TAPPI T 408 cm-07

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史蒂文 2024-12-18 8 58.5KB 7 页 12星币
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T 408 cm-07
OFFICIAL STANDARD − 1926
FOURTH REVISION − 1974
OFFICIAL TEST METHOD − 1982
REVISED − 1988
CLASSICAL METHOD − 1997
REVISED − 2007
©2007 TAPPI
The information and data contained in this document were prepared
by a technical committee of the Association. The committee and the
Association assume no liability or responsibility in connection with
the use of such information or data, including but not limited to any
liability or responsibility under patent, copyright, or trade secret laws.
The user is responsible for determining that this document is the
most recent edition published.
Approved by the Standard Specific Interest Group for this Test Method
TAPPI
CAUTION:
This Test Method may include safety precautions which are believed to be appropriate at the time of publication of the method. The intent of these
is to alert the user of the method to safety issues related to such use. The user is responsible for determining that the safety precautions are complete
and are appropriate to their use of the method, and for ensuring that suitable safety practices have not changed since publication of the method. This
method may require the use, disposal, or both, of chemicals which may present serious health hazards to humans. Procedures for the handling of
such substances are set forth on Material Safety Data Sheets which must be developed by all manufacturers and importers of potentially hazardous
chemicals and maintained by all distributors of potentially hazardous chemicals. Prior to the use of this method, the user must determine whether
any of the chemicals to be used or disposed of are potentially hazardous and, if so, must follow strictly the procedures specified by both the
manufacturer, as well as local, state, and federal authorities for safe use and disposal of these chemicals.
Rosin in paper and paperboard
1. Scope
1.1 This method describes empirical procedures for the quantitative determination of rosin in paper and
paperboard.
1.1.1 Total extractable resin includes rosin added as a sizing agent, natural resins from the pulp, fatty acids and
esters added as sizing and defoaming agents, and other natural and synthetic resins.
1.1.2 The quantitative procedures aimed at determining rosin in the presence of volatile or non-volatile neutral
extractives will include as rosin any fatty acid present in the alcohol extract.
1.2 Qualitative tests, indicating the presence or absence of rosin added as a sizing agent, will be found in
Section 12; Qualitative tests.
1.3 This method is not suitable for the quantitative determination of fatty acids and fatty salts in paper due to
partial esterification during extraction.
1.4 This method is not applicable to the determination of wet strength resins.
1.5 It has been found that melamine formaldehyde resin does not interfere with the rosin determination (1).
2. Significance
2.1 The reaction products of rosin size and aluminum salts are most commonly used internally to control
permeability of paper to aqueous liquids (sizing). Rosin content may be expected to bear some relationship to sizing
effectiveness; however, chemical and physical conditions during papermaking can have an overriding effect on the
relationship.
2.2 Rosin content of paper is generally conceded to affect permanence and physical properties of paper.
3. Definitions
3.1 Rosin (colophony) is a natural resin derived from pine gum, tall oil, and the solvent extract of pine
stumps, knots, and top wood. It is largely a mixture of resin acids combined with a small amount of neutral materials.
T 408 cm-07 Rosin in paper and paperboard / 2
3.2 Rosin, as used in this method, also refers to various chemically modified (fortified) rosins used in making
sizing agents.
4. Summary
4.1 The insoluble resinates present in the paper are hydrolyzed and dissolved by extraction with an acidulated
alcohol extraction solvent. The alcohol extract is then extracted with ether, in which nonresinous materials such as
inorganics, starch, and glue are insoluble, yielding a total extractable “resin.” Neutral materials (hydrocarbon waxes and
oils, esters, etc.) are separated from the total extract by saponification and extraction. Further details are given by Launer
(2). 4.2 If mineral matter is present which reacts with HC1 or is dissolved by it [see TAPPI T 421 “Qualitative
(Including Microscopic) Analysis of Mineral Filler and Mineral Coating of Paper”], the sample is pretreated with
aqueous HCl.
5. Apparatus
5.1 Extraction apparatus, Soxhlet, medium, 40 mm i.d. body, or equivalent.
5.2 Gooch crucible, 40-mL.
5.3 Glass fiber filter papers, 24-mm diameter.
5.4 Crucible holder, for 40-mL Gooch crucible.
5.5 Filtering flask with side tube, 250-mL.
5.6 Beakers, 250-mL.
5.7 Separatory funnels, two 250-mL or larger.
5.8 Reflux condenser and flask, 250-mL flask or larger.
5.9 Steam bath, for reflux condenser.
5.10 Glass wool or fritted glass filter
5.11 Drying oven, capable of maintaining an internal temperature of 105 ± 3°C.
5.12 Balance, having a capacity of at least 125 g and readable to ± 0.0001 g.
5.13 Chemical fume hood, having a face velocity of at least 24.4 m/min (80 ft/min) or as required by local
safety regulations.
6. Reagents and materials
6.1 Hydrochloric acid, concentrated HCl; also approximately 1M.
NOTE 1: CAUTION: handle with adequate ventilation, in a hood. Material is very corrosive and the breathing of fumes and contact with
the skin should be avoided.
6.2 Extraction solvent, mixture of 4 mL of concentrated HCL in 1000 mL of 95% ethanol.
6.3 Ether, diethyl, anhydrous, peroxide-free.
