Comparison of three wet digestion methods for the determination of plant sulphur by inductively coupled plasma atomic emission spectroscopy (ICP‐AES)

Abstract

Increased incidence of sulphur (S) deficiency in crops has led to a greater need for S determination in plant tissues. Among the methods available for measurement of S, inductively coupled plasma atomic emission spectrometry (ICP‐AES) has been proved to be accurate and rapid. This paper compares digestion with HNO₃‐HClO₄, fuming HNO₃‐KNO₃ and alkaline NaOBr prior to the S measurement by ICP‐AES. Both HNO₃‐HClO₄ and fuming HNO₃‐KNO₃ were found to give satisfactory results for five certified plant materials, with high accuracy and precision. The HNO₃‐HClO₄ method involved a rigid temperature control, with slow ramp rates and a final temperature (190°C) lower than the boiling point of HClO₄, to minimise the possibility of gaseous losses of S. Both methods can also be used for the simultaneous determination of phosphorus (P), calcium (Ca), magnesium (Mg), iron (Fe), zinc (Zn), copper (Cu), and manganese (Mn), and additionally potassium (K) with HNO₃‐HClO₄. In contrast, the alkaline NaOBr method was less suitable as a digestion procedure for S measurement by ICP‐AES, because it involved a large dilution factor and produced high blank values.     

Electrothermal atomic absorption spectroscopic determination of chromium in plant tissues

This method involves sample digestion in nitric, perchloric, and sulfuric acids. Chromium is concentrated by coprecipitation with ferric hydroxide. Redissolved iron is removed by liquid-liquid extraction, remaining silica is dissolved with hydrofluoric acid, and chromium is determined by electrothermal atomic absorption spectrometry. The sensitivity and detection limits for chromium approach those given by the manufacturers of the various instruments. Recovery studies and analysis of standard materials show that this method is reliable.     

Comparison of microwave digestion with conventional wet ashing and dry ashing digestion for analysis of lead, cadmium, chromium, copper, and zinc in shellfish by flame atomic absorption spectroscopy

A closed vessel microwave digestion procedure was developed for shellfish samples. This procedure was compared with wet and dry ash procedures for levels of lead, cadmium, chromium, copper, and zinc. Results obtained for microwave and conventional wet ash digestion were comparable. The dry ashing procedure produced results consistently lower than either of the other methods. Recoveries ranged from 80-92% for microwave and wet ashing procedures and 54-72% for the dry ashing procedure. Accuracy was also determined by analyzing lobster hepatopancreas marine reference material. Values for Pb, Cd, and Cr fell within the range specified for the reference material for all 3 digestion procedures; however, values were lower for Cu and Zn. Results of this study show that microwave digestion is comparable to wet ashing.     

Determination of trace elements in foods by HCl-HNO3 leaching and flame atomic absorption spectroscopy

Aluminum, iron, tin, zinc, calcium, magnesium, nickel, copper, chromium, cadmium, and potassium in foods can be extracted by HCl-HNO3 leaching and determined quantitatively using flame atomic absorption spectroscopy (AAS), with recoveries ranging from 90 to 110%. Thirty to 40 samples of almost any type of food sample can be analyzed routinely for 2 elements in 4-5 h. In contrast, one or 2 days are required when a wet-ash or dry-ash technique is used. Extraction consists of weighing 2-10 g samples into 125 mL Erlenmeyer flasks, adding 20 mL concentrated HCl-HNO3 (9 + 1), then heating in a 82- 93 degrees C water bath for 30 min. After cooling, samples are diluted to volume in 50 mL Nessler tubes and then filtered through No. 541 or 540 Whatman paper. The filtrate is analyzed directly by AAS.     

The determination of extractable plant available selenium from soils by electrothermal atomic absorption spectroscopy

Abstract

Plant available selenate was measured in a soil extract by electrothermal atomic absorption spectroscopy. Selenate in soil was first extracted with potassium sulfate then extracted into toluene fron an iodide‐sulfuric acid media. Aliquots of the toluene were injected into the graphite furnace for selenium determination. Quantities of extractable selenium measured using the electrothermal atomic absorption method compared favorably with the results of determinations using a fluorometric technique on aliquots of the soil extract. The simplicity of the procedure allowed for the precise determination of soil selenate in a brief period of time.     

