1、STD=BSI DD ENV LgBDO-ENGL 2000 lbZibb9 OBb7Lb7 420 M DRAFT FOR DEVELOPMENT Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrix ICs 77.120.60 NO COPYING WITHOUT BSI PERMISSIO
2、N EXCEPT AS PERMIITED BY COPYRIGHT LAW ID ENV 13800:2000 STD*BSI DD ENV L38OO-ENGL 2000 = Lb2qbbS 08b9170 or - mixture of nitric acidtartaric acid : or - mixture of nitric acid/fluoboric acid. Dilution of the test solution to a defined volume, and determination of the analyte concentration using one
3、 of the two techniques described in 3.2. 3.2 Instrumental techniques 3.2.1 Flame atomic absorption spectrometry (FAAS) The analyte concentration in the test solution is obtained by : - nebulization of the test solution into the flame of an atomic absorption spectrometer ; - measurement of the absorp
4、tion of the resonance line energy of the spectrum from the element at the relevant wavelength (absorbency) ; - comparison with that of matrix-matched calibration solutions of the same element. 3.2.2 Inductively coupled plasma emission spectrometry (ICP-ES) The analyte concentration in the test solut
5、ion is obtained by : - nebulization of the test solution into the plasma of an inductively coupled plasma optical emission spectrometer ; - measurement of the intensity of the emission signal from the spectrum of the elements to be determined at the relevant wavelength ; - comparison with that of ma
6、trix-matched calibration solutions of the same element. Page 6 ENV 13800:ZOOO 4 Apparatus 4.1 General Use ordinary apparatus as available in a chemical laboratory. All glassware and plastic ware to be used shall be cleaned with diluted nitric acid (5.2.2) and thoroughly rinsed with water. 4.2 Volume
7、tric glassware 4.2.1 IS0 1042:1983 class A. One-mark volumetric flasks of capacities 100 ml, 250 ml, 500 ml, and 1 O00 ml in accordance with 4.2.2 with IS0 648:19n class A. One-mark pipettes of capacities 2 ml, 5 ml, 10 ml, 15 ml, 20 ml, 25 ml, 50 ml and 100 ml in accordance 4.3 Plastlc ware The fol
8、lowing are required : - Polytetrafluoroethylene (PTFE) beakers of 250 ml capacity ; - Suitable PTFE covers ; - One-mark volumetric flasks of 1 O0 ml capacity. 4.4 Instruments 4.4.1 Flame atomic absorption spectrometer Flame atomic absorption spectrometer (FAAS) equipped with laminar flow burners sui
9、table for acetylene-air, hydrogen-air or acetylene-nitrous oxide flames, and with radiation sources such as hollow cathode lamps (HCL) or electrode-less discharge lamps (EDL) as appropriate to the element to be determined. The instrument shall be used in accordance with the manufacturers instruction
10、s and the performance checked (see the IS0 documents in preparation, numbers 00023056 and 00023057). DANGER exhausted externally. To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be 4.4.2 Inductively coupled plasma emission spectrometer Inductively coupled pla
11、sma emission spectrometer (ICP-ES), either a simultaneous instrument with the relevant wavelengths installed or a sequential instrument where a monochromator system allows the selection of wavelengths (see the IS0 document in preparation, number 00021288). The instrument shall be used in accordance
12、with the manufacturers instructions and the performances checked (see the IS0 document in preparation, number 00023058). DANGER exhausted externally. To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be STD.BS1 DD ENV 13800-ENGL 2000 Lb24bb9 Ob177 5T7 Page 7 EN
13、V 13800:2000 5 Reagents 5.1 General For all stages of analysis, unless otherwise stated, use only reagents of recognised analytical grade, preferably with an actual analysis, and only water of at least grade 2, as specified in IS0 3696. Prepare all solutions using the same container of each reagent.
