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1.
The paper presents a novel method for the separation/enrichment of Hg2+ using microcrystalline thymolphthalein loaded with ternary association complex prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of KI and dodecyl trimethyl ammonium bromide (DTAB) and thymolphthalein, various salts and acidity etc. on the enrichment yield of Hg2+ have been investigated to select the experimental conditions. The results showed that in the presence of 1.0 g NaCl, when the dosage of 0.1 M KI solution was 1.50 mL and 5.0 × 10−3 M dodecyl trimethyl ammonium bromide (DTAB) solution was 1.50 mL respectively, the water‐insoluble ternary association complex of (DTAB)2(HgI4) which produced by Hg2+ and I, DTAB cation (DTAB+) was quantificationally absorbed on the surface of microcrystalline thymolphthalein Therefore, Hg2+ was separated completely from Zn2+, Mn2+, Ni2+, Co2+, Fe3+, Al3+, Pb2+, Bi3+ and Cr3+ etc. by contolling acidity. The possible enrichment mechanism of Hg2+ was deduced. The proposed method has been successfully applied to the determination of Hg2+ in the sample of industrial waster water, and the results agreed well with the dithizone method. The recoveries were 94.5%∼106.5%, and the RSD was 2.0%∼2.8%.  相似文献   

2.
The paper presents a novel method for the flotation separation of Cu2+ using microcrystalline adsorption system prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of NH4SCN and octadecyl trimethyl ammonium bromide (OTMAB), various salts on the flotation yield of Cu2+ have been investigated to select the optimum experimental conditions. The possible flotation separation mechanism of Cu2+ was discussed. The results showed that under the optimum conditions, octadecyl trimethyl ammonium bromide cation (OTMAB+) reacted with SCN to produce the microcrystalline matter (Ms‐M) of (OTMAB+·SCN), the water‐insoluble ternary association complex of [Cu(SCN)4] (OTMAB)2 which produced by Cu2+ and SCN, OTMAB+ was quantificationally adsorbed on the surface of Ms‐M of (OTMAB2+·SCN) and was floated above water phase, the liquid‐solid phases were formed with clear interface. In this condition, K+, Na+, Ca2+, Mg2+, Al3+, Fe2+, Mn2+, Ni2+, Cd2+ and Co2+ could not be floated. Therefore, Cu2+ was separated completely from the above metal ions. A new method of determination of trace copper by flotation separation was established. The proposed method has been successfully applied to the determination of Cu2+ in plating waster water, and the results agreed well with AAS method. The recoveries were 93.3%~107.8%, and the RSD was 1.9%~2.1%.  相似文献   

3.
The paper presents a novel method for the flotation separation of Bi3+ using microcrystalline adsorption system prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of KI and dodecyl trimethyl ammonium bromide (DTMAB), various salts and acidity etc. on the flotation yield of Bi3+ have been investigated to select the optimum experimental conditions. The possible flotation separation mechanism of Bi3+ was discussed. The results showed that under the optimum conditions, dodecyl trimethyl ammonium bromide cation (DTMAB+ ) reacted with I? to produce themicrocrystalline matter (Ms‐M) of (DTMAB+·I?), the water‐insoluble ternary association complex of (DTMAB)3[BiI6] which produced by Bi3+ and I?, DTMAB+ was quantificationally adsorbed on the surface of Ms‐M of (DTMAB+·I?) and was floated above water phase, the liquid‐solid phases were formed with clear interface. In this condition, K+, Na+, Ca2+, Mg2+, Co2+, Ni2+, Mn2+, Zn2+, Fe2+ and Al3+ could not be floated. Therefore, Bi3+ was separated completely from the above metal ions. A new method for flotation separation and determination of bismuth using microcrystalline adsorption system was established. The proposed method has been successfully applied to the determination of Bi3+ in bismuthiferous drug samples, and the results agreed well with those obtained by pharmacopoeia method. The recoveries were 94.1%~106.8%, and the RSD was 1.5%~2.3%.  相似文献   

