Andrea Balla Kovács

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.

Renin overexpression leads to increased titin-based stiffness contributing to diastolic dysfunction in hypertensive mRen2 rats.

Hypertension (HTN) is a major risk factor for heart failure. We investigated the influence of HTN on cardiac contraction and relaxation in transgenic renin overexpressing rats (carrying mouse Ren-2 renin gene, mRen2, n = 6). Blood pressure (BP) was measured. Cardiac contractility was characterized by echocardiography, cellular force measurements, and biochemical assays were applied to reveal molecular mechanisms. Sprague-Dawley (SD) rats (n = 6) were used as controls. Transgenic rats had higher circulating renin activity and lower cardiac angiotensin-converting enzyme two levels. Systolic BP was elevated in mRen2 rats (235.11 ± 5.32 vs. 127.03 ± 7.56 mmHg in SD, P < 0.05), resulting in increased left ventricular (LV) weight/body weight ratio (4.05 ± 0.09 vs. 2.77 ± 0.08 mg/g in SD, P < 0.05). Transgenic renin expression had no effect on the systolic parameters, such as LV ejection fraction, cardiomyocyte Ca(2+)-activated force, and Ca(2+) sensitivity of force production. In contrast, diastolic dysfunction was observed in mRen2 compared with SD rats: early and late LV diastolic filling ratio (E/A) was lower (1.14 ± 0.04 vs. 1.87 ± 0.08, P < 0.05), LV isovolumetric relaxation time was longer (43.85 ± 0.89 vs. 28.55 ± 1.33 ms, P < 0.05), cardiomyocyte passive tension was higher (1.74 ± 0.06 vs. 1.28 ± 0.18 kN/m(2), P < 0.05), and lung weight/body weight ratio was increased (6.47 ± 0.24 vs. 5.78 ± 0.19 mg/g, P < 0.05), as was left atrial weight/body weight ratio (0.21 ± 0.03 vs. 0.14 ± 0.03 mg/g, P < 0.05). Hyperphosphorylation of titin at Ser-12742 within the PEVK domain and a twofold overexpression of protein kinase C-α in mRen2 rats were detected. Our data suggest a link between the activation of renin-angiotensin-aldosterone system and increased titin-based stiffness through phosphorylation of titins PEVK element, contributing to diastolic dysfunction.

Macro- and microelement contents of blue and red kernel corns

The role of special corns in human diets is increasing as a result of their favourable nutritional values. Little is known about mineral contents of different red and blue corns, although they may help to inhibit deficiency diseases mainly in the developing countries. During this study, mineral contents (15 elements) of 3 red and 9 blue corn varieties were examined with ICP-OES and ICP-MS. Highest contents of macroelements were as follows: P (3859.5±562.1 mg kg −1 ), K (4325.0±469.5 mg kg −1 ) and Mg (1450.0±104.6 mg kg −1 ) in the variety Black Mexican, S (1555.0±128.6 mg kg −1 ) in Santo Domingo Blue. In case of microelements, iron, zinc and selenium were highlighted. Except one genotype, iron contents were above 30 mg kg −1 . Blaumais, Hopi Turquoise and Hopi Blue contained more than 40 mg kg −1 (41.0–46.3), which were above values published in the literature (10.0 mg kg −1 in average). For zinc, we measured 15.2–31.5 mg kg −1 . Selenium contents (0.1–0.2 mg kg −1 ) were also higher than in the literat...

Effect of Application of Nitrogen and Different Nitrogen–Sulfur Ratios on the Quality and Quantity of Mustard Seed

A greenhouse experiment was conducted on a calcareous chernozem soil to investigate the effects of nitrogen (N) and sulfur (S) fertilization and their ratios on the yield and quality of white mustard (Sinapis alba L.). Four levels of N [0.5, 1, 1.5, and 2 g pot−1 N as ammonium nitrate (NH4NO3) and ammonium phosphate (NH4H2PO4)] in combination with three levels of applied N–S ratios [8, 4, 2; S as potassium sulfate (K2SO4) and sodium sulphate (Na2SO4)] were tested as treatments. Results indicated that a significant response to seed yield was observed for N and S application. Maximum yield, 24.8 g pot−1, was found when full doses of N and S were applied. Increasing N supply from 0.5 g pot−1 to 1 g pot−1 had little increasing effect in the oil content of the seed. Higher application of N doses (>1 g pot−1) decreased these values significantly. The maximum oil content (28%) was achieved with the 1 g N pot−1 treatment; the lowest values were observed in the pots applied with the highest N doses. Changes in the N content of the seed and straw showed a statistically significant increase with increasing N and S fertilization. Highest values in the seed and straw (5.96% and 0.87%, respectively) were observed by applying highest N and S doses. Seed and straw S levels were also observed to increase with increasing N rates and decreasing N–S ratio. Nitrogen doses significantly improved the quantities of essential amino acids with the exception of threonine, tyrosine, phenylalanine, and methionine. The amounts of these amino acids decreased with increasing N supply. When the N–S ratio decreased by increasing S, the quantities of valine, isoleucine, leucine, lysine, methionine, and cysteine increased significantly and the amount of tyrosine decreased. The quantities of nonessential amino acids with the exception of proline, histidine, and glycine increased with increasing N doses. In contrast, N rates decreased the amount of glycine. Decreasing the N–S ratio lowered the proline and arginine contents. The total amounts of essential amino acids slightly increased with increasing N rates and decreasing N–S ratio.

