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The process of transferring dry (H2O-free) solvents can be a time consuming process. While I was working in an inorganic/organometallic lab, I found the process of evacuating, closing, and opening to solvent to be a rather tedious, and in some cases, the process took in excess of one hour to transfer 500 mL of solvent (especially for higher boiling point solvents such as chlorobenzene, C6H5Cl, BP = 131°C, and others). I found that the process could be achieved using a continuous method, whereby a continuous vacuum could be applied with minimal solvent loss and a much faster transfer rate. I designed a modified Strauss flask, with an extra outlet, where a vacuum is applied.
Step 1: Have the vacuum transfer flask (VTF) hot from glassware oven; remove and attatch to Schlenk line, applying a vacuum at both the main connection and at the side; the vacuum line attached to the side should have a cold trap attached. Allow to cool.
Step 2: Attach to an adjacent port on the Schlenk line a flask containing the dried solvent (DS; usually containing sodium metal and benzophenone, or calcium hydride) to be purified. Deoxygenate using the vacuum, as necessary. Then, warm gently.
Step 3: Raise a cooling bath (liquid nitrogen or acetone / dry ice) to cool / freeze the VTF; if liquid nitrogen is used, during the solvent transfer it will need to be continuously replenished.
Step 4: Connect the VTF to the DS via the Schlenk line. Ensure that gas is not being fed to, nor vacuum applied directly to the Schlenk line. Vacuum should be applied through the side port of the VTF. This will cause the solvent to flow from the DS through the Schlenk line, through the main joint, and into the flask. The flow is directed first to the sides of the flask, which ensures that it will freeze on contact, and collect most of the solvent. (During this, the solvent in the DS should begin to boil vigorously.)
Step 5: Once the solvent is from the DS has finished transferring, seal off the VTF from the Schlenk line and the vacuum, equalizing pressure in the connection to the Schlenk line in order to remove the VTF.
(Drawn in Inkscape)
Leklthos (oil Flask)
Greek, Attic, black-figure, ca. 500 BC
Perseus flying away with the head of Medusa, while Pegasos springs from her severed neck.
Maker: Unknown
Color [Left]:Top Marigold Ctr Clear, Smoke Base; [ Right] Aqua Base
H= 7-1/2" Diam= 3-1/2" Base 1-1/4x2-3/4
Cat: Small
J&C Curtis
*.25 liter & Italy on base with additional markings
*Reverse side is concave
Roman glass yellow flasks, from around 1 to 200 AD. Glass has been made since 2500 BC. Techniques were developed and improved over the centuries. By about 100 AD, glass began to replace bronze and terracotta vessels for drinking, dining and storage of food and perfume. The ancients did not have the clear glass which is so familiar to us today. At the Getty Villa.
The Getty Villa is an art museum located about 19 miles (31 km) west of downtown Los Angeles, California. The site is built in the style of an ancient Roman palace. It houses ancient Greek, Roman and Etruscan art and artifacts dating from 6,500 BC to 400 AD. Items from after 400 AD are housed in a companion museum, the Getty Center, elsewhere in Los Angeles. I visited the Getty Villa on June 20, 2015.
Frascos romanos de vidrio amarillo, de hacia el año 1 al 200. El vidrio se ha fabricado desde 2500 aC. Las técnicas se inventaron y mejoraron a través de los siglos. Hacia el año 100, el vidrio empezó a reemplazar los recipientes de bronce y terracota para beber, comer y almacenar alimento y perfume. Los antiguos no tenían el vidrio transparente que es tan común hoy en día. En la Villa Getty.
La Villa Getty es un museo de arte situado como a 19 millas (31 km) al oeste del centro de Los Ángeles, California. El edificio está construido en el estilo de un antiguo palacio romano. Alberga arte y artefactos antiguos griegos, romanos y etruscos que datan de 6500 aC al año 400. Artículos de después del año 400 se encuentran en un museo asociado, el Centro Getty, en otro lugar de Los Ángeles. Visité la Villa Getty el 20 de junio de 2015.
Roman glass perfume flasks, from around 1 to 100 AD. Glass has been made since 2500 BC. Techniques were developed and improved over the centuries. By about 100 AD, glass began to replace bronze and terracotta vessels for drinking, dining and storage of food and perfume. The ancients did not have the clear glass which is so familiar to us today. At the Getty Villa.
The Getty Villa is an art museum located about 19 miles (31 km) west of downtown Los Angeles, California. The site is built in the style of an ancient Roman palace. It houses ancient Greek, Roman and Etruscan art and artifacts dating from 6,500 BC to 400 AD. Items from after 400 AD are housed in a companion museum, the Getty Center, elsewhere in Los Angeles. I visited the Getty Villa on June 20, 2015.
Frascos romanos de vidrio para perfume, de hacia el año 1 al 100. El vidrio se ha fabricado desde 2500 aC. Las técnicas se inventaron y mejoraron a través de los siglos. Hacia el año 100, el vidrio empezó a reemplazar los recipientes de bronce y terracota para beber, comer y almacenar alimento y perfume. Los antiguos no tenían el vidrio transparente que es tan común hoy en día. En la Villa Getty.
La Villa Getty es un museo de arte situado como a 19 millas (31 km) al oeste del centro de Los Ángeles, California. El edificio está construido en el estilo de un antiguo palacio romano. Alberga arte y artefactos antiguos griegos, romanos y etruscos que datan de 6500 aC al año 400. Artículos de después del año 400 se encuentran en un museo asociado, el Centro Getty, en otro lugar de Los Ángeles. Visité la Villa Getty el 20 de junio de 2015.
This is a hand built ceramic flask. It has been wood fired, where the wood ash from the firing lands on, and melts over the piece becoming the glaze. The cork has been wood burned by myself as well.
Accession number: 61.48
Place made: Italy
Date made: 16th century
Materials used: leather, wood
Powder flasks were small, portable containers designed to hold gunpowder. From the 1500s to the 1800s, powder flasks were indispensable for charging and priming firearms. Powder flasks were carried as a convenient way to store and use gunpowder for weapons until cartridges became more widespread in the 19th century. Many were highly decorated flasks, like this Florentine example, which displays Renaissance period decoration (16th Century). The original concept for the flask was a concealable and convenient way to carry and store fluids, an iteration of which started in the middle ages when people would use hollowed out fruit to store and carry water.
Larry & His Flask - July 17, 2011 - Warped Tour - Hartford, CT
Photo by Charlotte Zoller © 2011
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