CN112557478B - Method for distinguishing sodium phosphite and sodium hypophosphite of oxygen acid salts with different valence states of phosphorus - Google Patents
Method for distinguishing sodium phosphite and sodium hypophosphite of oxygen acid salts with different valence states of phosphorus Download PDFInfo
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910001379 sodium hypophosphite Inorganic materials 0.000 title claims abstract description 63
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 27
- 150000003839 salts Chemical class 0.000 title claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 239000002253 acid Substances 0.000 title claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 239000001301 oxygen Substances 0.000 title claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 5
- 239000011574 phosphorus Substances 0.000 title claims abstract description 5
- 230000010355 oscillation Effects 0.000 claims abstract description 163
- 239000000126 substance Substances 0.000 claims abstract description 75
- 229910020366 ClO 4 Inorganic materials 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 37
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 28
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 14
- 239000001230 potassium iodate Substances 0.000 claims description 14
- 229940093930 potassium iodate Drugs 0.000 claims description 14
- 235000006666 potassium iodate Nutrition 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000005764 inhibitory process Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 230000000452 restraining effect Effects 0.000 claims description 4
- GCDVVDACUSFVPY-UHFFFAOYSA-N 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetrazacyclotetradeca-7,14-diene Chemical compound CC1=NCCNC(C)(C)CC(C)=NCCNC(C)(C)C1 GCDVVDACUSFVPY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 114
- 238000001228 spectrum Methods 0.000 description 14
- 230000004069 differentiation Effects 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004451 qualitative analysis Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 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
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical class [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 102000036675 Myoglobin Human genes 0.000 description 1
- 108010062374 Myoglobin Proteins 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical class [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 210000004102 animal cell Anatomy 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Chemical class 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical class [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical class [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical class [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 150000004032 porphyrins Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001291 vacuum drying Methods 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
- 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
- G01N27/416—Systems
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A method for distinguishing sodium phosphite and sodium hypophosphite which are oxygen acid salts with different valence states of phosphorus, which is characterized by comprising the following steps: application "H 2 SO 4 ‑KIO 3 ‑[NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 The chemical oscillation system is used as a distinguishing solution, and the distinction between the sodium phosphite and the sodium hypophosphite is realized according to different influences of the sodium phosphite and the sodium hypophosphite on the oscillation of the system. The potential oscillation map provided by the distinguishing method has intuitiveness, can distinguish sodium phosphite and sodium hypophosphite conveniently and rapidly, and has simple equipment, high accuracy and easy operation and observation.
Description
Technical Field
The invention relates to a distinguishing method, in particular to a tetrazacyclotetradienyl nickel complex [ NiL](ClO 4 ) 2 A method for distinguishing sodium phosphite and sodium hypophosphite which are oxygen acid salts with different valence states of phosphorus by a catalytic chemical oscillation system comprises the steps of preparing a ligand L of 5,7,7,12,14, 14-hexamethyl-1, 4,8, 11-tetraazacyclotetradec-4, 11-diene, and belongs to the field of qualitative analysis chemistry.
Background
Sodium phosphite and sodium hypophosphite belong to the same element corresponding oxysalts and play a role in their respective fields. Sodium phosphite, molecular formula: na (Na) 2 HPO 3 Sodium phosphite can be used as a reducing agent to reduce metal salts of gold, silver, mercury, nickel, chromium, cobalt and the like to corresponding metals. Can also be used as an antioxidant for textile finishing, medicines and other industries. Sodium hypophosphite, molecular formula: naH (NaH) 2 PO 2 Sodium hypophosphite can replace stainless steel materials and is widely applied to industries such as electronics, machinery, petroleum, chemical industry, aviation, navigation, food, medicine and the like. The surface of nonmetallic materials such as plastics, ceramics, glass, quartz and the like can be metallized. Can also be used as catalyst and stabilizer for chemical reaction.
The two methods of distinction that have been reported to date include physical and chemical methods: 1. the physical method comprises the following steps: sodium phosphite, mostly in crystalline powder form; sodium hypophosphite is most commonly present in crystalline form. The method is only suitable for analysis of crystals, and has large limitation. 2. The chemical method comprises the following steps: sodium phosphite, heat stable; sodium hypophosphite is easy to explode when heated and is unstable. Although the method can realize the distinction between the two, the highly toxic gas phosphine is generated in the distinguishing process, and the environment is polluted. Therefore, it is necessary to find a qualitative analysis method which has good distinguishing effect, is simple and quick to operate, and has easy judgment of results. The two structures are shown in the structural formula (I)
The structure of sodium phosphite and sodium hypophosphite in the structural formula (I).
