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1、Reference number ISO 13317-2:2001(E) ISO 2001 INTERNATIONAL STANDARD ISO 13317-2 First edition 2001-04-15 Determination of particle size distribution by gravitational liquid sedimentation methods Part 2: Fixed pipette method Dtermination de la distribution granulomtrique par les mthodes de sdimentat
2、ion par gravit dans un liquide Partie 2: Mthode de la pipette fixe Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without lic
3、ense from IHS -,-,- ISO 13317-2:2001(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes 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
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6、ariat at the address given below. ISO 2001 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 addr
7、ess below or ISOs 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 copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved Copyright International Organization for S
8、tandardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) ISO 2001 All rights reservediii ContentsPage Foreword.iv Introduction
9、.v 1Scope 1 2Normative references1 3Terms, definitions and symbols.1 4Sampling.2 5The fixed position pipette (Andreasen) method.2 6Preparation.4 7Procedure.5 8Assay of fractions6 9Tests in duplicate and validation.6 10Calculation of results 7 11Reporting of results.7 Annex A (informative) Worked exa
10、mple8 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) iv ISO 2001 All right
11、s 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 fo
12、r 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
13、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
14、 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 part of ISO 13317 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Internatio
15、nal Standard ISO 13317-2 was prepared by Technical Committee ISO/TC 24, Sieves, sieving and other sizing methods, Subcommittee SC 4, Sizing by methods other than sieving. ISO 13317 consists of the following parts, under the general title Determination of particle size distribution by gravitational l
16、iquid sedimentation methods: ?Part 1: General principles and guidelines ?Part 2: Fixed pipette method ?Part 3: X-ray gravitational technique Annex A of this part of ISO 13317 is for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Lice
17、nsee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) ISO 2001 All rights reservedv Introduction This part of ISO 13317 describes a method to determine particle size distribution us
18、ing a fixed position pipette apparatus commonly referred to as the Andreasen pipette. The Andreasen pipette employs an incremental method of analysis which gives the mass distribution directly. In incremental methods, the solids concentration at the measurement level determines directly the proporti
19、on by mass of the analysis sample that consists of particles having a diameter less than that corresponding to the velocity of fall at the time of sampling. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001
20、Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo repro
21、duction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 13317-2:2001(E) ISO 2001 All rights reserved1 Determination of particle size distribution by gravitational liquid sedimentation methods Part 2: Fixed pipette method 1Scope This part of ISO 13317 describes a meth
22、od using a pipette to determine particle size distribution, typically in the size range 1 m to 100 m, by gravitational sedimentation in a liquid. NOTEThis part of ISO 13317 may involve hazardous materials operations and equipment. This part of ISO 13317 does not purport to address all the safety pro
23、blems associated with its use. It is the responsibility of the user of this part of ISO 13317 to establish appropriate safety and health practices and to determine the applicability of the regulatory limitations prior to its use. The method of determining the particle size distribution described in
24、this part of ISO 13317 is applicable to powders which can be dispersed in liquids or powders which are present in slurry form. The method is applicable to powders made up of particles having the same density and of comparable shape. Particles should not undergo any chemical or physical change in the
25、 suspension liquid. It is necessary that the particles have a density higher than that of the liquid. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 13317. For dated references, subsequent am
26、endments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 13317 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest editi
27、on of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 8213, Chemical products for industrial use Sampling techniques Solid chemical products in the form of particles varying from powders to coarse lumps. ISO 9276-1
28、, Representation of results of particle size analysis Part 1: Graphical representation. ISO 13317-1, Determination of particle size distribution by gravitational liquid sedimentation methods Part 1: General principles and guidelines. ISO 14887, Sample preparation Dispersing procedures for powders in
29、 liquids. 3Terms, definitions and symbols 3.1Terms and definitions For the purposes of this part of ISO 13317, the terms and definitions given in ISO 13317-1 apply. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/997
