CN110470642A - A kind of fluorescent test paper and its detection method of quick detection formaldehyde in air - Google Patents

A kind of fluorescent test paper and its detection method of quick detection formaldehyde in air Download PDF

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Publication number
CN110470642A
CN110470642A CN201910842207.6A CN201910842207A CN110470642A CN 110470642 A CN110470642 A CN 110470642A CN 201910842207 A CN201910842207 A CN 201910842207A CN 110470642 A CN110470642 A CN 110470642A
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formaldehyde
test paper
fluorescent test
air
fluorescence
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郭明
靳秀一
马少敏
魏恒
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Dalian University
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Dalian University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6428Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N2021/6417Spectrofluorimetric devices

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  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Optics & Photonics (AREA)
  • Molecular Biology (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention relates to the fluorescent test papers and its detection method of a kind of quickly detection formaldehyde in air, belong to optical field.Formaldehyde fluorescent test paper of the present invention; it is using the filter paper of 4- amino -3- amylene -2- ketone (FP) infiltration as substrate; it is exposed to certain time in certain density formaldehyde; a kind of substance 3 with strong fluorescence is generated using 4- amino -3- amylene -2- ketone and formaldehyde effect; 5- diacetyl -1; 4- dihydronaphthalene (DDL) is detected, excitation wavelength 360nm, fluorescence emission wavelengths 498nm.The concentration of formaldehyde and its fluorescence signal at 498nm are in a linear relationship.The present invention is simple with preparation method, miniature portable, detection time is short, has higher detection sensitivity and accuracy, can be realized the detection of fast accurate, has good practical application value.

