1、BRITISH STANDARD BS7463-1: 1991 ISO9184-1: 1990 Fibre furnish analysis of paper, board and pulps Part 1: General methodBS7463-1:1991 This British Standard, having been prepared under the directionof the Paper and PrintingStandards Policy Committee, was published underthe authority of the Standards B
2、oard and comes into effect on 28 June1991 BSI07-1999 The following BSI references relate to the work on this standard: Committee referencePAM/11 Draft for comment88/45954 DC ISBN 0 580 19825 1 Committees responsible for this British Standard The preparation of this British Standard was entrusted by
3、the Paper and Printing Standards Policy Committee (PAM/-) to Technical Committee PAM/11, upon which the following bodies were represented: British Fibreboard Packaging Association British Paper and Board Industry Federation (PIF) British Printing Industries Federation British Telecommunications plc
4、Envelope Makers and Manufacturing Stationers Association Her Majestys Stationery Office Man-made Fibres Producers Committee Ministry of Defence Pira (the Research Association for the Paper and Board, Printing and Packaging Industries) Post Office Society of British Printing Ink Manufacturers Univers
5、ity of Manchester Institute of Science and Technology Amendments issued since publication Amd. No. Date CommentsBS7463-1:1991 BSI 07-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope 1 2 Normative reference 1 3 Definitions 1 4 Principle 1 5 Reagents 1 6 Appa
6、ratus 2 7 Preparation of the test piece 2 8 Staining and preparation of fibre slides 3 9 Procedure 3 10 Expression of results 4 11 Test report 5 Annex A (informative) Weight factors 6 Annex B (informative) Bibliography for species identification of papermaking fibres 7 Table 1 Confidence limits 4 Ta
7、ble A.1 Weight factors 6 Publication(s) referred to Inside back coverBS7463-1:1991 ii BSI 07-1999 National foreword This Part of BS7463 has been prepared under the direction of the Paper and Printing Standards Policy Committee. It is identical with ISO9184-1:1990 “Paper, board and pulps Fibre furnis
8、h analysis Part 1: General method”, published by the International Organization for Standardization (ISO). A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British St
9、andard does not of itself confer immunity from legal obligations. Cross-reference International standard Corresponding British Standard ISO9184-2:1990 BS7463 Fibre furnish analysis of paper, board and pulps Part2:1991 Guide to staining (Identical) Summary of pages This document comprises a front cov
10、er, an inside front cover, pagesi andii, pages1 to8, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS7463-1:1991 BSI 07-1999 1 1 Scope This p
11、art of ISO9184 specifies the general performance of the test for fibre furnish analysis (see3.1) of paper, board and pulps. It is applicable to all kinds of pulps and to most papers and boards, including those containing more than one kind of fibre, taking into account different pulping processes. T
12、his method is less suitable to heavily impregnated or highly coloured papers and boards, which cannot be dispersed or decoloured without affecting the structure or the staining reactions of the fibres. 2 Normative reference The following standard contains provisions which, through reference in this
13、text, constitute provisions of this part of ISO9184. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this part of ISO9184 are encouraged to investigate the possibility of applying the most recent edition of the st
14、andard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO9184-2:1990, Paper, board and pulps Fibre furnish analysis Part2: Staining guide. 3 Definitions For the purposes of this part of ISO9184, the following definitions apply. 3.1 fibre furnis
15、h analysis determination of the fibre components of paper, board and pulp samples as regards the species of fibres and the method of processing the fibre furnish analysis may be carried out qualitatively or quantitatively 3.2 fibre coarseness, c means mass (oven dry) per unit length for a particular
16、 type of fibre, generally expressed in milligrams per metre 3.3 weight factor, f the ratio of the fibre coarseness of a particular type of fibre to that of a reference fibre NOTE 1Traditionally, cotton staple (rag) fibre was selected as the reference fibre to which all other fibres were compared. Th
17、e weight factor of cotton fibre was taken as1,00, and the fibre coarseness of that fibre was determined to be0,180mg/m. The weight factor of a particular type of fibre can be derived from its fibre coarseness by the expression 4 Principle The fibre furnish analysis is carried out under the microscop
