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Laboratory Fractional Steam Distillation Still

A Tool For Duplicating Fragrances

After receiving a promotion due in part to my material research I soon learned that a lab distillation still would be coming on board.  Sal Bocca, Pummelo Scents operations manager, pointed out that the extraction equipment although not widely used in analytical departments was state of the art.  It was an ideal first step in duplicating competitors fragrances.  Apparently there were only several stills currently in use for this purpose in the fragrance industry.

Late that winter, and early spring the individual components slowly started to arrive, and quickly filled up the small storage room. Pummelo Scents, is a family owned fragrance business currently generating over 20 million dollars in sales. The business is housed in a state of the art building containing twenty-five thousand square feet of space. The laboratory where the distillation still was originally set up was quite small, and I thought it would never fit.

Once the components finally arrived I received orders to construct the frame. A single photograph  was provided by Sal like the above quickly proved insufficient for my needs. Since no assembly instructions came with the still it was pretty much guess work where everything was going to be placed. The critical aspect of this part of the procedure is the actual placement of the six studs which are mounted on the wall.

From the studs, six short pieces of piping are placed in the socket or holder. The entire frame, or lattice work is then assembled, and held in place by locking devices. If you need to paint the laboratory for example, just loosen the keys on the six studs, and one can pop out the entire frame in one piece. Please don't try to do this with the delicate laboratory equipment mounted.

I consider myself to be a handy individual, however, I found the frame difficult to assemble for the lack of possessing the proper tools with poor instructions. Fortunately I have two friends who are quite handy. One morning they arrived, and proved their value. By lunch time everything was completed. Remember sheet rock commonly is installed in 4 x 8 sections which are then nailed on two by fours which are center to center approximately every thirty two inches.

If you take a look at the next picture  you should have installed a sink to the right of the evaporator. It is not a critical item but both the still, and the evaporator need a steady source of water. Just remember that once you are done with a project everything will have to be washed up, and reassembled. If you have to utilize the men's room for the cleaning procedure broken components, will generally occur. A fiberglass sink can be picked up at Home Depot, and installed by a qualified plumber at a reasonable price.

The following Monday morning I arrived at work, and found much to my surprise that the entire distillation equipment had already been assembled. I was hoping to meet personally with the company consultant. Apparently the individual was only available on a limited basis, and would only work with Sal the operations manager and company owner.

That first week we ran several extraction projects. At the beginning the instructions proved to be quite bewildering in there complexity, but was stimulating at the same time. Each distillation project required three to four hours to complete plus an additional hour to wash, clean and reassemble the individual components back to the original form. After the completion of each individual project I went home that evening, and carefully entered my observations of the day into a personal notebook.

Starting The Distillation Process:

Getting the still ready varies in part on the complexity of the product. For example, liquid shampoos, fabric softener, conditioners, soaps, and lotions are easy to handle. On the other hand aerosol products, shave cream, talc, powdery, and paper type wipes tend to be difficult. The liquid contents inside the product flask can be manipulated to four thousand milliliters. Remember that dense materials can expand in volume once subject to heat inside the product flask.  Usually two hundred grams of product will result in a successful extraction.

The first step is take a large 1,000 ml size beaker, and place it on the gram scale. Tare the scale back to zero, and then add 500 grams of distilled water. Next take your product, and add between two to three hundred grams. Blend the distilled water with contents thoroughly. Next, walk over to your still. Disengage the stem assembly, and gently lay it to the right of the main product flask. Since the assembly is round, and made of glass it could roll off the table. Take beaker in hand, and pour the contents through the middle neck of the three ported flask. From here I would add an additional 1,000 to 2,000 ml's of distilled water. Don't raise the water level past where you can see into the pot. Once things start cooking within the flask the molecular structure of materials can change in form.

