Furnace Atomic Absorption Spectrometry Method Research Articles

Rapid and Convenient Assessment of Trace Element Contamination in Agricultural Soils through Slurry-TXRF and Ecological Indices: The Ñuble Region, Chile as a Case Study

The study aims to evaluate the applicability of the slurry-TXRF method for estimating background contents and ecological indices in a rapid and convenient way. For this reason, the agricultural soils of the Itata Valley were used as a case study, where 48 soil samples were collected and analyzed. This rapid, minimally sample-intensive, and simultaneous multi-element quantification technique presented high accuracy but lower precision (approx. 20% RSD) compared to the classic total reflection X-ray fluorescence and flame/graphite furnace atomic absorption spectrometry methods, which require sample digestion. Due to the analytical characteristics of Slurry-TXRF, it can be concluded that the lower precision is likely compensated for, and this method represents a valuable alternative for the rapid and efficient assessment of trace element contamination in agricultural soils. The regional median concentrations of Cr, Ni, Cu, Zn, and Cd in the Itata Valley surface soils were found to be 63.7, 9.57, 31.0, 41.1, and 0.56 mg kg−1, respectively, with corresponding upper limits of 47.6, 6.82, 17.0, 30.7, and 0.284 mg kg−1. The ecological indices, including the geoaccumulation index, contamination factor, enrichment factor, and degree of contamination, suggest moderate levels of contamination in the region.

Development and validation of Graphite Furnace Atomic Absorption Spectrometry method and its application for clinical evaluation of blood lead levels among occupationally exposed lead smelting plant workers.

The growing interest in estimating the blood lead levels, for early detection of lead exposure, warranted a need for a validated analytical method for trace levels estimation of lead. The present study aimed to develop an analytical method for detecting trace amounts to elevated levels of lead in human blood using the Graphite Furnace Atomic Absorption Spectrometry technique and its application in evaluating blood lead levels among occupationally exposed individuals. The method validation was performed with standard test parameters including linearity, recovery, precision, method detection limit, and limit of quantification. The validation results for each performance parameter were in agreement with acceptable criteria as per standard guidelines. The correlation was observed as optimum linear (R2 = 0.998) between absorbance and lead concentration range from 0 to 10µg/dL. The recoveries for spiked samples ranged between 95 and 105%. The calculated value for the method detection limit was 0.16µg/dL and the limit of quantification was 0.51µg/dL. The precision for all spiked concentrations was below 10% of the relative standard deviation. Evaluation of lead exposure among occupationally exposed individuals revealed the study population had found average blood lead level (42.80 ± 12.47µg/dL), which was above the upper acceptable limit suggested by Occupational Safety and Health Administration, USA. The majority of system-specific symptoms were observed among study groups having mean blood lead levels above 40µg/dL. However, sociodemographic status and employment factors were found possible determinants of the prevalence of high blood lead levels.

Evaluation of Uncertainty in Determination of Lead in Milk and Dairy Products by Atomic Absorption Spectrometry

In the field of food safety inspection, researchers should fully consider the impact of measurement uncertainty to ensure the accuracy of the results, Especially when it affects the determination of detection results.This study is to establish the mathematical model of uncertainty, Synthesize and expand each uncertainty component .Finally, the uncertainty evaluation method for the determination of lead in milk and dairy products by atomic absorption spectrometry was established. Take milk powder as an example, the uncertainty of graphite furnace atomic absorption spectrometry method 1 in GB 5009.12-2017 National Food Aafety Standard Determination of Lead in Foods was evaluated by referring to JJF 1059.1-2012 Evaluation and Expression of Measurement Uncertainty. When the standard result of lead content in milk was 0.095 mg/kg, the synthetic standard uncertainty of the determination result was 0.0022 mg/kg, k=2, and the extended uncertainty was 0.005 mg/kg, and the result could be expressed as (0.095±0.005) mg/kg. The uncertainty of measurement results is mainly due to the uncertainty component introduced by test repeatability and standard solution concentration. Therefore, in the actual testing work, the accuracy and reliability of the results can be ensured by increasing the number of standard working fluid, using glass instruments with higher accuracy, and increasing the number of parallel samples.

