CN111521523B - Rapid detection method for migration of chemical substances in protective coating to wading pipe - Google Patents
Rapid detection method for migration of chemical substances in protective coating to wading pipe Download PDFInfo
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- CN111521523B CN111521523B CN202010290088.0A CN202010290088A CN111521523B CN 111521523 B CN111521523 B CN 111521523B CN 202010290088 A CN202010290088 A CN 202010290088A CN 111521523 B CN111521523 B CN 111521523B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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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
- G01N1/2226—Sampling from a closed space, e.g. food package, head space
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- 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
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- 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
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
Abstract
The invention discloses a rapid detection method for migration of chemical substances in protective paint to a pipe involved in water, which comprises the following steps: (1) preparing a sealing wading pipe; (2) preparation of a test piece to be tested: the test piece to be tested comprises a blank test piece and a migration test piece; selecting part of the sealed wading pipe prepared in the step (1) as a blank test piece; selecting part of the sealed wading pipe prepared in the step (1) as a migration test piece, wherein the migration test piece is prepared by coating protective paint on the part of the sealed wading pipe except for the plug; (3) migration experiment: respectively placing the test pieces to be tested prepared in the step (2) under the same migration experiment conditions to carry out a migration experiment; (4) Analysis and detection, including detection of protective paint, gas in the pipe, flushing fluid and pipe wall; the method is simple and quick, short in test period, high in accuracy, and suitable for the aspects of actual engineering detection, safety and sanitation of wading products, use functions and the like.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a rapid detection method for migration of chemical substances in protective coating to a wading pipe.
Background
With the progress of urbanization, the vigorous development of emerging areas, the continuous improvement of urbanization level and the continuous improvement of requirements of people on houses, the sustainable development of the building industry is not felt to be unintelligible. The water supply and drainage engineering is taken as an important component part of the whole building or municipal engineering, water is taken as an important resource penetrating into various industries, and the basic premise of maintaining survival of most organisms is provided, so that the establishment of a complete water supply and drainage system is directly related to the exertion of the whole functions of cities and the basic guarantee of daily life of people. In addition, along with the gradual increase of the health and safety demands of people on drinking water, higher demands are put forward on water delivery and distribution equipment and protective paint thereof in a water supply and drainage system.
The technical regulations of building water supply composite pipeline engineering, CJJ/T155-2011, prescribe that the pipeline is waterproof and anticorrosive by adopting paint when the pipeline is buried or laid on the surface. And in order to protect the wall or the pipe groove, it is very necessary to brush a protective layer outside the pipe. However, the quality problems of water supply and drainage and waterproof engineering still exist at the present stage, on one hand, due to the difference of materials and performances of wading pipes and protective coatings and the fact that part of developers are charged with the engineering protective coatings, on the other hand, due to the fact that construction modes are improper caused by lack of professional knowledge and skills, the problems of peculiar smell or water quality and the like are reported to a plurality of drinking water, and the related reports of chemical substances and carcinogens in the protective coatings are detected directly. At present, most of migration of chemical substances in the protective coating is concentrated in the food contact coating, the wading pipe is mainly concentrated in migration of organic compounds of the wading pipe, and no research on migration of chemical substances in the protective coating to the wading pipe is available.
The water quality is used as one of the final and most important indexes for evaluating water supply and drainage engineering, if the engineering quality does not reach the standard or the water quality problem is found after construction, the construction is carried out again with time and labor waste, and the water resource and resident health are caused to have the effect of being unable to be evaluated. According to molecular motion and diffusion effects, substances added in any material have the possibility of migrating to the substances or the environment which the substances are contacted with, so that a rapid detection method for migration of chemical substances in the protective coating to the immersed pipe is necessary to be established.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and innovatively provides a rapid detection method for migration of chemical substances in protective coating to a wading pipe.
