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CN202903751U - Simple and easy ultraviolet aging box capable of adsorbing volatile organisms in polymer sample - Google Patents

Simple and easy ultraviolet aging box capable of adsorbing volatile organisms in polymer sample Download PDF

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CN202903751U
CN202903751U CN 201220594735 CN201220594735U CN202903751U CN 202903751 U CN202903751 U CN 202903751U CN 201220594735 CN201220594735 CN 201220594735 CN 201220594735 U CN201220594735 U CN 201220594735U CN 202903751 U CN202903751 U CN 202903751U
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adsorption tube
sample chamber
sample
aging
volatile organic
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杜振霞
孙姝琦
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱,包括,老化箱箱体(1),样品室(2),紫外灯(3),吸附管(4),空气泵(5);老化箱箱体(1)内设置有用于放置样品(9)的样品室(2),在样品室(2)的顶部设有有用于对样品室内的样品(9)进行紫外老化的紫外灯(3);用于吸附并富集样品(9)在紫外老化过程中产生的挥发性有机物的吸附管(4)插入至样品室(2)中,吸附管(4)通过软管(8)与空气泵(5)相连。本实用新型可以在设定的温度和时间下采用紫外灯辐照聚合物样品,模拟在紫外线辐照下的老化情况,吸附管收集样品中的挥发性有机物,用于热解析-气质联用分析,测试样品在紫外线辐照下产生的挥发性有机物。

Figure 201220594735

A simple UV aging box that can absorb volatile organic compounds in polymer samples, including aging box body (1), sample chamber (2), UV lamp (3), adsorption tube (4), air pump (5) ; A sample chamber (2) for placing samples (9) is arranged inside the aging box (1), and an ultraviolet lamp for ultraviolet aging of samples (9) in the sample chamber is provided on the top of the sample chamber (2) (3); The adsorption tube (4) used to absorb and enrich the volatile organic compounds produced during the UV aging process of the sample (9) is inserted into the sample chamber (2), and the adsorption tube (4) passes through the hose (8) Connect to air pump (5). The utility model can use ultraviolet lamps to irradiate polymer samples at a set temperature and time to simulate the aging situation under ultraviolet radiation, and the adsorption tube collects volatile organic compounds in the samples for thermal analysis-gas chromatography analysis , to test the volatile organic compounds produced by the sample under ultraviolet irradiation.

Figure 201220594735

Description

一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱A Simple UV Aging Chamber for Adsorbing Volatile Organic Compounds in Polymer Samples

技术领域technical field

本实用新型涉及化学仪器技术领域,更具体地涉及一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱。The utility model relates to the technical field of chemical instruments, in particular to a simple ultraviolet aging box capable of absorbing volatile organic compounds in polymer samples.

背景技术Background technique

老化是聚合物材料的自然特性之一,是其合成、改性和应用中的一项重要指标。聚合物材料的老化受光、热、氧和湿度等气候因素的综合影响,但由于自然暴露试验耗时较长,且无法精确控制各种因素对材料的影响程度,因此,科研工作者们开发出各种人工加速老化试验方法来研究聚合物材料的老化机理。其中,紫外灯老化试验加速倍率高,可以在较短的时间内获得材料的耐老化性能,是常用的高分子材料人工加速老化试验方法之一。Aging is one of the natural characteristics of polymer materials and an important indicator in its synthesis, modification and application. The aging of polymer materials is affected by climate factors such as light, heat, oxygen and humidity. However, due to the long time-consuming natural exposure test and the inability to accurately control the influence of various factors on materials, researchers have developed Various artificial accelerated aging test methods are used to study the aging mechanism of polymer materials. Among them, the ultraviolet lamp aging test has a high acceleration rate and can obtain the aging resistance of the material in a relatively short period of time. It is one of the commonly used artificial accelerated aging test methods for polymer materials.

