SIST EN ISO 10271:2011
(Main)Dentistry - Corrosion test methods for metallic materials (ISO 10271:2011)
Dentistry - Corrosion test methods for metallic materials (ISO 10271:2011)
ISO 10271:2011 provides test methods and procedures to determine the corrosion behaviour of metallic materials used in the oral cavity. It is intended that the test methods and procedures in ISO 10271:2011 be referred to in the individual International Standards specifying such metallic materials.
ISO 10271:2011 is not applicable to instruments and dental amalgam and appliances for orthodontics.
Zahnheilkunde - Korrosionsprüfverfahren für metallische Werkstoffe (ISO 10271:2011)
Diese Internationale Norm legt Prüfverfahren und Prüfpläne zur Bestimmung des Korrosionsverhaltens metallischer
Werkstoffe fest, die in der Mundhöhle verwendet werden. Es ist vorgesehen, dass auf die
Prüfverfahren und Prüfpläne, die in dieser Internationalen Norm beschreiben werden, in den jeweiligen
internationalen Normen für metallische Werkstoffe, verwiesen wird.
Diese Internationale Norm ist nicht anwendbar auf Instrumente und zahnärztliches Amalgam sowie auf
kieferorthopädische Apparaturen.
Médecine bucco-dentaire - Méthodes d'essai de corrosion des matériaux métalliques (ISO 10271:2011)
L'ISO 10271:2011 spécifie des méthodes et des protocoles d'essai permettant de déterminer le comportement à la corrosion des produits métalliques utilisés dans la cavité buccale.
L'ISO 10271:2011 ne s'applique pas aux instruments, aux amalgames dentaires ni aux applications d'orthodontie.
Zobozdravstvo - Preskusne metode ugotavljanja korozije za kovinske materiale (ISO 10271:2011)
Ta mednarodni standard podaja preskusne metode in postopke za ugotavljanje korozijskih lastnosti kovinskih materialov, ki se uporabljajo v ustni votlini. Predvideva se, da se posamezni mednarodni standardi, ki določajo take kovinske materiale, sklicujejo na preskusne metode in postopke iz tega mednarodnega standarda. Ta mednarodni standard ne velja za instrumente, zobni amalgam in ortodontske naprave.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Zobozdravstvo - Preskusne metode ugotavljanja korozije za kovinske materiale (ISO 10271:2011)Zahnheilkunde - Korrosionsprüfverfahren für metallische Werkstoffe (ISO 10271:2011)Médecine bucco-dentaire - Méthodes d'essai de corrosion des matériaux métalliques (ISO 10271:2011)Dentistry - Corrosion test methods for metallic materials (ISO 10271:2011)11.060.10Dental materialsICS:Ta slovenski standard je istoveten z:EN ISO 10271:2011SIST EN ISO 10271:2011en,fr,de01-december-2011SIST EN ISO 10271:2011SLOVENSKI
STANDARDSIST EN ISO 10271:2002/AC:2006SIST EN ISO 10271:20021DGRPHãþD
SIST EN ISO 10271:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN ISO 10271
August 2011 ICS 11.060.10 Supersedes EN ISO 10271:2001English Version
Dentistry - Corrosion test methods for metallic materials (ISO 10271:2011)
Médecine bucco-dentaire - Méthodes d'essai de corrosion des matériaux métalliques (ISO 10271:2011)
Zahnheilkunde - Korrosionsprüfverfahren für metallische Werkstoffe (ISO 10271:2011) This European Standard was approved by CEN on 29 July 2011.
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 CEN-CENELEC 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 CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 10271:2011: ESIST EN ISO 10271:2011
EN ISO 10271:2011 (E) 2 Contents Page Foreword .3 SIST EN ISO 10271:2011
EN ISO 10271:2011 (E) 3 Foreword This document (EN ISO 10271:2011) has been prepared by Technical Committee ISO/TC 106 "Dentistry" in collaboration with Technical Committee CEN/TC 55 “Dentistry”, the secretariat of which is held by DIN. 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 February 2012, and conflicting national standards shall be withdrawn at the latest by February 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 10271:2001. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 10271:2011 has been approved by CEN as a EN ISO 10271:2011 without any modification.
