CN106226149A - A kind of preparation method of nitrogenous mixed active calibrating gas - Google Patents
A kind of preparation method of nitrogenous mixed active calibrating gas Download PDFInfo
- Publication number
- CN106226149A CN106226149A CN201610624372.0A CN201610624372A CN106226149A CN 106226149 A CN106226149 A CN 106226149A CN 201610624372 A CN201610624372 A CN 201610624372A CN 106226149 A CN106226149 A CN 106226149A
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- Prior art keywords
- gas
- preparation
- mixed active
- cylinder
- calibrating gas
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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
- G01N1/38—Diluting, dispersing or mixing samples
Abstract
The invention discloses the preparation method of a kind of nitrogenous mixed active calibrating gas, the method comprises the steps of: step 1, to treat that gas filling bottle accesses standard mixture charging device, open cylinder valve, in bottle, it is filled with the nitrogenous mixed active calibrating gas higher than finished product predetermined concentration, to 0.5 3MPa, closes cylinder valve;Step 2, takes off gas cylinder, stands 48 96h;Step 3, is vented gas cylinder, and evacuation 3 15 minutes;Step 4, closes vacuum pumping valve, opens filling valve, be filled with the nitrogenous mixed active calibrating gas higher than finished product predetermined concentration;Step 5, is filled with High Purity Nitrogen in proportion so that treat that the nitrogenous mixed active calibrating gas in gas filling bottle reaches predetermined concentration;Step 6, closes charging device and cylinder valve, takes off gas cylinder, and preparation completes.The preparation method that the present invention provides is used for preparing nitrogenous mixed active calibrating gas, and the production cycle is greatly shortened, and is shortened to 1 week by average 2 weeks, operates easier, and preparation technology more specification, Consumer's Experience is more preferable.
Description
Technical field
The present invention relates to the preparation technology of a kind of normal mixture body, it particularly relates to a kind of nitrogenous mixed active mark
The preparation method of quasi-gas.
Background technology
The safety equipment that hydrogen sulfide detector is important when being mud logging operation, inspection shaft operation.In nitrogen, hydrogen sulfide standard gas is
It is used for hydrogen sulfide detector is calibrated, it is ensured that detector normally works.But in preparing nitrogen during hydrogen sulfide standard gas, by
Often there is absorption and desorption phenomenon in hydrogen sulfide molecule with gas cylinder inwall, cause the stability of the calibrating gas made with uniform
Property decline.Manufacturer, in order to ensure stablizing of exfactory inspection data, needs repeatedly to test, extends the production cycle.User makes
During with, also the instability of factor value can cause the deviation measured.
Summary of the invention
It is an object of the invention to provide a kind of passivation technology, use in certain density nitrogen hydrogen sulfide mixed gas to fill waiting
Gas cylinder stands a period of time so that bottle wall reaches saturated to the absorption of hydrogen sulfide, prepares sulfur in nitrogen by user's requirement the most again
Change hydrogen calibrating gas, stability, uniformity, accuracy can be greatly enhanced, moreover it is possible to shorten the production cycle, meet client's need
Ask.
For reaching above-mentioned purpose, the invention provides the preparation method of a kind of nitrogenous mixed active calibrating gas, the method
Comprise the steps of:
Step 1, will treat that gas filling bottle accesses standard mixture charging device, open cylinder valve, and be filled with and make a reservation for higher than finished product in bottle
The nitrogenous mixed active calibrating gas of concentration, closes cylinder valve to 0.5-3MPa;
Step 2, takes off gas cylinder, stands 48-96h;
Step 3, is vented gas cylinder, and evacuation 3-15 minute;
Step 4, closes vacuum pumping valve, opens filling valve, be filled with the nitrogenous mixed active calibrating gas higher than finished product predetermined concentration;
Step 5, is filled with High Purity Nitrogen in proportion so that treat that the nitrogenous mixed active calibrating gas in gas filling bottle reaches predetermined concentration;
Step 6, closes charging device and cylinder valve, takes off gas cylinder, and preparation completes.
Preferably, described nitrogenous mixed active calibrating gas refers to fluohydric acid gas mark in hydrogen sulfide standard gas in nitrogen, nitrogen
Any one in ammonia calibrating gas in hydrogen chloride calibrating gas, nitrogen in quasi-gas, nitrogen.
Preferably, in step 1, described treats that gas filling bottle is preprocessed.Described pretreatment refers to, makes to treat that gas filling bottle is 80
DEG C high-temperature baking, evacuation 16 ~ 24 hours.
Nitrogenous mixed active calibrating gas preferably above finished product predetermined concentration refers to that its concentration is product predetermined concentration
10-15 times;It is more preferably 10 times.
Preferably, in step 1, it is filled with and closes to 1Mpa higher than the nitrogenous mixed active calibrating gas of finished product predetermined concentration
Cylinder valve.
Preferably, in step 2, stand 72h.
Preferably, in step 3, emptying gas cylinder refers to this being treated, gas filling bottle accesses the emptying of standard mixture charging device.
Preferably, in step 3, evacuation 3 minutes.
