1、BRITISH STANDARD BS ISO 13317-3:2001 Determination of particle size distribution by gravitational liquid sedimentation methods Part 3: X-ray gravitational technique ICS 19.120 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 13317-3:2001 This British Standard, having been
2、 prepared 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 37509 9 National foreword This British Standard reproduces verbatim ISO 13317-3:2001 and implem
3、ents it as the UK national standard. Together with BS ISO 13317-1:2001 and BS ISO 13317-2:2001 it supersedes BS 3406-2:1984, which is withdrawn.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
4、by methods 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 publications referred to in this document may be found in the BSI
5、 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 respons
6、ible 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 keep t
7、he 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 iv, pages 1 to 11 and a back cover. The BSI copyright date displayed in this
8、 document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsINTERNATIONAL STANDARD ISO 13317-3 First edition 2001-03-01 Reference number ISO 13317-3:2001(E) ISO 2001 Determination of particle size distribution by gravitational liquid sedimentation
9、 methods Part 3: X-ray gravitational technique Dtermination de la distribution granulomtrique par les mthodes de sdimentation par gravit dans un liquide Partie 3: Mthode aux rayons X par gravitISO 13317-3:2001(E) iiISO 13317-3:2001(E) iii Contents Page 1 Scope . 1 2 Normative references . 1 3 Terms
10、and definitions 1 4 Symbols 2 5 Sampling . 2 6 Representation of results 2 7 Principle 2 8 Apparatus . 3 9 Sample preparation 5 10 Procedure . 5 11 Tests in duplicate, validation and verification 6 12 Calculation of results 7 13 Test report 7 Annex A Example of typical report 9 Bibliography. 11ISO 1
11、3317-3:2001(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 sub
12、ject 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 (I
13、EC) 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 Intern
14、ational 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. Int
15、ernational Standard ISO 13317-3 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 gravitat
16、ional 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.INTERNATIONAL STANDARD ISO 13317-3:2001(E) 1 Determination of particle size distribution by gravi
17、tational liquid sedimentation methods Part 3: X-ray gravitational technique SAFETY PRECAUTIONS This part of ISO 13317 does not purport to address all of the safety considerations associated with its use. It is the responsibility of the user of this part of ISO 13317 to establish appropriate safety a
18、nd health practices and determine the applicability of the regulatory limitations prior to its use. 1 Scope This part of ISO 13317 describes a method for the determination of the particle size distribution of a powder dispersed in a liquid using gravity sedimentation. The measurement of the concentr
19、ation of solids settling in a liquid suspension is achieved by monitoring the incremental signal absorption from a beam of X-rays. 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
20、are present in slurry form. The typical particle size range for analysis is from about to about . The method is used for materials containing particles of the same chemical composition which produce adequate X-ray opacity. 2 Normative references The following normative documents contain provisions w
21、hich, through reference in this text, constitute 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
22、 of applying the most recent editions of 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 787-10, General methods of test for pi
23、gments and extenders Part 10: Determination of density Pyknometer method. 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, Representation of results of particle size analysis Part 1:
24、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 liquids. 3 Terms and definitions For the purposes of this par
25、t of ISO 13317, the terms and definitions given in ISO 13317-1 apply. 0,5 m 100 mISO 13317-3:2001(E) 2 4 Symbols For the purpose of this part of ISO 13317, the symbols given in ISO 13317-1 and the following apply. Stokes equivalent spherical diameter (m) (practical unit: micrometres, ) Suspending li
26、quid viscosity ( ), (practical unit: ) Sedimentation height (m) Sample density effective particle density ( ) Liquid density ( ) Acceleration due to gravity ( ) Sedimentation time, (seconds, s) Function of atomic number of sample elements in beam Concentration of sample in beam Attenuation of emerge
27、nt X-ray beam passing through the suspending fluid Attenuation of emergent X-ray beam through suspension at settling height , at time X-ray density 5 Sampling The sampling procedure according to ISO 13317-1 shall be followed. 6 Representation of results The results shall be represented according to
28、ISO 9276-1. 7P r i n c i p l e The concentration of dispersed sample is measured by attenuation of an X-ray beam. A stable, narrow, collimated beam of X-rays passes through a suspension of the sample: it is detected at a known height from the top of the sample cell. The sample cell is completely fil
29、led with sample suspension for the duration of the analysis. The settling height, , at which the particle concentration, , is determined, may be reduced during the analysis for the purpose of obtaining a more rapid analysis than would be possible if all measurements were made at the same value of, .
