CN111781241A - Liquid self-ignition point test sample injection device and application thereof - Google Patents

Liquid self-ignition point test sample injection device and application thereof Download PDF

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Publication number
CN111781241A
CN111781241A CN201910269681.4A CN201910269681A CN111781241A CN 111781241 A CN111781241 A CN 111781241A CN 201910269681 A CN201910269681 A CN 201910269681A CN 111781241 A CN111781241 A CN 111781241A
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sample
liquid
detection chamber
sample injection
injector
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CN201910269681.4A
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Chinese (zh)
Inventor
王双全
张*
厉鹏
张会光
吴保意
郭璐
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Chemical Registration Center Of Emergency Management Department
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Chemical Registration Center Of Emergency Management Department
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/50Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility
    • G01N25/52Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility by determining flash-point of liquids

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

The invention relates to a liquid self-ignition point test sample injection device and application thereof, and mainly solves the problems that in the prior art, the sample injection amount is not easy to control, the sample injection position is not fixed, whether sample injection is successful or not is not determined, the test result judgment is not accurate, and the repeatability is poor. The invention solves the problems well by adopting the technical scheme that the liquid auto-ignition point testing sample injection device is adopted, the sample injection bracket is connected with the main body of the liquid auto-ignition point testing device, one end of the sample injector is connected with the horizontal bracket of the sample injection bracket, the other end of the sample injector extends into the detection chamber, the detection chamber is positioned in the main body of the liquid auto-ignition point testing device, and the temperature control module is arranged around the detection chamber.

