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1、BRITISH STANDARD BS 3484-1: 1991 Incorporating Amendment No. 1 Record inks Part 1: Specification for blue-black inks Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 This British Standard, having been prepared under the directi
2、on of the Paper and Printing Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 31 January 1992 BSI 08-1999 First published April 1962 Second edition January 1992 The following BSI references relate to the work on this standard: Committee re
3、ference PAM/27 Draft for comment 91/39854 DC ISBN 0 580 20131 7 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Paper and Printing Standards Policy Committee (PAM/-) to Technical Committee PAM/27, upon which the following bodies were rep
4、resented: Association of Metropolitan Authorities British Office Systems and Stationery Federation HMSO Public Record Office Scottish Record Office Society of Archivists Society of Dyers and Colourists Writing Instruments Association Amendments issued since publication Amd. No.DateComments 8071Febru
5、ary 1994Indicated by a sideline in the margin Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 BSI 08-1999i Contents Page Committees responsibleInside front cover Forewordii 1Scope1 2Definitions1 3Ink description1 4Ink requirem
6、ents1 5Packaging1 Appendix A Standard reference ink2 Appendix B Determination of iron content2 Appendix C Determination of sediment3 Appendix D Determination of stability4 Appendix E Determination of ink performance4 Figure 1 Design of suitable holder4 Table 1 Standard solutions for calibration grap
7、h2 Publication(s) referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 ii BSI 08-1999 Foreword This Part of BS 3484 has been prepared under the direction of the Paper and Printing Standards Policy Commi
8、ttee. It supersedes BS 3484:1962 which is withdrawn. This specification calls for the use of substances and/or test procedures that may be injurious to health if adequate precautions are not taken. It refers only to technical suitability and in no way absolves the user of this standard from statutor
9、y obligations relating to health and safety at any stage of manufacture or use. In particular, attention is drawn to the preparation of the standard reference ink in Appendix A and the determination of colour fastness to light in Appendix E. A specification for permanent record inks is given in BS 3
10、484-2. 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 Standard does not of itself confer immunity from legal obligations. Summary of pages This document com
11、prises a front cover, an inside front cover, pages i and ii, pages 1 to 6, 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. Licensed Copy: shef
12、fieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 BSI 08-19991 1 Scope This Part of BS 3484 specifies performance and certain features of the composition of blue-black ink for archival purposes. Appendix A to Appendix E give details of tests for c
13、ompliance of the ink with this Part of BS 3484. NOTE 1The long-term durability of any document will also depend on the composition of the paper, etc. on which it is written. NOTE 2The titles of the publications referred to in this standard are listed on the inside back cover. 2 Definition For the pu
14、rposes of this Part of BS 3484 the following definition applies. 2.1 archival record ink an ink suitable for creating records which are required to remain legible for long periods of time 3 Ink description The ink shall be of the ferrous gallo-tannate type and shall write with an initial blue colour
15、 which develops to an intense black within 14 days. It shall conform in all respects to the standard reference ink described in Appendix A. 4 Ink requirements 4.1 Iron content When tested in accordance with one of the methods described in Appendix B, the ink shall contain not less than 4.5 g/L and n
16、ot more than 5.5 g/L of iron, calculated as metallic iron. 4.2 Freedom from sediment When assessed by the method described in Appendix C, the ink shall show no greater sediment than freshly prepared standard reference ink (see Appendix A). 4.3 Stability When tested in accordance with the method desc
17、ribed in Appendix D, the ink shall be free from deposits, surface growths and scales and shall be at least equal to freshly prepared standard reference ink (see Appendix A) in these respects. 4.4 Performance When tested in accordance with the methods described in Appendix E, the ink shall show: a) c
18、olour depth and intensity by incident and transmitted light at least equal to freshly prepared standard reference ink (see Appendix A) immediately after drying (see Appendix E); b) density of colour at least equal to that shown by freshly prepared standard reference ink after development, when teste
