ASTM F1877-2005e1 Standard Practice for Characterization of Particles.pdf

1、Designation: F1877 051Standard Practice forCharacterization of Particles1This standard is issued under the fixed designation F1877; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses

2、indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEFigures X2.18 and X2.19 were corrected and the units statement was added editorially in May 2010.1. Scope*1.1 This practice covers a series of procedures for charac

3、-terization of the morphology, number, size, and size distribu-tion of particles. The methods utilized include sieves, optical,SEM, and electrooptical.1.2 These methods are appropriate for particles produced bya number of different methods. These include wear testmachines (Test Method F732), total j

4、oint simulation systems(Guides F1714 and F1715), abrasion testing, methods forproducing particulates, such as shatter boxes or pulverizors,commercially available particles, and particles harvested fromtissues in animal or clinical studies.1.3 The debris may include metallic, polymeric, ceramic, oran

5、y combination of these.1.4 The digestion procedures to be used and issues ofsterilization of retrieved particles are not the subject of thispractice.1.5 A classification scheme for description of particle mor-phology is included in Appendix X3.1.6 The values stated in SI units are to be regarded ass

6、tandard. No other units of measurement are included in thisstandard.1.7 As a precautionary measure, removed debris fromimplant tissues should be sterilized or minimally disinfected byan appropriate means that does not adversely affect theparticulate material. This standard does not purport to addres

7、sall of the safety concerns, if any, associated with its use. It isthe responsibility of the user of this standard to establishappropriate safety and health practices and determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C242 Terminology of

8、Ceramic Whitewares and RelatedProductsC678 Test Method for Determination of Particle Size Dis-tribution of Alumina or Quartz Using Centrifugal Sedi-mentation3E11 Specification for Woven Wire Test Sieve Cloth and TestSievesE161 Specification for Precision Electroformed SievesE766 Practice for Calibra

9、ting the Magnification of a Scan-ning Electron MicroscopeE1617 Practice for Reporting Particle Size CharacterizationDataF561 Practice for Retrieval and Analysis of Medical De-vices, and Associated Tissues and FluidsF660 Practice for Comparing Particle Size in the Use ofAlternative Types of Particle

10、CountersF661 Practice for Particle Count and Size DistributionMeasurement in Batch Samples for Filter Evaluation Usingan Optical Particle Counter3F662 Test Method for Measurement of Particle Count andSize Distribution in Batch Samples for Filter EvaluationUsing an Electrical Resistance Particle Coun

11、ter3F732 Test Method for Wear Testing of Polymeric MaterialsUsed in Total Joint ProsthesesF1714 Guide for Gravimetric Wear Assessment of Pros-thetic Hip Designs in Simulator DevicesF1715 Guide for Wear Assessment of Prosthetic KneeDesigns in Simulator Devices33. Terminology3.1 Definitions of Terms S

12、pecific to This Standard:3.1.1 agglomerate, na jumbled mass or collection of twoor more particles or aggregates, or a combination thereof, heldtogether by relatively weak cohesive forces caused by weakchemical bonding or an electrostatic surface charge generatedby handling or processing.3.1.2 aggreg

13、ate, na dense mass of particles held togetherby strong intermolecular or atomic cohesive forces that isstable to normal mixing techniques, including high-speedstirring and ultrasonics.1This practice is under the jurisdiction ofASTM Committee F04 on Medical andSurgical Materials and Devices and is th

14、e direct responsibility of SubcommitteeF04.16 on Biocompatibility Test Methods.Current edition approved Nov. 1, 2005. Published November 2005. Originallyapproved in 1998. Last previous edition approved in 2003 as F1877 98 (2003)1.DOI: 10.1520/F1877-05E01.2For referenced ASTM standards, visit the AST

15、M website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International

16、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.3 aspect ratio (AR), na ratio of the major to the minordiameter of a particle, which can be used when the major axisdoes not cross a particle outline (see 11.3.3).3.1.4 elongation (E), nratio of the particle le

17、ngth to theaverage particle width (see 11.3.4).3.1.5 equivalent circle diameter (ECD), na measure of thesize of a particle (see 11.3.2 and Appendix X1).3.1.6 Feret diameter, nthe mean value of the distancebetween pairs of parallel tangents to a projected outline of aparticle.3.1.7 flocculate, na gro

18、up of two or more attached par-ticles held together by physical forces, such as surface tension,adsorption, or similar forces.3.1.8 form factor (FF), na dimensionless number relatingarea and perimeter of a particle, as determined in 11.3.6.3.1.9 irregular, adja particle that cannot be described asro