Description

A kind of fluorescent test paper and its detection method of quick detection formaldehyde in air
Technical field
The present invention relates to optical fields, and in particular to one kind quickly detects fluorescent test paper and its detection side of formaldehyde in air Method.
Background technique
Formaldehyde, also known as formaldehyde, are a kind of important Organic Ingredients, are a kind of gas of colourless irritant smell under room temperature Body is widely used in the industries such as impregnating fluid, weaving and timber since it is with the performances such as antisepsis and sterilization, wrinkle resistant, fire-retardant.In recent years Come, formaldehyde is classified as a kind of carcinogenic substance by international cancer research institution, the World Health Organization.Studies have shown that being chronically at containing excessive first In the environment of aldehyde, human skin mucous membrane, respiratory system etc. can be caused to seriously endanger, wherein due to using in newly-decorated room The materials such as wood based panel, paint, content of formaldehyde is higher, is the main inducing of many diseases, therefore the detection of formaldehyde in indoor air It is particularly important.
The method of detection formaldehyde mainly has gas chromatography, spectrophotometry etc. at present.Wherein gas chromatography operation is quasi- Really, high sensitivity, but due to needing large-scale gas chromatographicanalyzer device, operation is comparatively laborious, and to Operations Analyst personnel It is more demanding;And for classical analytical photometry, sensitivity is poor, and interference is more, and is difficult to realize quickly detect.So needing Develop a kind of highly sensitive, quick, easy and at low cost detection method.
Summary of the invention
The present invention provides the fluorescent test paper and its detection method of a kind of quickly detection formaldehyde in air, to impregnate the filter of FP Paper is substrate, the DDL with strong fluorescence is generated using the formaldehyde interaction in FP reagent and ambient enviroment, by measuring it The variation of fluorescence intensity achievees the purpose that detect content of formaldehyde.
Technical scheme is as follows: a kind of fluorescent test paper of quickly detection formaldehyde in air, with 4- amino -3- penta Alkene -2- ketone (FP) reagent infiltrates blank filter paper, is prepared.
The method for quickly detecting formaldehyde in air using the fluorescent test paper is claimed simultaneously in the present invention, and step is such as Under:
(1) it interacts: fluorescent test paper being placed in different concentration of formaldehyde under test gas environment and is interacted;
(2) fluorescence detection: using the fluorescence of fluorescent test paper under the conditions of Fluorescence Spectrometer determination step (1) different concentration of formaldehyde Spectrum;
(3) content of formaldehyde detects: fluorescent test paper being placed under test gas environment and is reacted, fluorescence light is then measured Spectrum, determines content of formaldehyde.
Further, the FP reagent is the FP solution for being 1% with the mass fraction that methanol dissolves;
Further, the blank filter paper is the common qualitative filter paper in laboratory;
Further, the blank filter paper specification is 10mm × 25mm;
Further, the fluorescent test paper that detection formaldehyde is made is the filter paper infiltrated with 100 μ L FP reagents, and Dry 5min at 60 DEG C;
Further, described that test paper is placed in the various concentration formaldehyde environment lower time as 10min;
It further, is measurement FP reagent using the fluorescence spectrum of Fluorescence Spectrometer measurement filter paper in the step (2) 3,5- diacetyl-DHN 1,4 dihydronaphthalene (DDL) fluorescence spectrum variation generated with formaldehyde reaction;
Further, the DDL, molecular formula are as follows: C11H15NO2;Generate its reaction structure formula are as follows:
Further, the fluorescence spectrum using Fluorescence Spectrometer detection DDL changes, excitation wavelength 360nm, With the raising of concentration of formaldehyde, the fluorescence spectrum at 498nm is gradually increased;
Further, the formaldehyde in the detection air is with air sampler with the traffic sampling 10L of 0.5L/min It is measured.
4- amino -3- amylene -2- ketone (FP) reagent can be reacted with formaldehyde (FA), and generating has the 3 of strong fluorescence, 5- diacetyl-Isosorbide-5-Nitrae-dihydronaphthalene (DDL) can measure the variation of its fluorescence signal by Fluorescence Spectrometer, and fluorescence intensity is with first Aldehyde concentration increases and reinforces, it is possible thereby to quantitative determine content of formaldehyde.Since fluorescence spectrum has specific excitation spectrum and spy Fixed emission spectrum, therefore fluorescence spectrum has preferable selectivity, can eliminate the interference of other materials.
Beneficial effects of the present invention are as follows: using the filter paper being easy to get as detection substrate, utilizing the phase of FP reagent and formaldehyde Interaction generates, and there is the substance of strong fluorescence to detect signal as fluorescence spectrum, and the formaldehyde fluorescent test paper preparation method is simple, Small and exquisite portable, easy to use, detection speed is fast, has good detection sensitivity and accuracy, the formaldehyde that can be detected Cmin is 1.78 × 10-3mg/m3, it is lower than GB/T18883-2002 Indoor Air Quality standards.But also sky may be implemented The measurement of content of formaldehyde in gas provides a kind of reliable method for the formaldehyde in detection air, has good practical application Value.
Detailed description of the invention
Fig. 1 is the fluorescent test paper and the folder of the fluorescent test paper made of polyethylene plastic film of detection formaldehyde prepared by the present invention;
Fig. 2 is the gas collecting device figure for detecting formaldehyde;
Fig. 3 is Fluorescence Spectrometer Test paper schematic diagram, and the angle of test paper and incident light is 45 degree;
Fig. 4 is fluorescence spectra (E of test paper under the conditions of various concentration formaldehydex=360nm);
Fig. 5 is the standard curve of fluorescence intensity change at 498nm.
Wherein: 1, fluorescent test paper, 2, PCV film, 3, window, 4, air inlet, 5, gas outlet, 6, detector, 7, light source, 8, stone English cuvette.
Specific embodiment
Further description of the technical solution of the present invention combined with specific embodiments below, but the present invention is not with any shape Formula is limited to embodiment content.
Test method described in embodiment is conventional method unless otherwise specified;Unless otherwise specified, the reagent and Biomaterial commercially obtains.
The preparation of 1 fluorescent test paper of embodiment
(1) weighing 0.1g 4- amino -3- amylene -2- ketone (FP) and being dissolved in 10mL methanol to get mass fraction is 1% FP reagent, shake up stand-by;
(2) blank filter paper for taking 10mm × 25mm, the FP reagent for taking 100 μ L to prepare drip on filter paper, are subsequently placed in 60 Dry 5min, the fluorescent test paper prepared are fixed in clamper made of polyethylene film in DEG C drying box, as shown in Figure 1;
(3) dried filter paper is respectively placed in the flow of 0.5L/min, the concentration that volume is 10L is 0mg/m3, 0.03mg/m3, 0.04mg/m3, 0.06mg/m3, 0.08mg/m3, 0.1mg/m310min in the obturator of different concentration of formaldehyde, As shown in Fig. 2, FP reagent is made sufficiently to interact with formaldehyde gas.
Embodiment 2 draws standard curve
Continuous mode is as shown in figure 3, setting fluorescence spectrum excitation wavelength Ex=360nm, the fluorescence spectrum for measuring filter paper become Change, measurement result is shown in Fig. 4.As seen from the figure, with the increase of concentration of formaldehyde, the photoluminescence spectrum intensity at 498nm is gradually increased, It and is in good gradient relation.In order to which the relationship of different concentration of formaldehyde and fluorescence intensity is better described, by concentration of formaldehyde Linear fit is carried out with fluorescence intensity, as shown in Figure 5.It can be seen that concentration of formaldehyde is in 0.03mg/m3~0.1mg/m3Model In enclosing and its fluorescence intensity is in good linear relationship, linearly dependent coefficient r=0.9982, equation of linear regression are as follows: y= 525576.42x+11795.30 (x, mg/m3).11 replications are carried out to blank value, be calculated detection be limited to 1.78 × 10-3mg/m3
The measurement of 3 formaldehyde in air content of embodiment
It uses air sampler using the flow collection room air 10L of 0.5L/min as under test gas, then uses FP reagent Filter paper and drying are infiltrated, 10min in the gaseous environment is placed in, measures its fluorescence spectrum with step described in embodiment 2, according to The calibration curve equation measured calculates, and obtaining surveyed formaldehyde in air content is 0.03mg/m3

Claims (10)

