ASTM D2929-89(2011)
(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 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 7.2.1.
General Information
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2011)
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
of the secondary sulfur Kα X rays emitted on irradiation of the
1.2 Using appropriate standards, the range of the procedure
sample with primary X rays of higher energy from an X-ray
is from approximately 10 ppm to 20% sulfur.
tube with a target of tungsten or chromium. The sulfur Kα
1.3 This test method is proposed specifically as an alterna-
radiation is diffracted with a suitable analyzing crystal and
tive to Test Methods D871, sections on Significance and Use,
detected with a flow-proportional counter. The entire path of
Apparatus, Reagents, Procedure and Calculation of Hydroxyl
the secondary radiation is purged with hydrogen or helium, or
Content,andTestMethodsD817,sectionsonSummaryofTest
evacuated to a pressure of 0.5 mm Hg or less. The intensity of
Method, Significance and Use, Apparatus, Reagents, and
thesulfurKαrays,asestablishedbyastandardcountingperiod
Procedure of Hydroxyl Content.As applied to cellulose esters
and corrected for background radiation, is then converted to
it measures the combined sulfur and sulfur in the accompany-
percent sulfur from calibration data.
ing inorganic salts.
4. Significance and Use
1.4 To determine combined sulfur, the sample, when
soluble, must first be reprecipitated into dilute acid to remove
4.1 This procedure provides a method for determining
the noncombined sulfur compounds.
sulfur content in cellulosic materials by nondestructive means.
Sulfur may be in the form of sulfate esters that may contribute
1.5 The values stated in SI units are to be regarded as the
to thermal instability. Sulfur can also be present as salts that
standard. The values given in parentheses are for information
can cause haze in solutions.
only.
1.6 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
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-
sten or chromium target X-ray tube; hydrogen or helium
2.1 ASTM Standards:
purgingsystemorvacuumsystemtoreach0.5mmHg(orless,
D817Test Methods of Testing CelluloseAcetate Propionate
if desired); 20-mil Soller slits; flow-proportional counter with
and Cellulose Acetate Butyrate
90% argon-10% methane gas mixture; and NaCl, ethylenedi-
D871Test 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 June 1, 2011. Published June 2011. Originally This test method is compiled from four techniques, by incorporating certain
approved in 1970. Last previous edition approved in 2006 as D2929–89(2006). features of each, as follows: “Sulfur in Cellulose Esters by X-ray Emission
DOI: 10.1520/D2929-89R11. 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” by Tripp, Piccolo, Mitcham and O’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 (2011)
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
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
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. 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 Kα X rays of the
7.1 InstrumentStandardizationPellet—Intimatelymixethyl standard samples according to 7.6.
cellulosephthalate,microcrystallinecellulose,orotherselected 7.3.4 Prepare a calibration curve relating sulfur Kα X-ray
matrix with finely divided cystine in a weight ratio of approxi- intensity expressed as net counts per second to percent sulfur.
mately 4:1. Press a portion into a pellet in the sample mold for
7.4 Treatment of Sample Prior to Analysis:
30 s using a pressure of 5000 lb on the mold. Make sure that
7.4.1 To analyze for total sulfur content, no treatment is
thethicknessofthesamplepelletis1.6mm( ⁄16in.)orgreater.
required prior to analysis. If the sample has a high absorbing
coating (for example, saran, PVC, etc.) remove them or a
7.2 Standardization of Instrument:
standard containing a matrix of those materials in equivalent
NOTE 2—Basic standardization techni
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