HR-CS SS GFAAS â Determination of Cd and Pb in sediment
HR-CS SS GFAAS â Determination of Cd and Pb in sediment
HR-CS SS GFAAS â Determination of Cd and Pb in sediment
You also want an ePaper? Increase the reach of your titles
YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.
contrAA ® solid protects waterbodies pollution <strong>and</strong>susta<strong>in</strong>s renaturation<strong>HR</strong>-<strong>CS</strong> <strong>SS</strong> <strong>GFAAS</strong> – <strong>Determ<strong>in</strong>ation</strong> <strong>of</strong> <strong>Cd</strong> <strong>and</strong> <strong>Pb</strong> <strong>in</strong><strong>sediment</strong>Application Report: AR_environment_e_0109 1/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de
IntroductionSediments act as archives, where chang<strong>in</strong>g conditions can be traced for heavy metal cycl<strong>in</strong>g <strong>in</strong> thegeo- <strong>and</strong> atmosphere. Thus the <strong>in</strong>creased emission <strong>of</strong> trace elements related to <strong>in</strong>dustrial orm<strong>in</strong><strong>in</strong>g activities is known to enhance significantly the total trace element concentrations <strong>in</strong> lake<strong>sediment</strong>s as compared to natural background levels. In this respect, the metal concentrationpr<strong>of</strong>ile <strong>in</strong> <strong>sediment</strong>s can be followed <strong>and</strong> besides active <strong>and</strong> passive contam<strong>in</strong>ation studies,renaturation programs <strong>of</strong> the water bodies can be configured.In the follow<strong>in</strong>g, a time efficient direct solid sampl<strong>in</strong>g technique for complex metallic matrices ispresented <strong>and</strong> the advantages <strong>of</strong> the simplified l<strong>in</strong>e selection <strong>in</strong> the absorption spectrum arehighlighted.ExperimentalSample preparationThe samples were analyzed directly without any further preparation.<strong>Determ<strong>in</strong>ation</strong>The measurements were performed with the High-Resolution Cont<strong>in</strong>uum Source AAS contrAA ®<strong>and</strong> the completely automatic solid autosampler <strong>SS</strong>A 600.Method parametersElement Wavelength T Pyr. T Atom. RampTypicalweightModifier[nm] [°C] [°C] [°C/s] [mg]<strong>Cd</strong> 228.8018 650 2000 1200 0.2 - 0.4 none<strong>Pb</strong> 368.3462 850 2450 1400 0.2 - 0.4 5 µL 0.1 % Pd(NO 3 ) 2Evaluation parametersElementEval. Measurement No. <strong>of</strong>BackgroundSpectral rangepixel timespectracorrection[s] [pixel] [nm]<strong>Cd</strong> 3 3 90 200 0.25 dynamic,with reference<strong>Pb</strong> 3 3 90 200 0.40 dynamic,with referenceApplication Report: AR_environment_e_0109 2/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de
Calibration<strong>Cd</strong><strong>Pb</strong>Solid calibration with reference material ME<strong>SS</strong>-2 (certif. conc.: 0.24 ± 0.01 mg/kg)Us<strong>in</strong>g different weights <strong>of</strong> ME<strong>SS</strong>-2 between 0.1 <strong>and</strong> 1.2 mgSt<strong>and</strong>ards: 1 replicate per statistic; <strong>in</strong>tegration mode: areaSamples: 5 replicates per statistic; <strong>in</strong>tegration mode: areaSolid calibration with reference material GBW 0831 (certif. conc.: 79 ± 12 mg/kg)Us<strong>in</strong>g different weights <strong>of</strong> GBW 0831 between 0.1 <strong>and</strong> 0.6 mgSt<strong>and</strong>ards: 1 replicate per statistic, <strong>in</strong>tegration mode: areaSamples: 5 replicates per statistic, <strong>in</strong>tegration mode: areaCalibration curvesElementnonl<strong>in</strong>ear<strong>Cd</strong> 228.8018 nmR² = 0.998Element<strong>Pb</strong> 368.3462 nmnonl<strong>in</strong>earR² = 0.997Application Report: AR_environment_e_0109 3/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de