Graphite furnace atomic absorption spectrometry for the determination of trace gallium in whole blood

Objective: To establish a graphite furnace atomic absorption spectrometry method for the determination of trace gallium in whole blood. Methods: From January to May 2021, the five factors of ashing temperature, ashing time, atomization temperature, atomization time and matrix modifier concentration in the determination of gallium in whole blood by graphite furnace atomic absorption spectrometry were optimized by using L(16) (4(5)) orthogonal test design. At the same time, within-run, between-run, spiking recovery test and other methodological indicators were tested. Results: Under the optimized detection conditions, the linear range of determination of gallium in whole blood by graphite furnace atomic absorption spectrometry was 0.29-100.00 μg/L (r=0.9991) . The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 10.0, 50.0, 80.0 μg/L concentration levels were 2.3%-4.4% and 1.5%-3.6%, the recovery rate of spiking was 98.1%-103.8%, and the detection limit of the method was 0.13 μg/L. Conclusion: Graphite furnace atomic absorption spectrometry for the determination of trace gallium in whole blood is easy to operate, has a wide linear range, low detection limit, accurate and reliable results, which is suitable for occupational health examinations and the determination of acute gallium poisoning.

Direct determination of zinc in plasma by graphite furnace atomic absorption spectrometry using palladium/magnesium and EDTA matrix modification with high temperature pyrolysis

A new graphite furnace atomic absorption spectrometry method is presented for the analysis of zinc in small volume biological samples.

Development of an Ionic Liquid Based Dispersive Liquid–Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry Method for Highly Selective and Sensitive Determination of Copper

Development of an Ionic Liquid Based Dispersive Liquid–Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry Method for Highly Selective and Sensitive Determination of Copper

Fluorene functionalized nanoporous SBA-15 incorporated into carbon paste electrode for trace copper determination

In this study, fluorene 3-[2-(2-aminoethylamino)ethylamino]propyl trimethoxy silane functionalized nanoporous SBA-15 was incorporated into carbon paste electrode for the potentiometric detection of Cu2+ ions in aqueous medium. With 15.5 wt% FT-SBA-15 proportion, the developed electrode exhibited wide dynamic range of 1.0 × 10−6–1.0 × 10−2 mol L−1 toward Cu2+ with a detection limit of 5.0 × 10−7 mol L−1 and a Nernstian slope of 29.6 ± 1.0 mV decade−1. The electrode displayed rapid response (~44 s), long-term stability (more than 6 months) and high sensitivity. Moreover, the potentiometric responses could be carried out with a wide pH range of 3.9–6.6. Finally, the proposed electrode was successfully used as an indicator electrode in potentiometric titration of copper ions with EDTA and to determine the concentration of copper ions in seawater, tap water and black tea samples. The results showed a good correlation with the data obtained by graphite furnace atomic absorption spectrometry method.

Aluminum content of human semen: Implications for semen quality

A deterioration of human semen quality has been observed over recent decades. A possible explanation could be an increased exposure to environmental pollutants, including aluminum. Our aim was to measure the aluminum concentration in the semen of 62 patients and to carry out a preliminary evaluation on its impact on specific semen parameters. For each patient, semen analyses were performed according to WHO guidelines. A graphite furnace atomic absorption spectrometry method was used to determine semen aluminum concentration. A cytological analysis using an aluminum-specific fluor, lumogallion, was also performed. The mean aluminum concentration in human semen was 339 μg/L. Patients with oligozoospermia had a statistically higher aluminum concentration than others. No significant difference was observed for other semen parameters. Cytological analysis showed the presence of aluminum in spermatozoa. This study provided unequivocal evidence of high concentrations of aluminum in human semen and suggested possible implications for spermatogenesis and sperm count.

Determination of Chromium in Biological Material by Electrothermal Atomic Absorption Spectrometry Method

Abstract Procedure for determination of chromium in biological materials by Zeeman graphite furnace atomic absorption spectrometry method using a Perkin-Elmer spectrometer equipped with hollow-cathode lamp at 357.9 nm was developed. The samples of animal tissues, food, and feed were digested in muffle furnace at 450ºC. The ash was dissolved in 1 N hydrochloric acid and the final solution was diluted in 0.2% nitric acid. Magnesium nitrate (1%) was used as a matrix modifier. The method was validated in terms of basic analytical parameters. The mean recoveries of chromium was 84.4% for muscle, 79.0% for canned meat, and 80.2% for feed, and analytical detection limit was 0.003 μg/g. Certified reference materials were used for analytical quality assurance. The proposed analytical procedure is well adapted for monitoring chromium content in food and feedstuffs. Content of total chromium in the tested samples (animal muscles and liver) was low and was situated in the range of 0.031-0.101 mg/kg (muscles) and 0.047-0.052 mg/kg (liver).

