1、January 2013 Translation by DIN-Sprachendienst.English price group 10No 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).IC
2、S 77.040.30!$L“1934156www.din.deDDIN EN 10200Chemical analysis of ferrous materials Determination of boron in steels Spectrophotometric method;English version EN 10200:2012,English translation of DIN EN 10200:2013-01Chemische Analyse von Eisenwerkstoffen Bestimmung von Bor in Stahl Spektralphotometr
3、isches Verfahren;Englische Fassung EN 10200:2012,Englische bersetzung von DIN EN 10200:2013-01Analyse chimique des matriaux ferreux Dtermination du bore dans les aciers Mthode spectrophotomtrique;Version anglaise EN 10200:2012,Traduction anglaise de DIN EN 10200:2013-01SupersedesDIN EN 10200:1992-05
4、www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 17pages12.12 DIN EN 10200:2013-01 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ECISS/TC 102 “Methods of chemical analys
5、is for iron and steel” (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was the Normenausschuss Eisen und Stahl (Iron and Steel Standards Committee), Working Committee NA 021-00-30 AA Analysenverfahren. Amendments This standard differs from DIN EN 10200:1992-05 as
6、follows: a) Annex A (informative) “Precision data” has been revised; b) the standard has been editorially revised. Previous editions DIN EN 10200: 1992-05 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 10200 October 2012 ICS 77.040.30 Supersedes EN 10200:1991English Version Chemical analysis o
7、f ferrous materials - Determination of boron in steels - Spectrophotometric method Analyse chimique des matriaux ferreux - Dtermination du bore dans les aciers - Mthode spectrophotomtrique Chemische Analyse von Eisenwerkstoffen - Bestimmung von Bor in Stahl - Spektralphotometrisches Verfahren This E
8、uropean Standard was approved by CEN on 17 August 2012. CEN members are bound to comply with the CEN/CENELEC Internal 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
9、 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 official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN memb
10、er 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 Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, Fra
11、nce, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES K
12、OMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 10200:2012: EEN 10200:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53
13、Principle 54 Reagents .55 Apparatus .66 Sampling .87 Procedure .88 Expression of results . 119 Test report . 11Annex A (informative) Precision data . 13Bibliography . 15DIN EN 10200:2013-01 EN 10200:2012 (E) 3 Foreword This document (EN 10200:2012) has been prepared by Technical Committee ECISS/TC 1
14、02 “Methods of chemical analysis for iron and steel”, the secretariat of which is held by SIS. 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 April 2013, and conflicting national standards shall
15、be withdrawn at the latest by April 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights other than those identified above. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This docum
16、ent supersedes EN 10200:1991. Since the previous edition, no technical changes have been made, but the text has been editorially revised. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard:
17、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, S
18、weden, Switzerland, Turkey and the United Kingdom. DIN EN 10200:2013-01 EN 10200:2012 (E) 4 Introduction The development of the method was carried out by a working group under French convenorship. The results of the inter-laboratory tests have shown that the determination of lower limit application
19、of the method should be 0,000 4 % (m/m) boron, based on a relative deviation not exceeding 10 % within 66 % confidence limits. However, further work has shown that the method may be used for lower boron contents if a higher relative deviation is acceptable. DIN EN 10200:2013-01 EN 10200:2012 (E) 5 1
20、 Scope This European Standard specifies a spectrophotometric method for the determination of boron in steels. The method is applicable to non-alloyed and alloyed steels with boron contents of 0,000 4 to 0,012 0 % (m/m). 2 Normative references The following documents, in whole or in part, are normati