14、 5.2 Nitric acid (“0,) 5.2.1 Concentrated nitric acid Nitric acid which p20 = 1,41 g/ml. 5.2.2 Nitric acid 1 :1 (vh) Add to one volume of water, the same volume of nitric acid (5.2.1) in a suitable container and mix thoroughly. This diluted acid is also used to clean the laboratory ware. 5.2.3 Nitri
15、c acid 1 :2 (vh) Add 200 ml nitric acid (5.2.1) to 400 ml water into a 1 O00 ml beaker and mix thoroughly. 5.3 Tartaric acid solution (C cover with a watch-glass and heat gently until dissolution is complete. Boil gently until nitrous fumes are expelled and then, allow to cool. Transfer into a 1 O00
16、 ml volumetric flask (4.2.1), make up to the mark with water and mix thoroughly. - _ STD*BSI DD ENV L38OO-ENGL 2000 = lb2ribb9 08b9178 ri33 Page 8 ENV 13800:2 5.7 Standard solutions 5.7.1 Standard solution (1gA) 5.7.1.1 General Eaher use commercially available certified standard solutions or prepare
17、 standard solutions as described in 5.7.1.2 to 5.7.1.12. 5.7.1.2 Solutions for silver, bismuth, cadmium, copper, nickel, thallium and zinc Weigh (1 ,WO f 0,001) g of the relevant metal of 99,9% (m/m) minimum purity and transfer into a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a wat
18、ch glass, and heat gently until dissolution is complete. Allow to cool, then transfer into a 1 O00 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. Store the silver solution in the dark. 5.7.1.3 Solution for aluminium The aluminium used for this solution shall be
19、in a form of clean wire, foil or pieces cut from an ingot. Do not use aluminium powder because of possible oxidation of its very large specific surface involved. Weigh (1,000 f 0,001) g of aluminium of 99,9 % (dm) minimum purity and transfer into a 250 ml beaker, add 10 ml hydrochloric acid (5.4), c
20、over with a watch glass, and heat gently until dissolution is complete. Allow to cool, then transfer into a 1 O00 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. NOTE If aluminium of high purity is used, it is possible to increase the dissolution rate by adding 1
21、 ml of nickel chloride solution (10911). If nickel and aluminium are to be determined together, use 1 ml of mercury (Il) chloride solution (lo) instead of the nickel chloride solution. 5.7.1 A Solution for arsenic Dry approximately 5 g of arsenic oxide (As203, 99,9 % (m/m) minimum purity) in an oven
22、 at (105 f 2)“C for two hours and allow to cool completely in a desiccator. Weigh (1,320 I 0,001) g of dried arsenic dioxide and transfer into a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a watch glass, and swirl until dissolution is complete. Transfer into a 1 O00 ml volumetric fla
23、sk (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.5 Solution for barium Dry approximately 5 g of barium carbonate (BaCO, 99,9 % (dm) minimum purity) in an oven at (105 f 2)“C for two hours and allow to cool completely in a desiccator. Weigh (1,437+ 0,001) g of dried barium ca
24、rbonate and transfer into a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a watch glass, and swirl until dissolution is complete. Transfer into a 1 000ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.6 Solution for calcium Dry approximately 5 g
25、 of calcium carbonate (Caco3, 99,9 % (dm) minimum purity) in an oven at (105 f 2)“C for two hours and allow to cool completely in a desiccator. Weigh (2,497 f 0,001) g of dried calcium carbonate and transfer into a 250 ml beaker, add 25 ml of water, then 75 ml of nitric acid (5.2.3), cover with a wa
26、tch glass and swirl until dissolution is complete. Transfer into a 1 WO ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.7 Solution for sodium Dry approximately 5 g of sodium chloide (NaCI, 99,9 % (m/m) minimum purity) in an oven at (105 f 2)“C for two hours
27、 and allow to cool completely in a desiccator. Weigh (2,542 f 0,001) g of dried sodium chloride and transfer into a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a watch glass and swirl until dissolution is STD*BSI DD ENV L3BOO-ENGL 2000 Lb24bb7 OBb9L79 37T Page 9 ENV 13800:ZOOO comple
28、te. Transfer into a 1 O00 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.8 Solution for sulphur Dry approximately 5 g of sodium sulphate (Na2S04, 99,9 % (m/m) minimum purity) in an oven at (105 * 2)“C for two hours and allow to cool completely in a desicca
29、tor. Weigh (4,430 k 0,001)s into a 250 ml beaker, add 75 ml of nitric acid (5.2.3), cover with a watch glass and swirl until dissolution is complete. Transfer into a 1000 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.9 Solution for antimony Dry approximat
30、ely 5 g of antimony oxide (Sb,O, 99,9% (m/m) minimum purity) in an oven at (105 * 2)“C for two hours and allow to cool completely in a desiccator. Weigh (1,197 k 0,001) g into a 250 ml beaker, add 25 ml water and 50 ml of hydrochloric acid (5.4), cover with a watch glass and swirl until dissolution
31、is complete. Transfer into a 1 O00 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.10 Solution for selenium Weigh (1,000 f 0,001) g of selenium of 99,9 % (m/m) minimum puriity into a 250 ml beaker, add 100 ml of nitric acid (5.2.2), cover with a watch glass
32、, and heat gently to initiate the reaction of dissolution. Cool if the reaction proceeds too vigorously. Allow to cool, then transfer into a 1000 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.1 1 Solution for tin Weigh (1,000 f 0,001) g of tin of 99,9% (m
