CN104458145B - A kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method - Google Patents
A kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method Download PDFInfo
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- CN104458145B CN104458145B CN201410798087.1A CN201410798087A CN104458145B CN 104458145 B CN104458145 B CN 104458145B CN 201410798087 A CN201410798087 A CN 201410798087A CN 104458145 B CN104458145 B CN 104458145B
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Abstract
The invention belongs to the detection technique field of gas cylinder, specifically related to a kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method, a kind of gas cylinder inner surface cleaning filling high-purity gas proposing and quality determining method, the cleaning of gas cylinder inner surface and quality determining method include cleaning method and air-tightness detection method；Cleaning method is that the gas cylinder priority after quality testing is qualified carries out CCl4 solution cleaning, isopropanol cleaning and deionized water cleaning first to after internal grinding, then to the gas cylinder heating, drying after cleaning, installs end plug and valve after then checking；Quality testing is to carry out air-leakage test, vacuum degree measurement and profit content detection to the gas cylinder installing end plug and valve.This invention ensures that the quality of high-purity gas, greatly reduce the pollution level of gas.
Description
Technical field
The invention belongs to the detection technique field of gas cylinder is and in particular to a kind of gas cylinder inner surface filling high-purity gas cleans
And quality determining method, such gas cylinder is mainly used in filling the non-aggressive high-purity gas of more than 99.999% purity.
Background technology
With the continuous development of modern industrial technology, microelectronics, Aero-Space, biological engineering, new material, accurate smelting
The high-technology fields such as gold, environmental science constantly increase to the high-purity gas demand such as electron level gas, special gas and calibrating gas
Plus it is desirable to also constantly increase.Purity filling of high-purity gas more than 99.999% selects high pressure gas with during accumulating more at this stage
Bottle, gas cylinder internal profit content etc. has a significant impact to high-purity gas purity.When gas cylinder internal oil content is more, store oxidisability
Gas seasonal epidemic pathogens know from experience the oil reaction of gas cylinder internal, produce impact to gas purity and even explode；When gas cylinder internal moisture is more,
The etching effect of etching gas in electronic gas can be deteriorated；Therefore, it is necessary to strictly control gas cylinder internal oil, moisture, from
And purity that gas cylinder internal store gas is effectively ensured, it is to avoid gas is contaminated；Pollution in gas cylinder include infiltration, absorption with
Chemical action etc., and the bright and clean and degree of drying of gas cylinder internal, also have a direct impact to high-purity gas purity.High-purity gas are got dirty
After dye, gas purity declines, and the objectionable impurities content such as internal particle, moisture increases so as to become substandard product.Therefore, it is
Ensure the purity of high-purity gas, need gas cylinder inner surface to be carried out process and the inner surface quality of gas cylinder is effectively examined
Survey.
Content of the invention
For solving above-mentioned technical problem, it is an object of the invention to provide a kind of gas cylinder inner surface cleaning filling high-purity gas
And air-tightness detection method.
