CN105043817A - Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution - Google Patents
Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution Download PDFInfo
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Abstract
The invention relates to a long-distance automatic sampling device for a liquid-state hydrogen fluoride solution. The device comprises a liquid storage pot, wherein an outlet liquid inlet of a liquid outlet pipe extends into the liquid storage pot, and an outlet liquid outlet is connected with a connecting pipe; the top of a sampling bottle is provided with a dismountable doubleport PTFE cutting sleeve bottle cap; a liquid inlet pipe penetrates through the doubleport PTFE cutting sleeve bottle cap, and the inlet liquid outlet extends into the sampling bottle and is positioned above the liquid level of a diluent; one end of an air outlet pipe penetrates through the doubleport PTFE cutting sleeve bottle cap, extends into the sampling bottle and is positioned above the liquid level of the diluent; the other end of the air outlet pipe is communicated with an air exhaust tank which is in dynamic sealing with a piston; and the movement of the piston is controlled through a controller electrically connected with an air cylinder. The invention also provides a sampling method of the long-distance automatic sampling device. In the sampling process, the long-distance automatic sampling device for the liquid-state hydrogen fluoride solution ensures the leakproofness of the system by matching of tanks, pipelines and valves, so that the system is completely isolated with the atmospheric environment, and no hydrogen fluoride air overflows.
Description
Technical field
The present invention relates to hydrofluoric sampling, relate more specifically to a kind of remote auto sampler and method thereof of liquid fluorinated hydrogen solution.
Background technology
Hydrofluorite is a kind of water white transparency fuming liquids, is the aqueous solution of hydrogen fluoride gas, in faintly acid, and irritant smell.Hydrofluorite can react with the compound of silicon and silicon the silicon tetrafluoride (energy etching glass) generating gaseous state, but does not play corrosive attack to plastics, paraffin, lead, gold, platinum.
In Aluminium Industry, hydrogen fluoride is used for the production of aluminum fluoride and cryolite, and synthesis is used for the CFC of cold-producing medium and gas-development agent, and synthetic polymer.In the process of uranium, uranium dioxide can be separately converted to green salt and hex by hydrogen fluoride, and hex can be used for the isotope of diffusion method or centrifuge method SEPARATION OF URANIUM.In Chemical Manufacture, hydrogen fluoride also can be used as alkylation, polymerization, condensation, isomerized catalyzer; Also can be used for etching and polished glass, stainless acid pickling and rust removing, metal casting desanding, the stabilizing agent of rocket propulsion oxygenant and the many chloric metal-salts of preparation.
Seemingly, for polar molecule also can be self-ionized, it is the fine solvent of many ionic crystalline compound for a lot of physicochemical property of liquid hydrogen fluoride and aqueous phase.Its liquid temperature scope is (-83.1 DEG C ~ 19.5 DEG C) more than 100 DEG C, and certainly dissociating of liquid hydrogen fluoride is as follows:
Liquid hydrogen fluoride can be used as the fine solvent of many villiaumites, and such as, 11 DEG C time, the liquid fluorinated Hydrogen Energy of 100g dissolves 30g sodium fluoride, thus forms the liquid fluorinated hydrogen solution of sodium fluoride.In actual mechanical process, because hydrogen fluoride is gaseous state at normal temperatures, and be the severe poisonous chemicals of severe corrosive, therefore, be usually difficult to that obtained liquid fluorinated hydrogen solution is dissolved in liquid hydrogen fluoride to villiaumite and carry out real-time online sample analysis.