In order to achieve the above purpose, the invention adopts the following technical scheme: a rapid detection method for migration of chemical substances in protective coating to a wading pipe is characterized by comprising the following steps:
(1) Preparation of sealed wading pipe
Cutting part of wading pipe, placing the wading pipe into an activated sampling pipe, sealing by adopting a plug, detecting air tightness, and standing by after the air tightness is qualified;
(2) Preparation of test piece to be tested
The test piece to be tested comprises a blank test piece and a migration test piece;
selecting part of the sealed wading pipe prepared in the step (1) as a blank test piece;
selecting part of the sealed wading pipe prepared in the step (1) as a migration test piece, wherein the migration test piece is prepared by coating protective paint on the part of the sealed wading pipe except for the plug;
(3) Migration experiment
Respectively placing the test pieces to be tested prepared in the step (2) under the same migration experiment conditions to carry out a migration experiment;
(4) Analytical detection
(4-1) performing gas chromatography-mass spectrometry on the protective coating used in the step (2);
(4-2) the test piece to be tested treated in the step (3) is tested as follows
Opening the test piece to be tested treated in the step (3), and collecting gas in a tube of the test piece to be tested for gas chromatography-mass spectrometry;
carrying out thermal desorption-gas-phase mass spectrometry on the sampling tube in the test piece tube to be tested after the treatment in the step (3);
pouring an organic solvent into the test piece to be tested treated in the step (3), repeatedly oscillating, collecting an organic solvent flushing liquid and carrying out gas chromatography-mass spectrometry analysis;
cutting a test piece to be tested which is washed by an organic solvent along the center of the inner diameter, wiping the inner surface and the outer surface by adopting an alcohol solvent and/or a ketone solvent respectively, then cutting a part between the inner wall and the outer wall, and detecting an environmental chamber, wherein the environmental chamber detection comprises the following steps:
and (3) placing the part between the inner wall and the outer wall in an environmental cabin to carry out migration experiment conditions, connecting the activated sampling tube with a gas extraction port of a constant-current sampling instrument after the migration experiment is finished, collecting gas in the environmental cabin, and carrying out thermal desorption-gas phase mass spectrometry analysis on the gas after the collection is finished.
According to the invention, by comparing the spectrograms of the migration test piece and the blank test piece, if chemical substances which are not present in the blank test piece are detected in the migration test piece, and the qualitative result of the mass spectrometer self-spectrum library is consistent with the qualitative result of the protective coating, the chemical substances in the protective coating can be judged to migrate into the wading pipe under the experimental condition.
According to some preferred aspects of the present invention, in step (1) and step (4), the sampling tube is a Tenax-Ta adsorption tube, respectively.
According to some specific and preferred aspects of the present invention, in step (1), the length of the cut wading pipe is 200mm or more.
According to some specific and preferred aspects of the present invention, in the step (2), the coating portion on the migration test piece is wrapped with aluminum foil, and the same portion as the coating portion of the migration test piece on the blank test piece is wrapped with aluminum foil. This operation may simulate certain construction schemes, namely sealing waterproof paint and the involved pipe in a closed environment.
According to the invention, in the step (3), the migration test conditions include a migration test temperature, a relative humidity and a migration test period, and further optionally include high-low temperature cycle, ultraviolet aging and artificial climate aging.
According to some preferred aspects of the invention, in step (4), the conditions of the gas chromatography-mass spectrometry analysis are:
chromatographic column: VF-1701ms; sample inlet temperature: 238-242 ℃; the split ratio is 38-42:1; carrier gas: helium with purity more than or equal to 99.999%; carrier gas flow rate: constant current mode, 0.8-1.2mL/min; programming temperature: the initial temperature is 35-45deg.C, the temperature is kept for 1-3min, the temperature is raised to 145-155 deg.C at 18-22deg.C/min, the temperature is kept for 5-7min, the temperature is raised to 255-265 deg.C at 33-37deg.C/min, and the temperature is kept for 2-4min;
ion source: an electron impact ionization (EI) source; transmission line temperature: 245-255 ℃; ion source temperature: 275-285 ℃; quadrupole temperature: 145-155 ℃; electron energy: 65-75eV; the measurement method comprises the following steps: qualitative and quantitative analysis is carried out in a retention time and mass spectrum full scanning mode; full scan range: m/z is 50-500.
According to some preferred aspects of the invention, in step (4), the thermal desorption-gas mass spectrometry conditions are:
adsorption tube: split-flow analysis is carried out, the analysis temperature is 275-285 ℃, and the temperature is kept for 6-10min;
cold hydrazine: purging time is 0.5-2min, split flow analysis is performed, low-temperature enrichment temperature is minus 25-35 ℃, heating rate Max is high Wen Jiexi temperature is 295-305 ℃, and analysis time is 2-4min;
chromatographic column: VF-1701ms; programming temperature: the initial temperature is 38-42 ℃, the temperature is kept for 3-5min, the temperature is raised to 145-155 ℃ at 12-18 ℃/min, the temperature is kept for 3-5min, the temperature is raised to 255-265 ℃ at 18-22 ℃/min, and the temperature is kept for 6-8min.
