CN108132221B - Method for detecting total phenol content in water - Google Patents
Method for detecting total phenol content in water Download PDFInfo
- Publication number
- CN108132221B CN108132221B CN201611088428.1A CN201611088428A CN108132221B CN 108132221 B CN108132221 B CN 108132221B CN 201611088428 A CN201611088428 A CN 201611088428A CN 108132221 B CN108132221 B CN 108132221B
- Authority
- CN
- China
- Prior art keywords
- water
- aqueous solution
- detecting
- content
- chloride aqueous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
-
- 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 detecting the total phenol content in water, which comprises the steps of activating 4-aminoantipyrine by copper tetraammine chloride under an alkaline condition to form a stable mixed solution, adding a phenolic compound to be detected for reaction, and comparing the absorbance change of the mixed solution before and after adding the phenolic compound reversely, so that the total content of the phenolic compound in an analyte can be quantitatively detected. The method has the advantages of avoiding toxic irritant oxidants such as potassium ferricyanide or potassium persulfate and the like which are usually used when 4-aminoantipyrine is used for detecting phenolic substances, along with simple and convenient operation, low cost, high analysis speed, low method detection limit and short analysis period.
Description
Technical Field
The invention relates to the technical field of detection and analysis, in particular to a method for detecting the content of total phenols in water.
Background
The phenol and the derivatives thereof have moderately toxic compounds, can enter the human body through skin mucosa, respiratory tract, oral cavity and other ways, and form denatured protein through chemical reaction with protein in the cell protoplasm to inactivate cells. Phenol and its derivatives enter human body at high concentration, and can cause acute poisoning and even coma and death. It is toxic to the nervous system, urinary system and digestive system. Meanwhile, the phenolic substances have great harm to the environment, and the phenol-containing wastewater flows into farmlands or underground water to cause pollution, so that the growth of crops and aquatic organisms is delayed and even the crops and the aquatic organisms die. Wherein 6 phenols are in the blacklist of preferential pollutants in water, and comprise phenol, m-cresol, pentachlorophenol, 2, 4-dichlorophenol, 2,4, 6-trichlorophenol and p-nitrophenol.
The method for measuring and analyzing the volatile phenol in the industrial wastewater is more, and the 4-aminoantipyrine spectrophotometry is commonly adopted in various countries at present, and the method for measuring the phenol is also adopted by the international organization for standardization. The method uses K3Fe(CN)6As an oxidizing agent, the complex formed is not very stable in water and water, and the color comparison is usually completed within 30min, otherwise the complex is decomposed. And potassium ferricyanide can generate a virulent substance under proper conditions in the environment, so that the environment is polluted.
Disclosure of Invention
Aiming at the problems, the invention provides a method for detecting the total phenol content in water, which comprises the steps of activating 4-aminoantipyrine by using copper tetraammine chloride water under an alkaline condition to form a stable mixed solution, then adding a phenolic compound for reaction, and comparing the change of absorbance of the mixed solution before and after adding the phenolic compound in a reverse manner, so that the total content of the phenolic compound in an analyte can be quantitatively detected. The method has the advantages of avoiding toxic irritant oxidants such as potassium ferricyanide or potassium persulfate and the like which are usually used when 4-aminoantipyrine is used for detecting phenolic substances, along with simple and convenient operation, low cost, high analysis speed, low method detection limit and short analysis period.
The invention relates to a method for detecting the content of total phenols in water, which is realized by the following technical scheme:
(1) preparing a copper chloride aqueous solution with the mass fraction of 1-20%; dropwise adding concentrated ammonia water with the mass fraction of 25-28% into copper chloride water, wherein the volume ratio of copper chloride aqueous solution to concentrated ammonia water is 1: 1-5; shaking up to obtain a clear tetrammine copper chloride aqueous solution A;
(2) preparing 1-10% 4-aminoantipyrine aqueous solution by mass fraction; sequentially mixing a copper tetrammine chloride aqueous solution and 4-aminoantipyrine A according to the volume ratio of 1-10: 2-100, adding the mixture into a test tube, shaking uniformly, and standing for 1-20 minutes to obtain a total phenol detection reagent B;
(3) adding a total phenol detection reagent B into a water sample to be detected, wherein the volume ratio of the total phenol detection reagent B to the water sample to be detected is 1-5: 0.1-20, mixing and standing for 1-20 minutes, detecting the change of absorbance at 540nm of an absorption spectrum, and calculating the content of total phenols in water.
