BS EN 16057-2012 Influence of metallic materials on water intended for human consumption Determination of residual surface lead (Pb) Extraction method《金属材料对人类饮用水的影响 残余表面铅(Pb)的测定 萃取.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 16057:2012Influence of metallic materialson water intended for humanconsumption Determinationof residual surface lead (Pb) Extraction methodBS EN 16057:2012 BRITISH STANDAR

2、DNational forewordThis British Standard is the UK implementation of EN 16057:2012.The UK participation in its preparation was entrusted to TechnicalCommittee EH/6, Effects of materials on water quality.A list of organizations represented on this committee can beobtained on request to its secretary.T

3、his publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimited 2012ISBN 978 0 580 69830 9ICS 67.250Compliance with a British Standard cannot confer immu

4、nity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 May 2012.Amendments issued since publicationDate Text affectedBS EN 16057:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16057 May 2012 ICS 67.250 English

5、Version Influence of metallic materials on water intended for human consumption - Determination of residual surface lead (Pb) - Extraction method Influence des matriaux mtalliques sur leau destine la consommation humaine - Dosage du plomb (Pb) rsiduel de surface - Mthode dextraction Einfluss metalli

6、scher Werkstoffe auf Wasser fr den menschlichen Gebrauch - Bestimmung des Rckstands an Oberflchenblei (Pb) - Extraktionsverfahren This European Standard was approved by CEN on 13 April 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for

7、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 any CEN member. This European Standard exists in three

8、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 versions. CEN members are the national standards bodie

9、s of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and Uni

10、ted Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE 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 16057:2012:

11、 EBS EN 16057:2012EN 16057:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Reagents .56 Apparatus .67 Test specimen 67.1 Method-control-sample (MCS) 67.1.1 Use of method control sample .67.1.2 Material of method-control-samp

12、le 67.1.3 Geometry 67.1.4 Manufacturing process for the MCS 77.2 Process sample (PS) .78 Test procedure .78.1 Method-control-sample (MCS) 78.2 Preparation of the test solution 78.3 Blank sample 88.4 Assembly of the test specimen 88.5 Extraction procedure .89 Control criteria for the method .910 Dete

13、rmination of residual surface lead (Pb) 1011 Test report . 11Bibliography . 12BS EN 16057:2012EN 16057:2012 (E) 3 Foreword This document (EN 16057:2012) has been prepared by Technical Committee CEN/TC 164 “Water supply”, the secretariat of which is held by AFNOR. This European Standard shall be give

14、n the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2012, and conflicting national standards shall be withdrawn at the latest by November 2012. Attention is drawn to the possibility that some of the elements of this document ma

15、y be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This European Standard is one of a series of test methods which support associated product standards. In respect of potential adverse effects on the quality of water int

16、ended for human consumption caused by metallic materials, attention is drawn to the fact that the relevant national regulations remain in force until the adoption of verifiable European acceptance criteria. Water intended for human consumption is hereafter referred to as “drinking water“ and means t

17、he same as the definition given at Article 2(1) of the Council Directive 98/83/EC on the quality of water intended for human consumption. This document describes a test method to determine the presence of lead (Pb) on the surface of copper alloys. According to the CEN/CENELEC Internal Regulations, t

18、he national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nethe

19、rlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16057:2012EN 16057:2012 (E) 4 Introduction During processing of lead containing copper alloys a lead film might be formed on the surface of the material. These lead layers

20、depend on the individual manufacturing process at the different production sites. The lead film on the inner surface of products will cause a lead release into the drinking water in the first weeks after a new product comes in contact with drinking water (short term behaviour). The lead release from

21、 the bulk material is not affected by the lead film on the surface and depends on the composition of the material. The bulk material can release lead for a long period (long term behaviour). It is possible to test materials for their lead release from the bulk material (EN 15664-1 and -2), so that p

22、roducts made of approved materials do not have to be tested for this characteristic. As the lead films on the surface depend on the individual manufacturing process, it is necessary to test the products or the manufacturing process. This test method is intended to be used as a process control method

