CN113219025B - Method for quantitatively detecting potassium bromate - Google Patents
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Abstract
The present invention relates to a quantitative detection method for KBrO 3 Is characterized in that: application of HCHO-NaHSO 3 ‑Na 2 SO 3 "pH clock reaction System as detection solution, KBrO with different concentrations according to the System 3 Different responses, i.e. different realization of induction time for KBrO 3 Is a quantitative analysis of (a). The invention relates to a pair KBrO 3 The quantitative analysis method has the characteristics of high accuracy, easiness in operation, convenience, quickness and the like.
Description
Technical Field
The invention relates to an analysis and detection method, in particular to a method for establishing HCHO-NaHSO 3 - Na 2 SO 3 "pH clock system as substrate, according to which KBrO is used for different concentrations 3 Different responses, i.e. different induction times, for potassium bromate (KBrO 3 ) The quantitative analysis method of (2) belongs to the analytical chemistry field.
Background
Potassium bromate with molecular formula of KBrO 3 The method is mainly used as an analysis reagent, an oxidant and a wool bleaching treatment agent. Has irritation to eyes, skin and mucous membrane, and can cause nausea, emesis, stomach ache, blood and diarrhea after oral administration, and has certain harm to environment. Bromate composed of bromate ions is a byproduct generated by sterilizing natural water sources such as mineral water, mountain spring water and the like by ozone, so that it is particularly important to ensure that the bromate content in the mineral water accords with the drinking water standard. Thus for KBrO 3 The detection of (c) becomes critical.
For KBrO 3 The detection method of (2) comprises inductively coupled plasma mass spectrometryA method, an atomic absorption method, a spectrophotometry method, an electrochemical method, a neutron activation method, a chemiluminescent method, and the like. However, such detection methods mostly require large equipment and the tests are currently expensive and unsuitable for on-site determination. Therefore, it is necessary to find a detection and analysis method which has good detection effect and is simple and convenient and quick to operate.
Disclosure of Invention
The invention aims at KBrO 3 Provides a new quantitative detection method, namely, HCHO-NaHSO is adopted 3 - Na 2 SO 3 "pH clock system is detection solution pair KBrO 3 Quantitative detection method based on the pH clock system for KBrO 3 A standard curve (working curve) method developed for the sensitive response of (a) a test sample. Specifically, "HCHO-NaHSO 3 - Na 2 SO 3 The pH clock reaction system is used as a detection solution, and a map of pH change along with time is recorded; when the pH clock reaction starts, a series of KBrO to be detected with different concentrations are respectively carried out 3 The sample solution is added into the pH clock system in an equal volume, and the KBrO to be detected is realized according to the difference of the induction time generated by the system when the concentration of the solution to be detected in the pH clock system is different 3 And (5) quantitatively detecting the sample.
According to KBrO 3 Establishing a working curve according to the relation between the concentration and the induction time in the pH clock system; wherein the abscissa is KBrO 3 The concentration in the pH-clocked system, the ordinate is the induction time t, when KBrO in the system 3 The concentration is 5.0X10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and KBrO 3 The concentration of (2) is linear once, thereby realizing the effect of KBrO in the sample 3 Is a quantitative detection of (a).
The quantitative detection method is different from the prior art in that the method applies HCHO-NaHSO 3 - Na 2 SO 3 "pH clock System as detection solution, and the System for different concentrations of KBrO 3 The response to KBrO is different, namely the induction time is different 3 Is a quantitative analysis of (a).
KBrO 3 After the detection of the solution (pHThe detected concentration range in the clock system) is 5.0X10 -4 -2.5×10 - 3 mol/L。
KBrO 3 When the pH value is detected in the detection solution (pH value clock system), the temperature of the pH value clock system is controlled to be any specific temperature in the range of 10-15 ℃.
