饮用水中（类）金属及其化合物检测方案

WBNION ICP APPLICATION ICP-25/E HORIBA REPORT VERY RAPID ANALYSIS OF SUPPLY WATER AND ANIMAL FEED Authors： A. COSNIER， Jobin Yvon， France Application： Environment， foodElements： 36 elements 1Introduction ICP-OES is a multi-element technique that allows for the analysis of more than 75 elements on thePeriodic Table in a variety of matrices. This Application Note examines the analysis of six water andanimal feed samples. 2' Principle 2.11Technique used Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES) was employed for theelemental analysis of water and animal feed samples. The sample is nebulized and then injected intoan argon plasma. It is decomposed， atomized and ionized whereby the atoms and ions are excited.We measure the intensity of the light emitted when the atoms or ions return to lower levels of energy.Each element emits light at characteristic wavelengths and these lines can be used for quantitativeanalysis after a calibration. 2.2Wavelength choice The choice of the wavelength in a given matrix can be made using the “profile" function， or by using"lmage"， which is rapid semi-quantitative analysis mode using multiple wavelengths. The principle isthe same in either case： record the scans of analytes at low concentration， and of the matrix. Bysuperimposing the spectra， we see possible interferences. Page： 1/7 3Sample preparation The separate samples were dissolved using different concentrations and volumes of acids dependingon the sample type. The weights of the samples and the volume and concentrations of acid used areaiven in the table below. Weight (g) Acid (mL) Chicken feed 2.01415 250 of 5% HCI Mineral vitamin supplement 1.0093 500 of 2% HCI Diet food 3.5955 100 of 5% HCI The elements， their concentrations and the names of the standards 4Calibration standards preparation Name of thestandard Element Solutions fromSPEX Concentration STDLOW All elements ofinterest 0 ppm STDQC19 As， Be， Ca， Cd， Co， Cr， Cu， Fe， Li， Mg，Mn， Mo， Ni， Pb， Sb，Se， Sr， Ti， Tl， V， Zn Zr QC21-100PLZR2-2Y 5 ppm STDQC7 K， Si， Al， B， Ba， Na，Ag QC7A-100 5 ppm except Si 2.5and K 50 ppm STDPSW P， S， W PLP9-2YPLS9-2Y PLW9-2Y 5 ppm STDHg，10% HNO： Hg PLHG4-2Y 1 ppm STDSn， 10% HCI Sn PLSN5-2Y 1 ppm 5Instrument specification The work was undertaken on a JY ULTIMA. The specifications of this instrument are listed below. SPECTROMETER： Mounting Czerny-Turner Focal length 1m Thermoregulation Yes Variable resolution Yes Nitrogen purge Yes Grating number of grooves 2400 gr/mm Orders 2 1 st order resolution 0.005 nm 2 nd order resolution 0.010 nm RF GENERATOR： Type of generator Solid state， crystalcontrolled Observation Radial Frequency 40.68 MHz Control of gas flowrate By computer Control of pump flow By computer Cooling Air 6Operating conditions The operating conditions are listed in the table below. Generator power 1200 W Plasma gas flowrate 12 L/min Auxiliary gas flowrate 0 L/min Sheath gas flowrate 0.2 L/min Nebulizer gas flowrate 0.8 L/min Nebulizer flowrate 2.8 bars (41 psi) Sample uptake 1 mL/min Type of nebulizer Parallel flow Type of spray chamber Cyclonic Argon humidifier No Injector tube diameter 3.0 mm Because the calibration was undertaken in water and the samples have various matrices， a highgenerator power was used to minimize the matrix effects. 