CN112255053A - Device for in-situ monitoring of formaldehyde release of customized furniture and application method - Google Patents

Device for in-situ monitoring of formaldehyde release of customized furniture and application method Download PDF

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CN112255053A
CN112255053A CN202011050744.6A CN202011050744A CN112255053A CN 112255053 A CN112255053 A CN 112255053A CN 202011050744 A CN202011050744 A CN 202011050744A CN 112255053 A CN112255053 A CN 112255053A
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formaldehyde
furniture
vacuum chuck
derivatization reagent
detected
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陈正毅
袁锟婷
李静丹
赵豪
黄雪梅
李丰玲
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Guilin Medical University
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Guilin Medical University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • G01N2001/2217—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption using a liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/067—Preparation by reaction, e.g. derivatising the sample

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Abstract

The invention discloses a device for monitoring formaldehyde release of customized furniture in situ and an application method thereof, wherein the device comprises a sample cell, a vacuum chuck and a separation membrane; a liquid storage cavity is arranged in the sample pool and used for loading a derivatization reagent for absorbing formaldehyde; the vacuum chuck is provided with an adsorption end and a conduction end, the adsorption end and the conduction end are communicated with each other, the adsorption end is used for adsorbing an object to be detected, the conduction end is detachably and hermetically connected with the sample cell, and the conduction end is communicated with the liquid storage cavity; the separation membrane is isolated between the conduction end and the liquid storage cavity and is used for allowing formaldehyde to enter the liquid storage cavity and isolating a derivatization reagent from flowing out of the liquid storage cavity; therefore, in the application process, the formaldehyde can be collected and detected only by adsorbing the vacuum sucker on the surface of the furniture to be detected, the furniture cannot be damaged, and the dilemma existing in the prior art is really solved.

Description

Device for in-situ monitoring of formaldehyde release of customized furniture and application method
Technical Field
The invention relates to the field of formaldehyde detection, in particular to a device for in-situ monitoring of formaldehyde release of customized furniture and an application method.
Background
With the rapid development of the customized furniture and building market, the quality control and inspection of toxic and harmful substances in furniture and decorative materials play an important role in building construction, scientific research and technical development. The method is not only a foundation and a necessary means for evaluating and controlling the quality of the building material, but also an important component for saving raw materials, developing building science and technology and ensuring engineering quality, and is an important link for monitoring the quality of the building material. However, the current sampling and detecting technology for formaldehyde in customized furniture and decoration materials still has defects, and the related standards are not perfect, so the main reasons for the situation are as follows:
1. the sample collection and detection lack traceability and cannot reflect timeliness. The formaldehyde release of wooden furniture is accumulative, long-term and diverse. The traditional indoor air sampling detection evaluation method (JGJ/T436-.
2. In the current regulations of indoor environmental pollution control specifications (2013 version) of GB 50325 and 2010 civil building engineering and physicochemical performance test methods of GB/T17657 and 2013 artificial boards for decorative surfaces, formaldehyde in furniture is collected mainly by a perforation method, a dryer method and a test cabin method, and the three methods, namely an ex-situ sampling method, are destructive to the furniture.
In order to solve the problems, a technical scheme which can be attached to formaldehyde release detection of furniture is urgently needed.
Disclosure of Invention
The invention aims to provide a device for monitoring formaldehyde release of customized furniture in situ and an application method thereof, so as to solve the problem that the existing furniture formaldehyde release detection scheme can damage the furniture.
In order to solve the technical problem, the invention provides a device for in-situ monitoring of formaldehyde release of customized furniture, which comprises a sample cell, a vacuum chuck and a separation membrane; a liquid storage cavity is arranged in the sample pool and used for loading a derivatization reagent for absorbing formaldehyde; the vacuum chuck is provided with an adsorption end and a conduction end, the adsorption end and the conduction end are communicated with each other, the adsorption end is used for adsorbing an object to be detected, the conduction end is detachably and hermetically connected with the sample cell, and the conduction end is communicated with the liquid storage cavity; the separation membrane separation in the conduction end with between the stock solution chamber, the separation membrane is used for supplying formaldehyde to enter into in the stock solution chamber, and the separation derivatization reagent flows out the stock solution chamber.
