CN104864263A - Preparation method of standard gases of volatile chlorinated hydrocarbon and liquid composition gasifying and filling device - Google Patents
Preparation method of standard gases of volatile chlorinated hydrocarbon and liquid composition gasifying and filling device Download PDFInfo
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- CN104864263A CN104864263A CN201510300334.5A CN201510300334A CN104864263A CN 104864263 A CN104864263 A CN 104864263A CN 201510300334 A CN201510300334 A CN 201510300334A CN 104864263 A CN104864263 A CN 104864263A
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Abstract
The invention relates to a preparation method of standard gases of volatile chlorinated hydrocarbon and a liquid composition gasifying and filling device. The liquid composition gasifying and filling device is characterized by comprising a digital heater, wherein the digital heater comprises a heater and a numerical control heating displayer for controlling the temperature of the heater; a gasification chamber is arranged in the heater; a liquid feeding opening communicated with the gasification chamber is in threaded connection to the top of the heater; a high-purity gas bottle is connected to one side of the liquid feeding opening through a blowing pipeline, and a pressure regulator is also arranged on the blowing pipeline; a bottle connecting part connected with a gas sample bottle is in threaded connection to the bottom of the heater. The liquid composition gasifying and filling device disclosed by the invention can be applied to the preparation of single-composition standard gases of volatile chlorinated hydrocarbon, and is also applied to the preparation of different numbers of mixed standard gases of volatile chlorinated hydrocarbon. The liquid composition gasifying and filling device disclosed by the invention is simple to operate, high in preparation efficiency and high in preparation repeatability, and can be widely applied to the preparation of standard gases of volatile chlorinated hydrocarbon.
Description
Technical field
The present invention relates to the preparation field of calibrating gas, particularly about a kind of volatile chlorinated hydrocarbon calibrating gas preparation method and liquid composition gasification filling device.
Background technique
Chlorohydrocarbon is the important organic synthesis intermediate of a class, is the initiation material of many organic syntheses.Wherein organic chlorohydrocarbon is widely used as solvent, industry and civilian washing agent, but these materials not only can injured skin, cause nervous centralis poisoning, the infringement of idioblast matter, heart etc. can also be caused, also harmful effect is had to liver, kidney, pancreas, some compounds may also have carcinogenic effect, and therefore all organic chlorides have larger toxicity.Chlorohydrocarbon depolarization small part in air comes from outside natural biological metabolism, is mainly derived from artificial pollution.The chlorine atom that chlorohydrocarbon discharges can play the effect of catalyzer to ozone decomposed, destroy atmospheric ozone layer.Carry out the mensuration to volatile chlorinated hydrocarbon in ambient air, basic data will be provided for volatile chlorinated hydrocarbon pollution surveys and control research, and for protection of the environment, ensure that people ' s health will all be significant.But the kind that volatile chlorinated hydrocarbon comprises is a lot, and volatile chlorinated hydrocarbon typically refers to the halogenated compound of boiling point below 200 DEG C, and the chlorohydrocarbon below nearly all 8 carbon below 5 halogen atoms all belongs to Volatile Organohalides.According to the difference of managerial demand and analytical technology ability, analytic target is also different.Such as, 27 kinds of halogenated hydrocarbon are included in 190 kinds of noxious pollutant lists in U.S.'s priority control air; Also part chlorohydrocarbon is comprised in Chinese environmental priority monitoring and control polluted articles.But China does not still have volatile chlorinated hydrocarbon Reference Material of Gases now, have a strong impact on the monitor and forecast of volatile chlorinated hydrocarbon in ambient air.
Reference Material of Gases generally adopts gas filling device high-purity gas dilution to be obtained.But chlorohydrocarbon volatile chlorinated hydrocarbon component boiling spread wide (as shown in table 1), existing gaseous state under normal temperature, also has liquid.And be that liquid composition is prepared Reference Material of Gases and be there are many technological difficulties under normal temperature, such as how to weigh the low volatile micro-liquid composition of boiling point, how will add Micro-volume liquid and add sample gas cylinder, how to ensure that liquid is gasified totally and how guarantees that liquid is not attached to the problems such as gas cylinder inwall.