KBrO using the pH clock system described above 3 The concentration range that can be detected is the experimentally determined optimal concentration range. Within this concentration range, the induction time versus KBrO 3 The concentration change has good response and the linear correlation coefficient is large. In addition, the concentration ranges of the components in the detection solution (pH clock system) are shown in table 1, and the optimal concentrations of the detection solution (pH clock system) obtained through a plurality of experiments are shown in table 2:
table 1: concentration of each component in a pH clock system
| HCHO(mol/ L) | NaHSO 3 (mol/L) | Na 2 SO 3 (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) | NaHSO 3 (mol/L) | Na 2 SO 3 (mol/L) |
| 0.051 | 0.0495 | 0.00495 |
The specific experimental steps are as follows:
1. preparing a detection solution (pH clock system) with the concentration range of 0.5mol/L to 2.5mol/L, wherein the temperature is controlled to be a specific temperature value between 10 ℃ and 15 ℃ and is kept unchanged; the prepared working electrode (pH composite electrode, lei Ci, E-331) was inserted into the solution, the other end of the working electrode was connected to a computer through a potential/temperature/pH integrated tester (ZHFX-595, jiaxing Disheng electronic technologies Co., ltd.), and after the chemical signal acquisition and analysis program in the computer was opened to set the acquisition time and sampling speed, the start key was clicked rapidly to monitor the pH of the solution. The computer records the acquired pH profile, i.e., pH clock profile, over time. When the 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 is started, and the pH clock pattern of the pH change along with time is recorded in the same way.
Basic parameters of the pH clock profile 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 the pH jump is changed to the pH corresponding to the end of the pH jump.
2. Establishing KBrO in the detection solution 3 Working curve of concentration versus pH induction time
Preparing KBrO with concentration of 0.5mol/L-2.5mol/L by using distilled water as solvent 3 The solution is taken as a sample solution and reacts at the pH clock systemSimultaneously, 40 mu L of sample solutions with different concentrations are respectively added into a pH clock system of 40mL by a liquid-transferring gun, so that KBrO in the system 3 The concentration is 5.0X10 -4 mol/L to 2.5X10 -3 mol/L; the response variable of the pH clock system is the induction time and is marked as t; KBrO when in system 3 When the concentration is different, the induction time t of the pH clock system is also different; by KBrO in the system 3 Concentrations are plotted on the abscissa and t is plotted on the ordinate; when KBrO is in the system 3 The concentration is 5.0X10 - 4 mol/L to 2.5X10 -3 Between mol/L, the pH clock system induction time t and KBrO 3 The concentration of (2) is linear once to obtain a working curve.
3. For KBrO 3 Quantitative detection of (2)
Adding a sample to be detected with unknown concentration into the pH clock system of the detection solution at the beginning of the reaction of the pH clock system, measuring the induction time (t) of the corresponding pH clock system, and obtaining KBrO in the detection system according to the corresponding relation between t and the concentration on the working curve 3 Further calculate KBrO in the sample to be measured 3 Is a concentration of (3).
Drawings
FIG. 1 is a graph showing the pH of a detection solution (pH clock system) with time when a sample to be detected is not added in example 1.
FIG. 2 is a schematic diagram of example 1, incorporating 5X 10 -4 mol/LKBrO 3 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 3 is a schematic diagram of example 1, incorporating 1X 10 -3 mol/L KBrO 3 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 4 shows the pH induction time t and KBrO in example 1 3 Working curves between concentrations.
FIG. 5 is a graph showing the pH of the test solution (pH clock system) with time when no sample to be tested was added in example 2.
FIG. 6 is a schematic diagram of example 2, incorporating 1.5X10 -3 mol/L KBrO 3 After that, the solution was detected (pH clock system) profile of pH over time.
FIG. 7 is a schematic diagram of example 2 incorporating 2X 10 -3 mol/L KBrO 3 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 8 is a graph showing the pH induction time t and KBrO in example 2 3 Working curves between concentrations.
FIG. 9 is a graph showing the pH of the test solution (pH clock system) with time when no sample to be tested was added in example 3.
FIG. 10 is a schematic diagram of example 3 incorporating 2X 10 -3 mol/L KBrO 3 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 11 is a diagram of example 3, incorporating 2.5X10 -3 mol/L KBrO 3 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 12 is a graph showing the pH induction time t and KBrO in example 3 3 Working curves between concentrations.
Detailed Description
Example 1
Application to HCHO-NaHSO 3 - Na 2 SO 3 "pH clock system as substrate as detection solution for KBrO 3 Quantitative analysis was performed. Equal volumes of KBrO at different concentrations 3 Sample solution is put into a pH clock system to establish KBrO in a detection system 3 The working curve (such as linear relation) of the relation between the concentration and the induction time achieves the detection of KBrO in a pH clock system 3 Further to calculate KBrO in the test sample 3 Is a concentration of (3).
(1) Preparing a detection solution
Firstly, distilled water is used for preparing HCHO solution with the concentration of 0.2mol/L and NaHSO with the concentration of 0.1mol/L respectively 3 And 0.01mol/L Na 2 SO 3 Is a mixed solution of (a) and (b). To a 50mL small beaker was added 10.0mL of distilled water and 19.8mL of NaHSO in sequence 3 - Na 2 SO 3 Mixing the solution, 10.2mL of 0.2mol/L HCHO solution to ensure "HCHO-NaHSO 3 - Na 2 SO 3 Groups in a pH clock systemThe concentration of the fraction is HCHO 0.051mol/L, naHSO 3 0.0495mol/L、Na 2 SO 3 0.00495mol/L, total volume 40mL, temperature was controlled at 12 ℃.
