Zoltán Gyori

A study of plant sample preparation and inductively coupled plasma emission spectrometry parameters

Abstract Adjustable parameters of an inductively coupled plasma emission spectrometer (ICP) are investigated and a digestion method of plant samples is developed which does not require the use of HC104. This HNO3‐H2O2 wet digestion method eliminates the hazards associated with hot, concentrated HClO4. The adjustable parameters of ICP are viewing height, forward power as well as the sample, coolant, auxiliary, and flushing gas flow rates, and the sample uptake flow rate. The digestion parameters examined are the type and amount of the applied acids (HNO3, HCl, and H2SO4), the temperature and duration of predigestion, the amount of H2O2, and the temperature and duration of digestion. Three plant samples (maize seed, wheat straw, and sunflower seed) and three dry weights are analyzed. The optimal parameters of the ICP spectrometer and HNO3‐H2O2 wet digestion for plants are determined. Optimal parameters of HNO3‐H2O2 wet digestion sample preparation: Optimal parameters of the ICP instrument:

Studies on soil sample preparation for inductively coupled plasma atomic emission spectrometry analysis

Abstract A wet digestion method of soil samples has been developed for analysis of “total” concentration (acid extraction) of elements by inductively coupled plasma emission spectrometry (ICP‐AES). This HNO3‐H2O2 wet digestion method is a simple, fast and safe sample preparation method with satisfactory accuracy and precision. The first examined condition was the applied digestion acid or acid mixture (HNO3, HNO3‐H2O2, HCl‐H2O2, HNO3‐HClO4, H2SO4‐H2O2), and the volume of concentrated nitric acid (65% HNO3). Temperature and duration of predigestion, volume of concentrated hydrogen‐peroxide (30 % H2O2), temperature and duration of digestion were also investigated. Two different kind of soil samples (a sandy soil with low humus content, calcareous chernozem with relatively high humus content), three different dry weight values and three different values for each parameters were chosen to investigate soil sample digestion in order to select the best parameters. A LABOR MIM Electronic Block Digest Apparatus was applied for sample preparation and numerous elements (e.g. Al, As, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Sr, Zn) have been measured by a LABTAM 8440M Inductively Coupled Plasma Emission Spectrometer. The optimum values of parameters to digest soil sample in an electronic block digest apparatus are: a) 1 g dry weight, b) 5 cm3 HNO3 as digestion acid, c) 30°C‐60°C temperature range for 30–60 minutes predigestion, d) 5 cm3 30% H2O2, e) 120 C temperature for 270 minutes digestion. Two soil samples were digested with four methods (block digestion, Milestone microwave, Prolabo focused microwave and Hungarian standard). Results of the two microwaves and detailed block digestion methods are in well agreement in the two soil samples. Finally three Standard Reference Materials were applied to compare the appropriate results. These results showed well agreement for all elements except for aluminium and iron content. The difference between certified and measured results is dependent on their concentrations in soil.A wet digestion method of soil samples has been developed for analysis of total concentration (acid extraction) of elements by inductively coupled plasma emission spectrometry (ICP-AES). This HNO 3 -H 2 O 2 wet digestion method is a simple, fast and safe sample preparation method with satisfactory accuracy and precision. The first examined condition was the applied digestion acid or acid mixture (HNO 3 , HNO 3 -H 2 O 2 , HCl-H 2 O 2 , HNO 3 -HClO 4 , H 2 SO 4 -H 2 O 2 ), and the volume of concentrated nitric acid (65% HNO 3 ). Temperature and duration of predigestion, volume of concentrated hydrogen-peroxide (30 % H 2 O 2 ), temperature and duration of digestion were also investigated. Two different kind of soil samples (a sandy soil with low humus content, calcareous chernozem with relatively high humus content), three different dry weight values and three different values for each parameters were chosen to investigate soil sample digestion in order to select the best parameters. A LABOR MIM Electronic Block Digest Apparatus was applied for sample preparation and numerous elements (e.g. Al, As, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Sr, Zn) have been measured by a LABTAM 8440M Inductively Coupled Plasma Emission Spectrometer. The optimum values of parameters to digest soil sample in an electronic block digest apparatus are: a) 1 g dry weight, b) 5 cm 3 HNO 3 as digestion acid, c) 30°C-60°C temperature range for 30-60 minutes predigestion, d) 5 cm 3 30% H 2 O 2 , e) 120°C temperature for 270 minutes digestion. Two soil samples were digested with four methods (block digestion, Milestone microwave, Prolabo focused microwave and Hungarian standard). Results of the two microwaves and detailed block digestion methods are in well agreement in the two soil samples. Finally three Standard Reference Materials were applied to compare the appropriate results. These results showed well agreement for all elements except for aluminium and iron content. The difference between certified and measured results is dependent on their concentrations in soil.