SIST EN ISO 10271:2011
SIST EN ISO 10271:2011
Reference numberISO 10271:2011(E)© ISO 2011
INTERNATIONAL STANDARD ISO10271Second edition2011-08-01Dentistry — Corrosion test methods for metallic materials Médecine bucco-dentaire — Méthodes d'essai de corrosion des matériaux métalliques
SIST EN ISO 10271:2011
ISO 10271:2011(E)
COPYRIGHT PROTECTED DOCUMENT
©
ISO 2011 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 2011 – All rights reserved
SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved iii Contents Page Foreword.iv Introduction.v 1 Scope.1 2 Normative references.1 3 Terms and definitions.1 4 Test methods.3 4.1 Static immersion test.3 4.2 Electrochemical test.6 4.3 Sulfide tarnish test (cyclic immersion).12 4.4 Sulfide tarnish test (static immersion).14 4.5 Static immersion test with periodic analysis.16 Annex A (informative)
Corrosion test method development.20 Bibliography.26
SIST EN ISO 10271:2011
ISO 10271:2011(E) iv © ISO 2011 – 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 10271 was prepared by Technical Committee ISO/TC 106, Dentistry, Subcommittee SC 2, Prosthodontic materials. This second edition cancels and replaces the first edition (ISO 10271:2001), which has been technically revised, in particular by the inclusion of two additional test methods. It also incorporates Technical Corrigendum ISO 10271:2001/Cor.1:2005. SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved v Introduction This International Standard was developed from the original Technical Report (ISO/TR 10271) as a result of worldwide demand for standard test methods to determine acceptability of metallic materials for oral restorations in relation to corrosion. Specific qualitative and quantitative requirements for freedom from biological hazard are not included in this International Standard, but it is recommended that reference be made to ISO 10993-1 and ISO 7405 for assessing possible biological or toxicological hazards. The testing of the corrosion behavior of metallic materials in dentistry is complicated by the diversity of the materials themselves, their applications and the environment to which they are exposed. Variation occurs between devices and within the same device during the exposure time. The type of corrosion behavior or effect can also vary with exposure time. Accordingly, it is not possible to specify a single test capable of covering all situations, nor is it a practical proposition to define a test for each situation. This International Standard, therefore, gives detailed procedures for test methods that have been found to be of merit as evidenced by considerable use. This second edition differs from the first edition by the addition of two new test methods. To supplement the existing static immersion test, a static immersion test with periodic analysis has been added. A major reason for the addition of this test is that the rate of corrosion of most dental metallic materials varies over time. Thus, the aim of this supplementary test is to provide information on this variation in the corrosion of a dental metallic material. A classification scheme to interpret the rate of corrosion of a tested material with time (i.e. steady, decreasing, increasing) was not included as part of the static immersion test with periodic analysis. It is intended to monitor the use of the test through appropriate working groups of ISO/TC 106 to ascertain whether a classification scheme is needed in a future revision of this International Standard. To supplement the sulfide tarnish test (cyclic immersion), a sulfide tarnish test (static immersion) has also been added to this second edition of ISO 10271. This test has been used successfully for many years to evaluate the corrosion of silver alloys. In addition, an informative annex (Annex A) is provided that sets out a procedure for each element of the test system such that a consistent approach can be taken for the development of further test methods. Equally, it is recognized that any element can represent only the current recommendation, but changes in the future are unlikely to change the framework. It is not the purpose of this International Standard to propose corrosion test methods for specific applications or to set limits as precise as those in the standard relating to the type of product and its application. SIST EN ISO 10271:2011
SIST EN ISO 10271:2011
INTERNATIONAL STANDARD ISO 10271:2011(E) © ISO 2011 – All rights reserved 1 Dentistry — Corrosion test methods for metallic materials 1 Scope This International Standard provides test methods and procedures to determine the corrosion behavior of metallic materials used in the oral cavity. It is intended that the test methods and procedures in this International Standard be referred to in the individual International Standards specifying such metallic materials. This International Standard is not applicable to instruments and dental amalgam and appliances for orthodontics. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1042, Laboratory glassware — One-mark volumetric flasks ISO 1942, Dentistry — Vocabulary ISO 3585, Borosilicate glass 3.3 — Properties ISO 3696, Water for analytical laboratory use — Specification and test methods ISO 6344-1, Coated abrasives — Grain size analysis — Part 1: Grain size distribution test ISO 7183, Compressed-air dryers — Specifications and testing 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 1942 and the following apply. 3.1 breakdown potential Ep least noble potential at which pitting or crevice corrosion, or both, initiates and propagates 3.2 corrosion physicochemical interaction between a metallic material and its environment that results in a partial or total destruction of the material or in a change of its properties SIST EN ISO 10271:2011
ISO 10271:2011(E) 2 © ISO 2011 – All rights reserved 3.3 corrosion potential Ecorr open-circuit potential measured under either service conditions, or laboratory conditions that closely approximate service conditions 3.4 corrosion product substance formed as a result of corrosion 3.5 crevice corrosion corrosion associated with and taking place in or near a narrow aperture or crevice 3.6 current density value of electric current per unit surface area flowing through a conductor 3.7 dynamic immersion test test in which the sample is exposed to a corrosive solution under conditions of relative motion between sample and solution 3.8 electrode potential potential difference between the sample and a reference electrode 3.9 electrolyte solution or liquid that conducts an electrical current by means of ions 3.10 open-circuit potential Eocp potential of an electrode measured with respect to a reference electrode or another electrode when no current flows 3.11 pitting corrosion localized corrosion which results in pits 3.12 potentiodynamic test test in which the electrode potential is varied at a preprogrammed rate and the relationship