CN109211883A - The chemiluminometry of concentration of hydrogen peroxide in a kind of detection solution - Google Patents
The chemiluminometry of concentration of hydrogen peroxide in a kind of detection solution Download PDFInfo
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- CN109211883A CN109211883A CN201710532530.4A CN201710532530A CN109211883A CN 109211883 A CN109211883 A CN 109211883A CN 201710532530 A CN201710532530 A CN 201710532530A CN 109211883 A CN109211883 A CN 109211883A
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
Abstract
The present invention relates to a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, the analytic approach measures the content of hydrogen peroxide in solution using the acridine sulfonamide of a class formation as luminous agent, compared with acridine ester type compound is as luminous agent, measurement result is accurate, and is not influenced by hydrogenperoxide steam generator pH.The chemiluminometry of concentration of hydrogen peroxide can be used for content of hydrogen peroxide detection in the fields such as chemical reagent, milk, industrial water, food processing in detection solution provided by the invention, it is compared with existing hydrogen peroxide detection technique, chemiluminescence detector need to be only equipped with, testing cost is low, easy to operate, detection rapidly and efficiently, after establishing standard curve, detection only needs a few minutes can be completed every time.
Description
Technical field
The present invention relates to a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, belong to chemiluminescence analysis
Field.
Background technique
Hydrogen peroxide is commonly called as hydrogen peroxide, is a kind of with strong oxidizing property, corrosive colourless transparent liquid.Hydrogen peroxide
As a kind of important chemical products in fields such as medicine, food, national defence, weaving, papermaking, the synthesis of chemical products and environmental protection
Middle extensive use is commonly used for disinfectant, bleaching agent, oxidant, liquid fuel, propellant etc., studies its detection method to peroxide
Concentration control and the safety evaluatio for changing hydrogen are significant.
Currently, the analysis method about concentration of hydrogen peroxide mainly has: conventional titration, electrochemical process, spectrophotometry,
Enzyme chemical method and chemoluminescence method etc..Wherein, the conventional titration of hydrogen peroxide be the oxidisability that is had according to hydrogen peroxide also
Originality, this method is easy to operate, but sensitivity is lower, and disturbing factor is more, and terminal discoloration is unobvious, and visual method is easy to produce mistake
Difference;Electrochemical process mainly includes polarography, amperometric titration and potentiostatic method, and the method is selectively preferable, but exists and be disturbed object
The disadvantages of matter is more, and reproducibility is poor;The sensitivity of spectrophotometry depends on the molar absorption coefficient of produced extinction material,
Its sensitivity is improved, the color developing agent for selecting that high molar absorption coefficient can be generated is needed;Enzyme chemical method has high sensitivity, single-minded
Property good and low detection limit advantage, but while measuring, needs using peroxidase, however the enzyme price is higher and easy in inactivation denaturation.
Chemiluminometry is according to a certain moment chemiluminescence intensity or chemiluminescence total amount in chemical reaction process
A kind of micro and trace analysis methods of respective components content in reaction are determined, since it has the highly sensitive, range of linearity
The feature that wide, equipment is simple and convenient to operate, easy to automate and analysis is quick, it has also become current chemical analysis field
One highly important research method.
Chemiluminescence can occur in the dilute alkaline soln for having hydrogen peroxide for acridinium ester or acridine sulfamide compound, but
It is to be influenced using the chemiluminometry of concentration of hydrogen peroxide in acridinium ester detection solution by hydrogenperoxide steam generator pH, i.e.,
Under different pH value, measurement same concentrations peroxide will appear it is different as a result, so as to cause measurement result accuracy
Low, method lacks the popularity and universality of application.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks present in the method for present analysis content of hydrogen peroxide, mention
For a kind of chemiluminometry of detection concentration of hydrogen peroxide not influenced by hydrogenperoxide steam generator pH.