Rapid digestion and flameless atomic absorption spectroscopy of mercury in fish: collaborative study

A collaborative study of the determination of mercury in fish has been completed in which wet oxidation of fish tissue in nitric acid, using vanadium as a catalyst, is compared with the AOAC official final action digestion technique, 25.103-25.105, involving a nitric-perchloric acid mixture. The study used tuna fish samples of known mercury content and included spike recovery studies in which methyl mercury solutions of known composition were provided to each laboratory. The study was designed to provide recovery information that bracketed the regulatory level of mercury in fish. The results indicate that the proposed digestion method is at least as precise and accurate as the AOAC method. The proposed method is also more rapid and less hazardous. It has been adopted as official first action.     

Enzymatic digestion-high-pressure homogenization prior to slurry introduction graphite furnace atomic absorption spectrometry for selenium determination in plant and animal tissues.

Homogenization using a new flat valve homogenizer in combination with enzymatic digestion with a crude protease was investigated as a means of releasing Se compounds from zoological and botanical matrixes prior to slurry introduction GFAAS. Timed trials with four zoological certified reference materials (CRMs), three botanical reference materials (RMs), and a food crop indicated that Se release into 5% (v/v) ethanol-0.03 M TRIS containing 20 mg of protease was quantitative after homogenization or became quantitative within 1 h of digestion at 60 degrees C. For each of the zoological RMs (whole egg powder, dogfish muscle, and dogfish liver), three passes through the homogenizer in the presence of protease provided a quantitative release of selenium, and incubation with the enzyme was not necessary. No separation of the Se between the liquid phase and the particulate phase was evident even after several days of subsequent storage at 4 degrees C. The botanical matrixes (three milled wheat RMs and a rapeseed sample) were more resistant to selenium release and required up to 1 h of digestion with protease at 60 degrees C. Alternatively, 10 passes through the homogenizing valve (in the presence of the enzyme) resulted in the quantitative release of analyte.     

不同前处理方法对秸秆金属元素原子吸收光谱分析结果的影响

秸秆中金属元素是关系农作物秸秆科学利用的重要组成部分,目前还没有统一的秸秆中金属元素原子吸收光谱(atomic absorption spectroscopy,AAS)测定方法标准,该研究采用原子吸收光谱测定黄芪(GBW10028)标准物质、玉米秸秆、小麦秸秆和棉花秸秆中金属元素含量,比较了不同前处理方法对样品中K、Cu、Fe、Zn和Mg分析结果的影响。结果表明:微波消解、干法灰化和湿法消解测定黄芪(GBW10028)标准物质中金属元素含量差异性显著(P<0.05),微波消解比干法灰化、湿法消解准确度高。微波消解对玉米秸秆、小麦秸秆和棉花秸秆中各金属元素的影响与黄芪(GBW10028)标准物质趋于一致。微波HNO3与微波HNO3-H2O2测定结果差异性不显著(P>0.05),微波HNO3比微波HNO3-H2O2和微波HNO3-H2SO4测定结果稳定。微波HNO3是进行秸秆样品金属元素含量测定时较准确简便的前处理方法。     

The analysis of pecan leaves by atomic absorption spectroscopy

Abstract

The analysis of plant tissue, generally leaves, is considered to be an important step in diagnosing and confirming a mineral element deficiency. The mineral element status of the plant can be accurately measured by the analysis of plant tissue if the tissue is properly sampled. Tissue analysis is often the best indication for recommending fertilizer or supporting nutrient spray treatments.

The development of a relatively fast and accurate method of analyzing plant tissue has been made possible with the advent of atomic absorption spectroscopic techniques.     

The determination of cadmium in soils,plants and fertilizers by dithizone extraction and atomic absorption spectroscopy

Abstract

Methods are proposed for the determination of cadmium in soils, plants and fertilizers.