In one embodiment, the inner wall of the port of the sample cell is provided with internal threads, and the outer part of the conduction end is provided with external threads; the device further comprises an adapter and a nut, wherein two ends of the adapter are communicated, external threads are arranged on the outer walls of the two ends of the adapter, one end of the adapter is in threaded connection with the inner wall of the port of the sample cell, the other end of the adapter is in threaded connection with the nut, and the nut is further in threaded connection with the outer wall of the conducting end; the separation membrane is blocked between the adaptor and the liquid storage cavity.
In one embodiment, the external threads on both ends of the adaptor are reverse threads.
In one embodiment, the adaptor and the sample cell are transparent.
In one embodiment, the vacuum chuck is a telescoping chuck.
In one embodiment, the separation membrane is a water-proof, gas-permeable membrane.
In one embodiment, the separation membrane is a lofty polytetrafluoroethylene membrane.
In order to solve the technical problem, the invention also provides an application method of the device for in-situ monitoring of formaldehyde release of the customized furniture, which is used for testing and comprises the following steps,
step S1, loading the derivatization reagent into the liquid storage cavity, and hermetically connecting the sample cell with the vacuum chuck, wherein the derivatization reagent contains acetylacetone;
s2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, and detecting the derivatization reagent by using an ultraviolet spectrophotometer to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
In order to solve the technical problem, the invention also provides an application method of the device for in-situ monitoring of formaldehyde release of the customized furniture, which is used for testing and comprises the following steps,
step S1, putting the derivatization reagent into the liquid storage cavity, and hermetically connecting the sample cell with the vacuum chuck, wherein the derivatization reagent contains 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazocene;
step S2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, adding a potassium periodate solution, placing, and detecting the derivatization reagent by using an ultraviolet spectrophotometer after placing to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
In order to solve the technical problem, the invention also provides an application method of the device for in-situ monitoring of formaldehyde release of the customized furniture, which is used for testing and comprises the following steps,
step S1, the derivatization reagent is filled in the liquid storage cavity, the sample pool is hermetically connected with the vacuum chuck, and the derivatization reagent contains 2, 4-dinitrophenylhydrazine acetonitrile;
step S2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, heating the derivatization reagent at a preset temperature for a preset time, and detecting by using a high performance liquid chromatograph to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
The invention has the following beneficial effects:
because the absorption end is used for adsorbing with the determinand, the separation membrane separation in the conduction end with between the stock solution chamber, the separation membrane is used for supplying formaldehyde to enter into stock solution intracavity and separation derivatization reagent flows the stock solution chamber, so in carrying out the application, only need with vacuum chuck absorption in the furniture surface that awaits measuring, then can realize the collection of formaldehyde and detect, can not cause the damage to furniture to the dilemma that prior art exists has been solved conscientiously.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view, partly in section, of a first embodiment of the apparatus according to the invention;
FIG. 2 is a schematic disassembled view of FIG. 1;
FIG. 3 is a schematic view, partly in section, of a second embodiment of the apparatus according to the invention;
FIG. 4 is a schematic illustration of the disassembled structure of FIG. 3;
FIG. 5 is a UV-Vis spectrum and a formaldehyde standard curve of the formaldehyde emission content of furniture according to the first embodiment of the application method of the present invention;
FIG. 6 is a UV-Vis spectrum and a formaldehyde standard curve of the formaldehyde emission content of furniture according to a second embodiment of the method for applying the present invention;
FIG. 7 shows a chromatogram of the formaldehyde emission content of furniture and a standard curve of formaldehyde according to a second embodiment of the method of applying the present invention.
