CN113219025A - Method for quantitatively detecting potassium bromate - Google Patents
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Abstract
The present invention relates to a method for quantitatively detecting KBrO3The method of (2), characterized by: by using "HCHO-NaHSO3‑Na2SO3"pH clock reaction system as detection solution for KBrO with different concentration3Different responses of (c), i.e. different implementation of induction time, for KBrO3Quantitative analysis of (3). The invention relates to a KBrO3The 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 for substrates, according to which KBrO is applied to different concentrations3The difference in response, i.e., the difference in induction time, was achieved for potassium bromate (KBrO)3) Belonging to the field of analytical chemistry.
Background
Potassium bromate with molecular formula KBrO3It is mainly used as analytical reagent, oxidant and wool bleaching agent. It has irritation to eyes, skin and mucosa, and can cause nausea, emesis, gastralgia, haematemesis, diarrhea, etc. after oral administration, and has certain harm to environment. Bromate formed by bromate ions is a byproduct generated after natural water sources such as mineral water, spring water and the like are disinfected by ozone, so that the guarantee that the content of bromate in the mineral water meets the drinking water standard is very important. Thus for KBrO3The detection of (2) becomes critical.
For KBrO3The detection method of (3) includes inductively coupled plasma mass spectrometry, atomic absorption, spectrophotometry, electrochemistry, neutron activation, chemiluminescence, etc. However, such detection methods mostly require large equipment and are currently expensive to test and unsuitable for on-site assays. Therefore, a method which has good detection effect and is used for detecting the defect of the defectThe simple and rapid detection and analysis method is very necessary.
Disclosure of Invention
The invention is directed to KBrO3Provides a new quantitative detection method, namely, HCHO-NaHSO3 - Na2SO3"pH clock system is the detection solution pair KBrO3The method for quantitative detection is based on the pH clock system to KBrO3A 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 KBrO to be detected with different concentrations3Adding the sample solution into the pH clock system in equal volume, and realizing the KBrO to be detected according to different induction times generated by the system when the concentration of the solution to be detected in the pH clock system is different3And (4) quantitatively detecting the sample.
According to KBrO3Establishing a working curve according to the relation between the concentration and the induction time in a pH clock system; wherein the abscissa is KBrO3Concentration in a pH clock system, the ordinate is the induction time t, when KBrO is present in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KBrO3The concentration of (A) is in a linear relation, so that the KBrO 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 KBrO of different concentrations in the system3The response of (c) is different, i.e. the induction time is different, the KBrO is realized3Quantitative analysis of (3).
KBrO3The concentration range to be detected in the detection solution (pH clock system) is 5.0X 10-4-2.5×10- 3mol/L。
KBrO3When detected in a detection solution (pH clock system), the temperature of the pH clock system is controlledAt any one specific temperature within the range of 10-15 ℃.
KBrO Using the above-described pH clock System3The concentration range that can be detected is an optimum concentration range determined experimentally. In this concentration range, the induction time is in accordance with KBrO3The 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 0.5-2.5 mol/L detection solution (pH clock system) according to the concentration range specified in Table 1, wherein the temperature is controlled to be a certain specific temperature value between 10 and 15 ℃ and is kept unchanged; 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 KBrO in detection solution3Working curve of the relationship between concentration and pH induction time
Distilled water is used as solvent to prepare KBrO with the concentration of 0.5mol/L-2.5mol/L3Taking the solution as a sample solution, and respectively adding 40 mu L of the series of sample solutions with different concentrations into a 40mL pH clock system by using a pipette when the reaction of the pH clock system is started so as to ensure that KBrO 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 in useKBrO in the System3When the concentrations are different, the induction time t of the pH clock system is also different; in the system of KBrO3The concentration is plotted on the abscissa and t is plotted on the ordinate; when KBrO is in the system3The concentration is 5.0 × 10- 4mol/L to 2.5X 10-3Between mol/L, the pH clock system induces time t and KBrO3The concentration of (A) is in a linear relation to obtain a working curve.
3. For KBrO3Quantitative 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 KBrO in the detection system according to the corresponding relation between t and concentration on the working curve3Further calculating KBrO 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 is a schematic representation of example 1, with the addition of 5X 10-4mol/LKBrO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 3 is a graph showing that in example 1, 1X 10 is added-3mol/L KBrO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 4 shows the pH induction times t and KBrO 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 KBrO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 7 is a graph showing that in example 2, 2X 10 was added-3mol/L KBrO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 8 is pH induction in example 2Time t and KBrO3Working 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, 2X 10 is added-3mol/L KBrO3Thereafter, 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 KBrO3Thereafter, the pH of the solution (pH clock system) was plotted against time.
FIG. 12 is the pH induction time t and KBrO in example 33Working curve between concentrations.
Detailed Description
Example 1
Application to "HCHO-NaHSO3 - Na2SO3"pH clock system as substrate as detection solution for KBrO3Quantitative analysis was performed. Adding KBrO with different concentrations in equal volume3Putting the sample solution into a pH clock system to establish KBrO 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 KBrO in the pH clock system3Further calculating KBrO 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 12 ℃.