In order to realize the sampling of liquid towards hydrogen fluoride solution, disclosed method is molten ice method and outside frozen water cooling method at present.But, these two kinds of sampling methods are all have the condition realization of certain pressure at got liquid fluorinated hydrogen solution, namely in container or pipeline, there is certain static pressure (or gravity), after opening container or pipe valve, under the effect of static pressure (or gravity), liquid fluorinated hydrogen solution flows in sampling jar with suitable flow velocity.Obviously, the sampling of these two kinds of methods is limited to this static pressure or gravity, then cannot realize the sampling of liquid towards hydrogen fluoride solution under the condition not possessing static pressure or gravity.In addition, the sampler of these two kinds of sampling methods of known application employs metal valve and fluorine material (PTFE, PFA and PVDF etc.) valve, because metal valve is subject to hydrogen fluoride corrosion in Long-Time Service process, corrosion product not only can pollute liquid hydrogen fluoride solution also can cause metal valve open difficulty and flow regulation difficult, and then affect the sealing of metal valve, cause potential safety hazard; Although the good corrosion resistance of fluorine material valve, its intensity is lower, and spool easily causes creep and affects sealing under long-term action of compressive stress, therefore there is potential safety hazard equally.And above-mentioned two kinds of sampling methods all deposit the problem of residual liquid hydrogen fluoride solution in sampling line after sampling, thus after removing sampling jar, liquid hydrogen fluoride at room temperature has steam and overflows, and there is security risk.
Summary of the invention
In order to solve above-mentioned prior art exist the problem depending on static pressure or gravity and sampling process in there is the potential safety hazards such as the residual fluorinated hydrogen of pipeline, the present invention aims to provide a kind of remote auto sampler and method thereof of liquid fluorinated hydrogen solution.
The invention provides a kind of remote auto sampler of liquid fluorinated hydrogen solution, comprising: fluid reservoir, in described fluid reservoir, accommodate liquid fluorinated hydrogen solution; Drain pipe, the fluid entrance of described drain pipe to stretch in described fluid reservoir and is positioned at below the liquid level of described liquid fluorinated hydrogen solution, and the eluate outlet of described drain pipe is connected with connecting pipe, and described connecting pipe is provided with variable valve; Sampling jar, accommodates thinning agent in described sampling jar, and the top of described sampling jar is provided with dismountable twoport PTFE cutting ferrule bottle cap; Feed tube, described feed tube extends through described twoport PTFE cutting ferrule bottle cap, the liquid inlet of described feed tube is connected with the eluate outlet of described drain pipe, the feed liquor outlet of described feed tube to be stretched in described sampling jar and is positioned at the ullage of described thinning agent, is provided with liquid feed valve between described liquid inlet and described twoport PTFE cutting ferrule bottle cap; Escape pipe, one end of described escape pipe to be stretched in described sampling jar through described twoport PTFE cutting ferrule bottle cap and is positioned at the ullage of described thinning agent, and the other end is connected with tank of bleeding, and the pipeline of escape pipe is provided with air outlet valve; Described bleed tank and piston dynamic seal (packing); The movement of piston is controlled by the controller be electrically connected with cylinder.
This remote auto sampler also comprises the wash-bottle for replacing described sampling jar, and described wash-bottle coordinates with described twoport PTFE cutting ferrule bottle cap.
This remote auto sampler also comprises the safety flack for replacing described sampling jar, and described safety flack coordinates with described twoport PTFE cutting ferrule bottle cap.
This remote auto sampler also includes magnetic stirring apparatus and PTFE stirrer, and described PTFE stirrer is placed in described sampling jar, and described magnetic stirring apparatus is arranged at the below of described sampling jar.
Described feed tube is connected with drain pipe by cutting sleeve type three-way joint with described connecting pipe.
Described drain pipe and described connecting pipe are respectively 1/4 inch of PFA pipe, described feed tube and described escape pipe are 1/8 inch of PFA pipe, described variable valve is 1/4 inch of PFA needle-valve, and described liquid feed valve is 1/8 inch of PTFE ball valve, and described air outlet valve is 1/8 inch of PTFE ball valve.
The feed liquor outlet of described feed tube is 4mm-6mm with the distance of the liquid level of described thinning agent.
Described programmable logic controller (PLC) is connected with cylinder by the pneumatic valve with source of the gas.
