Inductively Coupled Plasma Atomic Emission Spectrometry Analysis Research Articles

Analysis of Corrosion-Resistant Ruthenium-Doped Titanium Alloys by Inductively Coupled Plasma Atomic Emission Spectroscopy

A technique for analyzing new corrosion-resistant ruthenium-doped titanium alloys using inductively coupled plasma atomic emission spectrometry (ICP-AES) with microwave sample preparation is reported. The composition of a mixture of acids and the temperature and time parameters of sample preparation of titanium alloys under microwave heating in an autoclave ensuring quantitative conversion of the sample into a convenient analytical form without loss of volatile components for subsequent ICP-AES analysis are substantiated. Optimal conditions for the excitation of the analytical signal have been found, and analytical lines of elements without spectral noise have been selected. Samples of experimental melts of industrial titanium alloys of various classes, volumetrically doped with ruthenium, which are under development and are not yet commercially produced in the Russian Federation (alloy PT-7M + Ru, PT-3B + Ru, 5B + Ru, 37 + Ru, VT-22 + Ru) have been studied. The alloy samples contained the following alloying elements (wt %): Al (1.8–6.3); V (1.0–5.5); Mo (0.7–5.5); Zr (0.2–3.0); Cr (0.5–1.5); Fe (0.5–1.5); Ru (0.05–0.15). The correctness of the determination of alloying elements has been confirmed by analyzing standard samples by varying their mass and, in the case of ruthenium, by the “introduced–found” method. The developed method significantly reduces the time of analysis by combining the multielement ICP-AES method with microwave sample preparation, expands the list of detectable elements in titanium alloys, and improves the precision of the results of analysis.

Direct high sensitive determination of elements in gasoline, kerosene, and mineral oil solutions by inductively coupled plasma atomic emission spectrometry (ICP-AES)

Direct ICP-AES analysis of petroleum products, organic solvents and fuels is oftentimes possible only in the mode of radial plasma viewing and requires the use of special sample injection systems, the design of which depends significantly on the physical properties of the sample, in particular, on its volatility and viscosity. Volatile oil fractions and products (naphtha, gasoline), as well as and heavy and viscous oil fractions of and petroleum products (vacuum gas oil, fuel oil, thick lubricating oils) are the most problematic objects of analysis. We consider the possibility of direct analysis of the samples based on gasoline, kerosene and lubricating oils dissolved in kerosene using inductively coupled plasma atomic emission spectrometry (ICP-AES). The possibility of using various configurations of sample injection systems and modes of plasma viewing of vertically located torch for direct analysis of the samples based on kerosene and gasoline is considered. A significant improvement in the sensitivity of determination of the elements in gasoline and kerosene using an axial plasma viewing combined with optimal configurations of sample introduction systems and plasma burning modes is demonstrated.

Analysis of surfacing materials from cast carbide alloys using inductively coupled plasma atomic emission spectrometry (ICP-AES)

A technique for analysis of surfacing materials (cast cobalt-based carbide alloys) using by ICP-AES in combination with microwave autoclave sample preparation is developed. Composition of the acid mixture, temperature and time parameters of the sample preparation under microwave heating in an autoclave are specified, thus ensuring complete quantitative transfer of the sample into a convenient analytical form without losses of volatile components for the subsequent ICP-AES analysis. Analytic lines of the elements free from spectral interference were chosen to determine all the rated components in the casting materials from cast carbide alloys. Study of surfacing materials was carried out using alloys Pr-B3K-PrH-U10Kh63B5, Pr-B3K-P-PrN-U20Kh57B10 and TsN-2-E-190K62X29B5C2, containing the alloying elements (% wt.): Co (up to 65); Cr (28.0 – 32.0); W (4.0 – 11.0); Si (1.0 to 3.0); C (1.0 – 2.0); Ni (0.1 – 2.0); Mn (0.3 – 0.6) and Fe (up to 2.0). The correctness of determining rated element was confirmed in analysis of standard samples using sample weight variation. The developed technique was tested on industrial prototypes of surfacing materials made of cobalt-based cast carbide alloys of tested grades. The method is rapid (11-fold reduction in the time of analysis) and reagent-saving (by 12.5 times) procedure compared to single-element methods by 11 times and reduction of the volume of applied reagents. Combination of the multielement ICP-AES method with microwave sample preparation provides an increase in the accuracy of Si, Cr, Mn, Fe, Ni, and W determination in surfacing materials of cast carbide alloys within a range of rated concentrations.

