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Proper Operation of Vacuum Based Equipment
  • 00:00Overview
  • 00:43Common Vacuum Pump Designs and Characteristics
  • 02:58Preliminary Safety Precautions
  • 04:21Safety During and After Vacuum Operation
  • 05:56Summary

真空设备的正确运行

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Overview

源: 罗伯特· m Rioux, 阿杰萨特和 #38; 刘志峰, 宾夕法尼亚州立大学, 宾夕法尼亚大学公园, PA

许多实验室程序需要真空。这是最常规的实现在实验室的使用真空泵。除了在低压下工作外, 真空泵还可用于通过疏散和回填使反应堆或烧瓶中的大气迅速变化.

Principles

Procedure

1. 使用个人防护设备 安全眼镜、实验室大衣和面罩在与真空设备一起工作或靠近时必须利用。 必须使用防爆罩来防止飞溅的玻璃或因压力突然变化而产生的碎片. 2。使用适当的油管和设备 始终使用管材、玻璃器皿和其他额定使用真空的设备。使用不当会导致材料失效, 导致爆炸/爆. 定期检查玻璃和油管是否有缺陷/切口, 因为这些都很?…

Applications and Summary

Operations requiring vacuum have multiple hazards associated with them. Vessel implosion can lead to flying glass and other materials, the release of chemicals to the working environment, and potentially fire due to the condensation of liquid oxygen. Vacuum operations should be set up properly and only operated after potential risks have been identified and properly mitigated.

References

  1. NRC (National Research Council). Prudent Practices in the Laboratory. Handling and Management of Chemical Hazards. National Academy Press: Washington, DC, 2011.
  2. Laboratory Vacuum Pump Buyers' Guide, 2012.

Transcript

Vacuum pumps are employed in a wide array of laboratory procedures. Common examples include filtration, drying, degassing, evaporative coating, and mass spectrometry.

Pump equipment must be maintained and operated safely to prevent equipment failures, explosions and chemical release. This video will introduce several common pump designs, discuss common precautions to be observed when setting up vacuum equipment, and demonstrate operational safety.

Let’s begin by exploring various pump designs.

In rotary-vane pumps air and other gases are drawn through an inlet by a rotor. The gases are forced via an oil-sealed exhaust, which prevents backflow, to the outlet leaving the system. Rotary vane pumps can generate vacuums of ten to the negative three Torr. These pumps are self-lubricating, but require oil changes and are vulnerable to corrosion by water vapor.

In scroll pumps air passes through an inlet between two eccentric spiral scrolls, one fixed, the other orbiting. The motion compresses the air and pushes it toward the outlet. Vacuums of ten to the negative two Torr can be achieved. Scroll pumps are “dry” mechanisms – they do not require oil or water, but the scrolls must be periodically replaced as they wear down. Scroll pumps and rotary-vane pumps are suitable for distillation, filtration, and degassing.

A water aspirator is another type of pump often found in laboratories. In this type of pump water enters through an inlet to a high-speed nozzle, and exits as a low-pressure fluid jet. The gases are drawn in through a side port and forced to the outlet. Water aspirators produce vacuums of only 10 Torr. Although they easily connect to ordinary sink faucets, they require large amounts of water. Water aspirators are frequently used for drying and extraction.

Lastly, turbomolecular pumps produce ultrahigh vacuum. Air is forced in through alternating stator and turbine blades that drive the gas molecules through the outlet connected to a roughing pump. Turbomolecular pumps can produce vacuums as low as ten to the negative ten Torr, but require another pump to first lower the pressure to 1 Torr. Turbomolecular pumps are used for electron microscopy, crystal growth, and evaporative coating.

Now that you’re familiar with the designs, let’s examine personal protection and safety measures that should be observed before operating these vacuum pumps.

If possible, operate all vacuum equipment inside a fume hood with the sash lowered. Wear safety goggles and a face shield. These provide protection against chemicals and debris in case the glassware implodes under the vacuum.

Use glassware and equipment rated for use with the expected level of vacuum. Check the glassware and tubing for cracks or other defects. Defective or inappropriate equipment can easily implode under vacuum. Wrap glassware larger than 250 mL in tape, netting, or plastic, as a further precaution against flying debris.

If the procedure is known to generate corrosive vapors, select a pump that can withstand those vapors. Ensure the pump is clean and free from corrosion. For oil pumps, check the oil level and change the oil periodically.

Ensure the pump is level and balanced. Connect the pump outlet to the fume hood exhaust. Securely place tubing inside the hood to prevent the release of chemicals. Ensure all tubing is unrestricted, and that there are no leaks, especially near the flanges.

Now that the vacuum pump is set up, let’s examine safety considerations during and after pump operation.

Connect the pump inlet to the glassware via a cold trap. A cold trap is a glass container that protects the pump by freezing volatile organics evacuated from the apparatus.

During the procedure, the cold trap is submerged in dry ice or a Dewar of liquid nitrogen. Use cryogenic protective equipment when handling these coolants.

A potential hazard is the condensation of oxygen in the cold trap to yield highly explosive liquid nitrogen. To prevent its formation, start the vacuum pump and evacuate the apparatus before submerging the cold trap in liquid nitrogen. Never allow the cold trap to contact liquid nitrogen if not under vacuum, and never open the vacuum line to air with the cold trap in place.

Check the cold trap for condensed solvents and liquid oxygen regularly. If necessary empty the cold trap to prevent solvents entering the tubing and vacuum pump. If liquid oxygen, a light blue fluid, is visible, terminate the procedure and call for assistance, but do not stop the vacuum or remove the liquid nitrogen.

Once the procedure is complete, withdraw the cold trap from the coolant and then switch off the pump. Bleed the vacuum lines slowly before disconnecting the cold trap and pump, to prevent sudden pressurization.

You’ve just watched JoVE’s introduction to lab safety for vacuum-based equipment. You should now be familiar with different types of vacuum pumps, their potential hazards, and precautions to be observed to ensure safe operation. As always, thanks for watching!

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JoVE Science Education Database. JoVE Science Education. Proper Operation of Vacuum Based Equipment. JoVE, Cambridge, MA, (2023).