CN114923750B - Method for quantitatively detecting manganous chloride - Google Patents
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- CN114923750B CN114923750B CN202210534710.7A CN202210534710A CN114923750B CN 114923750 B CN114923750 B CN 114923750B CN 202210534710 A CN202210534710 A CN 202210534710A CN 114923750 B CN114923750 B CN 114923750B
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- 229910021380 Manganese Chloride Inorganic materials 0.000 title claims abstract description 10
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000011565 manganese chloride Substances 0.000 title claims abstract description 10
- 235000002867 manganese chloride Nutrition 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 67
- 230000006698 induction Effects 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 5
- 239000011572 manganese Substances 0.000 abstract description 5
- 238000004445 quantitative analysis Methods 0.000 abstract description 5
- 229910001437 manganese ion Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 60
- 239000000523 sample Substances 0.000 description 16
- 239000012488 sample solution Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000036962 time dependent Effects 0.000 description 6
- 239000012085 test solution Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 229940099607 manganese chloride Drugs 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000000209 wet digestion Methods 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001391 atomic fluorescence spectroscopy Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 235000008452 baby food Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000003969 polarography Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for quantitatively detecting manganous chloride, which is characterized by comprising the following steps of: application of HCHO-NaHSO 3 ‑Na 2 SO 3 "pH clock reaction System as detection solution, according to the System for different concentrations of divalent manganese ions Mn 2+ Different responses, i.e. different induction times, allow for quantitative analysis of manganous chloride. The quantitative analysis method for the manganous chloride 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 MnCl of different concentrations is prepared 2 Different response, i.e. different realization of induction time for MnCl 2 The quantitative analysis method of (2) belongs to the analytical chemistry field.
Background
Manganous chloride with molecular formula of MnCl 2 . Can be used for preparing pharmaceutical synthesis and feed auxiliary agent, analytical reagent, dye and pigment. Smelting magnesium alloy and aluminum alloy, producing brown-black bricks and tiles, and manufacturing pharmaceuticals and dry batteries. Can also be used as trace element fertilizer in agriculture. In addition, manganous chloride may be used as a conductive salt in electroplating. Manganese chloride is added into ferrous chloride iron plating solution to refine crystal grains, and the manganese chloride is also an antioxidant, so that the oxidation of ferrous iron can be inhibited. However, when the compound is used as a nutritional supplement (manganese enhancer), the content range of dairy products specified in China is 1.08-4.32 mg/kg, and the content range of infant foods is limited to 1.32-5.26 mg/kg. Thus for MnCl 2 Quantitative detection of (c) becomes critical.
At present for MnCl 2 The detection method of (2) comprises wet digestion treatment, microwave digestion method, atomic absorption spectrometry, atomic fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry (ICP-AES), colorimetry and polarography. However, the use of these methods often presents a number of unavoidable problems. For example: longer digestion time is required for wet digestion treatment, so that the sample consumption is high and the environmental pollution is serious; the spectrometry, although simple and easy to operate, requires expensive equipment and equipment maintenance costs, is costly and requires trained inspectors; colorimetric determination requires the assistance of a chromogenic solution and is cumbersome in steps. 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 MnCl 2 Provides a new quantitative detectionThe method is carried out by HCHO-NaHSO 3 - Na 2 SO 3 The pH clock system is a detection solution pair MnCl 2 Quantitative detection method based on the pH clock system for MnCl 2 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, respectively leading a series of MnCl to be detected with different concentrations 2 Adding the sample solution into a pH clock system in an equal volume, and detecting MnCl according to the concentration of the solution to be detected in the pH clock system 2 OH in solution and detection System - Combining the different induction time to realize the detection of MnCl 2 And (5) quantitatively detecting the sample.
MnCl in solution to be detected 2 The concentration in the pH clock system is the abscissa, the induction time t is the ordinate, a working curve is established according to the relation between the concentration of the solution to be detected in the pH clock system and the induction time, and MnCl in the system 2 The concentration is 5 multiplied by 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and MnCl 2 Is linear in relation to the concentration of MnCl in the sample 2 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 is for MnCl of different concentrations 2 The response of (a) is different, namely the induction time is different, and the MnCl is realized 2 Is a quantitative analysis of (a).
MnCl 2 The concentration range to be detected in the detection solution (pH clock system) is 5×10 -4 -2.5×10 -3 mol/L。
MnCl 2 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 5-10 ℃.