The reference numbers are as follows:
10. a sample cell; 11. a liquid storage cavity;
20. a vacuum chuck; 21. an adsorption end; 22. a conductive end;
30. a separation membrane;
40. an adapter;
50. and a nut.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
The present invention provides a device for in situ monitoring of formaldehyde emission from a custom-made furniture, a first embodiment of which is shown in fig. 1 and 2 and comprises a sample cell 10, a vacuum chuck 20 and a separation membrane 30; a liquid storage cavity 11 is arranged in the sample cell 10, and the liquid storage cavity 11 is used for loading a derivatization reagent for absorbing formaldehyde; the vacuum chuck 20 is provided with an adsorption end 21 and a conduction end 22, the adsorption end 21 and the conduction end 22 are communicated with each other, the adsorption end 21 is used for adsorbing an object to be detected, the conduction end 22 is detachably and hermetically connected with the sample cell 10, and the conduction end 22 is communicated with the liquid storage cavity 11; the separation membrane 30 is separated between the conduction end 22 and the liquid storage cavity 11, and the separation membrane 30 is used for allowing formaldehyde to enter the liquid storage cavity 11 and separating derivatization reagents from flowing out of the liquid storage cavity 11.
When in application, the sample cell 10 and the vacuum chuck 20 are disassembled, and then a derivatization reagent can be filled in the liquid storage cavity 11 of the sample cell 10; after the derivatization reagent is loaded, the separation membrane 30 is utilized to cover the liquid storage cavity 11, and after the sample cell 10 is hermetically connected with the vacuum sucker 20, the vacuum sucker 20 can be adsorbed on the surface of the furniture to be tested, so that the subsequent formaldehyde release amount detection can be carried out, the whole process cannot damage the furniture, the operation is simple and convenient, and the dilemma existing in the prior art is practically solved.
It should be noted that, in the illustrated orientation, the inner wall of the lower port of the sample cell 10 of this embodiment is provided with external threads, and the outer wall of the conducting end 22 is provided with external threads, so that the sample cell 10 and the conducting end 22 can be connected in a sealing manner by screwing the lower port of the sample cell 10 and the conducting end 22.
In addition, this embodiment is for improving vacuum chuck 20's adsorption affinity, and the preferred vacuum chuck 20 that sets up is telescopic sucking disc, and vacuum chuck 20's structure is similar with the flexible pipe that has the fold this moment, places vacuum chuck 20 behind the furniture surface that awaits measuring, only needs to press vacuum chuck 20, alright realize vacuum chuck 20 to the rapid absorption of the furniture that awaits measuring, and the simple operation has optimized the use greatly and has experienced.
A second embodiment of the device is shown in fig. 3 and 4, which is substantially identical to the first embodiment of the device except that the inner wall of the port of the sample cell 10 is provided with internal threads and the exterior of the conducting end 22 is provided with external threads; the device further comprises an adapter 40 and a nut 50, wherein two ends of the adapter 40 are communicated, external threads are arranged on the outer walls of two ends of the adapter 40, one end of the adapter 40 is in threaded connection with the inner wall of the port of the sample cell 10, the other end of the adapter 40 is in threaded connection with the nut 50, and the nut 50 is also in threaded connection with the outer wall of the conducting end 22; the separation membrane 30 is blocked between the adaptor 40 and the liquid storage cavity 11.
Therefore, during assembly, the liquid storage cavity 11 is covered by the separation membrane 30, then the upper end of the adapter 40 is in threaded connection with the inner wall of the port of the sample cell 10, the lower end of the adapter 40 is in threaded connection with the nut 50, and the nut 50 is in threaded connection with the conduction end 22; since the mechanical strength of the adaptor 40 and the nut 50 is higher than that of the vacuum chuck 20, the sealing connection stability between the sample cell 10 and the vacuum chuck 20 can be enhanced by adding the adaptor 40 and the nut 50.
In this embodiment, it is also preferable that the external threads of both ends of the adaptor 40 are reverse threads for the convenience of assembly, for example, if the upper end of the adaptor 40 is screwed with the sample cell 10 by clockwise rotation, the lower end of the adaptor 40 is screwed with the nut 50 by counterclockwise rotation, thereby facilitating the assembly and disassembly of the device.