The boiling point Schedule of table 122 kind of chlorohydrocarbon
| Sequence number | Component | Boiling point (DEG C) |
| 1 | Chloromethanes | -23.7 |
| 2 | Vinyl chloride | 13.4 |
| 3 | Chloroethanes | 12.4 |
| 4 | Vinylidene chloride | 31.6 |
| 5 | Dichloromethane | 39.7 |
| 6 | Anti-1,2-dichloroethene | 47.5 |
| 7 | 1,1-dichloroethane | 57.3 |
| 8 | Along 1,2-dichloroethene | 60.6 |
| 9 | Trichloromethane | 61.1 |
| 10 | 1,1,1-trichloroethanes | 74.0 |
| 11 | Carbon tetrachloride | 76.8 |
| 12 | 1,2-dichloroethane | 83.5 |
| 13 | Trichloroethylene | 87.2 |
| 14 | 1,2-dichloropropane | 96.4 |
| 15 | 1,1,2-trichloroethanes | 113.5 |
| 16 | Tetrachloroethylene | 121.2 |
| 17 | Chlorobenzene | 131.7 |
| 18 | 1,1,1,2-tetrachloroethanes | 138.2 |
| 19 | 1,1,2,2-tetrachloroethanes | 146.3 |
| 20 | M-dichlorobenzene | 173 |
| 21 | Paracide | 174.1 |
| 22 | O-dichlorohenzene | 180.5 |
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of easy and simple to handle, volatile chlorinated hydrocarbon calibrating gas preparation method that preparation efficiency is high, reproducible and liquid composition gasification filling device.
For achieving the above object, the present invention takes following technological scheme: a kind of liquid composition gasification filling device, it is characterized in that: it comprises a digitizing heating equipment, described digitizing heating equipment comprises a heating equipment and for controlling the numerical-control heating display device of heating equipment temperature; Described heating equipment inside is provided with a gasification chamber; Described heating equipment screw top connects a filling opening be communicated with described gasification chamber, and the side of described filling opening is connected with a high-purity gas bottle by scavenging pipeline, and described scavenging pipeline is also provided with a pressure regulator; The bottle connected element of described heating equipment bottom thread connection one for being connected with sample gas cylinder.
A packing ring is provided with, described gasification chamber and form confined space between described filling opening and bottle connected element between described gasification chamber upper end and described filling opening, between described gasification chamber lower end and described bottle connected element.
Described packing ring adopts exotic material preparation.
Described gasification chamber adopts the preparation of inertia exotic material, and temperature range is 0-300 degree, and through passivation.
The temperature-controlled precision of described digitizing heating equipment is 0.1 degree.
A kind of volatile chlorinated hydrocarbon calibrating gas preparation method, comprise the following steps: the concentration 1) first preparing volatile chlorinated hydrocarbon calibrating gas needed for basis is determined to prepare progression, calculate the weighed amount of often kind of chlorohydrocarbon component and diluent gas in preparation process at different levels according to the molal weight of volatile chlorinated hydrocarbon and concentration level, as the reference of filling quality actual in preparation process simultaneously; 2) adopt gasification pad device the chlorohydrocarbon component of various gaseous state and diluent gas to be filled with in sample gas cylinder by the mode of stepwise dilution, prepare benchmark mixed gas; 3) adopt liquid composition gasification filling device to carry out the filling of various liquid chlorohydrocarbon component, first by after the cleaning of sample gas cylinder also extracting vacuum, be connected on bottle connected element; According to the boiling point of each liquid chlorohydrocarbon component, digitizing heating equipment is arranged temperature required, each liquid chlorohydrocarbon component can fully be gasified, and guarantee that decomposition reaction and mutual reaction do not occur various liquid chlorohydrocarbon component; 4) after gasification chamber preheating, adopt lockable airtight liquid composition weigher to take the liquid chlorohydrocarbon component of various required quality respectively, and add from filling opening in gasification chamber, various liquid chlorohydrocarbon component is fully gasified; 5) open the valve of high-purity gas bottle, regulate pressure regulator, use diluent gas to purge gasification chamber, the liquid chlorohydrocarbon component after all gasifications is made to enter in the sample gas cylinder of lower end completely, afterwards, weigh the quality of sample gas cylinder, obtain the actual mass of the chlorohydrocarbon component be filled with; 6) to step 5) in be filled with the benchmark mixed gas of required quality in the sample gas cylinder that obtains, the quality weighing sample gas cylinder obtains the actual mass being filled with benchmark mixed gas; Afterwards, be filled with the diluent gas of required quality, and weighing obtains the actual mass being filled with diluent gas again, namely obtains the volatile chlorinated hydrocarbon calibrating gas of desired concn.