Analysis on heavy metal pollution in major seafoods from Zhoushan Fishery, China

Through reviewing data on surveys, tested materials especially on lead in Zhoushan fisheries, with ground lead, cadmium and methyl-mercury were analyzed and evaluated. According to the distribution of Zhoushan fisheries, we randomly selected a certain number of Zhoushan seafood as research objects from four counties or districts. Different kinds of seafood would include sea fish, seawater crustaceans, seawater soft-bodied animals and sea algae. The inedible parts of all the seafood were removed, and then the samples of the edible parts were grinding into homogenate. We measured the contents of lead and cadmium, using graphite furnace atomic absorption spectrometry method. The content of methylmercury was measured, using the gas chromatography (acid extraction method of mercaptoacetic cotton). Data from 2007 to 2009 was analyzed under SPSS software. (1) The average standardized rates were: lead as 3.90% (11/282), cadmium as 11.35% (32/282) and methylmercury as 2.84% (8/282). (2) Results from the comprehensive evaluation on the contents of metals showed the following rankings: seaweed (0.4513 mg/kg), marine molluscs (0.1155 mg/kg), marine crustaceans (0.0486 mg/kg), sea-fish (0.0419 mg/kg). (3) Results from the single-factor variance analysis showed that the accumulation of lead, cadmium and methylmercury in different types of seafood were: lead F = 35.683 (P < 0.001); cadmium F = 25.301 (P < 0.001); methylmercury F = 25.990 (P < 0.001). (4) Data on the safety analysis related to the different types of seafood on lead, cadmium, methylmercury food, the Chi-square tests showed as: lead χ(2) = 10.167, P < 0.05; cadmium χ(2) = 62.940, P < 0.001; methylmercury χ(2) = 20.960, P < 0.001. (5) Seafood in different years on lead, cadmium, methylmercury accumulation comparison, the Spearman correlation test results showed: lead P = 0.000, cadmium P = 0.974, methylmercury P = 0.024. (6) The contents of seafood lead, cadmium and methylmercury in different years that with statistically significant differences were as follows: lead χ(2) = 6.440, P < 0.05; cadmium χ(2) = 34.455, P < 0.001; methylmercury χ(2) = 5.226, P > 0.05. The situation of heavy metal pollution in different kinds of Zhoushan fisheries was different. Algae appeared the worst while sea fish, sea water crustaceans pollution were light, with lead and methylmercury mainly influencing sea algae and cadmium mainly in the sea algae, followed by seawater software class. The rates over standards of different kinds of seafood were different from each other, while the rates over standards of lead, cadmium and methylmercury in sea algae were the highest. Evaluated by pollution index, lead, methylmercury pollution was still low, but cadmium in the sea with mild pollution in algae seafood. In the recent three years, heavy metal lead pollution in seafood were worsened, while the cadmium, methylmercury pollution levels remained basically stable.

Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd+0.06% Mg+0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1μgkg−1 for arsenic and 0.2μgkg−1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8mg and 10mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a “cold finger” was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

Selective extraction of traffic-related antimony compounds for speciation analysis by graphite furnace atomic absorption spectrometry

Most traffic-related antimony air pollutants are derived from brake dust. Brake dust contains Sb 2S 3, used as a friction material in brake pads, and its high-temperature oxidation products, Sb 2O 3 or Sb 2O 4. Systematic investigations were carried out to find the most selective leaching conditions for these substances. First, solubility experiments of the pure potential compounds mentioned above were carried out. Then, the leaching of these compounds from home-made artificial dusts previously spiked with these compounds at the trace level was investigated. A 0.5 mol L − 1 citric acid solution proved to leach the whole Sb 2O 3 content while extracting less than 10% Sb 2S 3 and no Sb 2O 4 at all. It was found that Sb 2O 3 and Sb 2S 3 traces were soluble in a 6 mol L − 1 HCl solution, quantitatively and selectively. Graphite furnace atomic absorption spectrometry and hydride generation graphite furnace atomic absorption spectrometry methods were developed to determine the Sb content of the extracts. The proposed method proved to be applicable to settled dust containing traffic-related Sb compounds. The detection limits were 1.2 and 0.3 μg g − 1 for leaching by citric acid and HCl solution, respectively, which were adequate for Sb content determination in the urban dust studied. The reproducibility of the method expressed as relative standard deviation was about 7%. The results showed that the concentration of leachable Sb was 40 μg g − 1 in the settled dust of Budapest, about half of which corresponded to Sb 2O 3. The Sb 2O 4 content calculated as the difference of total and leachable fraction was about 10% with high uncertainty.