4.
ALI Moghimi 《中国化学》2007,25(5):640-644
A fast and simple method for preconcentration of Ni^2+, Cd^2+, Pb^2+, Zn^2+, Cu^2+ and Co^2+ from natural water samples was developed. The metal ions were complexed with sodium diethyldithiocarbamate (Na-DDTC), then adsorbed onto octadecyl silica membrane disk, recovered and determined by FAAS. Extraction efficiency, influence of sample volume and eluent flow rates, effects of pH, amount of Na-DDTC, nature and amount of eluent for elution of metal ions from membrane disk, break through volume and limit of detection have been evaluated. The effect of foreign ions on the percent recovery of heavy metal ions has also been studied. The limit of detection of the proposed method for Ni^2+, Cd^2+, Pb^2+, Zn^2+, Cu^2+ and Co^2+was found to be 2.03, 0.47, 3.13, 0.44, 1.24 and 2.05 ng·mL^-1, respectively. The proposed (DDTC) method has been successfully applied to the recovery and determination of heavy metal ions in different water samples.  相似文献   

5.
李全民  吴宏伟  刘国光 《化学学报》2006,64(11):1169-1172
建立了一种利用修饰有结晶紫(CV)的微晶酚酞作为固态吸附剂分离富集溶液中痕量Zn(II)的新方法, 富集后的Zn(II)含量可直接用光度法测定. 控制一定条件, Zn(II)能与常见阳离子Ni(II), Cd(II), Al(III), Ca(II), Mg(II), Co(II), Mn(II), Cu(II), Pb(II), Fe(III)等完全分离, 且富集时基本不受, , Br, Cl, I,等阴离子影响. 微晶酚酞对Zn(II)的吸附容量为25.8 mg/g; 富集因数可达200倍, 回收率在97.7%~102%之间, RSD小于2.7%. 该方法已成功应用于实际水样中Zn(II)的富集测定, 结果令人满意.  相似文献   

6.
《Analytical letters》2012,45(12):1987-1998
Abstract

The present work describes a novel method for cadmium preconcentration and separation with microcrystalline phenolphthalein. Phenolphthalein as an extractant modified by crystal violet was originally applied to cadmium extraction from aqueous solution. Cadmium(II) as CdI3 ? and CdI4 2? can associate with the cationic crystal violet (CV+) forming water‐insoluble ion‐association complexes (CdI3 ?) · (CV+) and (CdI4 2?) · (CV+)2, which are quantitatively adsorbed on microcrystalline phenolphthalein over the pH range from 1.0 to 6.0. All experimental parameters necessary for successful preconcentration and separation have been investigated and optimized. The study shows that common metal ions, such as Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III), cannot interfere with cadmium extraction in this microcrystalline system by controlling acidity. The extraction can be accomplished in 15 min. The interaction between CdI3 ?and CdI4 2? and CV+ plays an important role in the extraction process. The reported method was successfully applied to the preconcentration and separation of cadmium in synthetic samples and real samples with satisfactory results. The results proved that it is an efficient and attractive technique for cadmium preconcentration and separation at trace level.  相似文献   

7.
In the present work, ion-imprinted interpenetrating polymer network (IPN) gels were prepared by free radical/cationic hybrid polymerisation of acrylamide (AAm) and 1,4-butanediol vinyl ether (BVE). These gels were respectively used for separation of Cu2+, Ni2+ and Zn2+ ions in natural water samples. Experimental conditions for effective adsorption of metal ions were optimised with respect to different experimental parameters by column procedures in detail. The optimum pH value for the adsorption of Cu2+, Ni2+ and Zn2+ ions on these sorbents was 6.0. Complete elution of the adsorbed metal ions from the sorbent was carried out using 1.0 mol/L of HCl solution. The optimum sample flow rate and eluent flow rate were, respectively, 1.0 and 0.3 mL/min. Common coexisting ions did not interfere with the separation and determination of the target ions. The accuracy of the proposed method was validated by analysis of the standard reference material (GBW 08301, river sediment). The measured contents of metal ions in the reference material were in good agreement with the certified values. The presented method was successfully applied for the determination of Cu2+, Ni2+ and Zn2+ ions in three different water samples (well water, seawater and waste water).  相似文献   

8.
A simultaneous preconcentration and separation method for determination of trace amount of dissolved Ag+, Pb2+ and Pd2+ ions by modified octadecyl silica membrane disks with DBzDA18C6 was developed. The adsorbed metal complexes were eluted from disk with 10?mL of 4?M KCl and determined by flame atomic absorption spectroscopy. Several parameters such as anion effect, pH of sample solution, type of eluent, amount of ligand, sample and elution flow rate were evaluated. The effect of diverse ions on preconcentration was also investigated. A precocentration factor of 110 can easily be achieved depending on the volume of the sample. For 100?mL of the solution the linear dynamic rang were found to be 30–1000, 140–6000, 60–900?μg?l?1 for Ag+, Pb2+ and Pd2+, respectively. Based on three standard deviation of the blank the detection limit was obtained as 1.8, 8.0 and 4.2?μg?L?1 for Ag+, Pb2+, Pd2+, respectively. The formation constants of Ag+ and Pb2+ ions with DBzDA18C6 at 25?°C were determined from the molar conductance–mole ratio data. This method was applied for the determination of Ag+, Pb2+ and Pd2+ in environmental water, tea and soil samples.  相似文献   