热解析法也称为热脱附法,是在一定温度下通过载气对样品管或吸附管进行吹扫,使挥发和半挥发物从样品或吸附剂上脱附下来,在载气的作用下富集于冷阱,再通过瞬间加热冷阱进样后用于色谱分析。热解析法是一种近年来新兴的针对样品中挥发和半挥发性有机物的检测方法。热解析与气相色谱或气相色谱-质谱联用,在环境监测、材料测试、食品风味研究等方面有着广阔的应用。The thermal analysis method is also called the thermal desorption method. The sample tube or the adsorption tube is purged by the carrier gas at a certain temperature, so that the volatile and semi-volatile substances are desorbed from the sample or the adsorbent. It is enriched in the cold trap, and then injected into the cold trap by instantaneous heating for chromatographic analysis. Thermal analysis method is a new detection method for volatile and semi-volatile organic compounds in samples in recent years. Thermal analysis coupled with gas chromatography or gas chromatography-mass spectrometry has broad applications in environmental monitoring, material testing, and food flavor research.

发明内容Contents of the invention

本实用新型要解决的技术问题:The technical problem to be solved by the utility model:

为了克服现有技术中紫外辐照耐候性实验中不便收集聚合物样品中产生的挥发性有机物的问题,本实用新型提供了一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱,该老化箱能够模拟环境、材料等多类型样品中聚合物在紫外光辐照下的老化过程,并对过程中产生的挥发性有机物进行吸附和富集,使其能够对老化过程中产生的挥发性有机物进行分析测试。In order to overcome the problem of inconvenient collection of volatile organic compounds produced in polymer samples in the ultraviolet radiation weather resistance test in the prior art, the utility model provides a simple ultraviolet aging box that can absorb volatile organic compounds in polymer samples. The aging box can simulate the aging process of polymers in various types of samples such as environment and materials under ultraviolet light irradiation, and can absorb and enrich the volatile organic compounds produced in the process, so that it can absorb the volatile organic compounds produced in the aging process. Organic matter was analyzed for testing.

本实用新型的产品技术方案是:Product technical scheme of the present utility model is:

一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱,主要部件包括,老化箱箱体1,样品室2,紫外灯3,吸附管4,空气泵5;在老化箱箱体1内设置有用于放置样品9的样品室2,在样品室2的顶部设有有用于对样品室内的样品9进行紫外老化的紫外灯3;用于吸附并富集样品9在紫外老化过程中产生的挥发性有机物的吸附管4插入至样品室2中,吸附管4通过软管8与空气泵5相连。A simple ultraviolet aging box that can absorb volatile organic compounds in polymer samples, the main components include: aging box body 1, sample chamber 2, ultraviolet lamp 3, adsorption tube 4, air pump 5; inside the aging box body 1 A sample chamber 2 for placing the sample 9 is provided, and the top of the sample chamber 2 is provided with an ultraviolet lamp 3 for carrying out ultraviolet aging to the sample 9 in the sample chamber; An adsorption tube 4 for volatile organic compounds is inserted into the sample chamber 2 , and the adsorption tube 4 is connected to an air pump 5 through a hose 8 .

本实用新型设计的简易紫外老化箱,还设置有用于控制老化时间和老化温度的时间控制装置6和温度控制装置7。其中,时间控制装置6的控制端分别与空气泵5和温度控制装置7相连,与空气泵5相连是用于控制空气泵抽气时间,即吸附管循环吸附时间;与温度控制装置7相连是用于控制样品室加热时间。温度控制装置7的控制端与样品室2相连,用于控制样品室加热温度。The simple ultraviolet aging box designed by the utility model is also provided with a time control device 6 and a temperature control device 7 for controlling the aging time and aging temperature. Wherein, the control end of time control device 6 is connected with air pump 5 and temperature control device 7 respectively, is connected with air pump 5 and is used for controlling the air pumping time of air pump, i.e. adsorption tube cycle adsorption time; Used to control the heating time of the sample chamber. The control end of the temperature control device 7 is connected to the sample chamber 2 for controlling the heating temperature of the sample chamber.

吸附管4为商品吸附管,或添加了吸附剂的自制吸附管。The adsorption tube 4 is a commercial adsorption tube, or a self-made adsorption tube added with an adsorbent.