19、d in accordance with item a) of E.4; c) resistance to water at least equal to that of freshly prepared standard reference ink, when tested in accordance with item b) of E.4; d) resistance to fading not less than that of freshly prepared standard reference ink, when tested in accordance with item c)
20、of E.4. 5 Packaging Each bottle or container shall be legibly marked with the following information: a) the name, trademark or other means of identifying the manufacturer; b) the date or date code of manufacture; c) the number and date of this British Standard, i.e. BS 3484-1:19911). NOTE 1It is rec
21、ommended that bottles made from alkali free amber or plain glass should be used. Filled bottles when made from alkali free plain glass should be supplied in cartons or other containers which exclude light. The bottle should be kept in its container and care should be taken that the bottle is not lef
22、t open after use: the container should carry printed instructions to this effect. NOTE 2If stored in accordance with these recommendations the ink will conform with the requirements of this standard for a period of not less than 12 months. 1) Marking BS 3484-1:1991 on or in relation to a product rep
23、resents a manufacturers declaration of conformity, i.e. a claim by or on behalf of the manufacturer that the product meets the requirements of the standard. The accuracy of the claim is therefore solely the responsibility of the person making the claim. Such a declaration is not to be confused with
24、third party certification of conformity, which may also be desirable. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 2 BSI 08-1999 Appendix A Standard reference ink A.1 Reagents and apparatus NOTEAll reagents are general purp
25、ose grades. A.1.1 3,4,5-trihydroxybenzoic acid (gallic acid) (C7H6O5). A.1.2 Tannic acid (C14H10O9). A.1.3 Sulphuric acid c(H2SO4) = 18 mol/L. A.1.4 Iron(II) sulphate (FeSO4.7H2O). A.1.5 Phenol (C6H5OH). A.1.6 Blue dye, essentially free from organic and inorganic diluents or impurities Colour Index2
26、)42755 (acid blue 22) or 42780 (acid blue 93). A.1.7 Distilled water. A.1.8 Ordinary laboratory apparatus A.2 Preparation Dissolve 1 g of phenol and 3 g of the blue dye in about 100 mL of distilled water. Prepare 500 mL of hot distilled water and add, while stirring, 6.4 g of gallic acid and 19.5 g
27、of tannic acid. Dissolve 25 g of iron(II) sulphate in 300 mL of distilled water. Carefully add 3 g of sulphuric acid to the gallic and tannic acid solution and then, while stirring, add the iron(II) sulphate solution. Let the mixture stand for 24 h, filter, add the dye solution followed by sufficien
28、t distilled water to make up to 1 L. Allow to stand for another 24 h and refilter. Appendix B Determination of iron content B.1 Atomic absorption spectrometric method B.1.1 Principle A test solution of ink is prepared and aspirated into an acetylene-air flame. The absorption of the 248.3 nm line emi
29、tted by an iron hollow-cathode lamp is measured. B.1.2 Reagents B.1.2.1 Standard iron solution, corresponding to 0.2 g/L of iron. This solution may be prepared by dissolving 0.200 g of pure iron wire in the smallest possible quantity of hydrochloric acid, with a density of 1.19 g/mL, in a 1 000 mL o
30、ne-mark volumetric flask, making up to the mark with distilled water, followed by thorough mixing. 1 mL of this solution contains 0.2 mg of iron. B.1.2.2 Hydrochloric acid solution, approximately c(HCl) = 6 mol/L. B.1.2.3 Distilled water B.1.3 Apparatus B.1.3.1 Atomic absorption spectrometer, fitted
31、 with an acetylene and air burner. B.1.3.2 Iron hollow-cathode lamp B.1.3.3 Ordinary laboratory apparatus B.1.4 Preparation of the calibration graph B.1.4.1 Preparation of the standard matching solutions In each of a series of six 50 mL one-mark volumetric flasks, place 10 mL of the hydrochloric aci
32、d solution and then, respectively, the volumes of the standard iron solution given in Table 1. Dilute to the mark with distilled water and mix. Table 1 Standard solutions for calibration graph B.1.4.2 Adjustment of the apparatus Fit the iron hollow-cathode lamp in the apparatus, switch on the curren
33、t and allow to stabilize. Adjust the current, sensitivity and the aperture of the slit according to the characteristics of the apparatus. Adjust the waveband in the region of 248.3 nm to maximum absorbance. Adjust the pressure of the acetylene and of the air according to the characteristics of the b
34、urner. Adjust the aspiration rate to between 2 mL/min and 4 mL/min. B.1.4.3 Spectrometric measurement Aspirate the series of standard matching solutions (see Table 1) in succession into the flame and measure the absorbance for each. Take care to keep the aspiration rate constant. Spray water through