The present invention is that technical solution used by solving its technical problem is:
The present invention provides a kind of chemiluminometry for detecting concentration of hydrogen peroxide in solution, comprising the following steps:
(1) compound concentration range is the Hydrogen peroxide standard solution of B1%-B2%;
(2) establish standard curve: in a reservoir be added volume be A, the acridine sulfonamide that concentration is A ', sequentially add immediately
Volume is B, and the Hydrogen peroxide standard solution and volume of B1%-B2% concentration described in step (1) is C, the hydrogen-oxygen that concentration is C '
Change sodium solution, total number of photons in the D time is collected respectively, by between total number of photons and the concentration of Hydrogen peroxide standard solution
Corresponding relationship obtains linear standard curve;
(3) sample analysis detect: in Chemiluminescence Apparatus be added volume be A, the acridine sulfonamide that concentration is A ', immediately according to
It is secondary that the hydrogenperoxide steam generator to be measured that volume is B and the sodium hydroxide solution that volume is C, concentration is C ' is added, it collects in the D time
Total number of photons;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured;
It is as follows in the structural formula of the acridine sulfonamide:
Wherein, R, R ' are selected from one of alkyl itself and its substituent, and X, X ' are selected from sulfonyl, halogen, carboxyl, N- hydroxyl
One of succinimide;
' >=1.5 AA (BB2) and B=C=(1.5~3.3) A, AA '=(2 in the step (2) and step (3)
~5) CC '.
Preferably, the pH of the hydrogenperoxide steam generator to be measured is 1-9.
Preferably, the D time is at least 0-5 seconds.
Preferably, the volume A of the acridine sulfonamide is 20-100 μ L, and concentration A ' is 3-10mol/L.
Preferably, the volume B of the hydrogen peroxide solution is 50-150 μ L.
Preferably, it is 0.3-1mol/L that the volume C of the sodium hydroxide solution, which is 50-150 μ L, C ',.
Preferably, the B1% is 0.01%, B2% 0.8%-2%.
Preferably, the Hydrogen peroxide standard solution sealing is kept in dark place.
The beneficial effects of the present invention are:
(1) chemiluminometry provided by the invention for detecting concentration of hydrogen peroxide in solution uses a word used for translation of a class formation
Pyridine sulfonamide measures the content of hydrogen peroxide in solution, and compared with acridine ester type compound, measurement result is accurate, and has not received
The influence of hydrogen peroxide solution pH.
(2) chemiluminometry of concentration of hydrogen peroxide can be used for chemical examination in detection solution provided by the invention
Content of hydrogen peroxide detects in the fields such as agent, milk, industrial water, food processing, with existing hydrogen peroxide detection technique phase
Than, only need to be equipped with chemiluminescence detector, testing cost is low, easy to operate, detection rapidly and efficiently, after establishing standard curve,
Detection only needs a few minutes can be completed every time.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now illustrate of the invention specific
Embodiment.
Embodiment 1
The present embodiment provides a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, comprising the following steps:
(1) it prepares Hydrogen peroxide standard solution: the commercially available reagent of hydrogen peroxide is carried out by standard GB/T 6684-86
Chemical method calibration, is then diluted calibrated reference substance, and the concentration that hydrogen peroxide is made is 0.01%, 0.05%,
0.15%, 0.3%, 0.6%, 1.2% series of concentrations Hydrogen peroxide standard solution;
(2) establish standard curve: in Chemiluminescence Apparatus plus 50 μ L, concentration is the acridine sulfonamide of 3.6mol/L, immediately according to
It is secondary that series of concentrations Hydrogen peroxide standard solution described in 100 μ L steps (1) and 100 μ L, the hydrogen-oxygen that concentration is 0.36mol/L is added
Change sodium solution, total number of photons in 0-5S is collected respectively, by pair between total number of photons and the concentration of Hydrogen peroxide standard solution
It should be related to obtain a linear standard curve (as shown in Figure 1), linear equation are as follows: y=1461.6x+0.0173, coefficient R2
=0.9996, range of linearity 0-1.2%;
(3) sample analysis detects: being added in Chemiluminescence Apparatus plus 50 μ L, concentration are the acridine sulphonyl of 3.6mol/L
Amine is separately added into 100 μ L hydrogenperoxide steam generator to be measured and 100 μ L, the sodium hydroxide solution that concentration is 0.36mol/L immediately, receives
Collect total number of photons in 5S;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured.
Preferably, as follows in the structural formula of acridine sulfonamide described in the present embodiment:
The accuracy of the present embodiment method is tested:
With the present embodiment method measurement known content for 0.2%, the hydrogenperoxide steam generator of different pH is as a result as follows:
As it can be seen that the accuracy of the present embodiment method is good, it can be with the hydrogenperoxide steam generator of accurate quantitative analysis difference pH.