Now you are ready to get started. Go to your sink, and make sure that the ball valve is in the open position, and that water is flowing out from the discharge hose. Make sure that the water pressure is not to high. A light steady flow of water which you can feel with the palm of of your hand is all that you will need. Next click the toggle switch on the rheostat which regulates the small 1,000 boiler flask, and set the dial to the sixty position. Add one small boiling stone into this flask.

The stirrer assembly will now have to be assembled. It will consist of five pieces. The tit on the one end will hold the white paddle. Next take the eight inch long white plastic sleeve, and slide it down approximately half way down the rod. Remember if you try to slide the white plastic sleeve over the tit, the glass rod is broken. The glass sleeve which is threaded on one end will sit inside the fat glass nut which will then fit inside the center port. The white plastic nut will then screw loosely down onto the threaded glass sleeve keeping things in place. Connect the top part of the glass rod with a small piece of rubber hose to the metal adapter which sits underneath the stirrer motor.

Next connect the small rubber plugs which are held together by a foot long piece of tygon tubing. The plug which contains the small diameter six inch long glass pipe will fit snugly on top of the 1,000 boiler flask. The other rubber plug contains a twelve inch long glass pipette which will fit into the left side of the three ported product flask. Once you start the distillation process the contents within the flask tend to expand in volume. If the pipette has been adjusted correctly you will see the injected steam press down slightly on the surface. A light hissing emanating  from within the flask will reassure you that everything is running correctly.

Turn the toggle switch on the rheostat which is to the right of the main product flask, and set the dial to the fifty position. This will generally translate to a 110 degrees Fahrenheit temperature within the flask. Now turn on the stirrer motor. I would highly recommend a very low RPM setting. If the RPM setting is to high the stirrer rod will turn the paddle to quickly, and as as a result cause the contents in the main product flask to violently rotate. A RPM setting of five or six will be more then sufficient.

Keep in mind this still is a laboratory size steam distillation still. Basically the small boiler injects a steady stream of steam through the hose down the glass pipette onto the surface of the product within the flask. The product itself has been mixed with distilled water, and is under high heat. The stirrer motor slowly turns the glass stirrer rod at an even rate of revolutions per minute.

This forces vapors containing the much sought after fragrance, up the right vertical column sitting on top of the product flask to the cooling condenser horizontal tube. Once the vapors reach the open condenser port, the cooling water which surrounds the condenser will react with the hot vapors. Naturally as steam cools it will return to its natural form which in this case will be liquid. Its a slow process, and it will take approximately two to three hours to collect one hundred milliliters of liquid product. This beaker is referred to as a first fraction.

During the course of the extraction you will need to refill the one thousand milliliter small boiler flask several times with fresh distilled water. I would recommend keeping a mid size beaker heating on a hot plate for this purpose. You can add cool distilled water, but this will delay the distillation time. Make sure that you handle the beaker containing the boiling water with a heavy duty pair of leather gloves.

Once the product is safely inside the product flask, and everything is running smoothly I generally stay around in the lab for at least an hour. At the beginning of each distillation project the still will require small adjustments to place everything back in proper alignment. Remember each time you utilize the still all of the glass components will require thorough washing, drying, and assembly. Sometimes you can run ten projects in a row before a problem pops up.

I remember on one occasion I came back into the laboratory after unloading a truck, and found that the stirrer motor had increased in speed by itself. It took several months, and several broken glass stirrer rods before I could convince the operations manager that I had a defective stirrer motor. The vendor was contacted, and subsequently informed us that there indeed had been a product recall on the very same motor. For whatever reason I was never notified.

The only real tricky part in handling this still is correctly realigning the components after each project. For example, the stirrer motor is held in place by several heavy duty clamps. As the motor works it naturally vibrates, and will slowly loosen the locking keys. Even the glass condenser clamps will loosen. Sometimes you will have to adjust the lifting device which sits underneath the main product flask to a higher or lower position.

Another suggestion is to look at the stirrer assembly from the side. Try to align the glass rod somewhat vertically with the right ported glass column which sits on top of the product flask along with the horizontal, and vertical condenser tubes.