35、 the burner after each measurement. 2) Colour Index, Vol. 4, 3rd edition 1971, published by the Society of Dyers and Colourists, P.O. Box 244, Perkin House, 82 Grattan Road, Bradford BD1 2JB, West Yorks., United Kingdom, and by the American Association of Textile Chemists and Colorists, P.O. Box 122
36、15, Research Triangle Park, North Carolina 27709, USA. Volume of standard iron solution Corresponding mass of iron mL 0a 15 20 25 30 35 mg 0 3.0 4.0 5.0 6.0 7.0 a Blank test on reagents for calibration graph. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolle
37、d Copy, (c) BSI BS 3484-1:1991 BSI 08-19993 B.1.4.4 Plotting the graph Plot a graph, having the masses of iron in milligrams, see Table 1, (contained in 50 mL portions of the standard matching solutions) as abscissae and the corresponding values for the measured absorbance, reduced by the value of t
38、he absorbance measured in the blank test, as ordinates. B.1.5 Blank test Carry out a blank test at the same time as the determination following the same procedure and using the same amount of all reagents, but omitting the ink portion. B.1.6 Determination To each of two 50 mL one-mark volumetric fla
39、sks add 1 mL of the ink, 10 mL of the hydrochloric acid solution and make up to the mark with distilled water. Mix thoroughly and if the solution contains any suspended matter allow this to settle. Carry out the spectrometric measurements in accordance with B.1.4.3, after having adjusted the instrum
40、ent to zero absorbance against the blank test solution. B.1.7 Expression of results From the calibration graph, read the iron content equivalent to the mean absorbance determined in B.1.6, multiply by 1 000 and report the result in grams per litre to one decimal place. B.2 Titrimetric method B.2.1 P
41、rinciple An accurately known quantity of ink is decolourized, titrated with disodium EDTA and the iron content calculated from the titre. B.2.2 Apparatus B.2.2.1 pH meter B.2.2.2 Ordinary laboratory apparatus B.2.3 Reagents B.2.3.1 Concentrated sulphuric acid, c(H2SO4) = 18 mol/L. B.2.3.2 Sodium hyd
42、roxide solution, c(NaOH) = 4 mol/L. B.2.3.3 Sodium acetate solution, (NaC2H3O2.3H2O) 10 % m/m. B.2.3.4 Potassium permanganate solution (KMnO4) 2 % m/m. B.2.3.5 5-sulphosalicylic acid solution, 2 % m/m. B.2.3.6 Disodium EDTA solution, c(Na2C10H14N2O8) = 0.05 mol/L. B.2.3.7 Distilled water B.2.4 Proce
43、dure Weigh accurately to three decimal places about 5 g of ink into a tared 250 mL conical flask. Add 50 mL of distilled water and 2 mL of concentrated sulphuric acid. Add the potassium permanganate solution drop by drop until the flask contents turn a pale yellow colour, i.e. the ink has been decol
44、ourized. If the mixture is not clear, heat until any solid dissolves. Add the sodium hydroxide solution until the pH is approximately 1.8 then add the sodium acetate solution until the pH is in the range 2 to 3. Add 10 mL of the 5-sulphosalicylic acid solution (the mixture should turn purple) and he
45、at to 40 C to ensure the complex formation is complete. Allow to cool then titrate with the disodium EDTA solution to a yellow end-point. Repeat the procedure for another portion of ink. B.2.5 Calculation and expression of results Calculate the iron content of the ink, I, in grams per litre from the
46、 equation Express the result to one decimal place. Appendix C Determination of sediment C.1 Apparatus and reagent C.1.1 Test paper holder of acid resistant material, fitted with stainless steel clips, such that the chromatographic paper is held firmly but not in contact with the surface of the holde
47、r and of a size suitable for mounting a test paper 200 mm long and 20 mm wide. Figure 1 illustrates a suitable design of holder. C.1.2 Chromatographic paper3) C.1.3 pH meter C.1.4 Coverable, acid resistant container, of sufficient size to contain the test paper holder. C.1.5 Ordinary laboratory appa
48、ratus C.1.6 Sulphuric acid solution, adjusted to the pH of the ink. where Tis the mean titre of the two results, (in mL); mis the mean mass of the two ink samples (in g); is the density of the ink (in g/mL). 3) Whatman 3MM has been found to be suitable. I T m - - 2.7925= Licensed Copy: sheffieldun s
49、heffieldun, na, Wed Nov 29 08:44:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3484-1:1991 4 BSI 08-1999 C.2 Preparation of chromatograms C.2.1 Cut a strip of chromatographic paper about 200 mm long and about 20 mm wide. About 30 mm from one end lightly mark a cross in the centre with a blunt, soft leaded pencil, so as not to damage the surface of the paper. Make a mark 70 mm from the cross by lightly drawing a line across the paper. Mount the paper in the holder with the cross towards the lower clip. C.2.2 Shake the ink under test thoroughly and by means of