Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry methods

Solid sampling (SS) graphite furnace atomic absorption spectrometry (GFAAS) and solution-based (SB) methods of GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were elaborated and/or optimized for the determination of Cr, Fe and Mn trace elements used as dopants in lithium niobate optical crystals.     

Derivative flame atomic absorption spectrometry and its application in trace analysis

Flame atomic absorption spectrometry (FAAS) is an accepted and widely used method for the determination of trace elements in a great variety of samples. But its sensitivity doesn’t meet the demands of trace and ultra-trace analysis for some samples. The derivative signal processing technique, with a very high capability for enhancing sensitivity, was developed for FAAS. The signal models of conventional FAAS are described. The equations of derivative signals are established for FAAS, flow injection atomic absorption spectrometry (FI-FAAS) and atom trapping flame atomic absorption spectrometry (AT-FAAS). The principle and performance of the derivative atomic absorption spectrometry are evaluated. The derivative technique based on determination of variation rate of signal intensity with time (dI/dt) is different from the derivative spectrophotometry (DS) based on determination of variation rate of signal intensity with wavelength (dI/dλ). Derivative flame atomic absorption spectrometry (DFAAS) has higher sensitivity, lower detection limits and better accuracy. It has been applied to the direct determination of trace elements without preconcentration. If the derivative technique was combined with several preconcentration techniques, the sensitivity would be enhanced further for ultra-trace analysis with good linearity. The applications of DFAAS are reviewed for trace element analysis in biological, pharmaceutical, environmental and food samples.     

Solid phase extraction of trace amounts of Pb(II) in opium, heroin, lipstick, plants and water samples using modified magnetite nanoparticles prior to its atomic absorption determination

A new, simple, fast and reliable solid-phase extraction method has been developed for separation/preconcentration of trace amounts of Pb(II) using dithizone/sodium dodecyl sulfate-immobilized on alumina-coated magnetite nanoparticles, and its determination by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after eluting with 4.0?mol?L^?1 HNO₃. Optimal experimental conditions including pH, sample volume, eluent concentration and volume, and co-existing ions have been studied and established. Under the optimal experimental conditions, the preconcentration factor, detection limit, linear range and relative standard deviation of Pb(II) using FAAS technique were 280 (for 560?mL of sample solution), 0.28?ng?mL^?1, 1.4?C70?ng?mL^?1 and 4.6% (for 10?ng?mL^?1, n?=?10), respectively. These analytical parameters using GFAAS technique were 300 (for 600?mL of sample solution), 0.002?ng?mL^?1, 0.006?C13.2?ng?mL^?1 and 3.1% (for 5?ng?mL^?1, n?=?10), respectively. The presented procedure was successfully applied for determination of Pb(II) content in opium, heroin, lipstick, plants and water samples.     

Bismuth as a general internal standard for lead in atomic absorption spectrometry

Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A^Pb/A^Biversus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52–118% (without IS) to 97–109% (IS, LS FAAS); 74–231% (without IS) to 96–109% (IS, HR-CS FAAS); and 36–125% (without IS) to 96–110% (IS, LS GFAAS). The relative standard deviations (n = 12) were reduced from 0.6–9.2% (without IS) to 0.3–4.3% (IS, LS FAAS); 0.7–7.7% (without IS) to 0.1–4.0% (IS, HR-CS FAAS); and 2.1–13% (without IS) to 0.4–5.9% (IS, LS GFAAS).     

Determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn by Inductively Coupled Plasma Mass Spectroscopy or Flame Atomic Absorption Spectrometry after On-line Preconcentration and Solvent Extraction by Flow Injection System

The concentrations of Cd, Co, Cu, Mn, Ni, Pb, and Zn in natural and sea waters are too low to be directly determined with by flame atomic absorption spectrometry (FAAS) or graphite furnace atomic absorption spectrometry (GFAAS). Specific sample preparations are requested that make possible the determination of these analytes by preconcentration or extraction. These techniques are affected by severe problems of sample contamination. In this work Cd, Co, Cu, Mn, Ni, Pb, and Zn were determined by inductively coupled plasma mass spectroscopy (ICP-MS) or by atomic absorption spectrometry, in fresh and seawater samples, after on-line preconcentration and following solvent elution with a flow injection system. Bonded silica with octadecyl functional group C₁₈, packed in a microcolumn of 100-μl capacity, was used to collect diethyldithiocarbamate complexes of the heavy metals in aqueous solutions. The metals are complexed with a chelating agent, adsorbed on the C₁₈column, and eluted with methanol directly in the flow injection system. The methanolic stream can be addressed to FAAS for direct determination of Cu, Ni, and Zn, or collected in a vial for successive analysis by GFAAS. The eluted samples can be also dried in a vacuum container and restored to a little volume with concentrated HNO₃and Milli-Q water for analysis by ICP-MS or GFAAS.     