Embodiment 2
The present embodiment provides a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, comprising the following steps:
(1) it prepares Hydrogen peroxide standard solution: the commercially available reagent of hydrogen peroxide is carried out by standard GB/T 6684-86
Chemical method calibration, is then diluted calibrated reference substance, and the concentration that hydrogen peroxide is made is 0.01%, 0.05%,
0.3%, 0.6%, 1.2%, 2% series of concentrations Hydrogen peroxide standard solution;
(2) establish standard curve: in Chemiluminescence Apparatus plus 20 μ L, concentration is the acridine sulfonamide of 10mol/L, immediately successively
Series of concentrations Hydrogen peroxide standard solution described in 50 μ L steps (1) and 50 μ L are added, concentration is that the sodium hydroxide of 1mol/L is molten
Liquid collects total number of photons in 0-5S, by the corresponding relationship between total number of photons and the concentration of Hydrogen peroxide standard solution respectively
Obtain a linear standard curve (as shown in Figure 2), linear equation are as follows: y=1475.1x-0.2052, coefficient R2=
0.9996, range of linearity 0-2%;
(3) sample analysis detects: it is added in Chemiluminescence Apparatus plus 20 μ L, concentration is the acridine sulfonamide of 10mol/L,
It is separately added into the hydrogenperoxide steam generator to be measured and 50 μ L of 50 μ L immediately, concentration is the sodium hydroxide solution of 1mol/L, is collected in 5S
Total number of photons;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured.
Preferably, as follows in the structural formula of acridine sulfonamide described in the present embodiment:
The accuracy of the present embodiment method is tested:
With the present embodiment method measurement known content for 1.5%, the hydrogenperoxide steam generator of different pH is as a result as follows:
The pH of hydrogenperoxide steam generator | 1 | 3 | 5 | 7 | 9 |
Measure content of hydrogen peroxide | 1.48% | 1.51% | 1.49% | 1.45% | 1.53% |
Measurement result relative error | 1.3% | 0.7% | 0.7% | 3.3% | 2% |
As it can be seen that the accuracy of the present embodiment method is good, it can be with the hydrogenperoxide steam generator of accurate quantitative analysis difference pH.
Embodiment 3
The present embodiment provides a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, comprising the following steps:
(1) it prepares Hydrogen peroxide standard solution: the commercially available reagent of hydrogen peroxide is carried out by standard GB/T 6684-86
Chemical method calibration, is then diluted calibrated reference substance, and the concentration that hydrogen peroxide is made is 0.01%, 0.05%,
0.15%, 0.3%, 0.6%, 0.8%, series of concentrations Hydrogen peroxide standard solution;
(2) establish standard curve: in Chemiluminescence Apparatus plus 100 μ L, concentration is the acridine sulfonamide of 3mol/L, immediately successively
Series of concentrations Hydrogen peroxide standard solution described in 150 μ L steps (1) and 150 μ L are added, concentration is the sodium hydroxide of 1mol/L
Solution collects total number of photons in 0-5S respectively, by the corresponding pass between total number of photons and the concentration of Hydrogen peroxide standard solution
System obtains a linear standard curve (as shown in Figure 3), linear equation are as follows: y=1478.5x-0.0515, coefficient R2=
0.9999, range of linearity 0-0.8%;
(3) sample analysis detects: it is added in Chemiluminescence Apparatus plus 100 μ L, concentration is the acridine sulfonamide of 3mol/L,
It is separately added into the hydrogenperoxide steam generator to be measured and 150 μ L, the sodium hydroxide solution that concentration is 1mol/L of 150 μ L immediately, collects 6S
Interior total number of photons;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured.
Preferably, as follows in the structural formula of acridine sulfonamide described in the present embodiment:
The accuracy of the present embodiment method is tested:
With the present embodiment method measurement known content for 0.5%, the hydrogenperoxide steam generator of different pH is as a result as follows:
The pH of hydrogenperoxide steam generator | 1 | 3 | 5 | 7 | 9 |
Measure content of hydrogen peroxide | 0.498% | 0.501% | 0.493% | 0.485% | 0.506% |
Measurement result relative error | 0.4% | 0.2% | 1.4% | 3% | 1.2% |
As it can be seen that the accuracy of the present embodiment method is good, it can be with the hydrogenperoxide steam generator of accurate quantitative analysis difference pH.