Disclosure of Invention
The invention aims to provide a novel, convenient and quick distinguishing method for sodium phosphite and sodium hypophosphite, namely, application of NiL](ClO 4 ) 2 The distinguishing method of the catalytic chemical oscillating system for sodium phosphite and sodium hypophosphite is an electrochemical oscillating system method developed based on the sharp response of the complex catalytic chemical oscillating system for sodium phosphite and sodium hypophosphite. Specifically, samples (sodium phosphite and sodium hypophosphite) to be distinguished with the same concentration are respectively added into two groups of chemical oscillation systems, and the samples to be distinguished are distinguished according to different influences of the samples to be distinguished on the chemical oscillation systems: if the chemical oscillation is restrained after the solution to be distinguished is added, the oscillation is recovered after a period of restraining time, and meanwhile, the oscillation life is shortened when the chemical oscillation amplitude is reduced, the added sample to be distinguished is sodium phosphite; if the chemical oscillation amplitude is reduced after the solution to be distinguished is added, the oscillation life is shortened, but no inhibition time appears, the added sample to be distinguished is sodium hypophosphite, and the sample treatment time is short, the measuring condition is simple and easy to control, and the popularization and the application are convenient.
The invention solves the technical problems and adopts the following technical scheme:
the invention provides a distinguishing method for sodium phosphite and sodium hypophosphite, which is characterized in that:
distilled water is used as a solvent to prepare a solution of a sample to be distinguished;
application "H 2 SO 4 - KIO 3 - [NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 The chemical oscillation system is used as a distinguishing solution, the potential oscillation map of the chemical oscillation system is recorded, solutions of sodium phosphite and sodium hypophosphite of samples to be distinguished are respectively added into two groups of distinguishing solutions (chemical oscillation systems) at any stable potential lowest point, and qualitative analysis of the samples to be distinguished is realized according to different influences of the samples to be distinguished on the chemical oscillation system: if the chemical oscillation is restrained after the solution to be distinguished is added, the oscillation is recovered after a period of restraining time, and meanwhile, the oscillation life is shortened when the chemical oscillation amplitude is reduced, the added sample to be distinguished is sodium phosphite; if the chemical oscillation amplitude is reduced after the solution to be distinguished is added, the oscillation life is shortened, but no inhibition time appears, the added sample to be distinguished is sodium hypophosphite.
Any stable potential minimum point generated by oscillation refers to any potential minimum point from 3 rd to 25 th generated by oscillation.
The tetraazacyclotetradiene nickel complex of the invention is [ NiL](ClO 4 ) 2 Wherein ligand L is 5,7,7,12,14, 14-hexamethyl-1, 4,8, 11-tetraazacyclotetradec-4, 11-diene. [ NiL](ClO 4 ) 2 The structure is shown as (II)
Structural formula (II) [ NiL ]](ClO 4 ) 2 Is a structure of (a).
The structure of the complex is very similar to the key structure porphyrin ring of myoglobin, hemoglobin, chlorophyll and some metalloenzymes in a living body, and the complex is prepared by the following steps of](ClO 4 ) 2 The catalyzed chemical oscillation reaction is similar to biochemical oscillations within plant and animal cells. Therefore, the system has stable amplitude, long oscillation life and sharp response to sodium phosphite and sodium hypophosphite.
[NiL](ClO 4 ) 2 The preparation of (2) comprises two steps: 1) Preparation of L.2HClO 4 The method comprises the steps of carrying out a first treatment on the surface of the 2) From L.2HClO 4 Preparation of NiL](ClO 4 ) 2 。
1) Preparation of L.2HClO 4 ：
98.5mL of ethylenediamine was placed in a 500mL three-necked flask, and 126mL of 70% perchloric acid was slowly added dropwise with stirring over 120 minutes under ice-bath conditions. The initial reaction was vigorous with white smoke generation, so the drop rate was controlled to l drops every 5 seconds. The dropping speed can be accelerated properly as the reaction proceeds until the dropping is completed, and a transparent solution is obtained. 224mL of anhydrous acetone was added to the clear solution, still under ice-water bath, and stirred vigorously, the solution quickly becoming cloudy while forming a very viscous mixture. Still in the ice-water bath for 2-3 hours to allow for adequate reaction. The obtained product is transferred to a buchner funnel for suction filtration and separation, and is fully washed by acetone, thus obtaining pure white solid. Recrystallizing the pure self-colored solid in hot methanol-water solution, and vacuum drying with silica gel desiccant to obtain 80g white crystal L.2HClO 4 。
Reference is made to:
1.Curtis, N. F. and Hay, R. W. , J. Chem. Soc. , Chem. Commun. , 1966, p. 534.
