CN113219027B - A method for quantitatively detecting potassium iodate - Google Patents
A method for quantitatively detecting potassium iodate Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 10
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 title description 4
- 239000001230 potassium iodate Substances 0.000 title description 4
- 229940093930 potassium iodate Drugs 0.000 title description 4
- 235000006666 potassium iodate Nutrition 0.000 title description 4
- 238000001514 detection method Methods 0.000 claims abstract description 87
- 230000006698 induction Effects 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000000523 sample Substances 0.000 claims description 17
- 239000012488 sample solution Substances 0.000 claims description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 5
- 238000004445 quantitative analysis Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 53
- 239000011259 mixed solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 3
- ZOUPQAHVXDDBIS-UHFFFAOYSA-K trisodium;hydrogen sulfite;sulfite Chemical compound [Na+].[Na+].[Na+].OS([O-])=O.[O-]S([O-])=O ZOUPQAHVXDDBIS-UHFFFAOYSA-K 0.000 description 3
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 206010067997 Iodine deficiency Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 208000024799 Thyroid disease Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 235000010037 flour treatment agent Nutrition 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 208000021510 thyroid gland disease Diseases 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 230000004614 tumor growth Effects 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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Abstract
Description
技术领域technical field
本发明涉及一种分析检测方法，具体地说是建立“HCHO- NaHSO3 - Na2SO3”为底物的pH时钟体系，根据该体系对于不同浓度的KIO3的响应不同即诱导时间的不同实现对于碘酸钾（KIO3）的定量分析方法，属于分析化学领域。The present invention relates to an analysis and detection method, specifically to establish a pH clock system with "HCHO-NaHSO 3 -Na 2 SO 3 " as a substrate, and realize a quantitative analysis method for potassium iodate (KIO 3 ) according to the different responses of the system to different concentrations of KIO 3 , that is, the difference in induction time, and belongs to the field of analytical chemistry.
背景技术Background technique
碘酸钾，分子式为KIO3，是化学分析中的分析试剂。作为添加剂，如配制氧化还原滴定标准溶液，作氧化剂。对钽等元素进行微量分析。也用作络合剂、掩蔽剂、细菌抑制剂等。用作家畜饲料添加剂。动物饲料中作为调节缺碘的添加剂。用作小麦面粉处理剂、面团改质剂、食盐加碘剂。FDA（§184.1635，2000）规定可用于面包，最高限量为0.0075%（以小麦面粉量计）。我国规定可用于固体饮料，限量0.26～0.4mg/kg。可用作防止地方甲状腺病的加碘食盐或药剂。近年来碘酸钾作为抗肿瘤药物，发现在某种情况下具有抑制肿瘤生长的作用。因此对于KIO3的检测变得至关重要。Potassium iodate, molecular formula KIO 3 , is an analytical reagent in chemical analysis. As an additive, such as the preparation of redox titration standard solution, as an oxidizing agent. Trace analysis of elements such as tantalum. It is also used as complexing agent, masking agent, bacterial inhibitor, etc. Used as livestock feed additive. Animal feed as an additive to regulate iodine deficiency. Used as wheat flour treatment agent, dough modifier, salt iodizing agent. FDA (§184.1635, 2000) stipulates that it can be used in bread, and the maximum limit is 0.0075% (based on the amount of wheat flour). my country stipulates that it can be used in solid beverages, with a limit of 0.26-0.4mg/kg. It can be used as iodized salt or medicine to prevent endemic thyroid disease. In recent years, potassium iodate, as an antitumor drug, has been found to have the effect of inhibiting tumor growth under certain circumstances. Therefore, the detection of KIO 3 becomes crucial.
目前对于KIO3的检测方法包括电感耦合等离子体质谱法、原子吸收法、分光光度法、电化学法、中子活化法、化学发光法等。但是此类检测方法大多需要较大设备并且测试价格昂贵，不适合现场的测定。因此寻找一种检测效果好且操作简便快速的检测分析方法就显得十分必要。The current detection methods for KIO 3 include inductively coupled plasma mass spectrometry, atomic absorption method, spectrophotometry, electrochemical method, neutron activation method, chemiluminescence method and so on. However, most of these detection methods require large equipment and are expensive to test, so they are not suitable for on-site determination. Therefore, it is very necessary to find a detection and analysis method with good detection effect and simple and fast operation.