MnCl is prepared by using the pH clock system 2 The concentration range which can be detected is determined by experimentsIs present in the concentration range of interest. Within this concentration range, induction time vs MnCl 2 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) |
| 0.045-0.0625 | 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 40mL of detection solution (pH clock system) according to the concentration range specified in Table 1, wherein the temperature is controlled to be a specific temperature value between 5 and 10 ℃ 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.
Build MnCl in detection solution 2 Working curve of concentration versus pH induction time
Preparing MnCl with concentration of 0.5mol/L to 2.5mol/L by using distilled water as solvent 2 The solution is used as a sample solution, and 40 mu L of sample solutions with different concentrations are respectively added into a pH clock system of 40mL by a pipette while the reaction of the pH clock system is started, so that MnCl in the system 2 The concentration is 5 multiplied by 10 -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; mnCl in the system 2 When the concentration is different, the induction time t of the pH clock system is also different; by MnCl in the system 2 Concentrations are plotted on the abscissa and t is plotted on the ordinate; when the body is closedMnCl in the system 2 The concentration is 5 multiplied by 10 - 4 mol/L to 2.5X10 -3 Between mol/L, the induction time t of the pH clock system and MnCl 2 The concentration of (2) is linear once to obtain a working curve.
For MnCl 2 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 MnCl in the detection system according to the corresponding relation between t and the concentration on the working curve 2 Further calculate the concentration of MnCl in the sample to be measured 2 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/L MnCl 2 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 1.0X10 s -3 mol/L MnCl 2 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 MnCl in example 1 2 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 the addition of 1.0X10 in example 2 -3 mol/L MnCl 2 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 7 is a schematic diagram of example 2, incorporating 1.5X10 -3 mol/L MnCl 2 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 8 shows the pH induction time t and MnCl in example 2 2 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 diagram of example 3, incorporating 2.0X10 s -3 mol/L MnCl 2 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 MnCl 2 Then, a time-dependent profile of the pH value of the solution (pH clock system) was examined.
FIG. 12 shows the pH induction time t and MnCl in example 3 2 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 MnCl 2 Quantitative analysis was performed. Equal volume addition of MnCl of no use concentration 2 The sample solution is put into a pH clock system to establish MnCl in a detection system 2 The working curve (such as linear relation) of the relation between the concentration and the induction time achieves the detection of MnCl in a pH clock system 2 Further calculate MnCl in the sample to be measured 2 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 "the concentration of each component in the pH clock system is HCHO 0.051mol/L, naHSO 3 0.0495mol/L、Na 2 SO 3 0.00495mol/L, total volume 40mL, temperature was controlled at 8deg.C.
Simultaneously distilled water is used as solvent to prepare a series of MnCl with different concentrations 2 Sample solution.
(2) Obtaining a pH clock pattern
Graph of pH value of prepared detection solution with timeRecorded 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 220.0s for the blank. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one group, 40. Mu.L of 0.5mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 5X 10 -4 mol/L, mnCl added 2 Such that the induction time was prolonged to 281.7s as shown in FIG. 2; for the other group, 40. Mu.L of 1.0mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 1X 10 -3 mol/L, mnCl added 2 Such that the induction time became 299.6s as shown in FIG. 3. FIGS. 2 and 3 demonstrate the detection of MnCl in solution 2 The difference in concentration of (2) leads to a different induction time of the pH-clocked system, since MnCl is to be detected 2 OH newly generated from solution and clock system - Combined to form Mn (OH) 2 So that the time for the pH value of the clock system to rise is different. When MnCl is detected in the system 2 The concentration is 5 multiplied by 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 MnCl 2 The concentration in the detection system versus the induction time is plotted as shown in FIG. 4, where the abscissa is MnCl in the pH clock system 2 The ordinate is the induction time t, when MnCl is detected in the system 2 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time and MnCl 2 Is linear in terms of concentration, the linear equation is t=46140 c (MnCl 2 )+253.69, R 2 = 0.9563. Thus, mnCl in the sample can be realized 2 Is a quantitative detection of (a).
Example 2:
(1) Preparing a detection solution
Firstly, distilled water is used for preparing the components 0 respectively2mol/L HCHO solution, 0.1mol/L NaHSO 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 8deg.C.
