ASTM D5896-96(2001)

Standard Test Method for Carbohydrate Distribution of Cellulosic Materials

SCOPE
1.1 This test method covers the determination of the carbohydrate composition of cellulosic materials such as ground wood meal, chemically refined pulp, mechanical pulps, brownstocks, and plant exudates (gums) by ion chromatography. This test method is suitable for rapid, routine testing of large numbers of samples with high accuracy and precision. For a review of this technique, see Lee (1).
1.2 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 hazard statement, see Section 8.

General Information

• Status: Historical
• Publication Date: 31-Dec-2000
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 85.040 - Pulps
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaces: ASTM D5896-96 - Standard Test Method for Carbohydrate Distribution of Cellulosic Materials
• Effective Date: 01-Jan-2001
• Replaced By: ASTM D5896-96(2007) - Standard Test Method for Carbohydrate Distribution of Cellulosic Materials
• Effective Date: 01-Jun-2007

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5896–96(Reapproved2001)
Standard Test Method for
Carbohydrate Distribution of Cellulosic Materials
This standard is issued under the fixed designation D 5896; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope (1) sample preparation,
(2) total hydrolysis,
1.1 This test method covers the determination of the carbo-
(3) dilution,
hydrate composition of cellulosic materials such as ground
(4) SPE,
wood meal, chemically refined pulp, mechanical pulps, brown-
(5) ion chromatographic analysis, and
stocks, and plant exudates (gums) by ion chromatography.This
(6) calibration/calculation.
test method is suitable for rapid, routine testing of large
numbers of samples with high accuracy and precision. For a
5. Significance and Use
review of this technique, see Lee (1).
5.1 This test method requires total hydrolysis of carbohy-
1.2 This standard does not purport to address all of the
drate material to monosaccharides, and is thus applicable to
safety concerns, if any, associated with its use. It is the
any cellulosic or related material that undergoes substantial
responsibility of the user of this standard to establish appro-
hydrolysis, including cellulose derivatives such as cellulose
priate safety and health practices and determine the applica-
acetate.
bility of regulatory limitations prior to use. For hazard state-
5.2 The carbohydrate composition of a cellulosic material
ment, see Section 8.
can be expressed on the basis of the total initial sample, or on
2. Referenced Documents the basis of the carbohydrate portion of the sample.The former
requires quantitative handling and may require special knowl-
2.1 ASTM Standards:
edge of the other components present in order to establish the
D 1193 Specification for Reagent Water
absolute carbohydrate level or determine individual wood
D 1695 Terminology of Cellulose and Cellulose Deriva-
hemicelluloses such as galactoglucomannan, etc. Since the
tives
solid portion of purified pulps is almost all carbohydrate
3. Terminology (98 + %), the latter basis is often used to express the carbo-
hydrate distribution as a percent.
3.1 For standard terminology of cellulose and cellulose
5.3 If heated under alkaline conditions, isomeric sugars may
derivatives, see Terminology D 1695.
begin to appear in the chromatogram. The major impurity
3.2 Abbreviations:
present in purified pulps is saccharinic acids. These acidic
3.2.1 IC—ion chromatography,
components, and other anions such as sulfate, carbonate, and
3.2.2 SPE—solid phase extraction,
acetate are removed by a strong base anion exchange SPE, and
3.2.3 PAD—pulsed amperometric detector,
would need to be determined separately to get a more exact
3.2.4 PED—pulsed electrochemical detector,
carbohydrate distribution.
3.2.5 mM—millimolar.
6. Apparatus
4. Summary of Test Method
6.1 Blender.
4.1 IC analysis of cellulosics requires the following opera-
6.2 Screw Cap Culture Tubes, 25 by 150 mm, outside
tions:
diameter.
6.3 Refrigerator.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
6.4 Pressure Cooker.
and Related Coatings, Materials, andApplications and is the direct responsibility of
6.5 SPE Cartridges.
Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
6.6 Water Bath.
Current edition approved Jan. 10, 1996. Published March 1996.
The boldface numbers in parentheses refer to the list of references at the end of
6.7 Ion Chromatograph.
this test method.
6.8 Moisture Balance.
Annual Book of ASTM Standards, Vol 11.01.
4 6.9 Hot Plate.
Annual Book of ASTM Standards, Vol 06.03.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5896–96 (2001)
6.10 Pipets. HIGH-PERFORMANCE ION CHROMATOGRAPHY
12. Apparatus
TOTAL HYDROLYSIS
12.1 Ion Chromatograph—This equipment can be as-
7. Reagents and Materials
sembled from the individual components, or purchased as a
system.
7.1 Sulfuric Acid (72 6 0.1 weight %): To 1 volume of
12.2 Column—The column must be suitable for separating
water, add slowly while stirring vigorously 2 volumes of
monosaccharides and is generally protected by a suitable guard
concentrated sulfuric acid (sp gr 1.84). Standardize against an
column. A column packing material that works well is com-
alkaline standard, and adjust to 72 6 0.1 weight %.
posed of 10 µm beads of surface-sulfonated polystyrene/
8. Hazards divinylbenzene (2 % crosslinked), covered with porous latex
beads containing alkyl quaternary amine functionality.
8.1 Precaution: Wear eye protection and chemical resistant
gloves while working with strong acid.
13. Procedure
13.1 Perform the analysis using an ion chromatograph.
9. Summary of Procedure
13.2 Inject 100 µL of sample onto the analytical column.
9.1 The total hydrolysis of cellulosic material requires a
13.3 Detection is by PAD or PED in a pulsed amperometric
primary hydrolysis with strong mineral acid followed by a
mode using a gold working electrode.
secondary hydrolysis in dilute acid. The primary hydrolysis
13.4 Standardpulpsamplesaregenerallyrunisocraticallyat
results in the formation of a mixture of oligosaccharides; the
1 mL/min using an eluant of 2.5 mM sodium hydroxide to
secondary hydrolysis completes the conversion to monomeric
obtain baseline resolution of fucose (internal standard), arabi-
sugars.
nose, galactose, glucose, xylose, and mannose in less than 30
min. If other sugars are present, it may be necessary to alter the
10. Sampling, Test Specimens, and Test Units
eluant strength, or try a gradient approach.
10.1 Extract wood samples with ethanol to remove extrac-
13.5 Eluant is degassed and kept under helium (nitrogen
tives, then grind in a Wiley mill to pass a 40-mesh screen.
may be substituted for helium).
Disintegrate (fluff) dry pulp or paper samples in a blender.
13.6 A 0.5-mL/min flow of 0.3-M NaOH is added after the
Determine the moisture content using a moisture balance or
column, but prior to the detector to improve response.
similar device.
14. Calibration and Standardization
11. Pr
...