Cleaning up the first fraction is the next part of the procedure. Somewhere within your laboratory locate the metal ring stand which will hold your separatory flutes. Its a three foot long metal rod threaded on one end. The threaded end screws down into a metal holder or plate which will hold the rod containing your flutes in a secure up right position. Place this stand in a convenient location to the other side of the distillation equipment.

Next you will need the rings which are of two different sizes. The rings can be locked into place on the metal rod by a clamp like device located to the rear of the ring. At the back of this ring you will find a key which will tighten the clamp onto the rod by turning the key clockwise, and by loosening it by turning it counter clockwise. When you are finished with a separatory flute it can be quickly pushed out of your way to the back of the rod. The larger ring will hold the five hundred milliliter size flute, and the smaller ring will hold the two hundred fifty milliliter size flute.

The next part of the cleaning procedure will require ninety milliliters of liquid Freon. The Freon should be stored in amber colored containers, and kept away from the sun, and any source of direct heat. Hopefully you will have access to a refrigerator or a walk in cooler where the Freon can be stored under constant refrigeration. On one occasion I received a forty pound pail, and filled several small bottles before leaving for the day. I placed the cap back on the pail, and returned the following morning to find the contents had evaporated over night.

Freon is denser, and heavier than water, and will slowly absorb the fragrance which is contained within the first fraction. You will measure out a total of ninety milliliters of Freon in a three step process. Each step will force the distilled water to the top of the flute causing a separation to occur within your flute. As the Freon settles to the bottom it is actually cleaning the fragrance by removing the distilled water.

Next take the small one hundred milliliter size beaker which holds your first collected fraction, and pour the contents into a five hundred milliliter separatory flute. Absolutely make sure that the flute is spotlessly clean, and the the small stop cock valve at the bottom of the flask is in the closed position. If you inadvertently left the valve in the open position the contents will pour out. After filling the separatory flute place a white plastic stopper plug snugly on top of the flute.

Take a small beaker in hand and measure out thirty milliliters of Freon. Remove the plastic stopper plug, and place it on your laboratory table next to your stand. Pour the thirty milliliters of Freon into the large five hundred milliliter size separatory flute which contains your first fraction.  Place plastic stopper back on the top of your flute. Once the Freon mixes inside the separatory flute you will notice a large amount of agitation as it mixes with the distilled water. This is normal. A white plastic stopper plug will keep the Freon from evaporating.  Sometimes the built up pressure will force the plastic stopper plug off of the flute. If this occurs just replace the plug.

Carefully take large separatory flute off the ring holder. Turn the flute upside down with stopper plug resting firmly against the palm of your right hand. Please hold the flute with both of your hands, and be sure you don't accidentally hit the flute against anything in your laboratory.  Vigorously shake the flute, then release the built up pressure by slowly turning the small stop cock valve counter clockwise to the open position. Repeat this procedure two more times.

Place separatory flute back on the ring stand. Within minutes the Freon will fall to the bottom of the flute. Position the smaller two hundred fifty milliliter size flute directly under the bottom spout of your larger flute. Be sure to check that the smaller flute stop cock valve is also closed. Open the stop cock valve of the larger flute, and drain the Freon slowly to the line which separates the water from the Freon.

Re measure thirty milliliters of Freon, and pour contents into the five hundred milliliter size flute. Again, take flute in hand, and carefully shake contents, and release the pressure. Shake the flute, and release the pressure two more times. Place flute back on the ring stand. Wait a few minutes and you will once again see the Freon separate from the water. Re position the small flute underneath the spout of the larger flute. Drain the contents to just below the line separating the Freon from the water. Place plug back on small flute. Re measure another thirty milliliters of Freon into a small beaker, and repeat above procedure one more time.

