CN110132785B - Adhesive or coating moisture and total volatile organic content rapid determination equipment - Google Patents
Adhesive or coating moisture and total volatile organic content rapid determination equipment Download PDFInfo
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- CN110132785B CN110132785B CN201910395384.4A CN201910395384A CN110132785B CN 110132785 B CN110132785 B CN 110132785B CN 201910395384 A CN201910395384 A CN 201910395384A CN 110132785 B CN110132785 B CN 110132785B
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- 238000012360 testing method Methods 0.000 claims abstract description 191
- 238000001704 evaporation Methods 0.000 claims abstract description 167
- 230000008020 evaporation Effects 0.000 claims abstract description 167
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000003973 paint Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims description 138
- 239000012855 volatile organic compound Substances 0.000 claims description 37
- 239000002274 desiccant Substances 0.000 claims description 26
- 238000005259 measurement Methods 0.000 claims description 24
- 239000011491 glass wool Substances 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 239000003153 chemical reaction reagent Substances 0.000 description 11
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- 238000003556 assay Methods 0.000 description 9
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- 230000008859 change Effects 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- 229910021536 Zeolite Inorganic materials 0.000 description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 6
- 239000002808 molecular sieve Substances 0.000 description 6
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- 238000004891 communication Methods 0.000 description 4
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
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- 239000011630 iodine Substances 0.000 description 1
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- 210000000653 nervous system Anatomy 0.000 description 1
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- 230000001717 pathogenic effect Effects 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a device for rapidly determining the moisture content and total volatile organic matter content of an adhesive or a coating, which comprises at least one group of test channels, wherein each group of test channels comprises a sample test channel and a blank test channel, and a first evaporation device and a second evaporation device are placed in a constant-temperature heating device with a first set temperature during determination; the sample test channel further comprises a first connecting pipeline, the blank test channel further comprises a second connecting pipeline, and the first connecting pipeline and the second connecting pipeline are used for introducing dry gas with set flow rate to the first evaporation device and the second evaporation device after moisture determination conditions are determined according to the type of the adhesive or the paint. The measuring equipment provided by the invention has the advantages of high efficiency, economy and environmental protection in the measuring process, and accurate and stable measuring result.
Description
Technical Field
The invention relates to the technical field of analysis and detection of decorative materials, in particular to a device for rapidly determining the content of adhesive or paint moisture and total volatile organic compounds (Total Volatile Organic Compound, TVOC).
Background
In recent years, with the rapid development of social economy, the demand for decoration of offices and living places is increasing, and thus new building materials, particularly chemical synthetic building materials, are widely used. These building materials directly or indirectly release various pollutants, causing indoor air pollution. Wherein the volatile organic compounds are toxic to both the nervous system and respiratory system of the human body and can cause physical discomfort such as pathogenic building syndrome (Sick Building Syndrome, SBS). The Total Volatile Organic Compounds (TVOC) are taken as an important evaluation index of indoor volatile organic compound pollution, and are listed in the indoor air quality standard of China for evaluating the influence of the volatile organic compounds on health.
The water content and the Total Volatile Organic Compound (TVOC) content in the paint and the adhesive of the building decoration material are very important indexes, and are national mandatory standards. The total volatile organic compounds are security parameters which need to be strictly controlled, and all products need to be satisfied. At present, the determination of the Total Volatile Organic Content (TVOC) in the adhesive for the decoration material is carried out according to the method specified by annex F in GB 18583-2008; the determination of Total Volatile Organic Compounds (TVOC) in interior wall coatings was carried out according to the method specified in appendix B of GB 18582-2008; the Total Volatile Organic Compounds (TVOC) in the aqueous coating were measured according to the method specified in appendix A of GB 24410-2009.
These standards require that the moisture content of the total volatile organic compounds must be subtracted from the total volatile organic compound content measurement process, so that the moisture measurement is the key to the total volatile organic compound content measurement.
The current standard prescribed method is to measure moisture by karl fischer and gas chromatography, the most common method used in laboratories is karl fischer.
However, the prior karl fischer method for measuring moisture has the following defects: 1. the price of the instrument is high, and the price of the imported Karl Fischer moisture tester is about 15 ten thousand yuan each; 2. the preparation method is characterized in that a Karl Fischer reagent is needed to be prepared from iodine (I2), sulfur dioxide (SO 2), pyridine (C5H 5N) and methanol (CH 3 OH). Among them, pyridine (C5H 5N) in the list of class 2B carcinogens published by the international cancer research institute of the world health organization, these hazardous agents pose a threat to human health; 3. the karl fischer reagent is complex in configuration process, calibration is needed before use, the karl fischer reagent is extremely easy to fail, and the electrolytic electrode is also needed to be cleaned and maintained after use; 4. the sampling amount of the test sample is too small (less than 0.1 g), and the test error for the non-uniform sample is huge; 5. there are limitations to insoluble sample testing; 6. the karl fischer method is suitable for measuring trace moisture, and is not particularly suitable for water-based paint and adhesives.