Application of tandem calibration for the direct analysis of copper by inductively coupled plasma atomic emission spectrometry (ICP-AES)

A procedure has been proposed for the direct ICP-AES analysis of solid copper samples using spark sampling. Calibration curves have been obtained using multi-element reference solutions of analytes (MES). The internal standards are spectral lines of copper with the energy parameters (excitation and ionization potentials) similar to those of analytes. Standard Reference Material (SRM) of copper have been used for the estimation of performance characteristics. The absence of significant differences between the found and certified concentrations of analytes has been shown. The developed procedure of ICP-AES analysis of solid copper samples with spark sampling and calibration using MES provides the determination of up to 14 elements: Ag, As, Au, Cd, Fe, Mn, Ni, P, Pb, Pt, Sb, Se, Sn, Te, and Zn in the concentration range from n × 10−3 to n × 10−1 wt %.

Purification of metallurgical grade silicon by a microwave-assisted plasma process

A new microwave plasma process is developed to refine and purify metallurgical grade silicon (MG-Si) effectively. Inductively coupled plasma-atomic emission spectrometry analysis (ICP-AES) indicates that the concentrations of impurities in silicon decrease significantly in the process, particularly for phosphorus, whose average removal rate is close to 100% after microwave plasma treatment of only 5min. The underlying mechanisms of the ultra-high removal rate of impurity atoms are discussed in detail in this paper. The photoresponse switching behavior of n+-Si wafers that are made of as-purified silicon provides further evidence for the unique advantage arising from the use of microwave plasma in the purification of MG-Si.

Maltose and pectin assisted sol–gel production of Ce0.8Gd0.2O1.9 solid electrolyte nanopowders for solid oxide fuel cells

A novel sol–gel method has been developed for the production of high purity nanopowders of cerium gadolinium oxide (CGO, Ce0.8Gd0.2O1.9) solid solution using maltose as an organic chelating agent and pectin for gelation. The results of this investigation indicate that the final particle size of approximately 10 nm can be obtained after calcination of the predried gel at 500 °C for 2 hours in ambient air. An insight into the calcination process has been obtained by using simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA/DSC). Powder X-ray diffraction (XRD) confirms that all samples are single phase cubic CGO powders with no trace of impurity. The mean crystallite sizes calculated from XRD analysis using the Rietveld refinement method agree with the morphological features observed by transmission electron microscopy (TEM). The nanopowders produced in this study exhibit negligible strain as indicated by the Rietveld refinement procedure. The nominal composition of CGO has been found to be in excellent agreement with that determined by energy dispersive X-ray spectroscopy (EDS) and inductively coupled plasma-atomic emission spectrometry analysis (ICP-AES). The XRD and TEM analyses indicate that there is a significant influence of calcination temperature on the particle size which increases with increasing temperature for a fixed annealing time. This new sol–gel method is a cost effective, simple, environmentally friendly and non-toxic route for a large scale production of high purity single phase nanopowders of complex oxide functional ceramic materials at significantly low temperatures.

New methods for the direct determination of dissolved inorganic, organic and total carbon in natural waters by Reagent-Free™ Ion Chromatography and inductively coupled plasma atomic emission spectrometry

New methods have been developed and applied successfully for the determination of dissolved inorganic, organic and total carbon in water samples. The new methods utilize two instrumental setups, Reagent-Free™ Ion Chromatography (RF™-IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Dissolved inorganic carbon (DIC) was measured in untreated samples along with Cl −, F − and SO 4 2− using RF™-IC and by in-line mixing with 0.1 M HNO 3 to enhance CO 2 removal in the nebulizer, followed by ICP-AES analysis. Total dissolved carbon (TDC) was measured by in-line mixing with 0.1 M NaOH following ICP-AES analysis. Dissolved organic carbon (DOC) was obtained as the difference between DIC and TDC. Only non-volatile organic carbon could be detected by the present method. The workable limits of detection obtained in the present study were 0.5 mM (RF™-IC) and 0.1 mM (ICP-AES) for dissolved inorganic and organic carbon, respectively. The power of the new methods lies in routine analysis of DIC and DOC in samples of natural waters of variable composition and salinity using analytical techniques and facilities available in most laboratories doing water sample analysis. The techniques are sensitive and precise, can be automated using gas-tight sample vials and auto-samplers, and are independent of most elemental interferences with the exception of chloride overload by saline samples when using RF™-IC. The new methods were successfully applied for analysis of DIC and DOC in selected samples of natural and synthetic waters.