30、 The cumulative mass percent of sample present at a given sedimentation height is continuously determined. The X- ray signal attenuation at the known height is compared to the attenuation with suspending liquid and also to the attenuation with the homogeneously dispersed sample present in the liquid
31、. The attenuation of the emergent X-ray beam is proportional to the mass of powder in the beam, and is expressed by the following formula: (1) or (2) x St m Pa s mPa s h s kg m 3 l kg m 3 g 9,807 m s 2 t B C I 0 Ih t D lg 10 (I 0 =I) hC h I =I 0 exp (BC) C =(1=B) ln (I=I 0 )ISO 13317-3:2001(E) 3 The
32、 X-ray density, is expressed as follows: (3) also (4) thus (5) The Stokes diameter , corresponding to the X-ray density at settling height and time , is given by: (6) The X-ray density is proportional to the concentration , and thus mass, of sample in the beam. A plot of the X- ray density , taken a
33、s a function of time and , versus provides the cumulative mass distribution versus equivalent spherical diameter. 8A p p a r a t u s 8.1 Main apparatus The main apparatus (see Figure 1) typically consists of a temperature-controlled analysis compartment and mixing chamber; a plumbing system for circ
34、ulation of suspending liquid or sample suspension; an X-ray source/detector system and a control module for apparatus control, data acquisition and reduction. The sedimentation cell within the temperature-regulated analysis compartment may be repositioned throughout the analysis relative to the sign
35、al source and detector to reduce analysis time. Alternative designs, such as one in which the X-ray source and detector move while the sedimentation cell remains stationary, may also be used. The use of a magnetic stirrer should be avoided if magnetically susceptible particles are to be tested. The
36、dispersion may then be maintained by means of a mechanical stirrer. 8.2 Ancillary apparatus Ultrasonic bath, probe or high-speed mechanical stirrer capable of 500 revolutions to 1 000 revolutions per minute. D, D =BClge D = lg (I 0 =I) D =BClge = lg (I 0 =I) x St ht x st = 18h ( s l )gt 1=2 DC Dt h
37、p 18h= ( s l )gtISO 13317-3:2001(E) 4 Figure 1 Schematic of typical apparatus using the X-ray gravitational techniqueISO 13317-3:2001(E) 5 9 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 medi
38、um of adequate viscosity and X-ray transparency. The use of dispersing agents and ultrasonics or mechanical stirring to aid dispersion will be recorded. Typically of dispersed sample is required for the analysis. The sample concentration will be prepared in accordance with the manufacturers instruct
39、ions. Higher sample concentrations may be required with powders having a low X-ray absorptivity coefficient. Knowledge of the exact sample concentration is not required, but the influence of concentration should be checked. The minimum concentration of suspension compatible with the measuring method
40、 is preferred (see ISO 13317-1). The required sample concentration will typically produce a reduction in the beam signal of to relative to the signal observed with the suspending liquid. The sample may be dispersed in either an aqueous or an organic medium. Any liquid compatible with sample cell mat
41、erials and having low absorptivity for X-rays may be used. Typical liquids are water, glycols, kerosene, mineral oils, alcohols and mineral spirits. It is recommended that the viscosity of the suspending medium should have a value such that the largest particle to be measured has a Reynolds number o
42、f (see ISO 13317-1). Any temperature change of the suspension should be minimized during a measurement (see 10.3). The viscosity and density of the suspending liquid at the temperature of the analysis will be reported. The effective particle density of the sample is also reported. The suspending liq
43、uid, including dispersants at the analysis concentration, may be used as the displacement fluid to experimentally determine the effective particle density. 10 Procedure 10.1 General See ISO 13317-1 for guidance on restrictions of upper size limit and lower size limit, and on test conditions. The val
44、idity of the measurement will be dependent on the Stokes equation applying to creeping flow for the suspension under study. The lower size limitation will in part be a function of the ability of the system to minimize thermal convection and mechanical effects. Additionally, for the fine size fractio
45、n, Brownian motion effects may contribute to the vertical spread of particles of the same size originating from the same initial settling height. 10.2 Base-line determination Determine the attenuation of the X-ray signal with only suspending liquid in the sample cell ( solids). Where possible, a bas
46、e-line scan of the entire measuring portion of the cell is advised for subsequent correction of the corresponding sample suspension data. The base-line scan of the entire measuring portion of the cell is recommended as this will provide optimum correction for variability in the cell window thickness
47、, or non-parallel alignment of the cell windows. 10.3 Temperature equilibration Place the dispersed sample suspension in the mixing chamber, and circulate the suspension through the sample cell for typically to . Confirmation is obtained that the analysis compartment is operating within the specifie
48、d temperature band, preferably within of the temperature set point. 10.4 Bubble elimination Check for the presence of air bubbles in the sample cell either manually or automatically. If bubbles are detected, remove them by manual or automatic operation. If air bubbles are detected, make a further ch
49、eck prior to commencing the analysis. Repeat the bubble detection and elimination steps until confirmation is obtained that no bubbles are detected. 50 ml 10 % 30 % 6 0,25 0% 60 s 90 s 1KISO 13317-3:2001(E) 6 10.5 Concentration setting Whilst the suspension continues to circulate through the sample cell, determine the initial sample concentration setting, according to the manufacturers instructions. Depending on the apparatus, this will typically require either a manual setting of the point on the sa
