1、BRITISH STANDARD BS 3900-B8: 1986 ISO 3856-3: 1984 Methods of test for paints Part B8: Determination of “soluble” barium content ISO title: Paints and varnishes Determination of “soluble” metal content Part 3: Determination of barium content Flame atomic emission spectrometric method It is recommend
2、ed that this Part be read in conjunction with the general information in the introduction to BS3900, issued separately. UDC 667.61:620.1BS3900-B8:1986 This British Standard, having been prepared under the directionof the Pigments, Paintsand Varnishes StandardsCommittee, was published under the autho
3、rity ofthe Board of BSI and comes intoeffect on 31January1986 BSI 11-1999 The Committees responsible for this British Standard are shown inBS3900: Introduction. The following BSI references relate to the work on this standard: Committee referencePVC/10 Draft for comment78/51514 DC ISBN 0 580 14947 1
4、 Amendments issued since publication Amd. No. Date of issue CommentsBS3900-B8:1986 BSI 11-1999 i Contents Page National foreword ii 0 Introduction 1 1 Scope and field of application 1 2 References 1 3 Principle 1 4 Reagents and materials 1 5 Apparatus 1 6 Procedure 2 7 Expression of results 2 8 Test
5、 report 3 Publications referred to Inside back coverBS3900-B8:1986 ii BSI 11-1999 National foreword This Part of BS3900 has been prepared under the direction of the Pigments, Paints and Varnishes Standards Committee. It is identical with ISO3856-3:1984 “Paints and varnishes Determination of “soluble
6、” metal content” Part3“Determination of barium content Flame atomic emission spectrometric method” published by the International Organization for Standardization (ISO). It is assumed in the drafting of this standard that it will be used and applied by those who are appropriately qualified and exper
7、ienced. The procedures described in this standard are intended to be carried out by suitably trained and/or supervised personnel. The substances and procedures described may be injurious to health if inadequate precautions are taken. This standard refers only to its technical suitability and does no
8、t absolve the user from statutory obligations relating to health and safety. Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with thos
9、e used in British Standards; attention is drawn especially to the following. The comma has been used as a decimal marker. In British Standards, it is current practice to use a full point on the baseline as the decimal marker. In British Standards it is current practice to use the symbol “L” for litr
10、e rather than “l”. Wherever the words “International Standard” and “part of ISO3856” appear, referring to this standard, they should be read as “British Standard” and “Part of BS3900” respectively, and wherever the identification “ISO 3856-3” appears, it should be read as “BS3900:B8”. The Technical
11、Committee has reviewed the provisions of ISO385-1:1984, and ISO648:1977 to which reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. ISO385-1 is related to BS846 “Specification for burettes” and ISO648 is related to BS1583 “One-mark pipe
12、ttes”. The Technical Committee has reviewed the proposed provisions of ISO3696 to which reference is made in clause4 and has decided that they are acceptable for use in conjunction with this standard. ISO3696 is related to BS3978 “Water for laboratory use”. ISO3856, to which reference is made in cla
13、use0, is published in a number of Parts of BS3900. At the time of publication of this standard, the relationship between other Parts of BS3900 and Parts of ISO3856 was as follows: Cross-references International Standards Corresponding British Standards ISO 1042:1983 BS1792:1982 Specification for one
14、-mark volumetric flasks (Identical) ISO 6713:1984 BS 3900 Methods of test for paints Part B5:1986 Preparation of acid extracts from liquid paints or coating powders (Identical) Part of ISO 3856 Corresponding Part of BS 3900 BS 3900 Methods of test for paints ISO 3856-1:1984 a Part B6:1986 Determinat
15、ion of “soluble” lead content (Identical) ISO 3856-2:1984 Part B7:1986 Determination of “soluble” antimony content (Identical)BS3900-B8:1986 BSI 11-1999 iii Textual error. When adopting the text of the International Standard, the textual error given below was discovered. It has been marked in the te
16、xt and has been reported to ISO in a proposal to amend the text of the International Standard. In6.3, line 3, “absorbance” should be read as “emission”. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their cor
17、rect application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Part of ISO 3856 Corresponding Part of BS 3900 ISO 3856-4:1984 Part B9:1986 Determination of “soluble” cadmium content (Identical) ISO 3856-5:1984 Part B10:1986 Determination of hexavalent