The present invention also provides the sampling method of above-mentioned remote auto sampler, comprise: S1, close variable valve, open liquid feed valve and air outlet valve, moved by the described piston of cylinder described in described programmable logic controller (PLC) controls, thus negative pressure is produced in described tank of bleeding, force the described liquid fluorinated hydrogen solution in described fluid reservoir to enter in described sampling jar along described drain pipe and described feed tube; S2, is moved by the described piston reverses direction of cylinder described in described programmable logic controller (PLC) controls, thus produce malleation in described tank of bleeding, and forces the described liquid fluorinated hydrogen solution in described drain pipe and described feed tube to flow back in described fluid reservoir.
This remote auto sampling method also comprises: moved by the described piston of cylinder described in described programmable logic controller (PLC) controls, thus negative pressure is produced in described tank of bleeding, force the described liquid fluorinated hydrogen solution in described fluid reservoir to enter in described wash-bottle along described drain pipe and described feed tube, thus rinse is carried out to described drain pipe and described feed tube.
The present invention passes through remote auto sampler and the method thereof of provided liquid fluorinated hydrogen solution, realizes sampling, do not rely on the static pressure in fluid reservoir or gravity by cylinder operation; By the control of programmable logic controller (PLC) to piston movement, the quantitative sampling of liquid towards hydrogen fluoride solution can be realized; By utilizing programmable logic controller (PLC) to form negative pressure bleeding in tank, the remote sampling of liquid towards hydrogen fluoride solution can be realized; By specifically feed tube being chosen as 1/8 inch of PFA pipe, and liquid feed valve is chosen as 1/8 inch of PTFE ball valve, can realize the microsampling of liquid fluorinated hydrogen solution, and minimum sampling amount is 34mg; By forming malleation bleeding in tank, the liquid fluorinated hydrogen solution that can sample in rear pipeline flows back to fluid reservoir, and that guarantees without liquid hydrogen fluoride solution in pipeline is residual, greatly improves efficiency and the security of sampling.In a word, the remote auto sampler of liquid fluorinated hydrogen solution of the present invention is in sampling process, the sealing of system is ensure that by the cooperation of tank body, pipeline and each valve, make itself and atmospheric environment completely isolated, fluoride-free hydrogen overflows, and sampling process does not affect the normal operation of fluid reservoir, whole safe operation process, reliable, controlled, sampling amount is less, guarantees the authenticity of liquid hydrogen fluoride solution example.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the remote auto sampler of liquid fluorinated hydrogen solution of the present invention.
Embodiment
Below in conjunction with accompanying drawing, provide preferred embodiment of the present invention, and be described in detail.
As shown in Figure 1, the remote auto sampler of liquid fluorinated hydrogen solution of the present invention comprises fluid reservoir 1, drain pipe 2, sampling jar 3, feed tube 4, escape pipe 5, tank 6 of bleeding, cylinder 7, programmable logic controller (PLC) 8, pneumatic valve 9 and connecting pipe 10.
Wherein, accommodate liquid fluorinated hydrogen solution 11 in fluid reservoir 1, in sampling jar 3, accommodate thinning agent 31.Fluid reservoir 1 is communicated with by drain pipe 2 with sampling jar 3.The fluid entrance 21 of drain pipe 2 to stretch in fluid reservoir 1 and is positioned at below the liquid level of liquid fluorinated hydrogen solution 11, near the bottom preferably extending into fluid reservoir 1, eluate outlet 22 1 aspect of drain pipe 2 is communicated with air by connecting pipe 10 or is connected with other tank body pipeline, be communicated with sampling jar 3 by the liquid inlet 41 of feed tube 4 on the other hand, this connection is such as realized by cutting sleeve type three-way joint.The top of sampling jar 3 is provided with dismountable twoport PTFE cutting ferrule bottle cap 32, feed tube 4 and escape pipe 5 are each passed through twoport PTFE cutting ferrule bottle cap 32 and stretch in sampling jar 3, wherein, the feed liquor outlet 42 of feed tube 4 is positioned at the ullage 4mm-6mm place of thinning agent 31 in sampling jar 3; The suction inlet 51 of escape pipe 5 is positioned at the ullage of thinning agent 31.The outlet of escape pipe 5 is directly connected with tank 6 of bleeding.In sampling jar 3, the distance between the liquid level of suction inlet 51 and thinning agent 31 is greater than feed liquor and exports distance between 42 and the liquid level of thinning agent 31.Cylinder 7 has moveable piston 71, and tank 6 of bleeding carries out dynamic seal (packing) under the to-and-fro movement of piston 71.Programmable logic controller (PLC) 8 to be connected with cylinder 7 by the pneumatic valve 9 with source of the gas 91 (such as nitrogen) and for the movement of control piston 71.By means of programmable logic controller (PLC) 8, the fixing quantity of the displacement of pneumatic valve 9 pairs of pistons 71 can realize quantitative sampling and the microsampling of liquid fluorinated hydrogen solution 11.