According to the invention, the protective coating commonly used in the market can be detected by adopting the specific spectrum analysis conditions, and the detection result has high accuracy and good sensitivity.
According to some specific aspects of the invention, in step (4), the organic solvent is ethyl acetate and/or methanol, the alcoholic solvent is ethanol, and the ketone solvent is acetone.
According to some specific and preferred aspects of the invention, the preparation method further comprises a detection step of migration of the protective coating from inside to outside of the wading pipe.
According to some preferred and specific aspects of the invention, the detecting step comprises: sealing one end of the wading pipe, pouring protective coating from the other end of the wading pipe, sealing, detecting air tightness after sealing, vibrating to enable the protective coating to be uniformly distributed in the wading pipe after the air tightness is qualified, then placing the wading pipe in an environment cabin for migration experiments, connecting an activated sampling pipe with a gas sampling port of a constant-current sampling instrument after the experiments are finished, collecting gas in the environment cabin, and carrying out thermal desorption-gas mass spectrometry analysis on the gas after the collection is finished. The step can simulate the migration of chemical substances in the protective coating to the wading pipe under the closed environment condition, and can provide a certain technical support for the construction of extreme environments and the development of new directions of water supply and drainage industries.
According to a specific aspect of the invention, the collection of ambient cabin gas collects 6L of ambient cabin gas at a collection rate of 200 mL/min.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the method can simulate whether chemical substances in the protective coating can migrate to the wading pipe or not under the open use environment and the traditional construction mode, and in addition, the method also provides a certain research foundation for the influence of the external coating on water quality; meanwhile, the method can simulate the migration of chemical substances in the protective coating to the wading pipe under the condition of a closed environment, and can provide a certain technical support for the construction of extreme environments and the development of new directions of water supply and drainage industries.
2. The invention can change the migration experimental conditions according to the actual conditions and simulate the actual engineering conditions to the maximum extent. If the test temperature is increased according to the time-temperature equivalent principle, the experimental period can be greatly shortened, the detection efficiency can be improved, the common period of several months in the engineering can be shortened to 14d or even lower, and the method has important significance for the quality detection and monitoring of the actual engineering; for example, the thinner is added into the protective coating according to the practical engineering construction method (when the viscosity of the coating is too high and the coating is inconvenient to be scraped in practical engineering, the thinner can be added in an amount which is not more than 10 percent of the total amount of the coating so as to facilitate construction); in addition, the method can also add high-low temperature circulation, ultraviolet aging, artificial climate aging and other treatment steps according to actual requirements.
3. The vast majority of volatile organic compounds in the protective coating are various and complex in composition, but the vast majority of volatile organic compounds are low in content, so that the invention proposes that the gas in the tube in a Tenax-TA adsorption tube collecting and transferring experiment is used for TD-MS analysis, the Tenax-TA adsorption tube has good adsorption performance, strong adsorption capacity and high sensitivity, and finally whether chemical substances are transferred can be accurately judged through thermal analysis and mass spectrometry analysis; in addition, GC-MS analysis of gas and flushing liquid in the tube and TD-MS analysis of the tube wall are added in the detection method, and the combined analysis of a plurality of positions improves the precision of the detection method.
4. The result of the migration test piece in the method is compared with the blank test piece result, and is confirmed again with the mass spectrum qualitative result of the protective coating, so that false positive results caused by systematic errors and the like are eliminated to a certain extent, and the accuracy of the detection result is ensured.
5. The method has simple operation and extremely short detection period, can accurately and reliably evaluate whether chemical substances in the protective coating migrate into the wading pipe, is favorable for selecting proper construction materials on one hand, and can place pre-control and supervision before construction on the other hand, thereby maximally guaranteeing engineering quality and wading sanitation and safety.