Fish Consumption in an Area with High Incidence of Birth Defects in Cali, Colombia

ISEE-0628 Background: Clustering of rare birth defects (BD) in a poor area of Cali, Colombia, are reported since 2004, when a hospital-based registry was implemented (ECLAMC). Cases cluster in a poor and large “comuna” of the city (7.2%), near to a polluted river (Cauca river) and the municipal dump site. Objective: To characterize fish consumption in a group of childbearing age women, 15–34 years of age, in a community with clustering of BD. Methods: We developed a descriptive study of knowledge and practices about fish consumption. A multistage sampling strategy was used to select women with local health promoters. We applied a questionnaire to 380 non-pregnant women living >6 months in the community, and asked for consumption frequency and seasonality, fish types and origin, and perceived health effects. Additionally, we characterized chicken, meat and pork consumption, water use and local crop related practices. Fish species reported by women were analyzed using graphite furnace atomic absorption spectrometry methods to determine metals. Results: Women included were young (75% < 28 years) and most of them had no affiliation to social security (45%). They reported a high frequency of fish consumption: 43.7% at least weekly, 79.5% at least once in a year. Consumption is higher (67.8%) in April (Easter), and 11.4% reported consumption of Cauca river fishes. Women reported that fish may only cause short term gastrointestinal effects. Water for consumption comes exclusively from the municipal distribution network and practices related to crops were infrequent. We analyzed two types of fish species: fishes that eat sediment and predator fishes. In both species we found Cd, Hg and Pb, with Pb levels above FAO recommendations. Conclusions: Consumption of local fish is a potential route of exposure to pollutants during pregnancy, mainly Pb. Other exposures routes/pathways may interact with fish consumption.

Trace element analysis of silicon nitride powders by direct solid sampling graphite furnace atomic absorption spectrometry

A graphite furnace atomic absorption spectrometry method using direct solid sampling has been developed for the determination of Cr, Cu, Fe, K, Mn, Sb and Zn in powdered silicon nitride. Although during the atomization of all analytes excluding Zn, conversion of silicon nitride into silicon and silicon carbide was taking place and its essential part vaporized in the form of different species, no problems occurred with background correction. Calibration could be carried out by using calibration curves obtained with aqueous standard solutions. In the determination of Fe, before sampling, the platform bottom was covered with graphite powder in order to achieve quantitative vaporization and to increase the lifetime of the platform. For the latter reason, the use of graphite powder was advantageous in the determination of Cr and Cu, too. With sample masses up to about 2 mg applied per analysis cycle, the relative standard deviations were between 5 and 18% (n = 5). For the most sensitive conditions, limits of detection between 0.1 (Zn) and 2 ng g−1 (Fe) are achievable. The accuracy was checked by comparison of the results with those of four other methods including neutron activation analysis whereby good to reasonable agreement was achieved.

Determination of Lead in Serum by Graphite Furnace Atomic Absorption Spectrometry

ObjectiveA graphite furnace atomic absorption spectrometry method was developed for detecting lead in serum.MethodsSamples were automatically introduced and matrix modifiers were added.Samples were detected without being digested.ResultsWith experimental condition optimizing,detection limit was 4.60×10-12A/ng.The ranges of lead was 10-30μg/L,the recovery rate was 95.87%-105.41%.ConclusionThe method was reliable,fast and sensitivity.It was an ideal method to detect lead in serum.

Speciation of butyltin compounds in marine sediments and sea-shells by HG/GC/QFAAS

After optimisation of sample pretreatment and determination procedures, butyltin compounds were determined in selected marine sediments and biota using the hydride generation/gas chromatography/quartz furnace atomic absorption spectrometry method. Butyltins were detected in all surface sediment samples of Arcachon Bay, though at widely different concentrations (from a few ng g-1 in remote areas to 158 ng g-1 in marinas). The relative abundances of mono-, di- and tri-butyltin vary with the distance to point pollution sources and the depth of burial (i.e. the storage time). Half-life times of the three butyltin compounds were estimated in a marina sediment as close to 1.1, 1.9 and 2.1 years, respectively. Quite significant concentrations of butyltin compounds were measured in some commercial sea-shell samples.