NOTE 2: Material is highly flammable and must be handled with adequate ventilation, in a hood equipped with a down-draft exhaust system.
Avoid all potential ignition sources. Test the ether for the presence of peroxides by the following: To a 25-mL glass-stoppered
cylinder of colorless glass, add 10 mL of the ether to be tested and 1 mL of a freshly prepared 10% aqueous solution of potassium
iodide (1 g KI in 10 mL distilled water). Shake the cylinder and contents occasionally over a 1-h period. Protect the cylinder and
contents from light. At the end of the hour, view the contents of the cylinder transversely against a white background; no color
should be seen in either liquid. If color is seen, the ether contains peroxides and must not be used.
NOTE 3: To eliminate the explosion and fire hazards associated with anhydrous ether, dichloromethane may be used as a substitute. If this
is done, however, it must be so stated in the report, the values given in Section 11. Precision may not apply, and results may be
slightly different.
If neutral materials are to be separated:
3 / Rosin in paper and paperboard T 408 cm-07
6.4 Potassium hydroxide, approximately 0.5M alcoholic solution KOH: add 34 g reagent KOH pellets to
1000 mL of 95% ethanol, 90% methanol, or 99% 2-propanol, and dissolve by shaking. Let stand 24 h and decant clear
solution.
NOTE 4: Handle with care, avoiding contact with the skin and the breathing of mists during preparation.
6.5 Sodium chloride, NaCl crystals.
6.6 Sulfuric acid, approximately 2.5M H2SO4.
6.7 Methyl orange indicator.
7. Sampling and test specimens
Prepare from each test unit obtained in accordance with TAPPI T 400 “Sampling and Accepting a Single Lot of
Paper, Paperboard, Containerboard, or Related Product” two or more test specimens of at least 10 g each, cut into strips
about 6 x 40 mm (about 0.25 by 1.5 in.). Do not grind the paper, because additional nonresinous materials may then be
extracted.
NOTE 5: For paperboard, such as containerboard, pressboard, binder board, and pasted board, it is advisable to split material into thinner
portions to facilitate extraction of the resin whenever possible, prior to weighing.
8. Procedures
8.1 Procedure A to determine (total extractable resin).
8.1.1 Allow the specimen strips to reach moisture equilibrium with the atmosphere surrounding the balance and
weigh 5 to 7 g of strips to the nearest 0.01 g. Unless known to within 1%, determine the moisture content of a separate
specimen similarly conditioned, in accordance with TAPPI T 412 “Moisture in Paper and Paperboard.”
8.1.2 If the paper contains mineral matter which reacts with or is dissolved by HCl (see TAPPI T 421),
immerse the test specimen to be extracted in 1M HCl for 5 min, drain, wash free from acid, and dry at room temperature.
8.1.3 Place a thin layer of glass wool over the siphon tube entrance of the Soxhlet apparatus to prevent the
paper from blocking the tube. Crease the strips to be extracted with small zigzag folds and place them lengthwise in the
siphon cup of the extractor, taking care to avoid packing them tightly together.
NOTE 6: When using a Soxhlet extractor, it is permissible to weigh the paper in a coarse fritted glass thimble and place the thimble in the
extractor cup.
8.1.4 Add sufficient extraction solvent to the siphon cup to completely cover the specimen and allow to stand
for 5-10 min without draining. In addition, add to the extractor flask 1.5 times the volume required to fill the cup.
Extract at such a reflux rate that about 250-350 mL of solvent is distilled per hour. Extract for a period of 2 h for
uncoated or nonsurface-sized papers and 2.5 h for coated or surface-sized papers or for paperboards. Do not continue the
extraction much longer than specified, since additional high molecular weight materials other than rosin might be
extracted and reported as rosin.
8.1.5 When the extraction period is completed, transfer the solvent from the flask to a suitable beaker. Rinse
the flask several times with alcohol into the beaker and evaporate on the steam bath until the odors of alcohol and HCl
are no longer noticeable. Place the beaker in an oven at 105 ± 3°C for 15 min, cool to room temperature, and add 20 mL
of anhydrous ether. The rosin should dissolve in from 5 to 30 s unless covered by foreign materials, in which case it
should be scraped with a stirring rod.
8.1.6 Allow to stand 15 to 20 min to further the coagulation and settling of insoluble matter. Filter the solution
and about 20 mL of ether rinsings of the beaker through the Gooch crucible fitted with the glass fiber filter paper into the
filtering flask. Refilter the solution through the same paper if necessary to remove cloudiness. After filtering, rinse the
filter 3 times with less than 20 mL of ether and quantitatively transfer the ether solution from the flask to a carefully dried
and tared beaker.
8.1.7 Evaporate the ether to apparent dryness on the steambath, then dry in an oven at 105 ± 3°C for 15 min,
cool, and weigh to the nearest 0.001 g. Repeat the drying and weighing until the weight is constant to ± 0.001 g. If
weight loss is obtained on the third weighing, use Procedure C under 8.3 below.
CAUTION: Do not place ether-wet material in an oven with exposed electrical contact. Explosion and/or fire may result.
摘要:

TAPPI T 408 cm-07 是国际公认的纸浆、纸张及纸板行业标准测试方法,主要规定了通过硝酸-乙醇法测定纤维素材料中α-纤维素含量的详细操作流程与精度要求。该标准适用于评估纸浆的纯度、纤维结晶度及化学加工适应性,是造纸、纺织及纤维素衍生物生产领域质量控制与研发验证的关键依据。文档内容涵盖试剂制备、样品处理、过滤、称重及结果计算全步骤,强调实验条件对重复性的影响;其最新修订版本(cm-07)更新了安全注意事项与偏差控制条款,确保检测结果符合现代工业及国际贸易合规需求。对于从事纸浆分析、纤维

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作者:史蒂文 分类:国际标准 价格:12星币 属性:7 页 大小:58.5KB 格式:PDF 时间:2024-12-18

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