1、BSI Standards PublicationBS EN ISO 14453:2014Pulps Determination ofacetone-soluble matterBS EN ISO 14453:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO14453:2014. It supersedes BS EN ISO 14453:2000 which is withdrawn.The UK participation in its prepara
2、tion was entrusted to TechnicalCommittee PAI/11, Methods of test for paper, board and pulps.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible f
3、or its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 78108 7ICS 85.040Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and
4、Strategy Committee on 30 April 2014.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14453 April 2014 ICS 85.040 Supersedes EN ISO 14453:1998English Version Pulps - Determination of acetone-soluble matter (ISO 14453:2014) Ptes - Dterminati
5、on des matires solubles dans lactone (ISO 14453:2014) Faserstoff - Bestimmung acetonlslicher Bestandteile (ISO 14453:2014) This European Standard was approved by CEN on 15 February 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givi
6、ng this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three offi
7、cial versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of
8、 Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
9、Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide fo
10、r CEN national Members. Ref. No. EN ISO 14453:2014 EBS EN ISO 14453:2014EN ISO 14453:2014 (E) 3 Foreword This document (EN ISO 14453:2014) has been prepared by Technical Committee ISO/TC 6 “Paper, board and pulps” in collaboration with Technical Committee CEN/TC 172 “Pulp, paper and board” the secre
11、tariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2014, and conflicting national standards shall be withdrawn at the latest by October 2014. Attention is draw
12、n to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 14453:1998. According to the CEN-CENELEC Internal Regulations, the nati
13、onal standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lit
14、huania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14453:2014 has been approved by CEN as EN ISO 14453:2014 without any modification. BS EN ISO 14453:2014ISO 1445
15、3:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagent . 16 Apparatus . 26.1 Option A 26.2 Option B 26.3 Options A and B 27 Sampling and preparation of the sample 28 Procedure. 38.1 Extracti
16、on with acetone 38.2 Blanks 48.3 Evaporation of the solvent and drying of the extraction residue 49 Expression of results 410 Test report . 5Annex A (informative) Precision . 6Bibliography 8BS EN ISO 14453:2014ISO 14453:2014(E)ForewordISO (the International Organization for Standardization) is a wor
17、ldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on
18、 that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this d
19、ocument and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Direc
20、tives, Part 2. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development o
21、f the document will be in the Introduction and/or on the ISO list of patent declarations received. www.iso.org/patentsAny trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms
22、and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 6, Paper, board and pulps.This
23、 second edition cancels and replaces the first edition (ISO 14453:1997), which has been technically revised to include the use of automated extraction, and to add a new precision statement that complies with the requirements of ISO/TR 24498.iv ISO 2014 All rights reservedBS EN ISO 14453:2014ISO 1445
24、3:2014(E)IntroductionThe amount of acetone-soluble matter in pulp provides a measure of the content of wood extractives, often called resin. The acetone-soluble matter includes fatty acids, resin acids, fatty alcohols, sterols, diglycerides and triglycerides, steryl esters and waxes.In addition, ace
25、tone extracts of mechanical pulps may also contain phenolic compounds such as lignans. In the case of incompletely washed chemical pulps, the acetone extracts will also include dissolved kraft lignin.Metal soaps of fatty and resin acids, such as those present in unwashed or deinked pulp, are not ext
26、racted under the conditions specified in this International Standard. ISO 2014 All rights reserved vBS EN ISO 14453:2014BS EN ISO 14453:2014Pulps Determination of acetone-soluble matter1 ScopeThis International Standard describes the determination of acetone-soluble matter in pulp.It is applicable t
27、o all types of pulp. The lower limit of the determination is about 0,05 %. This limit can be lowered by increasing the amount of sample analysed.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application.