Determination of Cadmium in Wines Using Graphite Furnace Atomic Absorption Spectrometry with Zeeman Background Correction

A graphite furnace atomic absorption spectrometry method with Zeeman background correction for the direct determination of cadmium in grape wines is described. Use of ammonium dihydrogen phosphate, magnesium nitrate, and palladium nitrate as matrix modifiers was investigated. Palladium nitrate with 10% nitric acid was the most satisfactory matrix modifier. The methodological detection limit, calculated as 3σ/slope of the calibration curve, was 0.03 μg/liter for cadmium in wine. The sensitivity, calculated as the characteristic mass, was 0.4 pg. The use of palladium nitrate as a matrix modifier also results in excellent reproducibility (<10% RSD) at such low levels. This method is readily applicable to the determination of cadmium in wines without any sample preparation.

Graphite Furnace Atomic Absorption Spectrometry for the Determination of the Chromium Content of Selected U.S. Foods

A graphite furnace atomic absorption spectrometry method was used to determine the chromium content of selected foods following a modified dry ashing sample preparation procedure. Platform atomization is used and quantitation is accomplished using peak area measurements. Both direct calibration against aqueous standards and the use of method of additions provide accurate results. The method provides an instrumental detection limit of 5.6 pg chromium and a characteristic mass of 3.2 pg. This corresponds to a method detection limit of approximately 1 ng/g for a 20 μl injection of a digest of a typical 3-g sample diluted to a final volume of 10 ml. The method was validated using commercial standard reference materials. More than 40 frequently consumed foods were analyzed and the chromium content is reported. When available, data are compared with previous literature reports. There is, as expected, a reasonable amount of variability in the chromium content of some products. Those foods which are the best sources of chromium tend to be cereals and grains, vegetables, and fruits.

Determination of trace lithium in biological fluids using graphite furnace atomic absorption spectrophotometry: Variability of urine matrices circumvented by cation exchange solid phase extraction

A graphite furnace atomic absorption spectrometry method has been developed for the quantitative determination of submicromolar endogenous concentration of lithium in human plasma and urine using pyrolitically-coated graphite tubes in combination with ammonium nitrate matrix modification. This latter treatment could not completely abolish the interferences caused by the matrix, notably in urine samples. The variability of the urinary matrices required an additional standardization procedure by solid-phase extraction on strongly acidic cation exchange cartridges. Matrix-matched samples were used for the establishment of calibration curves with the addition-calibration method. Calibration curves were linear up to 0.72 μmol/l (1.0 > r2 > 0.99). The described method enables accurate measurements of trace-lithium in biological samples at concentrations down to 0.03 μmol/l with intra- and inter-day variabilities < 10%. The method was applied to the determination of trace-lithium levels in urine and plasma samples from healthy individuals enabling the calculation of its fractional excretion (FeLi) (median range 17.3%), a value which reflects the functional capacity of the kidney to reabsorb sodium and water at the proximal tubular portion of the nephron. This sensitive method can thus be used as an investigative and diagnostic tool in various renal pathophysiological conditions, in clinical research, and may also be applied to studies on the trace-lithium status of population in connection with psycho-affective disorders.

Application of experimental designs in optimization of a hydride generation quartz furnace atomic absorption spectrometry method for selenium determination

An optimization of the hydride generation quartz furnace atomic absorption spectrometry (HG-QFAAS) method used for selenium trace determination was performed. Experimental designs at two levels, including seven factors, were used, allowing the evaluation of the influence of each analytical variable on peak area, repeatability and signal-to-noise ratio (S/N). For peak area, the most significant factors are the helium and oxygen flow-rates. The NaBH4 flow-rate and hydride generator temperature have a strong significant effect on repeatability. No factor is really essential for the S/N. The detection limit is 1.5 ng of SeIV(3sb). The absorbance is found to be linear over the range 1.5–60 ng. A 3.72% relative standard deviation is obtained for six determinations of 10 ng of SeIV standard solution. A Community Bureau of Reference (BCR) certified reference material (CRM) 402 White Clover was studied, in order to control the quality of the determination. The total selenium contents were determined using the HG-QFAAS optimized method and then compared with the results given by an electrochemical method (differential pulse cathodic stripping voltammetry).