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Designation: F 1877 – 98

Standard Practice for

Characterization of Particles1
This standard is issued under the fixed designation F 1877; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope E 1617 Practice for Reporting Particle Size Characteriza-

1.1 This practice outlines a series of procedures for charac- tion Data2
terization of the morphology, number, size, and size distribu- E 766 Practice for Calibrating the Magnification of Scan-
tion of particles. The methods utilized include sieves, optical, ning Electron Microscopes (SEMs)
SEM, and electrooptical. F 561 Practice for Retrieval and Analysis of Implanted
1.2 These methods are appropriate for particles produced by Medical Devices, and Associated Tissues4
a number of different methods. These include wear test F 660 Practice for Comparing Particle Size in the Use of
machines, total joint simulation systems, abrasion testing, Alternative Types of Particle Counters2
methods for producing particulates, such as shatter boxes or F 661 Practice for Particle Count and Size Distribution
pulverizors, commercially available particles, and particles Measurement in Batch Samples for Filter Evaluation Using
harvested from tissues in animal or clinical studies. an Optical Particle Counter2
1.3 The debris may include metallic, polymeric, ceramic, or F 662 Method for Particle Count and Size Distribution in
any combination of these. Batch Samples for Filter Evaluation Using an Electrical
1.4 The digestion procedures to be used and issues of Resistance Particle Counter2
sterilization of retrieved particles are not the subject of this F 690 Particle Size Distribution of Alumina or Quartz by
practice. Electric Sensing Technique2
1.5 A classification scheme for description of particle mor- F 732 Practice for Reciprocating Pin-on-Flat Evaluation of
phology are included in Appendix X3. Friction and Wear Properties of Polymeric Materials for
1.6 As a precautionary measure, removed debris from Use in Total Joint Prostheses4
implant tissues should be sterilized or minimally disinfected by F 1714 Guide for Gravimetric Wear Assessment of Pros-
an appropriate means that does not adversely affect the thetic Hip Designs in Simulator Devices4
particulate material. This standard does not purport to address F 1715 Guide for Gravimetric Wear Assessment of Pros-
all of the safety concerns, if any, associated with its use. It is thetic Knee Designs in Simulator Devices4
the responsibility of the user of this standard to establish 3. Terminology
appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use. 3.1 Definitions of Terms Specific to This Standard:
3.1.1 agglomerate, n—a mass formed by the cementation of
2. Referenced Documents individual particles, probably by chemical forces.
2.1 ASTM Standards: 3.1.2 aggregate, n—a mass formed of mixtures of particu-
E 11 Specification for Wire-Cloth Sieves for Testing Pur- late and agglomerate particles having a binding force interme-
poses2 diate between agglomerates and flocculates. Formation of
E 20 Practice for Particle Size Analysis of Particulate Sub- aggregates can occur after sampling if the samples are improp-
stances in the Range of 0.2 to 75 µm by Optical Micros- erly kept or treated.
copy3 3.1.3 aspect ratio (AR), n—a ratio of the major to the minor
E 161 Specification for Precision Electroformed Sieves diameter of a particle, which can be used when the major axis
(Square Opening Series)2 does not cross a particle outline (see 11.3.3).
3.1.4 elongation (E), n—ratio of the particle length to the
average particle width (see 11.3.4).
3.1.5 equivalent circle diameter (ECD), n—a measure of the
1
This practice is under the jurisdiction of ASTM Committee F04 on Medical and size of a particle (see 11.3.2 and Appendix X1).
Surgical Materials and Devices and is the direct responsibility of Subcommittee
F04.16 on Biocompatibility.
3.1.6 Feret diameter, n—the mean value of the distance
Current edition approved April 10, 1998. Published March 1999.
2
Annual Book of ASTM Standards, Vol 14.02.
3 4
Discontinued 1994—Vol 14.02. Annual Book of ASTM Standards, Vol 13.01.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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F 1877
between pairs of parallel tangents to a projected outline of a conditions, such as the magnitude and rate of load application,
particle. device configuration, and test environment. Comparison of the
3.1.7 flocculate, n—a group of two or more attached par- morphology and size of particles produced in vitro with those
ticles held together by physical forces, such as surface tension, produced in vivo will provide valuable information regarding
adsorption, or similar forces. the degree to which the method simulates the in vivo condition
3.1.8 form factor (FF), n—a dimensionless number relating being modeled.
area and perimeter of a particle, as directed in 11.3.6.