9.
A simple, highly sensitive, accurate and selective method for the determination of trace amounts of Ni2+ ions in water samples is proposed. The method is based on the separation and preconcentration of Ni2+ on an octadecyl-bonded silica (ODBS) membrane disk modified by a recently synthesized Schiff’s base N,N′-bis (3-methylsalicylidene) ortho phenylene diamine (MSOPD) at pH 7. The synthesis of this extractant ligand is also described. The retained nickel on the membrane was eluted with 2×5 ml 0.5 M HNO3 and measured by flame atomic absorption spectrometry (FAAS) at 232.0 nm. The extraction efficiency and the influence of the type and least amount of eluent for the stripping of Ni2+ from the disks, pH, flow rates of sample solution and eluent, amount of MSOPD, effect of other ions, and breakthrough volume were evaluated. The maximum capacity of the membrane disks modified by 3 mg of MSOPD was found to be 146±4 μg Ni2+. The 3σ limit of detection of the method was 30 ng per 1000 ml and also an enrichment factor of 250 was obtained. The proposed method has been applied to the determination of nickel in several water samples with satisfactory results.  相似文献   

10.
Li Q  Ouyang R  Liu G 《Talanta》2004,64(4):906-911
A new method for cadmium separation and concentration with microcrystalline phenolphthalein modified by crystal violet (CV) was developed in the paper. In the presence of potassium iodide (KI) and CV, cadmium are quantitatively absorbed on microcrystalline phenolphthalein in the pH range 1.0-6.0 as the forms of water-insoluble ion-associated complexes (CdI3)·(CV+) and (CdI42−)·(CV+)2. Effect of different parameters such as phenolphthalein amount, stirring time, the concentration of CV and KI, various salts and metal ions was studied in detail. During the present study, a significant enhancement of the extraction of cadmium was observed. Cd(II) can be completely separated from Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III) in this microcrystalline system and well concentrated without the interference of these metal ions at high level. The possible reactive mechanism of cadmium concentration has been discussed. Analytical results obtained by this new method were very gratifying.  相似文献   

11.
A flow injection on-line coprecipitation preconcentration system with diethyldithiocarbamate (DDTC) chelate of copper used as the coprecipitate carrier was coupled with flame atomic absorption spectrometry (FAAS) for the determination of trace silver. Silver was on-line coprecipitated with DDTC-Cu(II) in 0.5 moL · L−1HCl, and the precipitate was collected in a knotted reactor. The precipitate was then dissolved by isobutyl methyl ketone and transported directly into the nebulizer–burner system of a flame atomic absorption spectrometer. A detection limit (3ς) of 0.6 μg · L−1was achieved for a loading period of 30 s, a relative standard derivation of 2.0% was obtained for 11 determinations of 20 μg · L−1Ag(I). Interference-free levels were 10 mg · L−1for Cd2+, 50 mg · L−1for Cu2+, 50 mg · L−1for Mn2+, 25 mg · L−1for Ni2+, 100 mg · L−1for Pb2+, 50 mg · L−1for Zn2+, 500 mg · L−1for Fe3+, and 2000 mg · L−1for Fe2+reduced from Fe3+by ascorbic acid. The developed method has been successfully applied to the determination of trace amount of silver in geological samples.  相似文献   

12.
Chelating resins based on biopolymers, specifically cellulose, offers a green analytical method for determination of metal ions at trace levels present in various samples. It offers a fast, accurate and simple method for separation and pre-concentration of metal ions at low concentrations, prior to their determination by instrumental method. Cellulose based chelating resin (CELL-GLY) has been synthesised by immobilising glycine on it. CELL-GLY was used for the determination of trace amounts of Cu2+ and Ni2+ from aqueous solutions before their determination by FAAS. The preparation of CELL-GLY involves simple steps, based on natural and easily available biopolymer cellulose, which makes its use as chelating resin is a green method. The Cu2+ and Ni2+ can be quantitatively recovered from the CELL-GLY in the pH range 4.8–6.9 and 6.9-7.8 respectively with a recovery of more than 95% for each of these metal ions. Recovery of these metal ions using CELL-GLY was quantitative up to 35 °C. The detection limits for copper and nickel by FAAS were 1.20 ppb and 1.40 ppb, respectively. The method was successfully employed for the determination of trace amounts of Cu2+ and Ni2+ in various samples.  相似文献   