23、 to assess the presence of lead films on the inner surface of products intended to come in contact with drinking water or to assess the efficiency of a manufacturing process to remove or minimise surface Pb, e.g. washing process to remove lead on surfaces. The implementation of an audit controlled p

24、rocess monitoring is an effective way to maintain safety of the products in the first weeks of their lifetime. This test method has been determined as a result of research programme Action 14/2005 objective A sponsored by DG Enterprise of the EU Commission. BS EN 16057:2012EN 16057:2012 (E) 5 1 Scop

25、e This European Standard describes a test method to determine the amount of lead on the surface of test specimens made from lead containing copper alloys. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its ap

26、plication. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. CEN/TS 13388:2008, Copper and copper alloys Compendium of compositions and products 3 Terms and definitions 3.1 method control sa

27、mple MCS tube of defined geometry made under defined conditions from a material of defined composition to check the extraction method Note 1 to entry: See 7.1.4. 3.2 process sample PS tube of defined geometry processed in the same way as a product 3.3 test specimen process sample or method control s

28、ample 3.4 extract test solution after the extraction procedure 3.5 extraction time time of contact between test solution and test specimen 4 Principle Lead films on the inner surface of a test specimen are dissolved by using a defined test solution. This procedure is repeated and each extract is ana

29、lyzed for lead. The total mass of the surface lead is calculated from the sum of the Pb removed. The method is sensitive to the concentration and age of the acids used for making up the test solution and the degree of shaking in the procedure, therefore, the effectiveness of the method is checked us

30、ing Method-Control-Samples. 5 Reagents The following chemicals shall be used: a) tetrafluoroboric acid (HBF4) 50% (m/m) CAS number 16872-11-0; b) sulphamidic acid (H3N-SO3) CAS number 5329-14-6. BS EN 16057:2012EN 16057:2012 (E) 6 All chemicals shall be analytical grade. NOTE Only use HBF4 solution

31、which has been stored at low temperatures (less than 8 C) in tightly closed bottles and in the dark to avoid degradation of the acid. 6 Apparatus The following apparatus shall be used: a) Volumetric flask (1l); b) Polyethylene (PE) bottles (20 ml to 50 ml); c) Test specimen caps made of inert materi

32、al (i.e. will not release lead or any other material that will adversely affect the test results) e.g. polyethene; d) Flat seal made of inert material; e) Sealing tape made of Polytetrafluoroethylene (PTFE); f) Stop watch; g) Optional: Mechanical shaker with a minimum amplitude of 20 mm and a deflec

33、tion rate of 4/s. 7 Test specimen 7.1 Method-control-sample (MCS) 7.1.1 Use of method control sample The MCS shall be used to verify the effectiveness of the extraction method. 7.1.2 Material of method-control-sample The MCS shall be made from CW614N - CuZn39Pb3. The value for lead shall be in the r

34、ange of 3,0 % 3,4 % Pb. The remainder of the composition including unavoidable impurities shall have the limits of the specification CW614N according to to CEN/TS 13388:2008. 7.1.3 Geometry The geometry shall be as in Figure 1. BS EN 16057:2012EN 16057:2012 (E) 7 Key A Dry machining B Length (mm) C

35、Diameter (mm) Figure 1 Test specimen dimensions 7.1.4 Manufacturing process for the MCS Starting with bar stock of MCS material with diameter 22 mm, bore out to diameter 16 mm then with a turning-tool to diameter 18 mm. The mean roughness shall be Ra = 0,8 m +/- 0,05 m by dry drilling. Make sure tha

36、t the machining diameter accuracy is at least of the tolerance 0,5 mm. Machining parameters: a) depth of cut: a = 1 mm; b) rotation speed: N = 630 1/min; c) feed rate: f = 0,066 mm/revolution; d) tool kit: using an cutting-tool holder for machining with hard-metal-pole and coolant hole; indexable in

