DIN EN ISO 14453-2014 Pulps - Determination of acetone-soluble matter (ISO 14453 2014) German version EN ISO 14453 2014《纸浆 丙酮可溶物的测定》.pdf

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1、September 2014 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).I

2、CS 85.040!%:Iw“2233884www.din.deDDIN EN ISO 14453Pulps Determination of acetone-soluble matter (ISO 14453:2014);English version EN ISO 14453:2014,English translation of DIN EN ISO 14453:2014-09Faserstoffe Bestimmung acetonlslicher Bestandteile (ISO 14453:2014);Englische Fassung EN ISO 14453:2014,Eng

3、lische bersetzung von DIN EN ISO 14453:2014-09Ptes Dtermination des matires solubles dans lactone (ISO 14453:2014);Version anglaise EN ISO 14453:2014,Traduction anglaise de DIN EN ISO 14453:2014-09SupersedesDIN EN ISO 14453:1998-12www.beuth.deDocument comprises pagesIn case of doubt, the German-lang

4、uage original shall be considered authoritative.1408.14 DIN EN ISO 14453:2014-09 2 A comma is used as the decimal marker. National foreword This document (EN ISO 14453:2014) has been prepared by Technical Committee ISO/TC 6 “Paper, board and pulps”, Working Committee WG 4 “Chemical Analysis” (Secret

5、ariat: SCC, Canada) in collaboration with Technical Committee CEN/TC 172 “Pulp, paper and board” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Papier, Pappe und Faserstoff (DIN Standards Committee Paper, Board and Pulps), Working Committ

6、ee NA 074-02-01 AA Chemisch-technische Prfverfahren fr Papier, Pappe, Faserstoff und Chemiezellstoff. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 638 DIN EN ISO 638 ISO 7213 DIN EN 27213 Amendments This standard differs from DIN EN

7、ISO 14453:1998-12 as follows: a) the use of automated extraction has been included; b) a new precision statement has been added that complies with the requirements of ISO/TR 24498; c) the standard has been editorially revised. Previous editions DIN 54354: 1968-07, 1977-11 DIN EN ISO 14453: 1998-12 N

8、ational Annex NA (informative) Bibliography DIN EN ISO 638, Paper, board and pulps Determination of dry matter content Oven-drying method DIN EN 27213, Pulps Sampling for testing EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14453 April 2014 ICS 85.040 Supersedes EN ISO 14453:1998English

9、Version Pulps - Determination of acetone-soluble matter Ptes - Dtermination des matires solubles dans lactone (ISO 14453:2014) Faserstoffe - Bestimmung acetonlslicher Bestandteile This European Standard was approved by CEN on 15 February 2014. CEN members are bound to comply with the CEN/CENELEC Int

10、ernal Regulations which stipulate the conditions for giving 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 an

11、y CEN member. This European Standard exists in three official 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 v

12、ersions. CEN members are the national standards bodies of 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, Norwa

13、y, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, 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 exploi

14、tation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14453:2014 E(ISO 14453:2014) (ISO 14453:2014) Contents DIN EN ISO 14453:2014-09 EN ISO 14453:2014 (E) 2 Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Pri

15、nciple 5 5 Reagent .5 6 Apparatus .6 6.1 Option A 6 6.2 Option B 6 6.3 Options A and B .6 7 Sampling and preparation of the sample 6 8 Procedure .7 8.1 Extraction with acetone 7 8.2 Blanks .8 8.3 Evaporation of the solvent and drying of the extraction residue .8 9 Expression of results 8 10 Test rep

16、ort 9 Annex A (informative) Precision 10 Bibliography 12 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 secretariat of which is held by DIN. This Eu

17、ropean 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 drawn to the possibility that some of the e

18、lements 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 national standards organizations of the fol

19、lowing 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, Lithuania, Luxembourg, Malta, Netherlands,

20、 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. DIN EN ISO 14453:2014-09 EN ISO 14453:2014 (E) 3 IntroductionThe am

21、ount 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, acetone extracts of mechanical

22、 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 extracted under the conditions

23、 specified in this International Standard.DIN EN ISO 14453:2014-09 EN ISO 14453:2014 (E) 4 1 ScopeThis International Standard describes the determination of acetone-soluble matter in pulp.It is applicable to all types of pulp. The lower limit of the determination is about 0,05 %. This limit can be l

24、owered 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. For dated references, only the edition cited applies. For undated references, the latest editi

25、on 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 definitionsFor the purposes of this document, the following terms and definitions apply.3.1acetone-so

26、luble 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 apparatus (Option A) or in a Soxtec1)apparatus or similar extraction equipment (Option B).NOTE

27、 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 extraction times and recovery of the main portion of the solvent12. Other extraction methods, such

28、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, including that reported in Annex A, no statistically significant differences were found betwe

29、en 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 Reagent5.1 Acetone (CH3COCH3), analytical reagent grade.WARNING Acetone is a highly flammable m

30、aterial; 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 commercially. This information is given for the convenience of users of this document and does not

31、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.DIN EN ISO 14453:2014-09 EN ISO 14453:2014 (E) 5 extraction should not be left unattended for any length of time. Caution should be taken to avoid open flame. Care

32、should be taken to avoid inhalation, ingestion, or body contact.6 ApparatusOrdinary laboratory equipment and the following.6.1 Option A6.1.1 Soxhlet extraction apparatus, with ground-glass joints, consisting of a Soxhlet extraction flask of 250 ml capacity, Soxhlet extraction tube, and a Graham or A

33、llihn-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 Electric 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 Extra

34、ction 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 (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

35、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 Weighing 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

36、 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 Sampling and preparation of the sampleObtain a representative sample of air-dry pulp sufficient to provide two 10 g test specimens and two specimens for determi

37、nation 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 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 an

38、other 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 representative of the sample received.Use protective gloves whenever handling the sample. Keep the sample in a refrigerator in polyethylene bags or in p

39、ackages 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 sample 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 dr

40、ying is recommended if the extracts are to be analysed for their chemical composition, in order to avoid possible oxidation of fatty and resin acids.DIN EN ISO 14453:2014-09 EN ISO 14453:2014 (E) 6 Cut or tear the test portions into small pieces, 1 cm by 1 cm. Tear flash-dried pulp into suitable pie

41、ces no more than 15 mm wide.8 Procedure8.1 Extraction with acetone8.1.1 Option ACarry out the extraction procedure in duplicate.Allow 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 tw

42、o separate specimens for the determination of the dry matter content as described in ISO 638. The mass of the test portion should 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

43、possible to increase the amount of sample extracted. It is also possible to extract two or more sample portions and combine the solvent 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

44、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 draining 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

45、 (5.1) corresponding to 1,5 times the volume of the extractor. Connect the condenser and start the extraction.Bring the solvent to 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 automate

46、d 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

47、on the extractives level and on the capacity of the extractor. The mass of the test portion should be adjusted so that the extract mass will exceed 5 mg. If the mass of extract is less than 5 mg, two or more sample portions can be extracted and the solvent portions can be combined before evaporation

48、. At the same time weigh two separate specimens for the determination of the dry matter content as described in ISO 638. Transfer the specimen to an extraction thimble (6.3.1).Add between 50 ml and 100 ml of acetone (5.1) to the extraction cup (6.2.2) and start the boiling. The test portion shall be covered with acetone. Select the temperature for extraction as recommended by the equipment manufacturer.Allow the test portion to boil for at least 15 min (see Note), and then move the extraction thimble to the r