Pressure-resistant glass bottle for chromatographic mass spectrometry

Abstract

A pressure-resistant glass bottle for chromatographic mass spectrometry comprises a bottle body, a conical opening is formed in the top of the bottle body, and the cross sectional area of the conical opening is gradually increased in the direction away from the bottle body; a threaded section is arranged at the top of the conical opening, a glass plug arranged in a matched abutting mode is arranged in the conical opening, an abutting threaded rod is arranged in the threaded section in a threaded mode, and the bottom of the abutting threaded rod abuts against the glass plug. The glass plug is additionally arranged at the conical opening of the bottle body, and the abutting threaded rod is matched, so that the double-sealing and pressure-bearing effects are achieved.

Description

Technical Field

[0001] This application relates to a pressure-resistant glass vial for chromatography-mass spectrometry analysis. Background Technology

[0002] Pressure-resistant glass bottles are widely used in organic synthesis, thermal melting, and pressure extraction. To maintain good sealing, rubber rings are typically used. However, under the corrosive effects of high-temperature solvents, substances within the rubber rings can leach out or decompose, contaminating the sample. Furthermore, during use, the PTFE threaded stoppers wear down and shed fine debris, further contaminating the sample. Additionally, when analyzing samples using chromatography / mass spectrometry, especially when analyzing trace compounds, contaminants in the sample can cause interference, making it difficult to determine the source of impurity peaks. Therefore, this severely impacts both qualitative and quantitative analysis using chromatography / mass spectrometry. Utility Model Content

[0003] To address the aforementioned problems, this application proposes a pressure-resistant glass vial for chromatographic and mass spectrometric analysis, comprising a vial body with a conical opening at the top. The cross-sectional area of ​​the conical opening gradually increases away from the vial body. A threaded section is provided at the top of the conical opening, and a glass stopper is fitted inside the conical opening to abut against it. A threaded rod is threaded into the threaded section, with its bottom abutting against the glass stopper. This application achieves both a double seal and pressure resistance by adding a glass stopper to the conical opening of the vial body and using a threaded rod to abut against it.

[0004] Preferably, a polytetrafluoroethylene (PTFE) explosion-proof cover is fitted over the outside of the bottle; the PTFE explosion-proof cover has several observation holes. This application uses a PTFE explosion-proof cover on the outside of the bottle, which improves the pressure resistance of the device and expands its application range.

[0005] Preferably, the glass stopper is a ground glass stopper; the glass stopper is a truncated cone.

[0006] Preferably, the top of the pressing threaded rod is provided with an enlarged operating protrusion.

[0007] Preferably, the top of the pressing threaded rod is provided with an enlarged operating protrusion, and a transition connecting section is provided between the enlarged operating protrusion and the pressing threaded rod.

[0008] Preferably, the bottom of the threaded rod has a bottom protrusion, and an annular groove is provided on the side of the bottom protrusion. A sealing ring is provided in the annular groove, and the bottom of the sealing ring abuts against the glass stopper; the sealing ring is a fluororubber sealing ring. This application, by using a glass stopper and an upper sealing ring to press against each other, isolates the solvent inside the bottle from contact with the sealing ring, effectively preventing trace contaminants such as antioxidants, plasticizers, alkanes, and oligomers that may be present in the sealing ring from contaminating the sample. Simultaneously, it effectively prevents solvent corrosion of the sealing ring, extending its service life.

[0009] Preferably, the top of the glass stopper is provided with two opposing vertical operating grooves; the vertical operating grooves are arc-shaped grooves.

[0010] Preferably, a connecting through hole is provided between the vertical operating slots, a connecting operating line is inserted into the connecting through hole, and the other end of the connecting operating line is inserted through the pressing threaded rod.

[0011] Preferably, a bottom arc plate is provided at the bottom of the bottle, and a stirring magnet is provided inside the bottom arc plate.

