CN110907404A - Method for determining trace hydrogen peroxide based on tetra-sulfo nickel phthalocyanine - Google Patents

Method for determining trace hydrogen peroxide based on tetra-sulfo nickel phthalocyanine Download PDF

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Publication number
CN110907404A
CN110907404A CN201911175377.XA CN201911175377A CN110907404A CN 110907404 A CN110907404 A CN 110907404A CN 201911175377 A CN201911175377 A CN 201911175377A CN 110907404 A CN110907404 A CN 110907404A
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China
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hydrogen peroxide
solution
scattering intensity
concentration
mol
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CN201911175377.XA
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唐宁莉
王文平
慕欣悦
王仪敏
黄信
张容珲
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Guilin University of Technology
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Guilin University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G01N21/51—Scattering, i.e. diffuse reflection within a body or fluid inside a container, e.g. in an ampoule
    • 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

Abstract

The invention discloses a method for measuring trace hydrogen peroxide based on tetra-sulfo nickel phthalocyanine. Respectively adding HAc-NaAc buffer solution and NiPcS into 11 colorimetric tubes4Adding 0.0, 0.003, 0.005, 0.006, 0.008, 0.013, 0.027, 0.054, 0.081, 0.108, 0.137mL of 1.2X 10‑ 5mol/L H2O2The solution was added with the nanogold solution after 15 minutes, diluted to 5mL after 2 minutes, and the scattering spectrum was scanned on a fluorescence photometer at λ ex = λ em. The addition of H is measured at a wavelength of 700nm2O2Scattering intensity of solution I700nmAnd without addition of H2O2Scattering intensity of reagent blank I0Calculating the difference DeltaI700nm=I700nm‑I0. The determination method has good selectivity and high sensitivity.