Furthermore, in order to facilitate the observation of the derivatizing reagent, it is preferable that the adaptor 40 and the sample cell 10 are transparent, for example, organic glass is used as a feasible way; at the moment, even if any disassembly operation is not carried out, the tester can still carry out visual observation on the derivatization reagent, thereby providing important help for improving the testing efficiency.
Furthermore, in order to ensure the water-proof and air-permeable properties of the separation membrane 30, the separation membrane 30 is preferably a water-proof and air-permeable membrane, for example, the separation membrane 30 is preferably a bulky polytetrafluoroethylene membrane, which can ensure that the derivatization reagent does not permeate into the vacuum chuck 20, and can ensure the smooth circulation of formaldehyde, thereby providing an important guarantee for the accuracy of the test.
In order to better explain the application mode of the device, the invention provides three specific application methods:
a first method of application comprises the following steps,
step S1, a derivatization reagent is filled in the liquid storage cavity 11, the sample cell 10 is hermetically connected with the vacuum chuck 20, and the derivatization reagent contains acetylacetone; specifically, in this case, the derivatization reagent is a receiving solution containing 350. mu.L of a 0.5% acetylacetone solution (containing 0.5g/mL ammonium acetate and 6% acetic acid);
s2, dropwise adding the formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck 20 onto the glass plate so that the vacuum chuck 20 surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, and detecting the derivatization reagent by using an ultraviolet spectrophotometer to obtain a formaldehyde content standard curve; specifically, the formaldehyde standard solution dripped on the glass plate is 100 mu L, adsorption is carried out for preset time of 48 hours, an ultraviolet spectrophotometer is used for detection, and a standard curve of absorbance at 414nm and formaldehyde content is drawn;
step S3, repeating the step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck 20 on the surface of the furniture to be detected, and then performing the operation consistent with the step S2 to obtain a formaldehyde detection signal of the furniture to be detected; namely, adsorption is carried out for a preset time of 48 hours, and an ultraviolet spectrophotometer is used for detection, and the absorbance at 414nm is read;
step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time; as can be seen from fig. 5, the linear range is 2.0-10.0mg/mL (RSD ═ 3.5%), the detection limit is 0.5mg/mL, and the formaldehyde emission per unit area and unit time of the furniture to be detected is as follows: 6.3mg/mL × 100 μ L/(32mm × 32mm × 3.14 × 48h) ═ 4.08mg · m-3·h-1。
A second method of application comprises the steps of,
step S1, a derivatization reagent is filled in the liquid storage cavity 11, the sample cell 10 is hermetically connected with the vacuum chuck 20, and the derivatization reagent contains 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazocene; specifically, the derivatization reagent is 0.5% 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazene with the receiving solution filled therein by 350 μ L;
step S2, dropwise adding the formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck 20 onto the glass plate so that the vacuum chuck 20 surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out a derivatization reagent, adding a potassium periodate solution, placing, and detecting the derivatization reagent by using an ultraviolet spectrophotometer after the placing is finished to obtain a formaldehyde content standard curve; specifically, 100 μ L of formaldehyde standard solution is dripped on the glass plate at the moment, 100 μ L of 0.5% potassium periodate solution is added after 24 hours of preset time adsorption, the glass plate is placed for 5 minutes to develop color completely, and then an ultraviolet spectrophotometer is used for detecting the color, and a standard curve of absorbance at 594nm and formaldehyde content is drawn;
step S3, repeating the step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck 20 on the surface of the furniture to be detected, and then performing the operation consistent with the step S2 to obtain a formaldehyde detection signal of the furniture to be detected; after 24 hours of preset time adsorption, adding 100 mu L of 0.5% potassium periodate solution, standing for 5 minutes for complete color development, detecting by using an ultraviolet spectrophotometer, and reading the absorbance at 594 nm;
step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time; as can be seen from fig. 6, the linear range is 1.0-5.0mg/mL (RSD ═ 5.5%), the detection limit is 0.05mg/mL, and the formaldehyde emission per unit area and unit time of the furniture to be tested is obtained by detection: 3.1mg/mL × 100 μ L/(32mm × 32mm × 3.14 × 24h) ═ 4.02mg · m-3·h-1。
A third method of application comprises the steps of,