When the copper chloride aqueous solution is prepared in the step (1), microwave ultrasonic or magneton stirring is used for uniform dispersion.
The volume ratio of the copper chloride aqueous solution to the concentrated ammonia water is preferably 1:1.
The volume ratio of the copper tetraammine chloride aqueous solution to the 4-aminoantipyrine A is preferably 1:10
Shaking up and standing for 5 minutes in the step (2).
The total phenol detection reagent B and the water sample to be detected in the step (3) are preferably selected to be 1:1.
the invention has the following advantages:
compared with the prior art, the invention has the beneficial effects that:
the detection method disclosed by the invention is simple and rapid to operate, avoids using a strong oxidant or a toxic substance, and accords with the concept of green chemistry.
Detailed description of the invention
The present invention is described in detail below with reference to the following embodiments, and it should be understood that the embodiments described are only a part of the embodiments of the present invention, and it should not be understood that the present invention is limited to the following embodiments, and all the technologies implemented based on the present invention should be considered as the scope of the present invention.
Example 1
In the embodiment of the invention, a method for detecting the content of total phenols in water comprises the following steps:
preparing a copper chloride aqueous solution with the mass fraction of 10%. Taking 1 part of copper chloride aqueous solution and 2 parts of strong ammonia water with the mass fraction of 25-28% in parts by volume. Dropwise adding concentrated ammonia water into the water of copper chloride, and shaking up to obtain a clear copper tetraammine chloride aqueous solution A.
Preparing 2 percent of 4-aminoantipyrine aqueous solution by mass fraction. Taking 10 parts by volume of 4-aminoantipyrine, putting the 4-aminoantipyrine into a test tube, taking 1 part of solution A, adding the solution A into the test tube, shaking up, and standing for 10 minutes to serve as a total phenol detection reagent B.
And taking 1 parts of the detection reagent B by volume, adding 1 part of the water sample to be detected, mixing, standing for 10 minutes, detecting the change of absorbance at 540nm of the absorption spectrum, and calculating the content of the total phenols in the water. The results are shown in Table 1.
Example 2
In the embodiment of the invention, a method for detecting the content of total phenols in water comprises the following steps:
preparing a copper chloride aqueous solution with the mass fraction of 5%. Taking 1 part of copper chloride aqueous solution and 3 parts of strong ammonia water with the mass fraction of 25-28% in parts by volume. Dropwise adding concentrated ammonia water into the water of copper chloride, and shaking up to obtain a clear copper tetraammine chloride aqueous solution A.
Preparing 4-aminoantipyrine aqueous solution with the mass fraction of 4%. And (2) putting 5 parts of 4-aminoantipyrine into a test tube, taking 2 parts of the solution A, adding the solution A into the test tube, shaking uniformly, and standing for 5 minutes to serve as a total phenol detection reagent B.
And taking 2 parts of the detection reagent B by volume, adding 3 parts of the water sample to be detected, mixing, standing for 10 minutes, detecting the change of absorbance at 540nm of the absorption spectrum, and calculating the content of the total phenols in the water. The results are shown in Table 1.
Example 3
In the embodiment of the invention, a method for detecting the content of total phenols in water comprises the following steps:
preparing a copper chloride aqueous solution with the mass fraction of 3%. Taking 2 parts of copper chloride aqueous solution and 5 parts of strong ammonia water with the mass fraction of 25-28% in parts by volume. Dropwise adding concentrated ammonia water into the water of copper chloride, and shaking up to obtain a clear copper tetraammine chloride aqueous solution A.
Preparing 3 percent of 4-aminoantipyrine aqueous solution by mass fraction. And (3) putting 7 parts by volume of 4-aminoantipyrine into a test tube, adding 2 parts by volume of the solution A into the test tube, shaking uniformly, and standing for 15 minutes to serve as a total phenol detection reagent B.
