CN110672762A - Chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition product and preparation method - Google Patents
Chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition product and preparation method Download PDFInfo
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Abstract
The invention discloses a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products and a preparation method thereof. The chromatographic microcolumn comprises a stainless steel tube body, a stationary phase, quartz wool and a sealing element; the stainless steel pipe body is uniformly filled with the stationary phase; quartz wool with preset filling length is respectively filled at two ends of the stainless steel tube body; the sealing element is sleeved at the pipe orifice of the stainless steel pipe body. SF can be separated by adopting the chromatographic microcolumn6Sulfuryl fluoride [ SO ] in decomposition product2F2]Hydrogen sulfide [ H ]2S]Carbonyl sulfide [ COS ]]Thionyl fluoride [ SOF ]2]Sulfur dioxide [ SO ]2]Carbon disulfide [ CS ]2]The sulfur-containing components have the characteristics of high column efficiency, good inertia, difficult damage, good sealing property, high separation degree, good repeatability and strong adsorption resistance to the sulfur-containing components.
Description
Technical Field
The invention relates to the technical field of sulfide separation by gas chromatography, in particular to a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products and a preparation method thereof.
Background
At present, gas chromatography is regarded as the most authoritative detection means as a mature, reliable and extremely high-accuracy detection method. Chromatography is used as an arbitration method when there are many differences in the detection methods. However, in the chromatographic detection method, if the chromatographic column does not separate the detection components well, the detection result has no meaning. The preparation and selection of the sufficient chromatographic column is crucial for the gas chromatographic analysis results.
The available glass tubular column of present detection to the sulphide, glass tubular column have the characteristics that inertia is good, the column is efficient, nevertheless fragile, inconvenient installation, the price is expensive difficult to be accepted by people. Another ptfe column is the most inert and easy to install, however, above 150 ℃, some low molecules (water vapor, oxygen, hydrogen, etc.) will permeate through the porous walls of the ptfe column, causing the stationary phase therein to be damaged, and the column efficiency is low, so that the maximum service temperature should not exceed 260 ℃. The chromatographic columns obtained by the pipes do not achieve ideal effects.
Disclosure of Invention
The invention aims to provide a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products and a preparation method thereof, and aims to solve the problems that the existing chromatographic column is fragile, inconvenient to install, expensive in price or low in column efficiency and limited in use temperature.
In order to achieve the purpose, the invention provides the following scheme:
for analysing sulfur hexafluoride (SF)6) A chromatographic microcolumn for decomposing sulfides in a sulfide, the chromatographic microcolumn comprising: the device comprises a stainless steel pipe body, a stationary phase, quartz wool and a sealing element;
the stainless steel pipe body is uniformly filled with the stationary phase; quartz wool with preset filling length is respectively filled at two ends of the stainless steel tube body; the sealing element is sleeved at the pipe orifice of the stainless steel pipe body.
Optionally, the stainless steel pipe body has an outer diameter of 1/16 ″, an inner diameter of 1mm to 1.2mm, and a length of 2m to 2.5 m.
Optionally, the stationary phase is a modified macromolecule with a granularity of 60-80 meshes.
Optionally, the preset filling length of the quartz wool is 3mm-4 mm.
Optionally, the sealing member comprises an outer surface layer gold-plated nut and a ferrule; the screw cap and the clamping sleeve are sleeved at the pipe orifice of the stainless steel pipe body; the nut is used for screwing the clamping sleeve.
A method of preparing a chromatographic microcolumn for the analysis of sulfides in sulfur hexafluoride hydrolysates, the method comprising:
preparing a stainless steel pipe body with a clean and smooth inner wall;
modifying the inner wall of the stainless steel pipe body to form a modified stainless steel pipe body;
filling a stationary phase and quartz wool in the stainless steel pipe body after the modification treatment;
and sleeving a sealing element at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn.
Optionally, prepare the clean smooth stainless steel body of inner wall, specifically include:
preparing a stainless steel pipe body with a clean and smooth inner wall; the stainless steel pipe body has an outer diameter of 1/16', an inner diameter of 1mm-1.2mm, and a length of 2m-2.5 m.