19、und or spherical. A set of standard nomenclature and refer-ence figures are given in Appendix X2.3.1.10 particle, nthe smallest discrete unit detectable asdetermined in test methods. A nanoparticle has at least onedimension less than 100 nm.3.1.11 particle breadth, ndistance between touch pointsof t

20、he shortest Feret pair, orthogonal to length.3.1.12 particle length, ndistance between touch points ofmaximum Feret pair. This value will be greater than or equal tothe maximum Feret diameter.3.1.13 rectangular, adja particle that approximates asquare or rectangle in shape.3.1.14 roundness (R), na m

21、easure of how closely anobject represents a circle as determined in 11.3.5.3.1.15 spherical, adja particle with a generally sphericalshape that appears round in a photograph.4. Summary of Practice4.1 Particles produced by implant wear in vivo in animal orclinical studies are harvested from tissues a

22、fter digestionutilizing methods, such as those in Practice F561. Particlesgenerated in vitro, or obtained from commercial sources, areused as received, or after digestion, if they were generated inprotein solutions, and further separation if there are signs ofaggregation. A two level analysis is pro

23、vided. For routineanalysis, the particles are characterized by the terms ofmorphology and by size using Feret diameters. For moredetailed studies, several methods are described that may beutilized for numerically characterizing their dimensions, sizedistribution, and number.5. Significance and Use5.

24、1 The biological response to materials in the form of smallparticles, as from wear debris, often is significantly differentfrom that to the same materials as larger implant components.The size and shape (morphology) of the particles may have amajor effect on the biological response; therefore, this

25、practiceprovides a standardized nomenclature for describing particles.Such a unified nomenclature will be of value in interpretationof biological tests of responses to particles, in that it willfacilitate separation of biological responses associated withshape from those associated with the chemical

26、 composition ofdebris.5.2 The quantity, size, and morphology of particles releasedas wear debris from implants in vivo may produce an adversebiological response which will affect the long term survival ofthe device. Characterization of such debris will provide valu-able information regarding the eff

27、ectiveness of device designsor methods of processing components and the mechanisms ofwear.5.3 The morphology of particles produced in laboratorytests of wear and abrasion often is affected by the testconditions, such as the magnitude and rate of load application,device configuration, and test enviro

28、nment. Comparison of themorphology and size of particles produced in vitro with thoseproduced in vivo will provide valuable information regardingthe degree to which the method simulates the in vivo conditionbeing modeled.6. Interferences6.1 Particles may form aggregates or agglomerates duringprepara

29、tion and storage. These would result in an increase inmeasured particle size and decrease in particle number. It isessential that care be taken to resuspend particles prior toanalysis and to note any effects of the dispersant used.6.2 Debris from wear tests or harvested from tissues maycontain a mix

30、ture of materials. Care should be taken to separatethe particles and methods utilized to determine the chemicalcomposition of the particles.6.3 Many automated particle counters operate on the as-sumption that the particles are spherical. These methods maynot be appropriate for nonspherical debris. A

31、dditional methodsshould be used to verify size using methods that take aspectratio into consideration, for example, SEM image analysis.7. Apparatus7.1 Scanning Electron Microscope (SEM) (see PracticeE766):7.1.1 Standard SEM equipment can be utilized for manystudies. In special instances, such as wit

32、h polymeric particles,a low acceleration voltage (1-2 kV) machine with a highbrightness electron source, such as a field emission tip, may beutilized.7.1.2 Elemental analysis may be accomplished with anenergy dispersive spectrometer (EDS) for energy dispersiveX-ray analysis (EDXA).7.2 Optical Micros

33、copeAn optical microscope operatingin the transmission mode may be utilized. Dark field illumina-tion may enhance visualization of some particles. Polarizedlight will facilitate identification of semicrystalline polymericmaterials.7.3 Automatic Particle Counters (see Practice F660):7.3.1 Image Analy

34、zerThis instrument counts particles bysize as those particles lie on a microscope slide.7.3.2 Optical CounterThis instrument measures the areaof a shadow cast by a particle as it passes a window. From thisarea the instrument reports the diameter of a circle of equalarea.7.3.3 Electrical Resistance C

35、ounterThis instrument mea-sures the volume of an individual particle. From that volumethe instrument reports the diameter of a sphere of equal volume(see Test Methods C678).F1877 05128. Reagents8.1 Particle-Free (0.2 m Filtered) Deionized Water, fornonpolymeric particles.8.2 Particle-Free (0.2 m Fil