[0012] Preferably, the threaded rod is a polytetrafluoroethylene rod. This application can effectively prevent trace substances that are difficult to clean from remaining on the sealing ring after the experiment from causing cross-contamination in the next experiment, thereby improving the accuracy of the experiment and facilitating the qualitative and quantitative analysis of trace organic matter in the sample by chromatography / mass spectrometry, ensuring the correctness of the analytical results.

[0013] This application can bring the following beneficial effects:

[0014] 1. This application achieves a double sealing and pressure-bearing function by adding a glass stopper to the conical opening of the bottle and cooperating with a threaded rod to resist pressure.

[0015] 2. This application has a polytetrafluoroethylene explosion-proof cover on the outside of the bottle, which improves the pressure resistance of this application and expands the scope of application of the device.

[0016] 3. This application isolates the solvent inside the bottle from contact with the sealing ring by setting a glass stopper and an upper sealing ring to press against each other. This effectively prevents trace contaminants such as antioxidants, plasticizers, alkanes, and oligomers that may be present in the sealing ring from contaminating the sample. At the same time, it can effectively prevent the solvent from corroding the sealing ring and extend the service life of the sealing ring.

[0017] 4. This application can effectively prevent trace substances that are difficult to clean from remaining on the sealing ring after the experiment from causing cross-contamination in the next experiment, thereby improving the accuracy of the experiment and facilitating the qualitative and quantitative analysis of trace organic matter in the sample by chromatography / mass spectrometry, ensuring the correctness of the analytical results. Attached Figure Description

[0018] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings:

[0019] Figure 1 This is a schematic diagram of the structure of this application.

[0020] Figure 2 This is a schematic diagram of a ground glass stopper.

[0021] Figure 3 The total ion chromatograms and mass spectra of the products of the reaction of hexadecanoic acid and methanol in two different apparatuses are shown.

[0022] Figure 4 The total ion chromatogram and mass spectrum of hexadecanoic acid hexadecanoate are shown.

[0023] Figure 5 This is the total ion chromatogram of the cyclohexane extract.

[0024] Figure 6 This is a distribution diagram of the group components of the cyclohexane extract. Detailed Implementation

[0025] To clearly illustrate the technical features of this solution, the following detailed description, in conjunction with the accompanying drawings, will be provided.

[0026] For structural parts, such as Figure 1-2 As shown, a pressure-resistant glass vial for chromatography-mass spectrometry analysis includes a vial body 1, a conical opening 2 at the top of the vial body 1, the cross-sectional area of ​​the conical opening 2 gradually increasing away from the vial body 1; a threaded section 3 at the top of the conical opening 2, a glass stopper 4 fitted inside the conical opening 2, and a pressing threaded rod 5 threaded inside the threaded section 3, the bottom of the pressing threaded rod 5 abutting against the glass stopper 4.

[0027] A polytetrafluoroethylene (PTFE) explosion-proof cover 6 is fitted over the outside of the bottle body 1; several observation holes 7 are provided on the PTFE explosion-proof cover 6. The glass stopper 4 is a ground glass stopper; the glass stopper 4 is a truncated cone. An enlarged operating protrusion 8 is provided at the top of the pressing threaded rod 5, and a transition connecting section 9 is provided between the enlarged operating protrusion 8 and the pressing threaded rod 5. A bottom protrusion 10 is provided at the bottom of the pressing threaded rod 5, and an annular groove 11 is provided on the side of the bottom protrusion 10. A sealing ring 12 is provided in the annular groove 11, and the bottom of the sealing ring 12 abuts against the glass stopper 4; the sealing ring 12 is a fluororubber sealing ring.

[0028] The top of the glass stopper 4 has two opposing vertical operating grooves 13; the vertical operating grooves 13 are arc-shaped grooves. A connecting through hole 14 is provided between the vertical operating grooves 13, and a connecting operating line (not shown in the figure) passes through the connecting through hole 14. The other end of the connecting operating line passes through the pressing threaded rod 5. A bottom arc-shaped plate 15 is provided at the bottom of the bottle body 1, and a stirring magnet 16 is provided within the bottom arc-shaped plate 15. The pressing threaded rod 5 is a polytetrafluoroethylene rod.

