Determination of Copper, Iron and Sodium in High Purity Alumina by Graphite Furnace Atomic Absorption Spectrometry with Suspension Injection
Key words: graphite furnace atomic absorption spectrometry; self-priming buckle back; copper, iron and sodium content in alumina, AA-1800. Determination of high purity alumina by suspension-self-priming background graphite furnace atomic absorption spectrometry Trace elements of copper, iron, sodium. The experiment optimized the ashing temperature, atomization temperature and graphite furnace atomic absorption working conditions such as self-priming background light, and determined the optimal measurement conditions. The sample test was calibrated with a standard aqueous solution. The accuracy of the method was determined by using alumina AKP-30 to dissolve the sample under high temperature and high pressure and concentrated sulfuric acid. The results of the analysis were compared with the results of other methods reported in the literature. Studies have shown that the method is simple and reliable, and is suitable for rapid determination of trace elements in alumina. The linear correlation of the calibration curve is greater than 0.999 0. The detection limits for copper, iron and sodium are 0.66, 2.5, 0.13 ng·g-1, respectively, and the relative standard deviation is less than 5.2%. Alumina is an advanced ceramic material and an essential component of many advanced ceramic materials. In recent years, it has developed rapidly at home and abroad, and is widely used in many high-tech industries such as electrical insulating materials and integrated circuit substrates. In order to improve the strength, toughness, compactness, thermal stability, transparency, photoelectric performance or lowering of sintering temperature, high purity is required (minor trace elements such as Fe, Cu, Na, etc. directly affect the structure of the material and Performance), ultrafine alumina powder raw material with a particle size of submicron or even nanometer, narrow particle size distribution range and good sintering activity.
At present, the trace element characterization of high-purity alumina lacks effective analytical testing methods, mainly because high-purity alumina is difficult to prepare into a liquid. Usually, the dissolution of alumina is carried out under high pressure or microwave using sulfuric acid [1], hydrochloric acid [2, 3], phosphoric acid [4, 5], mixed acid [6]. Detection techniques include inductively coupled plasma optical emission spectroscopy (ICP-AES) [3-10], electrothermal evaporation inductively coupled plasma mass spectrometry (ETVICP-MS) [1, 11-13], atomic absorption spectroscopy (AAS) [2, 14]. However, these methods require a processing time of consumption, and there are dangers and defects in contamination of reagents and containers. The suspension injection combines the advantages of liquid injection and solid injection, and has the characteristics that the sample does not need to be completely digested, and the total mass of the sample is high and the sensitivity is high. Making solid samples into suspensions is by far the most widely used solid injection method [8-14]. Suspension graphite furnace atomic absorption spectrometry combines the significant advantages of solid and liquid injection methods. It is a relatively mature technology and has been widely used as a routine analytical method in micro and trace metal elements in organic and inorganic complex matrices. Analytical determination [15].
The suspension does not require the sample to be prepared as a solution, so the particles will produce non-specific absorption during atomization compared to solution injection. It is also difficult to avoid atomization of the analyte and the substrate simultaneously by the temperature rise of the graphite furnace. Therefore, effective background correction is necessary. The self-priming background correction, also known as the Smith-Hieftje (S-H) method, is a method of background correction using a strong and weak pulse power supply to a hollow cathode lamp. It is a simple and easy to perform background correction method.
In this paper, the background of graphite furnace atomic absorption self-priming buckle is applied, and the contents of trace elements such as copper, iron and sodium in alumina are determined by direct injection of suspension and self-suction buckle background. Key words: graphite furnace atomic absorption spectrometry; self-priming buckle back; copper, iron and sodium content in alumina, AA-1800
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