13.
A series of macroporous dithiocarbamate chelate resins, III and V, and an oxidized resin, VI, with high adsorption capacity were prepared. The influence of various reaction conditions of amination, dithiocarboxylation, and oxidation were examined. The structure and the conversion of functional groups of resins were confirmed by IR spectra and elemental analysis. The adsorption capacities of Resin II for Hg2+, Cu2+, Zn2+, and Cd2+ are 4.40, 2.44, 1.77, and 1.36 mmol/g, respectively. The adsorption capacities of Resins V and VI for Cu2+. Zn2+, Ni2+, Co3+, Ag+, Hg2+, Cd2+, Pb2+, and Au3+ are 4.07–0.51 and 3.81–0.59 meq ion/g, respectively. The adsorption rate and the influence of pH on the adsorption percentage of the resins for metal ions were examined. Noble metal, transitional metal, and heavy metal ions can be quantitatively adsorbed by the resins. The adsorbed Cu2+, Pb2+, Cd2+, Co3+, and Ni2+ can be quantitatively eluted with 5N HNO3, and the presence of large amounts of Ca2+, Mg2+, Fe3+, and Al3+ did not interfere.  相似文献   

14.
《Analytical letters》2012,45(7):1307-1324
Abstract

A simple sensitive and selective spectrophotometric method has been developed for determination of some transition metal ions. It is based on the reaction of the metal ions with excess peri-dihydroxynaphthindenone in 80% v/v ethyl alcohol-water mixture at 30°C. The colored products obtained display maximum absorption band at 560–590 nm depending upon the type of transition metal ion used, and E1 cm 1% in the range 70–480. Under the optimum conditions results with an average recovery of 96%, (mean standard deviation ±3% are obtained for 6 different transition metal ions without any significant interference from Li+, Na+, K+, Cs+, Rb+, Ba2+, Sr2+, Ni2+, Bi3+, Co2+, Mn+2, Cd+2 and Al+3. Kinetic data reveal that the reaction proceeds via a second order route (first order with respect to either the metal cation or ligand). The activation parameters and a suggested mechanism have been presented, and the nature of bonding in the solid chelate products has been verified.  相似文献   

15.
微晶蒽分离富集测定痕量铜(II)   总被引:1,自引:0,他引:1  
王旭  郑立庆  李全民 《应用化学》2011,28(10):1208-1212
建立了一种利用微晶蒽吸附分离富集环境水样中痕量Cu(Ⅱ)的新方法。 研究表明,pH=3.0时, Cu(Ⅱ)与1-(2-吡啶偶氮)-2-萘酚形成红棕色螯合物被微晶蒽定量吸附,而Pb(Ⅱ)、Mn(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Cd(Ⅱ)、Zn(Ⅱ)、Fe(Ⅲ)和Al(Ⅲ)等完全留在溶液中,从而实现Cu(Ⅱ)与它们的分离。 该方法可直接用于1 L水样中痕量Cu(Ⅱ)的分离与富集,富集倍数达200倍,回收率91.0%~104.0%, 最低检出限为0.026 μg/L;应用于不同水样中Cu(Ⅱ)的测定,结果令人满意。  相似文献   

16.
An online mercury preconcentration and determination system consisting of cold vapor atomic absorption spectrometry (CV-AAS) coupled to a flow injection (FI) method was studied. The method was developed involving the determination of ng/L levels of mercury retained on the silver wool solid sorbent. Experimental conditions such as sample volume, flow rate, stability of the column and effect of foreign ions on the determination of trace amounts of mercury were optimized. The detection limit is 3 ng/L and dynamic range 10–250 ng/L require only 50 mL of sample. The relative standard deviations (RSD) of the determinations are below 4%. The presence of common metal ions, such as K+, Na+, Cu2+, Pb2+, Fe3+, Ni2+, and Mn2+, does not interfere with the measurement of mercury by this method. The method was successfully applied to the determination of mercury in water and wastewater samples.  相似文献   