The existing gas chromatography has similar defects, especially high equipment (consumable material) cost, small sampling amount, complex pretreatment and the like, and the sample needs to be dissolved by an organic solvent.
Therefore, the existing analytical detection technology for decorative materials is still to be improved and developed.
Disclosure of Invention
The invention mainly aims to provide the equipment for rapidly measuring the moisture and total volatile organic compounds content of the adhesive or the coating, which is efficient, economical and environment-friendly in the measuring process and accurate and stable in measuring result.
In order to achieve the above object, the technical scheme provided by the embodiment of the invention is as follows: the method comprises the steps of providing adhesive or paint moisture and total volatile organic content rapid determination equipment, wherein at least one group of test channels are arranged, each group of test channels comprises a sample test channel and a blank test channel, the sample test channel comprises a first evaporation device and a first drying device which is communicated with the first evaporation device and only absorbs moisture, and the blank test channel comprises a second evaporation device and a second drying device which is communicated with the second evaporation device and only absorbs moisture;
The first evaporation device comprises a chamber for accommodating an adhesive or paint test sample with set quality, the second evaporation device has the same structure as the first evaporation device, and the first evaporation device and the second evaporation device are placed in a constant temperature heating device with a first set temperature during measurement;
The sample test channel also comprises a first connecting pipeline which is communicated with the first moisture test device and the first drying device, the blank test channel also comprises a second connecting pipeline which is communicated with the second moisture test device and the second drying device, and the first connecting pipeline and the second connecting pipeline are used for determining moisture determination conditions according to the types of adhesives or coatings and introducing drying gas with set flow rates into the first evaporation device and the second evaporation device.
In order to realize the simultaneous operation of a plurality of groups of test channels, the dry air source is connected with each test channel through a valve.
Preferably, the first evaporation device of the sample testing channel is communicated with a drying air source, the first evaporation device is added with the test sample, and the first drying device is filled with activated drying agent; the second evaporation device of the blank test channel is communicated with the drying air source, the second evaporation device is not added with a test sample, and the second drying device is filled with an activated drying agent.
When the device is implemented, the first evaporation device and the second evaporation device have the same structure and comprise a chamber for accommodating an adhesive or paint test sample with set quality, and the chamber comprises a first air inlet and a first air outlet.
In order to maintain the constant weight of the evaporation device, the first air inlet and the first air outlet of the first evaporation device and the second evaporation device are provided with detachable evaporation bottle plugs.
The first drying device and the second drying device which only absorb moisture have the same structure and comprise a containing cavity, wherein the containing cavity is connected with a second air inlet, a second air outlet and a charging port for charging the activated drying agent.
In order to maintain the constant weight of the drying device, the first drying device, the second air inlet, the second air outlet and the charging port of the second drying device are provided with detachable drying bottle plugs.
Further, when the first drying device and the second drying device are measured, the charging port is sealed by the drying bottle plug, and glass wool filter layers are arranged at the positions of the second air inlet and the second air outlet of the first drying device and the second drying device.
Preferably, the first connecting pipeline and the second connecting pipeline adopt a silicone tube or a butyl tube.
When a test passage is arranged, the first connecting pipeline comprises a first connecting pipe and a second connecting pipe, the second connecting pipeline comprises a third connecting pipe and a fourth connecting pipe, the output of the valve is communicated with the first connecting pipe and the third connecting pipe, the first connecting pipe is communicated with the valve and the first evaporation device, and the second connecting pipe is communicated with the first evaporation device and the first drying device; the third connecting pipe is communicated with the valve and the second evaporation device, the fourth connecting pipe is communicated with the second evaporation device and the second drying device, and the drying air source is communicated with the valve through a flowmeter.
The beneficial effects of the embodiment of the invention are as follows: the adhesive or coating moisture and total volatile organic content rapid determination device of the embodiment is characterized in that a test sample moisture evaporation experiment and an air moisture evaporation experiment are established in the same test channel, and the moisture content in the same space of the same evaporation device is determined through the air moisture evaporation experiment; and the evaporation experiment of the test sample is adopted, the mass change of the first evaporation device filled in the test sample before and after the experiment is measured, and the water content in the test sample is subtracted, so that the accurate content of the total volatile organic compounds can be deduced.