33、/m) minimum purity into a 250 ml beaker, add 100 ml of hydrochloric acid (5.4), cover with a watch glass and heat gently until dissolution is complete. Allow to cool, then transfer into a 1000 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly. 5.7.1.12 Solution for
34、tellurium Weigh (1,000 k 0,001)s of tellurium of 99,9 % (m/m) minimum purity into a 250 ml beaker, add 100 ml of nitric acid (5.2.2), cover with a watch glass, and swirl until dissolution is complete. Transfer into a 1000 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoro
35、ughly. 5.7.2 Working standard solutions 5.7.2.1 selenium, tellurium, thallium and zinc (10 mg/l) Solutions of silver, arsenic, barium, bismuth, calcium, cadmium, copper, sodium, nickel, sulphur, Using a 10 ml pipette (4.2.2), transfer 10 ml of the relevant standard solution (5.7.1) into a 1 O00 ml v
36、olumetric flask (4.2.1). Add 150 ml of nitric acid (5.2.3), then make up to the mark with water and mix thoroughly. Each solution shall be prepared on the day of use. 5.7.2.2 selenium, tellurium, thallium and zinc (100 mgA) Solutions of silver, arsenic, barium, bismuth, calcium, cadmium, copper, sod
37、ium, nickel, sulphur, Using a 50 ml pipette (4.2.2), transfer 50 ml of the relevant standard solution (5.7.1) into a 500 ml volumetric flask (4.2.1). Add 75 ml of nitric acid (5.2.3), then make up to the mark with water and mix thoroughly. 5.7.2.3 Solutions of aluminium, antimony and tin (10 mgh) Us
38、ing a 10 ml pipette (4.2.2), transfer 10 ml of the relevant standard solution (5.7.1) into a 1 O00 ml volumetric flask (4.2.1). Add 20 ml of tartaric acid solution (5.3), 150 ml of nitric acid (5.2.3), then make up to the mark with water and mix thoroughly. Each solution shall be prepared on the day
39、 of use. _ STD*BSI DD ENV 13800-ENGL 2000 = 1b211bb7 08b718O O71 Page 10 ENV 13:2000 5.7.2.4 Solutions of aluminium, antimony and tin (100 mgil) Using a 50 ml pipette (4.2.2), transfer 50 ml of the relevant standard solution (5.7.1) into a 500 ml volumetric flask (4.2.1). Add 10 ml of tartaric acid
40、solution (5.3), 75 ml of nitric acid (5.2.3), then make up to the mark with water and mix thoroughly. 5.7.2.5 Multi element solutions (either 1 O mg/l or 1 O0 mgA) Provided that there are no reactions between the standard solutions (lgA), multi-element solutions may be prepared. For this purpose, tr
41、ansfer either 10 ml or 100 ml of each relevant standard solution (5.7.1) of the elements required into a 1000 ml volumetric flask (4.2.1). Add the appropriate volume of acid, then make up to the mark with water and mix thoroughly. The muki-element solution (10 mgh) shall be prepared on the day of us
42、e. 6 Sampling and sample preparation Sampling and preparation of the laboratory sample shall be carried out in accordance with EN 12402. 7 Procedure 7.1 Preparation of the test solution Because of the difficulties in maintaining antimony plus tin in solution of nitric acid, different possibilities f
43、or dissolution of the test sample are described. 7.1.1 Lead and lead alloys with antimony plus tin contents less than O,= %(din) Weigh (2,000 0,001) g of the laboratory sample and transfer this test portion into a 250 ml beaker. Add 25 ml nitric acid (5.2.3), cover with a watch glass, then warm on a
44、 hot plate until dissolution of the test portion is complete and all nitrous fumes have dissipated. Allow to cool, then transfer into a 100 ml volumetric flask (4.2.1), make up to the mark with water and mix thoroughly. NOTE If the solution obtained is not clear, prepare another test solution follow
45、ing 7.1.2. 7.1.2 Lead alloys with antimony plus tin contents greater than 0,05 % (mhn) Two possibilities of dissolution are described, either : - mixture of nitric acidhartaric acid ; or - mixture of nitric aciMluoboric acid. Tartaric acid can cause fouling of the burner in FAAS ; fluoboric acid can
46、 corrode nebulizer and torch in ICP. The analyst shall choose the dissolution method most suited to the particular analysis and instrument involved. 7.1.2.1 Dissolution in nitric acidltartaric acid Weigh (2,000 * 0,001) g of the laboratory sample and transfer this test portion into a 250 ml beaker.
47、Add 25 ml of nitric acid (5.2.3) and 10 ml of tartaric acid solution (5.3), cover with a watch-glass, then warm on a hot plate until dissolution of the test portion is complete and all nitrous fumes have dissipated. Allow to cool, then transfer into a 100 ml volumetric flask (4.2.1), make up to the
48、mark with water and mix thoroughly. STDOBSI DD ENV 13800-ENGL 2000 Lb24bb9 OBb7LBL T28 Page 11 ENV 13800:2000 7.1.2.2 Dissolution in nitric acidfluoboric acid Weigh (2,000 * 0,001) g of the laboratory sample and transfer this test portion into a 250 ml PTFE beaker (4.3) ; add 25 ml of nitric acid (5
49、.2.3) and 10 ml of fluoboric acid (5.5). Place a PTFE cover (4.3) on the beaker, then warm on a hot plate until dissolution of the test portion is complete and all nitrous fumes have dissipated. Allow to cool, then transfer into a 100 ml volumetric flask (4.2.1), make up to the mark with water and mix thoroughly. Immediately, transfer this test solution into a plastic flask to avoid any attack on the glassware. For the analysis of trace elements that can be removed from the glassware by the action of fluoboric acid, e.g. AI, Ca, Na, the test solution is transferre