36、tered) Methanol or Ethanol,for polymeric or mixed debris.8.3 Ultra-Cleaning Reagent, for apparatus or labware clean-ing.9. Specimen Preparation9.1 Specimens from explanted tissues from animal or clini-cal studies may need to be harvested and digested usingmethods, such as those described in Practice

37、 F561.9.2 Particles from in vitro cell culture tests also may need tobe digested and harvested.9.3 Centrifugation of particles from wear may be consid-ered, if necessary, at 400 g for 10 min, and resuspended inwater or methanol. Resuspended particles may be filtered inaccordance with Practice F561 p

38、rior to examination by SEM.10. Particle Imaging by Light or Scanning ElectronMicroscopy10.1 Images may either be captured electronically or pho-tographically for subsequent analysis.10.2 For the characterization and measurements to be accu-rate, it is essential that the particles be imaged at the la

39、rgestmagnification as possible. The magnifications in Table 1 arerecommended.10.3 For particle size distribution measurements, divideeach of the size ranges specified in Table 1, into 10 bins.11. Particle Characterization11.1 Particle Shape (Morphology)Refer to the photo-graphs and classify the morp

40、hology of the particles using thenomenclature in Appendix X2.11.2 Routine Particle Size Determination Using Feret Di-ameters:11.2.1 The use of multiple Feret diameters especially isuseful for spherical and rectangular particles.11.2.2 Determine the particle size and aspect ratio as themean of two Fe

41、ret diameters.11.2.3 Calculate the particle size distribution based on thevolume of solution used and the size of the filters.11.3 Detailed Particle Shape Analysis for Irregular ShapedParticles:11.3.1 Five particle dimensional measurements are providedusing examples shown in Appendix X1. One is a me

42、asure ofparticle size while the other four are shape descriptors.11.3.2 The Equivalent Circle Diameter (ECD) as a Measureof Particle Size:11.3.2.1 The ECD is defined as the diameter of a circle withan area equivalent to the area (A) of the particle and has theunits of length:ECD 54*A/p!12 (1)11.3.3

43、The Aspect Ratio (AR) is a Common Measure ofShape:11.3.3.1 The AR is the ratio of the major diameter (dmax)tothe minor diameter (dmin). The major diameter is the longeststraight line that can be drawn between any two points on theoutline. The minor diameter is the longest line perpendicular tothe ma

44、jor diameter:AR 5 dmax/dmin(2)11.3.4 The elongation (E), is similar to the AR except it ismore suited for the measurement of much longer particles,especially fibrilar particles, where the major axis line does notstay within the particle boundaries. Refer to particle types Aand C in Appendix X1.11.3.

45、4.1 The E is the ratio of the length (FL) to the breadth(FW):E 5 FL/FW (3)11.3.5 The roundness (R) is a measure of how closely aparticle resembles a circle. The R varies from zero to one inmagnitude with a perfect circle having a value of one.R 5 4A!/p dmax2! (4)where:A = area, anddmax= the maximum

46、diameter.11.3.6 The form factor (FF) is similar to R but is based onthe perimeter (p) of the particle outline rather than the majordiameter. The FF is more sensitive to the variations inroughness of the particle outline.FF 5 4pA/p2(5)where:p = perimeter of the particle outline.11.4 Other Particles S

47、ize Determination Methods:11.4.1 Particles larger than 20 m may be determined bysieves described in Specifications E11 and E161.11.4.2 Particles in liquid suspension may be sized as di-rected in Practice F661 or Test Method F662.12. Elemental Analysis12.1 SEM-EDS analysis should be conducted at a ma

48、gnifi-cation suggested in 10.2.12.2 Elemental analysis should be conducted for at least 10s for each particle. Since detailed compositional analysis is ofquestionable meaning for micron and submicron sized par-ticles, it is recommended that composition be determined basedon identification of key ele

49、mental peaks for the major elementslikely to be present in the sample.13. Report13.1 Report the following information (see Practice E1617):13.1.1 The source of the particles and materials and meth-ods for generation.13.1.2 Methods utilized to digest and separate the particles.13.1.3 Morphological description of the particles.13.1.4 Results of particle size and shape analysis.TABLE 1 Recommended Magnifications for Particle ImagingMagnification Particle Size Range (m)10000 0.1 to 1.01000 1 to 10100 10 to 100F1877 051314. Precision and Bias14.1 The pr