Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil

Chemistry Central Journal

Tiberiu Frentiu¹  Michaela Ponta¹  Raluca Hategan² 

[1] Faculty of Chemistry and Chemical Engineering, Babes-Bolyai University, 11 Arany Janos, 400028 Cluj-Napoca, Romania

[2] Regional Environmental Protection Agency, 99 Dorobantilor, 400609 Cluj-Napoca, Romania

关键词: Hazardous/priority hazardous metal;    Soil analysis;    Bland and Altman statistical method;    Inductively coupled plasma optical emission spectrometry;    High-resolution continuum source flame atomic absorption spectrometry;   

Others  :  787949
DOI  :  10.1186/1752-153X-7-43

 received in 2013-01-14, accepted in 2013-02-11,  发布年份 2013

【 摘 要 】

Background

The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil.

Results

The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94–106% in atomic absorption and 97–103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6–5.2% in atomic absorption, similar with that of 1.9–6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric methods for 95% confidence interval.

Conclusions

High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry.

【 授权许可】

   
2013 Frentiu et al.; licensee Chemistry Central Ltd.

【 图 表 】

Figure 1.

【 参考文献 】

• [1]Florek S, Becker-Ross H: High-resolution spectrometer for atomic spectrometry. J Anal At Spectrom 1995, 10:145-147.
• [2]Becker-Ross H, Florek S, Heitmann U, Weisse R: Influence of the spectral bandwidth of the spectrometer on the sensitivity using continuum source AAS. Fresen J Anal Chem 1996, 355:300-303.
• [3]Heitmann U, Schutz M, Becker-Ross H, Florek S: Measurements of the Zeeman-splitting of analytical lines by means of a continuum source graphite furnace atomic absorption spectrometer with linear charge coupled device array. Spectrochim Acta Part B 1996, 51B:1095-1105.
• [4]Welz B, Becker-Ross H, Florek S, Heitmann U: High-Resolution Continuum, Source AAS - the better way to do atomic absorption spectrometry. Weinheim, Germany: Wiley-VCH; 2005.
• [5]L’vov BV: A continuum source vs. line source on the way toward absolute graphite furnace atomic absorption spectrometry. Spectrochim Acta Part B 1999, 54B:1637-1646.
• [6]Welz B, Becker-Ross H, Florek S, Heitmann U, Vale MGR: High-resolution continuum-source atomic absorption spectrometry – What can we expect? J Braz Chem Soc 2003, 14:220-229.
• [7]Becker-Ross H, Florek S, Heitmann U, Huang MD, Okruss M, Radziuk B: Continuum source atomic absorption spectrometry and detector technology: a historical perspective. Spectrochim Acta Part B 2006, 61B:1015-1030.
• [8]Welz B, Borges DLG, Lepri FG, Vale MGR, Heitmann U: High-resolution continuum source electrothermal atomic absorption spectrometry – an analytical and diagnostic tool for trace analysis. Spectrochim Acta PartB 2007, 62B:873-883.
• [9]Welz B, Mores S, Carasek E, Vale MGR, Okruss M, Becker-Ross H: High-resolution continuum source atomic and molecular absorption spectrometry – a review. Appl Spectrosc Rev 2010, 45:327-354.
• [10]Taylor A, Branch S, Day MP, Patriarca M, White M: Atomic spectrometry update. Clinical and biological materials, foods and beverages. J Anal At Spectrom 2011, 26:653-692.
• [11]Resano M, Garcia-Ruiz E: High-resolution continuum source graphite furnace atomic absorption spectrometry: Is it as it sounds? A critical review. Anal Bioanal Chem 2011, 399:323-330.
• [12]Ren T, Zhao LJ, Cao J, Zhong RG: Determination of Pb, Cd and Cr in food by high resolution continuum source graphite furnace atomic absorption spectrometry. Spectrosc Spectr Anal 2012, 32:2566-2571.
