ASTM D2929-89(2006)
(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
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 D 871, sections on Significance and Use, Apparatus, Reagents, Procedure and Calculation of Hydroxyl Content, and Test Methods D 817, 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.
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 .
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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(Reapproved2006)
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.
1. Scope 3. Summary of Test Method
1.1 This test method covers determination of sulfur content 3.1 The sulfur content of cellulose, cellulose modification,
of cellulosic materials by X-ray fluorescence. orcellulosederivativeisdeterminedbymeasuringtheintensity
1.2 Using appropriate standards, the range of the procedure ofthesecondarysulfurKaXraysemittedonirradiationofthe
is from approximately 10 ppm to 20% sulfur. sample with primary X rays of higher energy from an X-ray
1.3 This test method is proposed specifically as an alterna- tube with a target of tungsten or chromium. The sulfur Ka
tive to Test Methods D871, sections on Significance and Use, radiation is diffracted with a suitable analyzing crystal and
Apparatus, Reagents, Procedure and Calculation of Hydroxyl detected with a flow-proportional counter. The entire path of
Content,andTestMethodsD817,sectionsonSummaryofTest the secondary radiation is purged with hydrogen or helium, or
Method, Significance and Use, Apparatus, Reagents, and evacuated to a pressure of 0.5 mm Hg or less. The intensity of
Procedure of Hydroxyl Content.As applied to cellulose esters thesulfurKarays,asestablishedbyastandardcountingperiod
it measures the combined sulfur and sulfur in the accompany- and corrected for background radiation, is then converted to
ing inorganic salts. percent sulfur from calibration data.
1.4 To determine combined sulfur, the sample, when
4. Significance and Use
soluble, must first be reprecipitated into dilute acid to remove
the noncombined sulfur compounds. 4.1 This procedure provides a method for determining
sulfur content in cellulosic materials by nondestructive means.
1.5 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information Sulfur may be in the form of sulfate esters that may contribute
to thermal instability. Sulfur can also be present as salts that
only.
can cause haze in solutions.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Apparatus
responsibility of the user of this standard to establish appro-
5.1 Wiley Mill, equipped with 60-mesh screen.
priate safety and health practices and determine the applica-
5.2 Sample Mold—Chrome steel die of a size depending on
bility of regulatory limitations prior to use. For a specific
the sample holder to be used.
hazard statement, see 7.2.1.
5.3 Laboratory Press, capable of exerting at least 5000 psi.
2. Referenced Documents
5.4 X-Ray Spectrograph, with following equipment: tung-
2.1 ASTM Standards: sten or chromium target X-ray tube; hydrogen or helium
purgingsystemorvacuumsystemtoreach0.5mmHg(orless,
D817 TestMethodsofTestingCelluloseAcetatePropionate
and Cellulose Acetate Butyrate if desired); 20-mil Soller slits; flow-proportional counter with
90% argon-10% methane gas mixture; and NaCl, ethylenedi-
D871 Test Methods of Testing Cellulose Acetate
amine dextro tartrate (EDT), or pentaerythritol (PET) analyz-
ing crystal.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
Current edition approved April 1, 2006. Published April 2006. Originally This test method is compiled from four techniques, by incorporating certain
approved in 1970. Last previous edition approved in 2000 as D2929–89(2000). features of each, as follows: “Sulfur in Cellulose Esters by X-ray Emission
DOI: 10.1520/D2929-89R06. Spectroscopy,” Eastman Kodak Co.; “ Sulfur in Cellulose Acetate by X-ray
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Fluorescence,” Tennessee Eastman Co.; “X-ray FluorescenceAnalysis of Modified
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Cottons”byTripp,Piccolo,MitchamandO’Connor. Textile Research Journal,Vol
Standards volume information, refer to the standard’s Document Summary page on 34, 1964, p. 773, and FMC Corp.,American Viscose Div. information furnished by
the ASTM website. L. H. Phifer and W. B. Swann.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2929–89 (2006)
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 Ka.
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
used to establish the calibration curve in a matrix as nearly
because of the use of thinner windows in the chromium tube. However,
identical to that of the sample as possible. Distribute the
either the chromium or the tungsten target tube is suitable for sulfur
sulfur-containingcomponentveryuniformlyinthematrix.The
analysis. If a pulse height analyzer is available as a part of the X-ray
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.
7.3.1.1 As a calibration standard for cellulose, microcrys-
6. Reagents
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. 143B.
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 Ka X rays of the
7.1 Instrument Standardization Pellet— Intimately mix
standard samples according to 7.6.
ethyl cellulose phthalate, microcrystalline cellulose, or other
7.3.4 Prepare a calibration curve relating sulfur Ka X-ray
selected matrix with finely divided cystine in a weight ratio of
intensity expressed as net counts per second to percent sulfur.
approximately 4:1. Press a portion into a pellet in the sample
7.4 Treatment of Sample Prior to Analysis:
mold for 30 s using a pressure of 5000 lb on the mold. Make
1 7.4.1 To analyze for total sulfur content, no treatment is
sure that the thickness of the sample pellet is 1.6 mm ( ⁄16 in.)
required prior to analysis. If the sample has a high absorbing
or greater.
coating (for example, saran, PVC, etc.) remove them or a
7.2 Standardization of Instrument:
standard containing a matrix of
...
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