ASTM D2929-89(2000)
(Test Method)Standard Test Method for Sulfur Content of Cellulosic Materials by X-ray Fluorescence
Standard Test Method for Sulfur Content of Cellulosic Materials by X-ray Fluorescence
SCOPE
1.1 This test method covers determination of sulfur content of cellulosic materials by X-ray fluorescence.
1.2 Using appropriate standards, the range of the procedure is from approximately 10 ppm to 20% sulfur.
1.3 This test method is proposed specifically as an alternative to Test Methods D871, Sections 29 to 33, and Test Methods D817, Sections 39 to 43. As applied to cellulose esters it measures the combined sulfur and sulfur in the accompanying inorganic salts.
1.4 To determine combined sulfur, the sample, when soluble, must first be reprecipitated into dilute acid to remove the noncombined sulfur compounds.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Note 3.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D2929–89(Reapproved2000)
Standard Test Method for
Sulfur Content of Cellulosic Materials by X-ray
Fluorescence
This standard is issued under the fixed designation D2929; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope radiation is diffracted with a suitable analyzing crystal and
detected with a flow proportional counter. The entire path of
1.1 This test method covers determination of sulfur content
the secondary radiation is purged with hydrogen or helium, or
of cellulosic materials by X-ray fluorescence.
evacuated to a pressure of 0.5 mm Hg or less. The intensity of
1.2 Using appropriate standards, the range of the procedure
thesulfurKarays,asestablishedbyastandardcountingperiod
is from approximately 10 ppm to 20% sulfur.
and corrected for background radiation, is then converted to
1.3 This test method is proposed specifically as an alterna-
percent sulfur from calibration data.
tive to Test Methods D871, Sections 29 to 33, and Test
Methods D817, Sections 39 to 43. As applied to cellulose
4. Significance and Use
esters it measures the combined sulfur and sulfur in the
4.1 This procedure provides a method for determining
accompanying inorganic salts.
sulfur content in cellulosic materials by nondestructive means.
1.4 To determine combined sulfur, the sample, when
Sulfur may be in the form of sulfate esters that may contribute
soluble, must first be reprecipitated into dilute acid to remove
to thermal instability. Sulfur can also be present as salts that
the noncombined sulfur compounds.
can cause haze in solutions.
1.5 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
5. Apparatus
only.
5.1 Wiley Mill, equipped with 60-mesh screen.
1.6 This standard does not purport to address all of the
5.2 Sample Mold—Chrome steel die of a size depending on
safety concerns, if any, associated with its use. It is the
the sample holder to be used.
responsibility of the user of this standard to establish appro-
5.3 Laboratory Press, capable of exerting at least 5000 psi.
priate safety and health practices and determine the applica-
5.4 X-Ray Spectrograph, with following equipment: tung-
bility of regulatory limitations prior to use. For a specific
sten or chromium target X-ray tube; hydrogen or helium
hazard statement, see Note 3.
purgingsystemorvacuumsystemtoreach0.5mmHg(orless,
2. Referenced Documents if desired); 20-mil Soller slits; flow proportional counter with
90% argon-10% methane gas mixture; and NaCl, ethylenedi-
2.1 ASTM Standards:
amine dextro tartrate (EDT), or pentaerythritol (PET) analyz-
D817 Test Methods of Testing Cellulose Acetate Propi-
2 ing crystal.
onate and Cellulose Acetate Butyrate
D871 Test Methods of Testing Cellulose Acetate
NOTE 1—Radiation from a chromium target tube appears to be more
effective than radiation from a tungsten target tube for exciting sulfur Ka.
3. Summary of Test Method
This may be because a larger part of the “white” radiation of the
chromium tube is at the longer wavelength region of the spectrum, or
3.1 The sulfur content of cellulose, cellulose modification,
because of the use of thinner windows in the chromium tube. However,
orcellulosederivativeisdeterminedbymeasuringtheintensity
either the chromium or the tungsten target tube is suitable for sulfur
ofthesecondarysulfurKaXraysemittedonirradiationofthe
analysis. If a pulse height analyzer is available as a part of the X-ray
sample with primary X rays of higher energy from an X-ray
instrumentation, its use is very helpful in reducing background radiation.
tube with a target of tungsten or chromium. The sulfur Ka
This test method is compiled from four techniques, by incorporating certain
This test method is under the jurisdiction of ASTM Committee D-1 on Paint features of each, as follows: “Sulfur in Cellulose Esters by X-ray Emission
and Related Coatings, Materials, andApplications and is the direct responsibility of Spectroscopy,” Eastman Kodak Co.; “Sulfur in Cellulose Acetate by X-ray
Subcommittee D01.36 on Cellulose and Cellulose Derivatives. Fluorescence,” Tennessee Eastman Co.; “X-ray FluorescenceAnalysis of Modified
Current edition approved Oct. 27, 1989. Published December 1989. Originally Cottons” by Tripp, Piccolo, Mitcham and O’Connor. Textile Research Journal, Vol
e1
published as D2929–70. Last previous edition D2929–70(1985) . 34, 1964, p. 773, and FMC Corp.,American Viscose Div. information furnished by
Annual Book of ASTM Standards, Vol 06.03. L. H. Phifer and W. B. Swann.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2929
Useofapulseheightanalyzerismandatoryforthedeterminationofsulfur
physical form of the matrix (powder, flake, pellet, or sheet) is
below 100 to 200 ppm level.
asignificantvariable.Foraccurateworkitmaybenecessaryto
have separate calibrations for each form of sample.
6. Reagents
7.3.1.1 As a calibration standard for cellulose, microcrys-
6.1 Ethyl Cellulose Phthalate.
talline cellulose containing intimately mixed known amounts
6.2 Microcrystalline Cellulose.
of cystine may be used.Achemical analysis of the standards is
6.3 Cystine, NIST primary standard No. 143B.
generally not necessary.
7.3.2 Prepare the samples for analysis according to 7.4 and
7. Procedure
7.5.
7.1 Instrument Standardization Pellet— Intimately mix
7.3.3 Measure the intensities of the sulfur Ka X rays of the
ethyl cellulose phthalate, microcrystalline cellulose, or other
standard samples according to 7.6.
selected matrix with finely divided cystine in a weight ratio of
7.3.4 Prepare a calibration curve relating sulfur Ka X-ray
approximately 4:1. Press a portion into a pellet in the sample
intensity expressed as net counts per second to percent sulfur.
mold for 30 s using a pressure of 5000 lb on the mold. Make
7.4 Treatment of Sample Prior to Analysis:
sure that the thickness of the sample pellet is 1.6 mm ( ⁄16 in.)
7.4.1 To analyze for total sulfur content, no treatment is
or greater.
required prior to analysis. If the sample has a high absorbing
7.2 Standardization of Instrument:
coating (for example, saran, PVC, etc.) remove them or a
standard containing a matrix of those materials in equivalent
NOTE 2—Basic standardization techniques and operating parameters
vary from instrument to instrument.The manufacturer’s literature and the
concentrations must be prepared.
analyst’s knowledge of the performance characteristics of the equipment
7.4.2 When analyzing for combined sulfur content, as in a
should be used as a guide in performing this function.
cellulose ester, remove the uncombined sulfur as follows:
7.2.1 Placeastandardizationpelletinthesampleholderand
7.4.2.1 Dissolve25gofsampleinapproximately300
...
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