Background and overview[1]
With the improvement of scientific and technological level in recent years, acidic chromogens have been widely used in chemical analysis. In chemical detection, acidic chromogens can form red or purple highly sensitive micellar complexes with the detected substance, and the content of the detected substance can be determined using spectrophotometry. Phenofluorenone (Molecular formula: C19H12O5, also called phenylfluorone; germanium reagent; 9-phenyl-2,3,7-trihydroxy-6-xanthone; 9-Phenyl-2,3,7-trihydroxy -6-fluorine is an acidic chromogen widely used in chemical detection. It is mainly used to detect selenium compounds in smelting products. It can also be used for the determination of Ge4+, Sn4+, In3+, MoO42- and TaO3-. Now prepare The method used for phenyfluorenone is to dissolve phloroglucinol triacetate in an acidified ethanol aqueous solution and then react with benzaldehyde to prepare phenyfluorenone. However, this method has poor control over the pH of the acidified ethanol aqueous solution, resulting in a The cycle is longer, usually about 15 to 20 days; at the same time, the purity of the prepared lumefantrine is low, and the sensitivity during the spectrophotometric detection process is poor.
Apply[2-4]
Phenofluorenone is an acidic chromogen widely used in chemical detection. It is mainly used to detect selenium compounds in smelting products. It can also be used for the determination of Ge4+, Sn4+, In3+, MoO42- and TaO3-. Examples of its application are as follows:
1) Determination of low-content germanium in zinc-baked sand includes the following steps: standard curve drawing, sample preparation, color reaction, blank control, calculation of germanium content, etc. First, dissolve all germanium with acid and exclude other impurities. To eliminate the interference of elements, phenyfluorenone is used to react with germanium, and the germanium content is measured based on the absorbance of the reaction complex. The method of the invention has simple operation, good reproducibility, small error in detection results and high accuracy. It also avoids the pollution caused by using the carbon tetrachloride method to extract germanium, and is suitable for popularization and use.
2) Preparation of a trivalent and pentavalent antimony ion detection test paper. The preparation method of the present invention includes the following steps: (1) Prepare impregnation solution: weigh 0.05g~0.25g phenyfluorenone reagent in a beaker, add 2.5mL of (1:1) sulfuric acid solution and a certain amount of absolute ethanol to make Dissolve it and adjust the volume to 50mL with absolute ethanol to prepare liquid A; weigh 0.10g~0.50g cetyltrimethylammonium bromide and dissolve it in 10mL absolute ethanol to prepare liquid B; weigh 0.03g Dissolve ~0.08g ascorbic acid in 10mL distilled water to prepare liquid C; weigh 0.1g~0.5g oxalic acid and dissolve it in 10mL absolute ethanol to prepare liquid D; mix liquid A, liquid B, liquid C and liquid D Dissolve, prepare an impregnation solution; (2) Soak the filter paper for 3 to 15 minutes, take it out, and dry it. The invention is simple to make, convenient to operate, sensitive to detection, good in stability, easy to save, does not require professional operation, and is particularly suitable for on-site rapid detection of antimony content.
3) Determine the germanium content in sea cucumbers. The results show that the total germanium content in sea cucumbers from different origins was measured. The sample was processed by ashing method, CTMAB was used as solubilizer, gelatin was used as stabilizer, and lumefantrine was used as chromogenic agent. The color was developed under acidic conditions, and the content of germanium in sea cucumbers was determined using spectrophotometry. This system has a maximum absorption peak at 503nm, the regression equation is A=1.0925C+0.16815, the linear range is 0.072~0.504μg/mL, r=0.9978, the recovery rate of the method is 98.54%~99.30%, and the RSD is 1.9%. This method has simple sample processing and high accuracy, and can be used to determine the content of germanium in sea cucumbers.
Preparation[1]
Phenofluorenone is prepared as follows:
(1). Dissolve 250g of phloroglucinol triacetate in a mixture of 150ml of 95% ethanol, 1300ml of water and 200ml of concentrated sulfuric acid at a temperature of 50°C;
(2). Add 250g of benzaldehyde, stir and leave for 8 days to obtain a yellow lumefantrine sulfate mixture;
(3). Filter the lumefantrine sulfate mixture to obtain lumefantrine sulfate crystals;
(4). Dissolve the sulfate crystals of lumefantrine in 3000 ml of water, neutralize it with 20% sodium hydroxide to make the pH = 4, and leave it for 12 hours to obtain orange-red lumefantrine precipitation;
(5). Wash the precipitated lumefantrine with water 4 times, then wash it with ethanol 2 times, and dry it under vacuum to obtain lumefantrine.
Main reference materials
[1] Preparation method of CN200810053574.X lumefantrine
[2] CN201610749282.4 Detection method of low-content germanium in zinc calcined sand
[3] CN201510035186.9 Preparation method and application of trivalent and pentavalent antimony ion detection test paper
[4] CN201711054840.6 A method for determining the content of germanium in sea cucumbers using spectrophotometry