• [13]Ren T, Zhao LJ, Zhong RG: Determination of aluminum in wheat flour food by microwave digestion-high resolution continuum source graphite furnace atomic absorption spectrometry. Spectrosc Spectr Anal 2011, 31:3388-3391.
• [14]Nunes AM, Acunha TS, Oreste EQ, Lepri FG, Vieira MA, Curtius AJ, Ribeiro AS: Determination of Ca, Cu, Fe and Mg in fresh and processed meat treated with tetramethylammonium hydroxide by atomic absorption spectrometry. J Braz Chem Soc 2011, 22:1850-1857.
• [15]Atilgan S, Akman S, Baysal A, Bakircioglu Y, Szigeti T, Ovari M, Zaray G: Monitoring of Pd in airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. Spectrochim Acta PartB 2012, 70B:33-38.
• [16]Castilho INB, Welz B, Vale MGR, de Andrade JB, Smichowski P, Shaltout AA, Colares L, Carasek E: Comparison of three different sample preparation procedures for the determination of traffic-related elements in airborne particulate matter collected on glass fiber filters. Talanta 2011, 88:689-695.
• [17]Araujo RGO, Rennan GO, Vignola F, Castilho INB, Borges DLG, Welz B, Vale MGR, Smichowski P, Ferreira SLC, Becker-Ross H: Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. Spectrochim Acta Part B 2011, 66B:378-382.
• [18]Araujo RGO, Welz B, Castilho INB, Vale MGR, Smichowski P, Ferreira SLC, Becker-Ross H: Determination of antimony in airborne particulate matter collected on filters using direct solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry. J Anal At Spectrom 2010, 25:580-584.
• [19]dos Santos LMG, Welz B, Araujo RGO, Jacob SDC, Vale MGR, Martens A, Martens IBG, Becker-Ross H: Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. J Agric Food Chem 2009, 57:10089-10094.
• [20]dos Santos LMG, Araujo RGO, Welz B, Jacob SDC, Vale MGR, Becker-Ross H: Simultaneous determination of Cd and Fe in grain products using direct solid sampling and high-resolution continuum source graphite furnace atomic absorption spectrometry. Talanta 2008, 78:577-583.
• [21]Resano M, Briceno J, Belarra MA: Direct determination of phosphorus in biological samples using a solid sampling-high resolution-continuum source electrothermal spectrometer: comparison of atomic and molecular absorption spectrometry. J Anal At Spectrom 2009, 24:1343-1354.
• [22]Borges AR, Becker EM, Lequeux C, Vale MGR, Ferreira SLC, Welz B: Method development for the determination of cadmium in fertilizer samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and slurry sampling. Spectrochim Acta Part B 2011, 66B:529-535.
• [23]Freire AS, Santelli RE: Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100 (R) resin. Spectrochim Acta Part B 2012, 71-72B:92-97.
• [24]Quadros DPC, Chaves ES, Lepri FG, Borges DLG, Welz B, Becker-Ross H, Curtius AJ: Evaluation of Brazilian and Venezuelan crude oil samples by means of the simultaneous determination of Ni and V as their total and non-volatile fractions using high-resolution continuum source graphite furnace atomic absorption spectrometry. Energy Fuel 2010, 24:5907-5911.
• [25]Dittert IM, Silva JSA, Araujo RGO, Curtius AJ, Welz B, Becker-Ross H: Simultaneous determination of cobalt and vanadium in undiluted crude oil using high-resolution continuum source graphite furnace atomic absorption spectrometry. J Anal At Spectrom 2010, 25:590-595.
• [26]Dittert IM, Silva JSA, Araujo RGO, Curtius AJ, Welz B, Becker-Ross H: Direct and simultaneous determination of Cr and Fe in crude oil using high-resolution continuum source graphite furnace atomic absorption spectrometry. Spectrochim Acta Part B 2009, 64B:537-543.
• [27]de Campos RC, Correia CLT, Vieira F, Saint Pierre TD, Oliveira AC, Goncalves R: Direct determination of P in biodiesel by high-resolution continuum source graphite furnace absorption spectrometry. Spectrochim Acta Part B 2011, 66B:352-355.