between current density and electrode potential is recorded 3.13 potentiostatic test test in which the electrode potential is maintained constant 3.14 sample totality of material for one type being tested, the group of all such specimens 3.15 set subgroup of the specimens of a sample SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved 3 3.16 specimen individual single example of an object for testing 3.17 static immersion test test in which the sample is exposed to a corrosive solution under conditions of effectively no relative motion between sample and solution 3.18 stress corrosion corrosion resulting from the combined action of static tensile stress and an electrolyte 3.19 synthetic saliva test medium that simulates the chemistry of natural saliva 3.20 tarnish surface discoloration due to the chemical reaction between a metallic material and its environment 3.21 zero-current potential potential at which cathodic and anodic currents are equal 4 Test methods 4.1 Static immersion test 4.1.1 Information required Composition, including hazardous elements, in accordance with the appropriate ISO standard is required. 4.1.2 Application This is an accelerated test that is intended to provide quantitative data on the metallic ion released from metallic materials under in vitro conditions relevant to those expected in the oral cavity. 4.1.3 Reagents 4.1.3.1 Lactic acid (C3H6O3), 90 %, analytical grade. 4.1.3.2 Sodium chloride (NaCl), analytical grade. 4.1.3.3 Water, complying with grade 2 of ISO 3696. 4.1.3.4 Ethanol or methanol (C2H5OH or CH3OH), analytical grade. 4.1.3.5 Compressed air, oil- and water-free, complying with ISO 7183. 4.1.4 Apparatus 4.1.4.1 Containers, of borosilicate glass, complying with ISO 3585 and with dimensions of approximately 16 mm inner diameter by 160 mm in height. 4.1.4.2 pH meter, with a sensitivity of at least ±0,05 pH units. SIST EN ISO 10271:2011
ISO 10271:2011(E) 4 © ISO 2011 – All rights reserved 4.1.4.3 Chemical analysis instrumentation, capable of measuring ion concentration in µg/ml (e.g. ICP and AAS). 4.1.4.4 Micrometer gauge, accurate to 0,01 mm. 4.1.4.5 Silicon carbide paper, complying with ISO 6344-1. 4.1.4.6 Volumetric flasks, of borosilicate glass, 1 000 ml, class A, complying with ISO 1042. 4.1.5 Solution preparation Prepare an aqueous solution comprising 0,1 mol/l lactic acid and 0,1 mol/l sodium chloride immediately before use. For example, dissolve (10,0 ± 0,1) g 90 % C3H6O3 (4.1.3.1) and (5,85 ± 0,005) g NaCl (4.1.3.2) in approximately 300 ml of water (4.1.3.3). Transfer into a 1 000 ml volumetric flask (4.1.4.6) and fill to mark. The pH shall be 2,3 ± 0,1. If not, the solution shall be discarded and reagents checked. 4.1.6 Samples 4.1.6.1 Fabrication 4.1.6.1.1 Cast Specimens shall be cast in accordance with the manufacturer's recommendations. 4.1.6.1.2 Prefabricated Prefabricated parts/devices shall be used in the as-received condition. 4.1.6.1.3 Other Specimens prepared by other methods, e.g. machined, sintered, eroded, etc., shall be tested in the as-manufactured condition after suitable cleaning. 4.1.6.2 Sampling The number of specimens shall be sufficient to provide at least two parallel sets. (The number of specimens in a set may vary.) 4.1.6.3 Sample surface area The total surface area of the sample shall be at least 10 cm2 after preparation. 4.1.6.4 Preparation 4.1.6.4.1 Cast samples Remove any sprues, runners or other projections from surface. Blast surfaces with 125 µm pure alumina to remove investment. If recommended, heat-treat according to the manufacturer's instructions. In the case of metal-ceramic materials, heat-treat for 10 min at the highest firing temperature recommended by the metallic material manufacturer and bench cool. Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.1.4.4)], from each surface using standard metallographic procedures unless specimens are being tested in the as-received SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved 5 condition. Use fresh abrasive paper for each metallic material. Finish with P1200 wet silicon carbide paper (4.1.4.5). If the described procedure is not applicable, treat the surfaces according to the manufacturer's instructions for clinical use.
Determine each sample surface area to the nearest 1 %. Clean surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4). Rinse with water (4.1.3.3). Dry with oil- and water-free compressed air (4.1.3.5). If a specimen contains any porosity visible on the surfaces being exposed to the solution, the specimen shall be rejected and replaced with a new one. 4.1.6.4.2 Machined, sintered, eroded or electroformed samples Heat-treat the specimens if recommended. Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.1.4.4)], from each surface using standard metallographic procedures unless specimens are being tested in the as-received condition. Use fresh abrasive paper for each metallic material. Finish with P1200 wet silicon carbide paper (4.1.4.5). Determine each sample surface area to within ±0,1 cm2. Clean surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4). Rinse with water (4.1.3.3). Dry with oil- and water-free compressed air (4.1.3.5). 4.1.6.4.3 Prefabricated parts/devices Treat the surfaces according to the manufacturer's instructions for clinical use. Determine each sample surface area to within ±0,1 cm2. Clean the surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4). Rinse with water (4.1.3.3). Dry with oil- and water-free compressed air (4.1.3.5). 4.1.7 Test procedure Parallel specimen sets shall be treated in identical fashion. If a set consists of one specimen, it shall be placed in a container (4.1.4.1) such that it does not touch the container surface except in a minimum support line or point. If a set consists of two or more specimens, they may be placed in the same or a number of separate containers, but if more than one is placed in a container they shall not touch. Record the pH of the solution. Add the solution to each container sufficient to produce a ratio of 1 ml of solution per 1 cm2 of sample surface area. The specimens shall be covered completely by the solution. Record the volume of solution to an accuracy of 0,1 ml. Close the container to prevent evaporation of the solution. Maintain at (37 ± 1) °C for 7 d ± 1 h. Remove the specimens and record the pH of the residual solution. Use an additional container (4.1.4.1) to hold a reference solution to be maintained in parallel with the solutions containing the specimens. The reference solution shall be used to establish the impurity level for each element of interest in the solution. Add approximately the same volume of solution as used for the solutions containing the specimens and record the volume to an accuracy of 0,1 ml. Close the container to prevent evaporation of the solution and maintain at (37 ± 1 ) °C for the same time period as the solutions containing the specimens. SIST EN ISO 10271:2011