Statistical validation of sulfate quantification methods used for analysis of acid mine drainage

Turbidimetric method (TM), ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES) with and without acid digestion have been compared and validated for the determination of sulfate in mining wastewater. Analytical methods were chosen to compare the performance of a portable field turbidimetric instrument and to validate the underlying assumption utilized in conversion of total sulfur to sulfate during ICP-AES analysis. Accuracy and precision of analytical techniques were compared to one another using control and field samples collected from a mine site using the Bonferroni multiple comparison test. Effects of sample dilution, filter pore size and acidification on sulfate quantification were also studied. The results showed that IC and ICP-AES with and without acid digestion provided excellent recoveries in the case of control samples (within 90–110%). These analytical methods also showed lower relative standard deviation for both control and field samples. On the other hand, performance of the turbidimetric method was severely affected by sample dilution and acidification, and also revealed poor sulfate recoveries for control samples ranging from 0 to 83.5%. Analysis of variance (ANOVA) was used to evaluate the response (sulfate concentration) obtained from factorial design. Analytical method had significant effect ( P < 0.0001) on the sulfate quantification. The interaction between determination method and sample dilution was more significant than other two-way interactions.

Atomemissionsspektralanalyse mit induktiv gekoppeltem Plasma (ICP-OES) von Granulomen zementierter und zementfreier Hüftendoprothesen Examination of granuloma of revised cemented or cementless total hip arthroplasties using inductively coupled plasma atomic emission spectrometry (ICP-OES)

Aseptic loosening is the most common problem in total hip arthroplasty (THA). One main aspect is inflammatory reaction against wear particles of the prosthesis materials. Analysing failure mechanisms in THA analysis of the particles and their element distribution of revised granulomatous tissue is essential to improve materials used in THA. 23 granulomas of revised THA due to aseptic loosening, 13 of which with metal on metal bearing (M/M), were analysed using inductively coupled plasma atomic emission spectrometry (ICP-OES). Elements Cr, Mn, Ni, Al, Cu, Zn, Cd, Ti, V, Zr, Nb and Fe could be detected. The maximum value of Cr was 23.88 ppb (parts per billion), Al 191.02 ppb, Ni 64.95 ppb and Zr 9.96 ppb. The highest value of Al could be found in cementless implants. The maximum value of the elements Cr and Ni could be detected in M/M. In cemented implants the highest value of Zr was found. The origin of Zr was the used bone cement in cemented THA. The elements Cr and Ni were significantly higher in M/M bearings. The highest value of Al was detected in granulomas of revised corund rough blasted cementless implants. The histopathologic findings of the revised M/M bearings have been published recently. Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-OES) could not show any differences of the alloying constituents in cases with or without allergic reactions. ICP-OES analysis seems to be not useful examination of histologic sections using SEM with cryotransfer unit.

Determination of Ru, Rh, Pd, Te, Mo and Zr in spent pressurized water reactor fuels by ion exchange and extraction chromatographic separations and inductively coupled plasma atomic emission spectrometric analysis

A study has been carried out on the quantitative analysis of Ru, Rh, Pd, Te, Mo and Zr, which are main components of undissolved materials dispersed in nitric acid dissolver solutions of spent pressurized water reactor (PWR) fuels, using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution of the insoluble residues filtrated from the dissolver solutions by acid digestion bomb technique and the separation of Ru, Rh, Pd, Te, Mo and Zr from U and transuranous elements in the filtrate by ion exchange, and di(2-ethylhexyl) phosphoric acid (HDEHP) extraction chromatography were discussed in detail. The applicability and versatility of the proposed separation procedure combined with ICP-AES analysis were evaluated by chemically characterizing the spent PWR fuels with burnups from 36,000 to 39,000 MWd/MtU.