所述的空气泵5还带有流量控制装置。The air pump 5 also has a flow control device.

应用本实用新型进行老化实验的方法如下:Apply the utility model to carry out the method for aging test as follows:

第一步,应用老化箱对聚合物样品进行紫外老化实验,使用吸附管吸附聚合物样品在老化过程中产生的挥发性有机物。The first step is to use the aging box to carry out ultraviolet aging experiments on the polymer samples, and use the adsorption tube to absorb the volatile organic compounds produced during the aging process of the polymer samples.

将聚合物样品放置在样品室中,打开紫外灯电源,同时,打开温度控制和时间控制装置,使用Tenax吸附管吸附老化过程中某一时间段聚合物产品在辐照过程中产生的挥发性有机物。Place the polymer sample in the sample chamber, turn on the power of the UV lamp, and at the same time, turn on the temperature control and time control devices, and use the Tenax adsorption tube to absorb the volatile organic compounds produced by the polymer product during the irradiation process for a certain period of time during the aging process .

第二步,气相色谱-质谱联用仪测试。The second step is gas chromatography-mass spectrometry test.

将采样后的吸附管放入热解析仪中加热,使脱附出来的挥发性有机物富集于热解析冷阱,瞬间高温加热冷阱,应用气相色谱或气质联用仪进行检测。Put the sampled adsorption tube into the thermal desorption instrument to heat, so that the desorbed volatile organic compounds are enriched in the thermal desorption cold trap, and the cold trap is heated at a high temperature instantaneously, and detected by gas chromatography or mass spectrometry.

气相色谱-质谱联用检测条件为:电子轰击电离源,毛细管色谱柱,恒温或程序升温。Gas chromatography-mass spectrometry detection conditions are: electron bombardment ionization source, capillary chromatographic column, constant temperature or programmed temperature rise.

本实用新型的有益效果是:The beneficial effects of the utility model are:

本实用新型能够高选择性地从多种聚合物样品中吸附和富集紫外老化过程中产生的挥发性有机物,通过热解析仪-气相色谱仪或热解析仪-气相色谱-质谱联用仪能够更加准确的测定样品中挥发性有机物的含量。The utility model can adsorb and enrich the volatile organic compounds produced in the ultraviolet aging process from various polymer samples with high selectivity, and the thermal desorption instrument-gas chromatograph or the thermal analyser-gas chromatography-mass spectrometer can More accurate determination of the content of volatile organic compounds in the sample.

附图说明Description of drawings

图1是可吸附聚合物样品中挥发性有机物的简易紫外老化箱结构示意图。Figure 1 is a schematic diagram of the structure of a simple UV aging chamber that can absorb volatile organic compounds in polymer samples.

图2是使用商品化Tenax吸附管吸附的60℃下、紫外光照24h的聚丙烯样品产生的挥发性有机物热解析-气质联用总离子流色谱图。Figure 2 is a thermal analysis-GC-GC chromatogram of volatile organic compounds produced by a polypropylene sample adsorbed at 60°C and exposed to ultraviolet light for 24 hours using a commercial Tenax adsorption tube.

图中,1老化箱箱体,2样品室,3紫外灯,4吸附管,5空气泵,6时间控制装置,7温度控制装置,8软管,9样品。In the figure, 1 aging box body, 2 sample chamber, 3 ultraviolet lamp, 4 adsorption tube, 5 air pump, 6 time control device, 7 temperature control device, 8 hose, 9 sample.

具体实施方式Detailed ways

实施例Example

(一)本实用新型的产品技术方案(1) Product technical solution of the utility model

结合图1所示,本实用新型的产品技术方案如下:In conjunction with shown in Figure 1, the technical product scheme of the utility model is as follows:

一种可吸附聚合物样品中挥发性有机物的简易紫外老化箱,包括老化箱箱体1,样品室2,紫外灯3,吸附管4,空气泵5,时间控制装置6,温度控制装置7。A simple ultraviolet aging box capable of absorbing volatile organic compounds in polymer samples, comprising an aging box body 1, a sample chamber 2, an ultraviolet lamp 3, an adsorption tube 4, an air pump 5, a time control device 6, and a temperature control device 7.