ISO 10271:2011(E) 6 © ISO 2011 – All rights reserved 4.1.8 Elemental analysis Use chemical analysis instrumentation (4.1.4.3) of adequate sensitivity. Analyze the solution qualitatively and quantitatively. Emphasis shall be on those elements indicated in 4.1.1, but if impurities are found in a concentration greater than 0,1 %, they shall also be reported. For each element of interest, subtract the value obtained for the element in the reference solution from the value obtained in the test solution. The elements boron, carbon, and nitrogen shall be disregarded. 4.1.9 Test report The test report shall contain the following information. a) Report the method of analysis and detection limits of all the analyzed elements. b) Report and justify any deviations from preparation of specimens (see 4.1.6.4) or test procedure (see 4.1.7). c) Report the number of specimens making up a set and the number of sets tested (see 4.1.6.2). d) From the elemental analysis of the corrosion solution (see 4.1.8), calculate and report the ion release for each element of each set (see 4.1.6.2) separately in µg/cm2/7 d. The elements indicated in 4.1.1 shall be reported as well as any others found. From this information, sum the ion release values for all the elements of each set to obtain the total metal ion release for the dental material. Average the results by dividing by the number of sets tested and report as the average total ion release for the dental material in µg/cm2/7 d. e) Report undissolved corrosion product like precipitates and discoloration of the specimen surface. 4.2 Electrochemical test 4.2.1 Information required Composition, including hazardous elements, in accordance with the appropriate material standard is required. 4.2.2 Application This test is intended to assess the corrosion susceptibility of metallic materials used in the oral cavity using potentiodynamic polarization. 4.2.3 Reagents 4.2.3.1 Lactic acid (C3H6O3), 90 %, chemically pure. 4.2.3.2 Sodium chloride (NaCl), analytical grade. 4.2.3.3 Sodium hydroxide (NaOH), analytical grade. 4.2.3.4 Water, complying with grade 2 of ISO 3696. 4.2.3.5 Argon or nitrogen gas, with a minimum purity of 99,99 %. 4.2.3.6 Ethanol or methanol (C2H5OH or CH3OH), analytical grade. 4.2.3.7 Acetone (C3H6O), analytical grade. SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved 7 4.2.4 Apparatus 4.2.4.1 Test cell, temperature-controlled, of borosilicate glass, complying with ISO 3585 [a double-walled cell is unnecessary if the test is carried out at (23 ± 2) °C]. 4.2.4.2 Scanning potentiostat, potential range ±1 600 mV, current output range 10–9 A to 10–1 A. 4.2.4.3 Potential measuring instrument, with input impedance > 1011 W and sensitivity/accuracy able to detect a change of 1 mV over a potential change of ±1 600 mV. 4.2.4.4 Current-measuring instrument, capable of measuring a current to within 1 % of the absolute value over a current range between 10–9 A and 10–1 A. 4.2.4.5 Working electrode (specimen holder). 4.2.4.6 Counter electrode(s), composed of high-purity vitreous carbon or platinum. 4.2.4.7 Reference electrode, either saturated calomel electrode (SCE) or Ag/AgCl electrode [saturated silver chloride electrode (SSE)]. 4.2.4.8 pH meter, with a sensitivity of ±0,05 pH units. 4.2.4.9 Silicon carbide paper, complying with ISO 6344-1. 4.2.4.10 Diamond paste,1 µm. 4.2.4.11 Micrometer gauge, accurate to 0,01 mm. 4.2.4.12 Light microscope, minimum magnification of ¥50. 4.2.5 Solution preparation Dissolve 9,0 g NaCl (4.2.3.2) in approximately 950 ml water (4.2.3.4). Adjust to pH 7,4 ± 0,1 using 1 % C3H6O3 (4.2.3.1) or 4 % NaOH (4.2.3.3). Dilute with water to 1 000 ml. 4.2.6 Samples 4.2.6.1 Fabrication 4.2.6.1.1 Cast Specimens shall be cast in accordance with the manufacturer's recommendations. 4.2.6.1.2 Prefabricated Prefabricated parts/devices shall be used in the as-received condition. 4.2.6.1.3 Other Specimens prepared by other methods, e.g. machined, sintered, eroded, etc., shall be tested in the as-manufactured condition after suitable cleaning. 4.2.6.2 Sampling At least four specimens shall be tested. SIST EN ISO 10271:2011
ISO 10271:2011(E) 8 © ISO 2011 – All rights reserved 4.2.6.3 Sample surface area The surface area of each specimen shall be not less than 0,1 cm2 after preparation. 4.2.6.4 Preparation Remove any sprues, runners or other projections from surface. Blast surfaces with 125 µm pure alumina to remove investment. If recommended, heat-treat according to the manufacturer's instructions. In the case of metal-ceramic materials, heat-treat for 10 min at the highest firing temperature recommended by the metallic material manufacturer and bench cool. Specimens shall be prepared with one flat surface exposed. A suitable contact shall be provided for connection to the electrochemical apparatus. The working electrode shall be prepared in a way that ensures the absence of crevices. The recommended procedure is that of embedding in epoxy resin that does not exhibit loss of electrical insulation during immersion. Instead of embedding, a specimen holder (4.2.4.5) may be used if the absence of crevices is confirmed by specimen examination after the test. Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.2.4.11)], from each free surface using standard metallographic procedures unless specimens are being tested in the as-received condition. Use fresh abrasive paper for each metallic material. Finish with P1200 wet silicon carbide paper (4.2.4.9) and end with 1 µm diamond paste (4.2.4.10). If the described procedure is not applicable, treat the surfaces according to the manufacturer's instructions for clinical use. Examine with a light microscope at ¥50 (4.2.4.12) for cracks or crevices at the specimen/resin interface. Replace the specimen if any cracks or crevices are found. Determine the area exposed to solution of each specimen to within 0,01 cm2. Manually clean surface with acetone (4.2.3.7). Clean surfaces ultrasonically in the following sequence: alcohol (4.2.3.6) and water (4.2.3.4) for 2 min each. Store in water (4.2.3.4) until transferred to test cell. 4.2.7 Test procedure 4.2.7.1 Test set-up An example of an electrochemical measuring circuit is shown in Figure 1. An example of an electrolytic cell is shown in Figure 2. Fill test cell with electrolyte. Test at room temperature (23 ± 2) °C. If there is a phase transition between room temperature and 37 °C, then a test temperature of (37 ± 1) °C shall be used. Place counter electrode(s) in the test cell followed by the reference electrode. Then place the working electrode in the test cell without immersion. Activate the magnetic stirrer. Bubble oxygen-free nitrogen or argon at a rate of about 100 cm3/min through the electrolyte for at least 30 min. Immerse the working electrode in the electrolyte. Adjust the reference electrode. Adjust gas flow-rate to give a slight bubbling. Begin measurement procedure.