3.1.9 irregular, adj—a particle that cannot be described as 6. Interferences
round or spherical. A set of standard nomenclature and refer- 6.1 Particles may form aggregates or agglomerates during
ence figures are given in Appendix X2. preparation and storage. These would result in an increase in
3.1.10 particle, n—the smallest discrete unit detectable as measured particle size and decrease in particle number. It is
determined in Test Methods. essential that care be taken to resuspend particles prior to
3.1.11 particle breadth, n—distance between touch points analysis and to note any effects of the dispersant used.
of the shortest Feret pair, orthogonal to length. 6.2 Debris from wear tests or harvested from tissues may
3.1.12 particle length, n—distance between touch points of contain a mixture of materials. Care should be taken to separate
maximum Feret pair. This value will be greater than or equal to the particles and methods utilized to determine the chemical
the maximum Feret diameter. composition of the particles.
3.1.13 rectangular, adj—a particle that approximates a
6.3 Many automated particle counters operate on the as-
square or rectangle in shape.
sumption that the particles are spherical. These methods may
3.1.14 roundness (R), n—a measure of how closely an
not be appropriate for nonspherical debris. Additional methods
object represents a circle as determined in 11.3.5.
should be used to verify size using methods that take aspect
3.1.15 spherical, adj—a particle with a generally spherical
ratio into consideration, for example, SEM image analysis.
shape that appears round in a photograph.
4. Summary of Practice 7. Apparatus
4.1 Particles produced by implant wear in vivo in animal or 7.1 Scanning Electron Microscope (SEM):
clinical studies are harvested from tissues after digestion 7.1.1 Standard SEM equipment can be utilized for many
utilizing methods, such as those in Practice F 561. Particles studies. In special instances, such as with polymeric particles,
generated in vitro, or obtained from commercial sources, are a low acceleration voltage (1-2 kV) machine with a high
used as received, or after digestion, if they were generated in brightness electron source, such as a field emission tip may be
protein solutions, and further separation if there are signs of utilized.
aggregation. A two level analysis is provided. For routine 7.1.2 Elemental analysis may be accomplished with an
analysis, the particles are characterized by the terms of energy dispersive spectrometer (EDS) for energy dispersive
morphology and by size using Feret diameters. For more X-ray analysis (EDXA).
detailed studies, several methods are described that may be 7.2 Optical Microscope—An optical microscope operating
utilized for numerically characterizing their dimensions, size in the transmission mode may be utilized. Dark field illumina-
distribution, and number. tion may enhance visualization of some particles. Polarized
light will facilitate identification of semicrystalline polymeric
5. Significance and Use materials.
5.1 The biological response to materials in the form of small 7.3 Automatic Particle Counters (see Practice F 660):
particles, as from wear debris, often is different significantly 7.3.1 Image Analyzer—This instrument counts particles by
from that to the same materials as larger implant components. size as those particles lie on a microscope slide.
The size and shape (morphology) of the particles may have a 7.3.2 Optical Counter—This instrument measures the area
major effect on the biological response; therefore, this practice of a shadow cast by a particle as it passes a window. From this
provides a standardized nomenclature for describing particles. area the instrument reports the diameter of a circle of equal
Such a unified nomenclature will be of value in interpretation area (see Practice F 661).
of biological tests of responses to particles, in that it will
7.3.3 Electrical Resistance Counter—This instrument mea-
facilitate separation of biological responses associated with
sures the volume of an individual particle. From that volume
shape from those associated with the chemical composition of
the instrument reports the diameter of a sphere of equal volume
debris.
(see Method F 662).
5.2 The quantity, size, and morphology of particles released
as wear debris from implants in vivo may produce an adverse
8. Reagents
biological response which will affect the long term survival of
the device. Characterization of such debris will provide valu- 8.1 Particle-Free (0.2 µm Filtered) Deionized Water, for
able information regarding the effectiveness of device designs nonpolymeric particles.
or methods of processing components and the mechanisms of 8.2 Particle-Free (0.2 µm Filtered) Methanol or Ethanol,
wear. for polymeric or mixed debris.
5.3 The morphology of particles produced in laboratory 8.3 Ultra-Cleaning Reagent, for apparatus or labware clean-
tests of wear and abrasion often is affected by the test ing.

