthodes d'analyse gravimétrique et gravimetrische und chemische Analyseverfahren (ISO
chimique (ISO 10111:2000) 10111:2000)
This European Standard was approved by CEN on 16 November 2001.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 10111:2001 E
worldwide for CEN national Members.
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SIST EN ISO 10111:2003
EN ISO 10111:2001 (E)
Foreword
The text of the International Standard from Technical Committee ISO/TC 107 "Metallic and
other inorganic coatings" of the International Organization for Standardization (ISO) has been
taken over as an European Standard by Technical Committee CEN/TC 262 "Metallic and
other inorganic coatings", the secretariat of which is held by BSI.
This European Standard shall be given the status of a national standard, either by publication
of an identical text or by endorsement, at the latest by June 2002, and conflicting national
standards shall be withdrawn at the latest by June 2002.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United
Kingdom.
Endorsement notice
The text of the International Standard ISO 10111:2000 has been approved by CEN as a
European Standard without any modification.
NOTE Normative references to International Standards are listed in annex ZA (normative).
2
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SIST EN ISO 10111:2003
EN ISO 10111:2001 (E)
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions
of any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications,
indicated by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 3892 2000 Conversion coatings on metallic materials - EN ISO 3892 2001
Determination of coating mass per unit area -
Gravimetric methods
3
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SIST EN ISO 10111:2003
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SIST EN ISO 10111:2003
INTERNATIONAL ISO
STANDARD 10111
First edition
2000-06-15
Metallic and other inorganic coatings —
Measurement of mass per unit area —
Review of gravimetric and chemical
analysis methods
Revêtements métalliques et autres revêtements inorganiques — Mesurage
de la masse surfacique — Présentation des méthodes d'analyse
gravimétrique et chimique
Reference number
ISO 10111:2000(E)
©
ISO 2000
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
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ii © ISO 2000 – All rights reserved
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .2
3 Terms and definitions .2
4 Principle.3
5 Special equipment .3
6 Preparation of test specimen .3
7 Measurement of coated area .4
8 Determination of mass of coating by chemical analysis.4
9 Gravimetric determination of mass of coating.5
10 Calculations.6
Annex A (normative) Reagents for selective dissolution of metal layers.7
Bibliography.13
© ISO 2000 – All rights reserved iii
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SIST EN ISO 10111:2003
ISO 10111:2000(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 3.
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 International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 10111 was prepared by Technical Committee ISO/TC 107, Metallic and other inorganic
coatings, Subcommittee SC 2, Test methods.
Annex A forms a normative part of this International Standard.
iv © ISO 2000 – All rights reserved
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SIST EN ISO 10111:2003
INTERNATIONAL STANDARD ISO 10111:2000(E)
Metallic and other inorganic coatings — Measurement of mass per
unit area — Review of gravimetric and chemical analysis methods
WARNING — The methods referred to in this International Standard can involve hazardous materials,
operations and equipment. This International Standard does not purport to address all of the safety
problems associated with its use. It is the responsibility of whoever uses this International Standard to
consult and establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to its use.
1 Scope
1.1 General
This International Standard outlines general methods for determining the average surface density over a measured
area of anodic oxide or of a coating deposited autocatalytically, mechanically, by chemical conversion, by
electrodeposition, by hot dip galvanizing and by vacuum using gravimetric and other chemical analysis procedures
that have attained some degree of national or international standardization.
A variety of procedures are described and include:
� gravimetric procedures for chemical or electrochemical dissolution of the coating or the substrate to determine
the coating surface density;
� analytical procedures that utilize dissolution of the coating for photometric or volumetric determination of the
coating surface density;
� non-destructive instrumental physical analysis of the coating to determine the surface density.
With the exception of the gravimetric method described in ISO 3892:—, this International Standard does not give
the measurement uncertainties of the methods cited.
1.2 Sources
The stripping methods cited in annex A are described in specifications in the open literature or have been used
routinely by at least one laboratory.
1.3 Restrictions
The procedures described can be used for many coating-substrate combinations. They cannot be used where
neither the coating nor substrate material can be completely removed, one from the other by chemical or physical
means and there is a constituent common to both that is not readily separated (e.g. nickel phosphorus alloy on
nickel).
NOTE The measurement of very thin coatings on very small pieces can result in a reduction in accuracy and a lack of
repeatability. Several measurements using a combination of different procedures on similar samples might overcome this
situation.
© ISO 2000 – All rights reserved 1
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
1.4 Limitations
In principle, the gravimetric procedures can be used to measure very thin coatings or to measure coatings over
2
small areas, but not thin coatings over small areas. The limits depend on the required accuracy; e.g., 2,5 mg/cm of
2 2 2
coating might require 1 cm , but 0,1 mg/cm of coating would require 25 cm to obtain 2,5 mg of coating. These
limitations do not apply to the chemical analysis methods.
The gravimetric method does not indicate the presence of bare spots or sites with thicknesses lower than the
specified minimum in the measuring areas. In addition, the single value obtained from each measuring area is the
mean thickness of that area. There can be no further mathematical analysis of this single value, for example, for
statistical process control purposes.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 2079:1981, Surface treatment and metallic coatings — General classification of terms.
ISO 2080:1981, Electroplating and related processes — Vocabulary.
ISO 2081:1986, Metallic coatings — Electroplated coatings of zinc on iron or steel.