Solid phase extraction of copper (II) by sorption on octadecyl silica membrane disk modified with a new Schiff base and determination with atomic absorption spectrometry

A simple, selective and reliable method for rapid extraction and determination of trace amounts of Cu (II) ions from aqueous samples using octadecyl-bonded silica membrane disks modified with bis-(3-methoxy salicylaldehyde)-1,6-diaminohexane and flame atomic absorption spectrometry (FAAS) is presented. Extraction efficiency, the influence of pH, flow rates, amount of ligand, and type and least amount of eluant were investigated. The linear dynamic range of the proposed method for Cu (II) ions was found in a wide concentration range of 1.0 (± 0.2)–150 (± 2) μg l^− 1. The detection limit and preconcentration factor of this method were found 30.0 (± 0.7) ng l^− 1 and 100 respectively. The reproducibility of the procedure is at the most 2.0%. The effects of various cationic interferences on the percent recovery of copper ion were studied. The method was used to the recovery of copper ion from different synthetic, alloys and biological samples.     

Preconcentration of trace silver with yeast for river water analysis

A new preconcentration method with yeast is presented. The method was evaluated for the determination of trace silver in river waters by graphite furnace atomic absorption spectrometry (GFAAS). A suitable cultivation bed for preconcentration of silver was 1.75 mg ml-1 2-ammonium hydrogen phosphate. The optimal cultivation time and temperature were 2 h and 25 degrees C. Under optimal conditions, silver in aqueous sample was concentrated to 6.9-fold by yeast. The detection limit was 4.6 pg ml-1 (3S/N) for silver in river water. The yeast preconcentration method was applied to the determination of silver in river waters. The recovery of spiked silver was in the range of 89 to 110%. By the preconcentration, it was found that ultra trace silver in river waters could be determined without interferences of matrix elements, after only the cultivation and with no chemical treatment.     

Preconcentration procedure using in situ solvent formation microextraction in the presence of ionic liquid for cadmium determination in saline samples by flame atomic absorption spectrometry

A simple in situ solvent formation microextraction methodology based on the application of ionic liquid (IL) as an extractant solvent and sodium hexafluorophosphate (NaPF₆) as an ion-pairing agent was proposed for the preconcentration of trace levels of cadmium. In this method cadmium was complexed with O,O-diethyldithiophosphate (DDTP) and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS). ISFME is a simple and rapid method for extraction and preconcentration of metal ions from sample solutions containing a high concentration of salt. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection (3 s) and the enhancement factor were 0.07 μg L⁻¹ and 78, respectively. The relative standard deviation (R.S.D.) was obtained 2.42%. The accuracy of the method was confirmed by analyzing certified reference materials for trace elements in seawater (GBW (E) 080040 seawater). The proposed method was successfully applied for the determination of cadmium in water samples and food grade salts.     

Comparison and evaluation of cloud point extraction and low-temperature directed crystallization as preconcentration tools for the determination of trace elements in environmental samples

A comparative study between cloud point extraction (CPE) and low-temperature directed crystallization (LTDC) is presented. Trace elements (Cd, Pb, Cr, Cu, Zn, Ni and Fe) were preconcentrated by both methods from model and natural water samples and the results were evaluated with respect to extraction efficiency, accuracy, precision, sample throughput and interferences. Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were used for the final measurements. The results indicate that these extraction and preconcentration procedures ensure the required accuracy and precision for the reliable identification and quantification of trace elements in natural waters. Drawbacks of each method identified can further assist the analyst towards a better application of each method depending on the target species, the detector employed and the application intended (routine analysis, trace analysis, speciation analysis, etc.).     

Determination of Cu, Zn and Cd in water by FAAS after preconcentration by baker’s yeast (Saccharomyces cerevisiae) immobilized on sepiolite

By using the adsorbent Saccharomyces cerevisiae immobilized on sepiolite an adsorption-elution method was developed for the preconcentration of Cu, Zn, and Cd followed by flame atomic absorption spectrometry (FAAS). Recoveries were 98.3 ± 0.4% for Cu, 94.2 ± 0.3% for Zn, and 99.04 ± 0.04% for Cd at 95% confidence level obtained by the column method. The influence of sea water matrix elements on the separation of the trace elements was also assessed by using the column procedure. The breakthrough capacities were found to be 74 μmol/g for copper, 128 μmol/g for zinc and 97 μmol/g for cadmium. After optimization the proposed method was applied to the trace metal determination in sea and river water. Received: 8 June 1998 / Revised: 8 September 1998 / Accepted: 16 September 1998     

Preconcentration of copper, nickel and zinc with Amberlite XAD-16 resin

Summary An adsorption-elution and atomic absorption spectrophotometric method using Amberlite XAD-16 is proposed for the preconcentration and determination of Cu, Ni and Zn. Optimum conditions for the preconcentration were investigated. Recoveries of the elements were found to be 82.4±0.3%, 95±3% and 71±1% for Cu, Zn and Ni, respectively, at 95% confidence level. The recoveries were increased to about 99% for Cu and Ni by complexing with 1-(2-pyridylazo)-2-naphthol (PAN). The effect of Na and K on the preconcentration of trace metals has also been investigated. The method was applied to a tap water.     