发明内容Contents of the invention
本发明旨在为KIO3提供一种新的定量检测方法，即以“HCHO- NaHSO3 - Na2SO3”pH时钟体系为检测溶液对KIO3进行定量检测的方法，本方法是基于该pH时钟体系对KIO3的敏感响应而开发的一种标准曲线（工作曲线）法。具体地说，应用“HCHO- NaHSO3 - Na2SO3”pH时钟反应体系作为检测溶液，记录pH随时间变化的图谱；当pH时钟反应开始时，分别将系列不同浓度的待检测KIO3样品溶液等体积加入到pH时钟体系中，根据待检测溶液在pH时钟体系中的浓度不同时，体系所产生的诱导时间的不同，实现对于待检测KIO3样品的定量检测。The present invention aims to provide a new quantitative detection method for KIO3 , that is, a method for quantitative detection of KIO3 using the "HCHO- NaHSO3 - Na2SO3 " pH clock system as the detection solution. This method is a standard curve (working curve) method developed based on the sensitive response of the pH clock system to KIO3 . Specifically, the “HCHO-NaHSO 3 -Na 2 SO 3 ” pH clock reaction system was used as the detection solution, and the graph of pH changing with time was recorded; when the pH clock reaction started, a series of different concentrations of the KIO 3 sample solutions to be detected were added in equal volumes to the pH clock system, and the quantitative detection of the KIO 3 samples to be detected was realized according to the different concentrations of the solutions to be detected in the pH clock system and the differences in the induction time produced by the system.
根据KIO3在pH时钟体系中的浓度和诱导时间的关系建立工作曲线；其中横坐标是KIO3在pH时钟体系中的浓度，纵坐标是诱导时间t，当体系中KIO3浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时，诱导时间t与KIO3的浓度成一次线性关系，据此可以实现对试样中KIO3的定量检测。The working curve was established according to the relationship between the concentration of KIO 3 in the pH clock system and the induction time; the abscissa is the concentration of KIO 3 in the pH clock system, and the ordinate is the induction time t. When the concentration of KIO 3 in the system is between 5.0×10 -4 mol/L and 2.5×10 -3 mol/L, the induction time t has a linear relationship with the concentration of KIO 3 , and the quantitative detection of KIO 3 in the sample can be realized accordingly.
本定量检测方法与现有技术的区别在于，本发明应用“HCHO- NaHSO3 - Na2SO3”pH时钟体系作为检测溶液，以及该体系对于不同浓度的KIO3的响应不同即诱导时间的不同，实现对于KIO3的定量分析。The difference between this quantitative detection method and the prior art is that the present invention uses the “HCHO-NaHSO 3 -Na 2 SO 3 ” pH clock system as the detection solution, and the response of the system to different concentrations of KIO 3 is different, that is, the induction time is different, so as to realize the quantitative analysis of KIO 3 .
KIO3在检测溶液（pH时钟体系）中的被检测的浓度范围为5.0×10-4-2.5×10-3mol/L。The detected concentration range of KIO 3 in the detection solution (pH clock system) is 5.0×10 -4 -2.5×10 -3 mol/L.
KIO3在检测溶液（pH时钟体系）中被检测时，pH时钟体系温度被控制在10-15℃范围内任意一个特定的温度。When KIO 3 is detected in the detection solution (pH clock system), the temperature of the pH clock system is controlled at any specific temperature within the range of 10-15°C.