The quick measuring equipment for the moisture and total volatile organic compound content of the adhesive or the coating is efficient, economical, convenient and environment-friendly in measuring process, accurate and stable in measuring result and high in reagent consumable recycling rate. In the air moisture evaporation experiment of the embodiment, the moisture can be measured by measuring the mass change of the first drying device and the second drying device in the high-temperature baking process before the total volatile organic compound content is measured, and the moisture content measurement is carried out without additional tests; the drying agent, the silica gel tube, the evaporation bottle stopper, the drying bottle stopper, the glass wool and other consumable materials of the measuring equipment are low in cost, reusable, and low in nitrogen consumable material cost; the test sample water evaporation experiment and the air water evaporation experiment process of the test equipment are simple and convenient to operate, and the test equipment does not need a calibration reagent and does not need to dissolve a sample; the measuring equipment of the embodiment is compared with the Karl Fischer method and the gas chromatography, so that the accuracy is higher; the measuring equipment of the embodiment eliminates errors caused by the problem of the sampling amount due to the large sampling amount of the test sample, and has good stability of the detection result; the experimental process of the measuring equipment of the embodiment does not use any organic reagent and other consumable materials of harmful reagents, and does not cause threat to the environment and human health; the reagent consumable of the measuring equipment has the performance of repeated use, reduces emission and provides sustainability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for rapidly determining the moisture content and the total volatile organic content of an adhesive or a coating according to an embodiment of the invention;
FIG. 2 is a schematic diagram of an embodiment of a device for rapidly determining moisture content and total volatile organic compounds content of an adhesive or coating material according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of another embodiment of a device for rapidly determining the moisture content and total volatile organic compounds content of a seed adhesive or coating material according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a structure of a set of test paths provided by an apparatus for rapidly measuring the moisture content and total volatile organic compounds content of an adhesive or a coating according to an embodiment of the present invention;
FIG. 5 is a perspective view of a first evaporation device and a second evaporation device of an apparatus for rapidly determining the moisture content and total volatile organic compounds content of an adhesive or a coating according to an embodiment of the present invention; and
Fig. 6 is a perspective view of a first drying device and a second drying device of the apparatus for rapidly determining the moisture content and total volatile organic compounds content of an adhesive or a coating according to an embodiment of the present invention.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications (such as up, down, left, right, front, and rear … …) are included in the embodiments of the present invention, the directional indications are merely used to explain the relative positional relationship, movement conditions, etc. between the components in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indications are correspondingly changed.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The invention relates to a device for rapidly determining the moisture content and total volatile organic compounds content of an adhesive or a coating, which combines a direct drying method with a drying agent, a 3A zeolite molecular sieve and water absorption characteristics, calculates the moisture content (H) by the mass difference of the drying agent before and after the test, and simultaneously subtracts the moisture content of a sample to determine the Total Volatile Organic Compounds (TVOC) content (omega).
The device for rapidly determining the moisture content and the total volatile organic compound content of the adhesive or the coating in the embodiment is characterized in that a test sample moisture evaporation experiment and a blank control experiment are established in the same test path, and the moisture content in the same space of the same evaporation device is determined through the blank control experiment; and the evaporation experiment of the test sample is adopted, the mass change of the first evaporation device filled in the test sample before and after the experiment is measured, and the water content in the test sample is subtracted, so that the accurate content of the total volatile organic compounds can be deduced.
The device for rapidly determining the moisture content and the total volatile organic compound content of the adhesive or the coating of the embodiment is provided with at least one group of test channels, each group of test channels comprises a sample test channel and a blank test channel, the sample test channel comprises a first evaporation device and a first drying device which is communicated with the first evaporation device and only absorbs moisture, and the blank test channel comprises a second evaporation device and a second drying device which is communicated with the second evaporation device and only absorbs moisture.
The experimental scheme is that a proper amount of adhesive or paint test sample is placed in a first evaporation device, also called an evaporation bottle, placed in a high-temperature heating device with a first set temperature, and connected with a first drying device 14 which only absorbs water, also called a drying bottle. The determination conditions are determined according to the type of the adhesive or the paint, dry gas such as high-purity nitrogen is continuously introduced for blowing, and the moisture content of the adhesive or the paint and the total volatile matter content including total organic matters and moisture are respectively determined within the time specified by the determination conditions. The total volatile matter content of the test sample is subtracted by the water content (H) of the water, and the total volatile organic matter (TVOC) content (omega) in the adhesive is calculated by subtracting the water content of the sample.