• [28]Aramendia M, Florez MR, Piette M, Vanhaecke F, Resano M: Al determination in whole blood samples as AlF via high-resolution continuum source graphite furnace molecular absorption spectrometry: potential application to forensic diagnosis of drowning. J Anal At Spectrom 2011, 26:1964-1973.
• [29]Nunes LS, Barbosa JTP, Fernandez AP, Lemos VA, dos Santos WNL, Korn MGA, Teixeira LSG: Multi-element determination of Cu, Fe, Ni and Zn content in vegetable oils samples by high-resolution continuum source atomic absorption spectrometry and microemulsion sample preparation. Food Chem 2011, 127:780-783.
• [30]de Oliveira SR, Raposo JL, Neto JAG: Fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn for foliar diagnosis using high-resolution continuum source flame atomic absorption spectrometry: feasibility of secondary lines, side pixel registration and least-squares background correction. Spectrochim Acta Part B 2009, 64B:593-596.
• [31]Oliveira SR, Neto JAG, Nobrega JA, Jones BT: Determination of macro- and micronutrients in plant leaves by high-resolution continuum source flame atomic absorption spectrometry combining instrumental and sample preparation strategies. Spectrochim Acta Part B 2010, 65B:316-320.
• [32]Brandao GC, Matos GD, Ferreira SLC: Slurry sampling and high-resolution continuum source flame atomic absorption spectrometry using secondary lines for the determination of Ca and Mg in dairy products. Microchem J 2011, 98:231-233.
• [33]Dessuy MB, de Jesus RM, Brandao GC, Ferreira SLC, Vale MGR, Welz B: Fast sequential determination of antimony and lead in pewter alloys using high resolution-continuum source flame atomic absorption spectrometry. Food Addit Contam Part A-Chem 2013, 30:202-207.
• [34]Raposo JL, Oliveira SR, Neto JAG, Nobrega JA, Jones BT: Determination of silicon in lubrication oil by high-resolution continuum source flame atomic absorption spectrometry using least-square background correction and internal standardization. Anal Lett 2011, 44:2150-2161.
• [35]Amorim VR, Neto JAG: Evaluation of lubricating oil preparation procedures for the determination of Al, Ba, Mo, Si and V by high-resolution continuum source FAAS. Anal Sci 2009, 25:95-100.
• [36]Resta V, Filho A, Gomes JA: Different lubricating oil treatments for the determination of Cu, Cr, Fe, Ni, Sb, Pb and Zn by HR-CS FAAS. Anal Lett 2008, 41:1555-1570.
• [37]Raposo JL, de Oliveira SR, Caldas NM, Neto JAG: Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry. Anal Chim Acta 2008, 627:198-202.
• [38]Huang MD, Becker-Ross H, Florek S, Heitmann U, Okruss M: Determination of phosphorus by molecular absorption of phophorus monoxide using a high-resolution continuum source absorption spectrometer and an air-acetylene flame. J Anal At Spectrom 2006, 21:338-345.
• [39]Ferreira RB, Oliveira SR, Franzini VP, Virgilio A, Raposo JL, Neto JAG: Evaluation of lines of phosphorus and potassium by high-resolution continuum source flame atomic absorption spectrometry for liquid fertilizer analysis. At Spectrosc 2011, 32:56-61.
• [40]Welz B, Lepri FG, Araujo RGO, Ferreira SLC, Huang MD, Okruss M, Becker-Ross H: Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces - a review. Anal Chim Acta 2009, 647:137-148.
• [41]Resano M, Florez MR: Direct determination of sulfur in solid samples by means of high-resolution continuum source graphite furnace molecular absorption spectrometry using palladium nanoparticles as chemical modifier. J Anal At Spectrom 2012, 27:401-412.
• [42]Virgilio A, Raposo JL, Cardoso AA, Nobrega JA, Neto JAG: Determination of total sulfur in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry. J Agric Food Chem 2011, 59:2197-2201.