2.Gang Hu, Panpan Chen, Wei Wang, Lin Hu, Jimei Song, LingguangQiu, Juan Song, E1ectrochimica Acta, 2007, Vol. 52, pp. 7996-8002.
3. Lin Hu, Gang Hu, Han-Hong Xu, J. Ana1. Chem. , 2006, Vol. 61, NO. 10, pp. 1021-1025.
4. hu Gang, doctor's paper, p25-27, fertilizer combination, 2005.
2) From L.2HClO 4 Preparation of NiL](ClO 4 ) 2 ：
11g Ni (AC) 2 4H 2 O and 21g of L.2HClO 4 Placing in 500mL three-necked flask, dissolving in 250mL methanol, refluxing in hot water bath for 3 hours, finally generating yellow precipitate, filtering, concentrating filtrate in hot water bath to l/2 of original volume, standing overnight, and crystallizing completely to obtain yellow crystal. The yellow crystals were transferred to a buchner funnel and washed with methanol, recrystallized in a hot ethanol-water solution and dried in vacuo to give 8g of [ NiL ]](ClO 4 ) 2 Bright yellowAnd (5) a crystal.
Reference is made to:
1. N. F. Curtis, J. Chem. Soc. Dolton Tran. , 1972, Vol. 13, 1357.
2. hu Gang, doctor's paper, p42-43, fertilizer combination, 2005.
The distinguishing method is different from the prior art in that the invention applies' H 2 SO 4 -KIO 3 -[NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 The chemical oscillation system is used as a distinguishing solution, and the sodium phosphite and the sodium hypophosphite are distinguished by different influences on the potential oscillation spectrum of the distinguishing solution.
Sodium phosphite and sodium hypophosphite in a distinguishable concentration range of 5.0X10 in a distinguishing solution (chemically oscillating system) -3 -2.25×10 -2 mol/L。
The concentration range which can be distinguished by the solution to be distinguished is the optimal concentration range which is determined through experiments. In the concentration range, the influence difference of sodium phosphite and sodium hypophosphite on the distinguishing solution is quite obvious, so that the distinguishing solution is easy to observe and analyze and easy to distinguish. In addition, the concentration ranges of the components in the discrimination solution (chemical oscillation system) are shown in table 1, and the optimal solution of the discrimination solution (chemical oscillation system) obtained through a plurality of experiments is shown in table 2:
table 1: concentration ranges of the components in the chemical oscillation system
| Sulfuric acid (mol/L) | Potassium iodate (mol/L) | [NiL](ClO 4 ) 2 (mol/L) | Malonic acid (mol/L) | Hydrogen peroxide (mol/L) |
| 0.0246468-0.025 | 0.0175-0.021 | 6.4875×10 -4 -8.65×10 -4 | 0.125-0.165 | 1.35-1.45 |
Table 2: optimal concentration of each component in chemical oscillation system
| Sulfuric acid (mol/L) | Potassium iodate (mol/L) | [NiL](ClO 4 ) 2 (mol/L) | Malonic acid (mol/L) | Hydrogen peroxide (mol/L) |
| 0.025 | 0.01855 | 8.65×10 -4 | 0.135 | 1.4 |
The specific experimental steps are as follows:
1. preparing a distinguishing solution according to the concentration range specified in Table 1, inserting a prepared working electrode (platinum electrode) and a reference electrode (calomel electrode) into the solution, connecting the other end of the working electrode to a data acquisition device (Go | LINK) through an amplifier (Instrument Amplifier), connecting the working electrode to a computer, opening a log lite program in the computer to set the acquisition time and the sampling speed, and then rapidly clicking a start key to monitor the potential of the solution, so as to obtain an acquired E-t curve (curve of potential value changing with time), namely a chemical potential oscillation map (at the moment, a sample to be tested is not added) to serve as a blank. And (3) respectively and rapidly adding the solutions of the samples to be distinguished into two groups of distinguishing solutions with the same concentration as each component in the blank control experiment at any stable potential minimum point generated by oscillation, and realizing qualitative analysis of the samples to be distinguished according to different oscillation responses of the samples to be distinguished to a chemical oscillation system. The method comprises the following steps: if the chemical oscillation is restrained after the solution to be distinguished is added, the oscillation is recovered after a period of restraining time, and meanwhile, the oscillation life is shortened when the chemical oscillation amplitude is reduced, the added sample to be distinguished is sodium phosphite; if the chemical oscillation amplitude is reduced after the solution to be distinguished is added, the oscillation life is shortened, but no inhibition time appears, the added sample to be distinguished is sodium hypophosphite.