Total volatile substances are all substances (moisture) which can be volatilized under the prescribed test conditions. Total volatile organics: all organic compounds which can be volatilized under the prescribed test conditions are generally referred to as any organic compound having an initial boiling point of less than or equal to 250℃under a standard atmospheric pressure of 101.3kPa, expressed as TVOC.
The method for rapidly determining the moisture and total volatile organic compound content of the adhesive or the coating is efficient, economical, convenient and environment-friendly in determination process, accurate and stable in determination result and high in reagent consumable recycling rate.
The following describes a method for rapidly determining the moisture and total volatile organic content of an adhesive or coating, which is useful for understanding the experimental principles and processes of the apparatus.
The method is illustrated by way of example with respect to a test path, as shown in fig. 4.
As shown in fig. 2 and 4, to ensure constant weight of the moisture measurement device, each test path further includes, prior to testing:
The first evaporation device 11 and the second evaporation device 12 are put into a constant temperature heating device with a third set temperature to be dried to constant weight, the mass difference before and after the drying process is not more than 0.3 mg, and the mass before the experiment of the first evaporation device 11 and the mass before the experiment of the second evaporation device 12 are recorded.
Referring to fig. 1, the method for rapidly determining the moisture content and the total volatile organic compound content of the adhesive or the coating according to the embodiment comprises the following steps:
step 101: a channel comprising a first evaporation device 11 and a first drying device 14 in communication therewith that absorbs only moisture, the blank test channel comprising a second evaporation device 12 and a second drying device 15 in communication therewith that absorbs only moisture;
step 102: drying the drying gas in the sample test channel and the blank test channel to discharge air moisture in the channel;
Step 103: when each test passage is tested, placing a set-quality adhesive or paint test sample on the first evaporation device 11 and connecting the sample test passage;
Step 104: heating the first evaporator and the second evaporator in a closed manner; step 105: when heating, determining measurement conditions according to the type of the adhesive or the paint, and introducing a drying gas with a set flow rate, such as high-purity nitrogen or air subjected to drying treatment, into the first evaporation device 11 and the second evaporation device 12, wherein the water content of the air is not more than 0.01%; and
Step 106: measuring the water content (H) in the adhesive or paint according to the mass change before and after the test of the first drying device 14 and the mass change before and after the test of the second drying device 15;
Step 107: the total volatile content (ω) in the adhesive or paint is determined from the mass change of the first evaporation device 11 after the test sample is added minus the sample moisture.
Wherein the step of heating the first evaporation device and the second evaporation device in a closed manner further comprises:
Placing the first evaporation device and the second evaporation device into a constant temperature heating device with a first set temperature;
the flow rate of dry gas, such as high purity nitrogen, is substantially uniform across the sample test channel and the blank test channel.
The heating device mode of the present embodiment is different according to the test sample, for different measurement conditions of different test samples.
As shown in fig. 2, for the same test sample, multiple sample test channels are connected in parallel in the heating device 3, for example, three sample test channels are provided, so as to complete an assay experiment for detecting multiple test samples at the same time.
As shown in fig. 3, or for test samples with different test temperatures, multiple groups of test channels are provided, and each group of test channels performs experiments on a corresponding heating device, such as a first test channel 1 and a second test channel 2, so as to complete measurement experiments of different types of test samples at the same time.
According to different measuring objects, the measuring conditions are determined according to the types of the adhesive or the paint:
when the adhesive or the coating is an amino resin adhesive, the measurement conditions comprise a first set temperature of 110+/-2 ℃ and a test time of 200+/-5 minutes;
when the adhesive or the coating is a phenolic resin adhesive, the measurement conditions comprise a first set temperature of 140+/-2 ℃ and a test time of 80+/-2 minutes;
when the adhesive or the coating is other adhesives, the measurement conditions comprise a first set temperature of 110+/-2 ℃ and a test time of 200+/-5 minutes;
When the adhesive or the paint is paint, the measurement conditions comprise a first set temperature of 110+/-2 ℃ and a test time of 200+/-5 minutes.
In practice, in the step of introducing a drying gas such as high purity nitrogen gas at a set flow rate into the first evaporation device 11 and the second evaporation device 12,
Ensure that the nitrogen flow rate of each split test path is stabilized at 500±50 ml/min;
The total flow rate of nitrogen from the dry gas source 6 is the sum of the flow rates of nitrogen from all of the branched test paths.