• [43]Huang MD, Becker-Ross H, Florek S, Heitmann U, Okruss M: Direct determination of total sulfur in wine using a continuum-source atomic-absorption spectrometer and an air-acetylene flame. Anal Bioanal Chem 2005, 382:1877-1881.
• [44]Baumbach G, Limburg T, Einax JW: Quantitative determination of sulfur by high-resolution graphite furnace molecular absorption spectrometry. Microchem J 2013, 106:295-299.
• [45]Bucker S, Acker J: Spectrometric analysis of process etching solutions of the photovoltaic industry – Determination of HNO3, HF, and H2SiO6 using high-resolution continuum source absorption spectrometry of diatomic molecules and atoms. Talanta 2012, 94:335-341.
• [46]Ozbek N, Akman S: Method development for the determination of fluorine in toothpaste via molecular absorption of aluminum mono fluoride using a high-resolution continuum source nitrous oxide/acetylene flame atomic absorption spectrophotometer. Talanta 2012, 94:246-250.
• [47]Ozbek N, Akman S: Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer. Spectrochim Acta Part B 2012, 69B:32-37.
• [48]Huang MD, Becker-Ross H, Florek S, Heitmann U, Okruss M: High-resolution contuinuum electrothermal absorption spectrometry of AlBr and CaBr for the determination of bromine. Spectrochim Acta Part B 2008, 63B:566-570.
• [49]Brandao GC, Lima DC, Ferreira SLC: The chemical generation of NO for the determination of nitrite by high-resolution continuum source molecular absorption spectrometry. Talanta 2012, 98:231-235.
• [50]Massart DL, Vandeginste BGM, Buydens IMC: Handbook of Chemometrics and Qualimetrics, Part A. Amsterdam: Elsevier; 1997.
• [51]Gunzler H: Accreditation and Quality Assurance in Analytical Chemistry. Berlin: Springer Verlag; 1994.
• [52]ISO 22036: Soil quality. Determination of trace elements in extracts of soil by inductively coupled plasma-atomic emission spectrometry (ICP-AES). 2008.
• [53]ISO 11047: Soil quality - Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc - Flame and electrothermal atomic absorption spectrometric methods. 1999.
• [54]Kaiser H: Die berechnung der nachweisempfindlichkeit. Spectrochim Acta 1947, 3:40-47.
• [55]Currie LA: Nomenclature in evaluation of analytical methods including detection and quantification capabilities. Pure Appl Chem 1995, 67:1699-1723.
• [56]Bland JM, Altman GD: Statistical methods for assessing agreement between two methods of clinical measurement. Lancet 1986, i:307-310.
• [57]Bland JM, Altman GD: Measuring agreement in method comparison studies. Stat Methods Med Res 1999, 8:135-160.
• [58]Lyon TDB, Fell GS, McKey K, Scott RD: Accuracy of multi-element analysis of human tissue obtained at autopsy using inductively coupled plasma mass spectrometry. J Anal At Spectrom 1991, 6:559-564.
• [59]Cheng ASH, Robson MD, Neubauer S, Selvanayagam J: Irreversible myocardial injury: Assessment with cardiovascular delayed-enhancement MR imaging and comparison of 1.5 and 3.0 T-Initial experience. Radiology 2007, 242:735-742.
• [60]Frentiu T, Ponta M, Anghel SD, Simon A, Marginean I, Cordos E: Statistical evaluation of Cu, Mn and Zn determinations in biological samples by radiofrequency capacitively coupled plasma atomic emission spectrometry using the Bland and Altman test. Microchim Acta 2003, 143:245-254.
• [61]Frentiu T, Ponta M, Levei E, Gheorghiu E, Kasler I, Cordos EA: Validation of the Tessier scheme for speciation of metals in soil using the Bland and Altman test. Chem Pap 2008, 62:114-122.
• [62]Frentiu T, Ponta M, Levei E, Senila M, Ursu M, Cordos E: Interlaboratory study on Cu, Pb and Zn determination in soil by inductively coupled plasma optical emission spectrometry using the Bland and Altman test. J Optoelectron Adv Mater 2007, 9:3505-3515.