ICP-AES analysis of some Mycenaean vases from the cemetery at Pylona, Rhodes

This paper presents the results of the chemical analyses by inductively coupled plasma atomic emission spectrometry (ICP-AES) of a selection of vases from the recent excavations of Mycenaean tombs at Pylona, Rhodes. The data are used to support and confirm the stylistic attributions of the vases as either local Rhodian products or mainland imports. It is suggested that the majority of the imports are from the Argolid, but that at least one other origin is likely as well. Two distinct compositional groups of ‘local’ pottery are also identified. Comparison is made with the data from the analyses of pottery from Ialysos and the veracity of the conclusions drawn from the earlier optical emission data is confirmed.

Effects of Echinostoma caproni infections on metallic ions in the intestinal mucosa of ICR mice

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to study metallic ions in the intestinal mucosa of ICR mice infected with Echinostoma caproni and the mucosa of uninfected control mice. Infected mucosa (n = 9 with about 100 mg wet weight per sample) were examined at 2 weeks p.i. in mice that were infected with about 25 worms per host. Uninfected mucosa (n = 9 with about 100 mg wet weight per sample) were examined in the same time frame as the infected mucosa. Five metals were measured in the mucosa by ICP-AES analysis, as follows: calcium, potassium, magnesium, sodium and zinc. There were no significant differences (Student's t-test, P > 0.05) in the concentrations of calcium, potassium or zinc in infected versus uninfected mucosa. The concentration of sodium was significantly greater (P < 0.05) in the mucosa of infected versus uninfected mucosa, but the situation was reversed in regard to magnesium.

Effects of Echinostoma caproni infections on metallic ions in the intestinal mucosa of ICR mice

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to study metallic ions in the intestinal mucosa of ICR mice infected with Echinostoma caproni and the mucosa of uninfected control mice. Infected mucosa (n = 9 with about 100 mg wet weight per sample) were examined at 2 weeks p.i. in mice that were infected with about 25 worms per host. Uninfected mucosa (n = 9 with about 100 mg wet weight per sample) were examined in the same time frame as the infected mucosa. Five metals were measured in the mucosa by ICP-AES analysis, as follows: calcium, potassium, magnesium, sodium and zinc. There were no significant differences (Student's t-test, P &gt; 0.05) in the concentrations of calcium, potassium or zinc in infected versus uninfected mucosa. The concentration of sodium was significantly greater (P &lt; 0.05) in the mucosa of infected versus uninfected mucosa, but the situation was reversed in regard to magnesium.

Preconcentration of some metals using metalfix chelamine resin prior to ICP-AES analysis

Preconcentration and separation of Ni, Pb and Cd have been investigated using the metalfix chelamine resin prior to inductively coupled plasma – atomic emission spectrometry (ICP-AES) under various experimental conditions. The recoveries of the analytes obtained with 95% confidence level were 92 ± 1% for Ni, 100 ± 4% for Pb and 93 ± 3% for Cd.

Direct determination of trace elements in niobium, tantalum and their oxides by inductively coupled plasma atomic emission spectrometry after microwave dissolution

Analytical schemes for the determination of trace elements in high-purity niobium, tantalum and their oxides are proposed. The schemes are based on microwave dissolution of the metals and oxides followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of impurities in the solutions. The possibilities of interelement and off-peak background corrections in ICP-AES analysis are discussed. The accuracy of the results obtained is confirmed by the determination of trace elements after a matrix sorption separation procedure. For a number of elements, a comparison of the results obtained by ICP-AES without and with the matrix separation procedure and by electrothermal atomic absorption spectrometry (ETAAS) shows good agreement. The limits of detection for direct ICP-AES determination are in the range 0.4*1.0 μg g −1 for Ba, Ca, Fe, Mg, Mn, Y and La; between 2.0 and 10.0 μ g −1 for B, Cd, Co, Cr, Cu, Hf, Mo, Na, Nb, Ni, Pb, Sr, Ti, Zr and Ta; and for K, Sb and W a detection limit of 20 μ g −1 is achieved. The schemes proposed are intended for rapid routine analysis.