利用上述pH时钟体系，KIO3可被检测的浓度范围是经实验确定的最优浓度范围。在该浓度范围内，诱导时间对KIO3浓度变化有很好的响应，线性相关系数大。另外，检测溶液（pH时钟体系）中各组分的浓度范围如表1所示，经过多次实验得到的检测溶液（pH时钟体系）的最佳浓度如表2所示：Using the above pH clock system, the detectable concentration range of KIO 3 is the optimal concentration range determined through experiments. In this concentration range, the induction time has a good response to the change of KIO 3 concentration, and the linear correlation coefficient is large. In addition, the concentration range of each component in the detection solution (pH clock system) is shown in Table 1, and the optimal concentration of the detection solution (pH clock system) obtained after many experiments is shown in Table 2:
表1：pH时钟体系中各组分的浓度Table 1: Concentrations of components in the pH clock system
表2：pH时钟体系中各组分的最佳浓度Table 2: Optimum concentrations of components in the pH clock system
具体实验步骤如下：The specific experimental steps are as follows:
1、按表1规定的浓度范围配制40mL检测溶液（pH时钟体系），其温度被控制在10-15℃之间的某一特定的温度值保持不变；将准备好的工作电极（pH复合电极，雷磁，E-331）插入溶液中，工作电极的另一端通过电位/温度/pH综合测试仪（嘉兴迪生电子科技有限公司，ZHFX-595）连接至电脑，打开电脑中化学信号采集分析程序对采集时间和取样速度进行设置后，迅速点击开始键对溶液进行pH监测。计算机记录所采集的pH随时间变化的曲线，即pH时钟图谱。当需要检测物质的时候，在pH时钟体系反应开始的同时迅速加入待检测物，按相同的方式记录pH随时间变化的pH时钟图谱。1. Prepare 40mL detection solution (pH clock system) according to the concentration range specified in Table 1, and its temperature is controlled at a specific temperature value between 10-15°C and remains unchanged; insert the prepared working electrode (pH composite electrode, Lei Magnetic, E-331) into the solution, and connect the other end of the working electrode to the computer through a potential/temperature/pH comprehensive tester (Jiaxing Disheng Electronic Technology Co., Ltd., ZHFX-595). Click the start button to monitor the pH of the solution. The computer records the curve of the collected pH changing with time, that is, the pH clock map. When a substance needs to be detected, the substance to be detected is quickly added at the same time as the reaction of the pH clock system starts, and the pH clock spectrum of pH changing with time is recorded in the same way.
pH时钟图谱的基本参数包括：The basic parameters of the pH clock map include:
诱导时间：从pH时钟体系反应开始到pH突跃所需的时间。Induction time: the time required from the start of the pH clock system reaction to the pH jump.
pH突跃范围：pH突跃开始对应的pH到pH突跃结束对应的pH。pH jump range: the pH corresponding to the start of the pH jump to the pH corresponding to the end of the pH jump.
2、建立检测溶液中KIO3浓度与pH诱导时间之间关系的工作曲线2. Establish a working curve for the relationship between the concentration of KIO 3 in the detection solution and the pH induction time
用蒸馏水为溶剂配制浓度为0.5mol/L到2.5mol/L的KIO3溶液作为样本溶液，在pH时钟体系反应开始的同时，分别用移液枪向40 mL的pH时钟体系中加入40μL所述系列不同浓度的样品溶液, 使得体系中KIO3浓度为5.0×10-4mol/L到2.5×10-3mol/L之间；pH时钟体系响应的变化量为诱导时间，记为t；当体系中的KIO3浓度不同时，pH时钟体系诱导时间t也不同；以体系中KIO3浓度为横坐标，以t为纵坐标作图；当体系中KIO3浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时，pH时钟体系诱导时间t与KIO3的浓度成一次线性关系，得到工作曲线。Use distilled water as a solvent to prepare KIO with a concentration of 0.5mol/L to 2.5mol/L3The solution is used as the sample solution. At the same time when the reaction of the pH clock system starts, add 40 μL of the sample solution of the series of different concentrations to the 40 mL pH clock system with a pipette gun, so that the KIO in the system3The concentration is 5.0×10-4mol/L to 2.5×10-3mol/L; the change in response of the pH clock system is the induction time, denoted as t; when the KIO in the system3When the concentration is different, the induction time t of the pH clock system is also different;3Concentration is the abscissa and t is the ordinate; when KIO in the system3Concentration at 5.0×10-4mol/L to 2.5×10-3Between mol/L, pH clock system induction time t and KIO3The concentration becomes a linear relationship, and the working curve is obtained.
3、对KIO3的定量检测3. Quantitative detection of KIO 3
将某浓度未知的待测试样在pH时钟体系反应开始时加入到检测溶液pH时钟体系中，可以测出对应的pH时钟体系的诱导时间（t），根据工作曲线上t与浓度之间的对应关系，可求得检测体系中KIO3的浓度，进而计算出待测试样中KIO3的浓度。Add a sample to be tested with an unknown concentration into the pH clock system of the detection solution at the beginning of the pH clock system reaction, and the induction time (t) of the corresponding pH clock system can be measured. According to the corresponding relationship between t and concentration on the working curve, the concentration of KIO in the detection system can be obtained, and then the concentration of KIO in the test sample can be calculated.
附图说明Description of drawings
图1是实施例1中，未加入待检测样品时，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 1 is a graph showing the pH value of the detection solution (pH clock system) changing with time in Example 1 when no sample to be detected is added.