Description

Liquid self-ignition point test sample injection device and application thereof
Technical Field
The invention relates to a liquid spontaneous ignition point test sample injection device and application thereof.
Background
The liquid self-ignition point is an important index for evaluating the fire risk of liquid compounds. The standard for testing the liquid spontaneous combustion point at present comprises GB/T21791 & lt 2008 & gt petroleum product spontaneous combustion temperature test method, GB/T21860 & lt 2008 & gt liquid chemical spontaneous combustion temperature test method, ASTM E659-2015 & lt test method for liquid chemical spontaneous combustion temperature, EC440-2008 A.15 spontaneous combustion temperature (liquid), and the test steps are as follows: 1 uniformly heating a detection chamber to a preset temperature; 2 adding a proper amount of sample into the detection chamber by using a syringe (liquid) or a funnel (solid); 3 observing whether the sample is burnt or not in a dark environment. According to the method that the injector or the funnel for the auto ignition point test directly adds samples to the combustion chamber at present, the sample introduction process cannot be seen, and due to the fact that the viscosities of chemicals to be tested are different, the sample introduction amount is not controlled well, the sample introduction position is not fixed, and whether sample introduction is successful or not is not determined (whether a sample is dropped or not, and the dropping position is not determined well). The test result judgment is inaccurate, the repeatability is poor, and the experiment efficiency is low due to repeated rechecking.
Disclosure of Invention
One of the technical problems to be solved by the invention is that the sample injection amount is not easy to control, the sample injection position is not fixed, whether the sample injection is successful or not is not determined, the test result is not accurate, and the repeatability is poor in the prior art, and the novel liquid autoignition point test sample injection device has the advantages of good sample injection amount control, fixed sample injection position, successful sample injection or not, accurate test result judgment, and good repeatability. The second technical problem to be solved by the present invention is to provide a use of the sample injection device for testing the self-ignition point of liquid corresponding to the first technical problem to be solved.
In order to solve one of the problems, the technical scheme adopted by the invention is as follows: a liquid spontaneous ignition test sampling device is characterized in that a sampling support is connected with a liquid spontaneous ignition test device main body, one end of a sampler is connected with a horizontal support of the sampling support, the other end of the sampler extends into a detection chamber, the detection chamber is located in the liquid spontaneous ignition test device main body, and a temperature control module is arranged around the detection chamber.
In the technical scheme, preferably, the sample injector can move up and down under the action of the sample injection support, and the moving distance can be controlled.
Among the above-mentioned technical scheme, preferably, can dismantle between injector and the kind support.
In the above technical solution, preferably, the up-and-down movement of the sample injector is realized by the up-and-down movement of the horizontal support on the vertical support.
In the above technical solution, preferably, the horizontal support is fixed at the top end of the vertical support, and the up-and-down movement of the sample injector is realized by driving the sample injector to move up and down by the connecting part of the horizontal support and the sample injector.
In the above technical solution, preferably, the up-and-down movement of the sample injector is controlled by a program of a liquid auto-ignition tester to realize automation.
In the above technical solution, preferably, the lower end of the sample injector extending into the detection chamber is provided with a medicine spoon.
In the above technical solution, preferably, when the liquid self-ignition point is tested, the sample to be tested is carried by the spoon at the lower end of the sample injector and enters the detection chamber with a predetermined temperature for testing.
In order to solve the second problem, the invention adopts the following technical scheme: the application of the liquid autoignition point test sampling device is used in the liquid autoignition point test.
The sampling device and the sampling method can enable the sampling process of the liquid spontaneous ignition point test to be more intuitive, the sampling amount is accurate and controllable, the sampling position is fixed, the repeatability is good, the test efficiency and the accuracy can be improved, and a better technical effect is obtained.
Drawings
FIG. 1 is a schematic view of the structure of the device of the present invention.
In fig. 1, 1 sample injector, 2 sample injection support, 3 temperature control module, 4 detection chamber.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
A liquid spontaneous ignition test sampling device is shown in figure 1, a sampling support is connected with a main body of the liquid spontaneous ignition test device, one end of a sample injector is connected with a horizontal support of the sampling support, the other end of the sample injector extends into a detection chamber, the detection chamber is located in the main body of the liquid spontaneous ignition test device, and a temperature control module is arranged around the detection chamber. The sample injector can move up and down under the action of the sample injection support, the moving distance can be controlled, and the sample injector and the sample injection support can be detached. The up-and-down movement of the sample injector is realized by the up-and-down movement of the horizontal bracket on the vertical bracket. The up-and-down movement of the sample injector is controlled by the program of the liquid auto-ignition point tester to realize automation. When the liquid is tested, the sample to be tested is carried by the medicine spoon at the lower end of the sample injector and enters the detection chamber with preset temperature for testing
The specific test comprises the following steps:
first, preparation phase
1. Cleaning a detection chamber, a temperature sensor, a sample injector and an observation mirror of the liquid spontaneous ignition point testing device, and adjusting the height of the sample injector to a proper height.
2. The detection chamber is thermostated at a predetermined temperature for at least 5 minutes.
Second, testing stage
1. And adding a certain amount of liquid or solid sample into the spoon of the sample injector, starting a sample injection program, and automatically entering the preset position of the detection chamber by the spoon at the lower end of the sample injector under the drive of the sample injector.
2. The sample that had been added to the test chamber at the predetermined temperature was observed in the dark for 10 minutes, or until spontaneous combustion occurred.
3. An air purge procedure is initiated to purge the detection chamber.
4. And (5) withdrawing the sample injector, and replacing and cleaning.
5. The next temperature point is set and thermostated for at least 5 minutes and the next test is started.