Basic parameters of the chemical potential oscillation spectrum include:
oscillation amplitude: the difference in potential between one lowest potential and the next highest potential during oscillation.
Oscillation period: the time required to go from one lowest (high) potential to the next lowest (high) potential during oscillation.
Highest potential: the highest potential point appears in the system during stable oscillation.
Lowest potential: the lowest potential point of the system appears when the oscillation is stabilized.
Time of inhibition (t) in ): the time required for oscillation to resume is from the time when oscillation is suppressed after the liquid to be measured is added.
Oscillation life: the time from the start to the end of the oscillation during the oscillation.
Drawings
FIG. 1 is an oscillation pattern of a discrimination solution (chemical oscillation system) in example 1 when a sample to be discriminated is not added.
FIG. 2 is a diagram of example 1, incorporating 5.0X10 s -3 And after the sodium phosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
FIG. 3 is a diagram of example 1, incorporating 5.0X10 -3 And after the sodium hypophosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
FIG. 4 is a diagram showing the oscillation pattern of the discrimination solution (chemical oscillation system) in example 2 when the sample to be discriminated is not added.
FIG. 5 is a schematic diagram of example 2, incorporating 1.0X10 s -2 And after the sodium phosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
FIG. 6 is a schematic diagram of the addition of 1.0X10 in example 2 -2 And after the sodium hypophosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
FIG. 7 is a diagram showing the oscillation pattern of the discrimination solution (chemical oscillation system) in example 3 when the sample to be discriminated is not added.
FIG. 8 is a graph of example 3, incorporating 2.25X10 -2 And after the sodium phosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
FIG. 9 is a graph of example 3, incorporating 2.25X10 -2 And after the sodium hypophosphite is mol/L, an oscillation response spectrum is obtained by a chemical oscillation system.
Detailed Description
Example 1:
this example demonstrates the feasibility of the method of distinguishing sodium phosphite from sodium hypophosphite according to the invention as follows:
(1) Preparing a solution
Firstly, preparing 0.025mol/L sulfuric acid as stock solution by using 98% concentrated sulfuric acid and distilled water, then respectively preparing 0.14mol/L potassium iodate solution and 0.0173mol/L [ NiL ] by using 0.025mol/L sulfuric acid solution](ClO 4 ) 2 Solution, 2mol/L malonic acid solution and 4mol/L hydrogen peroxide solution. Sequentially add to a 50mL small beaker16.0mL of 0.025mol/L sulfuric acid solution, 5.3mL of 0.14mol/L potassium iodate solution, 2.0mL of 0.0173mol/L [ NiL ]](ClO 4 ) 2 Solution, 2.7mL of 2mol/L malonic acid solution and 14.0mL of 4mol/L hydrogen peroxide solution to ensure "H 2 SO 4 - KIO 3 - [NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 "the concentration of each component in the chemical oscillation system is sulfuric acid 0.025mol/L, potassium iodate 0.01855mol/L, [ NiL ]](ClO 4 ) 2 8.65×10 -4 mol/L, malonic acid 0.135mol/L and hydrogen peroxide 1.4mol/L;
meanwhile, distilled water is used as a solvent to prepare a sodium phosphite solution and a sodium hypophosphite solution with the mol/L of 1.0 respectively.
