Designation: E 259 – 98

AMERICAN SOCIETY FOR TESTING AND MATERIALS

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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Practice for

Preparation of Pressed Powder White Reflectance Factor
Transfer Standards for Hemispherical and Bi-Directional
Geometries1
This standard is issued under the fixed designation E 259; 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.

INTRODUCTION

The internationally accepted standard of reflectance is the perfect reflecting diffuser. This ideal
reflecting surface reflects 100 % of the incident radiant power such that the radiance is the same for
all directions within the hemisphere above the surface. No physical realization of this standard exists.
Optical properties of standards prepared from pressed plaques of magnesium carbonate (MgCO3),
barium sulfate (BaSO4), or polytetrafluoroethylene (PTFE) can approximate an ideal standard. For
further information see CIE Publication No. 46 (1).2 The principal use of a white reflectance factor
standard is to transfer an absolute scale of reflectance to a more durable material or from one
instrument to another. In theory, it should be easy to do this transfer from first principles. In practice,
one is likely to need values for parameters that are unknown, proprietary, or require a high level of
skill. Some, but not all, of those parameters are discussed in this practice.

1. Scope 2. Referenced Documents

1.1 This practice covers procedures for preparing pressed 2.1 ASTM Standards:
powder transfer standards. These standards can be used in the E 284 Terminology of Appearance3
near-ultraviolet, visible and near-infrared region of the electro-
magnetic spectrum. Procedures for calibrating the reflectance 3. Terminology
factor of materials on an absolute basis are contained in CIE 3.1 Terms and definitions in Terminology E 284 are appli-
Publication No. 44 (2). Pressed powder standards are used as cable to this practice.
transfer standards for such calibrations because they have a 3.2 Definitions—The following definitions are particularly
high reflectance factor that is nearly constant with wavelength, important to this practice:
and because the geometric distribution of reflected flux re- 3.2.1 perfect reflecting diffuser—ideal reflecting surface that
sembles that from the perfect reflecting diffuser. neither absorbs nor transmits light, but reflects diffusely, with
1.2 The values stated in SI units are to be regarded as the the radiance of the reflecting surface being the same for all
standard. The values in parentheses are for information only. reflecting angles, regardless of the angular distribution of the
1.3 This standard does not purport to address all of the incident light. (1990)
safety concerns, if any, associated with its use. It is the 3.2.2 reflectance, r, n—ratio of the reflected radiant or
responsibility of the user of this standard to establish appro- luminous flux to the incident flux in the given conditions.
priate safety and health practices and determine the applica- [CIE]A
bility of regulatory limitations prior to use. 3.2.3 The term reflectance is often used in a general sense or
as an abbreviation for reflectance factor. Such usage may be
assumed unless the above definition is specifically required by
the context. (1989b)
1
This practice is under the jurisdiction of ASTM Committee E-12 on Color and 3.2.4 reflectance factor, R, n—ratio of the flux reflected
Appearance and is the direct responsibility of Subcommittee E12.02 on Spectro-
photometry and Colorimetry.
from the specimen to the flux reflected from the perfect
Current edition approved Oct. 10, 1998. Published March 1999. Originally reflecting diffuser under the same geometric and spectral
published as E 259 – 65. Last previous edition E 259 – 97.
2
conditions of measurement. [CIE]B(1988)
The boldface numbers in parentheses refer to the list of references at the end of
this practice. 4. Summary of Practice
4.1 Procedures are given for the preparation of white

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Annual Book of ASTM Standards, Vol 06.01.

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 E 259
6. Apparatus
6.1 The basic apparatus for producing a pressed powder
standard includes a powder press, powder containers and a
balance. There are presently two commercial suppliers of
powder presses.4 The press and receptacles can also be made in
a local machine shop. A suggested configuration is shown in
Fig. 1. The optical surface of the plaque should be pressed
against a surface of ground glass or poly(methyl methacrylate)
to provide a matte finish on the pressed plaque. Powder
receptacles should be at least 5 mm deep for BaSO4 and at least
10 mm deep for PTFE.