Simultaneously distilled water is used as solvent to prepare a series of MnCl with different concentrations 2 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 218.8s for blank control. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one group, 40. Mu.L of 1.0mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 1.0X10 -3 mol/L, mnCl added 2 Such that the induction time was prolonged to 300.0s as shown in fig. 6; for the other group, 40. Mu.L of 1.5mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 1.5X10 -3 mol/L, mnCl added 2 So that the induction time became 318.4s as shown in FIG. 7. FIGS. 6 and 7 demonstrate the detection of MnCl in solution 2 The difference in concentration of (2) leads to a different induction time of the pH-clocked system, since MnCl is to be detected 2 OH newly generated from solution and clock system - Combined to form Mn (OH) 2 So that the time for the pH value of the clock system to rise is different. When MnCl is detected in the system 2 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 in mol/L can be observed.
(3) Quantitative detection
According to MnCl 2 The concentration in the detection system versus the induction time is plotted as shown in FIG. 8, where the abscissa is MnCl in the pH clock system 2 The ordinate is the induction time t, when MnCl is detected in the system 2 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time and MnCl 2 Is linear in terms of concentration, the linear equation is t= 45900c (MnCl 2 )+254.05,R 2 = 0.9546. Thus, mnCl in the sample can be realized 2 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 8deg.C.
Simultaneously distilled water is used as solvent to prepare a series of MnCl with different concentrations 2 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 217.6s for a blank. Two sets of detection solutions with the same concentration of each component as the detection solution are additionally prepared. For one group, 40. Mu.L of 2.0mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 2.0X10 -3 mol/L, mnCl added 2 So that the induction time is prolonged335.9s is shown in fig. 10; for the other group, 40. Mu.L of 2.5mol/L MnCl was added to a pH clock system of 40mL at the same time as the reaction was started 2 Sample solution such that MnCl 2 The concentration in the detection solution was 2.5X10 -3 mol/L, mnCl added 2 The induction time was changed to 378.9s as shown in FIG. 11. FIGS. 10 and 11 demonstrate the detection of MnCl in solution 2 The difference in concentration of (2) leads to a different induction time of the pH-clocked system, since MnCl is to be detected 2 OH newly generated from solution and clock system - Combined to form Mn (OH) 2 So that the time for the pH value of the clock system to rise is different. When MnCl is detected in the system 2 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 MnCl 2 The concentration in the detection system versus the induction time is plotted as shown in FIG. 12, where the abscissa is MnCl in the pH clock system 2 The ordinate is the induction time t, when MnCl is detected in the system 2 Is at a concentration of 5X 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time and MnCl 2 Is linear in terms of concentration, the linear equation is t= 46020c (MnCl 2 )+253.97, R 2 = 0.9559. Thus, mnCl in the sample can be realized 2 Is a quantitative detection of (a).
Claims (4)
1. A quantitative detection method of manganous chloride is characterized in that:
preparing a sample MnCl to be detected by taking distilled water as a solvent 2 Is a solution of (a);
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 5-10 ℃ at any specific temperature, and when the pH clock reaction starts, the series of samples MnCl with different concentrations to be detected are respectively processed 2 Adding the solution into the pH clock system in an equal volumeAccording to the different concentration of the solution to be detected in the pH clock system, mnCl to be detected 2 OH in solution and detection System - By combining the different induction time generated, the MnCl of the sample to be detected is realized 2 Is used for quantitative detection of (a): mnCl in solution to be detected 2 The concentration in the pH clock system is the abscissa, the induction time t is the ordinate, a working curve is established according to the relation between the concentration of the solution to be detected in the pH clock system and the induction time, and MnCl in the system 2 The concentration is 5 multiplied by 10 -4 mol/L to 2.5X10 -3 Between mol/L, the induction time t and MnCl 2 Is linear in relation to the concentration of MnCl in the sample 2 Is used for quantitative detection of (a);
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。
2. The quantitative detection method according to claim 1, wherein: 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。
3. The quantitative detection method according to claim 1, wherein: mnCl 2 The concentration of the solution in the detection solution is in the range of 5X 10 -4 mol/L to 2.5X10 -3 mol/L。
4. The quantitative detection method according to claim 1, wherein: detection of MnCl 2 The temperature of the pH clock system was controlled at 8℃at the time of solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210534710.7A CN114923750B (en) | 2022-05-17 | 2022-05-17 | Method for quantitatively detecting manganous chloride |
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| 时钟反应系HCGO—HSO3-—SO32-的pH突跃法测定HSO3-盐的含量;黄承高 等;《分析化学》;19890731;第17卷(第7期);第615、619-621页 * |
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