On valve is arranged, connecting pipe 10, feed tube 4 and escape pipe 5 are respectively arranged with variable valve 100, liquid feed valve 43 and air outlet valve 53.
In the present embodiment, drain pipe 2 and connecting pipe 10 are 1/4 inch of PFA pipe, and feed tube 4 and escape pipe 5 are 1/8 inch of PFA pipe, and variable valve 100 is 1/4 inch of PFA needle-valve, and liquid feed valve 43 and air outlet valve 53 are 1/8 inch of PTFE ball valve.
Wherein, sampling jar 3 above can be replaced wash-bottle 3a and safety flack 3b, and this wash-bottle 3a and safety flack 3b coordinates with twoport PTFE cutting ferrule bottle cap 32 respectively.In the present embodiment, sampling jar 3, wash-bottle 3a and safety flack 3b are respectively PFA bottle.
This remote auto sampler also includes magnetic stirring apparatus and PTFE stirrer, and PTFE stirrer is placed in sampling jar 3 or wash-bottle 3a, and magnetic stirring apparatus is arranged at the below of sampling jar 3 or wash-bottle 3a.By the stirring of stirrer, the liquid in sampling jar 3 or wash-bottle 3a is dispelled the heat rapidly, prevents localized liquid excessively thermal evaporation.
The invention provides a kind of sampling method of above-mentioned remote auto sampler, first, close variable valve 100, open liquid feed valve 43 and air outlet valve 53, moved by the piston 71 of programmable logic controller (PLC) 8 control cylinder 7, thus in generation negative pressure in tank 6 of bleeding, force the liquid fluorinated hydrogen solution 11 in fluid reservoir 1 to enter in sampling jar 3 along drain pipe 2 and feed tube 4 and diluted by thinning agent 31; Then, by the piston 71 oppositely movement of programmable logic controller (PLC) 8 control cylinder 7, thus in generation malleation in tank 6 of bleeding, force the liquid fluorinated hydrogen solution 11 in drain pipe 2 and feed tube 4 to flow back in fluid reservoir 1.
In a most preferred embodiment, the invention provides a kind of sampling method of above-mentioned remote auto sampler, comprising:
(1) in wash-bottle 3a, load the deionized water of about 1/2 volume, PTFE stirrer is dropped in wash-bottle 3a, then be placed on magnetic stirring apparatus by wash-bottle 3a, the bottleneck of this wash-bottle 3a screws with twoport PTFE cutting ferrule bottle cap 32 and coordinates (sealing); Start magnetic stirring apparatus, make the rotating speed agitating deionized water of PTFE stirrer with 300rpm ~ 700rpm of wash-bottle 3a, close variable valve 100, open liquid feed valve 43, air outlet valve 53 and source of the gas 91, open programmable logic controller (PLC) 8 and pneumatic valve 9, press control system panel washing key, pneumatic valve 9 control cylinder 7 slowly pulls piston 71, now namely there is liquid fluorinated hydrogen solution 11 to flow in wash-bottle 3a along drain pipe 2 and feed tube 4 to be absorbed by deionized water, thus rinse is carried out to drain pipe 2 and feed tube 4.After rinse completes, again press washing key, pneumatic valve 9 control cylinder 7 promotes piston 71, and be pressed in fluid reservoir 1 by residual liquid fluorinated hydrogen solution 11 in drain pipe 2 and feed tube 4, closedown liquid feed valve 43 and air outlet valve 53 complete washing.