7. Reagents and Materials

NOTE 1—The collar and receptacle should be securely held in place
before pressing the powder. 7.1 Barium Sulfate—the barium sulfate should be of the
FIG. 1 Example Powder Press highest purity. It should be specially refined for optical and
spectroscopic use (3).
7.2 Polytetrafluoroethylene—the PTFE (4) should also be
reference standards of diffuse reflectance factor and diffuse specially refined for optical and spectroscopic use but some
radiance factor. The recommended materials are white powders commercial grades have been found to be acceptable substi-
that are pressed into plaques. These plaques provide close tutes. (5) There is currently no commercial source for small
approximations to the optical properties of the perfect reflect- quantities of optical grade PTFE powder. Large quantities
ing diffuser, and may be used to transfer a scale of absolute (drums) of commercial grade PTFE can be obtained from
reflectance to another material or to an instrument. manufacturers.

5. Significance and Use 8. Procedure

5.1 All commercial reflectometers measure relative reflec- 8.1 Store all powdered reflectance standards in tightly
tance. The instrument reading is the reflectance factor, the ratio capped glass containers. If the powder is purchased in plastic
of the light reflected by a reference specimen to that reflected containers, transfer it to a glass container as soon as possible.
by a test specimen. That ratio is dependent on specific Before using the powder, place it in a glass blender equipped
instrument parameters. with stainless-steel or PTFE-coated blades and pulverize to a
5.2 National standardizing laboratories and some research uniform consistency. Transfer the quantity of powder to be
laboratories measure reflectance on instruments calibrated used with stainless steel or PTFE-coated spoons. Perform the
from basic principles, thereby establishing a scale of absolute whole operation in a draft-free location, away from sources of
reflectance as described in CIE Publication No. 44 (2). These small particulate contamination, filters, sweaters, windows,
measurements are sufficiently difficult that they are usually left ovens, etc. Perform all measurements (weight, height, width,
to laboratories that specialize in them. depth, volume, area, etc.) with adequate precision to ensure
5.3 A standard that has been measured on an absolute scale that the final density is within 5 % of the specified value. The
could be used to transfer that scale to a reflectometer. While most reproducible standards are made by pressing the powder
such procedures exist, the constraints placed on the mechanical to a specific density. Thus, determine the mass of the powder to
properties restrict the suitability of some optical properties, be used from the volume of the receptacle.
especially those properties related to the geometric distribution 8.2 Barium Sulfate—Press BaSO4 to a density of 2000
of the reflected light. Thus, reflectance factor standards which kg/m3(2.0 gm/cm3) and a thickness of at least 5 mm. Press
are sufficiently rugged and able to be cleaned, depart consid- several specimens in succession. Select matched pairs to be
erably from the perfect diffuser in the geometric distribution of representative of the contents of the bottle of powder. Keep the
reflected radiance. pressed plaques in a covered desiccator when not in use. Some
5.4 The geometric distribution of reflected radiance from a suppliers of BaSO4 provide calibration values with each bottle
pressed powder plaque is sufficiently diffuse to provide a of powder, other suppliers provide only 3 or 4 quality reference
dependable calibration of a directional-hemispherical reflecto- checks and a reference to published values of reference
meter. Although pressed powder standards are subject to standards prepared from the powder. Table 1 gives the 6°/
contamination and breakage, the directional-hemispherical re- diffuse reflectance factor values for Eastman White Reflectance
flectance factor of pressed powder standards can be sufficiently Standard (3).
reproducible from specimen to specimen made from a given lot 8.2.1 Another description of this procedure is found in Ref.
of powder, so as to allow one to assign absolute reflectance (4).
factor values to all the powder in a lot.
5.5 This practice describes how to prepare white reflectance 4
Powder press conforming to ISO 2469 and DIN 5033 is available from Carl
factor standards from a powder in a manner that allows a Zeiss Canada, Ltd., 45 Valleybrook Drive, Don Mills, Ontario M3B-2S6, Canada,
standardizing laboratory to assign the absolute scale of reflec- Part Number 505866; and Technidyne Corporation, 100 Quality Avenue, New
tance to the plaque. Albany, IN 47150-2272, Part Number 176601.