Description

Method for determining trace hydrogen peroxide based on tetra-sulfo nickel phthalocyanine
Technical Field
The invention relates to a method for measuring trace hydrogen peroxide, in particular to a resonance scattering spectrometry method for measuring hydrogen peroxide based on tetrasulfophthalocyanine.
Background
Hydrogen peroxide is widely used in various fields of production and life as an important chemical reagent and chemical product. Meanwhile, hydrogen peroxide is an important participating substance in enzymatic reactions in biological and environmental processes, has very close relation with various biochemical reactions in environmental water bodies, and has important influence on the state of chemical substances in water environment. Therefore, the detection of the hydrogen peroxide content is of great significance in environmental analysis. Among many methods for measuring the hydrogen peroxide content, the resonance scattering spectroscopy has been gradually applied to the measurement of the hydrogen peroxide content in recent years due to its simple operation and high sensitivity. Tetrasulfo nickel phthalocyanine (NiPcS)4) The catalyst has the property of hydrogen peroxide mimic enzyme, can catalyze hydrogen peroxide to oxidize o-phenylenediamine (OPD) to generate an intermediate product 2, 3-diamino-5, 10-dihydrophenazine and a final product 2, 3-diaminophenazine, and 2 products can enable nano gold to generate an aggregation effect, so that a resonance scattering signal of a reaction system is enhanced. The method for quantitatively determining the hydrogen peroxide can be established according to the change of the resonance scattering intensity of the system caused by the change of the aggregation state of the nanogold before and after the reaction, and the method is not reported yet.
Disclosure of Invention
The invention aims to provide a resonance scattering spectrometry method for measuring trace hydrogen peroxide based on tetrasulfophthalocyanine.
The method comprises the following specific steps:
adding 0.06-0.12 mL of sodium acetate-sodium acetate (HAc-NaAc) buffer solution with pH5.4 into 11 colorimetric tubes with 5mL, and adding 0.04-0.12 mL of 1.0 × 10-6mol/L of tetra-sulfo nickel phthalocyanine (NiPcS)4) 0.09-0.14 mL of o-phenylenediamine (OPD) solution with the concentration of 0.01mol/L, and then 0.0, 0.003, 0.005, 0.006, 0.008, 0.013, 0.027, 0.054, 0.081, 0.108 and 0.137mL of o-phenylenediamine (OPD) solution with the concentration of 1.2 x 10 are added in sequence-5Reacting the hydrogen peroxide solution of mol/L for 15 minutes at room temperature, adding 0.3-0.8 mL of nanogold (AuNPs) solution with the concentration of 58.0 mu g/mL into each colorimetric tube, shaking up, continuously reacting for 1.5-3 minutes, diluting the solution to a scale with secondary distilled water, and scanning the solution on a fluorescence photometer by using a 1cm quartz cuvette in a mode of lambda ex lambda emA resonance scattering spectrum. The resonance scattering intensity I of the solutions with hydrogen peroxide added thereto was measured at a wavelength of 700nm700nmAnd the resonance scattering intensity I of a reagent blank solution without hydrogen peroxide0Calculating the difference DeltaI of the resonance scattering intensity700nm＝I700nm-I0Difference of resonant scattering intensity Δ I700nmWith a hydrogen peroxide concentration c of 7.29X 10-9～3.30×10-7Linear relation in mol/L range, linear regression equation is that delta I is 3.809 multiplied by 108c +2.657, correlation coefficient 0.9995, detection limit 2.43X 10-9mol/L; and filtering the pond water and the river water, measuring the resonance scattering intensity value by the same method by taking 0.2mL of filtrate, and calculating the content of hydrogen peroxide in the pond water and the river water.
The determination method has good selectivity and high sensitivity.
Drawings
FIG. 1 shows an embodiment of the present invention blank and 129.92 × 10-9mol/L H2O2The resonance scattering spectrogram of (1);
the labels in the figure are: a: blank; b: pH5.4 HAc-NaAc buffer solution-0.01 mol/L OPD-1.0X 10-6mol/LNiPcS4-129.92×10-9mol/L H2O2-AuNPs。
Detailed Description
Example (b):
to 11 5mL cuvettes, 0.08mL of a buffer solution of HAc-NaAc with pH5.4 and 0.08mL of a buffer solution of 1.0X 10-6NiPcS in mol/L40.12mL of 0.01mol/L OPD solution, and then 0.0, 0.003, 0.005, 0.006, 0.008, 0.013, 0.027, 0.054, 0.081, 0.108, and 0.137mL of 1.2X 10- 5After reacting for 15 minutes at room temperature with mol/L hydrogen peroxide solution, 0.6mL of 58.0 μ g/mL nanogold solution is added into each colorimetric cylinder, diluted to the scale with redistilled water, shaken up, and reacted for 2 minutes, and then a resonance scattering spectrum is scanned on a fluorescence photometer by using a 1cm quartz cuvette in a mode of λ ex ═ λ em. The resonance scattering intensity I of the solutions with hydrogen peroxide added thereto was measured at a wavelength of 700nm700nmAnd do notResonance scattering intensity of hydrogen peroxide-added reagent blank solution I0Calculating the difference DeltaI of the resonance scattering intensity700nm＝I700nm-I0Difference of resonant scattering intensity Δ I700nmWith a hydrogen peroxide concentration c of 7.29X 10-9～3.30×10-7Linear relation in mol/L range, linear regression equation is that delta I is 3.809 multiplied by 108c +2.657, correlation coefficient 0.9995, detection limit 2.43X 10-9mol/L; and filtering the pond water and the river water, measuring the resonance scattering intensity value by the same method by taking 0.2mL of filtrate, and substituting the measured value into the regression equation to calculate the content of the hydrogen peroxide in the pond water and the river water. The results of the spiking recovery experiments are shown in Table 1.
TABLE 1 Water sample analysis results (n ═ 5)
Sample (I) Measured value (10)-8mol/L) Recovery (%) RSD(％)
Pond water 10.165 100.9 2.0
River water 3.505 104.6 2.1
。