所述的老化箱箱体中,样品室2用于盛放样品9,紫外灯3用于产生紫外线辐照在样品上,时间控制装置6用于控制老化时间,温度控制装置7用于控制老化温度,在老化过程中,使用吸附管4吸附并富集样品产生的挥发性有机物,并通过空气泵5控制循环吸附的气流流速大小。吸附管4通过软管8与空气泵5相连。In the aging box, the sample chamber 2 is used to hold the sample 9, the ultraviolet lamp 3 is used to generate ultraviolet radiation on the sample, the time control device 6 is used to control the aging time, and the temperature control device 7 is used to control the aging time. During the aging process, the adsorption tube 4 is used to absorb and enrich the volatile organic compounds produced by the sample, and the air pump 5 is used to control the flow rate of the circulating adsorption air. The adsorption pipe 4 is connected with the air pump 5 through a hose 8 .

(二)本实用新型的应用方法技术方案(2) The technical scheme of the application method of the present utility model

(1)应用老化箱对聚合物样品进行老化实验,使用吸附管吸附聚合物样品在老化过程中产生的挥发性有机物。(1) Use an aging box to carry out aging experiments on polymer samples, and use adsorption tubes to absorb volatile organic compounds produced during the aging process of polymer samples.

使用前,将商品化的Tenax吸附管在350℃下老化15min,以去除其在空气中吸附的杂质。将老化后的Tenax吸附管安装到老化箱吸附管接口处。Before use, the commercial Tenax adsorption tube was aged at 350 °C for 15 min to remove the impurities adsorbed in the air. Install the aged Tenax adsorption tube to the interface of the aging box adsorption tube.

将100g聚丙烯样品放置在样品室中,打开紫外灯电源,同时打开温度控制和时间控制装置,设定温度为60℃。当时间控制装置显示老化24h后,使用Tenax吸附管吸附此时样品室内聚丙烯产品在辐照过程中产生的挥发性有机物。Place 100 g of polypropylene samples in the sample chamber, turn on the power of the ultraviolet lamp, and at the same time turn on the temperature control and time control devices, and set the temperature to 60°C. When the time control device shows aging for 24 hours, use the Tenax adsorption tube to absorb the volatile organic compounds produced by the polypropylene product in the sample chamber during the irradiation process.

(2)热解析-气质联用的测试(2) Thermal Desorption-Gas Chromatography Test

将Tenax吸附管取下,通过热解析-气质联用仪测试挥发性有机物。检测结果的总离子流色谱图如图2所示。The Tenax adsorption tube was removed, and the volatile organic compounds were tested by thermal desorption-mass spectrometer. The total ion current chromatogram of the detection results is shown in Figure 2.

在本实施例中,热解析-气质联用仪主要检测参数如下:In this embodiment, the main detection parameters of the thermal desorption-mass spectrometer are as follows:

仪器:英国Marks公司热解析仪,美国Agilent公司7890A-5975C气质联用仪。Instruments: thermal desorption instrument from Marks Company in the UK, 7890A-5975C gas spectrometer from Agilent Company in the United States.

热解析条件:脱附温度90℃,脱附时间5min,传输线温度200℃,冷阱温度-25℃,280℃解析。Thermal analysis conditions: desorption temperature 90°C, desorption time 5min, transfer line temperature 200°C, cold trap temperature -25°C, analysis at 280°C.

气相色谱条件:色谱柱HP-5MS(30m×0.25mm×0.25μm),程序升温,35℃保持5min,5℃/min升至200℃,保持5min。传输线温度200℃。载气He,流速1.0mL/min。Gas chromatography conditions: chromatographic column HP-5MS (30m×0.25mm×0.25μm), programmed temperature rise, 35°C for 5 minutes, 5°C/min to 200°C, and hold for 5 minutes. Transfer line temperature 200°C. Carrier gas He, flow rate 1.0mL/min.