The synthesis of new polymeric sorbent and its application in preconcentration of cadmium and lead in water samples

Metal determinations at low concentration levels (≤ng mL⁻¹) comprise one of most important targets in analytical chemistry. This interest also increases in different areas such as biology, medicine, environment and food samples. In spite of inherent high sensitivities obtained for electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma-mass spectrometry (ICP-MS), these techniques have some limitations depending on the concomitants. As a result, interest in preconcentration techniques still continues increasingly for trace metal determinations by flame atomic absorption spectrometry (FAAS) due to the high accuracy of this method.In this work, thioureasulfonamide resin was synthesized, characterized and applied as a new sorption material for determinations of cadmium and lead in water samples. The method is based on the sorption of Cd and Pb ions on the synthesized resin without using any complexing reagent. The optimization of experimental conditions was performed using factorial design including pH, amount of resin, contact time, first sample volume and final eluent volume. Using the experimental conditions defined in the optimization, the method was applied to the determination and preconcentration of Cd and Pb at ng mL⁻¹ level in natural water. Flame AAS was used for trace metal determinations. This method exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent and optimum pH of solution presents in acidic media. Consequently, 600- and 360-fold improvements in the sensitivity of FAAS were achieved by combining the slotted tube atom trap-atomic absorption spectrometry (STAT-FAAS) and the purposed enrichment method for Cd and Pb, respectively.     

Trends in sorption preconcentration combined with noble metal determination.

Nowadays much attention is being paid to the determination of trace amounts of noble metals in geological, industrial, biological and environmental samples. The most promising techniques, such as inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and electrothermal atomic absorption spectrometry (ETAAS) are characterized by high sensitivity. However, the accurate determination of trace noble metals has been limited by numerous interferences generated from the presence of matrix elements. To decrease, or eliminate, these interferences, the sorption preconcentration of noble metals is often used prior to their instrumental detection. A great number of hyphenated methods of noble metal determination using sorption preconcentration have been developed. This review describes the basic types of available sorbents, preconcentration procedures and preparations of the sorbent to the subsequent determination of noble metals. The specific features of instrumental techniques and examples of ETAAS, FAAS, ICP-AES, ICP-MS determinations after the sorption preconcentration of noble metals are considered. The references cited here were selected mostly from the period 1996 - 2006.     

分子印迹壳聚糖/凹土分离富集-火焰原子吸收光谱测定痕量铅

建立了用分子印迹壳聚糖/凹凸棒石（MICA）分离富集-火焰原子吸收光谱（FAAS）测定痕量铅的新方法。 在动态吸附条件下,系统地研究了溶液pH值、流速、洗脱条件和干扰离子对痕量铅分离富集的影响;在pH=4.5,上样流速为0.60 mL/min的条件下,铅能被MICA定量富集;吸附的铅可用1.0 mol/L HCl-0.1 mol/L 甲基异丁酮的乙醇溶液在流速为0.96 mL/min条件下完全洗脱;在优化条件下,MICA对铅的动态吸附容量为36.78 mg/g。 线性范围为0～1.28 mg/L,r=0.999 7,检出限（3σ,n=11）为0.73 μg/L,相对标准偏差为1.69%(n=6,ρ=0.08 mg/L),回收率在98.7%～101.4%之间。 该方法操作简便、线性关系良好、灵敏度和精密度高,应用于实际水样中痕量铅的测定,结果满意。     

Flow Injection Semi-online Preconcentration Graphite Furnace Atomic Absorption Spectrometry for Determination of Cadmium, Copper and Manganese

IntroductionGraphite furnace atomic absorption spectrome-try (GFAAS) is one of the most sensitive tech-niques for the determination of various elementswith detection limits in the range ofμg/ L to ng/ L.Despite the impressive detection power of the tech-nique,GFAAS can tbe routinely used to make di-rect analysis of some real samples with complexcomposition[1] . This is due to the matrix interfer-ence and/ or insufficient detection power. Conse-quently,separation and preconcentration proc…     

Determination of Cu, Zn and Cd in water by FAAS after preconcentration by baker’s yeast (Saccharomyces cerevisiae) immobilized on sepiolite