(2) Oscillation pattern
The potential oscillation pattern of the chemical oscillation system was recorded by a computer equipped with a log lite program, and FIG. 1 shows the results of the reaction at a typical concentration (sulfuric acid 0.025mol/L, potassium iodate 0.01855mol/L, [ NiL](ClO 4 ) 2 8.65×10 -4 mol/L, 0.135mol/L malonic acid and 1.4mol/L hydrogen peroxide), and the oscillation pattern of the sample to be detected is not added into the distinguishing solution, so as to serve as a blank control. 200. Mu.L of 1.0mol/L sodium phosphite and sodium hypophosphite are added to the two sets of discrimination solutions each having the same concentration as the above-mentioned concentration, respectively, so that the concentrations thereof in the discrimination solutions are 5.0X10 -3 The mol/L, the time of each addition is at the 6 th potential lowest point of the oscillation spectrum, and the obtained oscillation response spectrum is shown in figure 2 and figure 3 respectively.
(3) Differentiation of
Sodium phosphite and sodium hypophosphite have different reducing properties, and thus have different effects on a chemical oscillation system. As can be seen from comparing FIG. 2 and FIG. 3, the addition of sodium phosphite suppresses the chemical oscillation system, and the oscillation is recovered after a period of suppressing time, and the oscillation life is shortened due to the reduction of the chemical oscillation amplitude; the addition of sodium hypophosphite reduces the amplitude of the chemical oscillation system, shortens the oscillation life, but does not inhibit the occurrence of time. From the above experiments, it was found that the differentiation between sodium phosphite and sodium hypophosphite can be achieved by comparing the changes in the oscillation patterns.
Taking two 1.0mol/L solutions of samples to be distinguished (one of which is sodium phosphite solution and the other of which is sodium hypophosphite solution but not distinguished), and marking one of the solutions as a sample 1 and the other as a sample 2;
preparing two groups of chemical oscillation solutions with the same concentration of each component as the concentration, respectively collecting corresponding oscillation patterns, and respectively adding 200 mu L of 1.0mol/L of sample 1 and sample 2 at the 6 th potential lowest point to ensure that the concentration of each component in the distinguishing solution is 5.0x10 -3 mol/L。
Analysis and comparison show that: the addition of sample 1 suppressed the chemical oscillation system, and oscillation was resumed after a period of time accompanied by a decrease in the oscillation amplitude, and the oscillation lifetime was shortened (oscillation pattern corresponding to fig. 2, not corresponding to fig. 3), whereas the addition of sample 2 reduced the chemical oscillation system amplitude, and the oscillation lifetime was shortened, but no suppression time occurred (oscillation pattern corresponding to fig. 3, not corresponding to fig. 2). Therefore, sample 1 is a sodium phosphite solution and sample 2 is a sodium hypophosphite solution, and differentiation between sodium phosphite and sodium hypophosphite solutions is achieved.
Example 2:
this example demonstrates the feasibility of the method of distinguishing sodium phosphite from sodium hypophosphite according to the invention as follows:
(1) Preparing a solution
Firstly, preparing 0.025mol/L sulfuric acid as stock solution by using 98% concentrated sulfuric acid, then respectively preparing 0.14mol/L potassium iodate solution and 0.0173mol/L [ NiL ] by using 0.025mol/L sulfuric acid solution](ClO 4 ) 2 Solution, 2mol/L malonic acid solution and 4mol/L hydrogen peroxide solution; to a 50mL small beaker were added sequentially 16.0mL of 0.025mol/L sulfuric acid solution, 5.2mL of 0.14mol/L potassium iodate solution, 1.8mL of 0.0173mol/L [ NiL ]](ClO 4 ) 2 Solution, 2.8mL of 2mol/L malonic acid solution, 14.2mL of 4mol/L hydrogen peroxide solution to ensure "H 2 SO 4 - KIO 3 - [NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 "the concentration of each component in the chemical oscillation system is sulfuric acid 0.025mol/L, potassium iodate 0.0182mol/L, [ NiL ]](ClO 4 ) 2 7.785×10 -4 mol/L, malonic acid 0.14mol/L and hydrogen peroxide 1.42mol/L;
meanwhile, distilled water is used as a solvent to prepare a sodium phosphite solution and a sodium hypophosphite solution with the mol/L of 1.0 respectively.
(2) Oscillation pattern
The potential oscillation pattern of the chemical oscillation system is recorded by a computer provided with a log lite program, and the difference between oscillation responses generated by sodium phosphite and sodium hypophosphite is examined. FIG. 4 is a graph showing oscillation patterns when the solution was not added to the test sample, and used as a blank. To two groups of distinguishing solutions with the same concentration as the above concentration, 400 mu L of 1.0mol/L sodium phosphite solution and sodium hypophosphite solution are respectively added so that the concentration of each distinguishing solution is 1.0X10 - 2 The mol/L, the time of each addition is at the 6 th potential lowest point of the oscillation spectrum, and the obtained oscillation response spectrums are respectively shown in fig. 5 and 6.