质谱条件:电子轰击电离源,电子能量70eV,源温230℃,全扫描采集模式,质量范围40~500amu。Mass spectrometry conditions: electron bombardment ionization source, electron energy 70eV, source temperature 230°C, full scan acquisition mode, mass range 40~500amu.

Claims (4)

1. the simple and easy ultraviolet ageing case of volatile organic matter in the adsorbable polymer samples, critical piece comprises, ageing oven casing (1), sample chamber (2), uviol lamp (3), adsorption tube (4), pneumatic pump (5); It is characterized in that: be provided with in ageing oven casing (1) for the sample chamber (2) of placing sample (9), the top of (2) is provided with and is useful on the uviol lamp (3) that the sample in the sample chamber (9) is carried out ultraviolet ageing in the sample chamber; Be used for absorption and enriched sample (9) and be inserted in the sample chamber (2) at the adsorption tube (4) of the volatile organic matter that the ultraviolet ageing process produces, adsorption tube (4) links to each other with pneumatic pump (5) by flexible pipe (8).
2. simple and easy ultraviolet ageing case according to claim 1 is characterized in that: it also is provided with time-controlling arrangement (6) and temperature control equipment (7) for control digestion time and aging temperature; Wherein, the control end of time-controlling arrangement (6) links to each other with temperature control equipment (7) with pneumatic pump (5) respectively, and linking to each other with pneumatic pump (5) is to bleed the time for the control pneumatic pump, i.e. the adsorption tube circulation absorption time; Link to each other with temperature control equipment (7) is for Quality control chamber heat time heating time; The control end of temperature control equipment (7) links to each other with sample chamber (2), is used for Quality control chamber heating-up temperature.
3. simple and easy ultraviolet ageing case according to claim 1, it is characterized in that: adsorption tube (4) is the commodity adsorption tube, or has added the self-control adsorption tube of adsorbent.
4. simple and easy ultraviolet ageing case according to claim 1, it is characterized in that: described pneumatic pump (5) is also with volume control device.
CN 201220594735 2012-11-13 2012-11-13 Simple and easy ultraviolet aging box capable of adsorbing volatile organisms in polymer sample Expired - Fee Related CN202903751U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103335893A (en) * 2013-06-14 2013-10-02 哈尔滨工业大学 Resin asphalt ultraviolet aging testing equipment and testing method thereof
CN107490526A (en) * 2017-09-06 2017-12-19 中国工程物理研究院核物理与化学研究所 Macromolecule material aging effect the cannot-harm-detection device and its detection method
CN111157440A (en) * 2020-01-23 2020-05-15 北京市理化分析测试中心 Aging test chamber and test method capable of integrating the collection of aging products of polymer materials
CN113687056A (en) * 2021-07-28 2021-11-23 清华大学深圳国际研究生院 Device and method for simulating the release and real-time collection of harmful substances in plastic products

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103335893A (en) * 2013-06-14 2013-10-02 哈尔滨工业大学 Resin asphalt ultraviolet aging testing equipment and testing method thereof
CN107490526A (en) * 2017-09-06 2017-12-19 中国工程物理研究院核物理与化学研究所 Macromolecule material aging effect the cannot-harm-detection device and its detection method
CN107490526B (en) * 2017-09-06 2023-08-22 中国工程物理研究院核物理与化学研究所 Nondestructive testing device and method for aging effect of high polymer material
CN111157440A (en) * 2020-01-23 2020-05-15 北京市理化分析测试中心 Aging test chamber and test method capable of integrating the collection of aging products of polymer materials
CN111157440B (en) * 2020-01-23 2024-12-03 北京市理化分析测试中心 Aging test chamber and test method capable of integrating and collecting aging products of polymer materials
CN113687056A (en) * 2021-07-28 2021-11-23 清华大学深圳国际研究生院 Device and method for simulating the release and real-time collection of harmful substances in plastic products

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