Embodiment 4
The present embodiment provides a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, comprising the following steps:
(1) it prepares Hydrogen peroxide standard solution: the commercially available reagent of hydrogen peroxide is carried out by standard GB/T 6684-86
Chemical method calibration, is then diluted calibrated reference substance, and the concentration that hydrogen peroxide is made is 0.01%, 0.05%,
0.15%, 0.3%, 0.6%, 1% series of concentrations Hydrogen peroxide standard solution;
(2) establish standard curve: in Chemiluminescence Apparatus plus 30 μ L, concentration is the acridine sulfonamide of 5mol/L, immediately successively
Series of concentrations Hydrogen peroxide standard solution described in 100 μ L steps (1) and 100 μ L are added, concentration is the hydroxide of 0.3mol/L
Sodium solution collects total number of photons in 5S respectively, by the corresponding pass between total number of photons and the concentration of Hydrogen peroxide standard solution
System obtains a linear standard curve (as shown in Figure 4), linear equation are as follows: y=1470.6x-0.0847, coefficient R2=
0.9997, range of linearity 0-1%;
(3) sample analysis detects: it is added in Chemiluminescence Apparatus plus 30 μ L, concentration is the acridine sulfonamide of 5mol/L,
It is separately added into the hydrogenperoxide steam generator to be measured and 100 μ L, the sodium hydroxide solution that concentration is 0.3mol/L of 100 μ L immediately, collects
Total number of photons in 0-5S;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured.
Preferably, as follows in the structural formula of acridine sulfonamide described in the present embodiment:
The accuracy of the present embodiment method is tested:
With the present embodiment method measurement known content for 0.8%, the hydrogenperoxide steam generator of different pH is as a result as follows:
The pH of hydrogenperoxide steam generator | 1 | 3 | 5 | 7 | 9 |
Measure content of hydrogen peroxide | 0.798% | 0.801% | 0.793% | 0.795% | 0.803% |
Measurement result relative error | 0.25% | 0.13% | 0.88% | 0.63% | 0.38% |
As it can be seen that the accuracy of the present embodiment method is good, it can be with the hydrogenperoxide steam generator of accurate quantitative analysis difference pH.
The embodiment of the present invention 1-4 uses acridine sulfonamide, and acridine sulphonyl in the step (2) and step (3)
Amine, the volume of exciting agent concentration and hydrogenperoxide steam generator and concentration meet following relationship: AA ' >=1.5 (BB2) and A=B=
(2~5) C, AA '=(2~5) CC ', so that when measuring different hydrogenperoxide steam generators, it will not be because of hydrogenperoxide steam generator pH
The influence of value and influence measurement result.
The embodiment of the present invention 1-4, the time of Chemiluminescence Apparatus acquisition photon is 5S in the step (2) and step (3),
This is because for luminous efficiency up to 90% or more, the number of photons of acquisition this period of 5S can make quantitative result accurate in 5 seconds.
The embodiment of the present invention 1-4, the Hydrogen peroxide standard solution are prepared weekly, are saved at 4 DEG C, and standard can be made molten
Concentration of hydrogen peroxide in liquid remains unchanged, and guarantees the accuracy of measurement result.
Comparative example
The present embodiment provides a kind of chemiluminometries of concentration of hydrogen peroxide in detection solution, comprising the following steps:
(1) it prepares Hydrogen peroxide standard solution: the commercially available reagent of hydrogen peroxide is carried out by standard GB/T 6684-86
Chemical method calibration, is then diluted calibrated reference substance, and the concentration that hydrogen peroxide is made is 0.01%, 0.05%,
0.15%, 0.3%, 0.6%, 1.2%, 2.5% series of concentrations Hydrogen peroxide standard solution;
(2) establish standard curve: in Chemiluminescence Apparatus plus 50 μ L, concentration is the acridinium ester of 2.5mol/L, is successively added immediately
Enter series of concentrations Hydrogen peroxide standard solution described in 100 μ L steps (1) and 100 μ L, concentration is the sodium hydroxide of 0.25mol/L
Solution collects total number of photons in 0-5S respectively, by the corresponding pass between total number of photons and the concentration of Hydrogen peroxide standard solution
System obtains a linear standard curve (as shown in Figure 5), linear equation are as follows: y=1240.2x, coefficient R2=0.9998, line
Property range be 0-1.2%;
(3) sample analysis detects: it is added in Chemiluminescence Apparatus plus 50 μ L, concentration is the acridinium ester of 2.5mol/L, with
The sodium hydroxide solution that the hydrogenperoxide steam generator to be measured and 100 μ L concentration for being separately added into 100 μ L are 0.25mol/L, collects 0-
Total number of photons in 5S;
(4) result calculates: step (3) is surveyed into total number of photons and is compareed with step (2) established linear standard curve,
Then by can be calculated the content of hydrogen peroxide in hydrogenperoxide steam generator to be measured.