The present invention is owing to taking above technological scheme, it has the following advantages: 1, the present invention is owing to adopting digitizing heating equipment, it has accurately adjustable temperature control system, can ensure that liquid chlorohydrocarbon component fully gasifies, guarantee that the chemical reaction such as decomposition reaction, mutual reaction does not occur liquid chlorohydrocarbon component simultaneously, ensure that the accuracy of prepared calibrating gas is high.2, the present invention adopts inert material to make due to gasification chamber and packing ring etc., there is not any sorption and desorption effect, ensure that the value accuracy of Reference Material of Gases to chlorohydrocarbon component.3, the present invention is all sealed by Sealing due to each device joint, and whole system sealing is good, and ensure that in preparation process, various chlorohydrocarbon component is not revealed, Security is good.4, the present invention is easy and simple to handle, preparation efficiency is high, preparation favorable reproducibility, applied range, both the preparation of one-component volatile chlorinated hydrocarbon Reference Material of Gases had been applicable to, also be applicable to the volatile chlorinated hydrocarbon Reference Material of Gases preparation of varying number mixing simultaneously, thus can be widely used in the preparation of volatile chlorinated hydrocarbon calibrating gas.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
As shown in Figure 1, liquid composition of the present invention gasification filling device comprises a digitizing heating equipment 1, and digitizing heating equipment 1 comprises a heating equipment 2 and for controlling the numerical-control heating display device 3 of heating equipment temperature.Wherein, heating equipment 2 inside is provided with a gasification chamber 4.Heating equipment 2 screw top connects a filling opening 5 be communicated with gasification chamber 4, and the side of filling opening 5 is connected with a high-purity gas bottle 7 by scavenging pipeline 6, and scavenging pipeline 6 is also provided with a pressure regulator 8.The bottle connected element 9 of heating equipment 2 bottom thread connection one for being connected with sample gas cylinder.
In above-described embodiment, between gasification chamber 4 upper end and filling opening 5, between gasification chamber 4 lower end and bottle connected element 9, be provided with a packing ring 10, make gasification chamber 4 and form confined space between filling opening 5 and bottle connected element 9.
In the various embodiments described above, gasification chamber 4 adopts inertia exotic material to prepare, and temperature range is 0-300 degree, and through passivation.
In the various embodiments described above, packing ring 10 adopts exotic material to prepare, and does not adsorb chlorohydrocarbon component.
In the various embodiments described above, the temperature-controlled precision of digitizing heating equipment 1 is 0.1 degree.
Based on above-mentioned liquid composition gasification filling device, present invention also offers a kind of volatile chlorinated hydrocarbon calibrating gas preparation method, adopt different devices that the various chlorohydrocarbon components being in liquid and gaseous state under normal temperature are filled with sample gas cylinder respectively to prepare volatile chlorinated hydrocarbon calibrating gas, concrete, comprise the following steps:
1) concentration first preparing volatile chlorinated hydrocarbon calibrating gas needed for basis is determined to prepare progression, calculate the weighed amount of often kind of chlorohydrocarbon component and diluent gas in preparation process at different levels according to the molal weight of volatile chlorinated hydrocarbon and concentration level, as the reference of filling quality actual in preparation process simultaneously.