Drawings
FIG. 1 is a schematic diagram of an experiment for detecting outside-in migration in the detection method of the present invention;
FIG. 2 is a schematic diagram of an experiment for detecting the migration from inside to outside in the detection method of the present invention;
FIG. 3 is a total ion flow diagram of a portion of the test in example 1 of the present invention, wherein (a) the protective coating total ion flow diagram; (b) total ion flow diagram of gas in tube; (c) ethyl acetate rinse total ion flowsheet; 1: 3-ethyltoluene, 2: 2-ethyltoluene, 3:1,3, 5-trimethylbenzene;
FIG. 4 is a TD-MS spectrum of an adsorption tube in example 1 of the present invention;
FIG. 5 is a TD-MS spectrum of the pipe wall in example 1 of the present invention; 1: 3-ethyltoluene, 2: 2-ethyltoluene, 3:1,3, 5-trimethylbenzene;
FIG. 6 is a TD-MS spectrum of an adsorption tube in example 2 of the present invention; a: wading pipe 1#, b: wading pipe 2#, c: wading pipe 3#;
FIG. 7 is a TD-MS spectrum of the pipe wall in example 2 of the present invention; 1: 3-ethyltoluene, 2: 2-ethyltoluene, 3:1,3, 5-trimethylbenzene.
Detailed Description
The above-described aspects are further described below in conjunction with specific embodiments; it should be understood that these embodiments are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the scope of the following embodiments; the implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.
All starting materials are commercially available or prepared by methods conventional in the art, not specifically described in the examples below.
Example 1
This example provides a method for directing chemical substances in protective paint (Biogo-S single-component polyurethane waterproof paint, GB/T19250-2013 model S I N B in polyurethane waterproof paint) to wading pipe (wading pipe 1#, PPR hot and cold water pipe, GB/T18742.2-2017 part 2 of polypropylene pipe System for hot and cold water: S2.5 d in pipe) n 20×e n 3.4mm, available from Zhejiang pefloxacin new building materials, inc.), comprising the steps of:
(1) Preparation of sealed wading pipe
Cutting part of wading pipe (with the length of 200 mm) and placing the wading pipe into an activated Tenax-Ta adsorption pipe, adopting a plug of the same material for hot melt sealing, immersing the whole sealed wading pipe into bubble-free hot water, detecting air tightness by a hot tank bubble leakage detection method, and preparing 4 sealed wading pipes in total after the air tightness is qualified;
(2) Preparation of test piece to be tested
The test piece to be tested comprises a blank test piece and a migration test piece;
2 sealed wading pipes prepared in the step (1) are selected as blank test pieces;
selecting 2 sealed wading pipes prepared in the step (1) as migration test pieces, wherein the migration test pieces are prepared by coating protective paint on the parts except for plugs of the sealed wading pipes;
(3) Migration experiment
And (3) respectively placing the test pieces to be tested prepared in the step (2) under the same migration experiment conditions to carry out migration experiments, wherein the migration experiment conditions are as follows: uniformly coating 50g of protective coating (with reference to the actual engineering dosage of polyurethane waterproof coating, wherein the film forming thickness is about 2 mm) in plugs at two ends of a sealed wading pipe, then wrapping the sealed wading pipe by double-layer aluminum foils which are dried to constant weight, fastening two ends by iron wires, and placing the sealed wading pipe in a 50 ℃ oven for migration test, wherein the test period is 14d;
(4) Analytical detection
(4-1) performing gas chromatography-mass spectrometry on the protective coating used in the step (2);
(4-2) carrying out the following test on the test piece to be tested treated in the step (3):
after the migration experiment period is reached, a microporous electric drill can be used for rapidly drilling holes at the position of a wading pipe plug or rapidly cutting one end of the wading pipe by a cutter, then 0.5mL of gas in the pipe is extracted, and gas chromatography-mass spectrometry analysis is rapidly carried out;
quickly taking out a Tenax-TA adsorption tube in the wading tube after the gas in the tube is extracted, and carrying out thermal desorption-gas phase mass spectrometry analysis;
pouring ethyl acetate into a test piece which is subjected to migration test, repeatedly oscillating, collecting an organic solvent flushing liquid and carrying out gas chromatography-mass spectrometry analysis;
the test piece washed by ethyl acetate is cut along the center of the inner diameter, ethanol and/or acetone are respectively adopted to wipe the inner surface and the outer surface, then the part between the inner wall and the outer wall is cut and the detection of an environmental cabin is carried out, and the experimental conditions in the environmental cabin are as follows: the air exchange rate is 1 h/time, the temperature is 23+/-2 ℃, and the relative humidity is 50+/-5 percent.