Simultaneously distilled water is used as solvent to prepare a series of KBrO with different concentrations 3 Sample solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the prepared test solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no test sample added). As shown in fig. 1. The pH induction time was 145s for blank control. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one of the groups, 40. Mu.L of 0.5mol/L KBrO was added to a pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 5X 10 -4 mol/L, KBrO added 3 Such that the induction time was prolonged to 241s as shown in fig. 2; for the other group, 40. Mu.L of 1mol/L KBrO was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 1X 10 -3 mol/L, KBrO added 3 Such that the induction time became 251s as shown in fig. 3. FIGS. 2 and 3 demonstrate the detection of KBrO in solution 3 The difference in concentration of (2) leads to a difference in the induction time of the occurrence of the pH clock system. When KBrO is detected in a system 3 Is at a concentration of 5.0X10 -4 mol/L to 2.5X10 -3 The results of different induction times of the pH clock system due to different concentrations between mol/L can be observed.
(3) Quantitative detection
According to KBrO 3 The concentration in the assay system versus the induction time establishes an operating curve as shown in FIG. 4, wherein the abscissa is KBrO in the pH clock system 3 Concentration c (KBrO) 3 ) The ordinate is the induction time t, when KBrO is detected in the system 3 Is at a concentration of 5.0X10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and KBrO 3 Concentration c (KBrO) 3 ) In a linear relation, the linear equation ist=21000c(KBrO 3 )+229.9,R 2 = 0.9976. Thus, KBrO in the sample can be realized 3 Is a quantitative detection of (a).
Example 2:
(1) Preparing a detection solution
Firstly, distilled water is used for preparing HCHO solution with the concentration of 0.2mol/L and NaHSO with the concentration of 0.1mol/L respectively 3 And 0.01mol/L Na 2 SO 3 Is a mixed solution of (a) and (b). 9.5mL of distilled water solution and 20.0mL of NaHSO were added sequentially to a 50mL small beaker 3 - Na 2 SO 3 Mixing the solution, 10.5mL of 0.2mol/L HCHO solution to ensure "HCHO-NaHSO 3 - Na 2 SO 3 "the concentration of each component in the pH clock system is HCHO 0.0525mol/L, naHSO 3 0.05mol/L、Na 2 SO 3 0.005mol/L, total volume of 40mL, and temperature was controlled at 12 ℃.
Simultaneously distilled water is used as solvent to prepare a series of KBrO with different concentrations 3 Sample solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the prepared test solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no test sample added), as shown in FIG. 5. The pH induction time was 146s for blank control. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one of the groups, 40. Mu.L of 1.5mol/L KBrO was added to a pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 1.5X10 -3 mol/L, KBrO added 3 Such that the induction time was prolonged to 260s as shown in fig. 6; for the other group, 40. Mu.L of 2mol/L KBrO was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 2X 10 -3 mol/L, KBrO added 3 Such that the induction time became 272s as shown in fig. 7. FIGS. 6 and 7 demonstrate the detection of KBrO in solution 3 The difference in concentration of (2) leads to a difference in the induction time of the occurrence of the pH clock system. When KBrO is detected in a system 3 Is at a concentration of 5X 10 -4 mol/L to2.5×10 -3 The results of different induction times of the pH clock system due to different concentrations in mol/L can be observed.
(3) Quantitative detection
According to KBrO 3 The concentration in the assay system versus the induction time establishes an operating curve as shown in FIG. 8, wherein the abscissa is KBrO in the pH clock system 3 Concentration c (KBrO) 3 ) The ordinate is the induction time t, when KBrO is detected in the system 3 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and KBrO 3 Concentration c (KBrO) 3 ) In a linear relationship, the linear equation is t=21200c (KBrO 3 )+230.9,R 2 = 0.9954. Thus, KBrO in the sample can be realized 3 Is a quantitative detection of (a).