Optionally, the right the inner wall of stainless steel pipe body carries out modification treatment, forms the stainless steel pipe body after modification treatment, specifically includes:
soaking the inner wall of the stainless steel pipe body in a 10% hot sodium hydroxide solution, and washing the inner wall of the stainless steel pipe body to be neutral by water;
further soaking the inner wall of the stainless steel pipe body with 5% dilute hydrochloric acid, and then washing the inner wall of the stainless steel pipe body to be neutral;
and finally, carrying out sulfur passivation treatment on the inner wall of the stainless steel pipe body to enable inert substances resistant to sulfur corrosion to be attached to the surface of the inner wall of the stainless steel pipe body.
Optionally, the modified stainless steel tube body is filled with a stationary phase and quartz wool, and the method specifically includes:
filling quartz wool with a preset filling length at one end of the modified stainless steel tube body; the preset filling length is 3mm-4 mm;
one end of the stainless steel tube body filled with the modified quartz wool is connected with an air inlet of a vacuum pump, and the other end of the stainless steel tube body is connected with a container filled with a stationary phase; the stationary phase is a modified macromolecule with the granularity of 60-80 meshes;
keeping the vacuum pressure of the vacuum pump stable at 0.3mpa, pumping the stationary phase into the modified stainless steel pipe body, and uniformly filling the stationary phase in the modified stainless steel pipe body;
and disconnecting the vacuum pump, and filling quartz wool with a preset filling length at the other end of the modified stainless steel tube body.
Optionally, the mouth of pipe department cup joints the sealing member of stainless steel body, forms the chromatography microcolumn specifically includes:
carrying out gold plating treatment on the outer surface layers of the matched nut and clamping sleeve to form the nut and the clamping sleeve with gold plated outer surface layers;
and sleeving the nut with gold plated outer surface layer and the clamping sleeve at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products and a preparation method thereof, wherein the chromatographic microcolumn comprises a stainless steel tube body, a stationary phase, quartz wool and a sealing element; the stainless steel pipe body is uniformly filled with the stationary phase; quartz wool with preset filling length is respectively filled at two ends of the stainless steel tube body; the sealing element is sleeved at the pipe orifice of the stainless steel pipe body. SF can be separated by adopting the chromatographic microcolumn6Sulfuryl fluoride [ SO ] in decomposition product2F2]Hydrogen sulfide [ H ]2S]Carbonyl sulfide [ COS ]]Thionyl fluoride [ SOF ]2]Sulfur dioxide [ SO ]2]Carbon disulfide [ CS ]2]The sulfur-containing components have the characteristics of high column efficiency, good inertia, difficult damage, good sealing property, high separation degree, good repeatability and strong adsorption resistance to the sulfur-containing components.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings provided by the present invention without any creative effort.
FIG. 1 is a schematic structural diagram of a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products according to the present invention;
the numbers in the figures are respectively: 1 stainless steel tube body, 2 stationary phases, 3 quartz wool and 4 sealing elements.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products and a preparation method thereof, and aims to solve the problems that the existing chromatographic column is fragile, inconvenient to install, expensive in price or low in column efficiency and limited in use temperature.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a schematic structural diagram of a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride hydrolysate according to the present invention. Referring to fig. 1, the present invention provides a chromatographic microcolumn for analyzing sulfides in sulfur hexafluoride decomposition products, including: stainless steel body 1, stationary phase 2, quartz wool 3 and sealing member 4. The fixed phase 2 is uniformly filled in the stainless steel pipe body 1. The two ends of the stainless steel tube body 1 are respectively filled with quartz wool 3 with preset filling length. The sealing element 4 is sleeved at the pipe orifice of the stainless steel pipe body 1. And two ends of the stainless steel pipe body 1 are respectively sleeved with the sealing element 4. The chromatographic microcolumn pair separates SF6Sulfuryl fluoride [ SO ] in (sulfur hexafluoride) decomposition product2F2]Hydrogen sulfide [ H ]2S]Carbonyl sulfide [ COS ]]Thionyl fluoride [ SOF ]2]Sulfur dioxide [ SO ]2]Carbon disulfide [ CS ]2]The sulfur-containing components have the characteristics of high separation degree, good repeatability and strong adsorption prevention on the sulfur-containing components.