The environmental chamber detection comprises the following steps:
placing the part between the inner wall and the outer wall in an environmental cabin for a migration experiment, connecting an activated Tenax-TA adsorption tube with a gas extraction port of a constant-current sampling instrument after the migration experiment is finished, collecting 6L of environmental cabin gas at a collection speed of 200mL/min, and carrying out thermal desorption-gas phase mass spectrometry analysis on the gas after the collection is finished;
wherein in the step (4), the conditions of the gas chromatography-mass spectrometry analysis are as follows:
chromatographic column: VF-1701ms (30 m. Times.0.25 mm. Times.0.25 μm); sample inlet temperature: 240 ℃; the split ratio is 40:1; carrier gas: high purity helium (purity not less than 99.999%); carrier gas flow rate: constant flow mode, 1.0mL/min; programming temperature: the initial temperature was 40℃for 2min, 20℃per min to 150℃for 6min, and 35℃per min to 260℃for 3min.
Ion source: an electron impact ionization (EI) source; transmission line temperature: 250 ℃; ion source temperature: 280 ℃; quadrupole temperature: 150 ℃; electron energy: 70eV; the measurement method comprises the following steps: qualitative and quantitative analysis is carried out in a retention time and mass spectrum full scanning mode; full scan range: m/z is 50-500;
the conditions of the thermal desorption-gas phase mass spectrometry are as follows:
adsorption tube: split-flow analysis is carried out, the analysis temperature is 280 ℃, and the split-flow analysis is kept for 8min;
cold hydrazine: purging time is 1min, split flow analysis is carried out, low-temperature enrichment temperature is minus 30 ℃, heating rate is Max, temperature is 300 ℃ higher than Wen Jiexi, and analysis time is 3min;
chromatographic column: VF-1701ms (30 m. Times.0.25 mm. Times.0.25 μm); programming temperature: the initial temperature was 40℃for 4min, 15℃per min to 150℃for 4min, and then 20℃per min to 260℃for 7min.
(5) Analysis of results
(5-1) GC-MS analysis of protective coating
After a proper amount of protective coating is dissolved in ethyl acetate, GC-MS qualitative analysis is carried out, and the total ion flow diagram is shown in fig. 3 (a). Most of the protective coating has complex components, and most of the protective coating has low chemical substance content, but the protective coating has a large variety, and the workload of taking all the components as migration objects is very large. The migration object is mainly toluene substances when the migration occurs according to the NIST (National Institute of Standard and Technology) MS Search 2.2 spectrum library of the mass spectrometer, the toluene substances are not only volatile, but also have certain harm to water and human bodies, and in order to more accurately and conveniently study the migration of chemical substances in the protective coating into the PPR tube, toluene substances with low migration temperature and harmful to the human bodies are selected as migration reference objects, and particularly three toluene substances with large peak areas (concentrations) in a spectrogram and complete separation are respectively: 3-ethyltoluene, 2-ethyltoluene, 1,3, 5-trimethylbenzene, as shown in FIGS. 3 (b) and (c), and FIG. 3 (c) is a total ion flow diagram of ethyl acetate rinse in the test piece.
(5-2) migration analysis
As can be seen from FIG. 3 and the NIST MS Search 2.2 spectrum library combined with the mass spectrometer itself, the gas in the tube and ethyl acetate rinse both detected chemical species including 3 migration references.
Fig. 4 and 5 show the TD-MS spectra of the adsorption tube and the tube wall (the portion between the inner and outer walls) in the test piece, respectively, and as can be seen from fig. 4, 5 and the NIST MS Search 2.2 spectrum library combined with the mass spectrometer itself, the chemical substances including 3 migration references were detected in the release of the adsorption tube and the tube wall.
(6) Result determination
By comparing the GC-MS spectrograms of gas and flushing liquid in the tube in the migration test piece with the GC-MS spectrograms of the part between the adsorption tube and the inner and outer walls of the blank test piece, chemical substances which are not present in the blank test piece are detected in the migration test piece, and the qualitative result of a spectrum library of the mass spectrometer is consistent with the qualitative result of the protective coating, so that the chemical substances in the protective coating can be judged to migrate into the wading tube under the experimental condition.