18、 chromium content of solid matter (Identical) ISO 3856-6:1984 Part B11:1986 Determination of total chromium content of liquid matter (Identical) ISO 3856-7:1984 Part B12:1986 Determination of “soluble” mercury content (Identical) a Attention is drawn to a similar standard, BS3900-B3 “Determination o
19、f “soluble” lead in the solid matter in liquid paints: method for use in conjunction with The Control of Lead at Work Regulations,1980 (S.I. 1980 No. 1248)”. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages1to 4, an inside back cover and a back cove
20、r. 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.iv blankBS3900-B8:1986 BSI 11-1999 1 0 Introduction This International Standard is a part of ISO3856, Paints and varnishes Determin
21、ation of “soluble” metal content. 1 Scope and field of application This part of ISO3856 describes a flame atomic emission spectrometric (AES) method for the determination of the barium content of the test solutions prepared according to ISO6713 or other suitable International Standards. The method i
22、s applicable to paints having “soluble” barium contents in the range of about0,05 to5%(m/m). Other methods can be used by agreement between the interested parties but this method is the referee method in cases of dispute. 2 References ISO 385-1, Laboratory glassware Burettes Part1: General requireme
23、nts 1) . ISO 648, Laboratory glassware One-mark pipettes. ISO 1042, Laboratory glassware One-mark volumetric flasks. ISO 3696, Water for laboratory use Specifications 2) . ISO 6713, Paints and varnishes Preparation of acid extracts from paints in liquid or powder form. 3 Principle Aspiration of the
24、test solution into a dinitrogen monoxide/acetylene flame. Measurement of the radiation emitted by barium at a wavelength of553,5nm. The ionization of barium atoms in the flame is suppressed by addition of potassium chloride. 4 Reagents and materials During the analysis, use only reagents of recogniz
25、ed analytical grade and only water of at least grade3purity according to ISO3696. 4.1 Potassium chloride, 50g/l solution. 4.2 Hydrochloric acid, c(HCl) = 0,07 mol/l. Use the hydrochloric acid, identical to that used for the preparation of the test solutions in accordance with ISO6713. (See6.2.) 4.3
26、Dinitrogen monoxide, commercial grade, in a steel cylinder. 4.4 Acetylene, commercial grade, in a steel cylinder. 4.5 Barium, standard stock solution containing1g of Ba per litre. Either a) transfer the contents of an ampoule of standard barium solution containing exactly1g of Ba into a1000ml one-ma
27、rk volumetric flask, dilute to the mark with the hydrochloric acid (4.2) and mix well; or b) weigh, to the nearest1mg, 1,779g of barium chloride dihydrate (BaCl 2 .2H 2 O), dissolve in the hydrochloric acid (4.2) in a1000 ml one-mark volumetric flask, dilute to the mark with the same hydrochloric ac
28、id and mix well. 1 ml of this standard stock solution contains1mg ofBa. 4.6 Barium, standard solution containing20mg of Ba per litre. Prepare this solution on the day of use. Pipette 20ml of the standard stock solution (4.5) into a1000ml one-mark volumetric flask, dilute to the mark with the hydroch
29、loric acid (4.2) and mix well. 1 ml of this standard solution contains204g of Ba. 5 Apparatus For this test, the laboratory glassware shall be barium-free. Ordinary laboratory apparatus and 5.1 Flame atomic emission spectrometer, suitable for measurements at a wavelength of553,5nm and fitted with a
30、burner fed with dinitrogen monoxide and acetylene. 5.2 Pipettes, of a suitable volume (see6.2), complying with the requirements of ISO648. 5.3 Burettes, of capacity10 and50ml, complying with the requirements of ISO385-1. 5.4 One-mark volumetric flasks, of capacity50ml, complying with the requirement
31、s of ISO1042. If available: 5.5 Recording apparatus A compensating recorder is recommended. 1) At present at the stage of draft. (Partial revision of ISO/R385:1964.) 2) At present at the stage of draft.BS3900-B8:1986 2 BSI 11-1999 6 Procedure 6.1 Preparation of the calibration graph 6.1.1 Preparatio
32、n of the standard matching solutions Prepare these solutions on the day of use. Into a series of six50ml one-mark volumetric flasks(5.4), introduce from the burette (5.3), respectively, the volumes of the standard barium solution (4.6) shown in the following table, add5ml of the potassium chloride s
33、olution (4.1), dilute each to the mark with the hydrochloric acid (4.2) and mix well. 6.1.2 Spectrometric measurements Measure the emission of the standard matching solutions in the spectrometer (5.1), using the operating conditions specified by the manufacturer of the instrument. In order to determ
34、ine and correct for the constant background emission due to the presence of calcium, carry out a measurement at a suitable point close to the barium line or record the emission over a wavelength range from553,0 to554,0 nm. 6.1.3 Calibration graph Plot a graph having the masses, in micrograms, of Ba
