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Dynamic absorbance quantitative analysis method based on iodine-starch chromogenic system

A quantitative analysis and absorbance technology, which is applied in the field of chemical and spectral analysis and testing, can solve the problems of low reliability of analysis results and achieve high accuracy, easy operation and good reproducibility

Inactive Publication Date: 2013-12-25
SICHUAN AGRI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, it involves the absorbance photometric quantitative analysis method of iodine-starch chromogenic system. In "A spectrophotometric quantitative analysis method of iodine-starch chromogenic system" (China, 2013104091344[P]) published an iodine-starch chromogenic system. Color system stabilization method and quantitative analysis with spectrophotometry, the rest of the literature related to iodine-starch chromogenic absorbance photometric quantitative analysis methods have not reported on the solution to the unstable iodine-starch chromogenic system method, appointed conventional iodine-starch chromogenic method method and conventional absorbance photometry for quantitative analysis, the reliability of the analysis results is low

Method used

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  • Dynamic absorbance quantitative analysis method based on iodine-starch chromogenic system

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Embodiment 1

[0031] Embodiment 1: based on iodine-starch chromogenic system dynamic absorbance quantitative analysis precision test and establishment of standard curve, its operation steps:

[0032] (1) At room temperature, take a quartz cuvette with a volume of 4mL and an optical path of 1cm as the reaction vessel. The total volume of the reaction liquid is 3.50mL, leaving 0.5mL space for shaking well; transfer 1.00mL of 0.315 mmol / L potassium iodate standard Solution, transfer 50 μL of 6 mol / L hydrochloric acid solution, transfer 2.40 mL of 1% starch solution, transfer 50 μL of 100 g / L hydroxylamine hydrochloride, quickly cover and shake well, immediately put it into a photometer, and use 600 nm as the measurement wavelength to measure the dynamic absorbance ,get A max Value; according to this method in parallel 6 times, with 6 times of determination A max value calculation, RSD (%)=0.81%;

[0033] The invention establishes a dynamic absorbance quantitative analysis method based on...

Embodiment 2

[0036] Embodiment 2: IO in the dynamic absorbance quantitative analysis method system based on iodine-starch chromogenic system 3 - The initial concentration c and A max and A ' max Linear relationship inspection, its operation steps:

[0037] (1) Obtain different IOs according to the (2) step method of Example 1 3 - The initial concentration of the chromogenic system A max value;

[0038] (2) use figure 2 Method to process images and get different IO 3 - The initial concentration of the chromogenic system A ' max value;

[0039] (3) Use IO in the system 3 - The initial concentration c and A ' max Corresponding relationship between values ​​was analyzed by linear regression to obtain the correlation coefficient r ﹥0.9999;

[0040] IO in the system 3 - The initial concentration c with a large value of absorbance A max and A ' max Corresponding relationships can be established separately, and a good linear relationship can be obtained. In order t...

Embodiment 3

[0041] Embodiment 3: Determination of commercially available iodine (KIO 3 ) salt iodine content, its operation steps:

[0042] (1) Accurately weigh commercially available iodized salt (Chuanjing brand, Chengdu Salt Industry Company, the package indicates that it contains KIO 3 Measure 2100~3900μg / 100g) of iodine) 100.0g, heat and boil with 400mL distilled water to dissolve, cool to room temperature to crystallize, take the clear liquid and concentrate it to 50mL under reduced pressure, cool to room temperature to crystallize, clear liquid is transferred to a 100mL volumetric flask, and distilled water to volume , the iodine content of the prepared test solution is 21-39 μg / mL;

[0043] (2) Take a quartz cuvette with a volume of 4mL and an optical path of 1cm as the reaction vessel, transfer 0.80mL of 0.315 mmol / L potassium iodate standard solution, transfer 50μL of 6 mol / L hydrochloric acid solution, and transfer 2.60mL of 1% starch solution , transfer 50 μL of 100 g / L hydr...

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Abstract

The invention belongs to the technical field of chemical and spectral analysis and testing, and particularly discloses a dynamic absorbance quantitative analysis method based on an iodine-starch chromogenic system. The dynamic absorbance quantitative analysis method specifically comprises the steps: (1) at room temperature, respectively transferring a quantitative IO3-solution, a certain amount of starch and a certain amount of hydrochloric acid into a cuvette, and shaking evenly; (2) quickly transferring a certain quantity of reducing agents such as hydroxylamine hydrochloride, and immediately capping and shaking evenly; (3) measuring a dynamic value of system absorbance under a condition of 600nm wavelength; (4) obtaining a great value absorbance value Amax or a stoichiometric point absorbance value A'max by using a time-absorbance relation graph; (5) according to the steps (1)-(4) in the method, establishing a standard curve and measuring the concentration of an unknown solution IO3- by using the corresponding relationship of the initial concentration c of IO3- of the chromogenic system and the Amax or A'max. When being applied to the direct and indirect analysis of iodine amount, the dynamic absorbance quantitative analysis method has the advantages of easiness and convenience, accuracy, trace, rapidness, low price and the like, and also can be applied to the research on chemical reaction kinetics associated with the dynamic absorbance quantitative analysis method, thus having theory and application values.

Description

technical field [0001] The invention relates to the technical field of chemical and spectral analysis testing, in particular to a dynamic absorbance quantitative analysis method based on an iodine-starch color development system. Background technique [0002] The color reaction of iodine starch is a traditional and very classic chemical reaction. In aqueous solution, when I 2 The molecule penetrates into the helical structure of the starch, forming an I 2 - Starch clathrate, absorbs blue complementary color light, the solution is blue. I 2 -The color reaction of starch is a reversible reaction (I 2 +starch I 2 -starch inclusion compound), reach equilibrium under certain conditions, such as changing the reaction conditions, such as concentration, temperature, pH, etc., the balance will be broken, the concentration of the inclusion compound will change accordingly, and the absorbance will also change accordingly. I 2 Disproportionation is fastest in alkaline environmen...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N21/75
Inventor 甄铧张学毅王双燕武婷婷张祖民
Owner SICHUAN AGRI UNIV
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