In a specific embodiment, the first evaporation device 11 of the sample testing channel is communicated with the dry air source 6, the first evaporation device 11 is added with a test sample, and the first drying device 14 is filled with a drying agent; the second evaporation device 12 of the blank test channel is communicated with the dry air source 6, the second evaporation device 12 is not added with a test sample, and the second drying device 15 is filled with a drying agent.
The dry air source 6 is connected to each test channel through valves, the number of which is the same as the number of test channels.
Description of specific experiments:
1. Constant weight treatment:
The constant weight process is directed to the first evaporation device 11 and the second evaporation device 12, i.e., evaporation bottles. And (3) putting the first evaporation device 11 and the second evaporation device 12 into a constant-temperature heating device with a third set temperature for drying to constant weight, wherein the mass difference before and after the drying process is not more than 0.3 mg, recording the mass before the experiment of the first evaporation device 11 and the mass before the experiment of the second evaporation device 12, and putting into a dryer for standby. In this example, the third set temperature is 105 ℃.
2. Weighing of test samples:
Specific examples: after the test sample is fully stirred or uniformly shaken, 1.5-2.0 g of the test sample is accurately weighed into a first evaporation device 11 with constant weight in advance, the first evaporation device 11 is rotated, the test sample is paved on the inner wall of the first evaporation device 11 as much as possible, and the two ends of a first air inlet and a first air outlet of the first evaporation device 11 are immediately sealed for standby by an evaporation bottle stopper. The second evaporation apparatus 12 was used for a blank test without a test sample.
3. Activating a drying agent:
The desiccant activation process includes:
Using a 3A zeolite molecular sieve as a desiccant;
The 3A zeolite molecular sieve is baked and activated by a muffle furnace, wherein the baking temperature is 350-400 ℃, and the 3A zeolite molecular sieve is baked for 8 hours under one atmosphere;
Or vacuum pumping the muffle furnace by adopting a vacuum pump, wherein the baking temperature is 150 ℃, and baking is carried out for 5 hours under one atmosphere; and
And (3) cooling the activated 3A zeolite molecular sieve to about 200 ℃ in the air, and immediately transferring to a dryer for cooling and preserving for standby.
In the preferred embodiment, the desiccant is cooled and protected during storage by dry nitrogen to prevent adsorption of moisture in the air. The activated 3A zeolite molecular sieve is recommended for use within 6 months of sealed storage.
4. Preparation of a drying bottle:
Placing the first drying device 14 and the second drying device 15 into a constant temperature heating device with a second set temperature to dry to constant weight, wherein the quality difference before and after the drying process is not more than 0.3 mg;
Filling a small amount of glass wool into the air inlets and the air outlets of the first drying device 14 and the second drying device 15, and filling the first drying device 14 and the second drying device 15 with the drying agent treated by the activating step;
Sealing the three openings of the first drying means 14 and the second drying means 15 with a desiccating bottle stopper, weighing together with the desiccating bottle stopper; and
The constant weight mass of the first drying means 14 and the constant weight mass of the second drying means 15 were recorded to the nearest 0.1 mg.
Specific examples: after the first drying device 14 and the second drying device 15 are dried to constant weight, the difference of the quality of the first drying device and the second drying device is not more than 1 mg. And A, B, a small amount of glass wool is plugged into the second air inlets and the second air outlets of the first drying device 14 and the second drying device 15 to serve as a glass filter cotton layer. Then, the activated drying agent is filled in the first drying device 14 and the second drying device 15, the first drying device 14 and the second drying device 15 are immediately sealed by the glue drying bottle stopper, the second air inlet, the second air outlet and the charging port 143 are weighed together with the drying bottle stopper, and the quality is recorded.
5. Detection process
Before performing the test, the rapid assay device is shown in the embodiment of FIG. 4, and a test path is used, including a sample test channel and a blank test channel. The drying air source 6 is opened under the condition that the evaporation bottle is not connected in advance by a silica gel tube or a butyl rubber tube. The total flow rate of nitrogen in the dry air source 6 was controlled to be 2000.+ -.100 ml/min, and at this time, the air flow rate of each test channel was about 500 ml/min, and the air flow rate was calibrated by a flow calibrator and was empty for 3 minutes to blow off the moisture in the test channels.