Example 3:
(1) Preparing a detection solution
Firstly, distilled water is used for preparing HCHO solution with the concentration of 0.2mol/L and NaHSO with the concentration of 0.1mol/L respectively 3 And 0.01mol/L Na 2 SO 3 Is a mixed solution of (a) and (b). To a 50mL small beaker was added 10.2mL of distilled water solution, 20.0mL of NaHSO in sequence 3 - Na 2 SO 3 Mixing the solution, 9.8mL of 0.2mol/L HCHO solution to ensure "HCHO-NaHSO 3 - Na 2 SO 3 "the concentration of each component in the pH clock system is HCHO 0.049mol/L, naHSO 3 0.05mol/L、Na 2 SO 3 0.005mol/L, total volume of 40mL, and temperature was controlled at 12 ℃.
Simultaneously distilled water is used as solvent to prepare a series of KBrO with different concentrations 3 Sample solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the prepared test solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no test sample added). As shown in fig. 9. The pH induction time was 144s for the blank. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one of the groups, 40. Mu.L of 2mol/L KBrO was added to a pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 2.0X10 -3 mol/L, KBrO added 3 Such that the induction time was extended to 272s as shown in fig. 10; for the other group, 40. Mu.L of 2.5mol/L KBrO was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, such that KBrO 3 The concentration in the detection solution was 2.5X10 -3 mol/L, KBrO added 3 So that the induction time became 283s as shown in FIG. 11. FIGS. 10 and 11 demonstrate the detection of KBrO in solution 3 The difference in concentration of (2) leads to a difference in the induction time of the occurrence of the pH clock system. When KBrO is detected in a system 3 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 The results of different induction times of the pH clock system due to different concentrations between mol/L can be observed.
(3) Quantitative detection
According to KBrO 3 The concentration in the assay system versus the induction time establishes an operating curve as shown in FIG. 12, wherein the abscissa is KBrO in the pH clock system 3 Concentration c (KBrO) 3 ) The ordinate is the induction time t, when KBrO is detected in the system 3 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and KBrO 3 Concentration c (KBrO) 3 ) In a linear relationship, the linear equation is t=21600c (KBrO 3 )+229.6,R 2 =0.9969. Thus, KBrO in the sample can be realized 3 Is a quantitative detection of (a).
Claims (5)
1. KBrO 3 The quantitative detection method of (2) is characterized in that:
distilled water is used as a solvent to prepare a solution of a sample to be detected;
application of HCHO-NaHSO 3 - Na 2 SO 3 The pH clock reaction system is used as a detection solution, and a map of pH change along with time is recorded; the temperature of the pH clock system is controlled to be within the range of 10-15 ℃ at any specific temperature, when the pH clock reaction starts, the equal volumes of the series of sample solutions to be detected with different concentrations are respectively added into the pH clock system according to the following conditionsWhen the concentration of the solution to be detected in the pH clock system is different, the induction time generated by the system is different, so that the quantitative detection of the sample to be detected is realized;
the molar concentration ranges of the components in the detection solution are as follows: HCHO 0.045-0.0625mol/L, naHSO 3 0.045-0.0625mol/L、Na 2 SO 3 0.0045-0.00625mol/L；
The sample to be detected is KBrO 3 A solution.
2. The quantitative detection method according to claim 1, wherein: establishing a working curve according to the relation between the concentration of the solution to be detected in the pH clock system and the induction time; wherein the abscissa is the solution KBrO to be detected 3 Concentration in pH clock system, ordinate is induction time t; when KBrO is in the system 3 The concentration is 5.0X10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and KBrO 3 Is linear in relation to the concentration of KBrO in the sample 3 Is a quantitative detection of (a).
3. The quantitative detection 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, naHSO 3 0.0495mol/L、Na 2 SO 3 0.00495mol/L。
4. The quantitative detection method according to claim 1 or 2, characterized in that: KBrO 3 The concentration of the solution in the detection solution was detectable in the range of 5.0X10 -4 mol/L to 2.5X10 -3 mol/L。
5. The quantitative detection method according to claim 1 or 2, characterized in that: detection of KBrO 3 The temperature of the pH clock system was controlled at 12℃at the time of solution.
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| CN114184658B (en) * | 2021-12-13 | 2024-04-02 | 安徽大学 | Method for distinguishing potassium chlorate and potassium bromate |
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| 时钟反应系 HCHO-HSO_3~--SO_3~(2-)的 pH 突跃法测定 HSO_3~-盐的含量;黄承高;胡奇林;赵福祯;马璀;朱妙丽;;分析化学(07);619-621 * |
| 试用H_2O_2-KI-H_2SO_4-Na_2S_2O_3反应系列的"计时法"测定S_2O_3~(2-)盐的含量;黄承高;胡奇林;曹瑞;马兰英;于效东;;分析化学(09);824-827 * |
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