And taking 1 parts of the detection reagent B by volume, adding 15 parts of the water sample to be detected, mixing, standing for 10 minutes, detecting the change of absorbance at 540nm of the absorption spectrum, and calculating the content of the total phenols in the water. The results are shown in Table 1.
Example 4
In the embodiment of the invention, a method for detecting the content of total phenols in water comprises the following steps:
preparing a copper chloride aqueous solution with the mass fraction of 10%. Taking 1 part of copper chloride aqueous solution and 2 parts of strong ammonia water with the mass fraction of 25-28% in parts by volume. Dropwise adding concentrated ammonia water into the water of copper chloride, and shaking up to obtain a clear copper tetraammine chloride aqueous solution A.
Preparing 2 percent of 4-aminoantipyrine aqueous solution by mass fraction. Taking 10 parts by volume of 4-aminoantipyrine, putting the 4-aminoantipyrine into a test tube, taking 1 part of solution A, adding the solution A into the test tube, shaking up, and standing for 10 minutes to serve as a total phenol detection reagent B.
And taking 1 parts of the detection reagent B by volume, adding 1 part of the water sample to be detected, mixing, standing for 10 minutes, detecting the change of absorbance at 540nm of the absorption spectrum, and calculating the content of the total phenols in the water. The results are shown in Table 1.
Example 5
In the embodiment of the invention, a method for detecting the content of total phenols in water comprises the following steps:
preparing a copper chloride aqueous solution with the mass fraction of 7%. Taking 3 parts of copper chloride aqueous solution and 5 parts of strong ammonia water with the mass fraction of 25-28% in parts by volume. Dropwise adding concentrated ammonia water into the water of copper chloride, and shaking up to obtain a clear copper tetraammine chloride aqueous solution A.
Preparing 6 percent of 4-aminoantipyrine aqueous solution by mass fraction. Taking 1 part of 4-aminoantipyrine by volume part, putting the 4-aminoantipyrine into a test tube, taking 1 part of the solution A, adding the solution A into the test tube, shaking up, and standing for 10 minutes to serve as a total phenol detection reagent B.
And taking 1 parts of the detection reagent B by volume, adding 10 parts of the water sample to be detected, mixing, standing for 10 minutes, detecting the change of absorbance at 540nm of the absorption spectrum, and calculating the content of the total phenols in the water. The results are shown in Table 1.
TABLE 1
As can be seen from the results in Table 1, the detection method of the invention has the advantages of small actual dosage, simple and rapid operation, and less than 10% of relative error compared with the national standard method.
Claims (4)
1. A method for detecting the content of total phenols in water is characterized by comprising the following steps:
(1) preparing a copper chloride aqueous solution with the mass fraction of 1-20%; dropwise adding concentrated ammonia water with the mass fraction of 25-28% into copper chloride water, wherein the volume ratio of copper chloride aqueous solution to concentrated ammonia water is 1: 1-5; shaking up to obtain a clear tetrammine copper chloride aqueous solution A;
(2) preparing 1-10% 4-aminoantipyrine aqueous solution by mass fraction; sequentially mixing a copper tetrammine chloride aqueous solution and 4-aminoantipyrine according to a volume ratio of 1:10 adding the mixture into a test tube, shaking uniformly, and standing for 5 minutes to serve as a total phenol detection reagent B;
(3) adding a total phenol detection reagent B into a water sample to be detected, wherein the volume ratio of the total phenol detection reagent B to the water sample to be detected is 1-5: 0.1-20, mixing and standing for 1-20 minutes, detecting the change of absorbance at 540nm of an absorption spectrum, and calculating the content of total phenols in water.
2. The method for detecting the total phenol content in water according to claim 1, wherein microwave ultrasonic or magneton stirring is used for uniform dispersion when preparing the copper chloride aqueous solution.
3. The method for detecting the content of total phenols in water according to claim 1, wherein: taking the volume ratio of the copper chloride aqueous solution to the concentrated ammonia water as 1:1.