Again, the three step cleaning process utilizes a total of ninety milliliters of Freon. When you shake the Freon inside the separatory flute it acts like a magnet. The fragrance is slowly removed from the distilled water as the Freon falls to be bottom of the flute. The actual amount of fragrance which you will retrieve at the end of the process will be quite small.

In many instances you will end up with one or two grams of oil, and sometimes less. The actual amount depends in part in the amount of fragrance which is in the product, and how much product actually went into the product flask. Your gas chromatograph computer will only require several small drops or microns for analytical purposes.

After you have collected your first fraction prior to cleaning it with Freon I would recommend the following step as an automatic part of handling the still. Shut off the two rheostats which are connected to the small boiler, and product flask. Turn the stirrer motor RPM setting to zero, and shut it off. Next, pop the hose off the top of the glass stirrer rod. Take the two rubber stoppers off of the small boiler, and product flask.  Leave the water flow on since it will be needed later in the evaporator.

The glass components which are assembled to the main product flask are quite hot. If you attempt to disassemble the still prior to letting it cool down you can very easily have breakage problems. Remember you have generated a near vacuum condition which is under extremely high heat. By the time you place the small pear on the evaporator things should have sufficiently cooled down to allow you to slowly disassemble the individual components. Always wear heavy duty leather gloves when handling the still at this point. Careless handling of the equipment can cause personal injury.

Your first fraction has now been cleaned with Freon, and is sitting inside the two hundred fifty milliliter separatory flute on the bottom ring of your stand. The fraction will now have to be cleaned with a saturated distilled water solution containing sodium chloride. A twelve ounce amber colored bottle will be more than sufficient for this purpose. It should be kept in your refrigerator when not in use.

Fill the bottle with distilled water approximately eight tenths full. Take a plastic lined paper cup, and fill it a quarter way with sodium chloride powder. Take paper cup in hand, and bend it. Pour powder directly from the cup into your bottle. The amount which will go into the bottle will be enough to fill the bottom to an approximate quarter inch mark. Place cap back on top of bottle, and shake it vigorously. From time to time you will need to add fresh distilled water along with additional amounts of sodium chloride. The distilled water can only absorb so much of the granulated powder. If it gets hard at the bottom of the bottle just break it up, and shake.

Next you will measure out forty milliliters of saturated sodium chloride solution into a small beaker. Take plastic stopper plug off of the small separatory flute. Pour this solution into your small separatory flute containing the first fraction. Place white plastic stopper plug back on top of the flute. Take flute firmly in hand resting white stopper plug snugly against the palm of your right hand. Vigorously shake the flute with the small spout facing your laboratory ceiling. Open stock cock valve counter clockwise to release the pressure. Repeat this procedure two more times.

The saturated solution of sodium chloride will only be used once during this part of the cleaning procedure. In other words, you will measure out forty milliliters of this solution one time. Place separatory flute back on the ring stand. Again, you will notice an immediate separation of the Freon from the aqueous sodium chloride solution.

At the bottom of the flute will be ninety milliliters of Freon. At the top of the flute will be forty milliliters of the sodium chloride solution. Place a small Erlenmeyer flask underneath the spout of the separatory flute. The clamp at the rear of the ring can be adjusted up, and down the round metal rod by loosening the small locking key counter clockwise.

Be sure you tighten the clamp like device after you have correctly positioned the separatory flute over the open mouth of the Erlenmeyer flask. If the ring slips down the rod the glass separatory flute can break. Drain contents of your small separatory flute to just short of the line separating the Freon from the sodium chloride solution. Place glass stopper on top of the Erlenmeyer flute.

The next part of the cleaning procedure will require anhydrous sodium sulfate granular powder. Take a small spatula, and measure out several tea spoons from the small jar into your Erlenmeyer flask. Place glass stopper plug back on top of the flask. Pick up the flask, and rotate the contents several times. Visually check to see if there are any bubbles sitting on top of the anhydrous sodium sulfate which will fall to the bottom of the Erlenmeyer flask usually in the center. Bubbles will indicate the presence of water which will be removed with this procedure.