图2是实施例1中，加入5.0×10-4mol/LKIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 2 is a chromatogram of the pH value of the detection solution (pH clock system) changing with time after adding 5.0×10 -4 mol/L KIO 3 in Example 1.
图3是实施例1中，加入1.0×10-3mol/L KIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 3 is a chromatogram of the pH value of the detection solution (pH clock system) changing with time after adding 1.0×10 -3 mol/L KIO 3 in Example 1.
图4是实施例1中，pH诱导时间t与KIO3浓度之间的工作曲线。Fig. 4 is in embodiment 1, the working curve between pH induction time t and KIO 3 concentration.
图5是实施例2中，未加入待检测样品时，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 5 is a graph of the pH value of the detection solution (pH clock system) changing with time in Example 2 when no sample to be detected is added.
图6是实施例2中，加入1.5×10-3mol/L KIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 6 is a chromatogram of the pH value of the detection solution (pH clock system) changing with time after adding 1.5×10 -3 mol/L KIO 3 in Example 2.
图7是实施例2中，加入2.0×10-3mol/L KIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 7 is a graph showing the pH value of the detection solution (pH clock system) changing with time after adding 2.0×10 -3 mol/L KIO 3 in Example 2.
图8是实施例2中，pH诱导时间t与KIO3浓度之间的工作曲线。Fig. 8 is in embodiment 2, the working curve between pH induction time t and KIO 3 concentration.
图9是实施例3中，未加入待检测样品时，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 9 is a graph of the pH value of the detection solution (pH clock system) changing with time in Example 3 when no sample to be detected is added.
图10是实施例3中，加入2.0×10-3mol/LKIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 10 is a graph showing the change of pH value of the detection solution (pH clock system) with time after adding 2.0×10 -3 mol/L KIO 3 in Example 3.
图11是实施例3中，加入2.5×10-3mol/L KIO3后，检测溶液（pH时钟体系）pH值随时间变化的图谱。Fig. 11 is a graph showing the change of pH value of the detection solution (pH clock system) with time after adding 2.5×10 -3 mol/L KIO 3 in Example 3.
图12是实施例3中，pH诱导时间t与KIO3浓度之间的工作曲线。Fig. 12 is in embodiment 3, the working curve between pH induction time t and KIO 3 concentration.
具体实施方式Detailed ways
实施例1Example 1
应用以“HCHO- NaHSO3 - Na2SO3”为底物的pH时钟体系作为检测溶液，对KIO3进行定量分析。等体积加入不用浓度的KIO3样本溶液到pH时钟体系中，建立起检测体系中KIO3浓度与诱导时间之间关联的工作曲线（如线性关系），达到检测pH时钟体系中KIO3的目的，进而计算出待测试样中KIO3的浓度。The pH clock system with "HCHO-NaHSO 3 -Na 2 SO 3 " as the substrate was used as the detection solution for quantitative analysis of KIO 3 . Equal volumes of KIO 3 sample solutions with different concentrations were added to the pH clock system to establish a working curve (such as a linear relationship) between the concentration of KIO 3 in the detection system and the induction time to achieve the purpose of detecting KIO 3 in the pH clock system, and then calculate the concentration of KIO 3 in the sample to be tested.
(1) 配制检测溶液(1) Preparation of detection solution
首先用蒸馏水配制分别配制0.2mol/L的HCHO溶液、0.1mol/L的NaHSO3和0.01mol/L的Na2SO3的混合溶液。向50mL小烧杯中依次加入10.0mL 蒸馏水溶液、19.8mL NaHSO3 -Na2SO3混合溶液、10.2mL 0.2mol/L HCHO溶液，以保证“HCHO- NaHSO3 - Na2SO3”pH时钟体系中各组分的浓度为HCHO 0.051mol/L、NaHSO3 0.0495mol/L、Na2SO3 0.00495mol/L，总体积为40mL，温度被控制在14℃。Firstly, distilled water was used to prepare mixed solutions of 0.2 mol/L HCHO solution, 0.1 mol/L NaHSO 3 and 0.01 mol/L Na 2 SO 3 . Add 10.0mL distilled water solution, 19.8mL NaHSO 3 -Na 2 SO 3 mixed solution, 10.2mL 0.2mol/L HCHO solution to a 50mL small beaker in order to ensure that the concentration of each component in the “HCHO- NaHSO 3 - Na 2 SO 3 ” pH clock system is HCHO 0.051mol/L, NaHSO 3 0.0495mol/L, Na 2 SO 3 is 0.00495mol/L, the total volume is 40mL, and the temperature is controlled at 14°C.