1. a kind of fluorescent test paper of quickly detection formaldehyde in air, which is characterized in that soaked with 4- amino -3- amylene -2- ketone reagent Moisten blank filter paper, is prepared.
2. a kind of method for quickly detecting formaldehyde in air using fluorescent test paper described in claim 1, which is characterized in that step It is as follows:
(1) it interacts: fluorescent test paper being placed in different concentration of formaldehyde under test gas environment and is interacted;
(2) fluorescence detection: using the fluorescence light of fluorescent test paper under the conditions of Fluorescence Spectrometer determination step (1) different concentration of formaldehyde Spectrum;
(3) content of formaldehyde detects: fluorescent test paper being placed under test gas environment and is reacted, then measures fluorescence spectrum, really Determine content of formaldehyde.
3. fluorescent test paper as described in claim 1, which is characterized in that the 4- amino -3- amylene -2- ketone reagent is The methanol solution of the 4- amino -3- amylene -2- ketone of 1wt%.
4. fluorescent test paper as described in claim 1, which is characterized in that the blank filter paper is fixed on polyethylene film system At clamper in.
5. fluorescent test paper as described in claim 1, which is characterized in that 100 μ L 4- amino -3- penta of the blank filter paper The infiltration of alkene -2- ketone reagent, and the dry 5min at 60 DEG C.
6. the method that fluorescent test paper as claimed in claim 2 quickly detects formaldehyde in air, which is characterized in that the step (1) fluorescent test paper is placed under various concentration formaldehyde environment, with the flow velocity of 0.5L/min by gaseous sample 10L, stablizes the time It for 10min, is then measured, an air inlet and a gas outlet is arranged in sampler.
7. the method that fluorescent test paper as claimed in claim 2 quickly detects formaldehyde in air, which is characterized in that the step (2) using the fluorescence spectrum of Fluorescence Spectrometer measurement fluorescent test paper in, refer to measurement 4- amino -3- amylene -2- ketone reagent and first 3,5- diacetyl-DHN 1,4 dihydronaphthalene fluorescence spectrum variation that aldehyde reaction generates.
8. the method that fluorescent test paper as claimed in claim 7 quickly detects formaldehyde in air, which is characterized in that described 3,5- Diacetyl-Isosorbide-5-Nitrae-dihydronaphthalene excitation wavelength is 360nm, and with the raising of concentration of formaldehyde, the fluorescence spectrum at 498nm is gradually Enhancing.
9. the folder of the method that fluorescent test paper as claimed in claim 7 quickly detects formaldehyde in air, fluorescent test paper and incident light Angle is 45 degree.
10. the method that fluorescent test paper as claimed in claim 2 quickly detects formaldehyde in air, which is characterized in that the step Suddenly under test gas is to be obtained with air sampler with the flow velocity acquisition room air 10L of 0.5L/min in (3).
CN201910842207.6A 2019-09-06 2019-09-06 A kind of fluorescent test paper and its detection method of quick detection formaldehyde in air Pending CN110470642A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101535798A (en) * 2006-09-27 2009-09-16 独立行政法人产业技术综合研究所 Formaldehyde detecting material, formaldehyde detector, formaldehyde detecting method and formaldehyde detecting reagent
CN102978912A (en) * 2012-11-19 2013-03-20 东华大学 Preparation method of nanofiber membrane formaldehyde test paper
CN104897659A (en) * 2014-03-06 2015-09-09 苏州工业园区新国大研究院 Formaldehyde gas concentration detection method
CN106457240A (en) * 2014-01-14 2017-02-22 国家科学研究中心 Microfluidic device for analysis of flowing pollutants
CN108132242A (en) * 2016-12-01 2018-06-08 中国科学院大连化学物理研究所 A kind of preparation method and applications of formaldehyde gas on-line quick detection sensor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101535798A (en) * 2006-09-27 2009-09-16 独立行政法人产业技术综合研究所 Formaldehyde detecting material, formaldehyde detector, formaldehyde detecting method and formaldehyde detecting reagent
CN102978912A (en) * 2012-11-19 2013-03-20 东华大学 Preparation method of nanofiber membrane formaldehyde test paper
CN106457240A (en) * 2014-01-14 2017-02-22 国家科学研究中心 Microfluidic device for analysis of flowing pollutants
CN104897659A (en) * 2014-03-06 2015-09-09 苏州工业园区新国大研究院 Formaldehyde gas concentration detection method
CN108132242A (en) * 2016-12-01 2018-06-08 中国科学院大连化学物理研究所 A kind of preparation method and applications of formaldehyde gas on-line quick detection sensor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
M.N.DESCAMPS 等: "Real-time detection of formaldehyde by a sensor", 《SENSORS AND ACTUATORS B: CHEMICAL》 *
YOSHIO SUZUKI 等: "Portable Sick House Syndrome Gas Monitoring System Based on Novel Colorimetric Reagents for the Highly Selective and Sensitive Detection of Formaldehyde", 《ENVIRON.SCI.TECHNOL.》 *

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Application publication date: 20191119