CN107255628B - Formaldehyde detection reagent - Google Patents

Formaldehyde detection reagent Download PDF

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CN107255628B
CN107255628B CN201710438237.1A CN201710438237A CN107255628B CN 107255628 B CN107255628 B CN 107255628B CN 201710438237 A CN201710438237 A CN 201710438237A CN 107255628 B CN107255628 B CN 107255628B
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formaldehyde
detection reagent
color
mmol
metal ions
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CN107255628A (en
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张友玉
卢求钧
邓璐
李海涛
刘美玲
吴萃艳
姚守拙
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Hunan Normal University
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    • G—PHYSICS
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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    • G01—MEASURING; TESTING
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    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
    • 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
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract

The invention belongs to the technical field of formaldehyde content determination, and relates to a formaldehyde content detection reagent and a detection method thereof. The detection reagent preferably consists of an acidic solution, a color-developing agent and metal ions. The using method comprises the following steps: collecting gas to be detected, introducing the gas to be detected into an acidic solution, adding a color developing agent and metal ions, and uniformly mixing; after standing at room temperature for 20 minutes, the detection reagent was observed for color and fluorescence change. The formaldehyde detection reagent has the advantages of simple detection method, high speed, visual detection result, double detection signals and the like, and is easy to popularize.

Description

Formaldehyde detection reagent
Technical Field
The invention belongs to the technical field of formaldehyde content determination, and relates to a formaldehyde detection reagent.
Background
Formaldehyde is a colorless gas with a special pungent smell and is also an important basic organic chemical raw material. The formaldehyde molecule contains aldehyde group, and can be subjected to polycondensation reaction with phenol and the like to obtain the phenolic resin which is widely applied to various household materials such as paints, coatings, adhesives, plywood, shaving boards, pressed wood products and the like. However, over time, formaldehyde is slowly released therefrom, which can be as long as ten years, and results in the formaldehyde content in the indoor air exceeding a certain threshold.
Formaldehyde presents numerous hazards to human health, and exposure to formaldehyde poses many potential health risks, such as: the formaldehyde has stimulation effect on eyes and nose, and is easy to cause fatigue, headache, cough and the like; formaldehyde can cause upper respiratory tract infection and may cause central nervous system infectionNervous system injury and immune system disease; the long-term exposure to formaldehyde can also cause problems of chromosome abnormality, leukemia, pregnancy syndrome, hypomnesis, mental retardation and the like of the newborn. Based on this, the world health organization and the national institute of occupational safety and health of the United states set 0.08mg/m for formaldehyde respectively3And 0.10mg/m3Safe contact limit of (1). GB 50325-3. Therefore, the method is very important for detecting the formaldehyde in the environment so as to prevent the harm caused by the excessive formaldehyde in the environment.
So far, various formaldehyde detection methods have been developed, wherein the national standard detection methods in China include: phenol reagent spectrophotometry (GB/T16057-1995), 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazacyclopenta (AHMT) spectrophotometry (GB/T16129-1995), and acetylacetone spectrophotometry (HJ 601-2011). Among them, the phenol reagent method and the AHMT method have the problem of selectivity, and the acetylacetone method has the problem of difficulty in storing the reagents. Patent ZL201410500026.2 discloses a formaldehyde rapid detection reagent. The chemical name of the reagent is 2-amido-3- (3-amido-1H-benzo [ d ] imidazole) -pyridine, but the reagent is prepared by three steps of organic reactions and has the defects of complex process and time consumption. Patent ZL201410763297.7 discloses an ethoxyamine hydrochloride used for formaldehyde content detection and a determination method thereof. The method comprises the steps of reacting formaldehyde with ethoxy amine hydrochloride to generate ethoxy formaldehyde oxime, then carrying out high performance liquid chromatography analysis at the wavelength of 205nm, and calculating by a standard curve method to obtain a formaldehyde content value. However, this method has some limitations, such as the need for precise instruments, the need for professional operation, and long detection period, which are not suitable for rapid detection in the field.
It would therefore be of great interest to develop a new reagent and to be able to carry out an on-site, rapid and efficient determination of formaldehyde.
Disclosure of Invention
In view of the defects of the detection reagent, the invention aims to provide a novel reagent for detecting formaldehyde, thereby realizing the on-site, rapid and effective determination of the formaldehyde.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the formaldehyde detection reagent comprises the following specific formula and proportion:
1 ml-10 ml of acid solution
Developer 1 millimole-100 millimole
0.1 mmol-5 mmol of metal ions;
the acid solution is citric acid-citrate buffer solution or acetic acid-acetate buffer solution;
the color developing agent is o-phenylenediamine, 3',5,5' -tetramethyl benzidine or 2, 2-dinitro-bis (3-ethyl-benzene)
Thiazole-6-sulfonic acid) diammonium salt;
the metal ions are silver ions, iron ions or copper ions.
In a preferred scheme, the formaldehyde detection reagent comprises the following specific formula ratio:
2 ml-8 ml of acid solution
5-50 mmol of color developing agent
The mass of the metal ions is 0.2 mmol-5 mmol.
In a further preferred scheme, the formaldehyde detection reagent comprises the following specific formula ratio:
acid solution 5 ml
Developer 5 millimole
Metal ions 0.5 mmol.
The acidic solution is preferably a citric acid-citrate buffer.
The developer is preferably o-phenylenediamine.