18、e on a small quantity of stained fibres representative of the sample being tested: qualitatively, on the basis of the stain reactions and the morphological characteristics of the fibres; quantitatively, by counting the number of crossings of various kinds of fibres with the counting line and by tran
19、sforming the number of counts into the percentages by weight by the application of weight factors. 5 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 5.1 Sodium hydroxide, solution, about1% (m/m) containing10g sodi
20、um hydroxide (NaOH) per litre. 5.2 Hydrochloric acid, solution, about0,2% (m/m), containing5ml of concentrated hydrochloric acid(HCl) per litre. 5.3 Phosphoric acid, solution, about5% (m/m), containing35ml of85% (m/m) phosphoric acid(H 3 PO 4 ) per litre. 5.4 Aluminium sulfate, solution, about5% (m/
21、m), containing50g of aluminium sulfate Al 2 (SO 4 ) 3 per litre. 5.5 Potassium permanganate, solution, about6,5% (m/m) containing65g of potassium permanganate (KMnO 4 ) per litre. 5.6 Oxalic acid, solution, about5% (m/m), containing50g of oxalic acid (C 2 H 2 O 4 .2H 2 O) per litre. 5.7 Organic solv
22、ents, ethanol (C 2 H 5 OH), diethyl ether (C 2 H 5 OC 2 H 5 ), ethyl acetate (CH 3 COOC 2 H 5 ), acetone (CH 3 COCH 3 ), xylene C 6 H 4 (CH 3 ) 2 , toluene(C 7 H 8 ), chloroform (CHCl 3 ), tetrachloroethene (C 2 Cl 4 ) and trichloroethane (C 2 H 3 Cl 3 ). where f is the weight factor; c is the fibre
23、 coarseness, in milligrams per metre. f c 0,180 - =BS7463-1:1991 2 BSI 07-1999 6 Apparatus Ordinary laboratory equipment and 6.1 Microscope, equipped with a mechanical stage and cross-hair, central dot or horizontal line eye-pieces. Illumination: daylight lamp or normal vacuum lamp with daylight fil
24、ter. For the identification and counting of fibres a magnification of 40 to 120, and for the study of structural details 200 to 500 is recommended. 6.2 Dispersers, one for easily dispersible samples (low-speed agitator, etc.) and the other for more resistant samples (ultra-sonic disperser, high-spee
25、d macerator, etc.). 6.3 Infra-red lamp, or hot-plate, capable of being maintained at50 C to60 C. 6.4 Filtering devices 6.4.1 Round sieve, diameter50mm to70mm, with metal or plastic edge, height5mm to10mm. The sieve bottom shall be made of woven wire cloth, aperture size604m to804m. 6.4.2 Glass filte
26、r,200ml, with sintered disc, pore size154m to404m. 6.5 Dropper, a glass tube about100mm in length and internal diameter5mm to8mm, with one end carefully smoothed but not constricted, and the other end fitted with a rubber bulb. The dropper shall be designed to discharge approximately0,5ml. 6.6 Micro
27、scope slides, recommended size25mm 75mm. 6.7 Rectangular microscope cover glasses, recommended size22mm 32mm. 6.8 Dissecting needles 6.9 Petri dishes, or suitable shallow, covered dishes, approximatelly100mm to120mm in diameter. 6.10 Multiple counter, for recording counted fibres. 6.11 Dropper bottl
28、es,30ml or50ml. 7 Preparation of the test piece Take a test piece by tearing small pieces from different parts of the sample, about0,25g in total. For multilayered samples, take a test piece in accordance with7.3. 7.1 Ordinary samples 7.1.1 Boiling in water Place the test piece in a test tube or a s
29、mall beaker. Boil torn pieces in water for a few minutes, stirring occasionally, and disperse in a disperser(6.2). 7.1.2 Boiling in sodium hydroxide solution If the pieces cannot be completely dispersed in accordance with7.1.1, replace the pieces after filtering (see6.4) in the test tube or beaker.
30、Boil the pieces in sodium hydroxide solution(5.1) for a few minutes, with occasional stirring. NOTE 2Samples containing wool fibres or natural silk, should not be treated with sodium hydroxide, because wool and silk are soluble in alkali. Boiling in a sodium hydroxide solution can also affect the de
31、velopment of certain stains. Filter on a glass filter(6.4.2), wash twice with water and neutralize with hydrochloric acid(5.2) for several minutes. Wash several times with water and disperse in a disperser(6.2). 7.2 Specially treated samples If these treatments do not disperse the pieces, choose one
32、 of the treatments described in7.2.1 to7.2.4. 7.2.1 Wet-strength papers Place torn pieces of the sample in a beaker, add aluminium sulfate solution(5.4) or phosphoric acid solution(5.3) and boil for5min to30min, depending on the dispersing velocity. Decant the solution, wash with water and disperse.