Signal pr<strong>of</strong>ile <strong>and</strong> spectral vic<strong>in</strong>ityElementSignalpr<strong>of</strong>ile<strong>Cd</strong> 228.8018 nmCal. std. 4 (69.84 pg <strong>Cd</strong>)Sample: <strong>sediment</strong>Spectralvic<strong>in</strong>ityRed: background signalBlue: analyte signal3DspectrumCal. std. 4 (69.84 pg <strong>Cd</strong>)Sample: <strong>sediment</strong>Application Report: AR_environment_e_0109 4/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de
ElementSignalpr<strong>of</strong>ile<strong>Pb</strong> 283.3060 nmCal. std. 1 (22750 pg <strong>Pb</strong>)Sample: <strong>sediment</strong>Spectralvic<strong>in</strong>ityRed: background signalBlue: analyte signal3DspectrumCal. std. 1 (22750 pg <strong>Pb</strong>)Sample: <strong>sediment</strong>Application Report: AR_environment_e_0109 5/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de
Results <strong>and</strong> DiscussionThe spectral vic<strong>in</strong>ity <strong>of</strong> <strong>Cd</strong> <strong>and</strong> <strong>Pb</strong> show additional Fe l<strong>in</strong>es at 228.7262 nm <strong>and</strong> 368.304 nm. Dueto the high resolution <strong>of</strong> the spectrometer those signals could be separated from the analyte signal.High concentrations <strong>of</strong> <strong>Pb</strong> could be measured on an <strong>in</strong>sensitive absorption l<strong>in</strong>e.By measur<strong>in</strong>g <strong>of</strong> reference materials recovery rates <strong>of</strong> about 92 <strong>and</strong> 95 % could be reached,pro<strong>of</strong><strong>in</strong>g the analytical performance <strong>of</strong> the method employed.Element Sample Concentration[mg/kg]RSD[%]Recovery rate[%]<strong>Cd</strong>Sediment 0.26 ± 0.06 7.6 -CRM 280 (*) 1.48 ± 0.11 8.2 92.5<strong>Pb</strong>Sediment 47.1 ± 2.5 6.5 -CRM 277 (**) 139 ± 4 4.3 95.2(*) Reference material, certif. concentration <strong>of</strong> <strong>Cd</strong>: 1.6 ± 0.1 mg/kg(**) Reference material, certif. concentration <strong>of</strong> <strong>Pb</strong>: 146 ± 3 mg/kgConclusionAll absorption l<strong>in</strong>es <strong>of</strong> an element <strong>in</strong> the spectral range <strong>of</strong> 185–900 nm can be analyticallyevaluated by us<strong>in</strong>g a Xe short-arc lamp as a cont<strong>in</strong>uum lamp <strong>in</strong> the <strong>HR</strong>-<strong>CS</strong> AAS. The spectralbackground <strong>of</strong> the samples <strong>in</strong> the <strong>HR</strong>-<strong>CS</strong> AAS is always corrected directly on the analysis l<strong>in</strong>e,simultaneously <strong>and</strong> <strong>in</strong>dependently <strong>of</strong> the wavelength used, thus simplify<strong>in</strong>g the development <strong>of</strong> themethod <strong>and</strong> selection <strong>of</strong> l<strong>in</strong>es.By us<strong>in</strong>g direct solid sampl<strong>in</strong>g technique samples can be measured without time-consum<strong>in</strong>gpreparation. Thus, total analysis time <strong>and</strong> blank problems caused by chemicals used for samplepreparation are reduced the to a m<strong>in</strong>imum. Due to the availability <strong>of</strong> certified reference materials,same or similar calibration st<strong>and</strong>ards to the sample matrix could be applied.Application Report: AR_environment_e_0109 6/ 6Analytik Jena AG | Konrad-Zuse-Str. 1 | 07745 Jena/ Germany | www.analytik-jena.com | <strong>in</strong>fo@analytik-jena.de