Effects of boron, calcium and magnesium foliar fertilization on apple (Malus domestica) yields

Boron is one of the most important micronutrients for plants (Borchmann, 1975). Its peculiarity is that (differently from most of the microelements, but similarly to molybdenum) it can be found in the soil and in the plant as an anion (Bergmann and Neubert, 1976). Among the microelements, boron has the greatest effect on the yield quality and quantity of plants (Mengel, 1984). If it is not available in the necessary amount and form, then problems can be detected in flower formation and fertilization, furthermore, carbohydrate and lipid formation is also inhibited. As a secondary consequence, the strength of cell walls also decreases (Mirko, 1978) which increases the susceptibility of the plant to diseases (mainly to those caused by microorganisms).

The effect of N and N/S supply levels on oil and protein content in mustard seed ( Sinapis alba L. )

Introduction Yellow mustard (Sinapis alba L.) is a annual spring crop and has been grown mainly in Europe since last century. Yellow mustard seed is suitable for a wide range of applications. It is grown for its seed, as a salad plant, as a green fodder crop or as green manure. Mustard seed is a nutritious food ingredient. Climate of Hungary is favourable for the cultivation of mustard. In spite of that little information exists on its fertilization, on the mechanism of its nutrient-uptake and its fertilizer activity in the international (Ahmad et al. 1998, Asare et al. 1995) and hungarian (EOry et al. 1996, K&d&r 2002) scientific literature. In the present study, an attempt was made to increase the amount of information for the effects of N supply and N/S ratio on the sulphur, nitrogen (crude protein), oil content and yield of seed.

Determination of sulphur in plant extracts by ion chromatograph - Hydraulic high-pressure nebulizer - Inductively coupled plasma atomic emission spectrometer (IC/HHPN/ICP-AES)

The method for speciation and quantitative analysis of inorganic sulphur form, sulphate and organic sulphur compounds by using high performance ion chromatography (IC) with inductively coupled plasma atomic emission spectrophotometry (ICP-AES) has been developed. An ICP-AES was operated as a detector of IC. To achieve a lower detection limit a hydraulic high-pressure nebulizer was used for connection between IC and ICP. This hyphenated system was used for the separation and determination of organic sulphur compounds and sulphate ions. By using an anion exchange column, with 2.5 mM phthalic acid, adjusted with TRIS to pH=4.2, all of the organic sulphur forms were measured together as a first (pseudo) peak (Nieto and Frankenberger, 1985) at 2.0 min., while the sulphate ion was retained on the column and its peak appeared with retention time at 4.2 min. Other inorganic sulphur forms (sulphide, sulphite, thiosulphate etc.) were not detectable in the water extracts from the examined plants. The sulphide and sulphite peaks were observed between the organic sulphur and sulphate peaks, but the developed method was not optimised for their separation. The sulphur was detected on the polychromator of ICP-AES on 180.734 nm. The detection limits were 0.023 mg L -1 and 0.085 mg L -1 of sulphate-sulphur and of organic-sulphur respectively. Water extracts of standard wheat straw and grain samples were analysed.Abstract The method for speciation and quantitative analysis of inorganic sulphur form, sulphate and organic sulphur compounds by using high performance ion chromatography (IC) with inductively coupled plasma atomic emission spectrophotometry (ICP‐AES) has been developed. An ICP‐AES was operated as a detector of IC. To achieve a lower detection limit a hydraulic high‐pressure nebulizer was used for connection between IC and ICP. This hyphenated system was used for the separation and determination of organic sulphur compounds and sulphate ions. By using an anion exchange column, with 2.5 mM phthalic acid, adjusted with TRIS to pH=4.2, all of the organic sulphur forms were measured together as a first (pseudo) peak (Nieto and Frankenberger, 1985) at 2.0 min., while the sulphate ion was retained on the column and its peak appeared with retention time at 4.2 min. Other inorganic sulphur forms (sulphide, sulphite, thiosulphate etc.) were not detectable in the water extracts from the examined plants. The sulphide and sulphite peaks were observed between the organic sulphur and sulphate peaks, but the developed method was not optimised for their separation. The sulphur was detected on the polychromator of ICP‐AES on 180.734 nm. The detection limits were 0.023 mg L‐1 and 0.085 mg L‐1 of sulphate‐sulphur and of organic‐sulphur respectively. Water extracts of standard wheat straw and grain samples were analysed.

Analytical methods and quality assurance: 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.

Long-Term Effect of High Phosphorus Doses on Zinc Status of Maize on a Non-Calcareous Loamy Soil

The long-term effect of 87.3 kg/ha P on the yield elements and nutrient content of maize was studied at the Na tional Long-Term Fertilization Experiment of the Karcag Research Institute in Hungary. The soil of the experiment site is non-calcareous Luvic Phaeosem, and its soluble phosphorus (P) and zinc (Zn) content in 0–20 cm soil layer are: ammonium lactate P: 141.1 mg/kg and diethylene triamine pentaacetic acid (DTPA) Zn: 0.85 mg/kg, respectively. The effect of foliar Zn fertilization was studied at three levels of nitrogen (150, 200 and 250 kg/ha) and under 87.3 kg/ha P and 82.6 kg/ha K application in four replications. The applied Zn amount was 700 g/ha. We measured the grain yield and the thousand-kernel weight. Leaf and grain samples were analyzed for phosphorus, zinc, potassium, calcium, magnesium and manganese content. Foliar Zn application did not increase the yield significantly, but it enhanced the thousand-kernel weight. The element content did not change significantly – neither in leaves nor in kernels. Under the examined habitat circumstances even the long-term application of 87.3 kg/ha P dosage did not cause Zn deficiency to such an extent which would lead to significant yield depression of maize.