The present invention is to complete above-mentioned purpose to adopt the following technical scheme that：
A kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method, described gas cylinder inner surface cleaning and matter
Quantity measuring method includes cleaning method and air-tightness detection method；
The comprising the following steps that of described cleaning method：
1）Gas cylinder after qualified to the grinding of gas cylinder inner surface quality checks, confirms that gas cylinder inner surface does not exist and does not grind
The defect of area, oil stain, moisture and corrosion, such as gas cylinder inner surface existing defects, again gas cylinder inner surface is ground, until gas
It is qualified that bottle inner surface quality grinds；
2）CCl4 solution cleans：It is filled with the CCl4 solution being not less than gas cylinder volume 3/5 to gas cylinder internal, with rear enclosed gas cylinder
Two ends, after making gas cylinder horizontally rotate 1.5～2.5h, the CCl4 solution of gas cylinder internal are toppled over totally, are removed in gas cylinder with reaching
The purpose of portion's oil；
3）Isopropanol cleans：It is not less than to completing after the cleaning of CCl4 solution and not having to be filled with the gas cylinder that CCl4 solution remains
The isopropanol of gas cylinder volume 3/5, with rear enclosed gas cylinder two ends, after making gas cylinder horizontally rotate 1.5～2.5h, gas cylinder internal is different
Propanol is toppled over totally, to reach the purpose removing gas cylinder internal remaining oil, CCl4 solution；
4）Deionized water cleans：To complete isopropanol cleaning after and do not have aqueous isopropanol residual gas cylinder in be filled with not low
In the deionized water of gas cylinder volume 1/3, and add inorganic inhibitor, inorganic inhibition in every liter of deionized water in deionized water
The addition of agent is 3g, in order to prevent or to slow down gas cylinder corrosion；With rear enclosed gas cylinder two ends, gas cylinder is made to horizontally rotate 1～1.5h
Afterwards, the deionized water of gas cylinder internal is toppled over totally；And collect deionized water solution in toppling process, and oil therein is contained
Measure and detected whether related request is met with the oil content determining gas cylinder internal；
5）Heating, drying：Gas cylinder outer wall is heated, heating-up temperature is 110～150 DEG C, it is set to 3.5 heat time heating time～
5.5h, is filled with high pure nitrogen to gas cylinder internal in heating process, and carries out multiple evacuation process, completes backward gas cylinder internal
It is passed through high pure nitrogen；
6）Inspection：After being filled with the gas cylinder placement 20～40min of high pure nitrogen, extract a certain amount of gas in gas cylinder, to gas
Oil in body, water content are detected；When the content of Oil in circulating gas is not higher than 0.6ppm, water content is not higher than 2ppm and is conjunction
Lattice；Next process can be carried out, detection is unqualified, re-starts process, till detection is qualified after detection is qualified；
7）End plug and valve are installed：End plug and valve are installed on checking qualified gas cylinder.
The method carrying out quality testing to the gas cylinder after above-mentioned installation, described quality testing includes air-leakage test, true
Reciprocal of duty cycle detection and profit content detection；It comprises the following steps that：
1）Air-leakage test：
A, it is that 0.0015 inch of clearance gauge detects to the distance between cylinder port and end plug, with preliminary using thickness
Determine the sealing between gas cylinder and end plug, thus carrying out preliminary leak rate test；If detection is unqualified, re-start installation, with
Prop up gas cylinder to carry out scrapping process after disqualified upon inspection twice；
B, to gas cylinder internal charged pressure be 0.2～0.6MPa high pure nitrogen and high-purity helium gaseous mixture, High Purity Nitrogen
The weight of gas and high-purity helium is than for 15:1；Subsequently select Helium leak detector adopt suction gun method to cylinder port and end plug junction,
End plug is detected with the leak rate of valve junction；
C, the high pure nitrogen pouring gas cylinder operating pressure to gas cylinder internal carry out gas cylinder air-leakage test；To gas cylinder system
Carry out sealing propertytest qualified after, next process can be carried out, such as detect unqualified, then need again to process, until inspection close
Next process is proceeded to after lattice；
2）, dry evacuation：After air-leakage test is qualified, release the gas of gas cylinder internal, be subsequently charged with the height of 0.3MPa
Pure nitrogen gas, heat to gas cylinder outer wall after placing 2h, and heating carries out evacuation process simultaneously, until gas cylinder internal vacuum reaches
To index request；
3）, profit content detection：After the completion of drying evacuation process, it is filled with the high pure nitrogen of 0.2MPa to gas cylinder internal,
Detect the profit content in gas cylinder and in original high pure nitrogen after placing 12h respectively, and determine its numerical value whether in indication range
Within, if meeting index of correlation, product is qualified.
A kind of gas cylinder inner surface cleaning filling high-purity gas proposed by the present invention and air-tightness detection method, through this
Ming and Qing wash and quality testing after gas cylinder inner surface oil, water content and sealing meet related request；Meanwhile, gas cylinder is made to meet interior
Surface oil, water content are satisfied by filling the requirement of the high-purity gas that purity is not less than 99.999%, and sealing well waits and requires, and protect
Demonstrate,prove the quality of high-purity gas, greatly reduce the pollution level of gas.
