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New Methods For Determination Of Some Inorganic Metal Ions By Fluorescence And Resonance Rayleigh Scattering Spectrometry

Posted on:2017-12-25Degree:MasterType:Thesis
Country:ChinaCandidate:Y MiFull Text:PDF
GTID:2311330488987585Subject:Inorganic Chemistry
Abstract/Summary:PDF Full Text Request
Scientific and technological progress has brought great convenience to our life,at the same time,which has brought some problems of the environment and food safety,the harm of metal ions in the environment and food plays an important role in it.Choosing effective analysis method of detection for metal ions have great significance to life science,environmental science and natural science.Resonance Rayleigh scattering?RRS? was a new analysis method,which rose in the 90's of last century.It was welcomed by domestic and foreign scientific research workers because of its advantages of simplicity,rapidity,convenient and environmental friendly.It was a system testing by fluorescence method in the case of ?ex=?em.The determination of metal ions by Resonance Rayleigh scattering method has been a mature analysis method.This thesis accords to the interactions of anions of metal ions,inorganic ion color reagent and surface active agent have determined the aluminum,copper,antimony,cadmium,zinc and so on in the environment by Resonance Rayleigh scattering method and fluorescence method,specific content was as follows:?1? The introduction has mainly introduced the importance of the determination of metal ions,the conventional analytic technique, the development of Resonance Rayleigh scattering and the use of the method to determine metal ions.?2? Establishing new systems of determining Al??? by Resonance Rayleigh scattering method and fluorescence method.In acidic medium, using Aluminon?ATA?,chrome azurol S?CAS? as chromogenic agent,Cetyltrimethyl Ammonium Bromide?CTMAB? as surface active agent interacted with Al??? ions,formed ion association complexes by electrostatic and hydrophobic forces,then caused the increase of RRS intensity,and the RRS method for the determination of Al??? was established;also,Catalytic kinetic fluorescence method was established, which using Al??? as catalyst,catalyzed by KBrO3 oxidizing Morin, from the test it was found in certain concentration range,the maximum wavelength(?ATA=598.1nm,?CAS=670.7nm,?ex/?em=466.6nm/555.3nm?Morin?),scattering intensity and fluorescence intensity of systems,and Al??? concentration showed a linear correlation, three kinds of system of linear range were 0.020.16?g·mL-1?ATA?,0.020.12?g·mL-1?CAS?,590 ng·mL-1?Morin?, detection limit were 1.77ng·mL-1?ATA?, 0.94ng·mL-1?CAS?, 1.64ng·mL-1?Morin?,respectively.The optimum conditions of the three systems was optimized, ions interference of system was investigated and the reaction mechanism were discussed and found that system has good stability and selectivity,and the detection and analysis of real samples has satisfactory results.?3? Establishing two new systems of determining Cu? ??,which was based on the interaction between Cu? ??,methyl orange?MO? and CTMAB could form ion association complexes,and Cu? ?? catalytic KIO4 oxidizing ST.The results showed that Cu? ??,MO,CTMAB itself has no or with a very weak scattering peak using the RRS method,the increase of the scattering intensity in the system because of the form of larger ion association complexes when the three above interacted with each other.At ?=592nm,the scattering intensity and the linear range of Cu? ?? between 0.020.10?g·mL-1 is proportional,the detection limit is 0.98 ng mL-1;In the Catalytic kinetic fluorescence method, when add to the Cu??? in the system, the fluorescence intensity decreased significantly in ?=580nm,and Cu??? concentration in 2.5032.50ng·mL-1range and system lg?F0/F? was a linear relationship,the detection limit is 0.17ng·mL-1.Compared with two each other,Resonance Rayleigh scattering method has a wider linear range,detection limit lower fluorescence analysis,more sensitive experiments.The reaction conditions was optimized in the experimental process,and explored the relationship between the intensity of reaction with the material,and the use of two kinds test and analysis different sections of the Yellow River,tap water,laboratory waste water,recovery experiments were carried out,and the result is good.?4? Two new systems were established to determine Sb???:Sb???-KI-RhB and Sb???-KIO4-NR.The reaction conditions of the system were optimized and the interference of other ions for the system was investigated,as well as the reaction product for the ultimate effect of the system was discussed,and the result of analysis and detection of environmental samples reproduces well with satisfactory results.Sb???-KI-RhB,Sb???,KI,Rhodamine B?RhB? in H2SO4 medium of 0.08mol·L-1 of the system,the RRS level was increased because of the forming of ternary ion association complex,which was due to electrostatic attraction,intermolecular force, hydrophobic interaction, and the scattering intensity with the concentration of Sb? ?? was proportion in ?=623nm,the range was 2.00×10-72.56×10-6mol·L-1,the detection limit was 1.89×10-8mol·L-1;The reaction of KIO4 oxidize NR was more quick when Sb? ?? added in the system of Sb? ??-KIO4-NR,fluorescent intensity was weakened when the Sb??? continue added in the ?=638nm.And the concentration of Sb???in the range of 0.050.26?g·mL-1and lg?F0/F? to maintain a good linear relationship, detection limit was 0.16?g·mL-1.The results showed that the system performed a good anti-jamming and stability, and the determination effect was better.?5? Two new systems were established to determine Cd??? and Zn??? using Resonance Rayleigh scattering?RRS?.Cd???,KI,Methylene Blue?MB? formed ternary ion association complex[CdI4][MB]2 by mutual electrostatic and hydrophobic forces in acidicmedium and surface active agent of polyvinyl alcohol?PVA?,Zn???,KSCN,and neutral red?NR? formed an ion association complex [ZnSCN4][NR]2 by the actions with each other.The scattering intensity(?MB=592.6nm,?NR=594.5nm) of the system was increased and was proportional to the two metal ions in a linear range due to the increase of the molecular weight of the association and the influence of hydrophobic interaction.The linear range were8.00×10-81.20×10-7mol·L-1?MB?,0.050.50?g·mL-1?NR?.The detection limits were 3.90×10-8mol·L-1?MB?,1.9×10-5?g·ml-1?NR?,respectively.The interference of coexisting substances on the system was investigated,the reaction mechanism was discussed,the experimental conditions were optimized,and the Cd???,Zn??? was detected with Yellow River and Synthetic water,the stability and the effect were excellent and the recoveries were 98.9%101.3%?96.4%103.7%,respectively.
Keywords/Search Tags:Resonance Rayleigh Scattering Spectrum, Fluorescence Analysis, Inorganic ion color reagent, Metal Ions
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