4. the method for detecting the content of total phenols in water according to claim 1, wherein: and (3) mixing the total phenol detection reagent B and the water sample to be detected according to the volume ratio of 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611088428.1A CN108132221B (en) | 2016-12-01 | 2016-12-01 | Method for detecting total phenol content in water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611088428.1A CN108132221B (en) | 2016-12-01 | 2016-12-01 | Method for detecting total phenol content in water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108132221A CN108132221A (en) | 2018-06-08 |
| CN108132221B true CN108132221B (en) | 2020-09-04 |
Family
ID=62387957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611088428.1A Active CN108132221B (en) | 2016-12-01 | 2016-12-01 | Method for detecting total phenol content in water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108132221B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB774010A (en) * | 1953-10-16 | 1957-05-01 | Geigy Ag J R | Improvements relating to fluorescent stilbyl triazole compounds and to their use |
| CN101187637B (en) * | 2007-12-18 | 2010-05-19 | 四川大学 | Automatic analysis method for seawater phenols compounds |
| CN104345120A (en) * | 2014-03-10 | 2015-02-11 | 上海绿帝环保科技有限公司 | Detection reagent applied to detection of content of phenol in water |
-
2016
- 2016-12-01 CN CN201611088428.1A patent/CN108132221B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN108132221A (en) | 2018-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yuan et al. | Removal efficiency and possible pathway of odor compounds (2-methylisoborneol and geosmin) by ozonation | |
| Fecher et al. | Determination of iodine in food samples by inductively coupled plasma mass spectrometry after alkaline extraction | |
| Kazemzadeh et al. | Sequential flow injection spectrophotometric determination of nitrite and nitrate in various samples | |
| Monteiro et al. | Simplified version of the sodium salicylate method for analysis of nitrate in drinking waters | |
| US8133739B2 (en) | Reagent for measurement of concentration of lead, and method for measurement of concentration of lead | |
| Minamisawa et al. | Adsorption behavior of cobalt (II) on chitosan and its determination by tungsten metal furnace atomic absorption spectrometry | |
| Khalaf et al. | Spectrophotometric determination of phenol and resorcinol by reaction with p-aminophenol | |
| CA2829506C (en) | Method of determining a concentration of nitrate | |
| CN108132221B (en) | Method for detecting total phenol content in water | |
| CN103487432A (en) | Lead ion detection test paper, and preparation method and use method thereof | |
| Garrido et al. | Interference removal for cadmium determination in waste water and sewage sludge by flow injection cold vapour generation atomic absorption spectrometry | |
| CN104609636B (en) | A kind of method of utilizing ferrimanganic two-phase doped graphene to activate incretion interferent in single persulfate removal water | |
| CN105486671A (en) | Method for detecting mercury ions | |
| Ensafi et al. | Flow injection spectrophotometric determination of ultra trace amounts of oxalic acid | |
| Torró et al. | Flow-injection biamperometric determination of nitrate (by photoreduction) and nitrite with the NO− 2/I− reaction | |
| CN111537503B (en) | Sulfide analysis method and automatic analyzer | |
| Nemade et al. | Development and validation of UV spectrophotometric method for simultaneous estimation of nitrate and nitrite in water, soil, drug and vegetable samples | |
| Wang et al. | Determination of beryllium and selenium in human urine and of selenium in human serum by graphite-furnace atomic absorption spectrophotometry | |
| CN112697780B (en) | Mercury ion colorimetric detection method based on osmium nanoparticle oxidase activity | |
| Sun et al. | Flow injection analysis of tannic acid with inhibited electrochemiluminescent detection | |
| He et al. | Investigation on the interaction between dihydroxybenzene and Fe3+–H2O2–Rh6G system based on enhancing chemiluminescence | |
| Zhuang et al. | Determination of volatile phenols by a flow injection chemiluminescent quench method | |
| CN102451679A (en) | Nitric oxide oxidizing agent and its preparation method | |
| Naing | AMBIENT AMMONIA ANALYSIS VIA THE MODIFIED BERTHELOT’S REACTION | |
| Mohamed et al. | Sensitive determination of nitrite using its catalytic effect on the bromate oxidation of prochlorperazine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |