ASTM D5896-96(2019)e1

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: D5896 − 96 (Reapproved 2019)
Standard Test Method for
Carbohydrate Distribution of Cellulosic Materials
This standard is issued under the fixed designation D5896; 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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Section 8.1 was editorially updated in December 2019.
1. Scope 3. Terminology
3.1 For standard terminology of cellulose and cellulose
1.1 This test method covers the determination of the carbo-
derivatives, see Terminology D1695.
hydrate composition of cellulosic materials such as ground
wood meal, chemically refined pulp, mechanical pulps,
3.2 Abbreviations:
brownstocks, and plant exudates (gums) by ion chromatogra-
3.2.1 IC—ion chromatography,
phy. This test method is suitable for rapid, routine testing of
3.2.2 SPE—solid phase extraction,
large numbers of samples with high accuracy and precision.
3.2.3 PAD—pulsed amperometric detector,
For a review of this technique, see Lee (1). 3.2.4 PED—pulsed electrochemical detector,
3.2.5 mM—millimolar.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 IC analysis of cellulosics requires the following opera-
1.3 This standard does not purport to address all of the
tions:
safety concerns, if any, associated with its use. It is the
(1) sample preparation,
responsibility of the user of this standard to establish appro-
(2) total hydrolysis,
priate safety, health, and environmental practices and deter-
(3) dilution,
mine the applicability of regulatory limitations prior to use.
(4) SPE,
For hazard statement, see Section 8. (5) ion chromatographic analysis, and
(6) calibration/calculation.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
5.1 This test method requires total hydrolysis of carbohy-
Development of International Standards, Guides and Recom-
drate material to monosaccharides, and is thus applicable to
mendations issued by the World Trade Organization Technical
any cellulosic or related material that undergoes substantial
Barriers to Trade (TBT) Committee.
hydrolysis, including cellulose derivatives such as cellulose
acetate.
2. Referenced Documents
5.2 The carbohydrate composition of a cellulosic material
2.1 ASTM Standards:
can be expressed on the basis of the total initial sample, or on
D1193 Specification for Reagent Water
the basis of the carbohydrate portion of the sample.The former
D1695 Terminology of Cellulose and Cellulose Derivatives
requires quantitative handling and may require special knowl-
edge of the other components present in order to establish the
absolute carbohydrate level or determine individual wood
This test method is under the jurisdiction of ASTM Committee D01 on Paint
hemicelluloses such as galactoglucomannan, etc. Since the
and Related Coatings, Materials, andApplications and is the direct responsibility of
solid portion of purified pulps is almost all carbohydrate
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
(98 + %), the latter basis is often used to express the carbo-
Current edition approved Dec. 1, 2019. Published December 2019. Originally
approved in 1996. Last previous edition approved in 2012 as D5896 – 96 (2012).
hydrate distribution as a percent.
DOI: 10.1520/D5896-96R19E01.
5.3 Ifheatedunderalkalineconditions,isomericsugarsmay
The boldface numbers in parentheses refer to the list of references at the end of
this test method.
begin to appear in the chromatogram. The major impurity
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
present in purified pulps is saccharinic acids. These acidic
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
components, and other anions such as sulfate, carbonate, and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. acetate are removed by a strong base anion exchange SPE, and
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5896 − 96 (2019)
would need to be determined separately to get a more exact 11.5 Maintain pressure at 15 psi for 1 h.
carbohydrate distribution.
11.6 Cool to room temperature and dilute the sample to
avoid overloading the analytical column (usually a dilution
6. Apparatus
between 1 to 20 and 1 to 50 is adequate). Dilute with water
6.1 Blender.
containing a standard such that its concentration in the diluted
sample is 2 ppm. D-Fucose (6-deoxy-D-galactose) or 2-deoxy-
6.2 Screw Cap Culture Tubes, 25 by 150 mm, outside
D-glucose make good internal standards.
diameter.
11.7 Neutralization of the sample is not required, but
6.3 Refrigerator.
improved resolution may occur if the sample is adjusted to pH
6.4 Pressure Cooker.
6–6.5 during the dilution step. Neutralization is recommended
6.5 SPE Cartridges.
if the sample is to be stored before analysis.
6.6 Water Bath.
11.8 Prepare an anion exchange SPE cartridge with 5 mLof
water, pass 5 mL of sample through the cartridge, discarding
6.7 Ion Chromatograph.
the first 3 mL, and use the remaining 2 mL to fill a 0.5-mL
6.8 Moisture Balance.
injectionvial.Additional0.5-mLinjectionvialsmaybefilledif
6.9 Hot Plate.
multiple injections are planned.
6.10 Pipets.
11.9 Inject the samples onto an ion chromatograph operat-
ing as described in the following text.
TOTAL HYDROLYSIS
HIGH-PERFORMANCE ION CHROMATOGRAPHY
7. Reagents and Materials
12. Apparatus
7.1 Sulfuric Acid (72 6 0.1 weight %): To 1 volume of
water, add slowly while stirring vigorously 2 volumes of 12.1 Ion Chromatograph—This equipment can be as-
concentrated sulfuric acid (sp gr 1.84). Standardize against an
sembled from the individual components, or purchased as a
alkaline standard, and adjust to 72 6 0.1 weight %. system.
12.2 Column—The column must be suitable for separating
8. Hazards
monosaccharides and is generally protected by a suitable guard
8.1 Warning—Wear eye protection and chemical resistant
column. A column packing material that works well is com-
gloves while working with strong acid.
posed of 10 µm beads of surface-sulfonated polystyrene/
divinylbenzene (2 % crosslinked), covered with porous latex
9. Summary of Procedure
beads containing alkyl quaternary amine functionality.
9.1 The total hydrolysis of cellulosic material re
...