Soil is first dissolved by treatment with hydrofluoric and hydrochloric acids and plant material is digested with nitric‐perchloric‐sulphuric acids. The cadmium is then extracted from the resulting solutions as the dithizone complex. After destruction of the dithizone the cadmium is dissolved in dilute hydrochloric acid and determined by atomic absorption spectroscopy. Cadmium in phosphatic fertilizers is determined directly by atomic absorption measurement on hydrochloric acid digests of the fertilizer.

The proposed methods have precision adequate for the study of cadmium in soil‐plant systems, the limits of detection being: plant material, 0.004 ppm Cd; soils, 0.02 ppm; and phosphatic fertilizers, 1 ppm.     

Simple determination of nitrate in soils by second-derivative spectroscopy

A new and simple method for nitrate analysis in soil extracts and soil solution is described. The method uses the second derivative of the direct ultra-violet (UV) spectrum, available from most microprocessor-controlled spectrophotometers with a UV source. Results with the proposed method were similar to those obtained by the cadmium-reduction column and ion-chromatographic methods. The main advantages of the proposed technique are that it is simple, rapid, accurate and requires no sample pre-treatment, making it useful for routine analysis of large numbers of samples.     

Digestion of fish samples for mercury determination by flameless atomic absorption spectrophotometry.

Methods of digestion of fish samples for mercury determination by flameless atomic absorption spectrophotometry have been investigated. Digestion in Teflon bombs, Kjeldahl flasks, or borosilicate test tubes gives comparable precisions and mercury recoveries. Because of their cost and effect in limiting productivity, Teflon bombs were considered unnecessary for analysis of fish samples. Experiments with cooked and uncooked fish samples have confirmed that no appreciable loss of mercury occurs during baking 30 min at 170 degrees C.     

Direct and combined methods for the determination of chromium, copper, and nickel in honey by electrothermal atomic absorption spectroscopy

In the present work, direct methods for the determination of chromium, copper, and nickel in honey by electrothermal atomic absorption spectroscopy were developed using experimental design as an optimization tool. Once the optimum conditions for the individual methods were established, a direct method for the combined determination of the three elements was optimized using the response surface tool. Palladium was used as chemical modifier in all cases. Honey was diluted in water, hydrogen peroxide, and nitric acid. Triton X-100 was added to minimize the matrix effect and the viscosity of the sample. The RSD (better than 10%) and the analytical recovery (98-103%) were acceptable for all of the developed methods. Calibration graphs were used in the four methods to determine the concentration of the analytes in the sample. The detection limits of the combined method (0.21, 0.35, and 0.37 microg L(-)(1) for Cr, Cu, and Ni, respectively) were similar to those obtained for the individual methods (LOD = 0.17, 0.21, 0.33 microg L(-)(1) for Cr, Cu, and Ni, respectively). The direct-combined proposed method has been applied to the determination of chromium, copper, and nickel content in representative honey samples from Galicia (northwestern Spain). The concentrations found in the analyzed samples were in the range of (5.75 +/- 0.64)-(26.4 +/- 0.38) ng g(-)(1) of Cr, (79 +/- 7.8)-(2049 +/- 80) ng g(-)(1) of Cu, and (12.6 +/- 1.36)-(172 +/- 6.88) ng g(-)(1) of Ni.     

The determination of total lead in soil by atomic absorption spectrophotometry

A method is described for the determination of total lead in soil by atomic absorption spectrophotometry. The sample is digested with hot nitric acid. The dry residue is taken up in hydrochloric acid and excess iron is removed by extraction with acetylacetone‐chloroform. Lead is then extracted using the system DDC‐MIBK. The organic phase can be sprayed directly into the flame.

The method is not affected by elements occurring in contaminated soils. Iron is removed because a slow‐forming precipitate of the Fe‐DDC‐complex blocks the nebuliser system. The method is an improvement on other methods because no sulfuric acid is used for digestion, and therefore losses of lead by precipitation or occlusion are avoided. Tests confirm that the recommended method gives complete recovery of lead.

Lead can be determined in the range from 4 to 240 ppm in the soil. A standard soil sample has been analyzed, yielding a mean value of 125 μg Pb/g soil with a relative standard deviation of 2.4%.