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Gary S. Coyne - A Practical Guide to Materials, Equipment, and Technique.pdf
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446

Vacuum Systems

1.When possible, usea gas over a liquid.

2.Do not spray or squirt a liquid on. Usea cotton swab (or Kimwipe) to wipe it across parts of the system. Inaddition to safety, this method provides more control in finding leaks.

3.Solvents can damage parts of your system such as O-rings, causing a greater leak than theone you were originally trying to find. In addition, if the solvent drips on a water hose andcreates a hole, you then have a water leak and a mess. If it drips on electric wires, you mayhave a short.

4.All of the chemicals listed in Table 7.14 are dangerous to breathe or

have in contact with skin from short to extended periods of time. Some of the chemicals listed have severe OSHA restrictions foruse without a fume hood, andsome aretoxic chemicals andshould not beused at all (such ascarbon tetrachloride and xylene).

5.Do not have any open flames orsparks while working onleak detection. Unplug iongauges and other electrical equipment.

6.Besure to have plenty of ventilation andlimit yourself to thefirst three liquids in Table 7.14. These liquids are(relatively) the safest, andthey are the best from the list. Still, you should use a buddy system, and check with OSHA and/or local/state regulations to verify if there are

any legal restrictions onthe uses of any of these chemicals in your area.

7.When possible, select a low-vapor-pressure liquid over a high-vapor- pressure liquid toprovide faster cleanup time. Inaddition, nonpolar solvents aremore easily removed from glassware than polar solvents (for example, methanol vs. acetone).

8.When spraying probe gases on a vacuum system, be sure to start at the top with gases less dense than air and start at the bottom with gases denser than air.

Other aspects ofTurnbull's four factors will beconsidered further in Sec. 7.6.9.

7.6.7 The Tesla Coil

If you have a glass system andcanachieve a vacuum between approximately 10 to approximately 10~3 torr, then you can use a Tesla coil (sometimes called a "sparker") to look for moderate-size leaks. Because this range is the vacuum range of a mechanical vacuum pump, theTesla coil provides anexcellent tool for examining such systems.

The Tesla coil will ionize thegas molecules remaining in a vacuum systemand cause them to glow. Above pressures of about 10torr the gas molecules quench a discharge. That is, they aresoclose together they lose their extra energy bybumping into other molecules rather than giving off light. Below 10"3 torr, the mole-

Leak Detection and Location 7.6

 

 

 

447

_

~.

Insulated handle

 

Control knob •—^

 

r

 

 

Power cord ^ 3

 

> = ^ J ^ -

Wire on tip

Light-duty Tesla Coil

 

Power cord

 

 

Insulated handle

^~

 

Control knob

/

,

Heavy-duty Tesla Coil

Fig. 7.57 The lightand heavy-duty Tesla coil.

cules are too far apart and the mean free paths are too long to maintain a discharge.

As the tip of a Tesla coil is slowly waved within 1-3 cm of an evacuated glass vacuum system, the gases remaining will discharge with a glow characteristic of the gases within the system. If you bring theTesla coil near a leak, a large white spark will jump from thetip of the coil to thespecific leak spot. This event is very dramatic anddemonstrates the location of a leak in a very effective manner. The spark is actually seeking ground, and the leak provides a path to the discharge inside the vacuum system. In turn, this discharge (which is an electrical conductor) provides a path to themechanical pump for completion of the ground.

Metal components confound Tesla coil use: Their ground is easier to obtain than the ground found by passing through a glass leak andthepoorer conducting discharge within.

There area fewlimitations to theuseof a Tesla coil:

1.It cannot be used near metal clamps or glass-to-metal seals on a glass system. Themetal provides a ground for theelectric discharge, bypassing theionization of the gasinside thesystem.

2.A large quantity of very small holes mayprevent youfrom obtaining a decent vacuum. However, none of the holes may belarge enough for the Tesla coil to indicate a leak.

3.The self-contained Tesla coils often found in many labs are recommended by themanufacturers notto be used for longer than 10minutes of continuous operation. If your needs require long continuous useona consistent basis, heavy-duty Tesla coils are available that can be used continuously. These coils areeasily identified because they have small boxes (approximately 5 in. x 5 in. x 8 in) connected to their hand-held sections. These hand-held sections arethesame asthose found on standard light-duty Tesla coils (see Fig. 7.57).

4.TheTesla coil will not find a leak within a demountable (seals such as stopcocks orjoints) that is caused by poor application of grease or old stopcock grease that hassheared.

448

Vacuum Systems

5.The Tesla coil should not be used near O-ring joints because the coil can destroy the O-ring by burning a strip across its side.

6.The Tesla coil should not be used near intentionally thin sections of glass (such as a break-off) because it can punch a hole through such a section.

It is unlikely that a leak could develop on a glass tube that has not received stress or that has not been worked on by a glassblower. Therefore to save time, simply pass the Tesla coil around areas where glass sections have been joined (see Fig. 7.58).* If there is a twoor three-fingered clamp in an area that needs to be tested, the clamp must be removed to properly check the seal. To spark check for cracks around hooks placed near a joint, place a rubber stopper in the end of the joint and then open up the stopcock to evacuate that section.

