EN ISO 307:2003
(Main)Plastics - Polyamides - Determination of viscosity number (ISO 307:2003)
Plastics - Polyamides - Determination of viscosity number (ISO 307:2003)
Kunststoffe - Polyamide - Bestimmung der Viskositätszahl (ISO 307:2003)
Diese Internationale Norm legt ein Verfahren zur Bestimmung der Viskositätszahl (auch als reduzierte Viskositätszahl bezeichnet) von verdünnten Polyamid-lösungen in bestimmten, festgelegten Lösemitteln fest.
Das Verfahren ist auf Polyamide mit den Bezeichnungen PA 46, PA 6, PA 66, PA 69, PA 610, PA 612, PA 11, PA 12, PA 6T und PA MXD6, wie in ISO 1847-1 definiert, und Copolyamide und sonstige Polyamide anwendbar, die unter den festgelegten Bedingungen in einem der festgelegten Lösemittel löslich sind.
Das Verfahren ist nicht auf Polyamide anwendbar, die durch anionische Polymerisation von Laktamen oder mit Vernetzungsmitteln hergestellt wurden; derartige Polyamide sind normalerweise in den vorgeschriebenen Lösemitteln unlöslich.
Im Allgemeinen müssen die Polyamidproben in den aufgeführten Lösemitteln vollständig löslich sein und die in ihnen enthaltenen Additive (z. B. Verstärkungsfasern, Flammschutzmittel und Modifikatoren) dürfen sich nicht störend auf die Viskositätsmessung auswirken. Das Verfahren kann jedoch für die Überwachung der Herstellung von Mischungen angewandt werden, die Additive enthalten, die sich störend auf die Viskositäts-messung auswirken. In solchen Fällen hat die jeweilige Mischung eine bestimmte, in einem festgelegten Lösemittel gemessene Viskositätszahl, die an sich nicht von einem Lösemittel auf ein anderes Lösemittel umgewandelt werden kann, außer durch ein bestimmtes, die Mischung betreffendes Verhältnis, und die nur für den Vergleich von Produkten geeignet ist.
Die Viskositätszahl wird nach dem in ISO 1628-1 festgelegten allgemeinen Verfahren unter Beachtung der in dieser Internationalen Norm festgelegten besonderen Bedingungen bestimmt.
Die Bestimmung der Viskositätszahl eines Polyamids ergibt ein Maß für die relative Molekülmasse des Polymers.
Plastiques - Polyamides - Détermination de l'indice de viscosité (ISO 307:2003)
Polimerni materiali - Poliamidi - Določanje števila viskoznosti (ISO 307:2003)
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Plastics - Polyamides - Determination of viscosity number (ISO 307:2003)Plastiques - Polyamides - Détermination de l'indice de viscosité (ISO 307:2003)Kunststoffe - Polyamide - Bestimmung der Viskositätszahl (ISO 307:2003)Ta slovenski standard je istoveten z:EN ISO 307:2003SIST EN ISO 307:2003en83.080.20PlastomeriThermoplastic materialsICS:SIST EN ISO 307:20001DGRPHãþDSLOVENSKI
STANDARDSIST EN ISO 307:200301-december-2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 307August 2003ICS 83.080.20Supersedes EN ISO 307:1997English versionPlastics - Polyamides - Determination of viscosity number (ISO307:2003)Plastiques - Polyamides - Détermination de l'indice deviscosité (ISO 307:2003)Kunststoffe - Polyamide - Bestimmung der Viskositätszahl(ISO 307:2003)This European Standard was approved by CEN on 1 August 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 307:2003 E
EN ISO 307:2003 (E)2CORRECTED
2003-10-01ForewordThis document (EN ISO 307:2003) has been prepared by Technical Committee ISO/TC 61"Plastics" in collaboration with Technical Committee CEN/TC 249 "Plastics", the secretariat ofwhich is held by IBN.This European Standard shall be given the status of a national standard, either by publication ofan identical text or by endorsement, at the latest by February 2004, and conflicting nationalstandards shall be withdrawn at the latest by February 2004.This document supersedes EN ISO 307:1997.According to the CEN/CENELEC Internal Regulations, the national standards organizations ofthe following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland andthe United Kingdom.Endorsement noticeThe text of ISO 307:2003 has been approved by CEN as EN ISO 307:2003 without anymodifications.NOTE
Normative references to International Standards are listed in Annex ZA (normative).
