SIST EN ISO 11609:2000

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Zahnheilkunde - Zahnpasten - Anforderungen, Prüfverfahren und Kennzeichnung (ISO 11609:1995)Produits et matériel pour l'art dentaire - Dentifrice - Prescriptions, méthodes d'essai et marquage (ISO 11609:1995)Dentistry - Toothpastes - Requirements, test methods and marking (ISO 11609:1995)71.100.70SULSRPRþNLCosmetics. Toiletries11.060.01Zobozdravstvo na splošnoDentistry in generalICS:Ta slovenski standard je istoveten z:EN ISO 11609:1998SIST EN ISO 11609:2000en01-januar-2000SIST EN ISO 11609:2000SLOVENSKI
STANDARD



SIST EN ISO 11609:2000



SIST EN ISO 11609:2000



SIST EN ISO 11609:2000



SIST EN ISO 11609:2000



SIST EN ISO 11609:2000



INTERNATIONAL STANDARD First edition 1995-l 2-l 5 Dentistry - Toothpastes - Requirements, test methods and marking Produits et ma t&iel pour I’art den take - Dentifrice - Prescriptions, mbthodes d’essai et marquage Reference number IS0 11609:1995(E) SIST EN ISO 11609:2000



IS0 11609:1995(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be rep- resented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard IS0 11609 was prepared by Technical Committee ISO/TC 106, Dentistry, in collaboration with the International Dental Fed- eration (FDI). Annex A forms an integral part and C are for information only. of this International Standard. Annexes B 0 IS0 1995 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 l CH-1211 Geneve 20 l Switzerland Printed in Switzerland ii SIST EN ISO 11609:2000



INTERNATIONAL STANDARD o IS0 IS0 11609:1995(E) Dentistry - Toothpastes - Requirements, test methods and marking 1 Scope This International Standard specifies requirements and test methods for physical and chemical proper- ties, and for the marking and/or labelling of tooth- pastes for daily use by the public with a toothbrush to promote oral hygiene. NOTE 1 It is anticipated that guidelines on claimed or implied efficacy of toothpastes for the prevention or control of oral conditions will be published as an FDI Technical Report. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. POPE, D.G. Accelerated stability testing for production of drug product stability. Drugs and Cosmetics, pp. 54-62, 1980. 3 Definitions For the purposes of this International Standard, the definitions given in IS0 1942 and the following defini- tions apply. 3.1 dentifrice: Any substance or combination of substances specially prepared for the public for cleaning the accessible surfaces of teeth. 3.1 toothpaste: Any semi-solid dentifrice preparation presented in the form of a paste, cream or gel. NOTE 2 The product’s main constituents generally are an abrasive, humectants, a binder, a surfactant and a flavour- ing. Secondarily, the product may contain agents for oral health maintenance. 4 Requirements 4.1 Total fluoride IS0 1942: 1989, Dental vocabulary. IS0 3696: 1987, Water for analytical laboratory use - Specification and test methods. BS 5 136: 198 1, Specification for toothpastes. CTFA, In terna tional Cosmetic lngredien ts Dictionary. I ) SHELLIS, BP. A synthetic saliva for cultural studies of dental plaque. Archives Oral Biol., 23, pp. 485-489, 1978. The total fluoride concentration shall not exceed the limits set by national laws and regulations and in no case shall the total fluoride concentration exceed 0,15 % (m/m). When using containers, for example dispensing systems of various sorts, the total fluoride content per single unit shall not exceed 300 mg. Test in accordance with one of the procedures given in annex B or the EEC method[**]. Other validated methods of similar sensitivity and accuracy may be used (see references [20] and [21]. I) See note 4, clause 6. SIST EN ISO 11609:2000