Simultaneously, distilled water is used as a solvent to prepare a series of KBrO 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 145s 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 KBrO was added to a 40mL pH clock system at the same time the reaction started3Sample solution of KBrO3Concentration in the test solution was 5X 10-4mol/L, KBrO added3The induction time was extended to 241s as shown in FIG. 2; for the other set, 40. mu.L of 1mol/L KBrO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KBrO3Concentration in the test solution was 1X 10-3mol/L, KBrO added3So that the induction time becomes 251s as shown in FIG. 3. FIGS. 2 and 3 confirm that KBrO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KBrO in the detection 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 KBrO3The concentration in the assay system as a function of induction time was plotted as a working curve, as shown in FIG. 4, where the abscissa is KBrO in a pH clock system3Concentration c (KBrO)3) The ordinate is the induction time t when KBrO in the detection system3At a concentration of 5.0X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KBrO3Concentration c (KBrO)3) In a linear relationship, the linear equation is t =21000c (KBrO)3)+229.9,R2= 0.9976. Thereby realizing the KBrO in the sample3And (4) carrying out quantitative detection.
Example 2:
(1) preparing a detection solution
Firstly, the raw materials are prepared by distilled water respectively0.2mol/L HCHO solution, 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 ℃.
Simultaneously, distilled water is used as a solvent to prepare a series of KBrO 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 146s 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 1.5mol/L KBrO was added to a 40mL pH clock system at the same time the reaction started3Sample solution of KBrO3Concentration in the test solution was 1.5X 10-3mol/L, KBrO added3The induction time was extended to 260s as shown in FIG. 6; for the other set, 40. mu.L of 2mol/L KBrO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KBrO3Concentration in the test solution was 2X 10-3mol/L, KBrO added3So that the induction time becomes 272s as shown in FIG. 7. FIGS. 6 and 7 confirm that KBrO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KBrO in the detection system3At a concentration of 5X 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 KBrO3Establishing a working curve relating concentration to induction time in the detection system, e.g.FIG. 8 shows, wherein the abscissa is KBrO in a pH clock system3Concentration c (KBrO)3) The ordinate is the induction time t when KBrO in the detection system3At a concentration of 5X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KBrO3Concentration c (KBrO)3) In a linear relationship, the linear equation is t =21200c (KBrO)3)+230.9,R2= 0.9954. Thereby realizing the KBrO in the sample3And (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 ℃.
Simultaneously, distilled water is used as a solvent to prepare a series of KBrO 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 group, 40. mu.L of 2mol/L KBrO was added to a 40mL pH clock system at the same time the reaction started3Sample solution of KBrO3The concentration in the test solution was 2.0X 10-3mol/L, KBrO added3The induction time was extended to 272s as shown in FIG. 10; for the other group, 40. mu. L2.5mol/L KBrO was added to a 40mL pH clock system at the same time as the reaction started3Sample solution of KBrO3The concentration in the test solution was 2.5X 10-3mol/L, KBrO added3The induction time was changed to 283s as shown in FIG. 11. FIGS. 10 and 11 confirm that KBrO in the detection solution3The different concentrations of (a) result in different induction times for the presence of the pH clock system. When KBrO in the detection system3At a concentration of 5X 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 KBrO3Concentration versus induction time in the assay system a working curve was established as shown in FIG. 12, where the abscissa is KBrO in a pH clock system3Concentration c (KBrO)3) The ordinate is the induction time t when KBrO in the detection system3At a concentration of 5X 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KBrO3Concentration c (KBrO)3) In a linear relationship, the linear equation is t =21600c (KBrO)3)+229.6,R2= 0.9969. Thereby realizing the KBrO in the sample3And (4) carrying out quantitative detection.
Claims (5)
1. KBrO3The 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: HCHO 0.045-0.0625mol/L, NaHSO3 0.045-0.0625mol/L、Na2SO3 0.0045-0.00625mol/L；
The sample to be detected is KBrO3And (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 KBrO of the solution to be detected3Concentration in a pH clock system, the ordinate being the induction time t; when KBrO is in the system3The concentration is 5.0 × 10-4mol/L to 2.5X 10-3Between mol/L, induction time t and KBrO3The concentration of the KBrO in the sample is in a linear relation, thereby realizing the KBrO in the sample3And (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: KBrO3The 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 KBrO3The temperature of the pH clock system was controlled at 12 ℃ while in solution.
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| CN114184658A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
| CN114184659A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Distinguishing Fe2+And Fe3+Method (2) |
| CN114184660A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Hexavalent iron FeO with different valence states for distinguishing iron42-And ferric iron Fe3+Method (2) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114184658A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
| CN114184659A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Distinguishing Fe2+And Fe3+Method (2) |
| CN114184660A (en) * | 2021-12-13 | 2022-03-15 | 安徽大学 | Hexavalent iron FeO with different valence states for distinguishing iron42-And ferric iron Fe3+Method (2) |
| CN114184658B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
| CN114184660B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Hexavalent iron FeO with different valence states for distinguishing iron 42- And ferric iron Fe 3+ Is a method of (2) |
| CN114184659B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Distinguishing Fe 2+ And Fe (Fe) 3+ Is a method of (2) |
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