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F 1877
9. Specimen Preparation 11.3.3.1 The AR is the ratio of the major diameter (dmax) to
9.1 Specimens from explanted tissues from animal or clini- the minor diameter (dmin). The major diameter is the longest
cal studies may need to be harvested and digested using straight line that can be drawn between any two points on the
methods, such as those described in Practice F 561. outline. The minor diameter is the longest line perpendicular to
9.2 Particles from in vitro cell culture tests also may need to the major diameter:
be digested and harvested. AR 5 dmax/dmin (2)
9.3 Particles from wear tests should be centrifuged at atleast 11.3.4 The elongation (E), is similar to the AR except it is
400 g for 10 min, and resuspended in water or methanol. more suited for the measurement of much longer particles,
Resuspended particles may be filtered in accordance with especially fibrilar particles, where the major axis line does not
Practice F 561 prior to examination by SEM. stay within the particle boundaries. Refer to particle types A
10. Particle Imaging by Light or Scanning Electron and C in Appendix X1.
Microscopy 11.3.4.1 The E is the ratio of the length (FL) to the breadth
(FW):
10.1 Images may either be captured electronically or pho-
tographically for subsequent analysis. E 5 FL/FW (3)
10.2 For the characterization and measurements to be accu- 11.3.5 The roundness (R) is a measure of how closely a
rate, it is essential that the particles be imaged at the largest particle resembles a circle. The R varies from zero to one in
magnification as possible. The magnifications in Table 1 are magnitude with a perfect circle having a value of one.
recommended. R 5 ~4A!/~p dmax2! (4)
10.3 For particle size distribution measurements, divide
each of the size ranges specified in Table 1, into 10 bins. where:
A = area, and
11. Particle Characterization dmax = the maximum diameter.
11.1 Particle Shape (Morphology)—Refer to the photo- 11.3.6 The form factor (FF) is similar to R but is based on
graphs and classify the morphology of the particles using the the perimeter (p) of the particle outline rather than the major
nomenclature in Appendix X2. diameter. The FF is more sensitive to the variations in
11.2 Routine Particle Size Determination Using Feret Di- roughness of the particle outline.
ameters: FF 5 4pA/p2 (5)
11.2.1 The use of multiple Feret diameters especially is
useful for spherical and rectangular particles. where:
11.2.2 Determine the particle size and aspect ratio as the p = perimeter of the particle outline.
mean of two Feret diameters. 11.4 Other Particles Size Determination Methods:
11.2.3 Calculate the particle size distribution based on the 11.4.1 Particles larger than 20 µm may be determined by
volume of solution used and the size of the filters. sieves described in Specifications E 11 and E 161.
11.3 Detailed Particle Shape Analysis for Irregular Shaped 11.4.2 Particles in liquid suspension may be sized as di-
Particles: rected in Practice F 661 or Method F 662.
11.3.1 Five particle dimensional measurements are provided
using examples shown in Appendix X1.5 One is a measure of 12. Elemental Analysis
particle size while the other four are shape descriptors. 12.1 SEM-EDS analysis should be conducted at a magnifi-
11.3.2 The Equivalent Circle Diameter (ECD) as a Measure cation suggested in 10.2.
of Particle Size: 12.2 Elemental analysis should be conducted for at least 10
11.3.2.1 The ECD is defined as the diameter of a circle with s for each particle. Since detailed compositional analysis is of
an area equivalent to the area (A) of the particle and has the questionable meaning for micron and submicron sized par-
units of length: ticles, it is recommended that composition be determined based
1 on identification of key elemental peaks for the major elements
ECD 5 ~4*A/p!2 (1)
likely to be present in the sample.
11.3.3 The Aspect Ratio (AR) is a Common Measure of
Shape: 13. Report
13.1 Report the following information:
5
The examples provided were analyzed with the NIH Image Program by Landry 13.1.1 The source of the particles and materials and meth-
and Agarwal. A set of macros is available from the Department of Orthopaedics, ods for generation.
University of Texas Health Science Center at San Antonio. 13.1.2 Methods utilized to digest and separate the particles.
13.1.3 Morphological description of the particles.
TABLE 1 13.1.4 Results of particle size and shape analysis.
Magnification Particle Size Range (µm)
10000 0.1 to 1.0 14. Precision and Bias
1000 1 to 10
100 10 to 100 14.1 The precision and bias of this practice has not been
determined.