6. The test was run at 3 ℃ until the sample did not spontaneously ignite at a certain temperature, and was confirmed at least 3 times. This temperature is the self-ignition point of the sample.
[ example 2 ]
A liquid spontaneous ignition test sampling device is shown in figure 1, a sampling support is connected with a main body of the liquid spontaneous ignition test device, one end of a sample injector is connected with a horizontal support of the sampling support, the other end of the sample injector extends into a detection chamber, the detection chamber is located in the main body of the liquid spontaneous ignition test device, and a temperature control module is arranged around the detection chamber. The sample injector can move up and down under the action of the sample injection support, the moving distance can be controlled, and the sample injector and the sample injection support can be detached. The horizontal support is fixed on the top end of the vertical support, and the sample injector moves up and down by the up-and-down movement of the horizontal support and the sample injector driven by the connecting part of the horizontal support and the sample injector. The up-and-down movement of the sample injector is controlled by the program of the liquid auto-ignition point tester to realize automation. When the liquid is tested, the sample to be tested is carried by the medicine spoon at the lower end of the sample injector and enters the detection chamber with preset temperature for testing
The specific test comprises the following steps:
first, preparation phase
1. Cleaning a detection chamber, a temperature sensor, a sample injector and an observation mirror of the liquid spontaneous ignition point testing device, and adjusting the height of the sample injector to a proper height.
2. The detection chamber is thermostated at a predetermined temperature for at least 5 minutes.
Second, testing stage
1. And adding a certain amount of liquid or solid sample into the spoon of the sample injector, starting a sample injection program, and automatically entering the preset position of the detection chamber by the spoon at the lower end of the sample injector under the drive of the sample injector.
2. The sample that had been added to the test chamber at the predetermined temperature was observed in the dark for 10 minutes, or until spontaneous combustion occurred.
3. An air purge procedure is initiated to purge the detection chamber.
4. And (5) withdrawing the sample injector, and replacing and cleaning.
5. The next temperature point is set and thermostated for at least 5 minutes and the next test is started.
6. The test was run at 3 ℃ until the sample did not spontaneously ignite at a certain temperature, and was confirmed at least 3 times. This temperature is the self-ignition point of the sample.
[ example 3 ]
The acrylic primer liquid was tested for its self-ignition point under the conditions and procedures described in example 2.
1. Cleaning a detection chamber, a temperature sensor, a sample injector and an observation mirror of the liquid spontaneous ignition point testing device, and adjusting the height of the sample injector to a proper height.
2. The detection chamber was thermostated at 400 ℃ for 10 minutes.
3. And adding a certain amount of acrylic primer into the spoon of the sample injector, starting a sample injection program, and automatically feeding the spoon at the lower end of the sample injector into a preset position of the detection chamber under the drive of the sample injector.
4. The sample that had been added to the test chamber at the predetermined temperature was observed in the dark for 10 minutes without spontaneous combustion.
5. An air purge procedure is initiated to purge the detection chamber.
6. And (5) withdrawing the sample injector, and replacing and cleaning.
7. The test chamber was set to thermostatted at 430 ℃ for 10 minutes and the next test started without spontaneous combustion.
8. The procedure of 3-6 steps was repeated and the test was carried out at 460 ℃ with spontaneous combustion occurring.
9. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
10. The procedure of 3-6 steps was repeated and the test was carried out at 448 ℃ with spontaneous combustion occurring.
11. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
12. The procedure of 3-6 steps was repeated and the test was carried out at 448 ℃ with spontaneous combustion occurring.
13. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
The acrylic primer liquid was determined to have an auto-ignition point of 448 ℃.
[ COMPARATIVE EXAMPLE ]
If the injector described in this patent is not used, the injector is used for injecting. Example 3 was repeated to test the self-ignition point of the acrylic primer liquid.
1. Cleaning a detection chamber, a temperature sensor, a sample injector and an observation mirror of the liquid spontaneous ignition point testing device, and adjusting the height of the sample injector to a proper height.
2. The detection chamber was thermostated at 400 ℃ for 10 minutes.
3. A syringe is used to introduce a quantity of sample into the detection chamber. (in the process, a lot of uncertainty exists, 1, after a syringe sucks a viscous acrylic primer sample, the sample is injected into a dark and invisible detection chamber, the sample injection amount is not controlled well, 2, the dropping position of the sample is not controlled well, and the repeated injection is needed for a plurality of times to ensure the accuracy of the test result, 3, a tester ensures that the position of a needle head of the syringe can be seen in the sample injection process and is not hurt by the sudden explosion.)
4. The sample that had been added to the test chamber at the predetermined temperature was observed in the dark for 10 minutes without spontaneous combustion.
5. An air purge procedure is initiated to purge the detection chamber.
6. The temperature was maintained at 400 ℃ for 10 minutes, and a repeat of the test was carried out. (one temperature point will be tested at least twice because of the longer constant temperature time, about 15-30 minutes.)
7. The detection chamber is kept at the constant temperature of 430 ℃ for 10 minutes, and 3-6 steps are repeated to carry out the next test, so that spontaneous combustion does not occur.
8. The procedure of 3-6 steps was repeated and the test was carried out at 460 ℃ with spontaneous combustion occurring.
9. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
10. The procedure of 3-6 steps was repeated and the test was carried out at 448 ℃ with spontaneous combustion occurring.
11. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
12. The procedure of 3-6 steps was repeated and the test was carried out at 448 ℃ with spontaneous combustion occurring.
13. The procedure of 3-6 steps was repeated and the test was carried out at 445 ℃ without spontaneous combustion.
The acrylic primer liquid was determined to have an auto-ignition point of 448 ℃.
Compared with the prior injector for direct sample injection, the sample injection device disclosed by the invention has the following advantages:
1. the sampling amount is accurate, the sampling position is accurate, repeated tests are reduced, and the time can be saved by 40%.
2. When the sample is injected, the tester does not need to be entangled too close to the injection port for danger, and the two choices which are too far from the sample injection port are unclear, so that the operation of the tester is more leisurely.

