CN111398209A - Infrared spectrum method for measuring polyvinyl chloride content in hard polyvinyl chloride pipe - Google Patents
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- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 70
- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 14
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 28
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 238000011002 quantification Methods 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 238000004611 spectroscopical analysis Methods 0.000 claims 3
- 238000004458 analytical method Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000357 carcinogen Toxicity 0.000 description 2
- 239000003183 carcinogenic agent Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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Abstract
The invention discloses an infrared spectrum method for measuring polyvinyl chloride content in a rigid polyvinyl chloride pipe, which comprises the steps of measuring infrared spectrograms of a standard sample and a sample to be measured by using a Fourier transform infrared spectrometer with an ATR accessory, drawing a standard curve according to the relation between the peak ratio of a polyvinyl chloride characteristic absorption peak to a calcium carbonate characteristic absorption peak in the infrared spectrogram of the standard sample and the polyvinyl chloride content, and realizing rapid quantification of the sample to be measured through the standard curve. The invention has the advantages of little sample consumption, simple sample preparation and pretreatment, no reagent or consumable consumption basically, environmental protection and energy saving. The method can quickly and accurately realize the measurement of the content of the polyvinyl chloride (PVC) in the hard polyvinyl chloride (PVC-U) pipe and the pipe fitting. The method can reduce the time consumption of polyvinyl chloride content analysis from about 8 hours to about 10 minutes of the traditional chemical method, greatly improve the analysis speed and improve the working efficiency.
Description
Technical Field
The invention belongs to the technical field of infrared spectrum quantitative detection of polyvinyl chloride plastic pipe component analysis, and particularly relates to an infrared spectrum method for rapidly and accurately determining the content of polyvinyl chloride (PVC) in a rigid polyvinyl chloride (PVC-U) pipe and a pipe fitting.
Background
Rigid polyvinyl chloride (PVC-U) pipes and pipe fittings are widely used in drainage works of buildings, highways and railways. Particularly, with the rapid development of high-speed rails in China, the rigid polyvinyl chloride pipes and pipe fittings are widely used in the construction of drainage engineering of the high-speed rails. Polyvinyl chloride is a main component of rigid polyvinyl chloride pipes and pipe fittings, the content of the polyvinyl chloride is an important factor determining the performance of the pipes and the pipe fittings, in order to save cost, too much inorganic filler such as calcium carbonate is added into the product, so that the content of the polyvinyl chloride is too low, the physical properties such as impact resistance of the product are greatly reduced, and the long-term durability is adversely affected.
At present, the national standard GB/T20221-.
However, the methods for measuring the content of polyvinyl chloride in the rigid polyvinyl chloride pipes and the pipes related to the current domestic and foreign documents and standards are all traditional chemical methods such as gravimetric methods, volumetric methods and the like. Wherein, toxic carcinogenic tetrahydrofuran is used as an extraction solvent for the pretreatment of gravimetric samples, and a large amount of organic waste liquid is generated in the extraction process; the volumetric method can generate strong carcinogen dioxin during combustion and absorption of a sample, nitric acid is needed for acidification before titration, and the method does not accord with the development concept of green, health and environmental protection. And the analysis time of one sample in the traditional chemical method is more than 8 hours, the efficiency is too low, and time and labor are wasted.
Disclosure of Invention
The invention aims to provide an infrared spectrum method for rapidly and accurately measuring the content of polyvinyl chloride in rigid polyvinyl chloride pipes and pipe fittings aiming at the defects in the prior art. The invention is a brand new method for realizing quantitative analysis of the content of polyvinyl chloride in the hard polyvinyl chloride pipe and the pipe fitting by using the infrared spectroscopy, and compared with the traditional chemical method, the method has the advantages of small sample consumption, simple sample preparation and pretreatment, no reagent or consumable consumption, environmental protection and energy saving; and the analysis speed is high.