Then, the first evaporation device 11 and the second evaporation device 12 of the evaporation bottle are put into a high-temperature heating device, one end of the silica gel tube is connected with a drying air source 6 as shown in fig. 4, the other end of the silica gel tube is connected with the first evaporation device 11 and the second evaporation device 12, meanwhile, the drying bottle plugs of the second air outlets of the first drying device 14 and the second drying device 15 are opened, pure nitrogen of the drying air source 6 is not closed in the whole installation process, after the rapid measurement equipment is well connected, the total flow rate of the nitrogen is adjusted to 2000+/-100 milliliters/minute, and the temperature and the test time of the heating device are controlled according to the specified measurement conditions.
To ensure that the variations before and after the test do not become doped with other factors, the first evaporation device 11 and the second evaporation device 12 are taken out of the heating device at the end of the test;
Sealing the first evaporation device 11 by using an evaporation bottle plug used by an original sleeve, putting the first evaporation device into the dryer for cooling, and weighing the total mass of the first evaporation device and a test sample after the test;
At the same time, the first drying device 14 and the second drying device 15 were sealed using the desiccating bottle stopper 145, and the total mass of the desiccating agent and the test was measured, respectively.
6. Result calculation
In the calculation of the results, the water content of the adhesive or coating is calculated according to the formula (1):
H-the water content of the adhesive or coating, expressed as a percentage (%);
M-the mass of the test sample in grams (g);
m A -the total mass of the first drying device 14 and the desiccant after the test in grams (g);
m A0 -the total mass of the first drying device 14 and the desiccant prior to testing in grams (g);
m B -the total mass of the second drying device 15 and the drying agent after the test, in grams (g);
m B0 -the total mass of the second drying device 15 and the desiccant before the test, in grams (g);
the total volatile organic compound content in the adhesive is calculated according to the formula (2):
omega-the total volatile organic content of the adhesive or coating in grams per liter (g/L);
m A0 -the mass of the first evaporation apparatus 11 before the test, in grams (g);
M-the mass of the test sample in grams (g);
M A -the total mass of the test sample after the test and the first evaporation apparatus 11, in grams (g);
H-the water content of the adhesive or coating, expressed as a percentage (%);
ρ -the density of the test sample in grams per cubic centimeter (g/cm 3).
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Referring to fig. 3 to 6, the present embodiment relates to an apparatus for rapidly determining the moisture content and total volatile organic compounds content of an adhesive or a paint.
As shown in fig. 2, the rapid assay device includes a set of test paths for the same test sample. The heating device 3 is connected with multiple sample test channels in parallel, for example, three sample test channels are arranged, so as to complete the measurement experiment of detecting multiple test samples at the same time. The first sample testing path comprises a first evaporation device 11 and a first drying device 17. The second sample testing channel includes a second evaporation device 12 and a first drying device 18. The third sample testing channel comprises a first evaporation means 13 and a first drying means 19. The blank test channel comprises a second evaporation device 26 and a second drying device 27.
The rapid determination apparatus includes providing at least one set of test paths. In the embodiment shown in fig. 3, the rapid assay device comprises two sets of test paths, a first test path 1 and a second test path 2, respectively, for simultaneously performing assay experiments of different types of test samples. The first test path 1 comprises a sample test channel consisting of a first evaporation device 11 and a first drying device 14, and comprises a blank test channel consisting of a second evaporation device 12 and a second drying device 15. The first evaporation device 11 and the second evaporation device 12 complete the detection process in the heating device 5. The second test path 2 includes a sample test channel consisting of a first evaporation device 21 and a first drying device 24, and includes a blank test channel consisting of a second evaporation device 22 and a second drying device 25. The first and second evaporation devices 21 and 12 complete the detection process in the heating device 7.
In the embodiment shown in fig. 4, the rapid assay device comprises a test path.
Each set of test channels includes a sample test channel, a blank test channel, and a heating device. In the embodiment shown in fig. 4, the sample testing channel comprises a first evaporation means 11 and a first drying means 14 in communication therewith, which absorbs only moisture. The blank test channel comprises a second evaporation means 12 and a second drying means 15 in communication therewith which only absorbs moisture.
The first evaporation device 11 comprises a chamber for receiving a set mass of an adhesive or paint test sample. The chamber includes a first air inlet 112 and a first air outlet 113.
The second evaporation device 12 has the same structure as the first evaporation device 11, and the first evaporation device 11 and the second evaporation device 12 are placed in the constant temperature heating device 5 with a first set temperature during measurement.
The sample testing channel further comprises a first connecting line communicating the first evaporation device 11 and the first drying device 14. The blank test channel further comprises a second connecting pipeline for communicating the second evaporation device 12 and the second drying device 15. The first and second connecting lines are used to introduce a set flow rate of dry gas, such as high purity nitrogen, to the first and second evaporation devices 11 and 12 after determining the measurement conditions according to the type of adhesive or paint.
