CN114184660B - Hexavalent iron FeO with different valence states for distinguishing iron 42- And ferric iron Fe 3+ Is a method of (2) - Google Patents
Hexavalent iron FeO with different valence states for distinguishing iron 42- And ferric iron Fe 3+ Is a method of (2) Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 95
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 14
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 title claims abstract description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 230000006698 induction Effects 0.000 claims abstract description 42
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 230000002035 prolonged effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 91
- 239000000523 sample Substances 0.000 description 37
- 230000004069 differentiation Effects 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 230000010355 oscillation Effects 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000004451 qualitative analysis Methods 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- 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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/302—Electrodes, e.g. test electrodes; Half-cells pH sensitive, e.g. quinhydron, antimony or hydrogen electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
Hexavalent iron FeO with different valence states for distinguishing iron 4 2‑ And ferric iron Fe 3+ Is characterized in that: application of HCHO-NaHSO 3 –Na 2 SO 3 "pH clock System as a discrimination solution, feO according to the System 4 2‑ And Fe (Fe) 3+ Different response, i.e. induction time, to achieve FeO 4 2‑ And Fe (Fe) 3+ Is a distinction between (a) and (b). The pH clock map provided by the distinguishing method has intuitiveness, and can distinguish FeO conveniently and rapidly 4 2‑ And Fe (Fe) 3+ Moreover, the device is simple, high in accuracy and easy to operate and observe.
Description
Technical Field
The invention relates to an analysis and differentiation method, in particular to a method for establishing HCHO-NaHSO 3 - Na 2 SO 3 "pH clock system as substrate, according to the response of the system to different valence states (oxidation states) of iron element, i.e. different induction time, the system realizes the reaction to FeO 4 2- And Fe (Fe) 3+ The qualitative analysis method belongs to the analytical chemistry field.
Background
Iron (Fe) exists in various valence states, namely various oxidation numbers (Fe (VI), fe (III) and Fe (II)), and is one of the most widely distributed and abundant transition metals in the crust. Ferric iron Fe 3+ Is an ion formed after the iron atom loses 3 electrons, is the most stable ion of iron, has stronger oxidizing property, and is an important industrial agent. In humans, fe (III) plays an essential role in biological processes such as oxygen transport, cellular metabolism, enzyme catalysis, and electron transfer. Hexavalent iron FeO 4 2- The form of (Fe (VI)) plays a great role in purifying water because it can destroy the structure of algae and bacteria due to its strong oxidation. Since iron can exist in a variety of oxidation states, different oxidation states have different biochemical functions, distinguishing between different oxidation states of iron is critical to protecting human health and maintaining ecological balance.
In distinguishing the valence state (oxidation state) of iron element, there are conventionally different instruments such as ultraviolet-visible spectrophotometry (UV-Vis), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma spectrometry (ICP-OES). UV-Vis has the advantages of high sensitivity, good selectivity, etc., but the search for suitable ligands limits the use of the ultraviolet-visible spectrum. XPS measurement is accurate and high in sensitivity, but most of the measurement samples are solid, and X rays used by the instrument can reduce the high oxidation state of metal, so that the distinction of metals in different oxidation states is inaccurate. ICP-MS can rapidly detect multiple elements simultaneously. However, the method uses large-sized instruments, is expensive to measure, and cannot meet the requirement of on-site measurement. 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 hexavalent iron FeO 4 2- And ferric iron Fe 3+ Provides a novel, convenient and quick distinguishing method, namely, HCHO-NaHSO is adopted 3 - Na 2 SO 3 The pH clock reaction system is used for distinguishing the solution pair FeO 4 2- And Fe (Fe) 3+ Qualitative distinguishing method based on the pH clock system for FeO 4 2- And Fe (Fe) 3+ A clocking architecture developed for the sensitive response of (a). Specifically, "HCHO-NaHSO 3 - Na 2 SO 3 The pH clock reaction system is used as a distinguishing solution, the spectrum of the pH change along with time is recorded, and when the pH clock reaction starts, the samples (FeO 4 2- And Fe (Fe) 3+ ) The equal volume is added into a pH clock system, and the distinction of the samples to be distinguished is realized according to the difference of the induction time generated by the pH clock system: if the induction time of the pH clock is shortened after the solution to be distinguished is added, the added sample to be distinguished is FeO 4 2- The method comprises the steps of carrying out a first treatment on the surface of the If the induction time of the pH clock is prolonged after the solution to be distinguished is added, the added sample to be distinguished is Fe 3+ . The invention has short sample treatment time, simple and easily controlled measurement conditions, and is convenient to popularize and apply.
