Analytical methods of 铷 and 铯

First, chemical analysis

Chemical analysis is a classical analytical method, especially suitable for the determination of strontium and barium in high and medium concentrations. When the yttrium content in garnet is half the amount of bismuth , the weight method for precipitating strontium with sodium citrate (or potassium) (suitable for containing 20% ​​to 30% Ca 2 O). In the chemical analysis methods of ruthenium and osmium, because their ions have no obvious complexing ability, less precipitant, and large solubility product, the volumetric method is rarely used for analysis, but gravimetric analysis is used; mainly including platinum. Precipitating agents such as chloric acid method, perchlorate method, sodium tetraphenylborate method and tin tetrachloride method can separate potassium, strontium and barium from lithium and sodium, and quantitatively measure the total value. The large volume of strontium ions forms a salt with good selectivity, which can be separated from potassium and strontium, but it is difficult to separate from strontium.

Second, instrumental analysis

When the sample contains traces and a small amount of lanthanum and cerium, only instrumental analysis can be used. Among them, spectral analysis is the main method for determining ruthenium and osmium, including flame spectrophotometry, atomic absorption spectroscopy and atomic emission spectroscopy, and ion selective electrode. These methods have been developed to be more sophisticated and have been widely used in practice. With the development of analytical instruments in modern times, many new instruments for the analysis of 铷 and 出现 have appeared. Here are just a few of the commonly used methods:

The flame spectrophotometric detection of lanthanum and cerium is mostly carried out in advance. Solvent extraction is the fastest growing in the enrichment method. Because it facilitates the direct use of the extracted organic phase as a measuring solution and enhances the analytical line. A method for determining ruthenium and osmium without pre-concentration flame spectrophotometry by means of excitation light enhancement.

Atomic absorption spectroscopy uses a sharp line source from the measured element, with almost no line interference and very little temperature. The spectral lines of 铷 and 铯 are 780.0 and 852.1 nm, respectively. In recent years, graphite furnaces have developed rapidly in the absorption method. Many literatures have studied the interference of graphite atoms and the determination of the interference of ruthenium and osmium and the choice of matrix modifiers.

Atomic emission spectroscopy is mainly used for the detection of bismuth and antimony in minerals, ores and natural samples. Since the introduction of inductively coupled plasma light source (ICP) as a light source in the 1960s, it has developed extremely fast. Compared with traditional arc, flame and spark emission spectra, it has improved the sensitivity and precision of analysis, and has a wide linear range. The background interference is small and is used extensively in the analysis of 铷 and 铯.

In recent years, the electrochemical analysis method has developed extremely fast, especially based on the potential analysis method of various ion selective electrodes having characteristic selectivity to ruthenium and osmium, because of its simple equipment and low cost. High sensitivity, good selectivity, simple and fast, etc. have become a hot topic of research. The various types of ion selective electrodes appearing in the literature are listed in the table below. However, glass electrodes have been used to a minimum. Commercially available ion-selective electrodes of ruthenium and osmium are mostly various membrane electrodes.

Table 1 离子, 铯 ion selective electrode

Ion selective electrode carrier material

Select response ion

4,4'-di-tert-butyldibenzo--21-crown-7

Cs + , Rb +

O-phenyl-phenylene dioxymethylene bis(benzo-18-crown-6)

Cs +

PVC-crown ether (benzo-24-crown-8)

Cs +

Polymethylene toluene bridge

Cs + , Rb + , K +

1,3-alternating conformation double crown ether calixarene

Cs +

Double crown ether-PVC film

Rb +

Calix[6] arene ester-polyvinyl chloride film

Cs +

Tetraphenylboron + dibutyl phthalate + nitrobenzene + PVC

Cs +

Dibenzo-30-crown ether-10+2-nitrooctyl ether

Rb +

Or dioctyl dibenzoate + PVC

Rb + 55

Zeolite -polydimethylsiloxane

Cs + , Li + , K + , Na +

Dioctyl sebacate + aminomycin + PVC

Cs +

In addition to the above main methods, inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence spectrometry, proton induced X fluorescence analysis (PIXE), atomic fluorescence spectrometry (AFS), excited X fluorescence analysis (PIXE) ), chromatography, capillary electrophoresis, nuclear magnetic resonance spectroscopy, intracavity laser spectroscopy, neural network calculations, etc. are also used for the analysis of lanthanum and cerium.

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