Specific embodiment
In conjunction with specific embodiments the present invention is illustrated：
A kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method, described gas cylinder inner surface cleaning and matter
Quantity measuring method includes cleaning method and air-tightness detection method；
The comprising the following steps that of described cleaning method：
1）Gas cylinder after qualified to the grinding of gas cylinder inner surface quality checks, confirms that gas cylinder inner surface does not exist and does not grind
The defect of area, oil stain, moisture and corrosion, such as gas cylinder inner surface existing defects, again gas cylinder inner surface is ground, until gas
It is qualified that bottle inner surface quality grinds；
2）CCl4 solution cleans：It is filled with the CCl4 solution being not less than gas cylinder volume 3/5 to gas cylinder internal, with rear enclosed gas
Bottle two ends, after making gas cylinder horizontally rotate 1.5～2.5h, the CCl4 solution of gas cylinder internal are toppled over totally, to reach removing gas cylinder
The purpose of internal oil；
3）Isopropanol cleans：It is not less than to completing after the cleaning of CCl4 solution and not having to be filled with the gas cylinder that CCl4 solution remains
The isopropanol of gas cylinder volume 3/5, with rear enclosed gas cylinder two ends, after making gas cylinder horizontally rotate 1.5～2.5h, gas cylinder internal is different
Propanol is toppled over totally, to reach the purpose removing gas cylinder internal remaining oil, CCl4 solution；
4）Deionized water cleans：To complete isopropanol cleaning after and do not have aqueous isopropanol residual gas cylinder in be filled with not low
In the deionized water of gas cylinder volume 1/3, and add inorganic inhibitor, inorganic inhibition in every liter of deionized water in deionized water
The addition of agent is 3g, in order to prevent or to slow down gas cylinder corrosion；With rear enclosed gas cylinder two ends, gas cylinder is made to horizontally rotate 1～1.5h
Afterwards, the deionized water of gas cylinder internal is toppled over totally；And collect deionized water solution in toppling process, and oil therein is contained
Measure and detected whether related request is met with the oil content determining gas cylinder internal；
5）Heating, drying：Gas cylinder outer wall is heated, heating-up temperature is 110～150 DEG C, it is set to 3.5 heat time heating time～
5.5h, is filled with high pure nitrogen to gas cylinder internal in heating process, and carries out multiple evacuation process, completes backward gas cylinder internal
It is passed through high pure nitrogen；
6）Inspection：After being filled with the gas cylinder placement 20～40min of high pure nitrogen, extract a certain amount of gas in gas cylinder, to gas
Oil in body, water content are detected；When the content of Oil in circulating gas is not higher than 0.6ppm, water content is not higher than 2ppm and is conjunction
Lattice；Next process can be carried out, detection is unqualified, re-starts process, till detection is qualified after detection is qualified；
7）End plug and valve are installed：End plug and valve are installed on checking qualified gas cylinder.
The method carrying out quality testing to the gas cylinder after above-mentioned installation, described quality testing includes air-leakage test, true
Reciprocal of duty cycle detection and profit content detection；It comprises the following steps that：
1）Air-leakage test：
A, it is that 0.0015 inch of clearance gauge detects to the distance between cylinder port and end plug, with preliminary using thickness
Determine the sealing between gas cylinder and end plug, thus carrying out preliminary leak rate test；If detection is unqualified, re-start installation, with
Prop up gas cylinder to carry out scrapping process after disqualified upon inspection twice；
B, to gas cylinder internal charged pressure be 0.2～0.6MPa high pure nitrogen and high-purity helium gaseous mixture, High Purity Nitrogen
The weight of gas and high-purity helium is than for 15:1；Subsequently select Helium leak detector adopt suction gun method to cylinder port and end plug junction,
End plug is detected with the leak rate of valve junction；
C, the high pure nitrogen pouring gas cylinder operating pressure to gas cylinder internal carry out gas cylinder air-leakage test；To gas cylinder system
Carry out sealing propertytest qualified after, next process can be carried out, such as detect unqualified, then need again to process, until inspection close
Next process is proceeded to after lattice；
2）, dry evacuation：After air-leakage test is qualified, release the gas of gas cylinder internal, be subsequently charged with the height of 0.3MPa
Pure nitrogen gas, heat to gas cylinder outer wall after placing 2h, and heating carries out evacuation process simultaneously, until gas cylinder internal vacuum reaches
To index request；
3), profit content detection：After the completion of drying evacuation process, it is filled with the high pure nitrogen of 0.2MPa to gas cylinder internal,
Detect the profit content in gas cylinder and in original high pure nitrogen after placing 12h respectively, and determine its numerical value whether in indication range
Within, if meeting index of correlation, product is qualified.
