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.

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.

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.

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.

A novel method for the determination of trace copper in cereals by dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with flame atomic absorption spectrometry

A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient（r） of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.

Determination of Copper by Flame Atomic Absorption Spectrometry after Preconcentration with Activated Carbon Impregnated with a New Schiff Base

A simple and reliable method for the extraction and determination of trace amounts of copper（Ⅱ） ions using activated carbon （AC） impregnated by a new Schiff base 5-[（4-heptyloxyphenyl）azo]-N-（4-propyloxyphenyl）-salicylaldimine （HPPS） and atomic absorption spectrometry is presented. Recovery efficiency and the influence of pH value, volume of sample solution, effect of different eluents, and interfering ions were evaluated. The limit of detection （3σ） was 2.62 ng.mL^-1 and the relative standard deviation （n=10） was 1.5%. Under optimum conditions, the copper ions were concentrated 25 fold using 250 mL of sample solution and 10 mL of eluent. This procedure has been successfully applied to the determination of copper in different water samples.

Determination of Manganese in Tri Calcium Phosphate (TCP) by Atomic Absorption Spectrometry

Tricalcium phosphate Anhydrous Powder typically contains less than 10 ppm (mg/Kg) (w/w) manganese. This level can be determined utilizing Flame Atomic Absorption Spectrometer (AAS) and standard based on known standards. A number of analytical methods are presently used for the analysis of metals in the biochemical. The instrumental techniques available are Inductively Coupled Plasma (ICP/MS), X-Ray Fluorescence, UV-VIS Spectrophotometry, and Atomic Absorption Spectrometry. Flame AA has gained widespread acceptance as an analytical technique and is used for many applications. In this study, we have determined the amount of manganese metal present in Tricalcium Phosphate (TCP) using Flame Atomic Absorption Spectrophotometer. The method has high precision and accuracy. The percent recovery was found to be 99.8% for spiked sample. The results meet the requirement.

FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry （FAAS）. The Cu^2＋ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL-0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2. lng/mL in the original solution （3σ, n=9）. Determination of copper in standard ions showed that the proposed method has good accuracy （recovery was more than 95%）. The method was successfully applied for recovery and determination of copper in cereals food samples

Flow-Injection Flame Atomic Absorption Determination of Hexavalent Chromium with On-Line Preconcentration on an Anion Imprinted Polymer

A flow injection preconcentration system for the flame atomic absorption spectrometric determination of hexavalent chromium has been developed. The method employs on-line preconcentration of Cr(VI) on a minicolumn packed with Cr(VI)-imprinted poly(4-vinyl pyridineco-2-hydroxyethyl methacrylate) placed into a flow injection system. Hexava-lent chromium was eluted with a small volume of diluted hydrochloric acid into the nebulizer-burner system of a flame atomic absorption spectrometer. An enrichment factor of 550 and a 3σ detection limit of 0.04 μg·L-1 along a sampling frequency of 4 h-1 at a sample flow rate of 3.5 mL·min-1. The relative standard deviation is 2.9% for 1 μg·L-1 Cr(VI) (n = 11). The flow injection system proposed has the advantage of being simpler because the use of expensive and sophisticated instruments is avoided. Ease of use, continuous process and selectivity make this method suitable for Cr(VI) determination in different environmental samples such as sea and river waters, soils and sediments.

Preconcentration and Determination of Chromium Species Using Octadecyl Silica Membrane Disks and Flame Atomic Absorption Spectrometry

A novel and selective method for the fast determination of trace amounts of chromium species in water samples has been developed. The procedure is based on the selective formation of chromium diethyldithiocarbamate complexes at different pH in the presence of Mn（Ⅱ） as an enhancement agent of chromium signals followed by elution with organic eluents and determination by atomic flame absorption spectrometry. The maximum capacity of the employed disks was found to be （396±3） pg and （376±2） pg for Cr（Ⅲ） and Cr（Ⅵ）, respectively. The detection limit of the proposed method is 49 and 43 ng·L^-1 for Cr（Ⅲ） and Cr（Ⅵ）, respectively. The proposed method was successfully applied for determination of chromium species Cr（Ⅲ） and Cr（Ⅵ） in different water samples.

Determination of Ca,K,Mg and Fe in Four Fish Species by FAAS

A method for determining calcium （Ca）, potassium （K）, magnesium （Mg） and iron （Fe） in four fish species was opti- mized and validated. It included microwave mineralization of the samples and subsequent quantification by flame atomic absorption spectroscopy （FAAS） with Zeeman-effect background correction. Using HNO3 （65%） and H202 （33%） as extraction solutions, the optimal conditions of extraction were established as follows： 0.5 g of sample mass; microwave time program of 300 W/5 min and 600 W/5 min. The method was free of matrix interferences. The linear correlation coefficients were ≥0.9991, the recovery percentage of analytes was from 99.31% to 103.70% and the RSD （relative standard deviation） was lower than 2.06%. The detection limits obtained were 32.3, 43.2, 14.0 and 68.6ng mL^-1 for Ca, K, Mg and Fe in FAAS respectively. It is shown that the method is rapid, simple, sensitive and accurate. The method was applied to the studies of digestibility and measurement of these nutrients in samples of fish collected from Norway, Japan and China.