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 E 259
TABLE 1 6°/Diffuse Reflectance Factor of Eastman White TABLE 3 45°/0 Diffuse Reflectance Factor of Pressed PTFE
Reflectance Standard Pressed BaSO4 PowderA PowderA
Wavelength, nm Reflectance Factor Wavelength, nm Reflectance FactorB
300 0.968 380 1.002
350 0.979 390 1.003
400 0.987 400 1.005
450 0.991 410 1.006
500 0.991 420 1.006
550 0.992 430 1.007
600 0.992 440 1.007
650 0.992 450 1.008
700 0.992 460 1.008
750 0.992 470 1.009
800 0.992 480 1.009
850 0.991 490 1.009
900 0.990 500 1.010
950 0.988 510 1.010
1000 0.986 520 1.010
530 1.010
540 1.011
8.3 Polytetrafluoroethylene—Press PTFE to a density of 550 1.011
560 1.011
1000 kg/m3 (1.0 gm/cm3) and a thickness of at least 10 mm. 570 1.011
The spectral reflectance, which is a function of density, has a 580 1.011
broad maximum near this density. Prepare several specimens in 590 1.011
600 1.011
succession. Matched pairs are selected to be representative of 610 1.011
the contents of the container of powder. Keep the pressed 620 1.012
630 1.012
plaques in a desiccator when not in use. PTFE has a high 640 1.012
dielectric constant and can be very sensitive to airborne 650 1.012
particulates. Such contamination can make the material slightly 660 1.012
670 1.012
fluorescent and reduce its reflectance in the near-ultraviolet 680 1.012
spectral region. Table 2 lists the 6°/diffuse reflectance factor 690 1.012
values (6) and Table 3 lists the 45°/0° reflectance factor values 700 1.012
710 1.013
(7) of PTFE as determined by the National Institute of 720 1.014
Standards and Technology (NIST). 730 1.015
740 1.015
9. Precision and Bias 750 1.016
760 1.016
9.1 The National Institute of Standards and Technology and 770 1.017
the Inter-Society Color Council Project Committee 22, Mate- A
Density 5 1000 kg/m3 and thickness $ 5 mm.
rials for Instrument Calibration, have carried out collaborative B
Accurate to 6 0.003.
tests to determine the precision and bias of the preparation of
PTFE reflectance factor standards (8). The standard deviation
of three determinations of the reflectance factor of PTFE by the 6 0.005. From the 9 laboratories participating in the round-
NIST ranged from 0.0002 to 0.0008 over the spectral range 300 robin experiment, 17 specimens were returned. The results are
to 1000 nm. The measured reflectances of PTFE from two shown in Table 4 for the wavelength range 300 to 1000 nm.
manufacturers exhibited differences of from −0.002 to +0.004 9.2 The National Institute of Standards and Technology
over the same range with the largest differences near the ends carried out collaborative tests to determine the uncertanities in
of the range and a constant measurement uncertainty of the preparation of PTFE for use as transfer standards of
reflectance factor for the 45°/0° geometry. Duplicate pressings
TABLE 2 6°/Diffuse Reflectance Factor of Pressed PTFE
PowderA TABLE 4 Average and Standard Deviation of 6°/Diffuse
Wavelength, nm Reflectance Factor Reflectance Factors of 17 PTFE Plaques Prepared by 9
Laboratories
300 0.984
350 0.990 Reflectance Factor
400 0.993 Wavelength, nm
A Standard
450 0.993 Average
DeviationB
500 0.994
550 0.994 300 0.9792 0.0063
600 0.994 350 0.9883 0.0021
650 0.994 400 0.9911 0.0018
700 0.994 500 0.9919 0.0020
750 0.994 600 0.9915 0.0023
800 0.994 700 0.9914 0.0023
850 0.994 800 0.9912 0.0024
900 0.994 1000 0.9910 0.0024
950 0.994 A
Average Density 5 926.2 kg/m 3.
1000 0.994 B
Standard Deviation 5 85.7 kg/m3.