Next take a small beaker, and place a hollow stem wine glass into the beaker. Take a paper filter, and unfold it. Place the filter on top of the curved wine glass. Pour the contents of the Erlenmeyer flask through the paper filter, and into the beaker. Cover the small beaker with aluminum foil.

Before you go to your evaporator take a small pear and glass stopper, and place it inside an eight ounce paper cup. Turn the gram scale on, and tare the scale to zero. Place paper cup with glass pear and stopper on your gram scale, and record the the combined weight. If you kept track of the distilled water plus product which was used in the project you will be able to figure out your yield percentage quite easily. The fractional steam distillation stills accuracy according to Sal is at best fifty percent.

Take pear with paper cup in hand, and walk over to your evaporator. Carefully remove the small pear, and connect the open mouth of the pear to the glass coil which sits directly over the water bath. At the same time use your other hand, and place the small plastic green ring over the round glass lip of your pear snapping the ring it into place on the glass coil. Before you remove your hand be sure to check that the pear is sitting snugly on the coil.

You will next notice that there is a small glass angle shaped handle connected to a thin tubular plastic rod. This rod will slide through the center of the glass water coils, and stop at the top of the small pear which is sitting over your water bath. A vacuum is created by pulling the handle out, and then by resealing it into the top of the glass evaporator. Notice the whole which is centered on the neck of the handle aligns itself with another whole at the top of the evaporator.  Be careful aligning the two wholes. One can release the vacuum, and quickly create one by turning the handle slightly clockwise, or counter clockwise.

Situated slightly to the left of the evaporator is a thousand milliliter size flask which is connected to the left open port of the evaporator. It is held into place on the evaporator by a metal clamp like device. If you turn the small screw inside the clamp clockwise you will tighten the clamp, turning it counter clockwise will loosen the clamp. You will notice that it is sort of off center, and drooping slightly to the right. The flask position on the evaporator can easily be adjusted, but don't over tighten the clamp. If you exert to mush pressure you can break both the flask, and the neck of the evaporator causing considerable damage.

Next, you will find a small switch which is located on the base of the evaporator on the right hand side. It almost sits inside the base. The switch is activated by pressing it forward to the on position. Again, it will glow indicating that the evaporator is on. The selector panel is located in a square box which connects into your water bath, and evaporator with two coaxial cables. This will allow you to control the bath, and evaporator from this one panel.

To the front of the water bath there is another on off switch. Slide this switch to the on position. This switch will glow when it is turned on. However, one can not control the temperature of the bath with this switch. The temperature inside the bath can only be controlled with the round selector dial which is located to the front of the bath on the right hand corner.

To the left of the water bath there is a small control panel which is connected to the base of the water bath, and evaporator. It's a square box which sits inside the base of the evaporator.  The control panel will allow you to determine the bath temperature, and rotation speed of the evaporator.

The dial located on the top of the panel in the left front corner has three positions. The left position will be for the bath. The center position will allow you to control the evaporators rotation speed. The right position will allow you to control the vapor temperature within the evaporator. The rotation speed of the evaporator is a round dial located to the right of the main selector switch.

The evaporator can be lowered into the bath by a square shaped switch which is located on the back right corner of the control panel. By pushing the switch forward the entire assembly can be raised. By pushing the switch the other way one can lower the evaporator into the water bath.

Turn the control panels selector switch to the bath position. The temperature control dial for the bath is situated in front of the bath to the right. As you turn the dial slowly clockwise you will increase the temperature inside the bath. A small round LCD indicator light which is found to the left of the temperature dial will indicate the thermostat is on.

Please note, don't get to aggressive with the control device. It will take the bath ten to fifteen minutes before it reaches the desired temperature setting. The maximum temperature which should be kept in the bath is between forty one, and forty three degrees Celsius. The control device is not exactly precise, and the bath temperature can easily increase very quickly. One can read the temperature inside the bath by the small square LCD indicator which is located to the right of the evaporators up and down control switch. Once the desired temperature has been reached turn the round selector dial slightly counter clockwise.