Claims (10)

1. A liquid spontaneous ignition test sampling device is characterized in that a sampling support is connected with a liquid spontaneous ignition test device main body, one end of a sampler is connected with a horizontal support of the sampling support, the other end of the sampler extends into a detection chamber, the detection chamber is located in the liquid spontaneous ignition test device main body, and a temperature control module is arranged around the detection chamber.
2. The device for testing the auto ignition point of liquid according to claim 1, wherein the sample injector can move up and down under the action of the sample injection support, and the moving distance can be controlled.
3. The device according to claim 1, wherein the sample injector is detachable from the sample holder.
4. The device for testing the autoignition point of liquid according to claim 1, wherein the up and down movement of the sample injector is achieved by moving a horizontal support up and down on a vertical support.
5. The device according to claim 1, wherein the horizontal support is fixed at the top end of the vertical support.
6. The device according to claim 1, wherein the up and down movement of the sample injector is controlled by the program of the liquid auto-ignition tester to be automated.
7. The device according to claim 1, wherein a spoon is provided at the lower end of the sample injector extending into the detection chamber.
8. The device according to claim 7, wherein the liquid is tested by loading the sample to be tested into the testing chamber with a predetermined temperature from a spoon at the lower end of the injector.
9. The device for testing the auto ignition point of liquid sample as claimed in claim 1, wherein the up-and-down movement of the sample injector is achieved by driving the sample injector to move up and down by the connection part of the horizontal bracket and the sample injector.
10. A liquid autoignition point testing sample injection device according to claims 1-9, for use in liquid autoignition point testing.
CN201910269681.4A 2019-04-04 2019-04-04 Liquid self-ignition point test sample injection device and application thereof Pending CN111781241A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09304311A (en) * 1996-05-09 1997-11-28 Shimadzu Corp Spontaneous ignition testing device
CN201096736Y (en) * 2007-11-13 2008-08-06 冯俊博 Fully automatic self-ignition point tester
CN201555673U (en) * 2009-11-25 2010-08-18 中国石油天然气集团公司 Automatic sampling device for ignition temperature test of flammable liquids
CN102175719A (en) * 2011-01-10 2011-09-07 王利兵 CCD visualization self-ignition point tester
CN202256210U (en) * 2011-09-27 2012-05-30 浙江省化工研究院有限公司 Selfignition temperature tester
CN205038183U (en) * 2015-10-20 2016-02-17 中国石油化工股份有限公司 Liquid self -ignition point survey device
CN106404824A (en) * 2016-11-10 2017-02-15 上海市计量测试技术研究院 Solid spontaneous ignition point tester

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09304311A (en) * 1996-05-09 1997-11-28 Shimadzu Corp Spontaneous ignition testing device
CN201096736Y (en) * 2007-11-13 2008-08-06 冯俊博 Fully automatic self-ignition point tester
CN201555673U (en) * 2009-11-25 2010-08-18 中国石油天然气集团公司 Automatic sampling device for ignition temperature test of flammable liquids
CN102175719A (en) * 2011-01-10 2011-09-07 王利兵 CCD visualization self-ignition point tester
CN202256210U (en) * 2011-09-27 2012-05-30 浙江省化工研究院有限公司 Selfignition temperature tester
CN205038183U (en) * 2015-10-20 2016-02-17 中国石油化工股份有限公司 Liquid self -ignition point survey device
CN106404824A (en) * 2016-11-10 2017-02-15 上海市计量测试技术研究院 Solid spontaneous ignition point tester

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
霍明甲等: "智能化系统在自燃温度测试中的设计和应用", 《安全、健康和环境》 *

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