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 E 259
were made of the same PTFE in ten different laboratories. The and approximately 1.5 % at wavelengths below 500 nm in the
standard deviations of the measured reflectance factor, as a visible spectral region.
function of wavelength is shown in Table 5. Table 6 shows the 10. Keywords
measured reflectance factors, averages, and standard deviations
of four different drums of PTFE. The total uncertainty for the 10.1 bi–directional optical measuring system; hemispherical
transfer is approximately 1 % at wavelengths above 500 nm optical measuring system; integrating sphere; material stan-
dards; reflectance and reflectivity; transfer standards

TABLE 5 Difference From the Average of PTFE Powder Pressings Ten Laboratories (A-J) and Two Replicates (1-2)
Wavelength, nm
380 450 600 700 770
A1 0.002 0.004 0.002 0.003 0.004
A2 0.004 0.006 0.003 0.001 0.003
B1 -0.001 0.001 0.000 0.000 -0.007
B2 -0.005 0.000 -0.001 0.000 -0.001
C1 0.009 0.006 0.004 0.004 0.005
C2 -0.005 -0.005 -0.004 -0.006 -0.005
D1 0.001 0.002 0.001 0.001 0.002
D2 0.007 0.004 0.003 0.002 0.002
E1 -0.003 0.002 0.002 0.003 0.004
E2 -0.004 -0.004 -0.005 -0.006 -0.006
F1 0.000 -0.011 -0.004 0.008 0.004
F2 -0.001 0.000 0.001 0.001 0.001
G1 -0.002 -0.004 -0.004 -0.004 -0.005
G2 0.009 0.005 0.002 0.002 0.004
H1 -0.012 -0.006 -0.006 -0.008 -0.007
H2 0.010 0.001 0.000 0.001 0.002
I1 -0.003 0.000 -0.002 -0.001 0.000
I2 0.006 -0.002 0.002 0.002 0.005
J1 -0.010 -0.007 -0.005 -0.007 -0.004
J2 0.003 0.007 0.006 0.008 0.006

Standard Deviation (k52) 0.012 0.010 0.006 0.008 0.008

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TABLE 6 45°/0° Reflectance Factor of Pressed PTFE Powder From Different Drums of PTFE
Wavelength, nm
380 420 470 550 630 700 770
Drum 1 1.005 1.008 1.011 1.013 1.012 1.013 1.016
Drum 2 1.001 1.006 1.009 1.011 1.012 1.012 1.017
Drum 3 0.993 0.999 1.006 1.007 1.010 1.011 1.016
Drum 4 1.007 1.010 1.011 1.012 1.013 1.013 1.017

Mean 1.002 1.006 1.009 1.011 1.012 1.012 1.017

Standard Deviation 0.013 0.010 0.008 0.005 0.002 0.002 0.001

REFERENCES

(1) Publication CIE No. 46—A Review of Publications on Properties and (5) Spyak, P. R., Lansard, C., “Reflectance Properties of Pressed Algoflon
Reflection Values of Material Reflection Standards, available from F6: A Replacement Reflectance-Standard Material for Halon”, Applied
USNC/CIE. Request ordering information from Secretary USNC, Optics, Vol 36, No. 13, pp. 2963-2970 1997.
NIST, Room A317/220, Gaithersburg, MD 20899. (6) Weidner, V. R., and Hsia, J. J.,“ Reflection Properties of Pressed
(2) Publication CIE No. 44—Absolute Methods for Reflection Measure- Polytetrafluoroethylene Powder,” J. Opt. Soc. Am., Vol 71, 1981, pp
ments, available from USNC/CIE. Request ordering information from
856–861.
Secretary USNC, NIST, Room B306/220, Gaithersburg, MD 20899.
(3) Grum, F., and Wightman, T. E., “Absolute Reflectance of Eastman (7) Barnes, P. Y., Hasia, J. J., “45°/0° Reflectance Factors of Pressed
White Reflectance Standard”, Applied Optics, Vol 16, 1977, pp. Polytetrafluoroethylene (PTFE) Powder”, NIST Technical Note 1413,
2775–2776. U.S. Government Printing Office, Washington, D. C., 1995.
(4) Publication CIE No. 38—Radiometric and Photometric Characteris- (8) Weidner, V. R., Hsia, J. J., and Adams, B.,“ Laboratory Inter-
tics of Materials and Their Measurement, available from US NC/CIE. comparision Study of Pressed Polytetrafluoroethylene Powder Reflec-
Request ordering information from Secretary USNC, NIST, Room tance Standards,” Applied Optics, Vol 24, 1985, pp. 2225–2230.
B306/220, Gaithersburg, MD 20899.

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