Determination of manganese, sodium, lead, zinc and titanium in iron phosphate by atomic absorption spectrometry - Master's thesis - Dissertation

Determination of Manganese, Sodium, Lead, Zinc and Titanium in Iron Phosphate by Atomic Absorption Spectrometry

Key words: atomic absorption spectrometer; content of manganese, sodium, lead, zinc, titanium in iron phosphate; analysis instrument ; AA1800C; AA1800 iron phosphate is easily soluble in hydrochloric acid when heated, but hardly soluble in other acids, almost Insoluble in water, the unique properties of this substance can be used as a raw material for the manufacture of lithium iron phosphate batteries, as a catalyst and in the production of ceramics. The content of metal elements directly affects the properties of the substance, especially when making batteries. The amount of metal elements directly affects the conductivity of the battery. Therefore, it is of great significance to accurately detect the content of metal elements. In this paper, the method is used to dissolve iron phosphate by hydrochloric acid, and the content of various metal elements in iron phosphate is detected by atomic absorption spectrometry with good reproducibility. 1. Experimental part 1.1 Instruments and equipment AA1800 atomic absorption spectrometer, ultrapure water machine, vacuum drying oven, thermostat hot plate, manganese hollow cathode lamp, lead hollow cathode lamp, sodium hollow cathode lamp, zinc hollow cathode lamp, titanium Hollow cathode lamp. 1.2 Main reagents hydrochloric acid (excellent grade pure), hydrofluoric acid (excellent grade pure), metal ruthenium (99.9%), oxalic acid (excellent grade pure), sodium standard solution (1000ug/mL), lead standard solution (1000ug/mL) Zinc standard solution (1000ug/mL), titanium standard solution (1000ug/mL), manganese standard solution (1000ug/mL). 1.3 Sample processing method Two sets of 0.2000g samples were accurately weighed, placed in a 100mL polytetrafluoro beaker, added with 5mL hydrochloric acid, placed on a hot plate to heat the sample to a low temperature, the electric heating plate was turned off, and the heat of the electric heating plate was used to catch acid. When the digestion solution is about 1 mL, cool to room temperature, transfer the solution to a 50 mL polypropylene volumetric flask, rinse the polytetrafluorobeth with deionized water, and rinse the water into a volumetric flask to make up to volume. The same method is used to make the sample blank. 1.4 On-machine test Because the iron phosphate matrix is ​​more complicated, this paper makes a sample blank when processing the sample, calibrates the machine zero point with deionized water, and gradually tests according to the order of standard sample, sample blank and unknown sample. The working curve of the standard sample See the 1.5 working curve. 1.5 Working curve This paper uses the flame standard curve method to test the content of sodium, manganese and zinc. The lead and titanium contents are tested by the graphite furnace standard curve method. The obtained standard curve and correlation coefficient are slightly: 2. Results and discussion 2.1 Interference and elimination of sample pretreatment process In the process, try to use a PTFE beaker. When the sample is finished, try to use a polypropylene volumetric flask to avoid the influence of sodium in the glass container. In addition, at least two samples should be processed at the same time for sample comparison. When preparing the sodium standard solution and the sample solution, a 2% cesium chloride solution which is more ionizable than sodium should be added thereto to reduce the ionization of sodium. When measuring lead in a graphite furnace, each time a 20uL standard sample or an unknown sample is introduced, 5uL of a 0.1% ammonium dihydrogen phosphate solution is simultaneously used as a matrix modifier, and the background absorbance value is subtracted from the background. When the graphite furnace is used to measure titanium, the graphite tube is subjected to ruthenium coating, and the concentration of the coating ruthenium solution is preferably 60 g/L. In the specific test process of each group of samples, the sample blank should be deducted to avoid a positive deviation of the test results. 2.2 Test results Two test results of the same sample can be seen that the deviation between the two groups is small, which proves that the sample processing and test process are feasible. If the deviation between the two groups is large, the sample needs to be re-digested and re-tested. . Key words: atomic absorption spectrometer; content of manganese, sodium, lead, zinc, titanium in iron phosphate; aesthetic analyzer ; AA1800C; AA1800

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