(3) Differentiation of
Sodium phosphite and sodium hypophosphite have different reducing properties, and thus have different effects on a chemical oscillation system. As can be seen from comparing FIG. 5 and FIG. 6, the addition of sodium phosphite suppresses the chemical oscillation system, and the oscillation is recovered after a period of suppressing time, and the oscillation life is shortened due to the reduction of the chemical oscillation amplitude; the addition of sodium hypophosphite reduces the amplitude of the chemical oscillation system, shortens the oscillation life, but does not inhibit the occurrence of time. From the above experiments, it was found that the differentiation between sodium phosphite and sodium hypophosphite can be achieved by comparing the changes in the oscillation patterns.
Taking two 1.0mol/L solutions of samples to be distinguished (one of the solutions is sodium phosphite solution, the other solution is sodium hypophosphite solution, but the two solutions are not identified), and marking one of the solutions as a sample 1 and the other as a sample 2;
preparing two groups of chemical oscillation solutions with the concentration of each component being the same as that of the solution, respectively collecting corresponding oscillation patterns, and respectively adding 400 mu L of 1.0mol/L sample 1 and sample 2 at the 6 th potential minimum point to ensure that the concentration of each group of chemical oscillation solutions in the distinguishing solution is 1.0x10 -2 mol/L。
Analysis and comparison show that: the addition of sample 1 suppressed the chemical oscillation system, and oscillation was resumed after a period of time accompanied by a decrease in the oscillation amplitude, and the oscillation lifetime was shortened (oscillation pattern corresponding to fig. 5, not corresponding to fig. 6), whereas the addition of sample 2 reduced the chemical oscillation system amplitude, and the oscillation lifetime was shortened, but no suppression time occurred (oscillation pattern corresponding to fig. 6, not corresponding to fig. 5). Therefore, sample 1 is a sodium phosphite solution and sample 2 is a sodium hypophosphite solution, and differentiation between sodium phosphite and sodium hypophosphite solutions is achieved.
Example 3:
the feasibility of the distinguishing method of sodium phosphite and sodium hypophosphite according to the invention is verified according to the following steps:
(1) Preparing a solution
Firstly, preparing 0.025mol/L sulfuric acid as stock solution by using 98% concentrated sulfuric acid and distilled water, then respectively preparing 0.14mol/L potassium iodate solution and 0.0173mol/L [ NiL ] by using 0.025mol/L sulfuric acid solution](ClO 4 ) 2 Solution, 2mol/L malonic acid solution and 4mol/L hydrogen peroxide solution. Into a 50mL small beaker were successively added 15.5mL of 0.025mol/L sulfuric acid solution, 5.3mL of 0.14mol/L potassium iodate solution, 2.0mL of 0.0173mol/L [ NiL ]](ClO 4 ) 2 Solution, 3.0mL of 2mol/L malonic acid solution and 14.2mL of 4mol/L hydrogen peroxide solution to ensure "H 2 SO 4 - KIO 3 - [NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 "the concentration of each component in the chemical oscillation system is sulfuric acid 0.025mol/L, potassium iodate 0.01855mol/L, [ NiL ]](ClO 4 ) 2 8.65×10 -4 mol/L, malonic acid 0.15mol/L and hydrogen peroxide 1.42mol/L;
meanwhile, distilled water is used as a solvent to prepare a sodium phosphite solution and a sodium hypophosphite solution with the mol/L of 1.0 respectively.
(2) Oscillation pattern
The potential oscillation pattern of the chemical oscillation system is recorded by a computer equipped with a log lite program, and FIG. 7 is the oscillation pattern of the above-mentioned discrimination solution without the test sample added, to be used as a blankAnd (3) controlling. To two sets of discrimination solutions each having the same concentration as the above concentration, 900. Mu.L of a sodium phosphite solution and a sodium hypophosphite solution were added, respectively, in such a manner that the concentrations thereof in the discrimination solutions were 2.25X10 -2 The mol/L, the time of each addition is at the 6 th potential lowest point of the oscillation spectrum, and the obtained oscillation response spectrums are respectively shown in fig. 8 and 9.
