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1、INTERNATIONAL STANDARD IS0 14453 First edition 1997-08-I 5 Pulps - Determination of acetone-soluble matter Pites - Dktermina Con des ma C a=400net; p=iso; o=isocs; s=central Printed in Switzerland II Copyright International Organization for Standardization Provided by IHS under license with ISO Lice
2、nsee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 IS0 14453: 1997(E) Introduction This International Standard has been developed as a replacement for IS0 624:1974, Pulps - Determination of dich
3、loromethane soluble matter, the previous solvent extraction method for pulps. The reason for the replacement is the potential health hazard using dichloromethane, the use of which is restricted by law in some countries. For some pulps the results obtained according to this International Standard are
4、 on a higher level than those obtained with IS0 624. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS
5、-,-,- This page intentionally left blank Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERN
6、ATIONAL STANDARD o IS0 IS0 14453: 1997(E) Pulps - Determination of acetone-soluble matter 1 Scope This International Standard describes the determination of acetone-soluble matter in pulp. It is applicable to all types of pulp, except pulps made entirely or partly from waste paper. The lower limit o
7、f the determination is about 0,05 %. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, an
8、d parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 72 13: 1981, Pulps - Sampling fo
9、r testing. IS0 638:1978, Pulps - Determination of dry matter content. 3 Definition For the purposes of this International Standard, the following definition applies. 3.1 acetone-soluble matter: The amount of material that can be extracted with acetone from a sample of pulp by the method specified in
10、 this International Standard. 4 Principle The sample is extracted with acetone in a Soxhlet apparatus After at least 16 extraction cycles the solvent is evaporated and the residue is dried at 105 “C for 2 h and weighed. 5 Reagent 5.1 Acetone (CH3COCH3), analytical reagent grade. WARNING - Acetone is
11、 inflammable. Keep away from open fire. Do not use gas heaters. Follow pertinent safety regulations. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction o
12、r networking permitted without license from IHS -,-,- IS0 14453:1997(E) 6 Apparatus Ordinary laboratory equipment and 6.1 Soxhlet extraction apparatus, with ground-glass joints, having a 300 ml to 500 ml flask, a Soxhlet extractor and a water-cooled condenser. 6.2 Cellulose extraction thimbles, clea
13、ned by pre-extraction with acetone. 6.3 Glass fibre, cleaned by extraction with acetone. 6.4 Heater, for the extraction apparatus (hot-water bath or equivalent). 65 w hen Weighing subjected dishes, of aluminium or other lightweight to the dtyin g cycle described in clause 7. mate rial. Check that th
14、e dishes do not lose or gain mass 7 Sampling and preparation of the sample The procedure to be followed when sampling depends on the particular circumstances in each case. For sampling from lots and consignments of market pulp, the instructions in IS0 7213 are recommended. Use protective gloves when
15、ever handling the sample. Keep samples protected from ambient air in polyethylene bags or in packages of aluminium foil. Dry wet pulp at a temperature not exceeding 40 “C. Cut samples of pulp in sheet form into narrow strips to fit the extractor. Tear flash-dried pulp into suitable pieces no more th
16、an 15 mm wide. 8 Procedure Allow the sample to attain moisture equilibrium with the atmosphere near the balance. Weigh two samples of about IO g to the nearest 1 mg and a separate sample for determination of the dry matter content as described in IS0 638. Carry out the following extraction procedure
17、 in duplicate. Introduce into the draining tube of the extractor (6.1) a small wad of glass fibre (6.3). Place the pulp in the extractor (6.1). Use a cellulose extraction thimble (6.2) or place a porous porcelain disc or a wad of glass fibre (6.3) over the sample to prevent any loss. Check that no p
18、art of the sample extends above the top of the draining tube. Always use an extraction thimble (6.2) if the pulp is shredded or flash dried. Add a sufficient volume of acetone (5.1) to ensure that there are at least 50 ml of solvent remaining in the flask when the extractor is ready for siphoning. A
19、ssemble the extractor. Bring the solvent to boiling and continue the extraction until the extractor has emptied at least 16 times. The extraction time shall not be less than 3 h and preferably not more than 4 h. NOTE - If the re is a te ndency for the solvent beads or boiling chips in the extraction
20、 flasks. to become super-heated, resulting in uneven boiling, it is advisable to use glass 2 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networ
21、king permitted without license from IHS -,-,- IS0 IS0 14453: 1997(E) To facilitate the recovery of the acetone, stop the extraction just before the extractor is ready to empty. Check the extract for the presence of fibres and other visible solids. If necessary, filter the extract through a fritted g
22、lass filter of medium pore width. With the aid of small portions of acetone (5.1) transfer the extract quantitatively to a tared weighing dish (6.5). WARNING - In order to eliminate potential explosion hazards in the drying oven (next step), allow the remaining acetone to evaporate completely at a t
23、emperature not exceeding 40 OC. Finally dry the extraction residue in a drying oven at (105 + 2) “C for 2 h. Allow the dish to cool to room temperature in a desiccator. Weigh it to the nearest 0,l mg and calculate the mass of the residue. 9 Blanks Check at regular intervals that the blank value is n
24、egligible in comparison with the test result. Run the entire procedure exactly as usual, but without any sample. If P roperly done, this test should result i ,n no significant blank. If a significant blank value is obtained, try to eliminate the source , which, fo r example, may be impurities in the
25、 acetone used. 10 Expression of results For each single extraction, calculate the acetone-soluble matter content, expressed as a percentage of the oven-dry mass of the pulp sample, using the expression x =xlOO “1 where x ml is the acetone-soluble matter content, expressed as a percentage by mass; is
26、 the mass of the test portion, calculated on an oven-dry basis; m2 is the mass of the residue obtained after extraction by acetone and drying in the oven. Then calculate the mean result of parallel determinations and report it with two decimals. If the mean falls below 0,05 %, report the result as “
27、less than 0,05 %“, 11 Precision Four samples were analysed by 17 different laboratories distributed worldwide. Each laboratory was asked to follow the procedure in this International Standard exactly and, for each pulp, to report both values obtained. The results have been summarized as follows: 11
28、.l Repeatability The average deviation between dupiicates was between 3 % and 5 % of the average result for each particular pulp sample. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/2
29、3/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 14453: 1997(E) 0 IS0 11.2 Reproducibility The mean and the coefficient of variation of the reported results (each time the mean of duplicates) were as shown in table 1. Table 1 Pulp Bleached mechanical Birc
30、h sulfate, TCF Pine sulfate, ECF Hardwood sulfite TCF, totally chlorine free. ECF, elemental chlorine free. Mean value Coeff. of variation % % 0,68 999 0,18 8s 0,15 939 0,24 997 12 Test report The test report shall include the following particulars: a reference to this International Standard; b) dat
31、e and place of testing; c) complete identification of the samples tested; d) the results, expressed as a percentage of the oven-dry mass of the pulp sample; e) any departure from the standard procedure that may have affected the result. 4 Copyright International Organization for Standardization Prov
32、ided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- This page intentionally left blank Copyright International Organization for Standardization Provided by IHS
33、under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- This page intentionally left blank Copyright International Organization for Standardization Provided by IHS under licens
34、e with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- This page intentionally left blank Copyright International Organization for Standardization Provided by IHS under license with ISO L
35、icensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 14453: 1997(E) ICS 85.040 Descriptors: paper pulps, tests, chemical tests, determination of content, soluble matter, extraction methods. Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 19:50:26 MDTNo reproduction or networking permitted without license from IHS -,-,-