1、BRITISH STANDARD BS ISO 13317-2:2001 Determination of particle size distribution by gravitational liquid sedimentation methods Part 2: Fixed pipette method ICS 19.120 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 13317-2:2001 This British Standard, having been prepared
2、 under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 July 2001 BSI 07-2001 ISBN 0 580 37512 0 National foreword This British Standard reproduces verbatim ISO 13317-2:2001 and implements it a
3、s the UK national standard. Together with BS ISO 13317-1:2001 and BS ISO 13317-3:2001 it supersedes BS 3406-2:1984, which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee LBI/37, Sieves, screens and particle sizing, to Subcommittee LBI/37/4, Sizing by method
4、s other than sieving, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the
5、BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are resp
6、onsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and kee
7、p the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 9, and a back cover. The BSI copyright date d
8、isplayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsReference number ISO 13317-2:2001(E) INTERNATIONAL STANDARD ISO 13317-2 First edition 2001-04-15 Determination of particle size distribution by gravitational liquid sedime
9、ntation methods Part 2: Fixed pipette method Dtermination de la distribution granulomtrique par les mthodes de sdimentation par gravit dans un liquide Partie 2: Mthode de la pipette fixeISO 13317-2:2001(E) ii ISO 13317-2:2001(E)iii Contents Page Foreword.iv Introduction.v 1 Scope 1 2 Normative refer
10、ences 1 3 Terms, definitions and symbols.1 4 Sampling.2 5 The fixed position pipette (Andreasen) method.2 6 Preparation.4 7 Procedure .5 8 Assay of fractions6 9 Tests in duplicate and validation .6 10 Calculation of results 7 11 Reporting of results.7 Annex A (informative) Worked example8ISO 13317-2
11、:2001(E) iv 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 f
12、or 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 Internationa
14、l 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. Internati
15、onal 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
16、liquid 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.ISO 13317-2:2001(E)v Introduction This part of ISO 13317 describes a method to determine particle size
17、distribution using 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 direct
18、ly the proportion 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.INTERNATIONAL STANDARD ISO 13317-2:2001(E)1 Determination of particle size distribution by gravitational liquid sedimentation met
19、hods Part 2: Fixed pipette method 1 Scope This part of ISO 13317 describes a method using a pipette to determine particle size distribution, typically in the size range 1 m to 100 m, by gravitational sedimentation in a liquid. NOTE This part of ISO 13317 may involve hazardous materials operations an
20、d equipment. This part of ISO 13317 does not purport to address all the safety problems 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
21、to its use. The method of determining the particle size distribution described in 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 com
22、parable shape. Particles should not undergo any chemical or physical change in the suspension liquid. It is necessary that the particles have a density higher than that of the liquid. 2 Normative references The following normative documents contain provisions which, through reference in this text, c
23、onstitute provisions of this part of ISO 13317. For dated references, subsequent amendments 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 o
24、f the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 8213, Chemical products for industrial use Sampling techniques Solid chemical
25、 products in the form of particles varying from powders to coarse lumps. ISO 9276-1, 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
26、 and guidelines. ISO 14887, Sample preparation Dispersing procedures for powders in liquids. 3 Terms, definitions and symbols 3.1 Terms and definitions For the purposes of this part of ISO 13317, the terms and definitions given in ISO 13317-1 apply.ISO 13317-2:2001(E) 2 3.2 Symbols For the purposes
27、of this part of ISO 13317, the symbols given in ISO 13317-1 and the following apply. Size Symbol Unit Derivative unit Calibrated volume of the sedimentation vessel V l ml Volume of the pipette to the graduation mark V p lm l Mass of sample solids in 10 ml at time t 0 W 0 kg g Mass of sample solids i
28、n 10 ml at time t n W n kg g Pipette sampling height (or drop height) h n mc m Sample withdrawal time t n s Stokes diameter corresponding to withdrawal time t 0 x n m m Cumulative frequency by mass at withdrawal time t n ; it is equal to W n / W 0 F n Dimensionless Dimensionless 4 Sampling The sampl