The qualitative distinguishing method is different from the prior art in that the invention applies HCHO-NaHSO 3 - Na 2 SO 3 "pH clock System as a discrimination solution, and the System is for FeO 4 2- And Fe (Fe) 3+ The response of (a) is different, namely the induction time is different, and the effect of the (a) on FeO is realized 4 2- And Fe (Fe) 3+ Qualitative analysis of (c).
FeO 4 2- And Fe (Fe) 3+ The distinguishable concentration range in the distinguishing solution (pH clocking system) is 2.0X10 -4 -1.2×10 -3 mol/L。
The temperature of the pH clock system is controlled to be any specific temperature in the range of 20-25 ℃ when distinguishing the solution to be detected.
The concentration range which can be distinguished by the solution to be distinguished is the optimal concentration range which is determined through experiments. Within this concentration range, feO 4 2- And Fe (Fe) 3+ The difference of the influence on the distinguishing solution is obvious, the observation and analysis are easy, and the distinguishing is easy to realize. In addition, the concentration ranges of the components in the discrimination solution (pH clock system) are shown in table 1, and the optimal solution of the discrimination solution (pH clock system) obtained through a plurality of experiments is 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) |
| 0.045-0.0636 | 0.044-0.0635 | 0.0044-0.00635 |
Table 2: optimum concentration of each component in pH clock system
| HCHO(mol/ L) | NaHSO 3 (mol/L) | Na 2 SO 3 (mol/L) |
| 0.0525 | 0.0525 | 0.00525 |
The specific experimental steps are as follows:
1. preparing a solution to be distinguished (a pH clock system) according to the concentration range specified in the table 1, wherein the temperature of the solution is controlled to be a specific temperature value between 20 ℃ and 25 ℃ 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 over time, i.e., the pH clock profile (at which time the test sample has not been added) as a blank. The method comprises the steps of adding to-be-distinguished solutions with the same concentration of each component into two groups of distinguishing solutions, rapidly adding the to-be-distinguished solutions while starting the reaction of a pH clock system, recording a pH clock spectrum of which the pH changes with time in the same way, and inducing time according to different responses of the pH clock system to the to-be-distinguished samplesDifferent, qualitative analysis of the sample to be distinguished is realized. The method comprises the following steps: if the induction time of the pH clock is shortened after the solution to be distinguished is added, the added sample to be distinguished is FeO 4 2- The method comprises the steps of carrying out a first treatment on the surface of the If the induction time of the pH clock is prolonged after the solution to be distinguished is added, the added sample to be distinguished is Fe 3+ 。
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.
Drawings
FIG. 1 is a graph showing the pH of a discrimination solution (pH clock system) with time when a sample to be discriminated is not added in example 1.
FIG. 2 is a schematic diagram of example 1, incorporating 4.0X10 s -4 mol/L FeO 4 2- Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
FIG. 3 is a diagram of example 1, incorporating 4.0X10 -4 mol/L Fe 3+ Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
FIG. 4 is a graph showing the pH of the discrimination solution (pH clock system) with time when the sample to be discriminated is not added in example 2.
FIG. 5 is a diagram of example 2 incorporating 6.0X10 s -4 mol/L FeO 4 2- Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
FIG. 6 is a graph of example 2, incorporating 6.0X10 s -4 mol/L Fe 3+ Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
FIG. 7 is a graph showing the pH of the discrimination solution (pH clock system) with time when the sample to be discriminated is not added in example 3.
FIG. 8 is a graph of example 3, incorporating 8.0X10 s -4 mol/L FeO 4 2- Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
FIG. 9 is a graph of example 3, incorporating 8.0X10 s -4 mol/L Fe 3+ Later, a plot of the pH of the solution (pH clock system) over time was distinguished.