Claims (1)
1. a kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method it is characterised in that：Table in described gas cylinder
Face cleaning and quality determining method include cleaning method and quality determining method；
The comprising the following steps that of described cleaning method：
1）To gas cylinder inner surface quality grind qualified after gas cylinder check, confirm gas cylinder inner surface do not exist non-milling zone,
The defect of oil stain, moisture and corrosion, such as gas cylinder inner surface existing defects, again gas cylinder inner surface is ground, until gas cylinder
It is qualified that inner surface quality grinds；
2）CCl4 solution cleans：It is filled with the CCl4 solution being not less than gas cylinder volume 3/5 to gas cylinder internal, with rear enclosed gas cylinder two
End, after making gas cylinder horizontally rotate 1.5～2.5h, the CCl4 solution of gas cylinder internal is toppled over totally, to reach removing gas cylinder internal
The purpose of oil；
3）Isopropanol cleans：It is not less than gas cylinder to completing after the cleaning of CCl4 solution and not having to be filled with the gas cylinder that CCl4 solution remains
The isopropanol of volume 3/5, with rear enclosed gas cylinder two ends, after making gas cylinder horizontally rotate 1.5～2.5h, by the isopropanol of gas cylinder internal
Topple over clean, to reach the purpose removing gas cylinder internal remaining oil, CCl4 solution；
4）Deionized water cleans：It is not less than gas to completing after isopropanol cleaning and not having to be filled with the gas cylinder that aqueous isopropanol remains
The deionized water of bottle volume 1/3, and add inorganic inhibitor, inorganic inhibitor in every liter of deionized water in deionized water
Addition is 3g, in order to prevent or to slow down gas cylinder corrosion；With rear enclosed gas cylinder two ends, after making gas cylinder horizontally rotate 1～1.5h, will
The deionized water of gas cylinder internal is toppled over totally；And collect deionized water solution in toppling process, and oil content therein is entered
Whether row detection, meet related request with the oil content determining gas cylinder internal；
5）Heating, drying：Gas cylinder outer wall is heated, heating-up temperature is 110～150 DEG C, and heat time heating time is set to 3.5～5.5h,
It is filled with high pure nitrogen to gas cylinder internal in heating process, and carries out multiple evacuation process, complete backward gas cylinder internal and be passed through
High pure nitrogen；
6）Inspection：After being filled with the gas cylinder placement 20～40min of high pure nitrogen, extract a certain amount of gas in gas cylinder, in gas
Oil, water content detected；When the content of Oil in circulating gas is not higher than 0.6ppm, it is as qualified that water content is not higher than 2ppm；Inspection
Next process can be carried out, detection is unqualified, re-starts process, till detection is qualified after survey is qualified；
7）End plug and valve are installed：End plug and valve are installed on checking qualified gas cylinder；
The method carrying out quality testing to the gas cylinder after above-mentioned installation, described quality testing includes air-leakage test, vacuum
Detection and profit content detection；It comprises the following steps that：
1）Air-leakage test：
A, it is that 0.0015 inch of clearance gauge detects to the distance between cylinder port and end plug, to primarily determine that using thickness
Sealing between gas cylinder and end plug, thus carry out preliminary leak rate test；If detection is unqualified, re-start installation, with a gas
Bottle carries out scrapping process after disqualified upon inspection twice；