29、ing method given in ISO 13317-1 applies. 5 The fixed position pipette (Andreasen) method 5.1 Principle Samples are withdrawn from a suspension 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 depth h
30、 below the surface. After time, t, the sample withdrawn contains only those particles with Stokes diameters less than that of particles settling 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 i
31、s obtained directly by weighing the residue after removal of the suspending medium from each extracted sample. 5.2 Apparatus 5.2.1 Sedimentation vessel 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 vesse
32、l (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 base 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
33、scale should also be vertical and have an accuracy of 1mm.ISO 13317-2:2001(E)3 Key 1 Graduation mark 2 10 ml capacity 3 Discharge tube 4 Pipette bulb 5T w o - w a y t a p 6 Dome (vented) 7 Pipette capillary stem 8 Sedimentation vessel Figure 1 Fixed position pipette (Andreasen) 5.2.2 Pipette The pip
34、ette 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) is fused to the pipette with a ground- glass joint to fit the neck of the sedimentation vessel. The pipette bulb should
35、 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 sedimentation vessel when in position. The stem from the pipette bulb to the sampling inlet is constructed of capillary glass tu
36、be 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. NOTE A variation of the fixed position Andreasen pipette exists as the Leschonski modification. In this variation, the pipette is extended to the bottom of the vessel and the sample is typical
37、ly 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 volume matching that of the capillary is intended to remove the systematic positive error (i.e. over-estimation of the pe
38、rcentage 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 sample. In practice, differences between results obtained using these modifications and results using the Andreasen pip
39、ette method may not be significant for most materials.ISO 13317-2:2001(E) 4 5.3 Ancillary apparatus The ancillary apparatus includes: constant temperature enclosure. For prolonged analyses (greater than 1 h), a constant temperature bath is required into which the sedimentation vessel can be immersed
40、. 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, bottle shaker or high speed mechanical stirrer; balance, having an accuracy of 0,1 mg, or better; drying
41、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 beakers suitable for evaporation, of capacity not less than 20 ml or aluminium foil containers. Aluminium foil co
42、ntainers, 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 g for the glass containers. Since a difference in mass is required, a greater accuracy can result from the u
43、se 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 a
44、t least 3 600 s and a resolution of 1 s. 6 Preparation 6.1 Sample preparation A representative sample for analysis shall be taken according to ISO 8213. It shall be dispersed according to ISO 14887 in a suspending medium of adequate viscosity. Make up the test portion to give a concentration of abou
45、t 0,2 % by volume. Record the use of ultrasonics or mechanical stirring to aid dispersion. 6.2 Calibration of sedimentation vessel Determine the volume, (V), of the sedimentation vessel, to an accuracy of 0,3 %, by filling with distilled water up to the 20 ml mark with the pipette in position. Remov
46、e typically eight 10 ml samples and determine the final height h n after each withdrawal. 6.3 Calibration of pipette Clean and dry the pipette. Partly fill the sedimentation vessel with distilled water. Set the tap in the sampling position and suck water into the bulb up to the graduation mark. Turn
47、 the tap to the discharge position and allow the water to drain into a tared weighing container. Apply minimum pressure to blow any water remaining in the bulb and in the discharge tube into the weighing container. Weigh the container to the nearest 0,001 g and calculate the internal volume V p of t
48、he pipette. The values for the volume of the sedimentation vessel V, and the pipette volume V p , are used to calculate the sample concentrations in the sedimentation vessel and the pipette (see Table A.1). The calculated concentration using V and V p should agree (within statistical uncertainty) wi
49、th the initial concentration for samples extracted at time zero in Table A.1.ISO 13317-2:2001(E)5 6.4 Temperature Maintain the temperature in accordance with ISO 13317-1. 6.5 Withdrawal time calculation Calculate the withdrawal time for the first fraction using Stokes law in the following form: 1 2 sl1 18 h t gx (1) where x 1 is the Stokes diameter for the first fraction, which must not exceed the upper critical Stokes diameter, see ISO 13317-1. The initial height h is normally 20 cm, but other heights in the 10 cm to
