CN104677890A - Method for simply and rapidly detecting aniline - Google Patents
Method for simply and rapidly detecting aniline Download PDFInfo
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- CN104677890A CN104677890A CN201510067167.4A CN201510067167A CN104677890A CN 104677890 A CN104677890 A CN 104677890A CN 201510067167 A CN201510067167 A CN 201510067167A CN 104677890 A CN104677890 A CN 104677890A
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- aniline
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Abstract
The invention discloses a method for simply and rapidly detecting aniline. The method comprises the following steps: a. preparing a nano silver solution and an aniline standard solution; b. preparing a premixed liquid; c. carrying out chemiluminescence analysis and detection and making a standard curve; and d. determining to-be-detected liquid. According to the method disclosed by the invention, the problem of inconvenient operation caused by viscous polyphosphoric acid in a polyphosphoric acid medium system which is adopted by current chemical analysis and detection of aniline can be solved; by virtue of a classical chemiluminescence analysis system, entire operation experimental conditions are relatively moderate, the operation is easy and automatic analysis and operation are facilitated since the method is completed in a homogeneous system; analysis and testing time can be shortened to be within 10min. The developed method for detecting aniline has the advantages of being simple, rapid and sensitive.
Description
Technical field
The present invention relates to a kind of detection method, particularly a kind of method of simple and quick detection aniline.
Background technology
Aniline is a kind of important Organic Chemicals, is widely used in the art production process such as rubber, printing and dyeing, pharmacy, plastics, delft.Be considered to a kind of material of carcinogenicity, belong to high toxic material.Methemoglobin can be combined into haemoglobin in body, and haemoglobin and oxygen binding ability be declined cause human body poisoning.By sucking and absorption features, aniline can cause human body acute poisoning or slow poisoning, produces headache, dizzy, tired, decrease of memory, unsmooth breath, even the symptom such as death by suffocation, and long-term contact with aniline also can cause cancer.Therefore, aniline has become one of important Testing index of various countries' environmental protection, hygiene department, and China is listed in the pollutant of priority monitoring already.
The assay method of current aniline mainly contains spectrophotometric method, fluorescence method, electrochemical methods and chromatography etc.The sensitivity that these methods have is not high, interference large, bothers during some operating costs, and some instruments are expensive, it is high to require, not easily promote.Chemiluminometry have highly sensitive, instrument simple, analyze and realize the advantages such as robotization fast, easily, but it is also considerably less to use chemiluminescence analysis to detect the report of aniline.And there are some defects: owing to using polyphosphoric acids medium system, the viscosity that polyphosphoric acids has, brings a lot of inconvenience to operation.The more important thing is that increase (up to the 0.1M) viscosity along with polyphosphoric acids concentration increases, occur the problem of the division of luminous peak shape and poor reproducibility.Therefore, chemiluminescence analysis detects the place that aniline also has number of values to improve, and development is simple, rapid chemical luminesceence analysis detects the method for aniline highly significant.
Summary of the invention
The object of the invention is to provide a kind of method of simple, sensitive, quick detection aniline.After utilizing aniline and Nano Silver to interact, Nano Silver to the enhancing of luminol chemiluminescence signal, thus identifies aniline.
Technical scheme of the present invention is for achieving the above object:
A method for simple and quick detection aniline, comprises the steps:
A. the preparation of Nano silver solution and aniline standard solution: prepare Nano silver solution, the Nano Silver particle diameter in described Nano silver solution is 4-10nm; Prepare the aniline standard solution of variable concentrations;
B. the preparation of premixed liquid: the Nano silver solution getting same volume respectively with the aniline standard solution of variant concentration and liquid to be measured miscible, make premixed liquid respectively; The aniline standard solution of described variant concentration and liquid to be measured volume used identical;
C. the making of chemiluminescence analysis detection and typical curve: pipette premixed liquid that Nano silver solution makes with the aniline standard solution of variant concentration respectively in chemiluminescence pond, then inject respectively and institute's premixed liquid of getting isopyknic Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent, measured respectively by chemiluminescent analyzer and record chemiluminescence intensity, according to the luminous intensity of the aniline standard solution of variable concentrations, production standard curve;
D. liquid to be measured is measured: pipette premixed liquid that Nano silver solution and liquid to be measured makes in chemiluminescence pond, then inject isopyknic Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent, measured by chemiluminescent analyzer and record its chemiluminescence intensity, determining the concentration of aniline in liquid to be measured according to the typical curve made.