Claims (1)

1. A method for measuring trace hydrogen peroxide is characterized by comprising the following specific steps:
adding 0.06-0.12 mL of acetic acid-sodium acetate buffer solution with pH =5.4 into 11 colorimetric tubes with the concentration of 0.04-0.12 mL being 1.0 × 10-60.09-0.14 mL of o-phenylenediamine solution with the concentration of 0.01mol/L, and then 0.0, 0.003, 0.005, 0.006, 0.008, 0.013, 0.027, 0.054, 0.081, 0.108 and 0.137mL of o-phenylenediamine solution with the concentration of 1.2 multiplied by 10-5Reacting a hydrogen peroxide solution in mol/L for 15 minutes at room temperature, adding a nanogold solution with the concentration of 58.0 mu g/mL into each colorimetric tube in an amount of 0.3-0.8 mL, shaking up, continuously reacting for 1.5-3 minutes, diluting to a scale with secondary distilled water, and scanning a resonance scattering spectrum on a fluorescence photometer by using a 1cm quartz cuvette in a mode of lambda ex = lambda em; the resonance scattering intensity I of the solutions with hydrogen peroxide added thereto was measured at a wavelength of 700nm700nmAnd the resonance scattering intensity I of a reagent blank solution without hydrogen peroxide0Calculating the difference DeltaI of the resonance scattering intensity700nm=I700nm-I0Difference of resonant scattering intensity Δ I700nmWith a hydrogen peroxide concentration c of 7.29X 10-9～3.30×10-7Linear in mol/L range, and the linear regression equation is delta I =3.809 multiplied by 108c +2.657, correlation coefficient 0.9995, detection limit 2.43X 10-9mol/L; and filtering the pond water and the river water, measuring the resonance scattering intensity value by the same method by taking 0.2mL of filtrate, and calculating the content of hydrogen peroxide in the pond water and the river water.
CN201911175377.XA 2019-11-26 2019-11-26 Method for determining trace hydrogen peroxide based on tetra-sulfo nickel phthalocyanine Pending CN110907404A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103373751A (en) * 2012-04-26 2013-10-30 北京化工大学 Application of cationic iron arene complex serving as catalyst for photo-degradation of organic dye
CN104014371A (en) * 2014-06-16 2014-09-03 湖州师范学院 Calcium alginate supported metal phthalocyanine microsphere catalytic material and preparation method thereof
US20160205925A1 (en) * 2015-01-15 2016-07-21 Ariel-University Research And Development Company Ltd. Antimicrobial compositions made of a thermoplastic polymer and a photosensitizer
WO2017015145A2 (en) * 2015-07-17 2017-01-26 SeLux Diagnostics, Inc. Dissociable transition-metal nanoparticles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103373751A (en) * 2012-04-26 2013-10-30 北京化工大学 Application of cationic iron arene complex serving as catalyst for photo-degradation of organic dye
CN104014371A (en) * 2014-06-16 2014-09-03 湖州师范学院 Calcium alginate supported metal phthalocyanine microsphere catalytic material and preparation method thereof
US20160205925A1 (en) * 2015-01-15 2016-07-21 Ariel-University Research And Development Company Ltd. Antimicrobial compositions made of a thermoplastic polymer and a photosensitizer
WO2017015145A2 (en) * 2015-07-17 2017-01-26 SeLux Diagnostics, Inc. Dissociable transition-metal nanoparticles

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
AIHUI LIANG ET AL.，: "A Sensitive Resonance Scattering Spectral Assay for the Determination of Trace H2O2 Based on the HRP Catalytic Reaction and Nanogold Aggregation", 《JOURNAL OF FLUORESCENCE》 *
汪秋安: "《物理有机化学》", 31 December 2009, 湖南大学出版社 *
陈秋影等: "四磺基铁酞菁做为过氧化物模拟酶在过氧化氢及葡萄糖测定中的应用", 《分析化学》 *

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