SIST EN ISO 10271:2011
ISO 10271:2011(E) © ISO 2011 – All rights reserved 9 Key 1 potentiostat 2 counter electrode 3 reference electrode 4 working electrode
a Current measurement. b Potential measurement. Figure 1 — Schematic diagram of measuring circuit
Key 1 thermometer 5 reference electrode [saturated calomel electrode (SCE)] 9 magnetic agitator (motor) 2 counter electrode 6 saturated solution of KCl 10 double-walled vessel 3 working electrode 7 Luggin capillary 11 electrolyte 4 electrolytic bridge 8 magnetic stirrer (PTFE-coated) 12 bubbler (using nitrogen) a Gas outlet. b Water inlet. c Water outlet. Figure 2 — Schematic diagram of electrolytic cell SIST EN ISO 10271:2011
ISO 10271:2011(E) 10 © ISO 2011 – All rights reserved 4.2.7.2 Open-circuit potential measurement Record the open-circuit potential versus time curve for 2 h. Determine the open-circuit potential (Eocp) in mV (SCE) after immersion for 2 h ± 6 min. An example of a potential versus time curve is shown in Figure 3. 4.2.7.3 Potential measurements (anodic polarization) Start the potentiodynamic scan 5 min after finishing the open-circuit potential measurement at Eocp minus 150 mV. The potentiodynamic sweep rate should be 1 mV/s up to a current density threshold two decades greater than the current density recorded at breakdown
...
SLOVENSKI STANDARD
oSIST prEN ISO 10271:2009
01-september-2009
Dentalni kovinski materiali - Preskusne metode ugotavljanja korozije (ISO/FDIS
10271:2009)
Dental metallic materials - Corrosion test methods (ISO/FDIS 10271:2009)
Zahnheilkunde - Korrosionsprüfverfahren (ISO/FDIS 10271:2009)
Produits dentaires métalliques - Méthodes pour les essais de corrosion (ISO/FDIS
10271:2009)
Ta slovenski standard je istoveten z: prEN ISO 10271
ICS:
11.060.10 =RERWHKQLþQLPDWHULDOL Dental materials
oSIST prEN ISO 10271:2009 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 10271:2009
---------------------- Page: 2 ----------------------
oSIST prEN ISO 10271:2009
EUROPEAN STANDARD
DRAFT
prEN ISO 10271
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2009
ICS 11.060.10 Will supersede EN ISO 10271:2001
English Version
Dental metallic materials - Corrosion test methods (ISO/FDIS
10271:2009)
Produits dentaires métalliques - Méthodes pour les essais Zahnheilkunde - Korrosionsprüfverfahren (ISO/FDIS
de corrosion (ISO/FDIS 10271:2009) 10271:2009)
This draft European Standard is submitted to CEN members for parallel enquiry. It has been drawn up by the Technical Committee
CEN/TC 55.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 CEN Management Centre has the
same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN ISO 10271:2009: E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN ISO 10271:2009
prEN ISO 10271:2009 (E)
Contents Page
Foreword .3
2
---------------------- Page: 4 ----------------------
oSIST prEN ISO 10271:2009
prEN ISO 10271:2009 (E)
Foreword
This document (prEN ISO 10271:2009) has been prepared by Technical Committee ISO/TC 106 "Dentistry" in
collaboration with Technical Committee CEN/TC 55 “Dentistry”, the secretariat of which is held by DIN.
This document is currently submitted to the parallel Enquiry.
This document will supersede EN ISO 10271:2001.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association, and supports essential requirements of EC Directive(s).
Endorsement notice
The text of ISO/DIS 10271:2009 has been approved by CEN as a prEN ISO 10271:2009 without any
modification.
3
---------------------- Page: 5 ----------------------
oSIST prEN ISO 10271:2009
---------------------- Page: 6 ----------------------
oSIST prEN ISO 10271:2009
DRAFT INTERNATIONAL STANDARD ISO/DIS 10271
ISO/TC 106/SC 2 Secretariat: ANSI
Voting begins on: Voting terminates on:
2009-05-07 2009-10-07
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION
Dental metallic materials — Corrosion test methods
Produits dentaires métalliques — Méthodes pour les essais de corrosion
[Revision of first edition (ISO 10271:2001) and ISO 10271:2001/Cor.1:2005]
ICS 11.060.10
ISO/CEN PARALLEL PROCESSING
This draft has been developed within the International Organization for Standardization (ISO), and
processed under the ISO-lead mode of collaboration as defined in the Vienna Agreement.
This draft is hereby submitted to the ISO member bodies and to the CEN member bodies for a parallel
five-month enquiry.
Should this draft be accepted, a final draft, established on the basis of comments received, will be
submitted to a parallel two-month approval vote in ISO and formal vote in CEN.
To expedite distribution, this document is circulated as received from the committee secretariat.
ISO Central Secretariat work of editing and text composition will be undertaken at publication
stage.
Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du
secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au
Secrétariat central de l'ISO au stade de publication.
THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS.
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
©
International Organization for Standardization, 2009
---------------------- Page: 7 ----------------------
oSIST prEN ISO 10271:2009
ISO/DIS 10271
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 notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as permitted
under the applicable laws of the user's country, neither this ISO draft nor any extract from it may be
reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, photocopying,
recording or otherwise, without prior written permission being secured.