Further technical scheme, the preparation method of described Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent is: the concentration of luminol solution is 5 × 10
-5mol/L, superoxol concentration is 1 × 10
-2mol/L; Both volume ratios are 2:1.
Further technical scheme, the pH value of described Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent is 12.0.
The collocation method of each solution of the present invention is as follows:
Luminol solution: 4.43g luminol pressed powder to be dissolved in 20mL 0.10M NaOH solution and to be diluted to 1L, preparing 2.5 × 10
– 2m luminol stock solution.Keep in Dark Place a week to guarantee the stable of reagent properties before use.The working solution of luminol is obtained by the dilution of stock solution.
H
2o
2working solution when each use from 30% (w/w) H
2o
2(Solution on Chemical Reagents in Shanghai company) dilution obtains.Accurately take 0.93g aniline (Solution on Chemical Reagents in Shanghai company) with using secondary deionized water constant volume after a small amount of 0.1M diluted hydrochloric acid dissolution in 100mL volumetric flask, the aniline stock solutions of obtained 9.3g/L is placed in refrigerator and preserves, and is diluted to desired concn during use.Experimental water is secondary deionized water.
The preparation of Nano silver solution: glassware used in preparation process all uses chloroazotic acid (1:3HNO
3– HCl) soaking and washing, then use secondary deionized water cleaning down clean, dry for standby.Preparation process: the pH value of 20mL 0.1mol/L liquor argenti nitratis ophthalmicus is adjusted to 10 with ethylenediamine, add the methyl bromide amine (CTAB) of 0.01g 0.5g/L, completely after mixing, within 5 minutes, 5mL hydrazine hydrate is dropwise added under continuous stirring, above-mentioned solution at room temperature reacts 5 minutes, generates Nano silver solution.Be put in brown bottle, 4 DEG C of preservations are stand-by.Obtained Nano silver solution transmission electron microscope and uv-visible absorption spectra characterize.Nano Silver particle diameter in described Nano silver solution is 4-10nm.
The condition of whole operation experiments of the present invention is gentleer, is easy to operation, and completes in the system of a homogeneous phase, be conducive to the analysis operation of robotization; The analytical test time shorten of the method is within 10 minutes; Owing to being introduced in chemiluminescence reaction by the catalytic performance of Nano Silver, substantially increase sensitivity, detection limit reaches 8.2 × 10
– 12g/mL, an order of magnitude lower than the sensitivity of the existing chemiluminescence analysis method not having nano particle to participate in.
Accompanying drawing explanation
Fig. 1 chemiluminescence analysis detects the typical curve of aniline
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment
Embodiment 1
Production standard curve: configuration concentration is respectively 0.15 × 10
– 9g/mL, 0.32 × 10
– 9g/mL, 0.63 × 10
– 9g/mL, 6.3 × 10
– 9g/mL, 8.2 × 10
– 9g/mL, 28 × 10
– 9g/mL and 63 × 10
– 9the aniline standard solution of g/mL, then measures by method of the present invention, drawing standard curve.
Concrete mensuration process is as follows: (1) pipettes equal-volume Nano silver solution and aniline solution in a centrifuge tube, fully mixes, and acts on and within 5 minutes, makes to interact completely; (2) pipette above-mentioned Nano silver solution/aniline solution 200 μ L in chemiluminescence pond (40 × 14mm quartz ampoule), inject 200 μ L Shandong rice promise – hydrogen peroxide chemistry luminescence reagents (5 × 10
-5m luminol and 1 × 10
-2the volume ratio of M hydrogen peroxide is 2:1), measured by IFFL-D Flow Injection Analysis/Chemiluminescence instrument and record its chemiluminescence intensity.According to concentration and the corresponding chemiluminescence intensity drawing standard curve of aniline standard solution, as shown in Figure 1.