What the present invention provided prepares hydrogen sulfide standard gas in nitrogen with passivation technology and has the following technical effect that
1. shorten the production cycle.When using traditional method, average time is 2 weeks, and after using passivation technology instead, average time shortens
It it is 1 week.
2. simplify operation.Traditional method needs repeatedly to access charging device and carries out weighing operation, repeatedly accesses analytical tool
Carry out detection operation, the most only need to once weigh operation after using passivation technology and one-time detection operates.
3. preparation technology more specification.Traditional method relys more on the experience of operator, and skilled operator may weight
Replicate standby can completing for 2 times, but perhaps unskilled operator to repeat to prepare 4,5 times just can complete.Use passivation technology
After, as long as technological operation according to the rules, can prepare for 1 time.
4. customer satisfaction improves.When using traditional method, the customer satisfaction of this product is 90%, uses passivation technology
After, customer satisfaction brings up to 98%.
Detailed description of the invention
The invention provides the preparation method of a kind of nitrogenous mixed active calibrating gas, the method comprises the steps of:
Step 1, will treat that gas filling bottle accesses standard mixture charging device, open cylinder valve, and be filled with and make a reservation for higher than finished product in bottle
The nitrogenous mixed active calibrating gas of concentration, closes cylinder valve to 0.5-3MPa;
Step 2, takes off gas cylinder, stands 48-96h;
Step 3, is vented gas cylinder, and evacuation 3-15 minute;
Step 4, closes vacuum pumping valve, opens filling valve, be filled with the nitrogenous mixed active calibrating gas higher than finished product predetermined concentration;
Step 5, is filled with High Purity Nitrogen in proportion so that treat that the nitrogenous mixed active calibrating gas in gas filling bottle reaches predetermined concentration;
Step 6, closes charging device and cylinder valve, takes off gas cylinder, and preparation completes.
Described nitrogenous mixed active calibrating gas refer to fluohydric acid gas calibrating gas in hydrogen sulfide standard gas in nitrogen, nitrogen,
Any one in ammonia calibrating gas in hydrogen chloride calibrating gas, nitrogen in nitrogen.
Below in conjunction with specific embodiment (in nitrogen as a example by the preparation of hydrogen sulfide standard gas), the present invention is made further
Describing, these embodiments are merely to illustrate the present invention, are not limiting the scope of the invention.
Embodiment
In 4 liters of bottled 20 × 10-6 mol/mol (20ppm) nitrogen of preparation as a example by hydrogen sulfide standard gas, use passivation
Technique preparation process is as follows:
1. take one through pretreatment (80 DEG C of high-temperature bakings, evacuation 16 ~ 24 hours), and fill the 4 of front passed examination
Rise and treat gas filling bottle.
2. will treat that gas filling bottle accesses standard mixture charging device, and open cylinder valve, in bottle, be filled with 10 times of finished products dense
Degree, i.e. hydrogen sulfide mixed gas in 200 × 10-6 mol/mol (200ppm) nitrogen, to 1Mpa, close cylinder valve.
3. take off gas cylinder, stand 72 hours.
4. this is treated gas filling bottle access device, be vented gas cylinder, and evacuation 3 minutes.
5. close vacuum pumping valve, open filling valve, be filled with hydrogen sulfide in 200 × 10-6 mol/mol (200ppm) nitrogen and mix
Close gas, 44g.
6. it is filled with High Purity Nitrogen 396g.
7. closing charging device and cylinder valve, take off gas cylinder, preparation completes;In experimental stage, latter 24 ~ 72 hours are prepared
Detection data as shown in table 1 below:
Table 1: the hydrogen sulfide standard gas Concentration Testing data of 24 ~ 72 hours in the completed in nitrogen prepared by embodiment
By weighing value definite value, it is qualified to check, and dispatches from the factory.
Comparative example (tradition preparation process)
1, take one through pretreatment, and fill front passed examination 4 liters treat gas filling bottle;
2, will treat that gas filling bottle accesses standard mixture charging device, and open cylinder valve, open filling valve, be filled with 200 × 10-6
Hydrogen sulfide mixed gas in mol/mol (200ppm) nitrogen, 55g;
3, High Purity Nitrogen 385g it is filled with;
4, close charging device and cylinder valve, take off gas cylinder, complete 25ppm mixed gas preparation (consider possible adsorption,
Rule of thumb, preparation concentration is more slightly higher than client concentration);
5, detect after placing 24 hours, 21ppm;
6, detect after placing 48 hours, 18ppm;
7, detect after placing 72 hours, 17ppm;
8, detect after placing 96 hours, 17ppm;
9, this gas cylinder is accessed charging device, replenish hydrogen sulfide mixed gas 10g(empirical value in 200ppm nitrogen);
10, detect after placing 24 hours, 20ppm;
11, detect after placing 48 hours, 20ppm;
12, by detected value definite value, it is qualified to check, and dispatches from the factory.
Above-mentioned steps 5 ~ 11 may be repeated several times, if the concentration after Wen Ding is higher than the concentration of customer requirement, then needs to supplement
Enter High Purity Nitrogen dilution.