Requests for permission to reproduce should be addressed to 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
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
©
ii ISO 2009 – All rights reserved
---------------------- Page: 8 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Test methods . 3
Annex A (informative) Corrosion test method development . 20
Bibliography . 26
© ISO 2009 – All rights reserved iii
---------------------- Page: 9 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
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 10271 was prepared by Technical Committee ISO/TC 106, Dentistry, Subcommittee
SC 2, Prosthodontic materials.
This second edition cancels and replaces the first edition ISO 10271:2001 which has been technically revised, in
particular by the inclusion of two additional test methods.
Annex A of this International Standard is for information only.
iv © ISO 2009 – All rights reserved
---------------------- Page: 10 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
Introduction
ISO 10271 was developed from the original Technical Report (ISO/TR 10271) as a result of worldwide demand for
standard test methods to determine acceptability of metallic materials for oral restorations in relation to corrosion.
Specific qualitative and quantitative requirements for freedom from biological hazard are not included in this
international Standard, but it is recommended that in assessing possible biological or toxicological hazards,
reference should be made to ISO 10993-1 and ISO 7405.
The testing of the corrosion behaviour of metallic materials in dentistry is complicated by the diversity of the
materials themselves, their applications and the environment to which they are exposed. Variation occurs between
devices and within the same device during the exposure time. The type of corrosion behaviour or effect may also
vary with exposure time. Accordingly, it is not possible to specify a single test capable of covering all situations, nor
is it a practical proposition to define a test for each situation. This International Standard therefore gives detailed
protocols for test methods which have been found to be of merit as evidenced by considerable use.
This second edition differs from the first edition by the addition of two new test methods. A time-dependence
corrosion test has been added to supplement the existing static immersion test. A major reason for this test is that
the corrosion rate of most dental alloys is not constant over time. Thus, the aim of the time-dependence corrosion
test is to provide information on the corrosion rate of a dental alloy with time. An evaluation section to interpret the
long term corrosion behaviour of the tested alloys (i.e., steady, decreasing, increasing) was not included as part of
the time-dependence corrosion test. Instead, the data will be reported in a graph without attempting to interpret the
shape of the resulting curve. It is intended that ISO/TC 106/SC 2/WG 12 monitor the use of the time-dependence
corrosion test through the appropriate working groups in ISO/TC 106 and make any necessary changes to the
document in a future revision. To supplement the sulphide tarnish test (cyclic immersion), a sulfide tarnish test
(static immersion) has also been added to this second edition of ISO 10271. This test has been successfully used
for many years to evaluate the corrosion of silver alloys.
In addition, an informative annex (annex A) is provided that sets out a protocol for each element of the test system
such that a consistent approach may be taken for the development of further test methods. Equally, it is recognized
that any element can only represent the current recommendation, but changes in the future are unlikely to change
the framework
It is not the purpose of this International Standard to propose corrosion test methods for specific applications or to
set limits as precise as those in the standard relating to the type of product and its application.
© ISO 2009 – All rights reserved v
---------------------- Page: 11 ----------------------
oSIST prEN ISO 10271:2009
---------------------- Page: 12 ----------------------
oSIST prEN ISO 10271:2009
DRAFT INTERNATIONAL STANDARD ISO/DIS 10271
Dental metallic materials — Corrosion test methods
1 Scope
This international standard provides test methods and protocols to determine the corrosion behaviour of metallic
materials used in the oral cavity. It is intended that the test methods and protocols in this international standard be
referred to in the individual international standards specifying such metallic materials.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references,
only the edition cited applies. For undated references, the latest editions of the referenced documents, including
any amendments, applies.
ISO 3585, Borosilicate glass 3.3 — Properties.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 7183-2:1996, Compressed air dryers — Part 2: Performance ratings.
ISO 6344-1:1998, Coated abrasives – Grain size analysis - Part 1: Definitions and grain sized distribution test.
ISO 1942, Dentistry – Vocabulary.
3 Terms and definitions
For the purposes of this International Standard, the terms and definitions given in ISO 1942 and the following
apply.
3.1
breakdown potential
E
p
least noble potential at which pitting or crevice corrosion, or both, will initiate and propagate
3.2
corrosion
physicochemical interaction between a metallic material and its environment that results in a partial or total
destruction of the material or in a change of its properties
3.3
corrosion potential
E
corr
open-circuit potential measured under either service conditions, or laboratory conditions that closely approximate to
service conditions
3.4
corrosion product
substance formed as a result of corrosion
3.5
crevice corrosion
corrosion associated with and taking place in or near a narrow aperture or crevice
© ISO 2009 – All rights reserved 1
---------------------- Page: 13 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
3.6
current density
value of electric current per unit surface area flowing through a conductor
3.7
dynamic immersion test
test in which the sample is exposed to a corrosive solution under conditions of relative motion between sample and
solution
3.8
electrochemical corrosion
degradation occurring in an electrolyte as a result of electrochemical reactions
3.9
electrode potential
potential difference between the sample and a reference electrode
3.10
electrolyte
solution or liquid which will conduct an electrical current by means of ions
3.11
open-circuit potential
E
ocp
potential of an electrode measured with respect to a reference electrode or another electrode when no current
flows
3.12
pitting corrosion
localized corrosion which results in pits
3.13
potentiodynamic test
test in which the electrode potential is varied at a pre-programmed rate and the relationship between current
density and electrode potential is recorded
3.14
potentiostatic test
test in which the electrode potential is maintained constant
3.15
sample
the totality of material for one type to be tested, the group of all such specimens
3.16
set
a subgroup of the specimens of a sample
3.17
specimen
an individual single example of an object for testing
3.18
static immersion test
test in which the sample is exposed to a corrosive solution under conditions of effectively no relative motion
between sample and solution
2 © ISO 2009 – All rights reserved
---------------------- Page: 14 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
3.19
stress corrosion
corrosion resulting from the combined action of static tensile stress and an electrolyte
3.20
synthetic saliva
test medium that simulates natural saliva
3.21
tarnish
surface discolouration due to the chemical reaction between a metallic material and its environment
3.22
zero-current potential
potential at which cathodic and anodic currents are equal
4 Test methods
4.1 Static immersion test
4.1.1 Information required
Composition, including hazardous elements, in accordance with the appropriate ISO material standard is required.