Example 2
Substantially the same as in example 1, the only difference is that: in wading pipe No. 1 (PPR cold and hot water pipe, GB/T18742.2-2017 section 2 of Polypropylene pipe System for Cold and Hot Water: pipe) S2.5 d n 20×e n Two wading pipes are added on the basis of 3.4mm, which are purchased from Zhejiang pessary novel building materials, inc., and are respectively wading pipe 2# (PPR cold and hot water pipe, GB/T18742.2-2017, part 2 of Polypropylene pipe System for Cold and Hot Water: s2.5 d in tubing n 20×e n 3.4mm, available from Zhejiang Zhuo Ting building materials Co., ltd.), wading pipe 3# (PPR hot and cold water pipe, GB/T18742.2-2017 part 2 of Polypropylene piping for Cold and Hot Water: s2.5 d in tubing n 20×e n 2.3mm, available from Yonggao Co., ltd.).
The specific detection results are shown in table 1, fig. 6 is a TD-MS spectrum of the adsorption tube in 3 migration test pieces, fig. 7 is a TD-MS spectrum of the tube wall, and it can be seen from table 1, fig. 6 and fig. 7 that chemical substances including 3 migration references are detected in the detection results, that is, the used protective coating can migrate into 3 wading tubes under the migration conditions.
Table 1 migration test results for different wading pipes
Note that: and the pipe wall is the part between the inner wall and the outer wall, and all the chemical substances including 3 migration references in the protective coating are detected.
In conclusion, based on whether chemical substances in the protective coating in the water supply and drainage system can migrate into the wading pipe, the invention establishes a thermal desorption/gas chromatography-mass spectrometry combined method which is easy to operate, accurate and reliable. The influence factors of migration of the protective coating to the inside of the wading pipe are more, and the situation in actual engineering is more complex, so laboratory analysis on whether chemical migration of the protective coating and the wading pipe occurs before construction is very necessary, the method can shorten the actual test time to 14d, and the method has certain application value in the aspects of actual engineering detection, safety and sanitation of wading products, use functions and the like.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (7)
1. A rapid detection method for migration of chemical substances in protective coating to a wading pipe is characterized by comprising the following steps:
(1) Preparation of sealed wading pipe
Cutting part of wading pipe, placing the wading pipe into an activated sampling pipe, sealing by adopting a plug, detecting air tightness, and standing by after the air tightness is qualified;
(2) Preparation of test piece to be tested
The test piece to be tested comprises a blank test piece and a migration test piece;
selecting part of the sealed wading pipe prepared in the step (1) as a blank test piece;
selecting part of the sealed wading pipe prepared in the step (1) as a migration test piece, wherein the migration test piece is prepared by coating protective paint on the outer surface part of the sealed wading pipe except for a plug;
(3) Migration experiment
Respectively placing the test pieces to be tested prepared in the step (2) under the same migration experiment conditions to carry out a migration experiment; the migration experiment conditions comprise migration experiment temperature, relative humidity and migration experiment period;
(4) Analytical detection
(4-1) performing gas chromatography-mass spectrometry on the protective coating used in the step (2);
(4-2) the test piece to be tested treated in the step (3) is tested as follows
Opening the test piece to be tested treated in the step (3), and collecting gas in a tube of the test piece to be tested for gas chromatography-mass spectrometry;
carrying out thermal desorption-gas phase mass spectrometry on the sampling tube in the tube of the test piece to be tested after the treatment in the step (3);
pouring an organic solvent into the test piece to be tested treated in the step (3), repeatedly oscillating, collecting an organic solvent flushing liquid and carrying out gas chromatography-mass spectrometry analysis;
the method comprises the steps of cutting a test piece to be tested after washing by an organic solvent along the center of the inner diameter, wiping the inner and outer surfaces of the test piece to be tested cut along the center of the inner diameter by adopting an alcohol solvent and/or a ketone solvent respectively, cutting a part between the inner wall and the outer wall, and detecting an environmental cabin, wherein the environmental cabin comprises the following steps:
placing the part between the inner wall and the outer wall in an environmental cabin for a migration experiment, connecting an activated sampling tube with a gas extraction port of a constant-current sampling instrument after the migration experiment is finished, collecting gas in the environmental cabin, and carrying out thermal desorption-gas phase mass spectrometry analysis on the gas after the collection is finished;