Preferably, as follows in the structural formula of acridinium ester described in the present embodiment:
The accuracy of the present embodiment method is tested:
With the present embodiment method measurement known content for 0.2%, the hydrogenperoxide steam generator of different pH is as a result as follows:
The pH of hydrogenperoxide steam generator | 1 | 3 | 5 | 7 | 9 |
Measure content of hydrogen peroxide | 0.358% | 0.286% | 0.231% | 0.202% | 0.186% |
Measurement result relative error | 79% | 43% | 15.5% | 1% | 7% |
As it can be seen that the accuracy of this comparative example method is poor, it is not possible to the hydrogenperoxide steam generator of accurate quantitative analysis difference pH.
The chemiluminometry of concentration of hydrogen peroxide can be used for chemical reagent, ox in detection solution provided by the invention
Content of hydrogen peroxide detects in the fields such as milk, industrial water, food processing, compares with existing hydrogen peroxide detection technique, only
Chemiluminescence detector need to be equipped with, measurement result is accurate, testing cost is low, it is easy to operate, detection rapidly and efficiently, establish standard
After curve, detection only needs a few minutes can be completed every time, in addition, being measured using the acridine sulfonamide of structure of the present invention
The content of hydrogen peroxide in solution, compared with acridine ester type compound, measurement result not with the variation of hydrogenperoxide steam generator ph and
Variation.
Obviously, the above embodiments are merely examples for clarifying the description, does not limit the embodiments.For
For those of ordinary skill in the art, other various forms of variations or change can also be made on the basis of the above description
It is dynamic.There is no necessity and possibility to exhaust all the enbodiments.And obvious variation extended from this or change
It moves still within the protection scope of the invention.
Claims (8)
1. the chemiluminometry of concentration of hydrogen peroxide in a kind of detection solution, which comprises the following steps:
(1) compound concentration range is the Hydrogen peroxide standard solution of B1%-B2%;
(2) establish standard curve: in a reservoir be added volume be A, the acridine sulfonamide that concentration is A ', sequentially add volume immediately
For B, the Hydrogen peroxide standard solution of B1%-B2% concentration described in step (1) and the sodium hydroxide that volume is C, concentration is C '
Solution collects total number of photons in the D time, by corresponding between total number of photons and the concentration of Hydrogen peroxide standard solution respectively
Relationship obtains linear standard curve;
(3) sample analysis detect: in Chemiluminescence Apparatus be added volume be A, the acridine sulfonamide that concentration is A ', immediately successively plus
Enter the hydrogenperoxide steam generator to be measured that volume is B and the sodium hydroxide solution that volume is C, concentration is C ', collects total light in the D time
Subnumber;
(4) result calculates: step (3) being surveyed total number of photons and is compareed with step (2) established linear standard curve, then
By the content that can be calculated hydrogen peroxide in hydrogenperoxide steam generator to be measured;
It is as follows in the structural formula of the acridine sulfonamide:
Wherein, R, R ' are selected from one of alkyl and its substituent, and X, X ' are selected from sulfonyl, halogen, carboxyl, N- hydroxysuccinimidyl acyl
One of imines;
' >=1.5 AA (BB2) and B=C=(1.5~3.3) A, AA '=(2~5) in the step (2) and step (3)
CC '.
2. the chemiluminometry of concentration of hydrogen peroxide, the acridine sulphonyl in detection solution according to claim 1
The structural formula of amine is one of following structures:
3. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to claim 2, which is characterized in that institute
Stating the D time is at least 5 seconds.
4. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to any one of claim 1-3,
It is characterized in that, the volume A of the acridine sulfonamide is 20-100 μ L, and concentration A ' is 3-10mol/L.
5. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to any one of claim 1-3,
It is characterized in that, the volume B of the hydrogenperoxide steam generator is 50-150 μ L.
6. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to any one of claim 1-3,
It is characterized in that, it is 0.3-1mol/L that the volume C of the sodium hydroxide solution, which is 50-150 μ L, C ',.
7. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to claim 1 to 6,
It is characterized in that, which is characterized in that the B1% is 0.01%, B2% 0.8%-2%.
8. the chemiluminometry of concentration of hydrogen peroxide in detection solution according to claim 1 to 6,
It is characterized in that, the Hydrogen peroxide standard solution sealing is kept in dark place.
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