(3) Differentiation of
Sodium phosphite and sodium hypophosphite have different reducing properties, and thus have different effects on a chemical oscillation system. Comparing FIG. 8 and FIG. 9, it can be seen that the addition of sodium phosphite suppresses the chemical oscillation system, and the oscillation is recovered after a period of suppressing time, and the oscillation life is shortened due to the reduction of the chemical oscillation amplitude; the addition of sodium hypophosphite reduces the amplitude of the chemical oscillation system, shortens the oscillation life, but does not inhibit the occurrence of time. From the above experiments, it was found that the differentiation between sodium phosphite and sodium hypophosphite can be achieved by comparing the changes in the oscillation patterns.
Taking two 1.0mol/L solutions of samples to be distinguished (one of which is sodium phosphite solution and the other of which is sodium hypophosphite solution but not distinguished), and marking one of the solutions as a sample 1 and the other as a sample 2;
preparing two groups of chemical oscillation solutions with the concentration of each component being the same as that of the solution, respectively collecting corresponding oscillation patterns, and respectively adding 900 mu L of 1.0mol/L sample 1 and sample 2 at the 6 th potential minimum point to ensure that the concentration of each group of chemical oscillation solutions in the distinguishing solution is 2.25X10 -2 mol/L。
Analysis and comparison show that: the addition of sample 1 suppressed the chemical oscillation system, and oscillation was resumed after a period of time accompanied by a decrease in the oscillation amplitude, and the oscillation life was shortened (oscillation pattern corresponding to fig. 8, not corresponding to fig. 9), whereas the addition of sample 2 reduced the chemical oscillation system amplitude, and the oscillation life was shortened, but no suppression time occurred (oscillation pattern corresponding to fig. 9, not corresponding to fig. 8). Therefore, sample 1 is a sodium phosphite solution and sample 2 is a sodium hypophosphite solution, and differentiation between sodium phosphite and sodium hypophosphite solutions is achieved.
As can be seen from the examples above, sodium phosphite solutions and sodium hypophosphite solutions of lesser or greater concentrations can also be distinguished by the method of the present invention.
Claims (3)
1. A method for distinguishing sodium phosphite and sodium hypophosphite which are oxygen acid salts with different valence states of phosphorus, which is characterized by comprising the following steps:
distilled water is used as a solvent to prepare a solution of a sample to be distinguished;
application "H 2 SO 4 -KIO 3 -[NiL](ClO 4 ) 2 Malonic acid-H 2 O 2 The chemical oscillation system is used as a distinguishing solution, the potential oscillation map of the change of the potential of the chemical oscillation system along with time is recorded, and at any one potential minimum point among the 3 rd to 25 th potential minimum points generated by oscillation, the solutions of sodium phosphite or sodium hypophosphite which are samples to be distinguished are respectively added into the two groups of distinguishing solutions, and according to the difference of reducibility of the sodium phosphite and the sodium hypophosphite which are samples to be distinguished, the influence of the sodium phosphite and the sodium hypophosphite on the chemical oscillation system is different, so that the distinguishing of the samples to be distinguished is realized: if the chemical oscillation is restrained after the solution to be distinguished is added, the oscillation is recovered after a period of restraining time, and meanwhile, the oscillation life is shortened when the chemical oscillation amplitude is reduced, the added sample to be distinguished is sodium phosphite; if the chemical oscillation amplitude is reduced after the solution to be distinguished is added, the oscillation life is shortened, but no inhibition time appears, the added sample to be distinguished is sodium hypophosphite;
[NiL](ClO 4 ) 2 wherein L is 5,7,7,12,14,14-hexamethyl-1, 4,8, 11-tetraazacyclotetradec-4, 11-diene; the molar concentrations of the components in the distinguishing solution are: 0.0246468-0.025mol/L sulfuric acid, 0.0175-0.021mol/L potassium iodate, [ NiL ]](ClO 4 ) 2 6.4875×10 -4 -8.65×10 -4 mol/L, 0.125-0.165mol/L malonic acid and 1.35-1.45mol/L hydrogen peroxide.
2. The method according to claim 1, characterized in that: the molar concentration of each component in the solution was determined to be 0.025mol/L of sulfuric acid, 0.01855mol/L of potassium iodate, [ NiL ]](ClO 4 ) 2 8.65×10 -4 mol/L, malonic acid 0.135mol/L and hydrogen peroxide 1.4mol/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 5.0×10 -3 -2.25×10 -2 mol/L。
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