30、2545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) 2 ISO 2001 All rights reserved 3.2Symbols For the purposes of this part of ISO 13317, the symbols given in ISO 13317-1 and the following apply. SizeSymbolUnitDeri
31、vative unit Calibrated volume of the sedimentation vesselV l ml Volume of the pipette to the graduation markVplml Mass of sample solids in 10 ml at time t0W0kgg Mass of sample solids in 10 ml at time tnWn kgg Pipette sampling height (or drop height)hnmcm Sample withdrawal timetns Stokes diameter cor
32、responding to withdrawal time t0xnmm Cumulative frequency by mass at withdrawal time tn; it is equal to Wn/ W0 Fn DimensionlessDimensionless 4Sampling The sampling method given in ISO 13317-1 applies. 5The fixed position pipette (Andreasen) method 5.1Principle Samples are withdrawn from a suspension
33、 during sedimentation by means of a calibrated pipette at a series of known times after initial agitation with the tip of the pipette being at a known depthhbelow the surface. After time,t, the sample withdrawn contains only those particles with Stokes diameters less than that of particles settling
34、at rate h/t, since all particles larger than this will have settled below the sampling point. The cumulative undersize distribution by mass of the powder is obtained directly by weighing the residue after removal of the suspending medium from each extracted sample. 5.2Apparatus 5.2.1Sedimentation ve
35、ssel The sedimentation vessel is of glass of about 5 cm internal diameter and having a graduated scale from 0 cm to 20 cm marked on the side of the vessel (Figure 1). The graduated scale may be subdivided at 5 mm or 10 mm intervals. The zero graduation should be not less than 25 mm from the inside b
36、ase of the vessel so that the capacity, when filled to the 20 cm mark, is about 500 ml. It is important that the walls of the cylinder are vertical. The scale should also be vertical and have an accuracy of?1 mm. Copyright International Organization for Standardization Provided by IHS under license
37、with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) ISO 2001 All rights reserved3 Key 1Graduation mark 210 ml capacity 3Discharge tube 4Pipette bulb 5Two-way tap 6Dom
38、e (vented) 7Pipette capillary stem 8Sedimentation vessel Figure 1 Fixed position pipette (Andreasen) 5.2.2Pipette The pipette is fitted with a two-way tap and a side discharge tube. The capacity of the pipette to the graduation mark is 10 ml. A bell-shaped dome (with vent hole, not shown in Figure 1
39、) is fused to the pipette with a ground- glass joint to fit the neck of the sedimentation vessel. The pipette bulb should be shaped as in Figure 1. The inlet to the pipette stem should be level with the zero mark on the sedimentation vessel and the stem should be parallel to the walls of the sedimen
40、tation vessel when in position. The stem from the pipette bulb to the sampling inlet is constructed of capillary glass tube with a bore of not less than 1 mm nor more than 1,3 mm. The tube above the bulb should be a 3,5 mm bore. NOTEA variation of the fixed position Andreasen pipette exists as the L
41、eschonski modification. In this variation, the pipette is extended to the bottom of the vessel and the sample is typically withdrawn through four apertures around the circumference of the pipette at a fixed depth of about 30 mm above the bottom of the vessel. Additionally, a subsidiary bulb with a v
42、olume matching that of the capillary is intended to remove the systematic positive error (i.e. over-estimation of the percentage undersize) resulting from liquid retained in the capillary tube after each withdrawal. In this way, the sample residue is removed from the capillary before taking the next
43、 sample. In practice, differences between results obtained using these modifications and results using the Andreasen pipette method may not be significant for most materials. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Stand
44、ards 1/9972545001 Not for Resale, 04/21/2007 01:44:58 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13317-2:2001(E) 4 ISO 2001 All rights reserved 5.3Ancillary apparatus The ancillary apparatus includes: ?constant temperature enclosure. For prolonged analyses (greater
45、 than 1 h), a constant temperature bath is required into which the sedimentation vessel can be immersed. It is essential that no vibration be imparted to the sedimentation vessel during the analysis. See 6.3; ?dispersing vessel of appropriate dimensions; ?flexible spatula; ?ultrasonic bath or probe,
46、 bottle shaker or high speed mechanical stirrer; ?balance, having an accuracy of 0,1 mg, or better; ?drying oven capable of being maintained within the temperature range suitable for the evaporation of the suspending liquid, e.g. 378,15 K to 383,15 K for water; ?wide-mouthed weighing bottles or beak
47、ers suitable for evaporation, of capacity not less than 20 ml or aluminium foil containers. Aluminium foil containers, as purchased, may contain a layer of grease and should be oven dried before use. These are preferable to glass containers since they typically weigh about 1 g compared to 20 g to 30
48、 g for the glass containers. Since a difference in mass is required, a greater accuracy can result from the use of aluminium foil containers. With certain sample systems, filtration may be preferred; ?desiccator in which the sample containers can be cooled after drying. Some dispersing agents are hygroscopic and the sample may absorb moisture if allowed to cool in ambient conditions; ?timer with a range of at least 3 600 s and a resolutio