Once the pear is in place, the bath has been activated, and a vacuum has been created you will need to set the evaporators rotation speed. Turn the selector switch from the bath position to the revolutions per minute setting. Slightly to the right of the selector switch you will find a round dial which allows you to increase, and decrease the evaporators rotation.

You will notice to the rear of the evaporator below the glass condenser a round black knob like device. By turning the knob counter clockwise you can disengage the evaporators up, and down level. Once you reach the correct water level, or position turn the knob clockwise until you can not turn the knob any further. This locks the evaporator into a pre selected up and down range.

I would recommend a slow rotation speed between thirty to thirty five revolutions per minute. After you have lowered the pear partially into the bath be sure it is not entirely emerged into the bath. Be sure to double check the temperature setting. A small round amber colored indicator light in the front left corner of the bath will inform you that the heating element in on inside the bath. You can very easily over heat the bath with disastrous consequences. Always keep in mind that the pear is held in place on the glass coil by a small green plastic ring.

Remember, as the pear rotates inside the bath the heated water will cause the liquid Freon in the pear to turn into a vapor. Since a vacuum has been created within the evaporator the gaseous vapors will liquefy once they reach the cooling condenser coils. The Freon will then slowly trickle down into the thousand milliliter size flask which is sitting to the left of the pear. This will take approximately twenty to thirty minutes to complete.

The amount of fragrance left inside the pear at the conclusion of this procedure will vary with each project. During the course of eighty projects I have had results from as small as a third of a gram to several grams. I found that by adjusting the distilled water level upwards will normally increase the fragrance yield. Using more product will also increase the amount of fragrance at the end. Again, usage levels in products differ greatly depending in part on the cost of the fragrance, and odor parameters of the base product. The gas chromatograph computer will only require one or two drops for analytical purposes.

After the Freon has been removed you will need to raise the evaporator out of the bath.  Utilize the small square control device located in the rear right corner of the control panel. By pushing the switch towards the wall the evaporator can be raised out of the bath. Next, turn off the rotation. You will need to slide the front left corner dial to the RPM setting. Turn the right handed dial counter clockwise to the zero mark. The rotation of the evaporator will cease.

Before you remove the pear from the coil be sure to evacuate the vacuum inside the evaporator. This can be accomplished by aligning the condenser glass plug, or handle with has the long plastic tube with the open whole on the glass condenser. Turn the glass plug slowly, and at the same time hold onto the pear. If you align the two wholes to quickly its possible that the pressure created inside the evaporator could push your pear off the coil.

With the pear safely in hand retrieve your paper cup with glass stopper. Place pear in paper cup, and place glass stopper on top of the pear. There are several tests which can be utilized to verify the removal of the Freon. One method is to run hot tap water over the pear.  Another is to place the pear inside a beaker partially filled with water on a hot plate for a few minutes. A third method would be to raise the temperature inside the water bath after you have evacuated the vacuum. Be careful handling the pear at this point. Make sure you weigh the pear inside the paper cup.

After you have recorded the pears weight you will need to transfer the pears contents to a gas chromatograph sample vial. You will need a small three gram transfer pipette which will allow you to safely remove the fragrance from the pear. By squeezing the pipettes bulb you will be able to retrieve the sample from the pear, and place it inside the vial. Be sure to crimp a top onto the vial. You wouldn't want to loose the sample at this point.

As a rule of thumb I would recommend utilizing a minimum of two hundred grams of product for a successful extraction. You can be flexible with this figure depending on how much your customer has available to send to you. Again, the more product which goes into the still will generally result in a successful duplication.