EN ISO 307:2003 (E)3Annex ZA(normative)Normative references to international publicationswith their relevant European publicationsThis European Standard incorporates by dated or undated reference, provisions from otherpublications. These normative references are cited at the appropriate places in the text and thepublications are listed hereafter. For dated references, subsequent amendments to or revisions ofany of these publications apply to this European Standard only when incorporated in it byamendment or revision. For undated references the latest edition of the publication referred toapplies (including amendments).NOTE Where an International Publication has been modified by common modifications, indicatedby (mod.), the relevant EN/HD applies.PublicationYearTitleENYearISO 10421998Laboratory glassware - One-mark volumetric flasksEN ISO 10421999ISO 1628-11998Plastics - Determination of theviscosity of polymers in dilutesolution using capillaryviscometers - Part 1: GeneralprinciplesEN ISO 1628-11998ISO 1874-11992Plastics - Polyamide (PA)moulding and extrusion materials- Part 1: DesignationEN ISO 1874-12000ISO 64271992Plastics - Determination of matterextractable by organic solvents(conventional methods)EN ISO 64271998
Reference numberISO 307:2003(E)© ISO 2003
INTERNATIONAL STANDARD ISO307Fourth edition2003-08-15Plastics — Polyamides — Determination of viscosity number Plastiques — Polyamides — Détermination de l'indice de viscosité
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ISO 307:2003(E) © ISO 2003 — All rights reserved iii Contents Page Foreword.iv 1 Scope.1 2 Normative references.1 3 Terms and definitions.2 4 Principle.2 5 Reagents and materials.2 6 Apparatus.3 7 Preparation of test samples.4 8 Calculation of mass of test portion.5 9 Selection of solvent.6 10 Procedure.7 11 Expression of results.9 12 Repeatability and reproducibility.9 13 Relationship between the viscosity number determined in 96 % (by mass) sulfuric acid solution and viscosity number determined in various other solvents.9 14 Test report.18 Annex A (normative)
Determination of the concentration of commercial sulfuric acid [95 % (by mass) to 97 % (by mass)] and adjustment to 96 % (by mass).20
ISO 307:2003(E) iv © ISO 2003 — 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 307 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic materials. This fourth edition cancels and replaces the third edition (ISO 307:1994), which has been technically revised.
INTERNATIONAL STANDARD ISO 307:2003(E) © ISO 2003 — All rights reserved 1 Plastics — Polyamides — Determination of viscosity number 1 Scope This International Standard specifies a method for the determination of the viscosity number (also referred to as reduced viscosity) of dilute solutions of polyamides in certain specified solvents. The method is applicable to the polyamides designated PA 46, PA 6, PA 66, PA 69, PA 610, PA 612, PA 11, PA 12, PA 6T/66 and PA MXD6 as defined in ISO 1874-1, as well as to copolyamides and other polyamides that are soluble in one of the specified solvents under the specified conditions. The method is not applicable to polyamides produced by anionic polymerization of lactams or produced with crosslinking agents; such polyamides are normally insoluble in the specified solvents. In general, polyamide samples have to be completely soluble in the solvents mentioned, and the additives contained in them (e.g. reinforcement fibres, flame-retardants and modifiers) must not interfere with the viscosity measurement. However, the method can be used for production control of compounds containing additives which interfere with the viscosity measurement. In such cases, a particular compound in a particular solvent will have a specific viscosity number which, in principle, cannot be converted from one solvent to another except by means of a relationship specific to the compound concerned. Viscosity numbers converted in this way are only suitable for inter-product comparisons. The viscosity number is determined by the general procedure specified in ISO 1628-1, observing the particular conditions specified in this International Standard. The determination of the viscosity number of a polyamide provides a measure of the relative molecular mass of the polymer. 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 1042:1998, Laboratory glassware — One-mark volumetric flasks ISO 1628-1:1998, Plastics — Determination of the viscosity of polymers in dilute solution using capillary viscometers — Part 1: General principles ISO 1874-1:1992, Plastics — Polyamide (PA) moulding and extrusion materials — Part 1: Designation ISO 3105:1994, Glass capillary kinematic viscometers — Specifications and operating instructions ISO 3451-4:1998, Plastics — Determination of ash — Part 4: Polyamides ISO 6427:1992, Plastics — Determination of matter extractable by organic solvents (conventional methods) ISO 15512:1999, Plastics — Determination of water content