step S1, a derivatization reagent is filled in the liquid storage cavity 11, the sample cell 10 is hermetically connected with the vacuum chuck 20, and the derivatization reagent contains 2, 4-dinitrophenylhydrazine acetonitrile; specifically, the derivatization reagent is 2.0mg/mL 2, 4-dinitrophenylhydrazine with the content of 350 mu L in the receiving solution;
step S2, dropwise adding the formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck 20 onto the glass plate so that the vacuum chuck 20 surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, heating the derivatization reagent for a specified time at a preset temperature, and detecting by using a high performance liquid chromatograph to obtain a formaldehyde content standard curve; specifically, the formaldehyde standard solution dripped on the glass plate is 100 mu L, adsorption is carried out for a preset time of 1 hour, then the derivatization reagent is heated for 1 hour at a preset temperature of 70 ℃, a high performance liquid chromatograph is adopted for detection after the heating is finished, the detection wavelength is 367nm, and a peak area-formaldehyde content standard curve at 10.4min is drawn;
step S3, repeating the step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck 20 on the surface of the furniture to be detected, and then performing the operation consistent with the step S2 to obtain a formaldehyde detection signal of the furniture to be detected; the method comprises the steps of performing adsorption for a preset time of 1 hour, heating a derivatization reagent for 1 hour at a preset temperature of 70 ℃, detecting by using a high performance liquid chromatograph after heating is finished, wherein the detection wavelength is 367nm, and reading the peak area at the position of 0.4 min;
step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time; as can be seen from fig. 7, the linear range is 20-200 μ g/mL (RSD ═ 7.5%), the detection limit is 5 μ g/mL, and the formaldehyde emission per unit area and unit time of the furniture to be tested is obtained by detection: 130 μ g/mL × 100 μ L/(32mm × 32mm × 3.14 × 1h) ═ 4.01mg · m-3·h-1。
The three methods for detecting formaldehyde by derivatization have the following advantages and disadvantages:
the acetylacetone method can be used for directly carrying out in-situ detection, and after absorption, the method can be used for directly carrying out quantitative or semi-quantitative analysis according to the color depth without disassembling and adding additional reagents; but the sensitivity is poor and a longer absorption time is required.
The 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazacyclopental method is more sensitive than acetylacetone, but requires the addition of additional reagents for disassembly.
The high performance liquid chromatography has the advantages of highest sensitivity, good anti-interference performance and short absorption time, but the high performance liquid chromatography needs to be disassembled to complete the heating reaction, and the high performance liquid chromatography is a large instrument and is not beneficial to field detection.
In conclusion, the beneficial effects of the invention are as follows:
1. compared with the prior art, the device for monitoring the formaldehyde release of the customized furniture in situ is suitable for monitoring the formaldehyde release of the customized furniture, and can realize the integration of sampling and detection. The device is tightly adsorbed on the surface of the building material by utilizing the principle of a vacuum chuck 20, so that formaldehyde released by the building material passes through a separation membrane 30 and is absorbed by an absorption liquid; after corresponding chemical derivatization treatment, the product can be analyzed and quantified. In addition, the device has simple structure and small volume, and is convenient for in-situ sampling of furniture.
2. Compared with the prior art, the device provided by the invention overcomes the defect that the formaldehyde release of the customized furniture cannot be monitored in situ in real time in the traditional indoor formaldehyde detection method, and realizes fixed-point, timed and periodic detection of the formaldehyde release of the customized furniture.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (10)

1. A device for in-situ monitoring of formaldehyde release from customized furniture,
comprises a sample cell, a vacuum chuck and a separation membrane;
a liquid storage cavity is arranged in the sample pool and used for loading a derivatization reagent for absorbing formaldehyde;
the vacuum chuck is provided with an adsorption end and a conduction end, the adsorption end and the conduction end are communicated with each other, the adsorption end is used for adsorbing an object to be detected, the conduction end is detachably and hermetically connected with the sample cell, and the conduction end is communicated with the liquid storage cavity;
the separation membrane separation in the conduction end with between the stock solution chamber, the separation membrane is used for supplying formaldehyde to enter into in the stock solution chamber, and the separation derivatization reagent flows out the stock solution chamber.