In the present invention with molar concentration be 22 kinds of volatile chlorinated hydrocarbon calibrating gas of 1 μm of ol/mol be prepared as example, describe in detail.22 kinds of volatile chlorinated hydrocarbon component boiling spreads are wider, and under normal temperature, it comprises the chlorohydrocarbon component of 19 kinds of liquid chlorohydrocarbon components and 3 kinds of gaseous states.In order to ensure the accuracy of the calibrating gas prepared, adopting 4 grades to dilute preparation and completing.Meanwhile, to calculate in often kind of chlorohydrocarbon component and dilution preparation process at different levels the weighed amount of required diluent gas according to the concentration of volatile chlorinated hydrocarbon calibrating gas, the weighed amount of calculating is as the reference of the actual mass of filling in preparation process.
2) adopt gasification pad device the chlorohydrocarbon component of various gaseous state and diluent gas to be filled with in sample gas cylinder by the mode of stepwise dilution, prepare benchmark mixed gas.
Due in 22 kinds of volatile chlorinated hydrocarbon components, only comprise three kinds of gaseous state chlorohydrocarbon components, i.e. chloromethanes, chloroethanes and vinyl chloride, the preparation method of the benchmark mixed gas of 3 kinds of chlorohydrocarbons is: adopt gas cylinder cleaning equipment to clean sample gas cylinder, after weighing the quality of the sample gas cylinder cleaned, adopt gas recyclers and gas handling equipment respectively by 3 of required quality kinds of high-purity chloro appropriate hydrocarbon gas chloromethanes, after chloroethanes and vinyl chloride are filled with sample gas cylinder, and weigh the quality being at every turn filled with sample gas cylinder after chlorohydrocarbon component, the actual mass of the often kind of gaseous state chlorohydrocarbon component utilizing minusing to obtain being filled with.Afterwards, in this sample gas cylinder, be filled with the diluent gas of required quality, and again weigh sample gas cylinder quality, obtain the actual mass being filled with diluent gas.Now obtain chloromethanes, chloroethanes and vinyl chloride mixing reference gas.
3) liquid composition of the present invention gasification filling device is adopted to carry out the filling of various liquid chlorohydrocarbon component, first by after the cleaning of sample gas cylinder also extracting vacuum, be connected on the bottle connected element 9 of liquid composition of the present invention gasification filling device, according to the boiling point of each liquid chlorohydrocarbon component, liquid composition gasification filling device of the present invention is arranged temperature required, to ensure that each liquid chlorohydrocarbon component can fully gasify, and guarantee that decomposition reaction and mutual reaction do not occur various liquid chlorohydrocarbon component.
4) after gasification chamber 4 preheating, adopt lockable airtight liquid composition weigher to take the liquid chlorohydrocarbon component of various required quality respectively, and add in gasification chamber 4 from filling opening, the chlorohydrocarbon component of various liquid state is fully gasified.
5) valve of high-purity gas bottle 7 is opened, regulate pressure regulator 8, diluent gas is used to purge gasification chamber 4, the liquid chlorohydrocarbon component after all gasifications is made to enter in the sample gas cylinder of lower end completely, close sample gas cylinder valve, and weigh the quality of now sample gas cylinder, obtain the actual mass of the chlorohydrocarbon component be filled with.
6) to step 5) be filled with the benchmark mixed gas of required quality in the sample gas cylinder that obtains, the quality weighing sample gas cylinder obtains the actual mass being filled with mixing reference gas.Afterwards, be filled with the diluent gas of required quality, and weighing obtains the actual mass being filled with diluent gas again, can obtain the volatile chlorinated hydrocarbon calibrating gas of desired concn.According to the actual mass of above-mentioned obtained various components, the actual concentrations of volatile chlorinated hydrocarbon at calibrating gas of preparation can be calculated.
The various embodiments described above are only for illustration of the present invention; wherein the structure of each parts, Placement and preparation process etc. all can change to some extent; every equivalents of carrying out on the basis of technical solution of the present invention and improvement, all should not get rid of outside protection scope of the present invention.