Wherein, the stainless steel pipe body 1 has an outer diameter of 1/16 "(inches), an inner diameter of 1mm-1.2mm and a length of 2m-2.5 m. The invention adopts the stainless steel tube body with the outer diameter of 1/16' as the carrier, and has the characteristics of high column efficiency and large number of tower plates. In the actual use process, in order to facilitate installation, the middle part of the stainless steel pipe body 1 may be wound into a spiral shape, as shown in fig. 1.
The inner wall of the stainless steel pipe body 1 is clean and smooth, the inner wall of the stainless steel pipe body 1 is soaked in 10% hot sodium hydroxide solution and then washed to be neutral by water. Further processing, soaking with 5% diluted hydrochloric acid, and washing to neutrality. Finally, the stainless steel pipe body is subjected to sulfur passivation treatment, and inert substances resistant to sulfur corrosion are attached to the inner surface of the pipe body after passivation, so that the pipe body has strong chemical inertness, catalytic or chemical changes of the detected substances and the pipe body are prevented, and stable and reliable conditions are provided for detecting sulfides. The inert material that is resistant to sulfur corrosion is typically a passivation film.
The stationary phase 2 is a modified macromolecule with the granularity of 60-80 meshes, and the macromolecule stationary phase 2 has strong chemical inertia. In practical application, the stationary phase 2 can be made of polymer materials of the same series or the same properties of Porapak R, Porapak S and Porapakt.
The stationary phase 2 is uniformly filled in the stainless steel pipe body 1. During filling, one end of the stainless steel tube body 1 is filled with quartz wool 3, the end is connected with an air inlet of a vacuum pump, and the other end of the stainless steel tube body 1 is connected with a container filled with a stationary phase 2. The stationary phase 2 in the container is pumped into the stainless steel tube body 1 by vacuum pump. When the vacuum is pumped, the vacuum pressure of the vacuum pump is stabilized at 0.3mpa, and the filling volume of the stationary phase 2 is 2.3mL-2.8mL, so that the filling tightness of the stationary phase 2 is uniform and effective.
The two ends of the stainless steel tube body 1 are filled with the anti-adsorption quartz wool 3, the filling lengths are respectively 3mm-4mm, and the purpose is to ensure that the mobile phase has good permeability and prevent the stationary phase from being brought out by the mobile phase and being incapable of reacting with the measured substance.
The chromatographic micro-column is sealed by hard sealing with a 316L stainless steel cutting sleeve and a screw cap, and is characterized in that the screw cap and the outer layer of the cutting sleeve are plated with gold. Specifically, the sealing member 4 comprises a nut and a ferrule with gold-plated outer surface layers. The nut with the cutting ferrule all cup joints the mouth of pipe department of stainless steel body 1. The cutting ferrule has the tapering, the nut is used for screwing the cutting ferrule, through the nut extrusion cutting ferrule, produces deformation to reach sealed effect. The sealing member is generally connected between the chromatography micro-column and the detector or the switching valve of the gas chromatography for realizing the sealing connection between the chromatography micro-column and the detector or the switching valve.
The two ends of the stainless steel pipe body 1 are respectively sleeved with one sealing element 4, and the sealing element 4 is usually located at a position about 2mm away from the pipe orifice of the stainless steel pipe body 1. The outer surface layer of the sealing element 4 is subjected to gold plating treatment, so that the sealing element has strong chemical inertia, certain flexibility and ductility, is convenient to mount and dismount, and can be repeatedly used for multiple times to achieve the effect of no leakage.
The chromatographic micro-column for analyzing the sulfide by the gas chromatography disclosed by the invention has the characteristics of high column efficiency, good inertia, difficult damage, convenient installation and good sealing property through the improvement on the chromatographic column technology, is low in manufacturing cost, does not have the limitation of use temperature, and is an ideal chromatographic column for analyzing the sulfide at present.