同时以蒸馏水为溶剂，配制系列不同浓度的KIO3样品溶液。At the same time, distilled water was used as solvent to prepare a series of KIO 3 sample solutions with different concentrations.
（2）获得pH时钟图谱(2) Obtain pH clock map
配制好的检测溶液的pH值随时间变化的图谱由装有化学信号采集分析程序的计算机记录（未加入检测样品）。如图1所示。pH诱导时间为144.2s以作空白对照。另配置两组各组分浓度与上述检测溶液相同的检测溶液。对于其中一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL 0.5mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为5.0×10-4mol/L，加入的KIO3使得诱导时间延长为184s如图2所示；对于另一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL1.0mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为1.0×10-3mol/L，加入的KIO3使得诱导时间变为237s如图3所示。图2、图3证实了检测溶液中KIO3的浓度不同导致pH时钟体系出现的诱导时间不同。当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时,浓度不同导致pH时钟体系出现的诱导时间不同的结果都可以被观测到。The chromatogram of the pH value of the prepared detection solution changing with time is recorded by a computer equipped with a chemical signal acquisition and analysis program (no detection sample is added). As shown in Figure 1. The pH induction time was 144.2s as a blank control. Another two groups of detection solutions with the same concentration of each component as the above-mentioned detection solutions were prepared. For one of the groups, 40 μL of 0.5 mol/L KIO 3 sample solution was added to the 40 mL pH clock system at the same time as the reaction started, so that the concentration of KIO 3 in the detection solution was 5.0×10 -4 mol/L, and the added KIO 3 made the induction time prolong to 184s as shown in Figure 2; for the other group, 40 μL of 1.0 mol/L KIO 3 sample solution was added to the 40 mL pH clock system at the same time as the reaction started , so that the concentration of KIO 3 in the detection solution was 1.0×10 -3 mol/L, and the added KIO 3 made the induction time 237s , as shown in Figure 3 . Figure 2 and Figure 3 confirm that the different concentrations of KIO 3 in the detection solution lead to different induction times of the pH clock system. When the concentration of KIO 3 in the detection system is between 5.0×10 -4 mol/L and 2.5×10 -3 mol/L, different concentrations lead to different induction times of the pH clock system can be observed.
（3）定量检测(3) Quantitative detection
根据KIO3在检测体系中的浓度与诱导时间的关系建立工作曲线，如图4所示，其中横坐标是在pH时钟体系中的KIO3的浓度c(KIO3)，纵坐标是诱导时间t，当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时，诱导时间t与KIO3的浓度c(KIO3)成一次线性关系，线性方程为t=66400c(KIO3)+160.4,R2=0.9711。据此可以实现对试样中KIO3的定量检测。The working curve is established according to the relationship between the concentration of KIO3 in the detection system and the induction time, as shown in Figure 4, wherein the abscissa is the concentration c ( KIO3 ) of KIO3 in the pH clock system, and the ordinate is the induction time t. When the concentration of KIO3 in the detection system is between 5.0× 10-4 mol/L and 2.5× 10-3 mol/L, the induction time t has a linear relationship with the concentration c ( KIO3 ) of KIO3, and the linear equation is t =66400c(KIO 3 ) +160.4, R 2 =0.9711. Accordingly, the quantitative detection of KIO 3 in the sample can be realized.
实施例2：Example 2:
(1) 配制检测溶液(1) Preparation of detection solution
首先用蒸馏水配制分别配制0.2mol/L的HCHO溶液、0.1mol/L的NaHSO3和0.01mol/L的Na2SO3的混合溶液。向50mL小烧杯中依次加入9.5mL 蒸馏水溶液、20.0mL NaHSO3 -Na2SO3混合溶液、10.5mL 0.2mol/L HCHO溶液，以保证“HCHO- NaHSO3 - Na2SO3”pH时钟体系中各组分的浓度为HCHO 0.0525mol/L、NaHSO3 0.05mol/L、Na2SO3 0.005mol/L，总体积为40mL，温度被控制在12℃。Firstly, distilled water was used to prepare mixed solutions of 0.2 mol/L HCHO solution, 0.1 mol/L NaHSO 3 and 0.01 mol/L Na 2 SO 3 . Add 9.5mL distilled water solution, 20.0mL NaHSO 3 -Na 2 SO 3 mixed solution, 10.5mL 0.2mol/L HCHO solution to a 50mL small beaker in order to ensure that the concentration of each component in the "HCHO- NaHSO 3 - Na 2 SO 3 " pH clock system is HCHO 0.0525mol/L, NaHSO 3 0.05mol/L, Na 2 SO 3 0.005mol/L, the total volume is 40mL, and the temperature is controlled at 12°C.
