Determination of Mecruy at Trace Level in Natural Water Samples by Hydride Generation Atomic Absorption Spectrophotometry after Cloud Point Extraction Preconcentration

A method for the determination of trace mercury in water samples by hydride generation atomic absorption spectrophotometry after cloud point extraction was proposed in the present work. The effects of pH, concentration of surfactant, and equilibration time on cloud point extraction were discussed. The enhancement factor of 20 and the detection limit of 0.039 μg/L were obtained for mercury with relative standard deviation of 4.8% （n = 11）.

Concentration determination of gold nanoparticles by flame atomic absorption spectrophotometry

While engineered nanoparticles are widely used and maybe eventually released into the environment,natural nanoparticles are also commonly found in the Earth system.Nanoparticles may critically affect the geochemical migration of associated elements and pose potential threats to the ecological environment.It is necessary to establish an accurate and reliable method for measuring the concentration of nanoparticles.AAS is one of the most commonly used methods for the concentration determination of nanoparticles.However,till now,there has been no systematic report on how experimental variables affect AAS measurements.In this study,we used gold nanoparticles(AuNPs) as an example and studied the influences of a list of factors on the concentration determination of AuNPs by AAS,including digestion method,ionization interference,acidic medium,background correction method,and organic matter.We demonstrate that all these factors may have varying degrees of influence on the measured gold concentrations.When the gold colloid is digested at room temperature for more than 8 h or at 60℃ for more than 2 h,and the system contains a low concentration of organic matter,AAS can accurately measure the AuNP concentration at ppm-level.The deuterium lamp background deduction method is not recommended to use for samples with lower gold concentrations.

Separation/Enrichment of Copper and Silver Using Titanium Dioxide Nanoparticles Coated with Poly-Thiophene and Their Analysis by Flame Atomic Absorption Spectrophotometry

We report on the use of titanium dioxide nanoparticles (NPs) coated with poly-thiophene for the preconcentration of copper and silverions. The NPs were prepared by first modifying the surface of TiO2 NPs with vinyl groups and then copolymerizing them with vinyl thiophen. The resulting TiO2-polythiophene core-shell NPs were characterized by thermogravimetry, differential thermal analysis, scanning electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The experimental conditions such as pH value, adsorption and desorption time, type, concentration and volume of the eluent, break through volume, and effect of potentially interfering ions were optimized. The ions were then desorbed with hydrochloric acid and determined by FAAS. The limits of detection are 0.4 and 1.2 μg·L_1 for Cu(II) and Ag(I), respectively, and recoveries and precisions are >98.0%

Content Determination of Trace Elements in Several Vegetables by Atomic Absorption Spectrophotometry

The contents of Mn,Zn and Cu,three essential trace elements for human body,in Laminaria japonica,Auricularia auricula( L. ex Hook.) Underwood,Porphyra,Cucurbita pepo L.,Spinacia oleracea L. and Coriandrum sativum were determined by atomic absorption spectrophotometry. Vegetable samples were processed by wet digestion. The results showed that among the six vegetables,Mn had the highest content in A. auricula( 26. 60 μg/g) and the lowest content in C. pepo( 1. 22 μg/g); Zn had the highest content in Porphyra( 38. 07 μg/g)and the lowest content in L. japonica( 10. 32 μg/g); and Cu had the highest content in Porphyra( 10. 35 μg/g) and the lowest content in S. oleracea( 0. 61 μg/g). Each determination was repeated five times. The value of RSD was less than 10%,indicating high accuracy.

Evaluation of Analytical Procedures in the Determination of Trace Metals in Heavy Crude Oils by Flame Atomic Absorption Spectrophotometry

In the present work, four trace metals, V, Ni, Cu and Fe, have been determined in five crude oil samples of Eastern Baghdad area, Iraq by flame atomic absorption spectrophotometry. The crude oils are characterized with API gravity values in the range, 25 - 15. The V/Ni ratios for the studied crudes were in the range 3.7 to 5.4 and indicated a typical of the sapropelic-type organic matter. The Ni and V contents were correlated with API gravity where an increase of metal contents with the decrease in the API values could be observed. The plots of V and Ni versus sulfur indicated linear correlation. This is attributed to the increase of porphyrinic structures of the metals. The method of direct dilution (DD) with organic solvent and the standard addition (SA) were evaluated as compared with standard dry ashing-acid dissolution (DA). In most cases the DD method gave V and Ni concentrations that are higher than DA and for the heavier crude oil (API = 15) the DD results were significantly smaller than those of the DA method. The SA method can be a good solution to determine the trace metals in heavy crude oils provided that the addition must not exceed the levels of the metal concentration in the diluted samples.

Determination of Lead in Lime-preserved Egg by Microwave Digestion and Flame Atomic Absorption Spectroscopy

[Objectives] To establish a method for determining the lead content in lime-preserved eggs, to provide a theoretical basis for the quality control of production enterprises and the sampling and testing of supervision departments. [Methods] The lead content in lime-preserved eggs was measured by the microwave digestion and flame atomic absorption spectroscopy. [Results] The method had a correlation coefficient of r2=0.998 in the injection concentration range of 0-4 mg/L. The detection limit of the method was 0.008 2 mg/kg. In the range of 0.2 to 1.0 mg/kg addition concentration, the recovery rate of the method was 92.5%-108.0%, and the relative standard deviation(RSD) was <5%. [Conclusions] This method is accurate and reliable, simple and efficient, and is suitable for the detection of lead in lime-preserved eggs.