Analytical methods and quality assurance

Abstract A wet digestion method of soil samples has been developed for analysis of “total” concentration (acid extraction) of elements by inductively coupled plasma emission spectrometry (ICP‐AES). This HNO3‐H2O2 wet digestion method is a simple, fast and safe sample preparation method with satisfactory accuracy and precision. The first examined condition was the applied digestion acid or acid mixture (HNO3, HNO3‐H2O2, HCl‐H2O2, HNO3‐HClO4, H2SO4‐H2O2), and the volume of concentrated nitric acid (65% HNO3). Temperature and duration of predigestion, volume of concentrated hydrogen‐peroxide (30 % H2O2), temperature and duration of digestion were also investigated. Two different kind of soil samples (a sandy soil with low humus content, calcareous chernozem with relatively high humus content), three different dry weight values and three different values for each parameters were chosen to investigate soil sample digestion in order to select the best parameters. A LABOR MIM Electronic Block Digest Apparatus was applied for sample preparation and numerous elements (e.g. Al, As, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Sr, Zn) have been measured by a LABTAM 8440M Inductively Coupled Plasma Emission Spectrometer. The optimum values of parameters to digest soil sample in an electronic block digest apparatus are: a) 1 g dry weight, b) 5 cm3 HNO3 as digestion acid, c) 30°C‐60°C temperature range for 30–60 minutes predigestion, d) 5 cm3 30% H2O2, e) 120 C temperature for 270 minutes digestion. Two soil samples were digested with four methods (block digestion, Milestone microwave, Prolabo focused microwave and Hungarian standard). Results of the two microwaves and detailed block digestion methods are in well agreement in the two soil samples. Finally three Standard Reference Materials were applied to compare the appropriate results. These results showed well agreement for all elements except for aluminium and iron content. The difference between certified and measured results is dependent on their concentrations in soil.A wet digestion method of soil samples has been developed for analysis of total concentration (acid extraction) of elements by inductively coupled plasma emission spectrometry (ICP-AES). This HNO 3 -H 2 O 2 wet digestion method is a simple, fast and safe sample preparation method with satisfactory accuracy and precision. The first examined condition was the applied digestion acid or acid mixture (HNO 3 , HNO 3 -H 2 O 2 , HCl-H 2 O 2 , HNO 3 -HClO 4 , H 2 SO 4 -H 2 O 2 ), and the volume of concentrated nitric acid (65% HNO 3 ). Temperature and duration of predigestion, volume of concentrated hydrogen-peroxide (30 % H 2 O 2 ), temperature and duration of digestion were also investigated. Two different kind of soil samples (a sandy soil with low humus content, calcareous chernozem with relatively high humus content), three different dry weight values and three different values for each parameters were chosen to investigate soil sample digestion in order to select the best parameters. A LABOR MIM Electronic Block Digest Apparatus was applied for sample preparation and numerous elements (e.g. Al, As, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Sr, Zn) have been measured by a LABTAM 8440M Inductively Coupled Plasma Emission Spectrometer. The optimum values of parameters to digest soil sample in an electronic block digest apparatus are: a) 1 g dry weight, b) 5 cm 3 HNO 3 as digestion acid, c) 30°C-60°C temperature range for 30-60 minutes predigestion, d) 5 cm 3 30% H 2 O 2 , e) 120°C temperature for 270 minutes digestion. Two soil samples were digested with four methods (block digestion, Milestone microwave, Prolabo focused microwave and Hungarian standard). Results of the two microwaves and detailed block digestion methods are in well agreement in the two soil samples. Finally three Standard Reference Materials were applied to compare the appropriate results. These results showed well agreement for all elements except for aluminium and iron content. The difference between certified and measured results is dependent on their concentrations in soil.

