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Method for determining concentration of stable dispersion water solution C60

An aqueous solution and concentration technology, applied in the field of nanomaterials, can solve problems such as difficulty in ensuring complete extraction of C60, unoptimized reagent dosage ratio, and low measurement results, and achieve the effect of promoting in-depth application, easy operation, and rapid extraction process.

Active Publication Date: 2014-04-09
江苏皓海检测技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, only one extraction is carried out during the operation of this method, and the dosage ratio of various reagents is not optimized, and it is only carried out in the form of oscillation, so it is difficult to guarantee C 60 Completely extracted into the organic phase, so there are problems with low measurement results and poor precision
In addition, the method selects magnesium perchlorate as C 60 The destabilizing agent in the extraction process, which is a strong oxidant, can support combustion and has irritating effects on the eyes, skin, mucous membranes and upper respiratory tract, which makes the determination process have certain safety risks

Method used

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  • Method for determining concentration of stable dispersion water solution C60

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Embodiment 1

[0031] Measure solvent replacement method to prepare C with the present invention 60 Stabilize the concentration of the dispersed aqueous solution.

[0032] With the C prepared by solvent replacement method 60 Stable dispersed aqueous solution is the measurement object, take 5 parallel samples, and operate according to step (4)-step (8) in the above embodiment respectively, the measurement results are shown in Table 1. It can be seen from the table that the method proposed by the present invention measures the sample prepared by the solvent replacement method, and the deviation of the result obtained is very low, and has good precision.

[0033] Table 1

[0034] sample number 1 2 3 4 5 average value standard deviation The relative standard deviation Measured valuemg / L 7.471 7.426 7.383 7.462 7.391 7.427 0.040 0.5%

Embodiment 2

[0036] Determination delay stirring method of the present invention is used to prepare C 60 Stabilize the concentration of the dispersed aqueous solution.

[0037] C prepared by delayed stirring method 60 The stable dispersed aqueous solution is the measurement object, and the operation is performed according to the step (4)-step (8) in the above embodiment, and the measurement results are shown in Table 2. As can be seen from the table, the method proposed by the present invention measures the sample prepared by the delayed stirring method, and the deviation of the result obtained is very low, and has good precision.

[0038] Table 2

[0039] sample number 1 2 3 4 5 average value standard deviation The relative standard deviation Measured valuemg / L 1.828 1.883 1.902 1.825 1.910 1.870 0.041 2.2%

Embodiment 3

[0041] Adopt the method step (1)-step (6) that the present invention proposes, the C prepared by solvent replacement method 60 The stable dispersed aqueous solution is the measurement object, and calcium chloride and toluene with different volume ratios in step (4) are added to make C during the extraction process 60 The volume ratios of stable dispersed aqueous solution, calcium chloride solution and toluene are 1:1:1, 1:0.5:1, 1:1:0.5, 1:1:2, take 5 parallel samples for each method, and extract once , and the measurement results are shown in Table 3. According to the measurement results, select the best C 60 The volume ratio of stable dispersed aqueous solution, calcium chloride solution and toluene is 1:1:1, the extraction is relatively complete, the deviation of the obtained results is small, the precision of the method is high, and the consumption of extractant is not high.

[0042] table 3

[0043] Proportion sample number 1 2 3 4 5 average value ...

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Abstract

The invention relates to a method for determining the concentration of stable dispersion water solution C60. The method comprises the steps of firstly, preparing different concentrations of C60-Toluene standard solution, determining the absorbance at the wavelength of 334-336nm, performing linear regression to the concentration values and corresponding absorbance value, thus obtaining a standard curve; then taking stable dispersion water solution C60 to be determined, adding calcium chloride solution and toluene, wherein the ratio of the stable dispersion water solution to calcium chloride solution to toluene is 1:(0.5-1):(0.5-2); sealing, performing ultrasonic dispersion for 10-15min to form white emulsion, oscillating and standing to obtain a two-layer solution, freezing for 30-60min in the condition of minus 20 DEG C so as to entirely condense the water phase to be in a solid state and keep an organic phase under a liquid state; entirely absorbing the organic phase solution, determining the absorbance, and calculating the concentration of the C60 according to the standard curve; repeating the steps, adding the concentrations of the C60 obtained by twice extraction, thus obtaining the final determined concentration of the stable dispersion water solution C60 to be determined. The method is simple and fast to operate, and capable of performing batch determination.

Description

technical field [0001] The invention belongs to the field of nanomaterials, in particular to a method for measuring C by using ultraviolet spectrophotometry. 60 A method of stabilizing the concentration of a dispersed aqueous solution. Background technique [0002] Since its discovery in 1985, C 60 It has attracted much attention because of its unique micro-nano structure and excellent mechanical, electro-optical and chemical properties. At present, it has become a new type of nanomaterial widely studied and applied in many fields such as electronics, chemical industry, metallurgy, aerospace, military, environmental protection, medicine and biological engineering. but C 60 It is extremely hydrophobic and has a very low solubility (<10 -12 g / L), it is not easy to distribute evenly in water, thus limiting its application in many fields. In view of this, a variety of preparation C 60 Techniques for stabilizing dispersed aqueous solutions have been developed. These met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N1/38
Inventor 方华沈冰冰孙宇心荆洁王媛陆继来
Owner 江苏皓海检测技术有限公司
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