The invention further provides a preparation method of the chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products, which comprises the following steps:
preparing a stainless steel pipe body with a clean and smooth inner wall;
modifying the inner wall of the stainless steel pipe body to form a modified stainless steel pipe body;
filling a stationary phase and quartz wool in the stainless steel pipe body after the modification treatment;
and sleeving a sealing element at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn. The chromatographic micro-column separates sulfuryl fluoride (SO) from the chromatographic micro-column2F2]Hydrogen sulfide [ H ]2S]Carbonyl sulfide [ COS ]]Thionyl fluoride [ SOF ]2]Sulfur dioxide [ SO ]2]Carbon disulfide [ CS ]2]The equal sulfur-containing components have high separation degree, good repeatability and strong adsorption resistance to the sulfur-containing componentsThe characteristics of (1).
Wherein, prepare the clean smooth stainless steel body of inner wall, specifically include:
preparing a stainless steel pipe body with a clean and smooth inner wall; the stainless steel pipe body has an outer diameter of 1/16', an inner diameter of 1mm-1.2mm, and a length of 2m-2.5 m. The stainless steel tube with the outer diameter of 1/16' is used as a carrier, and has the characteristics of high column efficiency and large number of tower plates.
The right the inner wall of stainless steel body carries out modification treatment, forms the stainless steel body after modification treatment, specifically includes:
soaking the inner wall of the stainless steel pipe body in a 10% hot sodium hydroxide solution, and washing the inner wall of the stainless steel pipe body to be neutral by water;
further soaking the inner wall of the stainless steel pipe body with 5% dilute hydrochloric acid, and then washing the inner wall of the stainless steel pipe body to be neutral;
and finally, carrying out sulfur passivation treatment on the inner wall of the stainless steel pipe body, and attaching the inert substance resistant to sulfur corrosion to the surface of the inner wall of the stainless steel pipe body after passivation so that the stainless steel pipe body has strong chemical inertness, thereby preventing the detected substance from generating catalysis or chemical change with the pipe body and providing stable and reliable conditions for detecting sulfide.
The stainless steel pipe body after the modification treatment is filled with a fixed phase and quartz wool, and the method specifically comprises the following steps:
filling quartz wool with a preset filling length at one end of the modified stainless steel tube body; the preset filling length is 3mm-4 mm;
one end of the stainless steel tube body filled with the modified quartz wool is connected with an air inlet of a vacuum pump, and the other end of the stainless steel tube body is connected with a container filled with a stationary phase; the stationary phase is a modified macromolecule with the granularity of 60-80 meshes;
keeping the vacuum pressure of the vacuum pump stable at 0.3mpa, pumping the stationary phase into the modified stainless steel pipe body, and uniformly filling the stationary phase in the modified stainless steel pipe body;
and disconnecting the vacuum pump, and filling quartz wool with a preset filling length at the other end of the modified stainless steel tube body.
The two ends of the stainless steel tube body are filled with anti-adsorption quartz wool, the filling lengths are respectively 3mm-4mm, and the purpose is that the mobile phase has good permeability, and the stationary phase is prevented from being brought out by the mobile phase and cannot react with a measured substance.
The stationary phase has strong chemical inertia and is modified macromolecule with granularity of 60-80 meshes. During filling, one end of the chromatographic column is filled with quartz wool, the end is connected with an air inlet of a vacuum pump, the vacuum pressure of the pump is stabilized at 0.3mpa, and the filling volume of the stationary phase is 2.3mL-2.8mL, so that the filling tightness of the stationary phase is uniform and effective.
The mouth of pipe department of stainless steel body cup joints the sealing member, forms the little post of chromatogram specifically includes:
carrying out gold plating treatment on the outer surface layers of the matched nut and clamping sleeve to form the nut and the clamping sleeve with gold plated outer surface layers;
and sleeving the nut with gold plated outer surface layer and the clamping sleeve at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn.
The chromatographic micro-column is sealed by hard sealing with a 316L stainless steel nut and a ferrule. The outer surface layers of the nut and the clamping sleeve are subjected to gold plating treatment, so that the nut and the clamping sleeve have strong chemical inertia, certain flexibility and ductility, convenience in mounting and dismounting is realized, and the effect of no leakage can be achieved by repeated use.