The spark from a Tesla coil is very powerful and can punch its way through thin sections of glass (see Point 6 above). Keep the coil away from known thin sections in which you wish to maintain integrity, such as break-offs. Most texts on vacuum technique recommend that the Tesla coil not be allowed to sit over weak areas for fear of "punching" a hole through the glass. This author disagrees with this reticence because if there is not a hole in a potentially weak area now, there may very likely be one in the area some time in the future. Therefore, go ahead and provide some stress while you are in a position to do something about any holes that develop. Otherwise a hole may develop either in the middle of an experiment or when repair and/or personnel are not available or as convenient. In addition, It is important that all gauge controllers be turned off before initiating Tesla coil testing. The charge from the Tesla coil can destroy the controller's electronics.

Some extra Tesla coil tips are as follows:

Glass should be

f

\

Where there is no apparent distortion

checked for leaks in

V.

J

of the glass, it is unlikely that any

locations where glass

Jf\

I

glassblowing has taken place. A leak

has been sealed to

<^

_U

is therefore unlikely in these regions.

other pieces of glass.

^ ^ . f l

X

If glass was not properly annealed, cracks can also develop where hooks were attached.

Fig. 7.58 Suggested areas of testing with a Tesla coil.

An exception to this rule would be if a twoor three-fingered support clamp was overly tightened on a glass tube, causing the tube's wall to crack.

Leak Detection and Location 7.6

449

Table 7.15 Appearance of Discharges

in a Gas Discharge Tube at Low Pressures76

Gas

Negative Glow

Positive Column

Air

Blue

(Reddish)

Nitrogen

Blue

Yellow (red gold)

Oxygen

Yellowish white

Lemon

Hydrogen

Bluish pink (bright blue)

Pink (rose)

Helium

Pale green

Violet-red

Argon

Bluish

Deep red (violet)

Neon

Red-orange

Red-orange (blood red)

Krypton

Green

Xenon

Bluish white

Carbon monoxide

Greenish white

(White)

Carbon dioxide

Blue

(White)

Methane

Reddish violet

Ammonia

Yellow-green

Chlorine

Greenish

Light green

Bromine

Yellowish green

Reddish

Iodine

Orange-yellow

Peach blossom

Sodium

Yellowish green (whitish)

Yellow

Potassium

Green

Green

Mercury

Green (goldish white)

Greenish blue (greenish)

— indicates no distinctive color.

 

 

() indicates a different observer's opinion of the color.

1.Turn off some (or all) of the lights in a room so that any discharge from the coil can more easily be seen (it may also be necessary to close doors and/or cover windows). In addition, try not to face an open window.

2.A metal wire (such as copper or nichrome) wrapped around the tip of the Tesla coil (see Fig. 7.57) and bent in a rightangle can extend your reach and/or reach behind glassware.

The Tesla coil can also be used to make the vacuum line a discharge tube to light up probe gases or liquids. Gases or vapors in a vacuum will light up in specific colors from a discharge caused by a Tesla coil. A list of the colors that can be achieved with pure gases in a discharge tube can be seen in Table 7.15.

Table 7.15

(found in several books

or found as

a similar table in other

books ' o n

vacuum technology) provides the colors

of pure gases from dis-

charge tubes, which have very little to do with the discharge from the Tesla coil because of the following conditions:

1. The applied voltage and pressure can vary greatly.

450 Vacuum Systems

Table 7.16 Appearance of Discharges in Gases and Vapors at Low Pressures When Excited by a Tesla Coila

Gas

Color Observed in Discharge

Gas Mixed with Air

Air (room)

Soft violet

Same

Argon

Pale magenta

Pale magenta

CO2

Greenish white

Washed out magenta

Helium

Soft pink

Purplish magenta

Nitrogen

Too pale for magenta, not quite

Purple

 

purple

 

Oxygen

White

Pale magenta

Volatile Liquid

Color Observed in Discharge

Gas Mixed w/ Air

Acetone

Turquoise (then quickly to purple)

Void6 (then quickly to purple)

Dichloromethane

Bluish white

Void* (then quickly to bluish white)

Methanol

Void* (then slowly to soft violet)

Void* (then slowly to soft violet)

a From Journal of Chemical Ed.ucation, 68, pp. 526-528, (1991 Reproduced with permission.

*Void: a lack of discharge due to a loss of vacuum.

2.The Tesla coil discharge, in leak testing, is a through-glass discharge, whereas a discharge tube is a metal-electrode discharge.

3.The distance between electrodes in a discharge tube is fixed, as opposed to the distance between the Tesla coil and ground (this distance can vary constantly from as little as several centimeters to many meters during leak detection).

4.The colors indicated in the tables are for pure gases. In a working vacuum system there will always be some air and moisture mixed with the probe gases. There will also be a trace amount of hydrocarbon vapors (from the mechanical pump) as well as other gases and vapors that incidentally may be in the system.

Work by Coyne and Cobb provided a more effective list of discharge colors because the colors were observed in the act of actual leak detection. They are presented in Table 7.16. Their work demonstrated that spraying gases had limited success in leak indication, but moderate success when the item being tested was enclosed within the gas (by way of a bag). Vapors from applied liquids provided better indicators and more easily demonstrated the specific location of a leak.

If you have items with glass-to-metal seals or metal supports you wish to leakcheck with a Tesla coil, you can encase them in a bag. Initiate a discharge with the Tesla coil while filling the bag with a test gas, such as oxygen or helium. This procedure can help to verify whether or not there is a leak. However, it will not help locate the leak. To specifically locate the leak, you may wipe a probe liquid, such as acetone on a cotton swab, over the suspected areas while a discharge is main-

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