The result of experiment shows, along with the increase of concentration of aniline, chemiluminescence signal strengthens gradually.And 1.5 × 10
-10~ 6.3 × 10
-8in the concentration range of g/mL, the intensity of chemiluminescence signal becomes good correlativity with the logarithm value of concentration of aniline, and as shown in Figure 1, it detects and is limited to 8.2 × 10 typical curve
– 12g/mL (S/N=3).And to 6.3 × 10
-9the aniline replicate determination of g/mL 11 times, its relative standard deviation is 4.2%.Experimental result shows that the method detection limit is low, and precision is good.A high order of magnitude is wanted in the sensitivity of more current only chemiluminescence analysis method, and than more easily operating.
Embodiment 2-7
Embodiment 2-4 takes from water water sample, embodiment 5-7 gets lake water water sample and carries out recovery testu respectively according to above-mentioned experimental procedure, obtained the aniline content in each sample by typical curve, the addition (g/mL) of the aniline of 6 embodiments, measured value (g/mL), the recovery (%) and relative standard deviation (RSD) are as shown in table 1.Specific experiment step is as follows:
Take from water and lake water sample carries out recovery testu.After tap water and lake water being filtered with Medium speed filter paper respectively, dilute to volume in 100mL volumetric flask by secondary deionized water.Adopt standard addition method to carry out the experiment of the recovery, result is as shown in table 1.
The result of Measurement of Aniline in table 1 water sample
Experimental result shows, the method that the present invention sets up has good accuracy and precision, and the recovery is respectively 98.08% ~ 111.05%, RSD is 1.8% ~ 4.6%, analysis time is short, does not need to use large-scale instrument, can be used for the quick detection of aniline in water sample.
Interference measurement
Under these experimental conditions, in 8.6 × 10
– 9in g/mL aniline solution, add the NH of 1000 times respectively
4 +, NO
3 -, NO
2 -, SO
4 2-, SO
3 2-, CO
3 2-, P0
4 3-, 100 times, Zn
2+, Na
+, Ni
+, Cl
-, K
+, Cr
3+, the Cu of 10 times
2+, Al
3+, Ba
2+, Mg
2+, Ca
2+, Fe
3+etc. carrying out interference experiment, result shows all not interference measurements.In addition, common are the mensuration that machine thing phenol, acetic acid, ethyl acetate do not disturb aniline under normal concentration in water.
The method detecting aniline based on Nano Silver catalysis luminol chemiluminescence response analysis that the present invention sets up, overcome above-mentioned detection method shortcoming, have the following advantages: (1) uses the chemiluminescence analysis system of luminol-hydrogen peroxide classics, be easy to operation, the condition of whole operation experiments is gentleer, and complete in the system of a homogeneous phase, be conducive to the analysis operation of robotization; (2) the analytical test time shorten of the method is within 10 minutes; (3) owing to being introduced in chemiluminescence reaction by the catalytic performance of Nano silver solution, substantially increase sensitivity, detection limit reaches 8.2 × 10
– 12g/mL, than a highly sensitive order of magnitude of the existing chemiluminescence analysis method not having nano particle to participate in.
Find after deliberation when Nano Silver particle diameter is 4-10nm, just can obtain the luminescence system of aforementioned stable.