The chromatographic micro-column prepared by the preparation method has the characteristics of high separation degree, good repeatability and strong anti-adsorption property on sulfur-containing components, and provides a durable and efficient chromatographic column for detecting the sulfur-containing components by adopting a gas chromatography.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
The principles and embodiments of the present invention have been described herein using specific examples, which are presented solely to aid in the understanding of the apparatus and its core concepts; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products, said chromatographic microcolumn comprising: the device comprises a stainless steel pipe body, a stationary phase, quartz wool and a sealing element;
the stainless steel pipe body is uniformly filled with the stationary phase; quartz wool with preset filling length is respectively filled at two ends of the stainless steel tube body; the sealing element is sleeved at the pipe orifice of the stainless steel pipe body.
2. The chromatography microcolumn of claim 1, wherein the stainless steel tube body has an outer diameter of 1/16 ", an inner diameter of 1mm to 1.2mm, and a length of 2m to 2.5 m.
3. The micro-column according to claim 1, wherein the stationary phase is a modified polymer having a particle size of 60-80 mesh.
4. The chromatography microcolumn according to claim 1, wherein the preset packing length of the quartz wool is 3mm to 4 mm.
5. The chromatography microcolumn of claim 1, wherein the sealing member comprises an outer surface layer gold plated nut and ferrule; the screw cap and the clamping sleeve are sleeved at the pipe orifice of the stainless steel pipe body; the nut is used for screwing the clamping sleeve.
6. A method for producing a chromatographic microcolumn for analyzing sulfide in sulfur hexafluoride decomposition products, the method being used for producing the chromatographic microcolumn of claim 1; the preparation method comprises the following steps:
preparing a stainless steel pipe body with a clean and smooth inner wall;
modifying the inner wall of the stainless steel pipe body to form a modified stainless steel pipe body;
filling a stationary phase and quartz wool in the stainless steel pipe body after the modification treatment;
and sleeving a sealing element at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn.
7. The method according to claim 6, wherein the step of preparing the stainless steel pipe body with a clean and smooth inner wall specifically comprises:
preparing a stainless steel pipe body with a clean and smooth inner wall; the stainless steel pipe body has an outer diameter of 1/16', an inner diameter of 1mm-1.2mm, and a length of 2m-2.5 m.
8. The preparation method according to claim 6, wherein the modifying treatment is performed on the inner wall of the stainless steel pipe body to form the modified stainless steel pipe body, and specifically comprises:
soaking the inner wall of the stainless steel pipe body in a 10% hot sodium hydroxide solution, and washing the inner wall of the stainless steel pipe body to be neutral by water;
further soaking the inner wall of the stainless steel pipe body with 5% dilute hydrochloric acid, and then washing the inner wall of the stainless steel pipe body to be neutral;
and finally, carrying out sulfur passivation treatment on the inner wall of the stainless steel pipe body to enable inert substances resistant to sulfur corrosion to be attached to the surface of the inner wall of the stainless steel pipe body.
9. The preparation method according to claim 6, wherein the filling of the stainless steel tube body after the modification treatment with the stationary phase and the quartz wool specifically comprises:
filling quartz wool with a preset filling length at one end of the modified stainless steel tube body; the preset filling length is 3mm-4 mm;
one end of the stainless steel tube body filled with the modified quartz wool is connected with an air inlet of a vacuum pump, and the other end of the stainless steel tube body is connected with a container filled with a stationary phase; the stationary phase is a modified macromolecule with the granularity of 60-80 meshes;
keeping the vacuum pressure of the vacuum pump stable at 0.3mpa, pumping the stationary phase into the modified stainless steel pipe body, and uniformly filling the stationary phase in the modified stainless steel pipe body;
and disconnecting the vacuum pump, and filling quartz wool with a preset filling length at the other end of the modified stainless steel tube body.
10. The preparation method according to claim 6, wherein a sealing member is sleeved at the orifice of the stainless steel tube body to form the chromatographic microcolumn, and specifically comprises:
carrying out gold plating treatment on the outer surface layers of the matched nut and clamping sleeve to form the nut and the clamping sleeve with gold plated outer surface layers;
and sleeving the nut with gold plated outer surface layer and the clamping sleeve at the pipe orifice of the stainless steel pipe body to form the chromatographic microcolumn.
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