[0029] In use, thoroughly clean all components of this application, add the materials and solvents to bottle 1, and place the stirring magnet inside. Hold the glass stopper 4 by the handle and insert it into the conical opening 2, leveling it. Install the sealing ring 12, and then tighten the pressing threaded rod 5. Place the PTFE explosion-proof cover over the middle of bottle 1. Place the assembled device into the temperature-controlled magnetic stirring apparatus, and secure the upper part with an iron stand, then begin the experiment. After the experiment, wait for this application to cool to room temperature before unscrewing the pressing threaded rod 5, removing the sealing ring and the ground glass stopper 4, and taking out the experimental product.

[0030] To characterize the validity of this application, the following experiments were conducted:

[0031] Example 1:

[0032] S101: Clean the present application thoroughly and use a rotary evaporator to distill and purify methanol and petroleum ether to obtain refined methanol and refined petroleum ether.

[0033] S102: Weigh 0.5g of hexadecanoic acid and add it to 100mL of this application solution. Add a magnetic stir bar, 30mL of purified methanol, 0.1g of Novozyme 435 lipase catalyst, and 1.4g of molecular sieve. Insert the ground glass stopper and sealing ring, and tighten the threaded rod.

[0034] S103: Place this application in a water bath at 85°C, turn on magnetic stirring, and keep the temperature constant for 36 hours.

[0035] S104: After the reaction is complete, turn off the heating and stirring, cool to room temperature, unscrew the PTFE threaded plug, and remove the sealing ring and ground glass stopper.

[0036] S105: The reaction mixture obtained in S4 is transferred to a modified Soxhlet extractor and extracted with refined petroleum ether. The product is obtained by rotary evaporation.

[0037] S106: Analyze the product obtained in S5 using gas chromatography / mass spectrometry, such as... Figure 3 As shown, the total ion chromatogram (3a) and mass spectrum (3c) of the product were obtained. After analysis, the product was found to be methyl palmitate with a purity of 99.6%.

[0038] For comparison, a commercially available pressure-resistant glass bottle was purchased, which is similar to the apparatus described in this application except for the unground glass stopper and the explosion-proof cover. The above experimental steps were repeated under the same experimental conditions to obtain the reaction product. The product was analyzed using gas chromatography / mass spectrometry, as shown... Figure 3 As shown, the total ion chromatogram (3b), the mass spectrum of methyl palmitate (3c), and the mass spectrum of phosphorus-containing antioxidant impurities (3d) of the product were obtained. After analysis, it was found that the product was methyl palmitate with a purity of 98.9% and the content of phosphorus-containing antioxidant impurities was 1.1%.

[0039] Example 2:

[0040] S201: Clean the present application thoroughly and use a rotary evaporator to distill and purify the petroleum ether to obtain refined petroleum ether.

[0041] S202: Weigh 0.49g of hexadecanoic acid and 0.47g of hexadecyl alcohol and add them to 100mL of this application. Add a magnetic stir bar, 0.1g of Novozyme 435 lipase catalyst, and 1g of molecular sieve. Insert a ground glass stopper and sealing ring, and tighten the threaded rod.

[0042] S203: Place this application in a water bath at 85°C and fix it with an iron stand. Turn on the magnetic stirring and keep it at a constant temperature for 36 hours.

[0043] S204: After the reaction is complete, turn off the heating and stirring, cool to room temperature, unscrew the PTFE threaded plug, and remove the sealing ring and ground glass stopper.

[0044] S205: The reaction mixture obtained in S4 is transferred to a modified Soxhlet extractor and extracted with refined petroleum ether. The product is obtained by rotary evaporation.