(2) wash-bottle 3a is screwed off from twoport PTFE cutting ferrule bottle cap 32, utilize bottle cap sealing wash-bottle 3a.Simultaneously, the sampling jar 3 that a certain amount of thinning agent 31 and PTFE stirrer are housed to be placed on magnetic stirring apparatus and to be tightly connected with twoport PTFE cutting ferrule bottle cap 32, open liquid feed valve 43 and air outlet valve 53, press control system panel sampling key, pneumatic valve 9 control cylinder 7 slowly pulls piston 71 (piston displacement is relevant to required sampling amount), now namely has liquid fluorinated hydrogen solution 11 to be drawn in sampling jar 3 along drain pipe 2 and feed tube 4.After sampling completes, again press sampling key, pneumatic valve 9 control cylinder 7 promotes piston 71, and be pressed in fluid reservoir 1 by residual liquid fluorinated hydrogen solution 11 in drain pipe 2 and feed tube 4, closedown liquid feed valve 43 and air outlet valve 53 complete sampling.
(3) sampling jar 3 is screwed off from twoport PTFE cutting ferrule bottle cap 32, utilize bottle cap sealing sampling jar 3.Meanwhile, safety flack is connected with twoport PTFE cutting ferrule bottle cap 32, guarantees sealing.
Above-described, be only preferred embodiment of the present invention, and be not used to limit scope of the present invention, the above embodiment of the present invention can also make a variety of changes.Namely every claims according to the present patent application and description are done simple, equivalence change and modify, and all fall into the claims of patent of the present invention.The not detailed description of the present invention be routine techniques content.
Claims (10)
1. a remote auto sampler for liquid fluorinated hydrogen solution, is characterized in that, this remote auto sampler comprises:
Fluid reservoir (1), accommodates liquid fluorinated hydrogen solution (11) in described fluid reservoir (1);
Drain pipe (2), the fluid entrance (21) of described drain pipe (2) to stretch in described fluid reservoir (1) and is positioned at below the liquid level of described liquid fluorinated hydrogen solution (11), the eluate outlet (22) of described drain pipe (2) is connected with connecting pipe (10), described connecting pipe (10) is provided with variable valve (100);
Sampling jar (3), accommodates thinning agent (31) in described sampling jar (3), the top of described sampling jar (3) is provided with dismountable twoport PTFE cutting ferrule bottle cap (32);
Feed tube (4), described feed tube (4) is through described twoport PTFE cutting ferrule bottle cap (32), the liquid inlet (41) of described feed tube (4) is connected with the eluate outlet (22) of described drain pipe (2), feed liquor outlet (42) of described feed tube (4) to stretch in described sampling jar (3) and is positioned at the ullage of described thinning agent (31), is provided with liquid feed valve (43) between described liquid inlet (41) and described twoport PTFE cutting ferrule bottle cap (32);
Escape pipe (5), one end of described escape pipe (5) to be stretched in described sampling jar (3) through described twoport PTFE cutting ferrule bottle cap (32) and is positioned at the ullage of described thinning agent (31), the other end is connected with tank of bleeding (6), and the pipeline of escape pipe (5) is provided with air outlet valve (53); Described tank of bleeding (6) and piston (71) dynamic seal (packing); The movement of piston (71) is controlled by the controller be electrically connected with cylinder (7).
2. remote auto sampler according to claim 1, it is characterized in that, also comprise the wash-bottle (3a) for replacing described sampling jar (3), described wash-bottle (3a) coordinates with described twoport PTFE cutting ferrule bottle cap (32).
3. remote auto sampler according to claim 1, it is characterized in that, also comprise the safety flack (3b) for replacing described sampling jar (3), described safety flack (3b) coordinates with described twoport PTFE cutting ferrule bottle cap (32).
4. remote auto sampler according to claim 1, it is characterized in that, also include magnetic stirring apparatus and PTFE stirrer, described PTFE stirrer is placed in described sampling jar (3), and described magnetic stirring apparatus is arranged at the below of described sampling jar (3).