Validity of lowcost laboratory geochemistry for environmental applications

A little known alternative to highcost environmental analysis, especially in Europe, is the use of commercially available, lowcost exploration geochemical laboratory analysis. To test for suitable accuracy and precision, both indicated parameters were monitored during several sample runs for environmental examinations at a selected commercial geochemical laboratory using various digestive methods and ICP-AES (Inductively Coupled Plasma Atomic Emission Spectrometry). By evaluating duplicate samples and repeated measurements of internal standards and comparing the results with precision needed for environmental investigations, exploration geochemical analysis is found to be more than adequate for most elements and digestive methods in environmental applications. Accuracy is highest for total digestion ICP-AES analysis, with expectedly greater error margins for aqua regia digestion. Lowcost exploration geochemical analysis is an inexpensive analytical tool for screening, detailed investigations and monitoring of contaminated sites.

A Comparison of the Food Composition Table-based Estimates of Dietary Element Intake with the Values Obtained by Inductively Coupled Plasma Atomic Emission Spectrometry: An Experience in a Japanese Population

In order to make quantitative comparison between food composition table-based estimates and instrumental measures by inductively coupled plasma atomic emission spectrometry (ICP-AES), total food duplicates were collected from 232 adult women in 10 study regions in 9 Prefectures in Japan. Daily dietary intake of 5 elements, sodium (Na), potassium (K), phosphorus (P), calcium (Ca) and iron (Fe), were estimated from the weights of food items in each duplicate by use of food composition tables. Parallel to this the intakes were measured by wet-ashing of food duplicate homogenates followed by ICP-AES analysis. Because the emission intensity of K was significantly modified by Na co-present at various concentrations, K was measured after Na concentration was reduced to the value 150 mg/L by dilution. The comparison of the two sets of the results, the estimated values and the measured values, showed that the estimated values were significantly larger than the measured values in the cases of Na, K, Ca and P (the ratio of the estimated to the measured values: 118% for Na, 115% for K, 109% for Ca; and 130% for Fe), whereas the two values essentially agreed with each other in the case of P (ratio: 93%). The differences were too large for any nutritional evaluation to be made when the method of Bland and Altman is applied. The significance of the differences in relation to nutritional evaluation of element intake is discussed.

Determination of heavy metals in shellfish by flame atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry

Shellfish samples (clams, oysters and mussels) were analysed for Pb, Cd, Cu, Cr, Zn and Ni by flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) following wet-ash digestion. Split samples were taken for both FAAS and ICP-AES analysis. Vanadium was used as the internal standard for ICP-AES whereas 1.25% NaCl was added to the FAAS standards to correct for the high salt background associated with shellfish.The methods were compared for statistical significance using regression analysis, the F-test and Student's t-test. Precision and accuracy were determined by replicate analyses, recovery of added heavy metals and National Bureau of Standards (NBS) reference materials. Results obtained from regression analysis for the coefficient of determination or “goodness of fit” were all above the acceptable 0.80 level. The t-test showed that the methods were statistically similar for all metals tested at the 95% confidence level. Average percentage recoveries ranged from 80.2 to 100.7%. Heavy metals were added at approximate expected levels normally found in the shellfish.Accuracy, based on heavy metal levels determined by FAAS and ICP-AES versus certified values for NBS reference materials, varied with the individual reference materials tested. The over-all data obtained indicated that FAAS and ICP-AES showed good agreement for the determination of the heavy metals tested, ICP-AES providing a drastic reduction in analysis time following initial sample work-up.

Elemental analysis of welding fumes by X-ray fluorescence spectrometry

A method is described for the simultaneous multi-element determination of arsenic, cadmium, chromium, cobalt, copper, iron, lead, manganese, nickel, titanium, vanadium and zinc in welding fumes by wavelength dispersive X-ray fluorescence (XRF) spectrometry. Instrumental calibration is achieved by a thin-film dibenzyldithiocarbamate precipitation procedure based on standard metal solutions. The results obtained for the rapid and simple X-ray methodology described are found to be favourable in comparison with inductively coupled plasma atomic emission spectrometric analysis of synthetic and real samples. Details are given of the instrumental optimisation conditions and the interference characteristics for both the XRF and inductively coupled plasma atomic emission spectrometry (ICP-AES) techniques. The sampling strategy for welding fumes is considered with particular reference to the particle size distribution. The XRF analysis described compares favourably with ICP-AES analysis giving a sufficiently accurate method of analysis for the elements of interest without the need for lengthy sample preparation or calibration procedures.