The yield basically is the difference between the weight of the empty pear, and what's left when you evaporated the Freon from the full pear. The end yield can vary from as little as a tenth of a gram to several grams. Each project will have its own peculiarities, and nuances which will give you a different yield even if you are running lemon end dust five different times. My principal concern was achieving a successful extraction at the end of each individual project. Sal Bocca the companies operations manager would send the sample to an outside laboratory for gas chromatography duplication. I was always amazed at the accuracy.

You should also keep records, or notes on each individual project on a separate piece of paper. From time to time you will run into difficulties. By keeping accurate notes one can quickly resolve problems if they pop up again. Some times you will have to run the same product extraction several times before the fragrance is successfully duplicated.

Cleaning the equipment at the beginning will be confusion to say the least. Everything will have to be disassembled washed thoroughly in hot soapy water, dried, and then put back together. As soon as you take the pear off of the evaporator be sure to turn the ball valve off which is below your sink. Taking the water hoses off with the water running through them will only occur on one occasion.

After running a dozen projects you will start disassembling the still in stages. As dirty beakers, and separatory flutes become available I would recommend washing them up with warm soapy dish detergent. Once you collected the first fraction you should immediately turn of the two rheostats which regulate the heat for your boiler, and main product flask. After the main product flask cools for approximately thirty minutes the stirrer assembly can be easily disengaged from the product flask.

The stirrer assembly consists of five pieces. Be sure to slide the individual components off the smooth end of the glass rod. Again, you will only slide the white plastic sleeve once over the small tit sitting at the other end. When handling the still be sure to wear heavy duty leather gloves.

The hardest part in handling the still at the beginning is reassembling everything for the next project. One of the benefits which you have is the enclosed manual. For me everything was trial, and error. After the completion of fifteen projects you will know by sight, and sound if everything is aligned, and connected together correctly. You can control the position, and height of the product flask by the lift device sitting below the flask. The glass condenser tubes can be adjusted by the clamp like device which hold them into place both horizontally, and vertically.

Be careful handling the individual components. Everything is made of glass, and can easily break. Sometimes you will run fifteen or twenty projects in a row before a problem occurs.  Remember what I told you earlier keeping accurate notes on individual projects will increase your trouble shooting skills.

My definition of a pitfall is basically an unfortunate accident. The first thing which you have to remember about the still is many of the individual components are made out of glass.  Another important aspect in handling the still is once the project has been completed everything is extremely hot. Taking the glass columns, including the stirrer assembly apart when they are hot can result in broken glass, and a burned hand.

Keep accurate notes on each individual project. I will guarantee if you do something stupid once you will never make the same mistake twice. After a dozen or so projects your confidence will increase. Within months you can see quite quickly by sight, and sound if the still is set up, aligned properly, and operating correctly. Below are some things that you should avoid.

Pitfalls:

1. Dropping spatula into main product pot while stirrer assembly is rotating.

2. Breaking separatory flute by turning stop valve to hard with first fraction inside.

3. Flask containing Freon accidentally dropping into the bath.

4. Not covering water bath with saran wrap to keep out foreign material.

5. Breaking tit off stirrer assembly by accidentally sliding white plastic sleeve off wrong way.

6. Forgetting to turn on either of the two rheostats at the start of a distillation project.

7. Failure to turn water on at the start of the project.

8. Pouring first fraction into a open separatory flute.

9. Accidentally hitting a separatory flute against a laboratory table, and breaking it.

10. Over tightening the stop cock valve on a separatory flute containing the first fraction.

11. Taking tubing connection off with the water still flowing though the hose.

12. Tubing coming off small separate boiler.

13. Leaving top off of Freon can, and finding the liquid has evaporated over night.

14. Having a defective stirrer motor which increases in speed, and consequently breaks the glass stirrer rod.

15. Not carefully recording all observations especially with new products.

16. Finding Freon now fifty times more costly then several years ago.

17. Handling any of the hot glass components without heavy duty laboratory gloves.

18. Failure to notice separation within collected first fraction.

Perfume - "The Story of a Swindle"