21、vely referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 14284, Steel and iron Sampling and preparation of samples
22、 for the determination of chemical composition (ISO 14284) 3 Principle Dissolution of a test portion in hydrochloric and nitric acids. Decomposition of boron compounds (nitrides, etc.) with orthophosphoric and sulphuric acids at 290 C. Spectrophotometric measurement at a wavelength of 543 nm of the
23、complex formed between boric acid and curcumin in buffered acetic medium. 4 Reagents During the analysis, use only reagents of recognised analytical grade and distilled water or water of equivalent purity. 4.1 Pure iron, free of boron or of known low boron content. 4.2. Crystalline sodium hypophosph
24、ite monohydrate (NaH2PO2.H2O). 4.3 Hydrochloric acid, HCl (20= 1,19 g/ml). 4.4 Nitric acid, HNO3(20= 1,40 g/ml). 4.5 Sulphuric acid, H2SO4(20= 1,84 g/ml). 4.6 Orthophosphoric acid, H3PO4(20= 1,71g/ml). 4.7 Acetic acid free of aldehyde, CH3COOH (20= 1,05 g/ml). Test for absence of aldehyde: Place 20
25、ml of the acetic acid (4.7) to be tested and 1 ml of a 1 g/l solution of potassium permanganate (KMnO4) into a 50 ml beaker. In the absence of aldehyde, the initial violet colour of the potassium permanganate will persist; otherwise the solution will become brown, easily identifiable after 15 min. D
26、IN EN 10200:2013-01 EN 10200:2012 (E) 6 4.8 Mixture of acetic and sulphuric acids. Add in small portions whilst cooling under water and swirling, a volume of sulphuric acid (4.5) to an equal volume of acetic acid (4.7). 4.9 Acetic buffer solution. Dissolve 225 g of ammonium acetate in 400 ml of wate
27、r. Add 300 ml of acetic acid (4.7). Filter the solution obtained into a 1 000 ml polyethylene one-mark volumetric flask. Dilute to the mark with water and mix. 4.10 Sodium fluoride, 40 g/l solution. 4.11 Boron, 100 mg/l standard solution. Dissolve 0,285 8 g of boric acid in water in a 500 ml one-mar
28、k volumetric flask. Dilute to the mark with water and mix. Store this solution in a polyethylene flask. 1 ml of this solution contains 0,1 mg of boron. 4.12 Boron, 2 mg/l standard solution. Transfer 20 ml of the boron standard solution (4.11) into a 1 000 ml one-mark volumetric flask. Dilute to the
29、mark with water and mix. Store this solution in a polyethylene flask. 1 ml of this solution contains 2 g of boron. 4.13 Curcumin, 1,25 g/l acetic solution (prepared immediately before use). Dissolve 0,125 g of curcumin in 60 ml of acetic acid (4.7) in a polyethylene or quartz vessel. Heat at 40 C in
30、 a water bath and stir with a magnetic stirrer. After dissolution, cool and transfer into a 100 ml polyethylene one-mark volumetric flask. Dilute to the mark with acetic acid (4.7) and mix. 5 Apparatus Glassware containing boron shall not be used and shall be replaced by polyethylene and quartz vess
31、el rinsed with acetic acid (4.7), then with water and finally dried. 5.1 100 ml quartz beakers, with quartz covers (outside dimensions: 51 mm diameter and 70 mm height). 5.2 Aluminium alloy blocks, allowing a temperature of 290 C to be achieved and maintained in the test solutions throughout the fum
32、ing period. The block has holes designed to allow the location of the 100 ml quartz beakers and is heated by surface contact with a hotplate. NOTE Diagrams of these blocks are shown in Figures 1 and 2. The dimensions of the holes should be adapted to the dimensions of the quartz beakers available. 5
33、.3 50 ml polyethylene one-mark volumetric flasks. 5.4 100 ml polyethylene flasks. 5.5 Spectrophotometer, suitable for measuring absorbance at a wavelength of 543 nm, with 20 mm cells. DIN EN 10200:2013-01 EN 10200:2012 (E) 7 Dimensions in millimetres NOTE Adapt the dimensions of the holes according
34、to the dimensions of the beakers available. Figure 1 Example of circular aluminium alloy heating block DIN EN 10200:2013-01 EN 10200:2012 (E) 8 Dimensions in millimetres NOTE Adapt the dimensions of the holes according to the dimensions of the beakers available. Figure 2 Example of a rectangular alu
35、minium alloy heating block 6 Sampling Sampling shall be carried out in accordance with EN ISO 14284 or an appropriate national standard for steel and iron. The chips thickness shall be smaller than 1 mm. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,001 g, a test portion (m) as indicated belo