The metal ion is preferably a silver ion.
And mixing the raw materials according to a ratio, and uniformly stirring to obtain the formaldehyde detection reagent.
The detection method using the detection reagent comprises the following steps:
(1) collecting gas to be detected;
(2) introducing gas to be detected into an acidic solution, adding a color developing agent and metal ions, and uniformly mixing;
(3) standing for 20 minutes at room temperature, observing the color change of the detection reagent under natural light, and if the color is light yellow or colorless, proving that the concentration of formaldehyde in the gas to be detected is higher than 0.1mg/m3(ii) a Or observing the fluorescence intensity under an ultraviolet lamp with the wavelength of 365 nm, and if the fluorescence is light yellow or the fluorescence cannot be observed, proving that the concentration of formaldehyde in the gas to be detected is higher than 0.1mg/m3。
The invention is further explained and illustrated below
The principle of the invention is based on: the silver ions can oxidize o-phenylenediamine into 2, 3-diaminophenazine, the color of the o-phenylenediamine is changed from colorless to bright yellow correspondingly, and obvious yellow fluorescence appears under the illumination of an ultraviolet lamp with the wavelength of 356 nanometers. If formaldehyde exists in the system, the formaldehyde can react with o-phenylenediamine to consume the o-phenylenediamine, so that the yellow becomes light until fading, and the fluorescence intensity is weakened until no fluorescence exists.
When the formaldehyde reagent does not exist, the color of the detection reagent under natural light is bright yellow; when 20 micromoles per liter of formaldehyde exists in the formaldehyde reagent, the color of the detection reagent is basically colorless under natural light.
When the formaldehyde reagent does not exist, the detection reagent has obvious yellow fluorescence under an ultraviolet lamp; the formaldehyde reagent of the present invention exhibits substantially no fluorescence under an ultraviolet lamp having a wavelength of 356 nanometers in the presence of 20 micromoles per liter of formaldehyde.
If the accurate value of the formaldehyde concentration is to be obtained, the corresponding absorption peak or fluorescence peak intensity can be measured on an ultraviolet-visible spectrophotometer and a fluorescence spectrometer, and the accurate value of the formaldehyde concentration can be obtained by comparing with a standard curve.
Compared with the existing formaldehyde detection reagent, the invention has the innovation points that:
1. the formaldehyde detection reagent has high detection speed, and can finish formaldehyde detection within 20 minutes.
2. The detection result is visual, and the kit has double signals of color comparison and fluorescence, and can reduce detection errors caused by other interferences.
3. The formaldehyde detection reagent disclosed by the invention is low in manufacturing cost and easy for industrial production.
4. The formaldehyde detection reagent has simple and easy use method, does not need precise instruments, can be used by ordinary people for completing detection, and is easy to popularize.
Drawings
FIG. 1 is a UV-Vis spectrum of the formaldehyde reagent of the present invention in the absence of formaldehyde, and it can be seen from FIG. 1 that the detection reagent has a strong UV absorption peak at 446 nm in the absence of formaldehyde.
FIG. 2 is a fluorescence spectrum of the formaldehyde reagent of the present invention in the absence of formaldehyde, and it can be seen from FIG. 2 that the detection reagent has a strong fluorescence emission peak at 566 nm in the absence of formaldehyde.
FIG. 3 is a UV-Vis spectrum of the formaldehyde reagent of the present invention in the presence of 20. mu. mol/L formaldehyde, and it can be seen from FIG. 3 that the UV absorption peak at 446 nm of the detection reagent is significantly reduced in the presence of 20. mu. mol/L formaldehyde.
FIG. 4 is a fluorescence spectrum of the formaldehyde reagent of the present invention in the presence of 20. mu.mol/L formaldehyde, and it can be seen from FIG. 4 that the fluorescence emission peak of the detection reagent at 566 nm is significantly reduced in the presence of 20. mu.mol/L formaldehyde.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Introducing air to be detected into 5 ml of citric acid-sodium citrate buffer solution, adding 5 mmol of o-phenylenediamine and 0.5 mmol of silver ions, uniformly mixing, standing at room temperature for 20 minutes, and observing color and fluorescence changes to judge whether the concentration of formaldehyde is higher than 0.1mg/m3。
Example 2
To 10 ml of citric acid-sodium citrate buffer, air to be measured was introduced, and 20 mmol of o-phenylenediamine was added5 millimoles of silver ions, uniformly mixing, standing at room temperature for 30 minutes, and observing color and fluorescence changes to judge whether the concentration of formaldehyde is higher than 0.1mg/m3。
Example 3
Introducing air to be detected into 1 ml of citric acid-sodium citrate buffer solution, adding 1 mmol of o-phenylenediamine and 0.1 mmol of silver ions, uniformly mixing, standing at room temperature for 20 minutes, and observing color and fluorescence changes to judge whether the concentration of formaldehyde is higher than 0.1mg/m3。
Example 4
Introducing air to be detected into 8 ml of citric acid-sodium citrate buffer solution, adding 10 mmol of o-phenylenediamine and 1 mmol of silver ions, uniformly mixing, standing at room temperature for 20 minutes, and observing color and fluorescence changes to judge whether the concentration of formaldehyde is higher than 0.1mg/m3。
Verification experiment
The formaldehyde detection reagent provided by the invention is used for detecting 5 groups of air samples to be detected so as to judge whether the concentration of formaldehyde in the air samples to be detected is higher than 0.1mg/m3Meanwhile, the accuracy and reliability of the method are judged by a commercially available indoor air quality detector, and specific experimental results are shown in Table 1
TABLE 1 test results of examples 1-4
Figure BDA0001319085330000051
The verification experiment result shows that the detection result of the formaldehyde detection reagent is reliable.
Embodiments of the present invention are illustrated by way of example only, and the invention is not limited to the specific details and illustrations shown and described herein.