5. remote auto sampler according to claim 1, is characterized in that, described feed tube (4) is connected with drain pipe (2) by cutting sleeve type three-way joint with described connecting pipe (10).
6. remote auto sampler according to claim 1, it is characterized in that, described drain pipe (2) and described connecting pipe (10) are respectively 1/4 inch of PFA pipe, described feed tube (4) and described escape pipe (5) are 1/8 inch of PFA pipe, described variable valve (100) is 1/4 inch of PFA needle-valve, described liquid feed valve (43) is 1/8 inch of PTFE ball valve, and described air outlet valve (53) is 1/8 inch of PTFE ball valve.
7. remote auto sampler according to claim 1, is characterized in that, feed liquor outlet (42) of described feed tube (4) is 4mm-6mm with the distance of the liquid level of described thinning agent (31).
8. remote auto sampler according to claim 1, it is characterized in that, described controller is programmable logic controller (PLC) (8), and this programmable logic controller (PLC) (8) is connected with cylinder (7) by the pneumatic valve (9) with source of the gas (91).
9. a sampling method for the remote auto sampler according to any one of claim 1-8, is characterized in that, this remote auto sampling method comprises:
S1, close variable valve (100), open liquid feed valve (43) and air outlet valve (53), the described piston (71) being controlled described cylinder (7) by described programmable logic controller (PLC) (8) is mobile, thus negative pressure is produced in described tank of bleeding (6), force the described liquid fluorinated hydrogen solution (11) in described fluid reservoir (1) to enter in described sampling jar (3) along described drain pipe (2) and described feed tube (4);
S2, described piston (71) the oppositely movement of described cylinder (7) is controlled by described programmable logic controller (PLC) (8), thus malleation is produced in described tank of bleeding (6), the described liquid fluorinated hydrogen solution (11) of compeling in described drain pipe (2) and described feed tube (4) flows back in described fluid reservoir (1).
10. sampling method according to claim 9, it is characterized in that, this remote auto sampling method also comprises: the described piston (71) being controlled described cylinder (7) by described programmable logic controller (PLC) (8) is mobile, thus negative pressure is produced in described tank of bleeding (6), force the described liquid fluorinated hydrogen solution (11) in described fluid reservoir (1) to enter in described wash-bottle (3a) along described drain pipe (2) and described feed tube (4), thus rinse is carried out to described drain pipe (2) and described feed tube (4).
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| CN201510306065.3A CN105043817A (en) | 2015-06-04 | 2015-06-04 | Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution |
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| CN201510306065.3A CN105043817A (en) | 2015-06-04 | 2015-06-04 | Long-distance automatic sampling device and method for liquid-state hydrogen fluoride solution |
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| CN106442813A (en) * | 2016-11-03 | 2017-02-22 | 广东电网有限责任公司电力科学研究院 | Omniseal headspace sampling technology used for measuring dissolved contents in transformer oil |
| CN108204905A (en) * | 2016-12-20 | 2018-06-26 | 中核新能核工业工程有限责任公司 | A kind of device for being suitable for pressing hex metering sampling in hot tank |
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| CN112229832A (en) * | 2020-10-10 | 2021-01-15 | 宜宾海丰和锐有限公司 | Method for detecting content of metal ions in vinyl chloride monomer |
| CN112665919A (en) * | 2020-12-08 | 2021-04-16 | 中核二七二铀业有限责任公司 | Automatic electrolyte sampling device of medium-temperature electrolysis fluorine production equipment |
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| CN114127532A (en) * | 2019-07-17 | 2022-03-01 | 系统科技公司 | Chemical sampling device |
| CN112229832A (en) * | 2020-10-10 | 2021-01-15 | 宜宾海丰和锐有限公司 | Method for detecting content of metal ions in vinyl chloride monomer |
| CN112665919A (en) * | 2020-12-08 | 2021-04-16 | 中核二七二铀业有限责任公司 | Automatic electrolyte sampling device of medium-temperature electrolysis fluorine production equipment |
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Application publication date: 20151111 |