Preconcentration and Separation of Trace Copper in Water Samples with Nanometer-Size TiO_2 Colloid and Determination by FAAS

A new absorbent of nanometer-size TiO2 colloid for Cu（Ⅱ ） was studied in this work. The adsorption rate could reach above 99% when the pH values were at the range of 5-6. The adsorption balance time, adsorption capacities, and the eluent were investigated. A novel method of trace Cu（ Ⅱ ） preconcentration and separation with nanometer-size titanium dioxide colloid and determination by flame atomic absorption spectrometry （FAAS） was advanced. The detection limit （3a） of the method was 1.15 μg · L^-1, and the relative standard deviation （R.S.D） was 1.53% （n=6）. Environmental sample experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 95.9% and 97.8%.

TiO_2 nanotubes:A novel solid phase extraction adsorbent for the sensitive determination of nickel in environmental water samples

A novel method was developed for the sensitive determination of nickel in environmental water samples by using TiO2 nanotubes, a new nanomaterial, as solid phase extraction absorbent. In general, TiO2 nanomaterials were often used for catalytic degradation of pollutants in environmental field, and only a very few application in environmental analytic chemistry. In present work, TiO2 nanotubes was firstly used for the enrichment of nickel and the factors would influence the preconcentration performance were optimized. Under the optimal conditions, TiO2 nanotubes exhibited its good enrichment capacity for nickel and the detection limit of the proposed method was 1 ng· mL^-1. The proposed method was validated with real water samples, and excellent results were obtained with the spiked recoveries in the range of 94.4-99.2%, respectively.

STUDY ON THE ADSORPTION BEHAVIOR OF Pb(Ⅱ) ON NANOMETER ATTAPULGITE BY FAAS

The adsorptive behavior of nanometer attapulgite modified by acid to Pb（Ⅱ） was investigated by flame atomic absorption spectrometry （FAAS） in this paper. The mainly effect parameters ott the adsorptive efficiency of Pb（Ⅱ）, such as the acidity of the solution, the amount of attapulgite, oscillation time and static time were studied. Also the influencing factors of the recovery efficiency of Pb（Ⅱ）, including the concentration of hydrochloric acid, the volume of hydrochloric acid, oscillation time and static time were investigated. The adsorptive capacity of Pb（Ⅱ） on nanometer attapulgite was 26.5mg/g and the adsorptive capacity of first cycle and second cycle regenerated nanometer attapulgite were 26.5mg/g and 26.3mg/g, respectively. The results obtained indicated that the regenerated effect was good.

A magnetic adsorbent based on salicylic acid-immobilized magnetite nano-particles for pre-concentration of Cd(II) ions

In this research,an eco-friendly magnetic adsorbent based on Fe_(3)O_(4)/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method.The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy,X-ray diffraction,and Fourier transform infrared spectroscopy.The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II)ions from synthetic solutions.Some experimental factors affecting the extraction efficiency were investigated and optimized.Following elution with acetic acid(pH 3.5),the pre-concentrated analyte was quantified by flame atomic absorption spectrometry.In optimal conditions,a linear calibration graph was achieved in the concentration range of 0.2–30 ng·mL^(−1) with a determination coefficient(R^(2))of 0.9953.The detection limit,the enhancement factor,inter-and intra-day relative standard deviations(for six consecutive extractions at the concentration level of 10 ng·mL^(−1))were 0.04 ng·mL^(−1),100,2.38%and 1.52%,respectively.To evaluate the accuracy of the method,a certified reference material(NIST SRM 1643e)was analyzed,and there was a good agreement between the certified and the measured values.It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8%and 103.2%.

Use of 2-(tert-butoxy)-N-(3-carbamothioylphenyl)acetamide and graphene oxide for separation and preconcentration of Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ) and Zn(Ⅱ) ions in different samples

A simple and selective method using a column packed with graphene oxide（GO） as a solid phase extractant has been developed for the multi-element preconcentration of Fe（Ⅲ）,Ni（Ⅱ）,Cu（Ⅱ） and Zn（Ⅱ）ions prior to flame atomic absorption spectrometric determinations.The method is based on the sorption of mentioned ions on synthesized GO using 2-（tert-butoxy）-N-（3-carbamothioylphenyl）acetamide as a chelating agent.Several parameters on the extraction and complex formation were optimized.Under the optimized conditions（pH 6,flow rate 9 mL/min）,metal ions were retained on the column,then quantitatively eluted by HNO3solution（5 mL,3.0 mol/L）.The preconcentration factor was calculated as250.The detection limits for the analyte ions of interest were found in the range of 0.11 ng/mL（Ni2＋） to0.63 ng/mL（Cu2＋）.The column packed with GO was adequate for metal ions separation in matrixes containing alkali,alkaline earth,transition and heavy metal ions.

Ultrasound-assisted emulsification solidified floating organic drop microextraction for the determination of trace amounts of copper in water samples

A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorption spectrometry,for the extraction and determination of trace copper in water samples.1-(2-Pyridylazo)-2-naphthol(PAN)was used as chelating agent.Microextraction efficiency factors(including extraction solvent type,extraction volume,time,temperature,and pH),the amount of the chelating agent,and salt effect were investigated and optimized.Under the optimum extraction conditions,figures of merit of the proposed method were evaluated.The calibration graph was linear in the range of 20–600 mg·L^(–1)with a detection limit of 0.76 mg·L^(–1).The relative standard deviation(R.S.D)for ten replicate measurements of 20 and 400 mg·L^(–1)of copper was 3.83%and 2.65%,respectively.Finally,the proposed method was applied to tap water,river water,and sea water,and accuracy was assessed through the analysis of certified reference water or recovery experiments.