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
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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
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