CN113219027A - Method for quantitatively detecting potassium iodate - Google Patents
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Abstract
The invention relates to a kit for quantitative detection3The method of (2), characterized by: by using "HCHO-NaHSO3‑Na2SO3"pH clock reaction system as detection solution for KIO of different concentration3Different responses of (c), i.e. different implementation of induction time for KIO3Quantitative analysis of (3). The invention relates to a pair KIO3The quantitative analysis method has the characteristics of high accuracy, easiness in operation, convenience, rapidness and the like.
Description
Technical Field
The invention relates to an analysis and detection method, in particular to an establishment of HCHO-NaHSO3 - Na2SO3"pH clock System as substrate, according to which KIO is applied at different concentrations3The difference in response, i.e., the difference in induction time, was achieved for potassium iodate (KIO)3) Belonging to the field of analytical chemistry.
Background
Potassium iodate with molecular formula of KIO3Is an analytical reagent in chemical analysis. As an additive, for example, a redox titration standard solution is prepared as an oxidizing agent. And carrying out microanalysis on elements such as tantalum and the like. Also as complexing agents, masking agents, bacterial inhibitors, and the like. Can be used as feed additive for livestock. The animal feed can be used as additive for regulating iodine deficiency. Used as wheat flour treating agent, dough modifier, salt and iodine agent. FDA regulation (§ 184.1635, 2000) is applicable to bread, with a maximum limit of 0.0075% (based on wheat flour). The Chinese regulation can be used for solid beverages, and the limit is 0.26-0.4 mg/kg. Can be used as iodized salt or medicine for preventing endemic thyroid diseases. In recent years, potassium iodate has been found to have an effect of inhibiting tumor growth in some cases as an antitumor agent. Thus for KIO3The detection of (2) becomes critical.
For KIO at present3The detection method comprisesInductively coupled plasma mass spectrometry, atomic absorption, spectrophotometry, electrochemistry, neutron activation, chemiluminescence, and the like. However, most of these detection methods require large equipment and are expensive to test, which is not suitable for on-site measurement. Therefore, it is necessary to find a detection analysis method with good detection effect and simple and fast operation.
Disclosure of Invention
The invention is directed to KIO3Provides a new quantitative detection method, namely, HCHO-NaHSO3 - Na2SO3"pH clock system is the detection solution pair KIO3The method for quantitative detection is based on the KIO detection by the pH clock system3A standard curve (working curve) method developed for sensitive response. In particular, the use of "HCHO-NaHSO3 - Na2SO3The pH clock reaction system is used as a detection solution, and a graph of pH changing along with time is recorded; when the pH clock reaction starts, respectively mixing a series of KIO to be detected with different concentrations3Adding the sample solution into the pH clock system in equal volume, and realizing KIO detection according to different induction times generated by the pH clock system when the concentration of the solution to be detected in the pH clock system is different3And (4) quantitatively detecting the sample.
According to KIO3Establishing a working curve according to the relation between the concentration and the induction time in a pH clock system; wherein the abscissa is KIO3Concentration in a pH clock system, the ordinate is the induction time t, when KIO is present in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KIO3The concentration of (A) is in a linear relationship, so that the KIO in the sample can be realized3And (4) carrying out quantitative detection.
The difference between the quantitative detection method and the prior art is that the invention applies HCHO-NaHSO3 - Na2SO3"pH clock System as detection solution, and the System for KIO of different concentrations3The response of (2) is different, namely the induction time is different, and the KIO is realized3Quantitative analysis of (3).
KIO3In the detection solutionThe concentration range to be detected in the liquid (pH clock system) is 5.0X 10-4-2.5×10-3mol/L。
KIO3When the test solution (pH clock system) is tested, the temperature of the pH clock system is controlled to be any specific temperature within the range of 10-15 ℃.