4.1.2 Application
This test is intended to provide quantitative data on the metallic ion released from metallic materials under in vitro
conditions relevant to but more aggressive than those expected in the oral cavity.
4.1.3 Reagents
4.1.3.1 Lactic acid (C H O ), 90 %, analytical grade.
3 6 3
4.1.3.2 Sodium chloride (NaCl), analytical grade.
4.1.3.3 Water, complying with grade 2 of ISO 3696:1987.
4.1.3.4 Ethanol or methanol (C H OH or CH OH), analytical grade.
2 5 3
4.1.3.5 Oil- and water-free compressed air, complying with ISO 7183.
4.1.4 Apparatus
4.1.4.1 Borosilicate glass containers, complying with ISO 3585 and with dimensions of approximately 16
mm inner diameter by 160 mm in height.
4.1.4.2 pH meter, the sensitivity of the pH meter should be at least ±0,05 pH units.
4.1.4.3 Chemical analysis instrumentation, capable of measuring ion concentration in g/ml (e.g., ICP and
AAS).
4.1.4.4 Micrometer gauge, accurate to 0,01 mm.
4.1.4.5 Silicon carbide paper, complying with ISO 6344-1:1998
© ISO 2009 – All rights reserved 3
---------------------- Page: 15 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
4.1.5 Solution preparation
Prepare an aqueous solution comprising 0,1 mol/l lactic acid and 0,1 mol/l sodium chloride immediately before use.
For example, dissolve 10,0 0,1 g 90 % C H O (4.1.3.1) and 5,85 0,005 g NaCl (4.1.3.2) in approximately
3 6 3
300 ml of water (4.1.3.3). Dilute to 1 000 10 ml with water. The pH shall be 2,3 0,1. If not, the solution shall be
discarded and reagents checked.
4.1.6 Samples
4.1.6.1 Fabrication
4.1.6.1.1 Casting alloys
Specimens shall be cast in accordance with the manufacturer's recommendations.
4.1.6.1.2 Prefabricated
Prefabricated parts/devices shall be used in the as-received condition.
4.1.6.1.3 Other
Specimens prepared by other methods, e.g. machined, sintered, eroded, etc., shall be tested in the as-
manufactured condition after suitable cleaning.
4.1.6.2 Sampling
The number of specimens shall be sufficient to provide at least two parallel sets. (The number of specimens in a
set can vary.)
4.1.6.3 Sample surface area
2
The total surface area of the sample shall be at least 10 cm after preparation.
4.1.6.4 Preparation
4.1.6.4.1 Cast samples
Remove any sprues, runners or other projections from specimen surface. Blast surfaces with 125 m pure alumina
to remove investment.
If recommended, heat-treat casting alloys following the manufacturer's instructions. Heat-treat all metal-ceramic
alloys for 10 min in air at the highest temperature recommended by the alloy manufacturer and bench cool.
Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.1.4.4)], from each
surface using standard metallographic procedures unless specimens are to be tested in the as-received condition.
Use fresh abrasive paper for each alloy. Finish with P1200 wet silicon carbide paper (4.1.4.5). If the described
procedure is not applicable, treat the surfaces according to the manufacturer’s instructions for clinical use.
Determine each sample surface area to the nearest 1 %.
Clean surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4). Rinse with water (4.1.3.3). Dry with oil- and
water-free compressed air (4.1.3.5).
If a specimen contains any unexpected porosity visible on the surfaces to be exposed to the solution, the specimen
must be rejected and replaced with a new one.
4.1.6.4.2 Machined, sintered, eroded or electroformed samples
Heat-treat the specimens if recommended.
4 © ISO 2009 – All rights reserved
---------------------- Page: 16 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.1.4.4)], from each
surface using standard metallographic procedures unless specimens are to be tested in the as-received condition.
If the specimens are prefabricated parts, these shall be tested in the as-received condition. Use fresh abrasive
paper for each alloy. Finish with P1200 wet silicon carbide paper (4.1.4.5).
2
Determine each sample surface area to within 0,1 cm .
Clean surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4).
Rinse with water (4.1.3.3). Dry with oil- and water-free compressed air (4.1.3.5).
4.1.6.4.3 Prefabricated parts/devices
Treat the surfaces according to the manufacturer’s instructions for clinical use.
2
Determine each sample surface area to within 0,1 cm .
Clean the surfaces ultrasonically for 2 min in ethanol or methanol (4.1.3.4).
Rinse with water (4.1.3.3). Dry with oil- and water-free compressed air (4.1.3.5).
4.1.7 Test procedure
Parallel specimen sets shall be treated in identical fashion. If a set consists of one specimen, it shall be placed in a
container (4.1.4.1) such that it does not touch the container surface except in a minimum support line or point. If a
set consists of two or more specimens, they may be placed in the same or a number of separate containers, but if
more than one is placed in a container they shall not touch.
Record the pH of the solution. Add the solution to each container sufficient to produce a ratio of 1 ml of solution
2
per 1 cm of sample surface area. The specimens shall be covered completely by the solution. Record the volume
of solution to an accuracy of 0,1 ml. Close the container to prevent evaporation of the solution. Maintain at (37 1)
°C for 7 d 1 h. Remove the specimens and record the pH of the residual solution.