33、 If the pieces are not dispersible, proceed to7.2.3. NOTE 3Hypochlorite bleach has also been found effective for dispersing these products. 7.2.2 Vegetable parchment and papers of highly beaten pulp Place torn pieces of the sample in potassium permanganate solution(5.5) in a beaker and allow to stan
34、d for1h. Decant the solution, wash the pieces, treat with oxalic acid solution(5.6), wash again and disperse. 7.2.3 Impregnated or specially bonded samples having chemically or physically durable inter-fibre bonds No general rule can be given. Extraction, cold or hot, with organic solvents(5.7) may
35、often facilitate the disintegration. Choose the solvent so that is does not affect the fibres. 7.2.4 Coloured samples In the unlikely event that after disintegration the fibres are still coloured to such an extent as to render their identification difficult, methods depending on the characteristics
36、of the dyestuff may be used to remove the colour. These methods include the extraction, oxidation and reduction treatments with the requisite reagents in normal laboratory use.BS7463-1:1991 BSI 07-1999 3 7.3 Multilayered samples When the paper or board sample is expected to be multilayered and two o
37、r more layers are to be analysed separately, proceed as follows. From the sample, cut five pieces, about5cm 5cm in size, and immerse in hot water (about70 C) until the pieces can be separated into the component layers. If separation is difficult, use sodium hydroxide solution(5.1) instead of water.
38、If the separated layers seem to contain fibres from the neighbouring layers, try to remove them by rubbing them gently while wet. Treat the layers as separate test pieces and proceed in accordance with7.1. 8 Staining and preparation of fibre slides The method of staining and preparation of slides de
39、pends on the stain used. Choose the appropriate stain from the staining guide (see ISO9184-2) and perform the staining of the fibres on the slide or in the test tube. NOTE 4While the stains recommended in ISO9184-2 have proven effective for differentiating various fibre types, there are a number of
40、other stains which can be usefully employed in certain cases. These stains are described in a number of published references, many of which are given inAnnex B. 8.1 Staining on a slide The fibre slide for staining can be prepared either from a dilute fibre suspension or from a filtered fibre pad. 8.
41、1.1 Preparation from the fibre suspension Dilute about one-half of the dispersed fibre suspension (see clause7) in a beaker to a concentration of about0,05% (m/m). By means of a dropper(6.5), transfer about0,5ml of the suspension on to a clean, grease-free microscope slide(6.6), and disperse the fib
42、res evenly with a dissecting needle(6.8) or by tapping the slide gently. Dry the fibre slide on the hot-plate or under the infra-red lamp(6.3) and allow to cool. Apply the stain according to the relevant method and put on a cover glass(6.7) avoiding air bubbles. Allow to stand for1min to2min and dra
43、in off the surplus stain preferably by tilting the long edge of the slide into contact with a blotter. 8.1.2 Preparation from the fibre pad Filter one-half of the dispersed fibre suspension (see clause7) on a sieve(6.4.1) or on a glass filter(6.4.2). Place the filtered fibre pad in a small covered d
44、ish(6.9) and keep it from drying during the analysis. Transfer a small amount of the fibre pad to the slide and remove excess water with blotting paper. Apply the stain according to the prescribed method, and distribute the fibres evenly with dissecting needles(6.8). Apply a cover glass(6.7) and rem
45、ove excess solution with blotting paper, taking care to avoid flocculation of the fibres. The best result is obtained if the fibre slide is tilted and blotted edgewise. 8.2 Staining in a test tube Take a specimen from the filtered fibre pad (see8.1.2) and perform the staining in a test tube accordin
46、g to the relevant method. After staining prepare the fibre slide according to8.1.1 or8.1.2 using water instead of stain. More detailed instructions for staining and preparation are given in the relevant staining methods. 9 Procedure Because the colours developed by certain stains are unstable, the a
47、nalysis should be carried out after the slide has been prepared. 9.1 Qualitative analysis Place the stained fibre slide on the mechanical stage of the microscope(6.1). Slowly and systematically, traverse the slide, either horizontally or vertically, line by line, so that the entire fibre field is ex
48、amined. Identify the species of fibres and the methods of processing on the basis of the morphological characteristics (seeAnnex B) and the colours obtained by staining (see the staining tests). Examine at least two slides. In cases where there are fibres that are difficult to identify, examine one
49、or more additional slides. Previous experience and knowledge of the stain reactions and of the structural details of the most common papermaking fibres are essential for the identification 1) . 1) A catalogue listing the reference pulps available can be obtained from the TAPPI Library, Institute of Paper Science and Technology,5754th Street, N.W., Atlanta, GA,30318, USA.BS7463-1:1991 4 BSI 07-1999 9.2 Quantitative analysis With the mechanical stage move the fibre slide so that the centre marking of the eyepiece is3mm to5mm from t
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