CN108508056A - A kind of method of accurate quantification trace solid free-radical contents - Google Patents

A kind of method of accurate quantification trace solid free-radical contents Download PDF

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Publication number
CN108508056A
CN108508056A CN201810114127.4A CN201810114127A CN108508056A CN 108508056 A CN108508056 A CN 108508056A CN 201810114127 A CN201810114127 A CN 201810114127A CN 108508056 A CN108508056 A CN 108508056A
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China
Prior art keywords
sample
radical contents
accurate quantification
free
solid free
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CN201810114127.4A
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Chinese (zh)
Inventor
汪
汪一
熊哲
向军
胡勋
陈元静
许凯
苏胜
胡松
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/10—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using electron paramagnetic resonance

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  • Physics & Mathematics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The present invention relates to a kind of methods of accurate quantification trace solid free-radical contents.Sample is only 2~10mg needed for being tested in method provided by the invention, and sample consumption is small, is applicable to the few test of sample size；This method is ground uniform after mixing sample to be tested with potassium bromide, make sample comminution at subtle even particulate dispersion in potassium bromide, increase sample to be tested amount, also avoids the test error caused by the difference of sample geometry and accumulation shape, improve measuring accuracy.

Description

A kind of method of accurate quantification trace solid free-radical contents
Technical field
The present invention relates to free radical quantitative measurement technology fields more particularly to a kind of accurate quantification trace solid free radical to contain The method of amount.
Background technology
Substance containing unpaired electronics equal available electron EPR spectrometer (EPR) is detected.Electron paramagnetic resonance Technology so far physics, semiconductor, organic chemistry, the chemistry of complex, radiation chemistry, chemical industry, Marine Chemistry, catalyst, Biology, biochemistry, medicine, environmental science, geological exploration etc. are widely used in many fields.Free radical it is accurate It is quantitative, it is the key that the technology deeply utilizes.As a kind of coal tar free radical in patent CN103105409A quantitatively detects Method, the standard specimen for using known free-radical contents establish standard curve and are quantified.However, EPR detections are very sensitive, survey The subtle change of strip part all can generate large effect, even if can have larger survey if establishing standard curve to result Measure error.The key of EPR quantitative tests is sensitivity, stability and repeatability.
When being quantified to sample free-radical contents, geometry, temperature, resonant cavity quality (the Q- factors), microwave work( Rate, the parameters such as modulation amplitude have direct influence to result.By control to test equipment and maintenance and to test environment Accurately control, temperature, resonant cavity quality (the Q- factors), microwave power, the parameters such as modulation amplitude can be in multiple measure Keep good consistency.However, when detection sample size is less, since Sample tube size is relatively large, lead to sample itself Geometry and accumulation shape when test be difficult to keep completely the same in multiple measure, even result in resonant cavity quality (the Q- factors) also changes, and further results in that final measurement result is less reproducible, leads to the error measured.
If being avoided that the test process sample geometry of itself and accumulating influence of the present situation to test result, it will pole The stability and repeatability that big raising EPR is quantitatively detected, improve the accuracy of measurement.Therefore, a set of perfect be directed to is established The free radical accurate quantitative analysis method of micro-example is very necessary.
Invention content
For the above problem existing for existing small sample test, it is micro now to provide a kind of reproducible accurate quantification The method of solid free radical content.
Specific technical solution is as follows：
A kind of method of accurate quantification trace solid free-radical contents, has the feature that, includes the following steps：
1) a small amount of sample to be tested, is taken, is weighed, it is m to record its quality1；
2) the spectroscopic pure potassium bromide being completely dried on a small quantity, is taken, is weighed, it is m to record its quality2；
3) sample to be tested is mixed with potassium bromide, and grinds the fine powder to be formed and be uniformly mixed；
4) a certain amount of fine powder, is taken, is weighed, it is m to record its quality3, fine powder is fitted into sample cell, and make its densification It is distributed in the bottom of sample cell；
5), sample cell is put into resonator and is measured, according to calibration curve method, obtains its free-radical contents f (S1), it calculates Free-radical contents f (S in sample to be tested2) be：
The method of above-mentioned accurate quantification trace solid free-radical contents, also has the feature that, 2mg in step 1)≤ m1≤10mg。
The method of above-mentioned accurate quantification trace solid free-radical contents, also has the feature that, 20mg in step 2) ≤m2≤100mg。
The method of above-mentioned accurate quantification trace solid free-radical contents, also has the feature that, 20mg in step 4) ≤m3≤50mg。
The method of above-mentioned accurate quantification trace solid free-radical contents, also has the feature that, will be thin in step 4) Powder is fitted into sample cell, and by sample cell centrifugal treating, fine powder densification is made to be distributed in the bottom of sample cell.
It can be compared by the test result of sample to be tested and the standard sample of multiple and different free-radical contents in the present invention, root According to the test result and its free-radical contents of standard specimen, standard curve is drawn, you can the base content that gains freedom and EPR test results Functional relation f (S).
The advantageous effect of said program is：
(1) sample is only 2~10mg needed for being tested in method provided by the invention, and sample consumption is small, is applicable to sample The few test of product amount；
(2) it is ground uniformly after this method mixes sample to be tested with potassium bromide, keeps sample comminution uniform at subtle particle It is scattered in potassium bromide, increases sample to be tested amount, also avoid same sample sample when retest process is because of test every time Test error caused by the difference of geometry and accumulation shape (resonant cavity quality Q factor), improves measuring accuracy.
Description of the drawings
Fig. 1-Fig. 4 is the reperformance test result schematic diagram of 4 different coal tar samples in the embodiment of the present invention；
Fig. 5 is reperformance test result schematic diagram in existing conventional techniques.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art obtained under the premise of not making creative work it is all its His embodiment, shall fall within the protection scope of the present invention.
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase Mutually combination.
The invention will be further described in the following with reference to the drawings and specific embodiments, but not as limiting to the invention.
Include the following steps in the method for determining amount trace solid free-radical contents provided in this embodiment：It takes a small amount of to be measured Sample weighs, and it is m to record its quality1, 2mg≤m1≤10mg；The spectroscopic pure potassium bromide being completely dried on a small quantity is taken, is weighed, record Its quality is m2, 20mg≤m2≤100mg；Sample to be tested is mixed with potassium bromide and grinds the fine powder to be formed and be uniformly mixed；It takes A certain amount of fine powder weighs, and it is m to record its quality3, 20mg≤m3≤ 50mg, fine powder is fitted into sample cell, and by sample Pipe centrifugal treating makes fine powder densification be distributed in the bottom of sample cell；Sample cell is put into resonator and is measured, and by its freedom Base signal S1Free-radical contents standard curve is substituted into, its free-radical contents f (S are obtained1), calculate to obtain free-radical contents f in sample to be tested (S2) be：
Fig. 1-Fig. 4 is the reperformance test result schematic diagram of 4 different coal tar samples in the embodiment of the present invention；Fig. 5 is existing There is reperformance test result schematic diagram in routine techniques.Shown in Fig. 1-Fig. 4, carried out using the test method provided in the present invention When the parallel testing of 4 different sample sets, experiment curv is tested twice and is identical, the test provided in the present invention is provided Method relative to when being measured using routine techniques in Fig. 5 have more excellent repeatability.
It these are only preferred embodiments of the present invention, be not intended to limit the implementation manners and the protection scope of the present invention, it is right For those skilled in the art, it should can appreciate that and all be replaced with being equal made by description of the invention and diagramatic content It changes and obviously changes obtained scheme, should all be included within the scope of the present invention.