Use an additional container (4.1.4.1) to hold a reference solution to be maintained in parallel with the solutions
containing the specimens. The reference solution shall be used to establish the impurity level for each element of
interest in the solution. Add approximately the same volume of solution as used for the solutions containing the
specimens and record the volume to an accuracy of 0,1 ml. Close the container to prevent evaporation of the
solution and maintain at (37 1) °C for the same time period as the solutions containing the specimens.
4.1.8 Elemental analysis
Use chemical analysis instrumentation (4.1.4.3) of adequate sensitivity. Analyse the solution qualitatively and
quantitatively. Emphasis shall be on those elements listed in (4.1.1), but if impurities are found in a concentration
greater than 0,1 %, they shall also be reported. For each element of interest, subtract the value obtained for the
element in the reference solution from the value obtained in the test solution. Elements such as Boron, Carbon, or
Nitrogen should be disregarded.
4.1.9 Test report
The test report shall contain the following information:
a) report the method of analysis and detection limits of all the analyzed elements;
b) report and justify any deviations from preparation of specimens (4.1.6.4) or test procedure (4.1.7);
c) report the number of specimens making up a sample;
2
d) report each element of each test separately in g/cm 7 days.
e) each element listed in accordance with 4.1.1 shall be reported as well as any others found.
© ISO 2009 – All rights reserved 5
---------------------- Page: 17 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
4.2 Electrochemical test
4.2.1 Information required
Composition, including hazardous elements, in accordance with the appropriate material standard is required.
4.2.2 Application
This test is intended to assess the corrosion susceptibility of metallic materials used in the oral cavity using
potentiodynamic polarization.
4.2.3 Reagents
4.2.3.1 Lactic acid (C H O ), 90 %, analytical grade.
3 6 3
4.2.3.2 Sodium chloride (NaCl), analytical grade.
4.2.3.3 Sodium hydroxide (NaOH), analytical grade.
4.2.3.4 Water, complying with grade 2 of ISO 3696:1987.
4.2.3.5 Argon or nitrogen gas, with a minimum purity of 99,99%.
4.2.3.6 Ethanol or methanol (C H OH or CH OH), analytical grade.
2 5 3
4.2.3.7 Acetone (C H O), analytical grade.
3 6
4.2.4 Apparatus
4.2.4.1 Temperature-controlled borosilicate glass test cell, complying with ISO 3585 (a double-walled cell
is unnecessary if the test is carried out at (23 2)°C).
–9 –1
4.2.4.2 Scanning potentiostat, potential range 1 600 mV, current output range 10 A to 10 A.
11
4.2.4.3 Potential measuring instrument, with input impedance 10 and sensitivity/accuracy able to
detect a change of 1 mV over a potential change of 1 600 mV.
4.2.4.4 Current-measuring instrument, capable of measuring a current to within 1 % of the absolute value
–9 –1
over a current range between 10 A and 10 A.
4.2.4.5 Working electrode (specimen holder).
4.2.4.6 Counter electrode(s), composed of high purity vitreous carbon or platinum.
4.2.4.7 Reference electrode, either saturated calomel electrode (SCE) or Ag/AgCl electrode (saturated silver
chloride electrode [SSE]).
4.2.4.8 pH meter, the sensitivity of the pH meter should be ±0,05 pH units.
4.2.4.9 Silicon carbide paper, complying with ISO 6344-1:1998.
4.2.4.10 1 m diamond paste.
4.2.4.11 Micrometer gauge, accurate to 0,01 mm.
4.2.4.12 Light microscope, minimum magnification of 50.
6 © ISO 2009 – All rights reserved
---------------------- Page: 18 ----------------------
oSIST prEN ISO 10271:2009
ISO/CD 10271
4.2.5 Electrolyte preparation
Dissolve 9,0 g NaCl (4.2.3.2) in approximately 950 ml water (4.2.3.4). Adjust to pH 7,4 0,1 using 1 % C H O
3 6 3
(4.2.3.1) or 4 % NaOH (4.2.3.3). Dilute with water to 1 000 ml.
4.2.6 Samples
4.2.6.1 Fabrication
4.2.6.1.1 Casting alloys
Specimens shall be cast in accordance with the manufacturer’s recommendations.
4.2.6.1.2 Prefabricated samples
Prefabricated parts/devices shall be used in the as-received condition.
4.2.6.1.3 Other
Specimens prepared by other methods, e.g. machined, sintered, eroded, etc., shall be tested in the as-
manufactured condition after suitable cleaning.
4.2.6.2 Sampling
At least four specimens shall be tested.
4.2.6.3 Sample surface area
2
The surface area of each specimen shall be not less than 0,1 cm .
4.2.6.4 Preparation
If the specimen is cast, remove any sprues, runners or other projections from its surface. Blast surfaces with
125 m pure alumina to remove investment.
If recommended, heat-treat casting alloys following the manufacturer’s instructions. Heat-treat all metal-ceramic
alloys for 10 min in air at the highest temperature recommended by the alloy manufacturer and bench cool.
Specimens shall be prepared with one flat surface exposed. A suitable contact shall be provided for connection to
the electrochemical apparatus.
The working electrode shall be prepared in a way that ensures the absence of crevices. The recommended
procedure is that of embedding in epoxy resin, which does not exhibit loss of electrical insulation during immersion.
Instead of embedding, a specimen holder (4.2.4.5) may be used if the absence of crevices is confirmed by
specimen examination after the test.
Remove at least 0,1 mm, measured using a measuring instrument [e.g. micrometer gauge (4.2.4.11)], from each
free surface using standard metallographic proc
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.