Detailed Description
Example 1:
this example demonstrates FeO according to the invention as follows 4 2- And Fe (Fe) 3+ Feasibility of the distinguishing method:
(1) Preparing a 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 8.5mL of distilled water solution, 21.0mL of NaHSO in sequence 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 0.0525mol/L、Na 2 SO 3 0.00525mol/L, total volume 40mL, temperature was controlled at 23 ℃.
At the same time, distilled water is used as solvent to prepare K of 0.1mol/L 2 FeO 4 Solution and FeCl 3 A solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the formulated discrimination solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no discrimination sample was added). As shown in fig. 1. The pH induction time was 245s for the blank. Two sets of distinguishing solutions with the same concentration of each component as the distinguishing solution are additionally configured. For one of the groups, 160. Mu.L of 0.1mol/L K was added to a pH clock system of 40mL at the same time as the reaction was started 2 FeO 4 Sample solution, so that K 2 FeO 4 The concentration in the separating liquid was 4.0X10 -4 mol/L, K added 2 FeO 4 Shortening the induction time to 223s is shown in FIG. 2; for the other group, 160. Mu.L of 0.1mol/L FeCl was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, so that FeCl 3 In distinguishing solutionsThe concentration is 4.0X10 -4 mol/L, feCl added 3 Such that the induction time was extended to 275s as shown in figure 3.
(3) Differentiation of
FeO 4 2- And Fe (Fe) 3+ Is different in oxidation ability. FeO (FeO) 4 2- Has stronger oxidizing ability and can be matched with a pH clock substrate HSO 3 - Reacting; and Fe (Fe) 3+ Is unable to oxidize HSO 3 - Will only be in contact with OH in solution - Combined to form Fe (OH) 3 . Thus, feO 4 2- The addition of (2) shortens the induction time, while Fe 3+ The addition of (3) allows for an extended induction time. As can be seen by comparing FIG. 2 with FIG. 3, K 2 FeO 4 The addition of the pH clock shortens the induction time of the pH clock; feCl 3 The addition of (3) allows for an extended induction time of the pH clock. As can be seen from the above experiments, the change of the induction time of the pH clock system can be compared to realize the K 2 FeO 4 And FeCl 3 Is a distinction between (a) and (b).
Taking two 0.1mol/L solutions of samples to be distinguished (one of which is K 2 FeO 4 Solution, the other is FeCl 3 Solution, but not yet distinguished), one of which is labeled sample 1 and the other sample 2;
preparing two groups of pH clock system solutions with the same concentration as the above components, respectively collecting corresponding disturbance maps, and respectively adding 160 μL of 0.1mol/L sample 1 and sample 2 at the beginning of the pH clock to make the concentration of each component in the distinguishing solution be 4.0X10 -4 mol/L。
Analysis and comparison show that: the addition of sample 1 resulted in a shortened induction time of the pH clock (oscillation pattern corresponding to fig. 2, not corresponding to fig. 3), while the addition of sample 2 resulted in a prolonged induction time of the pH clock (oscillation pattern corresponding to fig. 3, not corresponding to fig. 2). Thus, sample 1 is K 2 FeO 4 Solution, sample 2 was FeCl 3 Solution to achieve K 2 FeO 4 And FeCl 3 Solution differentiation.
Example 2:
this example demonstrates FeO according to the invention as follows 4 2- And Fe (Fe) 3+ Feasibility of the distinguishing method:
(1) Preparing a 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 8.4mL of distilled water solution, 20.8mL of NaHSO in sequence 3 - Na 2 SO 3 Mixing the solution, 10.8mL 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 0.054mol/L, naHSO 3 0.052mol/L、Na 2 SO 3 0.0052mol/L, total volume 40mL, and temperature was controlled at 23 ℃.
At the same time, distilled water is used as solvent to prepare K of 0.1mol/L 2 FeO 4 Solution and FeCl 3 A solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the formulated discrimination solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no discrimination sample was added). As shown in fig. 4. The pH induction time was 245s for the blank. Two sets of distinguishing solutions with the same concentration of each component as the distinguishing solution are additionally configured. For one of the groups, 240. Mu.L of 0.1mol/L K was added to a pH clock system of 40mL at the same time as the reaction was started 2 FeO 4 Sample solution, so that K 2 FeO 4 The concentration in the separating liquid was 6.0X10 -4 mol/L, add K 2 FeO 4 The post induction time was reduced to 214s as shown in figure 5; for the other group, 240. Mu.L of 0.1mol/L FeCl was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, so that FeCl 3 The concentration in the discrimination solution was 6.0X10 -4 mol/L, feCl added 3 Such that the induction time was prolonged to 297s as shown in figure 6.