The above embodiment is only that the preferred embodiment of the present invention is described; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (3)
1. a method for simple and quick detection aniline, is characterized in that, comprise the steps:
A. the preparation of Nano silver solution and aniline standard solution: prepare Nano silver solution, the Nano Silver particle diameter in described Nano silver solution is 4-10nm; Prepare the aniline standard solution of variable concentrations;
B. the preparation of premixed liquid: the Nano silver solution getting same volume respectively with the aniline standard solution of variant concentration and liquid to be measured miscible, make premixed liquid respectively; The aniline standard solution of described variant concentration and liquid to be measured volume used identical;
C. the making of chemiluminescence analysis detection and typical curve: pipette premixed liquid that Nano silver solution makes with the aniline standard solution of variant concentration respectively in chemiluminescence pond, then inject respectively and institute's premixed liquid of getting isopyknic Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent, measured respectively by chemiluminescent analyzer and record chemiluminescence intensity, according to the luminous intensity of the aniline standard solution of variable concentrations, production standard curve;
D. liquid to be measured is measured: pipette premixed liquid that Nano silver solution and liquid to be measured makes in chemiluminescence pond, then inject isopyknic Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent, measured by chemiluminescent analyzer and record its chemiluminescence intensity, determining the concentration of aniline in liquid to be measured according to the typical curve made.
2. detect the method for aniline as claimed in claim 1, it is characterized in that, the preparation method of described Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent is: the concentration of luminol solution is 5 × 10
-5mol/L, superoxol concentration is 1 × 10
-2mol/L; Both volume ratios are 2:1.
3. detect the method for aniline as claimed in claim 1, it is characterized in that, the pH value of described Lu meter Nuo – hydrogen peroxide chemistry luminescence reagent is 12.0.
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| CN201510067167.4A CN104677890A (en) | 2015-02-09 | 2015-02-09 | Method for simply and rapidly detecting aniline |
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|---|---|---|---|
| CN201510067167.4A CN104677890A (en) | 2015-02-09 | 2015-02-09 | Method for simply and rapidly detecting aniline |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290319A (en) * | 2016-08-04 | 2017-01-04 | 福建工程学院 | A kind of method of silver ion in chemiluminescence detection water sample |
Citations (3)
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|---|---|---|---|---|
| CN2068418U (en) * | 1989-12-21 | 1991-01-02 | 西南石油学院 | Batch liquid-removing apparatus for chemical test |
| CN103293145A (en) * | 2013-05-16 | 2013-09-11 | 赫利森（厦门）生物科技有限公司 | Chemiluminescence reagent |
| CN104122255A (en) * | 2014-07-15 | 2014-10-29 | 东南大学 | Aniline solid phase electrochemiluminescence detection method |
-
2015
- 2015-02-09 CN CN201510067167.4A patent/CN104677890A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2068418U (en) * | 1989-12-21 | 1991-01-02 | 西南石油学院 | Batch liquid-removing apparatus for chemical test |
| CN103293145A (en) * | 2013-05-16 | 2013-09-11 | 赫利森（厦门）生物科技有限公司 | Chemiluminescence reagent |
| CN104122255A (en) * | 2014-07-15 | 2014-10-29 | 东南大学 | Aniline solid phase electrochemiluminescence detection method |
Non-Patent Citations (5)
| Title |
|---|
| F. GARCIA SANCHEZ ET AL.: "P-phenol derivatives as enhancers of the chemiluminescent luminol-horseradish peroxidase-H,02 reaction : substituent effects", 《JOURNAL OF LUMINESCENCE》 * |
| TANT¸A SP˘ATARU ET AL.: "Detection of aniline at boron-doped diamond electrodes with cathodic stripping voltammetry", 《TALANTA》 * |
| YINGYING QI ET AL.: "Effect of aggregated silver nanoparticles on luminol chemiluminescence system and its analytical application", 《SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY》 * |
| 樊雪梅等: "Luminol － H2 O2 － 纳米银化学发光体系测定5-磺基水杨酸", 《分析试验室》 * |
| 陈昀等: "环境样品中苯胺类化合物检测方法的研究进展", 《广州化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290319A (en) * | 2016-08-04 | 2017-01-04 | 福建工程学院 | A kind of method of silver ion in chemiluminescence detection water sample |
| CN106290319B (en) * | 2016-08-04 | 2019-04-05 | 福建工程学院 | A kind of method of silver ion in chemiluminescence detection water sample |
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Application publication date: 20150603 |