Determination of Chromium and Zinc in Soil by Microwave Digestion and Flame Atomic Absorption Spectrometry

[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.

Rapid Determination of Cd in Squilla by Mixed Acid Leaching-flame Atomic Absorption Method

[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 （5：1） and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.

Determination of Five Metallic Elements in Guoshangye from Guizhou by Microwave Digestion-flame Atomic Absorption Spectrometry

In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu- oshangye. The sample was subjected to microwave digestion with HNO3 and H2O2, and detected by the standard curve method. The results showed that Guoshangye contained abundant trace elements which rates of these trace elements were in the curacy and satisfactory. were necessary for human. The recovery range of 96%-103%. The method is ac-

Determination of Trace Elements in Potatoes by Flame Atomic Absorption Spectrometry

[Objective] This study aimed to analyze the contents of trace elements in potatoes from different production areas in Qinghai Province. [Method] By flame atomic absorption spectrometry （FAAS）, the contents of various trace elements in potatoes were determined. [Result] Potatoes contain abundant trace elements such as Cu, Zn, Fe, Mn, Ca, K and Mg. To be specific, the contents of Ca, K and Mg were relatively high. [Conclusion] By using FAAS, the relative standard deviation was 1.17%-2.75% and the recovery rate was 97%-99.5%, indicating accurate and reli-able results with high precision.

Determination of Ultratrace Amounts of Copper(Ⅱ) in Water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry （ETAAS） after cloud point extraction （ CPE ）. 1-（ 2-Pyridylazo ） -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu （ Ⅱ ）. This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.

Determination of total arsenic by photo-decomposition of organoarsenic compounds and hydride generation electrothermal atomic absorption spectrometry

A method was developed for the determination of total arsenic concentration in less than ng/ml level by decomposition of organoarsenicals using photo -oxidation combined with in situ trapping of arsenic hydride on a palladium coated graphite tube with subsequent atomization and detection by AAS. The organoarsenicals include monomethylarsenic, dimethylarsenic, arsenobetaine, arsenocholine, o -aminobenzenarsenate and p -aminobenzenarsenate. The method is simple and sensitive. Detection limit was obtained from different arsenic compounds over the range from 0. 058 to 0.063 ng/ml as As (based on three times of the standard deviation of 10 blank measurements) and the relative standard deviations for ten replicate measurements were from 2.0 to 3.8%. The calibration curves of arsenic compounds including inorganic and organic arsenicals were linear over the range from 0.1 to 3.0 ng/ml as As. The recommended method has been applied to the determination of total arsenic in tap and lake water samples at ng/ml levels.

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.

Determination of Trace Amounts of Nickel (Ⅱ) by Graphite Furnace Atomic Absorption Spectrometry Coupled with Cloud Point Extraction

A new method based on the cloud point extraction（CPE） for separation and preconcentration of nickel（Ⅱ） and its subsequent determination by graphite furnace atomic absorption spectrometry（GFAAS） was proposed, 8-hydroxyquinoline and Triton X-100 were used as the ligand and surfactant respectively. Nickel（Ⅱ） can form a hy-drophobic complex with 8-hydroxyquinoline, the complex can be extracted into the small volume surfactant rich phase at the cloud point temperature（CPT） for GFAAS determination. The factors affecting the cloud point extraction, such as pH, ligand concentration, surfactant concentration, and the incubation time were optimized. Under the optimal conditions, a detection limit of 12 ng/L and a relative standard deviation（RSD） of 2.9% were obtained for Ni（Ⅱ） determination. The enrichment factor was found to be 25. The proposed method was successfully applied to the determination of nickel（Ⅱ） in certified reference material and different types of water samples and the recovery was in a range of 95%―103%.

On-line Preconcentration of Trace Nickel from Electrolytic Manganese Using Minicolumn Packed Activated Carbon for Electrothermal Atomic Absorption Spectrometry

The online flow injection preconcentration and electrothermal atomic absorption spectrometry method were used for the determination of trace nickel in electrolytic manganese samples by sorption on a conical minicolumn packed with activated carbon at pH 9.0. The nickel was eluted from the minicolumn with 10%(v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10mL was obtained. The detection limit (DL) of nickel with the use of the preconcentration method was 13ng·g -1in the original solid sample. The precision for 10 replicate determinations at 150ng·g -1 nickel concentration was 5.2% relative standard deviation (RSD). The calibration graph was linear with a correlation coefficient of r=0.9996 up to concentration of 660ng·g -1 nickel.

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Determination of Iron in Layered Crystal Sodium Disilicate and Sodium Silicate by Flame Atomic Absorption Spectrometry with Boric Acid as a Matrix Modifier

The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry （FAAS） were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.

Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

Determination of Trace Iron in High Purity Sodium Fluoride by Graphite Furnace Atomic Absorption Spectrometry

A method is described for the direct determination of iron in high purity sodium fluoride using graphite furnace atomic absorption spectrometry. Interferences caused by the matrix are investigated. It is shown that the ashing temperature can be increased to 1 400°C and matrix interferences eliminated, the sensitivity of iron increased in 1. 27 fold by the addition of nickel nitrate. The method is applied to the determination of iron in sodium fluoride and satisfactory results are obtained.