7Wavelength selection and analytical conditions The method is from our Semi-quantitative method， which is a simple and fast method to accuratelydetermine 35 elements in 2 minutes. The calibration is made with two points， 0 and 5 mg/L for mostelements. These standards are prepared in deionized water. The most sensitive lines for each of the elements were used for analysis and， in some cases； we usedtwo lines because of known interferences. Element Slits (um) Analysis mode Integration time (sec) All elements 20x15 Gauss 0.1-0.3 Element Wavelength(nm) Background correction(nm) Integration time (s) Ag 328.07 -0.0379 0.1 AI 308.21 +0.0434 0.1 Al 396.15 -0.0397/+0.0399 0.1 As 189.04 -0.0246 0.3 B 249.77 -0.0422 0.1 Ba 455.40 -0.0381 0.1 Be 313.04 -0.0423 0.1 Bi 223.06 +0.0417 0.3 Ca 317.93 -0.058 0.1 Cd 228.80 +0.0501 0.1 Co 228.62 -0.0398 0.1 Cr 267.72 -0.0252 0.1 Cu 324.75 +0.0335 0.1 Fe 259.94 -0.0255 0.1 Hg 194.16 -0.0348/+0.0355 0.2 K 766.49 -0.0458 0.1 Li 670.78 -0.067 0.1 Mg 279.81 +0.0329 0.1 Mn 257.61 -0.0387 0.1 Mo 202.03 -0.0423 0.1 Na 589.89 -0.0424 0.1 Ni 221.65 -0.0337 0.1 P 178.23 -0.0231 0.1 Pb 220.35 -0.0259 0.3 181.98 +0.0164 0.1 Sb 206.83 -0.0299 0.3 ICPJBNWON A PP LICATION ICP-25/E HORIBA REPORT Se 196.03 -0.0198 0.3 Si 251.61 -0.0252 0.1 Sn 189.99 -0.0221 0.1 Sr 407.77 +0.0641 0.1 Ti 337.28 -0.045 0.1 TI 190.86 -0.035 0.3 292.40 -0.024 0.1 311.07 +0.0439 0.1 W 207.91 -0.0256 0.1 Zn 213.86 +0.041 0.1 Zr 343.82 -0.0519 0.1 8Discussion In each of the samples， 35 elements were analyzed although， in the results presented here， only theelements that could be compared with certified samples are shown. As the calibration curve wasbetween 0 and 5 ppm， the samples were diluted by 10 when required. Both the diluted and undilutedresults are presented. 8.1 Waters. 19161 24160 Element Analysis(mg/L) Reference(mg/L) Analysis ICP-OES (ug/L) Reference(ug/L) AnalysisAAS (ug/L) Al 1.51 1.42±0.41 155.2 132.9 140 As 85.2 84 79 Cd 3.30 3.66±0.44 4.9 5.0 5.1 Cr 2.85 2.93±0.74 24.9* 11.7 10.4 Cu 1.11 1.14±0.12 18.1 <40 Fe 5.11 5.25±0.81 Hg 16.5 46.7 44 Mn 3.23 3.32±0.28 Mo 53.4 52.0 54 Ni 0.50 0.55±0.12 12.7 10.5 11.0 Pb 107.7 98.8 93 Zn 1.15 1.16±0.09 121.6 108.8 108 *High concentration due to an interference on the left part of the peak. ICP APPLICATION ICP-25/E HORIBA REPORT 8.2 Animal feed PROVENDER 5918 (2.0577 g in 250mL HCI5%) Element Sample-not diluted Sample-10 fold dilution Reference Ca 1.91 g/kg 2.2 2.1±0.5 Cu 8.5mg/kg 3.9±1.7 Mg 1.40 g/kg 1.58 1.7±0.2 P 1.54 g/kg 1.51 1.7±0.4 Zn 45.8 mg/kg 51.4±7.6 Cu and Zn were not determined in the diluted solution， because the concentration was already low inthe original solution. 8.3 Chicken feed Chicken Feed 5920 (2.0415 g in 250 mL HCI 5%) Element Sample · not diluted Sample- 10 fold dilution Reference Ca 0.84% 1.05% 0.91 ±0.09 Cu 17.7 mg/kg 14±4 Fe 162 mg/kg K 0.68% 0.81% 0.75±0.07 Mg 0.15% 0.16% 0.16±0.02 Mn 85.3 mg/kg 84±8 Na 0.14% 0.16% 0.14±0.02 P 0.56% 0.59% 0.59±0.05 Page： 6/7 8.4 Diet product and Mineral vitamin supplement Mineral vitamin supplement 2198a(1.0093 g in 500 mL of 2%HCI) Diet product 401 (3.8955 g in 100 mL of 5%HCI) Element Analysis Reference Analysis Reference As 0.3 mg/kg(

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