A study of the yield stability of winter wheat varieties

In our long-term experiment the analyses of stability were conducted in one shorter (years 2001–2003) and one longer (years 1994–2003) periods by using different numbers (2–6) of varieties in each one of the periods. The results of our research proved that the method, applied can be efficiently used to analyse the environmental responses, the behaviour under varying environmental conditions of different varieties. Varieties can adapt themselves differently to favourable and unfavourable environmental conditions. In general, varieties (e.g. older varieties, like Mv 15, Mv 20, and new varieties, like Lupus, Mv Emese) that give relatively good yields under unfavourable conditions (2–3 t ha −1 environmental average) will utilise improving environmental conditions (7–8 t ha −1 environmental average) to a lesser extent and vice versa. Varieties Mv 21, GK Othalom and Mv Palotas (a currently cultivated variety) made good use of intensive growing conditions. The data in this paper may assist in choosing varieties ...

Sulphur content of winter wheat grain in long term field experiments

Abstract Sulphur is an essential element for both plants and animals. Decreasing sulphur deposition from the air, and the use of more concentrated phosphate fertilizers that contain less sulphur, has led to reports of sulphur deficiencies for winter wheat. Sulphur deficiency significantly effects production and quality of winter wheat. Sulphur deficiency decreases grain size and baking quality because of formation of disulfide bonds formed from the sulphydryl groups of cysteine. This effects the viscoelasticity of dough. The purpose of this study was to evaluate the effect of NPK fertilization on sulphur concentration in winter wheat grain on different soil types. We analyzed wheat grain, grown at various locations where fertiliser had been applied for many years in places throughout Hungary, for sulphur content. These experiments were conducted using the identical varieties and fertiliser treatments at eight locations. At a separate location, additional varieties were also evaluated. The sulphur contents of the grains were determined by using ICP‐AES equipment. The sulphur contents of winter wheat varieties in Hungary averaged 1500 mg/kg and the difference between the varieties was as much as 120 mg/kg. The sulphur contents are influenced not only by sulphur fertilisers, but nitrogen fertilisers as well. Due to the strong N‐S relationships, fluctuations in protein contents also caused decreases/increases in the sulphur contents of the wheat grain. The N‐S relationship could be described by using a mathematical linear function. Annual applications of 100 kg/ha superphosphate, containing more than 10 kg sulphur, provide sufficient sulphur to produce a 5 t/ha grain yield. This study suggests that a 1500 mg/kg value for sulphur content in winter wheat grain is sufficient to maintain good yield and grain quality.

Heavy metal dispersion detected in soils and plants alongside roads in Hungary

ABSTRACTSoil and plant samples from roadside areas contaminated with toxic by-products of vehicular traffic (for example, lead compounds from leaded fuel, metal contaminants derived from spare parts) were analysed in the case of five Hungarian sampling sites. The analyses were carried out with a new analytical method which is based on the use of a high performance sample introduction unit in the conventional ICP spectrometry. By using this system, significantly lower detection limits were obtained related to the conventional ICP—AES method. The analysis results showed a close correlation between the daily mean volume of traffic and metals accumulated in the soil samples. On the other hand, using this method similar heavy metal profiles were gained, i.e. the total and plant-available heavy metal concentrations were the highest in the 0–1 m region from the road, and the further sampling points (0–90 m) showed significantly lower and lower heavy metal contents until at about 90 m distance from the road, wher...

