Photoelectrochemical method for quantitatively detecting monovalent thallium
A quantitative detection and photoelectrochemical technology, applied in the field of semiconductor nanomaterial photoelectrochemical sensors, achieves the effects of strong adhesion, good detection performance and cost reduction
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Embodiment 1
[0048]Embodiment 1: the acquisition of the working curve when the pH=2 of thallium nitrate solution
[0049] (1) Preparation of indium sulfide thin film electrodes: Cut fluorine-doped tin oxide (FTO) electrodes into 1.5x2.5 cm, and then ultrasonically clean them with detergent powder, ethanol and deionized water for 30 min, and dry naturally. Take two pieces of FTO that have been cleaned and dried, with the conductive side facing down, and put them into the polyvinyl fluoride reactor. Measure 30 mL of absolute ethanol in a 50 mL beaker, add 0.4399 g of indium trichloride tetrahydrate while stirring and wait for it to completely dissolve, then add 0.2255 g of thioacetamide (TAA), and stir magnetically at room temperature until The solution is light yellow, and 10 ml of the light yellow solution is measured with a graduated cylinder, and poured into a polyvinyl fluoride reactor prepared with an FTO glass sheet with the conductive surface facing down. The reaction kettle was mov...
Embodiment 2
[0056] Embodiment 2: the acquisition of the working curve when the pH=6 of thallium nitrate solution
[0057] The pH of the thallium nitrate solution in step (2) in Example 1 is adjusted to 6, all the others remain unchanged, repeat Example 1, and obtain ΔI vs. The linear relationship of concentration, that is, the working curve at pH=6, specifically as Figure 5 shown.
[0058] from Figure 5 It can be seen that the concentration of Tl that we can measure is 0.625 μM, that is, the detection limit is 0.625 μM. However, under the condition of pH=2, for the same Tl concentration, the ΔI value is larger than that at pH=6, and the detection current is more obvious. In other words, the photoelectric detection method for monovalent thallium induced by the surface state of the crystal material proposed by us is more obvious under high acidity conditions. Therefore, the subsequent selectivity test, anti-interference test and actual sample test are all carried out under the conditi...
Embodiment 3
[0059] Example 3: Detection of thallium concentration in actual aqueous solution and its accuracy characterization
[0060] (1) Take 100 mL of tap water (Guangzhou University University Town Campus) and Pearl River water (Guangzhou University Town Pearl River Water System), centrifuge for 5 minutes (10,000 rpm), and then filter the supernatant with a microporous membrane (0.22 μm). The content of thallium in these two real samples was determined by analytical chemistry spike recovery method at pH 2. The results showed that no monovalent thallium was detected in the two water samples. Add 2, 5, and 8 μM monovalent thallium to the two water samples respectively to obtain six water samples to be tested;
[0061] (2) repeat the step (1) of embodiment 1, obtain sulfur-rich indium sulfide electrode In 2 S 3 , the prepared sulfur-rich indium sulfide electrode In 2 S 3 In the water sample to be tested with a pH value of 2 and a volume of 10 mL, the temperature is 50°C for 20 minu...
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