17.
Separation and determination of some common metal ions was achieved with methyl 3‐amino‐3‐(pyridin‐3‐yl)propanoate dihydrochloride (MAPP) as an ion‐pairing reagent and pyridine as a detectable counter‐ion for indirect UV detection at 254 nm. The effects of the complexing reagent and chromophore concentrations, applied voltage, and organic solvent content on the separation were investigated. The optimized separation was carried out in a running electrolyte containing 16 mM MAPP and 20 mM pyridine at pH 4.0 and was successfully applied to the qualitative and quantitative analysis of Li+, Na+, Mg2+, Ca2+, Ba2+, Ni2+, and Zn2+ in pharmaceutical vitamin preparations and various water samples.  相似文献   

18.
A method for solid phase extraction of trace metals such as Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+ using nanometer-sized alumina coated with chromotropic acid prior to determination by inductively coupled plasma atomic emission spectrometry (ICP-AES) has been developed. Various influencing parameters on the separation and preconcentration of trace metals, pH, flow rate, sample volume, amount of adsorbent, concentration of eluent and sorption kinetics have been studied. The detection limits for Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+ were found to be 0.14, 0.62, 0.22, 0.54, 0.27, 0.28, 0.53 and 0.38 ng ml− 1, respectively. The adsorption capacity of the solid phase adsorption material is 10.3, 11.3, 14.5, 16.4, 15.1, 11.7, 15.4 and 16.8 mg g− 1 for Cd2+, Cr6+, Cu2+, Fe3+, Mn2+, Ni2+, Pb2+ and Zn2+, respectively. The preconcentration factor was obtained in the range of 50-100 for all studied metal ions. Coexisting ions over a high concentration range have not shown any significant effects on the determination of aforesaid metal ions. The accuracy of the proposed method was tested by standard reference materials (NIST 1643e: water, NIST 1573a: tomato leaves and NIST 1568a rice flour) and natural waters and the results obtained were in good agreement with the certified values.  相似文献   

19.
We report on a simple and reliable method for the determination of trace cadmium ion using a glassy carbon electrode (GCE) modified with cupferron, ß-naphthol and MWCNTs. The operational mechanism consists of several steps: first, the ligand cupferron on the modified electrode reacts with Cd2+ ion to form a chelate compound. Next, this chelate is adsorbed by the carrier ß-naphthol following the principle of organic co-precipitation. Finally, the coprecipitated complex is detected by the GCE. This scheme is interesting because it combines preconcentration and electrochemical detection. Two linear responses are obtained, one in the concentration range of 5.0?×?10?11 to 1.6?×?10?8 M, the other in the range of 1.6?×?10?8 to 1.42?×?10?6 M, with a lower detection limit of 1.6?×?10?11 M. This modified GCE does not suffer from significant interferences by Cu(II), Hg(II), Ag(I), Fe(III), Pb(II), Cr(III), Zn(II), NO3?, Cl?, SO 4 2? ions and EDTA. The response of the electrode remained constant for at least 3 weeks of successive operation. The method presented here provides a new way for the simultaneous separation, enrichment, and electrochemical detection of trace cadmium ion.
Figure
Separation, enrichment and electrochemical detection of trace cadmium ion were simultaneously and synchronously carried through on the electrode modified with cupferron, ß-naphthol, and multiwalled carbon nanotubes. It shows higher selectivity, excellent sensitivity and good stability.  相似文献   

20.
A rapid and reliable capillary zone electrophoresis method for the determination of inorganic cations was developed. The complete separation of K+, Ba2+, Ca2+, Na+, Mg2+, Mn2+, Ni2+, Cd2+, Li+ and Cu2+ can be achieved in 4 min with a simple electrolyte composed by 10 mM imidazole as the carrier buffer and background absorbance provider and acetic acid as the complexing agent (pH 3.60). Injection was performed hydrostatically by elevating the sample at 10 cm for 30 s. The running voltage was +25 kV at room temperature. Indirect UV-absorption detection was achieved at 185 nm. The detection limit was in the range between 0.06 mg/l (Mg2+) and 0.57 mg/l (K+) and the quantification limits ranged from 0.10 mg/l (Ni2+) to 0.80 mg/l (Cu2+). The calibration graphs were linear in the concentration range from the quantification limit till at least 1 g/l in K+, 10 mg/l in Ba2+, Ca2+, Mg2+, Mn2+, Ni2+ and Cd2+, 40 mg/l in Na+ and 12 mg/l in Li+ and Cu2+. The repeatability, intraday and interday analysis were ≤1.55% and ≤3.64% for migration time and ≤3.38% and ≤3.63% for peak area. The method developed has been applied to several beverage samples with only a simple dilution and filtration treatment of the sample. The proposed method is simple, fast, cheap and it is achieved with common products in either laboratory. For these reasons, it is a very useful method for routine analysis.  相似文献   

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