ISO 307:2003(E) 2 © ISO 2003 — All rights reserved ASTM D 789-98, Standard Test Methods for Determination of Relative Viscosity and Moisture Content of Polyamide (PA) JIS K 6920-2:2000, Plastics — Polyamide (PA) moulding and extrusion materials — Part 2: Preparation of test specimens and determination of properties 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 1628-1 and the following apply. 3.1 viscosity number VN 〈of a polymer〉 the value given by the equation 01VN1cηη=−× (1) where η is the viscosity of a solution of the polymer in a specified solvent; η0 is the viscosity of the solvent, expressed in the same units as η; c is the concentration, in grams per millilitre, of the polymer in the solution. NOTE The viscosity number is usually expressed in millilitres per gram. 4 Principle The times of flow of a solvent and a solution of the polyamide at a concentration of 0,005 g/ml in the solvent are measured at 25 °C, the same viscometer being used for both measurements. The viscosity number is calculated from these measurements and from the known concentration of the solution. 5 Reagents and materials Use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. WARNING — Avoid contact with the skin and inhalation of any vapours of the solvents and cleaning liquids. 5.1 Solvents 5.1.1 Sulfuric acid, (96 ± 0,15) % (by mass) solution. For the determination of the concentration of commercial sulfuric acid [95 % (by mass) to 97 % (by mass)] and adjustment to 96,0 % (by mass), see Annex A. 5.1.2 Formic acid, (90 ± 0,15) % (by mass) solution. The solvent shall be stored in a brown glass bottle. Its concentration shall be checked at least every 2 weeks. It shall not contain more than 0,2 % (by mass) of acetic acid or methyl formate.
ISO 307:2003(E) © ISO 2003 — All rights reserved 3 5.1.3 m-Cresol, meeting the following specifications: appearance: clear and colourless m-cresol content: 99 % (by mass) min. o-cresol content: 0,3 % (by mass) max. water content: 0,13 % (by mass) max. m-Cresol of the required purity can be obtained by distillation of chemically pure m-cresol, preferably in vacuo. To avoid oxidation, nitrogen should preferably be used for pressure compensation. The purity of the solvent may be checked by gas chromatography. The solvent shall be stored in a brown glass bottle. 5.2 Cleaning liquids 5.2.1 Chromic acid solution, prepared by mixing equal volumes of sulfuric acid (ρ = 1,84 g/ml) and a saturated solution of potassium dichromate. If required, the chromic acid solution may be replaced by other, equally effective cleaning liquids. 5.2.2 Acetone, freshly distilled. 6 Apparatus 6.1 Vacuum drying cabinet, pressure less than 100 kPa. 6.2 Balance, accurate to 0,1 mg. 6.3 Volumetric flask, capacity 50 ml, complying with the requirements of ISO 1042, fitted with a ground-glass stopper. 6.4 Shaking apparatus or magnetic stirrer. 6.5 Sintered-glass filter, with a pore size between 40 µm and 100 µm (grade P 100), or stainless-steel sieve, with apertures of about 0,075 mm2. 6.6 Viscometer, of the suspended-level Ubbelohde type, complying with the requirements of ISO 3105. The essential dimensions of the viscometer are shown in Figure 1. For use with the formic acid solution (5.1.2), the inside diameter of the capillary shall be 0,58 mm ± 2 % (complying with the requirements of size No. 1 of ISO 3105). For use with the sulfuric acid solution (5.1.1) or m-cresol (5.1.3), the inside diameter of the capillary shall be 1,03 mm ± 2 % (complying with the requirements of size No. 2 of ISO 3105). Other types of viscometer listed in ISO 3105 may be used, provided that the results are equivalent to those of the Ubbelohde viscometer specified above. However, in cases of dispute, an Ubbelohde viscometer shall be used. 6.7 Thermostatic bath, capable of being maintained at 25 °C ± 0,05 °C. 6.8 Stop-watch, accurate to 0,1 s. 6.9 Centrifuge.