(3) Differentiation of
FeO 4 2- And Fe (Fe) 3+ Is different in oxidation ability. FeO (FeO) 4 2- Has stronger oxidizing ability and can be matched with a pH clock substrate HSO 3 - Reacting; and Fe (Fe) 3+ Is unable to oxidize HSO 3 - Will only be in contact with OH in solution - Combined to form Fe (OH) 3 . Thus, feO 4 2- The addition of (2) shortens the induction time, while Fe 3+ The addition of (3) allows for an extended induction time. As can be seen by comparing FIG. 5 with FIG. 6, K 2 FeO 4 The addition of the pH clock shortens the induction time of the pH clock; feCl 3 The addition of (3) allows for an extended induction time of the pH clock. As can be seen from the above experiments, the change of the induction time of the pH clock system can be compared to realize the K 2 FeO 4 And FeCl 3 Is a distinction between (a) and (b).
Taking two 0.1mol/L solutions of samples to be distinguished (one of which is K 2 FeO 4 Solution, the other is FeCl 3 Solution, but not yet distinguished), one of which is labeled sample 1 and the other sample 2;
preparing two groups of pH clock system solutions with the same concentration of each component as the concentration, respectively collecting corresponding disturbance maps, and respectively adding 240 mu L of 0.1mol/L sample 1 and sample 2 at the beginning of the pH clock so that the concentration of each group of pH clock system solutions in the distinguishing solution is 6.0X10 -4 mol/L。
Analysis and comparison show that: the addition of sample 1 resulted in a shortened pH clock induction time (oscillation pattern corresponding to fig. 5, not corresponding to fig. 6), while the addition of sample 2 resulted in an extended pH clock induction time (oscillation pattern corresponding to fig. 6, not corresponding to fig. 5). Thus, sample 1 is K 2 FeO 4 Solution, sample 2 was FeCl 3 Solution to achieve K 2 FeO 4 And FeCl 3 Solution differentiation.
Example 3:
this example demonstrates FeO according to the invention as follows 4 2- And Fe (Fe) 3+ Feasibility of the distinguishing method:
(1) Preparing a solution
Firstly, distilled water is used for preparing HCHO solution with 0.2mol/L respectively,NaHSO of 0.1mol/L 3 And 0.01mol/L Na 2 SO 3 Is a mixed solution of (a) and (b). To a 50mL small beaker was added 11.0mL of distilled water solution, 19.0mL of NaHSO in sequence 3 - Na 2 SO 3 Mixing the solution, 11.0mL 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 0.055mol/L, naHSO 3 0.0475mol/L、Na 2 SO 3 0.00475mol/L, total volume 40mL, temperature was controlled at 23 ℃.
At the same time, distilled water is used as solvent to prepare K of 0.1mol/L 2 FeO 4 Solution and FeCl 3 A solution.
(2) Obtaining a pH clock pattern
The profile of the pH of the formulated discrimination solution over time was recorded by a computer equipped with a chemical signal acquisition analysis program (no discrimination sample was added). As shown in fig. 7. The pH induction time was 245s for the blank. Two sets of distinguishing solutions with the same concentration of each component as the distinguishing solution are additionally configured. For one of the groups, 320. Mu.L of 0.1mol/L K was added to a pH clock system of 40mL at the same time as the reaction was started 2 FeO 4 Sample solution, so that K 2 FeO 4 The concentration in the separating liquid was 8.0X10 -4 mol/L, add K 2 FeO 4 The post induction time was reduced to 205s as shown in figure 8; for the other group, 320. Mu.L of 0.1mol/L FeCl was added to the pH clock system of 40mL at the same time as the reaction was started 3 Sample solution, so that FeCl 3 Concentration in the discrimination solution was 8.0X10 -4 mol/L, feCl added 3 The induction time was prolonged to 313s as shown in FIG. 9.