2. The apparatus of claim 1,
the inner wall of the port of the sample cell is provided with internal threads, and the outer part of the conduction end is provided with external threads;
the device further comprises an adapter and a nut, wherein two ends of the adapter are communicated, external threads are arranged on the outer walls of the two ends of the adapter, one end of the adapter is in threaded connection with the inner wall of the port of the sample cell, the other end of the adapter is in threaded connection with the nut, and the nut is further in threaded connection with the outer wall of the conducting end;
the separation membrane is blocked between the adaptor and the liquid storage cavity.
3. The apparatus of claim 2, wherein the external threads on both ends of the adaptor are counter-threaded.
4. The apparatus of claim 2, wherein the adaptor and the sample cell are both transparent.
5. The apparatus of claim 1, wherein the vacuum chuck is a telescoping chuck.
6. The device of claim 1, wherein the separation membrane is a water-proof, gas-permeable membrane.
7. The apparatus of claim 6, wherein the separation membrane is a lofty polytetrafluoroethylene membrane.
8. A method of using the device for in situ monitoring of formaldehyde emission from custom-made furniture, wherein the device of claim 1 is used for testing, comprising the steps of,
step S1, loading the derivatization reagent into the liquid storage cavity, and hermetically connecting the sample cell with the vacuum chuck, wherein the derivatization reagent contains acetylacetone;
s2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, and detecting the derivatization reagent by using an ultraviolet spectrophotometer to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
9. A method of using the device for in situ monitoring of formaldehyde emission from custom-made furniture, wherein the device of claim 1 is used for testing, comprising the steps of,
step S1, putting the derivatization reagent into the liquid storage cavity, and hermetically connecting the sample cell with the vacuum chuck, wherein the derivatization reagent contains 4-amino-3-hydrazine-5-mercapto-1, 2, 4-triazocene;
step S2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, adding a potassium periodate solution, placing, and detecting the derivatization reagent by using an ultraviolet spectrophotometer after placing to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
10. A method of using the device for in situ monitoring of formaldehyde emission from custom-made furniture, wherein the device of claim 1 is used for testing, comprising the steps of,
step S1, the derivatization reagent is filled in the liquid storage cavity, the sample pool is hermetically connected with the vacuum chuck, and the derivatization reagent contains 2, 4-dinitrophenylhydrazine acetonitrile;
step S2, dropwise adding a formaldehyde standard solution onto a glass plate, adsorbing the vacuum chuck onto the glass plate so that the vacuum chuck surrounds the formaldehyde standard solution, adsorbing the formaldehyde standard solution for a preset time, taking out the derivatization reagent, heating the derivatization reagent at a preset temperature for a preset time, and detecting by using a high performance liquid chromatograph to obtain a formaldehyde content standard curve;
step S3, repeating step S2 on the premise of changing the concentration of the formaldehyde standard solution to obtain standard curves of formaldehyde content corresponding to different concentrations;
step S4, repeating the operation of step S1, then absorbing the vacuum chuck on the surface of the furniture to be detected, and then performing the operation consistent with the operation of step S2 to obtain a formaldehyde detection signal of the furniture to be detected;
and step S5, comparing the formaldehyde content standard curve with the formaldehyde detection signal to obtain the formaldehyde emission amount of the furniture to be detected in unit area and unit time.
CN202011050744.6A 2020-09-29 2020-09-29 Device for in-situ monitoring of formaldehyde release of customized furniture and application method Pending CN112255053A (en)

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CN101949897A (en) * 2010-06-30 2011-01-19 北京六角体科技发展有限公司 Method for detecting pre-treatment of nitrofurans metabolite
CN203337553U (en) * 2013-07-23 2013-12-11 海南出入境检验检疫局检验检疫技术中心 Rapid test packet for formaldehyde emission amount
CN209086233U (en) * 2018-11-05 2019-07-09 瞿芬 Formaldehyde examination device and air treatment system
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