The object of the invention can be achieved by the following technical measures:
the infrared spectrum method for measuring the content of polyvinyl chloride in the rigid polyvinyl chloride pipe comprises the following steps: the method comprises the following steps of directly measuring infrared spectrograms of a standard sample and a test sample by using an ATR accessory, drawing a standard curve according to the relation between the peak height ratio of a polyvinyl chloride characteristic absorption peak to a calcium carbonate characteristic absorption peak in the infrared spectrogram of the standard sample and the content of polyvinyl chloride, and realizing rapid quantification of the sample to be measured through the standard curve, wherein the method comprises the following steps:
a. sample preparation:
preparing standard pipe samples with polyvinyl chloride contents of 50%, 60%, 70%, 80% and 90%, respectively, cutting the standard samples with different polyvinyl chloride contents and the pipe samples to be tested into slices with the thickness controlled to be less than or equal to 0.5mm, wiping the surfaces with alcohol, and airing for later use;
b. sequentially placing standard pipe samples on an ATR sample table, pressing a pressure head to ensure that the samples are fully contacted with ATR crystals, and respectively collecting infrared spectrograms of the standard samples with different contents;
c. establishing a standard working curve by taking the polyvinyl chloride content of the standard pipe sample as a vertical coordinate according to the obtained infrared spectrogram of the standard pipe sample and taking the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak as a horizontal coordinate;
d. b, placing the pipe sample to be detected obtained in the step a on an ATR sample table, pressing a pressure head tightly, and collecting an infrared spectrogram of the sample to be detected; and calculating the polyvinyl chloride content of the sample on the working curve according to the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak in the spectrogram of the pipe sample to be detected within the same wave number range as the standard pipe sample.
Further, the ATR crystal of the present invention is a diamond crystal.
In the invention, when the infrared spectrum is collected, the parameters of the infrared spectrometer are set as the collection wave number range: 4000cm-1To 400cm-1(ii) a Resolution 4cm-1(ii) a Diaphragm: 100.
the infrared spectrum method quantitative analysis standard working curve is in a wave number range of 1220cm-1To 1285cm-1The maximum peak height and wave number range of polyvinyl chloride characteristic peak is 855cm-1To 890cm-1And establishing a standard working curve by taking the maximum peak height ratio of the characteristic peak of the calcium carbonate as the abscissa and the polyvinyl chloride content of the standard sample as the ordinate.
The principle and the beneficial effects of the invention are as follows:
the determination method does not need to use toxic and harmful organic solvents such as tetrahydrofuran and the like to extract the sample, and does not generate organic waste liquid; the sample does not need to be burnt, and carcinogens such as dioxin and the like are not generated; strong acid and strong alkali such as potassium hydroxide and nitric acid are not needed; the analysis process is green, safe and pollution-free; meanwhile, the whole analysis process only takes about 10 minutes, the operation is simple and convenient, and the analysis efficiency is greatly improved compared with the traditional method. The polyvinyl chloride content of the polyvinyl chloride pipe measured by the method is 50-90%, and the method is accurate and reliable in analysis result and easy to popularize.
The test results of the detection by the invention are as follows:
(1) the linear correlation coefficient of the standard working curve detected by the invention is 0.99986.
(2) The accuracy and precision of the detection by the invention are shown in Table 1
TABLE 1
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention will be further described below with reference to the accompanying drawings:
the infrared spectrum method for rapidly and accurately measuring the content of polyvinyl chloride (PVC) in the hard polyvinyl chloride (PVC-U) pipe and the pipe fitting comprises the following steps: directly measuring infrared spectrograms of a standard sample and a test sample by using an ATR accessory, drawing a standard curve according to the relation between the peak height ratio of a polyvinyl chloride characteristic absorption peak to a calcium carbonate characteristic absorption peak in the infrared spectrogram of the standard sample and the content of polyvinyl chloride, and realizing the rapid quantification of the sample to be measured by the standard curve, wherein the method comprises the following steps (see figure 1):
a. sample preparation:
preparing standard pipe samples with polyvinyl chloride contents of 50%, 60%, 70%, 80% and 90%, respectively, cutting the standard samples with different polyvinyl chloride contents and the pipe samples to be tested into slices with the thickness controlled to be less than or equal to 0.5mm, wiping the surfaces with alcohol, and airing for later use;
b. sequentially placing standard pipe samples on an ATR sample table, pressing a pressure head to ensure that the samples are fully contacted with ATR crystals, and respectively collecting infrared spectrograms of the standard samples with different contents;
c. establishing a standard working curve by taking the polyvinyl chloride content of the standard pipe sample as a vertical coordinate according to the obtained infrared spectrogram of the standard pipe sample and taking the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak as a horizontal coordinate;
d. b, placing the pipe sample to be detected obtained in the step a on an ATR sample table, pressing a pressure head tightly, and collecting an infrared spectrogram of the sample to be detected; and calculating the polyvinyl chloride content of the sample on the working curve according to the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak in the spectrogram of the pipe sample to be detected within the same wave number range as the standard pipe sample.