B, to gas cylinder internal charged pressure be 0.2～0.6MPa high pure nitrogen and high-purity helium gaseous mixture, high pure nitrogen with
The weight of high-purity helium is than for 15:1；Helium leak detector is subsequently selected to adopt suction gun method to cylinder port and end plug junction, end plug
Detected with the leak rate of valve junction；
C, the high pure nitrogen pouring gas cylinder operating pressure to gas cylinder internal carry out gas cylinder air-leakage test；Gas cylinder system is carried out
After sealing propertytest is qualified, next process can be carried out, such as detect unqualified, then need again to process, until after the assay was approved
Proceed to next process；
2）, dry evacuation：After air-leakage test is qualified, release the gas of gas cylinder internal, be subsequently charged with the High Purity Nitrogen of 0.3MPa
Gas, heats to gas cylinder outer wall after placing 2h, and heating carries out evacuation process simultaneously, until gas cylinder internal vacuum reaches finger
Mark requires；
3）, profit content detection：After the completion of drying evacuation process, it is filled with the high pure nitrogen of 0.2MPa to gas cylinder internal, place
Detect the profit content in gas cylinder and in original high pure nitrogen after 12h respectively, and determine its numerical value whether within indication range,
If meeting index of correlation, product is qualified.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105499229B (en) * | 2015-11-27 | 2017-08-25 | 洛阳双瑞特种装备有限公司 | A kind of high-pressure bottle inner surface oil removing water-eliminating method and detection method |
| CN106180097B (en) * | 2016-07-22 | 2018-06-01 | 洛阳双瑞特种装备有限公司 | A kind of oil removing clean method for filling gases at high pressure gas cylinder inner surface |
| CN106153275A (en) * | 2016-08-18 | 2016-11-23 | 洛阳双瑞特种装备有限公司 | A kind of gas pressure vessel air-leakage test and helium leak test method |
| KR102012795B1 (en) * | 2018-03-07 | 2019-11-04 | 주식회사 엔케이 | Cylinder assembly method for ultra-high purity gas filling |
| CN108687574B (en) * | 2018-05-31 | 2020-12-08 | 苏州金宏气体股份有限公司 | High-purity gas steel cylinder treatment process |
| CN109290318A (en) * | 2018-08-14 | 2019-02-01 | 新兴能源装备股份有限公司 | A kind of container inner wall method for cleaning |
| CN111974773B (en) * | 2019-05-23 | 2022-04-12 | 中国科学院大连化学物理研究所 | Method for cleaning air bag for collecting exhaled air |
| CN111469042A (en) * | 2020-04-16 | 2020-07-31 | 浙江西亚特电子材料有限公司 | Gas cylinder processing system and processing method for ultrapure gas |
| CN111715642A (en) * | 2020-07-02 | 2020-09-29 | 重庆凯益特种气体有限公司 | Gas cylinder cleaning method |
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| TW503123B (en) * | 2000-09-08 | 2002-09-21 | Boc Group Inc | Plasma drying and passivation of compressed gas cylinders |
| CN100549227C (en) * | 2008-04-01 | 2009-10-14 | 南京特种气体厂有限公司 | A kind of method for processing internal wall of ultrapure silane gas cylinder |
| CN101922004A (en) * | 2010-08-20 | 2010-12-22 | 南京特种气体厂有限公司 | Method for treating inner wall of high-pressure seamless steel gas cylinder |
| CN102218705B (en) * | 2011-04-01 | 2012-10-31 | 苏州金宏气体股份有限公司 | Treatment method of gas cylinder used for storing electronic grade ultra-pure gas |
| CN202438906U (en) * | 2012-02-07 | 2012-09-19 | 南京特种气体厂有限公司 | Automatic device for treating inner wall of steel gas cylinder used for containing ultra-pure silane |
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Address after: 471000, Binhe Road, hi tech Development Zone, Henan, Luoyang, 32 Patentee after: CSSC Shuangrui (Luoyang) special equipment Co.,Ltd. Address before: 471000, Binhe Road, hi tech Development Zone, Henan, Luoyang, 32 Patentee before: LUOYANG SUNRUI SPECIAL EQUIPMENT Co.,Ltd. |
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