Compared with comparative example from above-described embodiment, hydrogen sulfide standard in nitrogen prepared by the passivation technology of the employing present invention
Gas, the production cycle is greatly shortened, shortened to 1 week by average 2 weeks, operate easier, preparation technology more specification, Consumer's Experience
More preferably.
Although present disclosure has been made to be discussed in detail by above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read foregoing, for the present invention's
Multiple amendment and replacement all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the preparation method of a nitrogenous mixed active calibrating gas, it is characterised in that the method comprises the steps of:
Step 1, will treat that gas filling bottle accesses standard mixture charging device, open cylinder valve, and be filled with and make a reservation for higher than finished product in bottle
The nitrogenous mixed active calibrating gas of concentration, closes cylinder valve to 0.5-3MPa;
Step 2, takes off gas cylinder, stands 48-96h;
Step 3, is vented gas cylinder, and evacuation 3-15 minute;
Step 4, closes vacuum pumping valve, opens filling valve, be filled with the nitrogenous mixed active calibrating gas higher than finished product predetermined concentration;
Step 5, is filled with High Purity Nitrogen in proportion so that treat that the nitrogenous mixed active calibrating gas in gas filling bottle reaches predetermined concentration;
Step 6, closes charging device and cylinder valve, takes off gas cylinder, and preparation completes.
2. preparation method as claimed in claim 1, it is characterised in that described nitrogenous mixed active calibrating gas refers in nitrogen
Any one in ammonia calibrating gas in hydrogen chloride calibrating gas, nitrogen in fluohydric acid gas calibrating gas, nitrogen in hydrogen sulfide standard gas, nitrogen
Kind.
3. preparation method as claimed in claim 1, it is characterised in that in step 1, described treats that gas filling bottle is preprocessed.
4. preparation method as claimed in claim 3, it is characterised in that described pretreatment refers to, makes to treat that gas filling bottle is at 80 DEG C
High-temperature baking, evacuation 16 ~ 24 hours.
5. preparation method as claimed in claim 1, it is characterised in that higher than the nitrogenous mixed active standard of finished product predetermined concentration
Gas refers to 10-15 times that its concentration is product predetermined concentration.
6. preparation method as claimed in claim 1, it is characterised in that higher than the nitrogenous mixed active standard of finished product predetermined concentration
Gas refers to 10 times of finished product predetermined concentrations of its concentration.
7. preparation method as claimed in claim 1, it is characterised in that in step 1, be filled with higher than finished product predetermined concentration is nitrogenous
Mixed active calibrating gas closes cylinder valve to 1Mpa.
8. preparation method as claimed in claim 1, it is characterised in that in step 2, stand 72h.
9. preparation method as claimed in claim 1, it is characterised in that in step 3, emptying gas cylinder refers to this bottle graft to be inflated
Enter the emptying of standard mixture charging device.
10. preparation method as claimed in claim 1, it is characterised in that in step 3, evacuation 3 minutes.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111840743A (en) * | 2020-07-21 | 2020-10-30 | 清远市联升空气液化有限公司 | Preparation method of standard mixed gas for treating persistent pulmonary artery height of newborn |
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CN103143293A (en) * | 2013-03-29 | 2013-06-12 | 淄博祥龙测控技术有限公司 | Standard mixed gas preparation device |
CN104888635A (en) * | 2015-06-11 | 2015-09-09 | 中国船舶重工集团公司第七一八研究所 | Device and method for compounding multiple cylinders of mixed gas |
CN204816244U (en) * | 2015-06-11 | 2015-12-02 | 中国船舶重工集团公司第七一八研究所 | Weigh device of many bottles of standard gas mixtures of cofabrication on line |
CN105547797A (en) * | 2015-12-23 | 2016-05-04 | 上海神开气体技术有限公司 | A method of rapidly preparing a low-concentration well-logging standard gas mixture |
CN105757447A (en) * | 2016-03-07 | 2016-07-13 | 常州蓝翼飞机装备制造有限公司 | Method for reducing water content of gas in welding gas cylinder |
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2016
- 2016-08-02 CN CN201610624372.0A patent/CN106226149A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103143293A (en) * | 2013-03-29 | 2013-06-12 | 淄博祥龙测控技术有限公司 | Standard mixed gas preparation device |
CN104888635A (en) * | 2015-06-11 | 2015-09-09 | 中国船舶重工集团公司第七一八研究所 | Device and method for compounding multiple cylinders of mixed gas |
CN204816244U (en) * | 2015-06-11 | 2015-12-02 | 中国船舶重工集团公司第七一八研究所 | Weigh device of many bottles of standard gas mixtures of cofabrication on line |
CN105547797A (en) * | 2015-12-23 | 2016-05-04 | 上海神开气体技术有限公司 | A method of rapidly preparing a low-concentration well-logging standard gas mixture |
CN105757447A (en) * | 2016-03-07 | 2016-07-13 | 常州蓝翼飞机装备制造有限公司 | Method for reducing water content of gas in welding gas cylinder |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111840743A (en) * | 2020-07-21 | 2020-10-30 | 清远市联升空气液化有限公司 | Preparation method of standard mixed gas for treating persistent pulmonary artery height of newborn |
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Application publication date: 20161214 |