[0045] S206: Analyze the product obtained in S5 using gas chromatography / mass spectrometry, such as... Figure 4 As shown, the total ion chromatogram and mass spectrum of the product were obtained. After analysis, the product was determined to be hexadecanoic acid hexadecyl ester with a purity of 99.3%.

[0046] Example 3

[0047] S301: Fresh low-rank coal is crushed, passed through a 200-mesh sieve, and vacuum dried to obtain experimental raw materials; this application is disassembled and cleaned; cyclohexane is distilled and purified using a rotary evaporator to obtain refined cyclohexane.

[0048] S302: Add 2g of the experimental material obtained in S1 to this application, add a stirring magnet, add 50mL of purified cyclohexane; place the cleaned ground glass stopper into the neck of the glass bottle body and tighten it, then put in the sealing ring and tighten the pressing thread rod.

[0049] S303: Place this application in a 90°C magnetically stirred water bath, turn on the magnetic stirring, and maintain the temperature for 2 hours.

[0050] S304: After extraction, turn off heating and stirring, cool to room temperature, unscrew the PTFE threaded plug, and remove the sealing ring and ground glass stopper.

[0051] S305: Filter the extraction mixture obtained in S4 to obtain a cyclohexane extract. Remove the solvent from the extract by rotary evaporation to obtain a cyclohexane extract with an extraction rate of 0.7%.

[0052] S306: The cyclohexane extract obtained in S5 was analyzed using gas chromatography / mass spectrometry, such as... Figure 5 As shown, the total ion current chromatogram was obtained. Figure 6 As shown, the extract contained 112 organic compounds detectable by gas chromatography / mass spectrometry. Among them, alkanes, aromatics, and hopanes were present in relatively high amounts, accounting for 27.2%, 25.4%, and 19.6%, respectively. The compound with the highest content was arsenic. Phthalate plasticizers and phosphorus-containing antioxidants were not detected.

[0053] The above are merely embodiments of this application and are not intended to limit the scope of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of the claims of this application.

Claims

1. A pressure-resistant glass vial for chromatographic and mass spectrometric analysis, characterized in that: The device includes a bottle body with a conical opening at the top, the cross-sectional area of ​​which gradually increases away from the bottle body; a threaded section at the top of the conical opening; a glass stopper that abuts against the conical opening; and a threaded rod that abuts against the glass stopper at the bottom of the threaded section.

2. The pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 1, characterized in that: A polytetrafluoroethylene (PTFE) explosion-proof cover is fitted over the outside of the bottle; several observation holes are provided on the PTFE explosion-proof cover.

3. The pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 1, characterized in that: The glass stopper is a ground glass stopper; the glass stopper is a truncated cone.

4. The pressure-resistant glass vial for chromatographic mass spectrometry analysis as described in claim 1, characterized in that: An enlarged operating protrusion is provided at the top of the pressing threaded rod, and a transition connecting section is provided between the enlarged operating protrusion and the pressing threaded rod.

5. The pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 4, characterized in that: The bottom of the threaded rod is provided with a bottom protrusion, and an annular groove is provided on the side of the bottom protrusion. A sealing ring is provided in the annular groove, and the bottom of the sealing ring abuts against the glass plug. The sealing ring is a fluororubber sealing ring.

6. The pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 1, characterized in that: The top of the glass stopper is provided with two opposing vertical operating grooves; the vertical operating grooves are arc-shaped grooves.

7. A pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 6, characterized in that: A connecting through hole is provided between the vertical operating slots, and a connecting operating line is inserted into the connecting through hole. The other end of the connecting operating line is inserted through the pressing threaded rod.

8. The pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 1, characterized in that: A bottom arc plate is set at the bottom of the bottle, and a stirring magnet is set inside the bottom arc plate.

9. A pressure-resistant glass vial for chromatographic and mass spectrometric analysis as described in claim 1, characterized in that: The threaded rod used for pressing is made of polytetrafluoroethylene.

Images