IS0 11609:1995(E) 0 IS0 4.2 Heavy metals 4.8 Stability The maximum concentration shall not exceed the limits set by national laws and regulations. In no case shall the total heavy metal concentration in the tooth- paste be greater than 20 mg/kg. The toothpaste shall show no signs of deterioration which may affect compliance with this International Standard after being subjected to the ageing pro- cedure specified in 5.4. Test in accordance with reference [I 01, [I I] or [I 21, or other validated method of similar sensitivity and accuracy. 4.3 Alkalinity When tested in accordance with 5.2.1, the toothpaste shall have a pH below 10,5. 4.4 Demineralization Toothpastes having a pH of less than 5,5 shall be tested for demineralization in accordance with 5.2.2. The enamel lost from teeth exposed to the test shall not exceed that lost from teeth exposed to the control treatment or shall comply with the requirements of the enamel abrasion test (5.2.2.2). 4.5 Compatibility with oral tissues The toothpaste should not cause irritation or damage to the oral tissue when used as intended by the manufacturer. Test in accordance with 5.2 and 5.3. NOTE 3 Specific qualitative and quantitative require- ments for freedom from biological hazards are not included in this International Standard, but it is recommended that reference should be made to lSO/TR 7405rll and IS0 10993-I (*I when assessing possible biological or toxicological hazards. 4.6 Microbiology Testing for microbiological contamination shall be carried out according to reference [9] or references 131, 141 and 151. 4.7 Abrasivity The abrasivity of the toothpaste shall not exceed the following limits for dentin: - 2,5 times, if using the procedure specified in annex A, or - 2 times, if using the procedure specified in BS 5136, that of the primary reference material. Test in accordance with 5.3 or any other validated method of similar sensitivity and accuracy. 4.9 Readily fermentable carbohydrates The toothpaste shall not contain readily fermentable carbohydrates. Compliance shall be established by the absence of such compounds in the complete formula or by performing tests in accordance with commonly used analytical methods. 5 Test methods 5.1 Visual inspection The toothpaste shall show no signs of deterioration (e.g. separation, discoloration, viscosity/extension difficulties) after being stored according to the accel- erated ageing procedures specified in 5.4.1. This attests to its compliance with this International Stan- dard. Examine under a bright light with normal visual acuity without magnification. 5.2 Determination of pH and enamel demineralization 5.2.1 Determination of pH Suspend one part by mass of the toothpaste into three parts by mass of water for analytical laboratory use complying with IS0 3696 (grade 2). Determine the pH of the suspension within 10 min, using a pH- meter with a glass and calomel electrode assembly. 5.2.2 Determination of enamel demineralization or abrasion (low pH compositions) The toothpaste shall comply with the requirements of either 5.2.2.1 or 5.2.2.2. 5.2.2.1 Enamel demineralization For toothpaste procedure. with a pH below 5,5, use the fo Ilowing Prepare radioactive human enamel (see annex A or B) in a manner that will provide a uniform surface area on all specimens. Perform the irradiation of the specimens in accordance with the procedure for radioactive abrasion tests. Cover the remainder of the enamel with an acid-resistant varnish. Immerse the specimens promote a slight protein in . fl artificial saliva for 1 h to Im simu lating oral condi- 2 SIST EN ISO 11609:2000



0 IS0 IS0 11609:1995(E) tions. Immerse the specimens individually in 20 ml of I:3 slurries of the test toothpaste in artificial saliva. Stir the slurries constantly and uniformly; maintain continual immersion. Use double-distilled or deionized water (IS0 3696) as a negative control. After immersion for 24 h analyse the slurries for the level of radioactivity (3*P). To pass the test, the enamel lost to the slurries shall not be more than that lost to the water control. 5.2.2.2 Enamel abrasion If the pH of the toothpaste is below pH 5,5, then it shall not remove more than four times the level of human enamel compared to that removed by BS 5136 toothpaste modified as follows: use the toothpaste as a 3:l artificial saliva/toothpaste slurry. If tested using the Hefferren procedure (annex A), the toothpaste shall not remove more than twice the amount of enamel removed by the reference abrasive when both the toothpaste and the reference abrasive are used as a 3:l artificial saliva/toothpaste/abrasive slurry. Test in accordance with annex A or BS 5136. Other validated methods of similar sensitivity and accuracy may be used. 5.3 Determination of abrasivity Determine the mean relative abrasivity compared to the primary reference sample, or any other reference material calibrated to the primary reference sample for human dentin, using the method specified in annex A or BS 5136. Other validated methods of similar sensitivity and accuracy may be used; see for example references [14], [I51 and [16]. 3 months or under such conditions of time and tem- perature as will simulate storage at room temperature for 30 months. 5.4.2 Shelf-life The toothpaste shall meet the requirements of this International Standard 30 months after manufacture. 5.4.3 Container and/or dispensing system The container and/or dispensing system shall not have contaminated the toothpaste inside so as to affect its compliance with this International Standard after being subjected to the ageing procedure described in 5.4.1. 6 Marking and labelling With the exception of dispensing systems and small single units, packaging shall be marked with the following information: a) the word “toothpaste” or equivalent as defined in 32 . - I b) the brand name; c) name and address of manufacturer or responsible distributor; d) batch or lot number; e) a list of ingredients: a complete declaration ac- cording to the CTFA International Cosmetic In- gredients Dictionary, or with descriptive names of ingredients; identification of ingredients shall be consistent with the dictionary, which states how the declaration should be made and the ingredi- ents identified; f 1 5.4 Determination of stability g 5.41 Accelerated ageing procedure The toothpaste shall meet the requirements of this International Standard after storage at 40 “C for net volume, in millilitres, and/or net mass, in grams; ) expiration date, if the period of stabi is less than 30 months. lity (shelf-life) NOTE 4 After 1997, CTFA guidelines ceeded by INCI guidelines (International for Cosmetic Ingredients). will be suc- Nom enclature SIST EN ISO 11609:2000