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F 1877
15. Keywords
15.1 biocompatibility; morphology; particles; SEM; wear
debris

APPENDIXES

(Nonmandatory Information)

X1. SAMPLE FIGURES FOR CALCULATION OF PARTICLE SIZE AND SHAPE

X1.1 See Fig. X1.1.

X2. NOMENCLATURE FOR PARTICLE MORPHOLOGY DESCRIPTION

X2.1 This collection is not intended to be all inclusive, but X2.1.2.4 Angulated (Fig. X2.8).11
rather to provide a frame work for describing the morphology X2.1.2.5 Fines, too small to characterize accurately (Fig.
of particles. X2.9).6
X2.1.3 Globular:
NOTE X2.1—These figures are used as illustrative examples. Sources X2.1.3.1 Clumped, florets, cauliflower (Fig. X2.10).12
are indicated in parentheses (used with permission). X2.1.3.2 Agglomerated, diffuse (Fig. X2.11).13
X2.1.1 Spherical or Spheroidal: X2.1.4 Flakes:
X2.1.1.1 Smooth, round (Fig. X2.1).6 X2.1.4.1 Smooth (Fig. X2.12).12
X2.1.4.2 Roughened (Fig. X2.13).12
X2.1.1.2 Smooth, oblong (Fig. X2.1).6 X2.1.4.3 Irregular (Fig. X2.14).13
X2.1.1.3 Agglomerated, red blood cell - like (Fig. X2.2).7 X2.1.4.4 Shards (probably thin cross sections of flakes)
X2.1.1.4 Rough (Fig. X2.3).6 (Fig. X2.15).6
X2.1.1.5 Spongy, porous (Fig. X2.4).8 X2.1.5 Fibrillar:
X2.1.5.1 Straight (Fig. X2.16).7
X2.1.2 Granular, Irregular:
X2.1.5.2 Twisted (Fig. X2.17 and Fig. X2.18).7
X2.1.2.1 Smooth (Fig. X2.5).9 X2.1.5.3 Hammer head (Fig. X2.19 and Fig. X2.18).13
X2.1.2.2 Rough (Fig. X2.6).10 X2.1.5.4 Tadpole (Fig. X2.19).13
X2.1.2.3 Porous (Fig. X2.7).10 X2.1.5.5 Seahorse (Fig. X2.18).13
X2.1.6 Sharps or Shards:
X2.1.6.1 Flakes, stacked sheets (Fig. X2.20).14
X2.1.6.2 Rectangular, fibers (Fig. X2.21).15
X2.1.6.3 Lathe-like (Fig. X2.22).10
X2.1.6.4 Cuttle fish (Fig. X2.23).12
11
Lerouge S., Huk O., Yahia L.H., Sedel L., “Characterization of In Vivo Wear
6
Lalor, P., donated photographs from Howmedica R and D laboratories. Debris from Ceramic-Ceramic Total Hip Arhroplasties,” J Biomed Mater Res,
7
Szivek J.A., donated sample set. 32:627-633, 1996.
8 12
Jacobs J.J., and Urban R.M., donated photograph. Hailey J.L., Ingham E., Stone M., Wroblewski B.M., Fisher J., “Ultra-High
9
Margevicius K.J., Bauer T.W., McMahon J.T., Brown S.A., Merritt K.,“ Molecular Weight Polyethylene Wear Debris Generated In Vivo and in Laboratory
Isolation and Characterization of Debris in Membranes Around Total Joint Prosthe- Tests: the Influence of Counterface Roughness,” Proc Inst Mech Eng, 210:3-10,
ses,” J Bone Joint Surg, 76A:1664-1675, 1994. 1996.
10 13
Kieswetter K., Bauer T.W., Brown S.A., Van Lente F., Merritt K, “Character- Campbell, P., donated photographs.
14
ization of Calcium Phosphate Powders by ESCA and EDXA,” Biomaterials, Shanbhag A.S., donated photograph.
15
15:183-188, 1994. Bauer T.W., donated photograph.