ISO 307:2003(E) 4 © ISO 2003 — All rights reserved 7 Preparation of test samples 7.1 General Polyamide test samples for the determination of the viscosity number shall be completely soluble in the solvents mentioned, and the additives contained in them (reinforcement fibres, flame-retardants and modifiers) shall not interfere with the viscosity measurement, or it shall be possible to separate the additives quantitatively from the solution as with glass and carbon fibres, for instance. If the content of these additives is greater than 2 % (by mass), it shall be determined quantitatively to allow the exact test portion size to be calculated (see Table 1). Exception: an extracted sample if it contains extractable additives (see 7.2). Table 1 — Determination of additives in polyamide samples in order to be able to calculate the correct test portion size Property determined Test method Additives determinable Remarks See Subclause Low-molecular-mass fractions Plasticizers Stabilizers Extractable-matter content ISO 6427 Slip agents Extract sample before measurement (thus no correction necessary to size of test portion) 7.2 Polymer modifiers (e.g. ethylene and E/P copolymers) Carbon fibres Residue on hydrolysis in dilute hydrochloric acid (no ash) — Organic flame-retardants Check solubility (if necessary, also determine ash and residue on dissolution) 7.3 Carbonates Metal powders Pigments Residue in 90 % (by mass) formic acid solution (no ash) — Organic flame-retardants
7.4 Glass fibres Silicates Ash (no oxide conversion) ISO 3451-4 Inorganic flame-retardants If necessary, increase size of test portion 7.5
7.2 Samples with extractable ingredients The ground polymer remaining after extraction in accordance with ISO 6427 shall be dried by heating for 3 h at 100 °C under vacuum and used as the test sample. 7.3 Samples with auxiliaries (non-hydrolysable and without ash) that are insoluble in hydrochloric acid, e.g. polymer modifiers, carbon fibres and certain flame-retardants Preliminary tests shall be carried out to determine whether the sample is completely soluble in the solvent to be used, i.e. that it does not form particles of gel.
ISO 307:2003(E) © ISO 2003 — All rights reserved 5 The fraction of polymer modifier and other additives that are insoluble in hydrochloric acid is determined from the hydrolysis residue and the correct amount of polyamide sample to be weighed out is calculated using Equation (3). If carbon fibres that can be detected in the hydrolysis residue under an optical microscope are present, they shall be filtered off from the solution of the polyamide sample by means of a filter crucible with a glass frit. 7.4 Samples with auxiliaries that are soluble in dilute hydrochloric acid and/or cannot be determined from the ash owing to oxide formation, e.g. carbonates, metal powders and certain pigments The residue on dissolution in 90 % (by mass) formic acid is determined as follows: Shake or stir the polyamide sample for several hours at room temperature in about 10 times its own volume of 90 % (by mass) formic acid using the procedure described in 10.2. Separate off the solid residue by filtration. Carefully wash the residue with 90 % (by mass) formic acid and then with acetone. Subsequently dry for 3 h at 100 °C under a vacuum. Weigh. 7.5 Samples with auxiliaries with determinable ash, e.g. glass fibres and silicates The ash is determined by the method specified in ISO 3451-4, and the amount of polyamide sample to be weighed out is calculated using Equation (3). When necessary, filter the solution of the sample through a filter crucible with a glass frit before making the measurement. NOTE Any glass fibres of the usual dimensions contained in the sample will sediment completely after 3 h to 4 h. In such cases, the test solution can be decanted for the measurement and thus does not need to be filtered. 8 Calculation of mass of test portion 8.1 Polyamides with extractable-matter content not greater than 2,00 % (by mass) Calculate the mass mc, in milligrams, of the test portion as follows: c1232501100mwww=++− (2) where w1 is the water content of the sample, expressed as a percentage by mass, determined in accordance with ISO 15512; w2 is the content o
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