As shown in fig. 3, in order to realize simultaneous operation of multiple sets of test channels, the dry gas source 6 is connected to each test channel through a valve, such as valve 16, the number of which is the same as the number of test channels.
The first evaporation device 11 of the sample test channel is communicated with the drying air source 6, the first evaporation device 11 is added with a test sample, and the first drying device 14 is filled with activated drying agent; the second evaporation device 12 of the blank test channel is communicated with the drying air source 6, the second evaporation device 12 is not added with a test sample, and the second drying device 15 is filled with activated drying agent.
In order to maintain the constant weight of the evaporation device, the first air inlet 112 and the first air outlet 113 of the first evaporation device 11 and the second evaporation device 12 are provided with removable evaporation bottle stoppers.
The first drying device 14 and the second drying device 15 that only absorb moisture have the same structure and include a receiving chamber 141, and the receiving chamber 141 is connected to a second air inlet 142, a second air outlet 144, and a charging port 143 for charging an activated desiccant.
In order to maintain a constant weight of the drying apparatus, the first drying apparatus 14 and the second air inlet 142, the second air outlet 144 and the filling opening 143 of the second drying apparatus 15 are provided with removable drying stoppers 145.
The first drying device 14 and the second drying device 15 are sealed by the dry bottle stopper 145, and glass filter cotton layers are arranged at the positions of the second air inlet and the second air outlet of the first drying device 14 and the second drying device 15 when measured.
The first connecting pipeline and the second connecting pipeline adopt a silicone tube or a butyl tube.
With continued reference to fig. 4, when a test path is provided, the first connection pipe includes a first connection pipe 131 and a second connection pipe 133, and the second connection pipe includes a third connection pipe 132 and a fourth connection pipe 134. The output of the valve 16 communicates with the first connection pipe 131 and the third connection pipe 132. The first connecting pipe 131 communicates the valve 16 with the first evaporation device 11, and the second connecting pipe 133 communicates the first evaporation device 11 with the first drying device 14. The third connecting pipe 132 connects the valve 16 with the second evaporation device 12, the fourth connecting pipe 134 connects the second evaporation device 12 with the second drying device 15, and the drying air source 6 connects the valve 16 through the flow meter 61.
In this embodiment, the first evaporation device 11 and the second evaporation device 12 as evaporation bottles may be made of glass or other materials, such as metal, ceramic, polytetrafluoroethylene, etc., as the first drying device 14 and the second drying device 15 as drying bottles. The first evaporation device 11 and the second evaporation device 12 need to withstand high temperatures, for example 200 ℃.
The first connecting pipeline and the second connecting pipeline of the rapid determination device are preferably made of silicone tubes, and other pipeline materials which are resistant to high temperature and easy to connect, such as butyl rubber tubes, can be used. The connection between the components of the rapid determination device may be a sleeve connection, a snap-on connection or a hinge connection, and requires that the tightness of the connection be ensured. The rapid assay device of this embodiment describes only two and one test path embodiments, it being understood that the simultaneous assay of multiple test samples may be achieved by adding test paths. The heating time and temperature set in the measurement conditions of the rapid measurement device can be adjusted at any time according to the characteristics of the product.
The device for rapidly determining the moisture content and the total volatile organic compound content of the adhesive or the coating in the embodiment is characterized in that a test sample moisture evaporation experiment and a blank control experiment are established in the same test path, and the moisture content in the same space of the same evaporation device is determined through the blank control experiment; and the evaporation experiment of the test sample is carried out, the mass change of the first evaporation device 11 filled in the test sample before and after the experiment is measured, and the water content in the test sample is subtracted, so that the accurate content of the total volatile organic compounds can be deduced.
