ASTM D5896-96(2007)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5896 − 96 (Reapproved 2007)
StandardTest 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.
1. Scope 3.2.5 mM—millimolar.
1.1 This test method covers the determination of the carbo-
4. Summary of Test Method
hydrate composition of cellulosic materials such as ground
4.1 IC analysis of cellulosics requires the following opera-
wood meal, chemically refined pulp, mechanical pulps, brown-
tions:
stocks, and plant exudates (gums) by ion chromatography.This
(1) sample preparation,
test method is suitable for rapid, routine testing of large
(2) total hydrolysis,
numbers of samples with high accuracy and precision. For a
(3) dilution,
review of this technique, see Lee (1) .
(4) SPE,
1.2 The values stated in SI units are to be regarded as
(5) ion chromatographic analysis, and
standard. No other units of measurement are included in this
(6) calibration/calculation.
standard.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 This test method requires total hydrolysis of carbohy-
responsibility of the user of this standard to establish appro-
drate material to monosaccharides, and is thus applicable to
priate safety and health practices and determine the applica-
any cellulosic or related material that undergoes substantial
bility of regulatory limitations prior to use. For hazard state-
hydrolysis, including cellulose derivatives such as cellulose
ment, see Section 8.
acetate.
5.2 The carbohydrate composition of a cellulosic material
2. Referenced Documents
can be expressed on the basis of the total initial sample, or on
2.1 ASTM Standards:
the basis of the carbohydrate portion of the sample.The former
D1193 Specification for Reagent Water
requires quantitative handling and may require special knowl-
D1695 Terminology of Cellulose and Cellulose Derivatives
edge of the other components present in order to establish the
absolute carbohydrate level or determine individual wood
3. Terminology
hemicelluloses such as galactoglucomannan, etc. Since the
3.1 For standard terminology of cellulose and cellulose
solid portion of purified pulps is almost all carbohydrate
derivatives, see Terminology D1695.
(98 + %), the latter basis is often used to express the carbo-
hydrate distribution as a percent.
3.2 Abbreviations:
3.2.1 IC—ion chromatography,
5.3 Ifheatedunderalkalineconditions,isomericsugarsmay
3.2.2 SPE—solid phase extraction,
begin to appear in the chromatogram. The major impurity
3.2.3 PAD—pulsed amperometric detector,
present in purified pulps is saccharinic acids. These acidic
3.2.4 PED—pulsed electrochemical detector,
components, and other anions such as sulfate, carbonate, and
acetate are removed by a strong base anion exchange SPE, and
would need to be determined separately to get a more exact
This test method is under the jurisdiction of ASTM Committee D01 on Paint
carbohydrate distribution.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
6. Apparatus
Current edition approved June 1, 2007. Published June 2007. Originally
approved in 1996. Last previous edition approved in 2001 as D5896 - 96 (2001).
6.1 Blender.
DOI: 10.1520/D5896-96R07.
The boldface numbers in parentheses refer to the list of references at the end of
6.2 Screw Cap Culture Tubes, 25 by 150 mm, outside
this test method.
diameter.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.3 Refrigerator.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.4 Pressure Cooker.
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D5896 − 96 (Reapproved 2007)
6.5 SPE Cartridges. 6–6.5 during the dilution step. Neutralization is recommended
if the sample is to be stored before analysis.
6.6 Water Bath.
11.8 Prepare an anion exchange SPE cartridge with 5 mLof
6.7 Ion Chromatograph.
water, pass 5 mL of sample through the cartridge, discarding
6.8 Moisture Balance.
the first 3 mL, and use the remaining 2 mL to fill a 0.5-mL
6.9 Hot Plate. injectionvial.Additional0.5-mLinjectionvialsmaybefilledif
multiple injections are planned.
6.10 Pipets.
11.9 Inject the samples onto an ion chromatograph operat-
TOTAL HYDROLYSIS
ing as described in the following text.
7. Reagents and Materials
HIGH-PERFORMANCE ION CHROMATOGRAPHY
7.1 Sulfuric Acid (72 6 0.1 weight %): To 1 volume of
12. Apparatus
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.
8. Hazards
12.2 Column—The column must be suitable for separating
8.1 Precaution: Wear eye protection and chemical resistant monosaccharides and is generally protected by a suitable guard
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/
9. Summary of Procedure divinylbenzene (2 % crosslinked), covered with porous latex
beads containing alkyl quaternary amine functionality.
9.1 The total hydrolysis of cellulosic material requires a
primary hydrolysis with strong mineral acid followed by a
13. Procedure
secondary hydrolysis in dilute acid. The primary hydrolysis
13.1 Perform the analysis using an ion chromatograph.
results in the formation of a mixture of oligosaccharides; the
secondary hydrolysis completes the conversion to monomeric
13.2 Inject 100 µL of sample onto the analytical column.
sugars.
13.3 Detection is by PAD or PED in a pulsed amperometric
mode using a gold working electrode.
10. Sampling, Test Specimens, and Test Units
13.4 Standardpulpsamplesaregenerallyrunisocraticallyat
10.1 Extract wood samples with ethanol to remove extrac-
1 mL/min using an eluant of 2.5 mM sodium hydroxide to
tives, then grind in a Wiley mill to pass a 40-mesh screen.
...