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F 1877

FIG. X1.1 Sample Figures for Calculation of Particle Size and Shape

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F 1877

FIG. X2.1 Spherical or Spheroidal—Smooth, Round or Oblong FIG. X2.4 Spherical or Spheroidal—Spongy, Porous

FIG. X2.2 Spherical or Spheroidal—Agglomerated Red Blood FIG. X2.5 Granular, Irregular—Smooth
Cell-Like

FIG. X2.6 Granular, Irregular—Rough

FIG. X2.3 Spherical or Spheroidal—Rough

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F 1877

FIG. X2.7 Granular, Irregular—Porouss

FIG. X2.10 Globular—Clumped, Florets, Cauliflower

FIG. X2.8 Granular, Irregular—Angulated

FIG. X2.11 Globular—Agglomerated, Diffuse

FIG. X2.9 Granular, Irregular—Fines Too Small to Characterize

Accurately

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F 1877

FIG. X2.12 Flakes—Smooth

FIG. X2.13 Flakes—Roughened

FIG. X2.14 Flakes—Irregular

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F 1877

FIG. X2.15 Flakes—Shards

FIG. X2.18 Fibrillar—Seahorse / Hammerhead / Twisted

FIG. X2.16 Fibrillar—Straight

FIG. X2.19 Fibrillar—Humerhead / Tadpole

FIG. X2.17 Fibrillar—Twisted

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F 1877

FIG. X2.20 Sharps or Shards—Flakes, Stacked Sheets

FIG. X2.21 Sharps or Shards—Rectangular Fibers

FIG. X2.22 Sharps or Shards—Lathe-Like

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F 1877

FIG. X2.23 Sharps or Shards—Cuttlefish

X3. RATIONALE

X3.1 Establishment and use of a standardized nomenclature names to each type. Thus, communication between investiga-
for describing particulate debris is critical for a wide range of tors should be more precise.
studies regarding implants and devices. By using a common The detailed methods of calculating particle shape have been
vocabulary for particle description, biological responses to developed by M. E. Landry and C. M. Agrawal at the
different shapes of debris can separated from other factors such University of Texas Health Science Center at San Antonio and
as chemistry. Matching morphology of debris produced in the are the basis for a Masters of Science in Engineering thesis by
laboratory with that produced in vivo will better refine the M. E. Landry at the University of Texas at Austin. These
accuracy of laboratory test methods. Characterization of debris
methods are provided as a way to numerically describe
produced in vivo will help in assessment of device perfor-
complicated particle shapes. While not all measurements need
mance.
to be made, standardization of these methods should provide an
The sample morphologies provided are not intended to be all additional data set for description of the wide variety of particle
inclusive of those published in the literature. The intent is to morphologies generated in vivo and in vitro.
provide illustrative examples of morphologies and to assign

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F 1877

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