The quick measuring equipment for the moisture and total volatile organic compound content of the adhesive or the coating is efficient, economical, convenient and environment-friendly in measuring process, accurate and stable in measuring result and high in reagent consumable recycling rate. The blank test of the embodiment can measure the moisture by measuring the mass change of the first drying device 14 and the second drying device 15 in the high-temperature baking process before the total volatile organic compound content measurement, and the moisture content measurement does not need to be additionally tested; the measuring equipment of the embodiment has low cost, low cost of consumable materials such as the activated drying agent, pure nitrogen and the like, and can be reused; the test sample water evaporation test and the blank control test of the measuring equipment are simple and convenient to operate, and the measuring equipment does not need a calibration reagent and does not need to dissolve a sample; the measuring method and the measuring equipment of the embodiment are compared with the Karl Fischer method and the gas chromatography, so that the accuracy is higher; the measuring method and the measuring device of the embodiment eliminate errors caused by the problem of the sampling amount because of the large sampling amount of the test sample, and the detection result has good stability; the method and the equipment for measuring the biological activity of the human body in the embodiment do not use any organic reagent and other consumable materials of harmful reagents in the experimental process, and cannot cause threat to the environment and the human health; the assay method and apparatus of the present embodiments provide for reagent consumables that are reusable, reduce emissions, and provide sustainability.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the specification and drawings of the present invention or direct/intermittent application in other related technical fields are included in the scope of the invention.
Claims (3)
1. The quick testing equipment for the moisture content and the total volatile organic compound content of the adhesive or the coating is characterized by comprising at least one group of testing passages, wherein each group of testing passages comprises a sample testing passage and a blank testing passage which does not contain a testing sample, the sample testing passage comprises a first evaporation device and a first drying device which is communicated with the first evaporation device and only absorbs moisture, and the blank testing passage comprises a second evaporation device and a second drying device which is communicated with the second evaporation device and only absorbs moisture;
The first evaporation device comprises a chamber for accommodating an adhesive or paint test sample with set quality, the second evaporation device has the same structure as the first evaporation device, and the first evaporation device and the second evaporation device are placed in a constant temperature heating device with a first set temperature during measurement;
The sample test channel further comprises a first connecting pipeline communicated with the first evaporation device and the first drying device, the blank test channel further comprises a second connecting pipeline communicated with the second evaporation device and the second drying device, and the first connecting pipeline and the second connecting pipeline are used for introducing drying gas with set flow rate to the first evaporation device and the second evaporation device after determining moisture determination conditions according to the types of adhesives or coatings;
the test device also comprises a dry air source, wherein the dry air source is connected with each test passage through a valve;
The first evaporation device of the sample test channel is communicated with the drying air source, the first evaporation device is added with a test sample, and the first drying device is filled with activated drying agent; the second evaporation device of the blank test channel is communicated with the drying air source, the second evaporation device is not added with a test sample, and the second drying device is filled with an activated drying agent;
The first evaporation device and the second evaporation device have the same structure and comprise a containing chamber for containing an adhesive or paint test sample with set quality, and the containing chamber comprises a first air inlet and a first air outlet;
The first air inlet and the first air outlet of the first evaporation device and the second evaporation device are provided with removable evaporation bottle plugs;
The first drying device only absorbing moisture and the second drying device have the same structure and comprise a containing cavity, wherein the containing cavity is connected with a second air inlet, a second air outlet and a charging port for charging an activated drying agent;
the first drying device, the second air inlet, the second air outlet and the charging port of the second drying device are provided with detachable drying bottle plugs;
And when the first drying device and the second drying device are used for measurement, the charging port is sealed by the drying bottle plug, and glass wool filter layers are arranged at the positions of the second air inlets and the second air outlets of the first drying device and the second drying device.
2. The apparatus for rapidly determining the moisture and total volatile organic content of an adhesive or a coating according to claim 1, wherein the first connecting pipeline and the second connecting pipeline are silicone tubes or butyl tubes.
3. The apparatus for rapidly determining moisture and total volatile organic compounds content of an adhesive or a paint according to claim 1, wherein when a test path is provided, the first connecting pipe comprises a first connecting pipe and a second connecting pipe, the second connecting pipe comprises a third connecting pipe and a fourth connecting pipe, the output of the valve is communicated with the first connecting pipe and the third connecting pipe, the first connecting pipe is communicated with the valve and the first evaporation device, and the second connecting pipe is communicated with the first evaporation device and the first drying device; the third connecting pipe is communicated with the valve and the second evaporation device, the fourth connecting pipe is communicated with the second evaporation device and the second drying device, and the drying air source is communicated with the valve through a flowmeter.
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| CN110658347A (en) * | 2019-10-11 | 2020-01-07 | 天津市滨海新区塘沽滨海建筑工程质量检测中心有限公司 | Automatic formaldehyde detection equipment and formaldehyde detection method |
| CN110975536A (en) * | 2019-11-22 | 2020-04-10 | 北京普瑞亿科科技有限公司 | Multi-channel vaporization detection platform and application thereof |
| CN111307649A (en) * | 2020-03-12 | 2020-06-19 | 北京市环境保护科学研究院 | Method for detecting content of volatile organic compounds in asphalt |
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