Claims (5)

1. a kind of method of accurate quantification trace solid free-radical contents, which is characterized in that include the following steps：
1) a small amount of sample to be tested, is taken, is weighed, it is m to record its quality1；
2) the spectroscopic pure potassium bromide being completely dried on a small quantity, is taken, is weighed, it is m to record its quality2；
3) sample to be tested is mixed with the potassium bromide, and grinds the fine powder to be formed and be uniformly mixed；
4) a certain amount of fine powder, is taken, is weighed, it is m to record its quality3, the fine powder is fitted into sample cell, and make it Densification is distributed in the bottom of the sample cell；
5), sample cell is put into resonator and is measured, its free-radical contents f (S are obtained according to calibration curve method1), it calculates described to wait for Free-radical contents f (S in sample2) be：
2. the method for accurate quantification trace solid free-radical contents according to claim 1, which is characterized in that in step 1) 2mg≤m1≤10mg。
3. the method for accurate quantification trace solid free-radical contents according to claim 1, which is characterized in that in step 2) 20mg≤m2≤100mg。
4. the method for accurate quantification trace solid free-radical contents according to claim 1, which is characterized in that in step 4) 20mg≤m3≤50mg。
5. according to the method for claim 1-4 any one of them accurate quantification trace solid free-radical contents, which is characterized in that The fine powder is fitted into the sample cell in step 4), and by the sample cell centrifugal treating, keeps the fine powder fine and close It is distributed in the bottom of the sample cell.
CN201810114127.4A 2018-02-05 2018-02-05 A kind of method of accurate quantification trace solid free-radical contents Pending CN108508056A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112630252A (en) * 2020-11-05 2021-04-09 浙江大学 Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4668714A (en) * 1984-08-30 1987-05-26 Japan Atomic Energy Research Institute Molded dosimeter containing a rubber and powdered crystalline alanine
SU1603266A1 (en) * 1988-12-13 1990-10-30 Институт Торфа Ан Бсср Calibration specimen for epr-spectroscopy
CN103105409A (en) * 2013-01-16 2013-05-15 华东理工大学 Method for detecting free radical ration in coal tar
CN103472083A (en) * 2013-09-17 2013-12-25 上海大学 Method for detecting influence of electron beam irradiation on free radical concentration of coal by virtue of electron paramagnetic resonance

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4668714A (en) * 1984-08-30 1987-05-26 Japan Atomic Energy Research Institute Molded dosimeter containing a rubber and powdered crystalline alanine
SU1603266A1 (en) * 1988-12-13 1990-10-30 Институт Торфа Ан Бсср Calibration specimen for epr-spectroscopy
CN103105409A (en) * 2013-01-16 2013-05-15 华东理工大学 Method for detecting free radical ration in coal tar
CN103472083A (en) * 2013-09-17 2013-12-25 上海大学 Method for detecting influence of electron beam irradiation on free radical concentration of coal by virtue of electron paramagnetic resonance

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李佃平 等: "《矿井综放工作面自然发火的早期预控技术及应用》", 31 May 2011, 煤炭工业出版社 *
郑榕萍 等: "标准曲线法测定煤中自由基含量", 《波谱学杂志》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112630252A (en) * 2020-11-05 2021-04-09 浙江大学 Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole
CN112630252B (en) * 2020-11-05 2022-04-01 浙江大学 Nondestructive testing method for stability of tablet containing antioxidant butyl hydroxy anisole

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