By using the adsorbent Saccharomyces cerevisiae immobilized on sepiolite an adsorption-elution method was developed for the preconcentration of Cu, Zn, and Cd followed by flame atomic absorption spectrometry (FAAS). Recoveries were 98.3 ± 0.4% for Cu, 94.2 ± 0.3% for Zn, and 99.04 ± 0.04% for Cd at 95% confidence level obtained by the column method. The influence of sea water matrix elements on the separation of the trace elements was also assessed by using the column procedure. The breakthrough capacities were found to be 74 μmol/g for copper, 128 μmol/g for zinc and 97 μmol/g for cadmium. After optimization the proposed method was applied to the trace metal determination in sea and river water.     

Determination of trace silver in environmental samples by room temperature ionic liquid-based preconcentration and flame atomic absorption spectrometry

We report on a new method for preconcentration of silver ion at trace level in environmental samples, and its subsequent determination by flame atomic absorption spectrometry (FAAS). The room temperature ionic liquid (RTIL) 1-butyl-3-methylimidazolium hexafuorophosphate and the chelator 5-(4-dimethylaminobenzylidene)-rhodanine were used for extraction. Ag(I) was back-extracted from the organic phase into thiosulfate solution and then determined via FAAS. The effects of pH, concentration of chelating agent, extraction time and temperature, amounts of ionic liquid, ionic strength and potentially interfering ions were studied. Under optimized conditions, the enhancement factor is 30 was achieved. The detection limit (3???) is 0.28?ng?mL^?1, and the relative standard deviation is 4.1% for 7 replicate determinations at 5?ng?mL^?1 of Ag(I). The method was validated by analysis of certified reference materials and applied to the determination of Ag(I) in environmental samples with satisfactory results.

Determination of lead traces in water and liqueurs by derivative atom trapping flame atomic absorption spectrometry

 A new method for the direct determination of lead traces using derivative atom trapping flame atomic absorption spectrometry (DAT-FAAS) with an improved water-cooled stainless steel trapping equipment in an air-acetylene flame was investigated. The optimum conditions concerning the sensitivity were studied. For a 1 min collection, the characteristic concentration (given as derivative absorbance of 0.0044) and the detection limit (3s) were 1.4 ng/mL and 0.27 ng/mL, respectively. This is 361 and 74-fold better than those of the conventional flame atomic absorption spectrometry (FAAS) and comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). The detection limit and sensitivity of DAT-FAAS for a 3 min collection time were 2 and 3 orders of magnitude higher than those of conventional FAAS. The present method was applied to the determination of lead in water and liqueur samples with a recovery range of 94–108% and a relative standard deviation of 3.5–5.6%. Received: 10 January 1996/Revised: 9 December 1996/Accepted: 20 December 1996     

环境水样中痕量铅的中孔分子筛Al-MCM-41分离富集-火焰原子吸收法测定

建立了中孔分子筛Al-MCM-41分离富集-火焰原子吸收光谱法测定水样中痕量铅的新方法。采用扫描电镜(SEM)、红外光谱(IR)等检测方法对自制的中孔分子筛Al-MCM-41吸附材料进行了表征,优化了中孔分子筛Al-MCM-41对试液中痕量铅的吸附和解吸条件。在pH5.5时,室温振荡20 min,中孔分子筛Al-MCM-41能定量、快速吸附水中的痕量Pb2+,其静态饱和吸附容量为2.5 mg/g。吸附在中孔分子筛Al-MCM-41上的Pb2+可用0.2 mol/L EDTA完全洗脱。其他金属离子共存不影响铅的测定。洗脱铅后的吸附材料经再生可循环使用10次以上。Pb2+的线性范围为0.5~30 mg/L,富集后方法检出限(3σ)为0.05μg/L,对5 mg/L的Pb2+溶液平行测定11次,相对标准偏差为1.2%,加标回收率为98%~104%。该方法用于环境水样中铅的测定,结果满意。     

Graphite Furnace Atomic Absorption Spectrometry Determination and On-line Preconcentration of Palladium

Palladium was determined in pharmaceuticals by direct graphite furnace atomic absorption spectrometry (GFAAS) method. The detection limit was 0.1 μg/g in 5% solution; the recovery of 0.5–2.0 μg/g Pd spike was close to 100%. The flow injection GFAAS method was worked out using oxime and iminodiacetic acid ethyl cellulose (IDAEC) microcolumns for preconcentration of Pd in aqueous and 50% methanol solutions. The optimal pH range for preconcentration was 2–5. At 20-fold enrichment the detection limits for Pd were 0.39 μg/liter for oxime cellulose and 0.42 μg/liter for IDAEC.