同时以蒸馏水为溶剂，配制系列不同浓度的KIO3样品溶液。At the same time, distilled water was used as solvent to prepare a series of KIO 3 sample solutions with different concentrations.
（2）获得pH时钟图谱(2) Obtain pH clock map
配制好的检测溶液的pH值随时间变化的图谱由装有化学信号采集分析程序的计算机记录（未加入检测样品），如图5所示。pH诱导时间为144.1s以作空白对照。另配置两组各组分浓度与上述检测溶液相同的检测溶液。对于其中一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL1.5mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为1.5×10-3mol/L，加入的KIO3使得诱导时间延长为260s如图6所示；对于另一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL2.0mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为2.0×10-3mol/L，加入的KIO3使得诱导时间变为301s如图7所示。图6、图7证实了检测溶液中KIO3的浓度不同导致pH时钟体系出现的诱导时间不同。当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L,浓度不同导致pH时钟体系出现的诱导时间不同的结果都可以被观测到。The time-varying spectrum of the pH value of the prepared detection solution was recorded by a computer equipped with a chemical signal acquisition and analysis program (no detection sample was added), as shown in FIG. 5 . The pH induction time was 144.1s as a blank control. Another two groups of detection solutions with the same concentration of each component as the above-mentioned detection solutions were prepared. For one of the groups, at the beginning of the reaction, 40 μL of 1.5 mol/L KIO 3 sample solution was added to the 40 mL pH clock system, so that the concentration of KIO 3 in the detection solution was 1.5×10 -3 mol/L, and the added KIO 3 made the induction time extended to 260s as shown in Figure 6; for the other group, at the same time as the reaction started, 40 μL of 2.0 mol/L KIO 3 sample solution was added to the 40 mL pH clock system, The concentration of KIO 3 in the detection solution was 2.0×10 -3 mol/L, and the addition of KIO 3 made the induction time 301s , as shown in FIG. 7 . Figure 6 and Figure 7 confirm that the different concentrations of KIO 3 in the detection solution lead to different induction times of the pH clock system. When the concentration of KIO 3 in the detection system is between 5.0×10 -4 mol/L and 2.5×10 -3 mol/L, different concentrations lead to different induction times of the pH clock system can be observed.
（3）定量检测(3) Quantitative detection
根据KIO3在检测体系中的浓度与诱导时间的关系建立工作曲线，如图8所示，其中横坐标是在pH时钟体系中的KIO3的浓度c(KIO3)，纵坐标是诱导时间t，当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时，诱导时间t与KIO3的浓度c(KIO3)成一次线性关系,线性方程为t=66800c(KIO3)+158.6,R2=0.98。据此可以实现对试样中KIO3的定量检测。Establish a working curve according to the relationship between the concentration of KIO3 in the detection system and the induction time, as shown in Figure 8, where the abscissa is the concentration c ( KIO3 ) of KIO3 in the pH clock system, and the ordinate is the induction time t. When the concentration of KIO3 in the detection system is between 5.0× 10-4 mol/L and 2.5× 10-3 mol/L, the induction time t has a linear relationship with the concentration c( KIO3 ) of KIO3, and the linear equation is t=6 6800c( KIO 3 ) +158.6, R 2 =0.98. Accordingly, the quantitative detection of KIO 3 in the sample can be realized.