37、sert (hard metal). Blow oil-free compressed air through the coolant hole for cooling and swarf removal. 7.2 Process sample (PS) The process sample shall be manufactured according to the production process to be tested in terms of composition, surface and process parameters. The geometry shall be as

38、in Figure 1, with the exception of the mean roughness. This parameter shall be to the same as the product specification whose production process is tested. 8 Test procedure 8.1 Method-control-sample (MCS) The MCS shall be used on a regular basis, the frequency being determined according to the quali

39、ty assurance procedure of the laboratory, to show the effectiveness of the extraction method. 8.2 Preparation of the test solution The test solution shall be freshly prepared for each test. Starting with a one-litre volumetric flask carry out the following: BS EN 16057:2012EN 16057:2012 (E) 8 a) add

40、 10,0 g 0,05 g of sulphamidic acid (5(b); b) add approximately 200 ml of demineralized water and shake thoroughly to dissolve the sulphamidic acid; c) add 15,0 ml 0,05 ml of tetrafluoroboric acid (5(a); d) dilute to 1 litre with demineralized water. 8.3 Blank sample Take a sample of the test solutio

41、n as blank sample for the determination of the blank value. Determine the lead content of the blank sample. If the lead content exceeds 1 mg/l the test solution cannot be used: discard and start again with fresh reagents. 8.4 Assembly of the test specimen Assemble the test specimen as shown in Figur

42、e 2. Key A step 1 B step 2 C step 3 D step 4 E step 5 Figure 2 Illustration of the assembly procedure of test specimen 8.5 Extraction procedure a) Prepare 10 labelled PE bottles. b) Blow out the test specimen with dry oil-free air and make sure that there is no swarf in the bore. c) Wrap sealing tap

43、e around one end of the test specimen and close this prepared end with a test specimen cap (see Figure 2, steps 1 to 4). d) Add to the test specimen exactly 15,0 ml 0,05 ml of the test solution. e) Close the open end with a flat seal and a PE-cap (Figure 2, step 5). f) Start shaking within 30 s afte

44、r adding the test solution. BS EN 16057:2012EN 16057:2012 (E) 9 g) Shake the test specimen in the longitudinal direction, either horizontally or vertically, with a minimum amplitude of 20 mm. Ensure the test specimen goes through shaking deflections at a rate of 4 per s (see Figure 3). h) Shake the

45、test specimen for 120 s. i) Open the end with the flat seal and a PE-cap and pour the extract from the test specimen into the first or sequential labelled PE bottle within 30 s after finishing the shaking. j) Immediately repeat the extraction procedure with this test specimen from point e) above ano

46、ther nine times (in total 10 times). k) Analyze the extract of each of the 10 PE bottles. Key A = 4 deflections in one second B = deflection 40 mm minimum C = one second D = amplitude 20 mm minimum E = center 1,2,3,4 = number of deflections The deflection is defined as the sum of the amplitude to on

47、e side and to the other side during the shaking procedure. Figure 3 Schematic description of the shaking procedure NOTE It is recommended to test only one test specimen at a time in order to meet the prescribed extraction time. 9 Control criteria for the method For verification of the method by usin

48、g MCS the following criteria shall be met: First extract: cPb 1 200 mg/l 5thto 10thextract: cPb 5-10 10 mg/l where cPb, j= concentration of Pb of the jthextract in mg/l BS EN 16057:2012EN 16057:2012 (E) 10 10 Determination of residual surface lead (Pb) Correct the analytical results for the blank va

49、lue. List the Pb contents of the extract as a function of the extraction time as shown in Table 1 and plot the Pb concentration versus cumulative time in a diagram (see Figure 4). Table 1 Results table Extract 1 2 3 4 5 6 7 8 9 10 Extraction time (s) 120 120 120 120 120 120 120 120 120 120 Cumulative time (s) 120 240 360 480 600 720 840 960 1080 1200 cPb(mg/l) Key 1 = Concentration of Pb (mg/l) 2 = Cumulative time (s) Figure 4 Diagram (Example) Calculate the total