36、w: m = 1 g 0,05 g for boron contents less than 0,006 %; m = 0,5 g 0,03 g for boron contents from 0,006 % to 0,012 %. NOTE For steel grades with nickel and cobalt total content greater than 30 %, do not take a test portion larger than 0,5 g. DIN EN 10200:2013-01 EN 10200:2012 (E) 9 7.2 Blank test Wit
37、hin each analytical series and in parallel with the analysis of the samples, carry out the analysis of pure iron test portions (4.1), having a mass corresponding to that of the test portions (see 7.1), following the same procedure and using the same quantities of all the reagents. The absorbance of
38、the blank test solution (bA ) and that of the corresponding blank compensating solution (bcA ) are thus obtained. 7.3 Determination 7.3.1 Preparation of the test solution Place the test portion (7.1) in a 100 ml quartz beaker and add 10 ml hydrochloric acid (4.3) and 5 ml of nitric acid (4.4). Cover
39、 the beaker with a quartz cover and leave it at ambient temperature in order to avoid possible loss of boron at higher temperatures. Wait until dissolution is complete or until the end of the effervescence for samples which are difficult to dissolve. Then add carefully 10 ml of orthophosphoric acid
40、(4.6) and 5 ml of sulphuric acid (4.5). Heat to copious white sulphuric fumes, swirling from time to time in order to recover any particles attached to the sides of the beaker. Place the beaker in a hole of the aluminium alloy block (5.2) and place the block on a heat source allowing a temperature o
41、f 290 C to be obtained in the solutions. Maintain the heating for 30 min, taking care to replace the quartz cover after the appearance of white fumes. NOTE The temperature of 290 C 5 C is obtained by calibration of the heat source by means of a thermometer, graduated from 0 to 350 C, immersed in a b
42、eaker identical to those used for the test and containing the same amounts of the dissolution reagents. Remove the beaker from the heat source and allow to cool. Dilute the syrupy solution with 30 ml of water. Warm whilst stirring. Remove from the heat source. Then add carefully 5 ml of hydrochloric
43、 acid (4.3) and bring to the boil. Add 3 g of sodium hypophosphite (4.2). Allow to boil gently for 15 min. Remove from the heat source and allow to cool. Transfer the solution quantitatively into a 50 ml polyethylene one-mark volumetric flask. Dilute to the mark with water and mix. 7.3.2 Formation o
44、f the coloured complex Transfer 1,0 ml of the test solution obtained in accordance with 7.3.1 into a 100 ml polyethylene flask (5.4) previously cleaned and dried. Add into the flask, whilst swirling in a circular movement to avoid contact with the stopper, the following volumes of reagents: 6,0 ml o
45、f the mixture of acetic and sulphuric acids (4.8), avoiding contact of the pipette with the neck and sides of the flask; mix; 6,0 ml of the curcumin acetic solution (4.13); stopper the flask and mix. Allow to stand for 2 h 30 min for complete development of the colour. Then add: 1,0 ml of orthophosp
46、horic acid (4.6) to stabilise the colour. Shake and allow to stand for 30 min; 30,0 ml of the acetic buffer solution (4.9). The solution turns orange. Stopper and shake. Allow to stand for exactly 15 min. DIN EN 10200:2013-01 EN 10200:2012 (E) 10 7.3.3 Compensating solution Transfer 1,0 ml of the te
47、st solution obtained in accordance with 7.3.1 into a 100 ml polyethylene flask (5.4) previously cleaned and dried. Add 0,2 ml of sodium fluoride solution (4.10) to the bottom of the flask. Carefully swirl the small volume of solution. Allow to stand for 1 h. Continue as in 7.3.2. from “Add into the
48、flask, whilst swirling in a circular movement“. 7.3.4 Spectrophotometric measurements NOTE In order to carry out the spectrophotometric measurements on all the solutions whilst waiting exactly 15 min after the addition of the acetic buffer solution, it is advisable to divide them into a series of 6 measurements, i.e. 12 flasks. In fact, for long series of measurements where the waiting time cannot be strictly adhered to, the formation of a cloudiness in the solu
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