实施例3：Example 3:
(1) 配制检测溶液(1) Preparation of detection solution
首先用蒸馏水配制分别配制0.2mol/L的HCHO溶液、0.1mol/L的NaHSO3和0.01mol/L的Na2SO3的混合溶液。向50mL小烧杯中依次加入10.2mL 蒸馏水溶液、20.0mL NaHSO3 -Na2SO3混合溶液、9.8mL 0.2mol/L HCHO溶液，以保证“HCHO- NaHSO3 - Na2SO3”pH时钟体系中各组分的浓度为HCHO 0.049mol/L、NaHSO3 0.05mol/L、Na2SO3 0.005mol/L，总体积为40mL，温度被控制在12℃。Firstly, distilled water was used to prepare mixed solutions of 0.2 mol/L HCHO solution, 0.1 mol/L NaHSO 3 and 0.01 mol/L Na 2 SO 3 . Add 10.2mL distilled aqueous solution, 20.0mL NaHSO 3 -Na 2 SO 3 mixed solution, 9.8mL 0.2mol/L HCHO solution to a 50mL small beaker in order to ensure that the concentration of each component in the "HCHO- NaHSO 3 - Na 2 SO 3 " pH clock system is HCHO 0.049mol/L, NaHSO 3 0.05mol/L, Na 2 SO 3 0.005mol/L, the total volume is 40mL, and the temperature is controlled at 12°C.
同时以蒸馏水为溶剂，配制系列不同浓度的KIO3样品溶液。At the same time, distilled water was used as solvent to prepare a series of KIO 3 sample solutions with different concentrations.
（2）获得pH时钟图谱(2) Obtain pH clock map
配制好的检测溶液的pH值随时间变化的图谱由装有化学信号采集分析程序的计算机记录（未加入检测样品）。如图9所示。pH诱导时间为144s以作空白对照。另配置两组各组分浓度与上述检测溶液相同的检测溶液。对于其中一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL2.0mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为2.0×10-3mol/L，加入的KIO3使得诱导时间延长为301s如图10所示；对于另一组，在反应开始的同时，向40 mL的pH时钟体系中加入40μL2.5mol/L的KIO3样品溶液，使得KIO3在检测溶液中的浓度为2.5×10-3mol/L，加入的KIO3使得诱导时间变为3181s如图11所示。图10、图11证实了检测溶液中KIO3的浓度不同导致pH时钟体系出现的诱导时间不同。当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时,浓度不同导致pH时钟体系出现的诱导时间不同的结果都可以被观测到。The chromatogram of the pH value of the prepared detection solution changing with time is recorded by a computer equipped with a chemical signal acquisition and analysis program (no detection sample is added). As shown in Figure 9. The pH induction time was 144s as a blank control. Another two groups of detection solutions with the same concentration of each component as the above-mentioned detection solutions were prepared. For one of the groups, at the beginning of the reaction, 40 μL of 2.0 mol/L KIO 3 sample solution was added to the 40 mL pH clock system, so that the concentration of KIO 3 in the detection solution was 2.0×10 -3 mol/L, and the added KIO 3 made the induction time prolong to 301s as shown in Figure 10; for the other group, at the same time as the reaction started, 40 μL of 2.5 mol/L KIO 3 sample solution was added to the 40 mL pH clock system , so that the concentration of KIO 3 in the detection solution was 2.5×10 -3 mol/L, and the added KIO 3 made the induction time 3181s, as shown in Figure 11 . Figure 10 and Figure 11 confirm that the different concentrations of KIO 3 in the detection solution lead to different induction times of the pH clock system. When the concentration of KIO 3 in the detection system is between 5.0×10 -4 mol/L and 2.5×10 -3 mol/L, different concentrations lead to different induction times of the pH clock system can be observed.
（3）定量检测(3) Quantitative detection
根据KIO3在检测体系中的浓度与诱导时间的关系建立工作曲线，如图12所示，其中横坐标是在pH时钟体系中的KIO3的浓度c(KIO3)，纵坐标是诱导时间t，当检测体系中KIO3的浓度在5.0×10-4mol/L到2.5×10-3mol/L之间时，诱导时间t与KIO3的浓度c(KIO3)成一次线性关系,线性方程为t=66600c(KIO3)+158.7,R2=0.981。据此可以实现对试样中KIO3的定量检测。Establish a working curve according to the relationship between the concentration of KIO3 in the detection system and the induction time , as shown in Figure 12, where the abscissa is the concentration c ( KIO3 ) of KIO3 in the pH clock system, and the ordinate is the induction time t. When the concentration of KIO3 in the detection system is between 5.0× 10-4 mol/L and 2.5× 10-3 mol/L, the induction time t has a linear relationship with the concentration c( KIO3 ) of KIO3 . The linear equation is t=66600c(KIO 3 )+158.7, R 2 =0.981. Accordingly, the quantitative detection of KIO 3 in the sample can be realized.
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