IS0 11609:1995(E) Annex A (normative) Abrasivity test procedure (Hefferren) 0 IS0 A.1 Scope This annex identifies the specific procedures for determination of dentifrice abrasivity using the ADA laboratory method. A.2 Sampling A representative sample shall be taken from at least two batches. A.3 Procedure A.3.1 Standard reference abrasive The standard reference abrasive is from a specific lot of calcium pyrophosphate held by the Monsanto Company? A.3.2 Apparatus A.3.2.1 Brushing machine A crossbrushing machine is the apparatus of choice.*) The apparatus should ha,ve eight positions for holding specimens. A toothbrush shall be positioned to pass reciprocally over the mounted specimens with a designated tension on the brush while immersed in a dentifrice slurry. The distance traversed by the brush should not be longer than the brush head, so that the specimen does not lose contact with the brush. The mechanism for holding the dentifrice slurry may vary with different machine designs, but should allow for easy removal of the slurry sample. It is important to have some mechanism for agitation of the slurry while the brushing is taking place. A convenient method to accomplish this is to attach rubber mixing vanes just below the brush head. As the brushing takes place, these vanes will prevent the abrasive from settling to the bottom of the slurry container. A.3.2.2 Radioactivity detector The two recommended methods for determination of the radioactivity of the used dentifrice slurries are a Geiger-Mijller planchet counter or liquid scintillation detector. The use of the Geiger counter requires that the samples be dried under defined controlled condi- tions. The liquid scintillation method has the advan- tage of reading directly from the slurry. Counting should be done for a period expected to reduce the alpha value for counting error to less than 2 %. Counting should be performed for a minimum of 1 000 counts and at least 1 min. The number of brushing strokes may be increased if counting times become too long. A.3.3 Presentation of tooth specimens A.3.3.1 Dentin specimens A.3.3.1 .I Selection Human root dentin of extracted permanent teeth are used as the substrate. Single-rooted teeth that were vital at extraction should be selected. An exception, because of the small size, are mandibular incisors: these should not be used. The specimen should be at least 14 mm long and 2 mm wide at the narrow end. All roots shall be caries-free and free of anatomical defects. After extraction, the roots should be stored in neutralized 4 % formaldehyde solution. A.3.3.1.2 Preparation Scrape the roots clean of all soft tissue and cemen- turn. Then remove the crown and the root tips using a separating disc under a flow of water. 1) Calcium pyrophosphate is an example of a suitable product available commercially. This information is given for the con- venience of users of this International Standard and does not constitute an endorsement by IS0 of this product. A sample of the material may be obtained by contacting the company at the address below and requesting the ADA abrasion standard. Slight shifts (< 10 %) in abrasivity between lots have been reported. Monsanto Company, Detergent Division, 800 N. Lindbergh Boulevard, St. Louis, MO, USA 63167. 2) The drawings and blueprints for the machine may be obtained from the American Dental Association. 4 SIST EN ISO 11609:2000



0 IS0 IS0 11609:1995(E) A.3.3.11.3 Irradiation A.3.4 Toothbrushes For each set of eight specimens to be irradiated, add one or two extra roots for use in correction factors. Pack the specimens in 4 % formaldehyde solution and submit to a nuclear reactor for irradiation. The neutron flux should be sufficient to produce about 1 mCi of 3*P beta radiation after several hours. Elevated tem- peratures in the reactor should be avoided. It is also advisable to shield the samples from fast neutrons and gamma radiation. Handling of the irradiated specimens should be done with care using good laboratory practice. The specimens should not be used during the first half-life because of excess radia- tion and should be used before the end of the third half-life because of lack of activity. The half-life of 3*P is 14,3 days so the usable life-span of a set of teeth is 4 weeks. A.3.3.1.4 Mounting of specimens The specimens should be mounted individually in cold- cure methyl methacrylate denture resin: the type of mould used will depend upon the holder on the brushing machine. The specimens should be mounted so that they protrude above the resin surface in a buccal/lingual orientation \ by at least 2 mm. The brushing surface of the root shall be parallel in buc- Cal/lingual orientation to the resin holder and situated so that the brushing will take place perpendicular to the long dimension of the root. Storage of the mounted specimens should be in 4 % formaldehyde. A.3.3.2 Enamel specimens A.3.3.2.1 Selection Selection criteria for enamel specimens are the same as for dentin. The enamel specimens should be ob- tained from human maxillary incisors. A.3.3.2.2 Preparation The entire labial surface of the specimen is used after removing the root. Clean the enamel in the same way as the root. A.3.3.2.3 Irradiation Irradiation of the enamel is identical to the method used with the roots. The roots and enamel specimens may be packed together for submission to the reac- tor. A.3.3.2.4 Mounting Mount the enamel specimens in the same way as the roots. The labial surface shall protrude 2 mm and be parallel to the resin surface. The toothbrushes used should have nylon bristles of medium hardness. The bristle ends should lie in a plane rather than in serrated or end-raised tuft design. The bristle length should be about 10 mm. A 50-tuft medium-texture Pepsodent brush is a commercially avai
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