Claims (6)
1. a liquid composition gasification filling device, it is characterized in that: it comprises a digitizing heating equipment, described digitizing heating equipment comprises a heating equipment and for controlling the numerical-control heating display device of heating equipment temperature; Described heating equipment inside is provided with a gasification chamber; Described heating equipment screw top connects a filling opening be communicated with described gasification chamber, and the side of described filling opening is connected with a high-purity gas bottle by scavenging pipeline, and described scavenging pipeline is also provided with a pressure regulator; The bottle connected element of described heating equipment bottom thread connection one for being connected with sample gas cylinder.
2. a kind of liquid composition gasification filling device as claimed in claim 1, it is characterized in that: between described gasification chamber upper end and described filling opening, between described gasification chamber lower end and described bottle connected element, be provided with a packing ring, described gasification chamber and form confined space between described filling opening and bottle connected element.
3. a kind of liquid composition gasification filling device as claimed in claim 2, is characterized in that: described packing ring adopts exotic material preparation.
4. a kind of liquid composition gasification filling device as claimed in claim 1, is characterized in that: described gasification chamber adopts the preparation of inertia exotic material, and temperature range is 0-300 degree, and through passivation.
5. a kind of liquid composition gasification filling device as claimed in claim 1, is characterized in that: the temperature-controlled precision of described digitizing heating equipment is 0.1 degree.
6. adopt a volatile chlorinated hydrocarbon calibrating gas preparation method for liquid composition gasification filling device as described in any one of claim 1-5, comprise the following steps:
1) concentration first preparing volatile chlorinated hydrocarbon calibrating gas needed for basis is determined to prepare progression, calculate the weighed amount of often kind of chlorohydrocarbon component and diluent gas in preparation process at different levels according to the molal weight of volatile chlorinated hydrocarbon and concentration level, as the reference of filling quality actual in preparation process simultaneously;
2) adopt gasification pad device the chlorohydrocarbon component of various gaseous state and diluent gas to be filled with in sample gas cylinder by the mode of stepwise dilution, prepare benchmark mixed gas;
3) adopt liquid composition gasification filling device to carry out the filling of various liquid chlorohydrocarbon component, first by after the cleaning of sample gas cylinder also extracting vacuum, be connected on bottle connected element; According to the boiling point of each liquid chlorohydrocarbon component, digitizing heating equipment is arranged temperature required, each liquid chlorohydrocarbon component can fully be gasified, and guarantee that decomposition reaction and mutual reaction do not occur various liquid chlorohydrocarbon component;
4) after gasification chamber is preheated, adopt lockable airtight liquid composition weighing means to take the liquid chlorohydrocarbon component of various required quality respectively, and add from filling opening in gasification chamber, various liquid chlorohydrocarbon component is fully gasified;
5) open the valve of high-purity gas bottle, regulate pressure regulator, use diluent gas to purge gasification chamber, the liquid chlorohydrocarbon component after all gasifications is made to enter in the sample gas cylinder of lower end completely, afterwards, weigh the quality of sample gas cylinder, obtain the actual mass of the chlorohydrocarbon component be filled with;
6) to step 5) in be filled with the benchmark mixed gas of required quality in the sample gas cylinder that obtains, the quality weighing sample gas cylinder obtains the actual mass being filled with benchmark mixed gas; Afterwards, be filled with the diluent gas of required quality, and weighing obtains the actual mass being filled with diluent gas again, namely obtains the volatile chlorinated hydrocarbon calibrating gas of desired concn.
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Cited By (2)
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| CN108953989A (en) * | 2018-08-07 | 2018-12-07 | 李晨天 | Alternating temperature pressure swing type liquefied gas transfer device |
| CN113685720A (en) * | 2021-08-25 | 2021-11-23 | 国网重庆市电力公司电力科学研究院 | C5-PFK rapid inflation system and inflation method |
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| CN113685720A (en) * | 2021-08-25 | 2021-11-23 | 国网重庆市电力公司电力科学研究院 | C5-PFK rapid inflation system and inflation method |
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