in the step (1) and the step (4), the sampling pipes are Tenax-Ta adsorption pipes respectively;
in the step (4), the conditions of the gas chromatography-mass spectrometry analysis are as follows:
chromatographic column: VF-1701ms; sample inlet temperature: 238-242 ℃; the split ratio is 38-42:1; carrier gas: helium with purity more than or equal to 99.999%; carrier gas flow rate: constant current mode, 0.8-1.2mL/min; programming temperature: the initial temperature is 35-45deg.C, the temperature is kept for 1-3min, the temperature is raised to 145-155 deg.C at 18-22deg.C/min, the temperature is kept for 5-7min, the temperature is raised to 255-265 deg.C at 33-37deg.C/min, and the temperature is kept for 2-4min;
ion source: an electron bombardment ionization source; transmission line temperature: 245-255 ℃; ion source temperature: 275-285 ℃; quadrupole temperature: 145-155 ℃; electron energy: 65-75eV; the measurement method comprises the following steps: qualitative and quantitative analysis is carried out in a retention time and mass spectrum full scanning mode; full scan range: m/z is 50-500;
in the step (4), the conditions of thermal desorption-gas phase mass spectrometry are as follows:
adsorption tube: split-flow analysis is carried out, the analysis temperature is 275-285 ℃, and the temperature is kept for 6-10min;
cold hydrazine: purging time is 0.5-2min, split flow analysis is carried out, low-temperature enrichment temperature is minus 25-35 ℃, high Wen Jiexi temperature is 295-305 ℃, and analysis time is 2-4min;
chromatographic column: VF-1701ms; programming temperature: the initial temperature is 38-42 ℃, the temperature is kept for 3-5min, the temperature is increased to 145-155 ℃ at 12-18 ℃/min, the temperature is kept for 3-5min, the temperature is increased to 255-265 ℃ at 18-22 ℃/min, and the temperature is kept for 6-8min;
by comparing the spectrograms of the migration test piece and the blank test piece, if chemical substances which are not present in the blank test piece are detected in the migration test piece, and the qualitative result of the mass spectrometer self-spectral library is consistent with the qualitative result of the protective coating, the chemical substances in the protective coating can be judged to migrate into the wading pipe under the experimental condition; wherein the chemical substances comprise 3-ethyltoluene, 2-ethyltoluene and 1,3, 5-trimethylbenzene.
2. The method for rapid detection of chemical migration into a wading pipe according to claim 1, wherein in step (1), the length of the wading pipe cut out is 200mm or more.
3. The method for rapidly detecting migration of chemical substances in protective paint to a pipe involved in water according to claim 1, wherein in the step (2), a coating part on the migration test piece is wrapped with aluminum foil, and the same part as the coating part of the migration test piece on the blank test piece is wrapped with aluminum foil.
4. The method for rapid detection of chemical migration to a pipe in question according to claim 1, wherein in step (3), the migration test conditions further include high and low temperature cycles, uv aging and artificial weathering.
5. The method for rapidly detecting the migration of chemical substances in protective paint to a pipe involved in water according to claim 1, wherein in the step (4), the organic solvent poured into the test piece to be detected after the treatment in the step (3) is ethyl acetate and/or methanol;
in the step (4), in the process of wiping the inner and outer surfaces of the test piece to be tested cut along the center of the inner diameter, the alcohol solvent is ethanol, and the ketone solvent is acetone.
6. The method for rapid detection of chemical migration into a wading pipe in accordance with claim 1, further comprising the step of detecting migration of the protective coating from inside to outside of the wading pipe.
7. The method for rapid detection of chemical migration to a pipe in question in a protective coating according to claim 6, wherein the detection step comprises: sealing one end of the wading pipe, pouring protective coating from the other end of the wading pipe, sealing, detecting air tightness after sealing, vibrating to enable the protective coating to be uniformly distributed in the wading pipe after the air tightness is qualified, then placing the wading pipe in an environment cabin for migration experiments, connecting an activated sampling pipe with a gas sampling port of a constant-current sampling instrument after the experiments are finished, collecting gas in the environment cabin, and carrying out thermal desorption-gas mass spectrometry analysis on the gas after the collection is finished.
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