Studies on parameters of inductively coupled plasma spectrometer

Abstract Analytical aspects of different adjustment of parameters of an inductively coupled plasma atomic emission spectrometer (ICP‐AES) were investigated. The ICP‐AES was a LABTAM 8440M (now called GBC) spectrometer. Since at many times, the elemental concentration of the analyte is near to the detection limit, the lowest possible detection limit has to be reached. When the signal‐to‐background ratio (SBR) is maximized, the detection limit is the smallest. This is the reason why the effects of each adjustable parameters on the signal‐to‐background ratios were investigated. Seven adjustable parameters can be analyzed in this equipment: (i) viewing height, (ii) forward power, (iii) sample gas, (iv) coolant gas, (v) auxiliary gas, (vi) flushing gas, and (vii) sample uptake flow rates. Furthermore aerosol distribution by droplet size and nebulization efficiency were also examined applying three different sample gas flow rates and four elements [iron (Fe), magnesium (Mg), manganese (Mn), and nickel (Ni)]. Th...

A simple and inexpensive method for chromium speciation in soil extracts

Abstract Chromium (Cr) appears in two stable forms in nature as Cr(III) and Cr(VI). Hexavalent chromium (CrO4 2‐; Cr2O7 2‐) is very toxic and carcinogenic, while inorganic Cr(III), however, is essential for mammals. Only two methods, atomic absorption and inductively coupled plasma atomic emission (ICP) spectrometry, provide information on the total amount of Cr in a test solution. This is the reason that several efforts have been made with regard to Cr speciation. Either an acidic or a basic activated aluminum oxide and a reversed phase C‐18 column or an ion exchanger column are used for the separation of chromium(III) from chromium(VI) in FIA and HPLC analyses. In our experiments, acidic‐activated aluminum oxide was used for separation. This alumina was placed into a silicon tube and connected to an ICP spectrometer between the nebulizer and peristaltic pump. The average grain size of the alumina was large enough that the solution could be pumped through the micro column. Acidic‐activated aluminum oxide...

Sampling Strategies for Testing and Evaluation of Soil Contamination in Riparian Systems at the Tisza River Basin, Hungary

During the year 2000, two significant pollution waves came from Romanian mines to Hungary and went along the Tisza River, causing serious damage to the ecosystem of the river. The first one, cyanide pollution, at the end of January had an instantaneous effect on the living system; the second, heavy‐metal pollution in March, resulted in a long‐term effect. The heavy‐metal pollution that arrived with floods had two results. On the one hand, increased water speed decreased the grade of sedimentation in the riverbed, and on the other hand, river flooding introduced contaminated water and sediment to the floodplain. After the withdrawal of the flood, a few centimeters of grey sediment remained in the floodplain. Subsequent floods in 2000 and 2001 resuspended and diluted the contaminated sediment on the floodplain. Heavy metals (primarily lead, zinc, cadmium) deposited on the floodplain may have a potential time bomb effect. The aim of this study was to investigate the copper, cadmium, zinc, and lead contamination and bio‐availability on the floodplain applying a novel sampling strategy.

Potential Dissipation of Atrazine in the Soil Unsaturated Zone: a Comparative Study in Four European Countries†

A European-wide project has been undertaken to establish the potential for dissipation of atrazine in the soil subsurface environment. Samples were obtained, avoiding contamination, in four countries (Belgium, Greece, Hungary and UK) and laboratory studies carried out. In order to make comparisons between results from each laboratory, a ring experiment was carried out using common methodology for sampling, extraction and analytical techniques. Subsurface materials from each country were distributed to the other countries. Atrazine dissipation was determined in each country for all materials under the same laboratory conditions. The results of this comparative study showed generally good agreement between all laboratories. Significant potential microbiological dissipation was detected in certain samples. Where differences occurred between laboratories this was attributed to small, spatially heterogeneous microbial populations in the subsurface materials.