28、For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 7213, Pulps Sampling for testingISO 638, Paper, board and pulps Determination of dry matter content Oven-drying method3 Terms and definit
29、ionsFor the purposes of this document, the following terms and definitions apply.3.1acetone-soluble matteramount of material that can be extracted with acetone from a sample of pulp by the method specified in this International Standard4 PrincipleA pulp sample is extracted with acetone in a Soxhlet
30、apparatus (Option A) or in a Soxtec1)apparatus or similar extraction equipment (Option B).NOTE Extraction with a Soxtecapparatus is carried out with boiling solvent instead of condensed solvent as is the case with the Soxhlet extraction. The main advantages of the Soxtecsystem are much shorter extra
31、ction times and recovery of the main portion of the solvent12. Other extraction methods, such as Accelerated Solvent Extraction (ASE), can produce different results and are not within the scope of this International Standard2. As reported in Reference 2 and based on several interlaboratory studies3,
32、 including that reported in Annex A, no statistically significant differences were found between the two extraction methods.After extraction, the solvent is evaporated and the residue is dried at a temperature of 105 C.The content of acetone-soluble matter is reported as a percentage of dry pulp.5 R
33、eagent5.1 Acetone (CH3COCH3), analytical reagent grade.WARNING Acetone is a highly flammable material; therefore only approved electric or steam heating shall be used. The entire procedure must be performed in a chemical fume hood and the 1) Soxtec is an example of a suitable product available comme
34、rcially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products may be used if they can be shown to lead to the same results.INTERNATIONAL STANDARD ISO 14453:2014(E) ISO 2014 All rights reserved
35、1BS EN ISO 14453:2014ISO 14453:2014(E)extraction should not be left unattended for any length of time. Caution should be taken to avoid open flame. Care should be taken to avoid inhalation, ingestion, or body contact.6 ApparatusOrdinary laboratory equipment and the following.6.1 Option A6.1.1 Soxhle
36、t extraction apparatus, with ground-glass joints, consisting of a Soxhlet extraction flask of 250 ml capacity, Soxhlet extraction tube, and a Graham or Allihn-type condenser.NOTE For pulp samples with a low content of acetone-soluble matter, an extractor with a larger volume may be needed.6.1.2 Elec
37、tric heater, with a suitable capacity, giving an extraction rate of at least 4 cycles per hour. A hot water bath can also be used.6.2 Option B6.2.1 Extraction apparatus of the Soxtectype, or equivalent.6.2.2 Aluminium or glass cups for extraction.6.3 Options A and B6.3.1 Extraction thimbles, alundum
38、 (aluminium oxide), porosity RA 98; fritted glass, coarse porosity; or cellulose pre-extracted with acetone (5.1).6.3.2 Boiling beads, made of porcelain or similar material, pre-extracted with acetone (5.1).6.3.3 Glass fibre wool, pre-extracted with acetone.6.3.4 Glass filter, of porosity 3.6.3.5 We
39、ighing dishes, of aluminium or other lightweight material. Check that the dishes do not lose or gain mass when subjected to the drying cycle described in Clause 7.6.3.6 Drying oven, ventilated, capable of maintaining an air temperature of (105 2) C.6.3.7 Balance, with a precision of 0,1 mg.7 Samplin
40、g and preparation of the sampleObtain a representative sample of air-dry pulp sufficient to provide two 10 g test specimens and two specimens for determination of dry matter content. If it is found (or known) that the mass of the extract from 10 g does not exceed 5 mg, a greater mass of sample will
41、be required. For sampling from lots and consignments of market pulp, the sample shall be taken in accordance with ISO 7213. If the analysis is made on another type of sample, report the origin of the sample and, if possible, the sampling procedure, and ensure that the specimens taken in Clause 8 are
42、 representative of the sample received.Use protective gloves whenever handling the sample. Keep the sample in a refrigerator in polyethylene bags or in packages of aluminium foil. For long-term storage, samples should be placed in a freezer.If the dry matter content is below 90 %, allow the whole sa
43、mple to air-dry overnight at room temperature or in a drying oven at a temperature not exceeding 40 C.NOTE Freeze-drying instead of air-drying or oven drying is recommended if the extracts are to be analysed for their chemical composition, in order to avoid possible oxidation of fatty and resin acid
44、s.2 ISO 2014 All rights reservedBS EN ISO 14453:2014ISO 14453:2014(E)Cut or tear the test portions into small pieces, 1 cm by 1 cm. Tear flash-dried pulp into suitable pieces no more than 15 mm wide.8 Procedure8.1 Extraction with acetone8.1.1 Option ACarry out the extraction procedure in duplicate.A
45、llow the sample to attain moisture equilibrium with the atmosphere near the balance. Weigh two specimens of about 10 g each to the nearest 1 mg. At the same time, weigh two separate specimens for the determination of the dry matter content as described in ISO 638. The mass of the test portion should
46、 be adjusted so that the extract mass will exceed 5 mg. For samples with a low content of acetone-soluble matter, an extractor with a larger volume can be used to make it possible to increase the amount of sample extracted. It is also possible to extract two or more sample portions and combine the s
47、olvent portions before evaporation.Transfer one specimen to the extractor (6.1.1). Use a cellulose extraction thimble (6.3.1) or place a porous porcelain disc or a wad of glass fibre wool (6.3.3) over the specimen to prevent any loss. Check that no part of the specimen extends above the top of the d
48、raining tube. Always use an extraction thimble if the pulp is shredded or flash dried.To the extraction flask (6.1.1) add the boiling beads (6.3.2) and a volume of acetone (5.1) corresponding to 1,5 times the volume of the extractor. Connect the condenser and start the extraction.Bring the solvent t
49、o a boil and adjust the rate of emptying the extractor to at least 4 times per hour. The total extraction time shall be no less than 4 h.8.1.2 Option BOperate the automated extraction apparatus according to the manufacturers instructionsCarry out the extraction procedure in duplicate.Allow the sample to attain moisture equilibrium with the atmosphere near the balance.Weigh two specimens of about 5 g to 10 g each to the nearest 1 mg. The mass of the specimens depends on the extractives level and on the capacity of the extractor