(3) Differentiation of
FeO 4 2- And Fe (Fe) 3+ Is different in oxidation ability. FeO (FeO) 4 2- Has stronger oxidizing ability and can be matched with a pH clock substrate HSO 3 - Reacting; and Fe (Fe) 3+ Is unable to oxidize HSO 3 - Will only be in contact with OH in solution - Combined to form Fe (OH) 3 . Thus, feO 4 2- Is added with (a)The induction time is shortened, and Fe 3+ The addition of (3) allows for an extended induction time. As can be seen by comparing FIG. 8 with FIG. 9, K 2 FeO 4 The addition of (2) shortens the induction time of the pH clock; feCl 3 The addition of (3) allows for an extended induction time of the pH clock. As can be seen from the above experiments, the change of the induction time of the pH clock system can be compared to realize the K 2 FeO 4 And FeCl 3 Is a distinction between (a) and (b).
Taking two 0.1mol/L solutions of samples to be distinguished (one of which is K 2 FeO 4 Solution, the other is FeCl 3 Solution, but not yet distinguished), one of which is labeled sample 1 and the other sample 2;
preparing two groups of pH clock system solutions with the same concentration as the above components, respectively collecting corresponding disturbance maps, and respectively adding 320 μl of 0.1mol/L sample 1 and sample 2 at the beginning of pH clock to make their concentration in the distinguishing solution 8.0X10 -4 mol/L。
Analysis and comparison show that: the addition of sample 1 resulted in a shortened pH clock induction time (oscillation pattern corresponding to fig. 8, not corresponding to fig. 9), while the addition of sample 2 resulted in an extended pH clock induction time (oscillation pattern corresponding to fig. 9, not corresponding to fig. 8). Thus, sample 1 is K 2 FeO 4 Solution, sample 2 was FeCl 3 Solution to achieve K 2 FeO 4 And FeCl 3 Solution differentiation.
As can be seen from the examples above, a smaller or larger concentration of K 2 FeO 4 FeCl 3 Solutions can also be distinguished by the method of the invention.
Claims (4)
1. Hexavalent iron FeO with different valence states for distinguishing iron 4 2- And ferric iron Fe 3+ Is characterized in that:
distilled water is used as a solvent to prepare a solution of a sample to be distinguished;
application of HCHO-NaHSO 3 -Na 2 SO 3 "pH clock system as differential solutionA liquid, recording a profile of pH changes over time; the pH clock system temperature is controlled at any specific temperature within the range of 20-25 ℃, and at the same time of starting the reaction, the FeO of the sample to be distinguished with the same concentration is respectively added into the two groups of distinguishing solutions 4 2- And Fe (Fe) 3+ According to FeO 4 2- And Fe (Fe) 3+ The oxidation capability of the sample to be distinguished is different, so that the induction time generated by a pH clock system is different, and the sample to be distinguished is distinguished: if the induction time of the pH clock is shortened after the solution to be distinguished is added, the added sample to be distinguished is FeO 4 2- The method comprises the steps of carrying out a first treatment on the surface of the If the induction time of the pH clock is prolonged after the solution to be distinguished is added, the added sample to be distinguished is Fe 3+ ；
The molar concentrations of the components in the distinguishing solution are: HCHO 0.045-0.0636mol/L, naHSO 3 0.044-0.0635mol/L、Na 2 SO 3 0.0044-0.00635mol/L。
2. The method according to claim 1, characterized in that: the molar concentration of each component in the distinguishing solution is HCHO 0.0525mol/L, naHSO 3 0.0525mol/L、Na 2 SO 3 0.00525mol/L。
3. The method according to claim 1, characterized in that: the distinguishable concentration range of the sample to be distinguished in the distinguishing solution is 2.0X10 -4 -1.2×10 -3 mol/L。
4. The method according to claim 1, characterized in that: the temperature of the pH clock system was controlled at 23℃when distinguishing the solutions to be measured.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111517709.5A CN114184660B (en) | 2021-12-13 | 2021-12-13 | Hexavalent iron FeO with different valence states for distinguishing iron 42- And ferric iron Fe 3+ Is a method of (2) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111517709.5A CN114184660B (en) | 2021-12-13 | 2021-12-13 | Hexavalent iron FeO with different valence states for distinguishing iron 42- And ferric iron Fe 3+ Is a method of (2) |
Publications (2)
| Publication Number | Publication Date |
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