ASTM D2929-89(2019)e1
(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
SIGNIFICANCE AND USE
4.1 This procedure provides a method for determining sulfur content in cellulosic materials by nondestructive means. Sulfur may be in the form of sulfate esters that may contribute to thermal instability. Sulfur can also be present as salts that can cause haze in solutions.
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 on Significance and Use, Apparatus, Reagents, Procedure and Calculation of Hydroxyl Content, and Test Methods D817, sections on Summary of Test Method, Significance and Use, Apparatus, Reagents, and Procedure of Hydroxyl Content. 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 7.2.1.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: D2929 − 89 (Reapproved 2019)
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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Section 6.3 primary standard name was updated in October 2019.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers determination of sulfur content
D817Test Methods of Testing CelluloseAcetate Propionate
of cellulosic materials by X-ray fluorescence.
and Cellulose Acetate Butyrate
1.2 Using appropriate standards, the range of the procedure
D871Test Methods of Testing Cellulose Acetate
is from approximately 10 ppm to 20% sulfur.
3. Summary of Test Method
1.3 This test method is proposed specifically as an alterna-
tive to Test Methods D871, sections on Significance and Use,
3.1 The sulfur content of cellulose, cellulose modification,
Apparatus, Reagents, Procedure and Calculation of Hydroxyl
orcellulosederivativeisdeterminedbymeasuringtheintensity
Content,andTestMethodsD817,sectionsonSummaryofTest
of the secondary sulfur Kα X rays emitted on irradiation of the
Method, Significance and Use, Apparatus, Reagents, and
sample with primary X rays of higher energy from an X-ray
Procedure of Hydroxyl Content.As applied to cellulose esters
tube with a target of tungsten or chromium. The sulfur Kα
it measures the combined sulfur and sulfur in the accompany-
radiation is diffracted with a suitable analyzing crystal and
ing inorganic salts.
detected with a flow-proportional counter. The entire path of
the secondary radiation is purged with hydrogen or helium, or
1.4 To determine combined sulfur, the sample, when
evacuated to a pressure of 0.5 mm Hg or less. The intensity of
soluble, must first be reprecipitated into dilute acid to remove
thesulfurKαrays,asestablishedbyastandardcountingperiod
the noncombined sulfur compounds.
and corrected for background radiation, is then converted to
1.5 The values stated in SI units are to be regarded as the
percent sulfur from calibration data.
standard. The values given in parentheses are for information
only.
4. Significance and Use
1.6 This standard does not purport to address all of the
4.1 This procedure provides a method for determining
safety concerns, if any, associated with its use. It is the
sulfur content in cellulosic materials by nondestructive means.
responsibility of the user of this standard to establish appro-
Sulfur may be in the form of sulfate esters that may contribute
priate safety, health, and environmental practices and deter-
to thermal instability. Sulfur can also be present as salts that
mine the applicability of regulatory limitations prior to use.
can cause haze in solutions.
For a specific hazard statement, see 7.2.1.
1.7 This international standard was developed in accor- 5. Apparatus
dance with internationally recognized principles on standard-
5.1 Wiley Mill, equipped with 60-mesh screen.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barriers to Trade (TBT) Committee.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
This test method is compiled from four techniques, by incorporating certain
This test method is under the jurisdiction of ASTM Committee D01 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. 1, 2019. Published October 2019. Originally Cottons” by Tripp, Piccolo, Mitcham and O’Connor. Textile Research Journal,Vol
approved in 1970. Last previous edition approved in 2011 as D2929–89(2011). 34, 1964, p. 773, and FMC Corp.,American Viscose Div. information furnished by
DOI: 10.1520/D2929-89R19E01. L. H. Phifer and W. B. Swann.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D2929 − 89 (2019)
5.2 Sample Mold—Chrome steel die of a size depending on the detector voltage about midway on the plateau. Set the
the sample holder to be used. minimum pulse rejection voltage at about 5 V and the ∆E at
about 10 V. Observe the intensity without the pulse height
5.3 Laboratory Press, capable of exerting at least 5000 psi.
analyzer on. With the pulse height analyzer on, change either
5.4 X-Ray Spectrograph, with following equipment: tung-
the amplifier gain control or the detector voltage until as near
sten or chromium target X-ray tube; hydrogen or helium
as possible the same intensity as without the analyzer is
purgingsystemorvacuumsystemtoreach0.5mmHg(orless,
obtained. Then increase or decrease the ∆E control just until a
if desired); 20-mil Soller slits; flow-proportional counter with
maximum intensity is reached.
90% argon-10% methane gas mixture; and NaCl, ethylenedi-
7.3 Calibration for Measurement of Sulfur:
amine dextro tartrate (EDT), or pentaerythritol (PET) analyz-
7.3.1 Select five or more representative cellulosic samples
ing crystal.
whose sulfur contents, as determined by chemical analysis
NOTE 1—Radiation from a chromium target tube appears to be more
according to Test Methods D817 or D871, completely cover
effective than radiation from a tungsten target tube for exciting sulfur Kα.
the required range. Since X-ray fluorescence intensities are
This may be because a larger part of the “white” radiation of the
functions of concentrations per unit volume, prepare standards
chromium tube is at the longer wavelength region of the spectrum, or
because of the use of thinner windows in the chromium tube. However, used to establish the calibration curve in a matrix as nearly
either the chromium or the tungsten target tube is suitable for sulfur
identical to that of the sample as possible. Distribute the
analysis. If a pulse height analyzer is available as a part of the X-ray
sulfur-containingcomponentveryuniformlyinthematrix.The
instrumentation, its use is very helpful in reducing background radiation.
physical form of the matrix (powder, flake, pellet, or sheet) is
Useofapulseheightanalyzerismandatoryforthedeterminationofsulfur
asignificantvariable.Foraccurateworkitmaybenecessaryto
below 100 to 200 ppm level.
have separate calibrations for each form of sample.
6. Reagents
7.3.1.1 As a calibration standard for cellulose, microcrys-
talline cellulose containing intimately mixed known amounts
6.1 Ethyl Cellulose Phthalate.
ofcystinemaybeused.Achemicalanalysisofthestandardsis
6.2 Microcrystalline Cellulose.
generally not necessary.
6.3 Cystine, NIST primary standard No. 143D.
7.3.2 Prepare the samples for analysis according to 7.4 and
7.5.
7. Procedure
7.3.3 Measure the intensities of the sulfur Kα X rays of the
7.1 In
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