Using the above-mentioned pH clock system, KIO3The concentration range that can be detected is an optimum concentration range determined experimentally. In this concentration range, the induction time is given to KIO3The concentration change has good response and large linear correlation coefficient. In addition, the concentration ranges of the components in the test solution (pH clock system) are shown in table 1, and the optimum concentrations of the test solution (pH clock system) obtained through a plurality of experiments are shown in table 2:
table 1: concentration of Components in a pH clock System
| HCHO(mol/ L) | NaHSO3 (mol/L) | Na2SO3 (mol/L) |
| 0.045-0.625 | 0.045-0.0625 | 0.0045-0.00625 |
Table 2: optimum concentration of each component in pH clock system
| HCHO(mol/ L) | NaHSO3 (mol/L) | Na2SO3 (mol/L) |
| 0.051 | 0.0495 | 0.00495 |
The specific experimental steps are as follows:
1. preparing 40mL of detection solution (pH clock system) according to the concentration range specified in Table 1, wherein the temperature of the detection solution is controlled to be constant at a certain specific temperature value between 10 and 15 ℃; inserting the prepared working electrode (pH composite electrode, Remao, E-331) into the solution, connecting the other end of the working electrode to a computer through a potential/temperature/pH comprehensive tester (ZHFX-595, Jiaxing Dinsheng electronic technology Co., Ltd.), opening a chemical signal acquisition analysis program in the computer to set acquisition time and sampling speed, and then quickly clicking a start key to monitor the pH of the solution. The computer records the collected curve of the change of the pH along with the time, namely a pH clock map. When a substance needs to be detected, the substance to be detected is rapidly added at the same time when the reaction of the pH clock system starts, and the pH clock map of the change of pH along with time is recorded in the same way.
Basic parameters of the pH clock map include:
induction time: the time required from the start of the reaction of the pH clock system to the pH jump.
pH jump range: the pH corresponding to the beginning of a pH jump to the pH corresponding to the end of a pH jump.
2. Establishment of KIO in detection solution3Working curve of the relationship between concentration and pH induction time
Preparing KIO with concentration of 0.5mol/L to 2.5mol/L by using distilled water as solvent3The solutions were used as sample solutions, and the reaction was started in a pH clock system of 40mL using pipette gunsAdding 40 mu L of the sample solution with different concentrations in the series to ensure that KIO is contained in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3mol/L is between; the variation of the response of the pH clock system is induction time which is marked as t; when KIO is present in the system3When the concentrations are different, the induction time t of the pH clock system is also different; in the system of KIO3The concentration is plotted on the abscissa and t is plotted on the ordinate; when KIO is in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3Between mol/L, pH clock system induces time t and KIO3The concentration of (A) is in a linear relation to obtain a working curve.
3. To KIO3Quantitative detection of
Adding a sample to be detected with unknown concentration into the pH clock system of the detection solution when the reaction of the pH clock system starts, measuring the induction time (t) of the corresponding pH clock system, and obtaining the KIO in the detection system according to the corresponding relation between t and concentration on the working curve3To further calculate the KIO in the sample to be measured3The concentration of (c).
Drawings
FIG. 1 is a graph showing the change of pH with time of a test solution (pH clock system) in example 1 without adding a sample to be tested.
FIG. 2 shows that in example 1, 5.0X 10-4mol/LKIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 3 is a graph of example 1, with 1.0X 10-3mol/L KIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 4 shows the pH induction times t and KIO in example 13Working curve between concentrations.
FIG. 5 is a graph showing the change of pH with time of the test solution (pH clock system) in example 2 without adding the sample to be tested.
FIG. 6 is a graph of example 2, with 1.5X 10-3mol/L KIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 7 shows that in example 2, 2.0X 10 is added-3mol/L KIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 8 shows the pH induction times t and KIO in example 23Working curve between concentrations.
FIG. 9 is a graph showing the change of pH with time of the test solution (pH clock system) in example 3 without adding the sample to be tested.
FIG. 10 is a graph showing that in example 3, 2.0X 10 was added-3mol/LKIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 11 is a graph of example 3, with the addition of 2.5X 10-3mol/L KIO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 12 is the pH induction times t and KIO in example 33Working curve between concentrations.
Detailed Description
Example 1
Application to "HCHO-NaHSO3 - Na2SO3"pH clock system as substrate as detection solution for KIO3Quantitative analysis was performed. Equal volume addition of KIO at different concentrations3Putting the sample solution into a pH clock system to establish KIO in a detection system3The working curve (such as linear relation) of the correlation between the concentration and the induction time is used for detecting the KIO in the pH clock system3To further calculate KIO in the sample to be measured3The concentration of (c).