ISO 2082:1986, Metallic coatings — Electroplated coatings of cadmium on iron or steel.
ISO 2093:1986, Electroplated coatings of tin — Specification and test methods.
ISO 2106:1982, Anodizing of aluminium and its alloys — Determination of mass per unit area (surface density) of
anodic oxide coatings — Gravimetric method.
1)
ISO 3892:— , Conversion coatings on metallic materials — Determination of coating mass per unit area —
Gravimetric methods.
ISO 4522-1:1985, Metallic coatings — Test methods for electrodeposited silver and silver alloy coatings — Part 1:
Determination of coating thickness.
ISO 4524-1:1985, Metallic coatings — Test methods for electrodeposited gold and gold alloy coatings — Part 1:
Determination of coating thickness.
ISO 7587:1986, Electroplated coatings of tin-lead alloys — Specification and test methods.
ISO 8407: 1991, Corrosion of metals and alloys — Removal of corrosion products from corrosion test specimens.
3 Terms and definitions
For the purposes of this standard, the terms and definitions given in ISO 2079 and ISO 2080 apply.
1) To be published. (Revision of ISO 3892:1980)
2 © ISO 2000 – All rights reserved
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
4Principle
The mass of a coating over a measured area is determined by:
a) weighing the test specimen before and after dissolving the coating in a reagent or electrolyte that does not
attack the substrate or
b) weighing the coating after dissolving the substrate in a reagent that does not attack the coating or
c) dissolving both the coating and the substrate, or the coating alone, and quantitatively analysing the resulting
solution.
The surface density of the coating is calculated from the mass and area measurements and its thickness is based
on the mass, area and density of the coating material.
5 Special equipment
Certain specialized chemical, electrochemical and chemical analysis equipment is required for some of the specific
methods referred to in Table A.1. (See clauses 8 and 9.)
6 Preparation of test specimen
6.1 Size
The specimen shall be large enough to permit area and mass measurement of adequate accuracy. (See clauses 8
and 9.)
6.2 Shape
The shape of the test specimen should be such that the surface area can be readily measured without difficulty. A
rectangular or circular test specimen is usually suitable.
6.3 Edge condition
If the area to be measured is small and has to be known accurately, the edges may need to be dressed to remove
smeared coating, to remove loose burrs and to provide well-defined and (for rectangles) straight edges. This should
2
be considered for areas less than 100 mm .
One method of dressing the edges of a rectangular specimen involves clamping the specimen between two plastic
or metal blocks with the edge of the specimen flush with the edges of the blocks and then grinding and polishing
the edges metallographically.
6.4 Heat treatment
If the substrate has to be dissolved in such a way as to leave the coating intact, it may be desirable to first treat the
2
test specimen so that the coating will not curl up tightly or fall apart. Some gold deposits of 1,5 mg/cm (< 0,9�m)
will fall apart when their substrates are dissolved, but will support themselves after heat treatment at 120�Cfor 3h.
If the thickness of a coating (instead of its surface density) is being determined, a heat treatment that could change
the density of the coating material shall not be used.
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
7 Measurement of coated area
7.1 Measurement method
Since the accuracy of the area measurement shall be greater than the desired accuracy of the surface density
measurement, the method of measuring the area depends on the desired accuracy and the specimen size.
The measurement uncertainty of the gravimetric method is normally less than 5 % over a wide range of thicknesses
(see ISO 3892).
7.2 Surface measuring equipment
The area can be measured with a planimeter, but it is usually determined by linear measurements. Often a
micrometer or vernier calliper is used. For large areas, however, a rule may do.
For maximum accuracy, a measuring microscope shall be used.
It may be difficult to measure directly the area of threaded articles with sufficient accuracy in which case the area
shall be determined from drawings or published tables.
7.3 Number of measurements
Because circular or rectangular specimens will not be perfectly circular or rectangular, each dimension shall be
measured in three places. For a rectangle, the length of each edge and the length and width through the centre
shall be measured and an average obtained for each dimension.
NOTE In the case of a cylinder, one would normally measure the diameter and length. In specifications for metallic coated
wire (fencing) that has been electroplated or coated by other processes, the length of the wire specimen is not measured, but is,
in effect, calculated from the mass (which is measured anyway), the radius and the density of the substrate material as follows:
m
l �
2
�r �
s
where
l is the length;
m is the mass;
r is the radius;
� is the density of the substrate.
s
8 Determination of mass of coating by chemical analysis
The chemical analysis method is very general. Both coating and substrate are dissolved in a suitable reagent and
then the resulting solution is analysed for the coating material. For each coating-substrate-reagent combination,
there may be several analytical methods.
4 © ISO 2000 – All rights reserved
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SIST EN ISO 10111:2003
ISO 10111:2000(E)
9 Gravimetric determination of mass of coating
9.1 Specimen size
Since the measurement uncertainty of the mass measurement shall be less than the desired measurement
uncertainty of the surface density measurement, the test specimen shall be large enough for the coating to be
weighed with the desired accuracy.
9.2 Gravimetric analysis equipment
A balance is required for gravimetric analysis, but the required sensitivity of the balance depends on the size of the
test specimen, the coating thickness (coating mass) and the required accuracy of the measurement. The analytical
balance shall be capable of weighing to an accuracy of 0,1 mg for weighing the test pieces under examination
before and after dissolution of the coatings. For anodic and cathodic dissolution, a constant d.c. source is
...
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