Claims (3)

1. The formaldehyde detection reagent is characterized by comprising the following specific formula:
1 ml-10 ml of acid solution
Developer 1 millimole-100 millimole
0.1 mmol-5 mmol of metal ions;
the acidic solution is a citric acid-citrate buffer solution;
the color developing agent is o-phenylenediamine;
the metal ions are silver ions;
the detection method using the detection reagent comprises the following steps:
(1) collecting gas to be detected;
(2) introducing gas to be detected into an acidic solution, adding a color developing agent and metal ions, and uniformly mixing;
(3) standing for 20 minutes at room temperature, observing the color change of the detection reagent under natural light, and if the color is light yellow or colorless, proving that the concentration of formaldehyde in the gas to be detected is higher than 0.1mg/m3(ii) a Or observing the fluorescence intensity under an ultraviolet lamp with the wavelength of 365 nm, and if the fluorescence is light yellow or the fluorescence cannot be observed, proving that the concentration of formaldehyde in the gas to be detected is higher than 0.1mg/m3。
2. The formaldehyde detection reagent according to claim 1, wherein the formaldehyde detection reagent comprises the following specific formula:
2 ml-8 ml of acid solution
5-50 millimoles of color-developing agent
Metal ions 0.2 mmol to 5 mmol.
3. The formaldehyde detection reagent according to claim 2, wherein the formaldehyde detection reagent comprises the following specific formula:
acid solution 5 ml
Developer 5 millimole
Metal ions 0.5 mmol.
CN201710438237.1A 2017-06-12 2017-06-12 Formaldehyde detection reagent Active CN107255628B (en)

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CN108444962B (en) * 2018-03-05 2021-01-12 北京化工大学 Perylene-based formaldehyde colorimetric probe and formaldehyde fluorescent test paper, and preparation method and use method thereof
CN108760705A (en) * 2018-06-05 2018-11-06 华侨大学 The fluorescence analysis method of benzoyl peroxide in a kind of detection flour
CN111686699B (en) * 2019-03-13 2022-10-14 宁波方太厨具有限公司 Formaldehyde adsorption material and preparation method thereof
CN110940654B (en) * 2019-12-30 2022-02-01 杭州柘大飞秒检测技术有限公司 Detection method of citral

Citations (2)

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Publication number Priority date Publication date Assignee Title
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CN106243098A (en) * 2016-04-06 2016-12-21 新疆大学 One class condensed hetero ring al thiosemicarbazides fluorescent quenching type mercury ion probe

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104181154A (en) * 2014-06-26 2014-12-03 郑州大学 Formaldehyde detection agent and method
CN106243098A (en) * 2016-04-06 2016-12-21 新疆大学 One class condensed hetero ring al thiosemicarbazides fluorescent quenching type mercury ion probe

Non-Patent Citations (3)

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Title
Cu(I)-MOF: naked-eye colorimetric sensor for humidity and formaldehyde in single-crystal-to-single-crystal fashion;Yang Yu,et.al;《Chem. Commun.》;20141231;第50卷;第1445页右栏-第1446页右栏，图3-图5 *
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LÉGRÁDI LÁSZLÓ.Kis mennyiségűformaldehid és formaldehid-dimetilacetál egymás melletti kimutatása.《Magyar Kémiai Folyóirat》.1963,第69卷 *

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