(1) Preparing a detection solution
Firstly, distilled water is used for preparing 0.2mol/L HCHO solution and 0.1mol/L NaHSO3And 0.01mol/L of Na2SO3The mixed solution of (1). To a 50mL beaker were added 10.0mL of the aqueous solution distilled, followed by 19.8mL of NaHSO3 - Na2SO3Mixed solution, 10.2mL of 0.2mol/L HCHO solution, to ensure "HCHO-NaHSO3 - Na2SO3"the concentration of each component in the pH clock system is HCHO 0.051mol/L, NaHSO3 0.0495mol/L、Na2SO30.00495mol/L, total volume 40mL, temperature controlled at 14 ℃.
Meanwhile, distilled water is used as a solvent to prepare a series of KIO with different concentrations3A sample solution.
(2) Obtaining a pH clock map
The profile of the pH of the prepared test solution as a function of time was recorded by a computer equipped with a chemical signal acquisition analysis program (no test sample was added). As shown in fig. 1. The pH induction time was 144.2s for blank control. Two groups of detection solutions with the same component concentration as the detection solution are additionally arranged. For one group, 40. mu.L of 0.5mol/L KIO was added to a 40mL pH clock system at the same time the reaction started3Sample solution of KIO3The concentration in the test solution was 5.0X 10-4mol/L, KIO added3The induction time was extended to 184s as shown in FIG. 2; for the other group, 40. mu. L1.0mol/L of KIO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KIO3The concentration in the test solution was 1.0X 10-3mol/L, KIO added3So that the induction time becomes 237s as shown in FIG. 3. FIGS. 2 and 3 demonstrate the KIO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KIO is detected in the system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3The results of the different induction times of the pH clock system, which are caused by the different concentrations, can be observed between mol/L.
(3) Quantitative detection
According to KIO3Concentration versus induction time in the assay system a working curve was established as shown in FIG. 4, where the abscissa is KIO in a pH clock system3Concentration c (KIO)3) The ordinate is the induction time t, when KIO is detected in the system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KIO3Concentration c (KIO)3) In a linear relationship, the linear equation is t =66400c (KIO)3)+160.4,R2= 0.9711. Therefore, KIO in the sample can be realized3And (4) carrying out quantitative detection.
Example 2:
(1) preparing a detection solution
Firstly, distilled water is used for preparing 0.2mol/L HCHO solution and 0.1mol/L NaHSO3And 0.01mol/L of Na2SO3The mixed solution of (1). Into a 50mL beaker were added 9.5mL of distilled water solution, 20.0mL of NaHSO in that order3 - Na2SO3Mixed solution, 10.5mL of 0.2mol/L HCHO solution, to ensure "HCHO-NaHSO3 - Na2SO3"the concentration of each component in the pH clock system is HCHO 0.0525mol/L, NaHSO3 0.05mol/L、Na2SO30.005mol/L, a total volume of 40mL, and a temperature controlled at 12 ℃.
Meanwhile, distilled water is used as a solvent to prepare a series of KIO with different concentrations3A sample solution.
(2) Obtaining a pH clock map
The profile of the pH of the prepared test solution as a function of time was recorded by a computer equipped with a chemical signal acquisition analysis program (without addition of test sample) as shown in FIG. 5. The pH induction time was 144.1s for blank control. Two groups of detection solutions with the same component concentration as the detection solution are additionally arranged. For one group, 40. mu. L1.5mol/L of KIO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KIO3Concentration in the test solution was 1.5X 10-3mol/L, KIO added3The induction time was extended to 260s as shown in FIG. 6; for the other group, 40. mu. L2.0mol/L of KIO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KIO3The concentration in the test solution was 2.0X 10-3mol/L, KIO added3So that the induction time becomes 301s as shown in FIG. 7. FIGS. 6 and 7 demonstrate the KIO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KIO is detected in the system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3The results of different induction times of the pH clock system due to different concentrations of mol/L can be observed.
(3) Quantitative detection
According to KIO3Concentration versus induction time in the assay system a working curve was established as shown in FIG. 8, where the abscissa is KIO in a pH clock system3Concentration c (KIO3) of (A), the ordinate being the induction time t, when KIO is present in the test system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KIO3Concentration c (KIO)3) In a linear relationship, the linear equation is t =66800c (KIO)3)+158.6,R2= 0.98. Therefore, KIO in the sample can be realized3And (4) carrying out quantitative detection.
Example 3:
(1) preparing a detection solution
Firstly, distilled water is used for preparing 0.2mol/L HCHO solution and 0.1mol/L NaHSO3And 0.01mol/L of Na2SO3The mixed solution of (1). To a 50mL beaker were added 10.2mL of distilled water solution, 20.0mL of NaHSO in that order3 - Na2SO3Mixed solution, 9.8mL of 0.2mol/L HCHO solution, to ensure "HCHO-NaHSO3 - Na2SO3"the concentration of each component in the pH clock system is HCHO 0.049mol/L, NaHSO3 0.05mol/L、Na2SO30.005mol/L, a total volume of 40mL, and a temperature controlled at 12 ℃.
Meanwhile, distilled water is used as a solvent to prepare a series of KIO with different concentrations3A sample solution.
(2) Obtaining a pH clock map
The profile of the pH of the prepared test solution as a function of time was recorded by a computer equipped with a chemical signal acquisition analysis program (no test sample was added). As shown in fig. 9. The pH induction time was 144s for blank control. Two groups of detection solutions with the same component concentration as the detection solution are additionally arranged. For one set, 40. mu. L2.0mol/L of KIO was added to a 40mL pH clock system at the same time the reaction started3Sample solution of KIO3The concentration in the test solution was 2.0X 10-3mol/L, KIO added3So that the induction time is prolongedIs 301s as shown in FIG. 10; for the other group, 40. mu. L2.5mol/L of KIO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KIO3The concentration in the test solution was 2.5X 10-3mol/L, KIO added3So that the induction time became 3181s as shown in FIG. 11. FIGS. 10 and 11 demonstrate the KIO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KIO is detected in the system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3The results of the different induction times of the pH clock system, which are caused by the different concentrations, can be observed between mol/L.
(3) Quantitative detection
According to KIO3Concentration versus induction time in the assay system a working curve was established as shown in FIG. 12, where the abscissa is KIO in a pH clock system3Concentration c (KIO)3) The ordinate is the induction time t, when KIO is detected in the system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KIO3Concentration c (KIO)3) In a linear relationship, the linear equation is t =66600c (KIO)3)+158.7,R2= 0.981. Therefore, KIO in the sample can be realized3And (4) carrying out quantitative detection.
Claims (5)
1. KIO3The method for quantitative determination of (1), characterized in that:
preparing a solution of a sample to be detected by using distilled water as a solvent;
by using "HCHO-NaHSO3 - Na2SO3The pH clock reaction system is used as a detection solution, and a graph of pH changing along with time is recorded; the temperature of the pH clock system is controlled to be any specific temperature within the range of 10-15 ℃, when the pH clock reaction starts, a series of sample solutions to be detected with different concentrations are respectively added into the pH clock system in equal volume, and the quantitative detection of the samples to be detected is realized according to the different induction times generated by the pH clock system when the concentrations of the solutions to be detected in the pH clock system are different;
the molar concentration ranges of the components in the detection solution are as follows: HCHO0.045-0.0625mol/L, NaHSO30.045-0.0625mol/L、Na2SO30.0045-0.00625mol/L；
The sample to be detected is KIO3And (3) solution.
2. The quantitative determination method according to claim 1, characterized in that: establishing a working curve according to the relation between the concentration of the solution to be detected in a pH clock system and the induction time; wherein the abscissa is the solution KIO to be detected3Concentration in a pH clock system, the ordinate being the induction time t; when KIO is in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KIO3The concentration of the KIO is in a linear relation, so that the KIO in the sample is obtained3And (4) carrying out quantitative detection.
3. The quantitative determination method according to claim 1 or 2, characterized in that: the molar concentration of each component in the detection solution is HCHO 0.051mol/L, NaHSO30.0495mol/L、Na2SO30.00495mol/L。
4. The quantitative determination method according to claim 1 or 2, characterized in that: KIO3The detectable concentration range of the solution in the detection solution is 5.0X 10-4mol/L to 2.5X 10-3mol/L。
5. The quantitative determination method according to claim 1 or 2, characterized in that: detecting KIO3The temperature of the pH clock system was controlled at 12 ℃ while in solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114184657A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Method for distinguishing potassium chlorate from potassium iodate |
| CN114184658A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
| CN114184657B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Method for distinguishing potassium chlorate and potassium iodate |
| CN114184658B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
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| CN113219027B (en) | 2023-07-21 |
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