DIN EN 16057-2012 Influence of metallic materials on water intended for human consumption - Determination of residual surface lead (Pb) - Extraction method German version EN 16057 .pdf

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1、-XO7UDQVODWLRQE,16SUDFKHQGLHQVW(QJOLVKSULFHJURXS1RSDUWRIWKLVWUDQVODWLRQPDEHUHSURGXFHGZLWKRXWSULRUSHUPLVVLRQRI,1HXWVFKHV,QVWLWXWIU1RUPXQJH9%HUOLQ%HXWK9HUODJ*PE+%HUOLQ*HUPDQKDVWKHHFOXVLYHULJKWRIVDOHIRU*HUPDQ6WDQGDUGV ,11RUPHQ , b) sulphamidic acid (H3N-SO3) CAS number 5329-14-6. DIN EN 16057:2012-07 E

2、N 16057:2012 (E) 6 All chemicals shall be analytical grade. NOTE Only use HBF4 solution 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

3、) Polyethylene (PE) bottles (20 ml to 50 ml); c) Test specimen caps made of inert material (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) S

4、top watch; g) Optional: Mechanical shaker with a minimum amplitude of 20 mm and a deflection 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-sa

5、mple The MCS shall be made from CW614N - CuZn39Pb3. The value for lead shall be in the range 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

6、as in Figure 1. DIN EN 16057:2012-07 EN 16057:2012 (E) 7 Key A Dry machining B Length (mm) C 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 dia

7、meter 18 mm. The mean roughness shall be Ra = 0,8 m +/- 0,05 m by dry drilling. Make sure that 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: u

8、sing an cutting-tool holder for machining with hard-metal-pole and coolant hole; indexable insert (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

9、 be tested in terms of composition, surface and process parameters. The geometry shall be as 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) Th

10、e MCS shall be used on a regular basis, the frequency being determined according to the quality 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 o

11、ne-litre volumetric flask carry out the following: DIN EN 16057:2012-07 EN 16057:2012 (E) 8 a) add 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);

12、 d) dilute to 1 litre with demineralized water. 8.3 Blank sample Take a sample of the test solution 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 w

13、ith fresh reagents. 8.4 Assembly of the test specimen Assemble the test specimen as shown in Figure 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 sp

14、ecimen with dry oil-free air and make sure that there is no swarf in the bore. c) Wrap sealing tape 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) Clos

15、e the open end with a flat seal and a PE-cap (Figure 2, step 5). f) Start shaking within 30 s after adding the test solution. DIN EN 16057:2012-07 EN 16057:2012 (E) 9 g) Shake the test specimen in the longitudinal direction, either horizontally or vertically, with a minimum amplitude of 20 mm. Ensur

16、e the test specimen goes through shaking deflections at a rate of 4 per s (see Figure 3). h) Shake the 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

17、shaking. j) Immediately repeat the extraction procedure with this test specimen from point e) above another 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

18、 E = center 1,2,3,4 = number of deflections The deflection is defined as the sum of the amplitude to one 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 t

19、he prescribed extraction time. 9 Control criteria for the method For verification of the method by using 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 DIN EN 16057:2012-07 EN 1605

20、7:2012 (E) 10 10 Determination of residual surface lead (Pb) Correct the analytical results for the blank value. 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 Resu

21、lts 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 mass of Pb (mPb) from e

22、xtract 1-5 according to: =51,iSiPbPbVcmwhere cPb, j= concentration of Pb of the jthextract in mg/l; DIN EN 16057:2012-07 EN 16057:2012 (E) 11 mPb = Total mass of extracted lead in the first five extracts in mg; VS= Volume of the test solution in litre (see 8.5, d). 11 Test report The test-report sha

23、ll contain: a) name and address of the test institute; b) name(s), function(s) and signature(s) or equivalent identification of person(s) authorizing the test report; c) unique identification number, signature and title or an equivalent marking of person (s) accepting technical responsibility for th

24、e test report and date of issue; d) name and address of the customer; e) name and address of the manufacturer of the MCS; f) reference to this standard; g) all details required for the complete identification of the process sample (PS); 1) chemical composition of the PS; 2) surface characteristics o

25、f the PS; 3) description of the manufacturing steps used to produce the PS; 4) description of the production process to be tested; h) date of starting and finishing the test; i) details of any deviation from the procedure specified; j) specification of the analytical devices used; k) diagram lead co

26、ncentration versus the cumulative time for testing PS; l) diagram lead concentration versus the cumulative time for MCS; m) results (results table, diagram, total mass of lead (Pb). DIN EN 16057:2012-07 EN 16057:2012 (E) 12 Bibliography 1 EN 15664-1, Influence of metallic materials on water intended for human consumption Dynamic rig test for assessment of metal release Part 1: Design and operation 2 EN 15664-2, Influence of metallic materials on water intended for human consumption Dynamic rig test for assessment of metal release Part 2: Test waters DIN EN 16057:2012-07