Further, the ATR crystal of the present invention is a diamond crystal.
In the invention, when the infrared spectrum is collected, the parameters of the infrared spectrometer are set as the collection wave number range: 4000cm-1To 400cm-1(ii) a Resolution 4cm-1(ii) a Diaphragm: 100.
the infrared spectrum method quantitative analysis standard working curve is in a wave number range of 1220cm-1To 1285cm-1The maximum peak height and wave number range of polyvinyl chloride characteristic peak is 855cm-1To 890cm-1And establishing a standard working curve by taking the maximum peak height ratio of the characteristic peak of the calcium carbonate as the abscissa and the polyvinyl chloride content of the standard sample as the ordinate.
Claims (4)
1. An infrared spectrum method for measuring the content of polyvinyl chloride in a rigid polyvinyl chloride pipe is characterized by comprising the following steps: the method comprises the following steps of directly measuring infrared spectrograms of a standard sample and a test sample by using an ATR accessory, drawing a standard curve according to the relation between the peak height ratio of a polyvinyl chloride characteristic absorption peak to a calcium carbonate characteristic absorption peak in the infrared spectrogram of the standard sample and the content of polyvinyl chloride, and realizing rapid quantification of the sample to be measured through the standard curve, wherein the method comprises the following steps:
a. sample preparation: preparing standard pipe samples with polyvinyl chloride contents of 50%, 60%, 70%, 80% and 90%, respectively, cutting the standard samples with different polyvinyl chloride contents and the pipe samples to be tested into slices with the thickness controlled to be less than or equal to 0.5mm, wiping the surfaces with alcohol, and airing for later use;
b. sequentially placing standard pipe samples on an ATR sample table, pressing a pressure head to ensure that the samples are fully contacted with ATR crystals, and respectively collecting infrared spectrograms of the standard samples with different contents;
c. establishing a standard working curve by taking the polyvinyl chloride content of the standard pipe sample as a vertical coordinate according to the obtained infrared spectrogram of the standard pipe sample and taking the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak as a horizontal coordinate;
d. b, placing the pipe sample to be detected obtained in the step a on an ATR sample table, pressing a pressure head tightly, and collecting an infrared spectrogram of the sample to be detected; and calculating the polyvinyl chloride content of the sample on the working curve according to the ratio of the maximum peak height of the polyvinyl chloride characteristic peak to the maximum peak height of the calcium carbonate characteristic peak in the spectrogram of the pipe sample to be detected within the same wave number range as the standard pipe sample.
2. The infrared spectroscopic method for determining the polyvinyl chloride content in rigid polyvinyl chloride tubing as set forth in claim 1, wherein: the ATR crystal is a diamond crystal.
3. The infrared spectroscopic method for determining the polyvinyl chloride content in rigid polyvinyl chloride tubing as set forth in claim 1, wherein: when the infrared spectrum is collected, the parameters of the infrared spectrometer are set as the collection wave number range: 4000cm-1To 400cm-1(ii) a Resolution 4cm-1(ii) a Diaphragm: 100.
4. the infrared spectroscopic method for determining the polyvinyl chloride content in rigid polyvinyl chloride tubing as set forth in claim 1, wherein: in the wave number range 1220cm-1To 1285cm-1The maximum peak height and wave number range of polyvinyl chloride characteristic peak is 855cm-1To 890cm-1And establishing a standard working curve by taking the maximum peak height ratio of the characteristic peak of the calcium carbonate as the abscissa and the polyvinyl chloride content of the standard sample as the ordinate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113075155A (en) * | 2021-02-22 | 2021-07-06 | 青岛中化新材料实验室检测技术有限公司 | Infrared spectrum method for measuring content of polyvinyl chloride in polyvinyl chloride pipe |
| CN114280002A (en) * | 2021-12-16 | 2022-04-05 | 宜宾五粮液股份有限公司 | Abnormal fermented grain spectrum screening method based on characteristic peak determination |
| CN115343248A (en) * | 2022-06-24 | 2022-11-15 | 航天科工防御技术研究试验中心 | Semi-quantitative analysis method for plasticizer content in nitrile rubber by infrared spectroscopy |
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| CN115343248A (en) * | 2022-06-24 | 2022-11-15 | 航天科工防御技术研究试验中心 | Semi-quantitative analysis method for plasticizer content in nitrile rubber by infrared spectroscopy |
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