35、contained in1ml of the standard matching solutions as abscissae and the corresponding values of the emission, corrected for background emission, as ordinates. 6.2 Test solutions 6.2.1 Pigment portion of the liquid paint and paint in powder form Pipette a suitable volume (volume V 3 ) of each of the
36、solutions obtained by the procedure described in sub-clause8.2.3 of ISO6713 into50ml one-mark volumetric flasks (5.4) so that the barium concentration of each test solution will be within the calibration range. Add5ml of the potassium chloride solution (4.1), dilute to the mark with the hydrochloric
37、 acid (4.2) and mix well. 6.2.2 Liquid portion of the paint Pipette a suitable volume (volume V 4 ) of each of the solutions obtained by the procedure described in sub-clause9.3 of ISO6713 into50ml one-mark volumetric flasks (5.4) so that the barium concentration of each test solution will be within
38、 the calibration range. Add5ml of the potassium chloride solution (4.1), dilute to the mark with the hydrochloric acid (4.2) and mix well. 6.2.3 Other test solutions Pipette a suitable volume of each of the solutions obtained by the specified or agreed procedure into50ml one-mark volumetric flasks (
39、5.4) so that the barium concentration of each test solution will be within the calibration range. Add5ml of the potassium chloride solution (4.1), dilute to the mark with the hydrochloric acid (4.2) and mix well. 6.3 Determination Measure first the emission of the hydrochloric acid(4.2) in the spect
40、rometer (5.1) after having adjusted it as described in6.1.2. Then measure the absorbance of each test solution (6.2) three times and, afterwards, that of the hydrochloric acid again. Finally, re-determine the emission of the standard matching solution No. 4 (6.1.1) in order to verify that the respon
41、se of the apparatus has not changed. If the emission of a test solution is higher than that of the standard matching solution with the highest barium concentration, dilute the test solution appropriately (dilution factor F) with a known volume of the hydrochloric acid (4.2). 7 Expression of results
42、7.1 Calculations 7.1.1 Pigment portion of the liquid paint Calculate the mass of “soluble” barium in the hydrochloric acid extract, obtained by the method described in sub-clause8.2.3 of ISO6713, using the equation where a 0 is the barium concentration, in micrograms per millilitre, of the blank tes
43、t solution prepared by the method described in sub-clause 8.4 of ISO6713; a 1 is the barium concentration, in micrograms per millilitre, of the test solution obtained from the calibration graph; Standard matching solution No. Volume of the standard barium solution (4.6) Corresponding concentration o
44、f Ba in the standard matching solution ml 4g/ml 0 a1 2 3 4 5 0 2 5 10 20 40 0 0,8 2 4 8 16 a Blank matching solution.BS3900-B8:1986 BSI 11-1999 3 F 1 is the dilution factor referred to in6.3; m 0 is the mass, in grams, of “soluble” barium in the hydrochloric acid extract; V 1 is the volume, in milli
45、litres, of the hydrochloric acid plus ethanol used for the extraction described in sub-clause 8.2.3 of ISO6713 (assumed to be77ml); V 3 is the volume, in millilitres, of the aliquot portion of the hydrochloric acid plus ethanol extract taken for the test (6.2.1). Calculate the “soluble” barium conte
46、nt of the pigment portion of the paint, using the equation where C Ba1 is the “soluble” barium content, of the pigment portion of the paint, expressed as a percentage by mass of the paint; m 1 is the mass, in grams, of the test portion taken to prepare the solution described in sub-clause 8.2.3 of I
47、SO 6713; P is the pigment content of the liquid paint, expressed as a percentage by mass, obtained by the appropriate method described in clause 6 of ISO6713. 7.1.2 Liquid portion of the paint Calculate the mass of barium in the solution (extract), obtained by the method described in sub-clause 9.3
48、of IS06713, using the equation where b 0 is the barium concentration, in micrograms per millilitre, of the blank test solution prepared by the method described in sub-clause 6.5 of ISO6713; b 1 is the barium concentration, in micrograms per millilitre, of the test solution obtained from the calibrat
49、ion graph; F 2 is the dilution factor referred to in 6.3; m 2 is the mass, in grams, of barium in the liquid portion of the paint; V 2 is the volume, in millilitres, of the solution obtained by the method described in sub-clause9.3 of ISO6713 (= 100 ml); V 4 is the volume, in millilitres, of the aliquot portion of the solution taken for the test. Calculate the barium content of the liquid portion of the paint, using the equation where C Ba2 is the barium content, of the liquid portion of the paint, expressed as a percentage by mass of the paint; m 3 is
