Air-free Techniques
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Air-free Techniques
Air-free techniques refer to a range of manipulations in the chemistry laboratory for the handling of Compound (chemistry), compounds that are air-sensitive. These techniques prevent the compounds from reacting with components of air, usually water and oxygen; less commonly carbon dioxide and nitrogen. A common theme among these techniques is the use of a fine (100–10−3 Torr) or high (10−3–10−6 Torr) vacuum to remove air, and the use of an inert gas: preferably argon, but often nitrogen. The two most common types of air-free technique involve the use of a glovebox and a Schlenk line, although some rigorous applications use a high-vacuum line. In both methods, glassware (often Schlenk tubes) are pre-dried in ovens prior to use. They may be flame-dried to remove adsorbed water. Prior to coming into an inert atmosphere, vessels are further dried by ''purge-and-refill'' — the vessel is subjected to a vacuum to remove gases and water, and then refilled with inert gas. This ...
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Laboratory
A laboratory (; ; colloquially lab) is a facility that provides controlled conditions in which scientific or technological research, experiments, and measurement may be performed. Laboratories are found in a variety of settings such as schools, universities, privately owned research institutions, corporate research and testing facilities, government regulatory and forensic investigation centers, physicians' offices, clinics, hospitals, regional and national referral centers, and even occasionally personal residences. Overview The organisation and contents of laboratories are determined by the differing requirements of the specialists working within. A physics laboratory might contain a particle accelerator or vacuum chamber, while a metallurgy laboratory could have apparatus for casting or refining metals or for testing their strength. A chemist or biologist might use a wet laboratory, while a psychologist's laboratory might be a room with one-way mirrors and hidden ...
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Reagents
In chemistry, a reagent ( ) or analytical reagent is a substance or compound added to a system to cause a chemical reaction, or test if one occurs. The terms ''reactant'' and ''reagent'' are often used interchangeably, but reactant specifies a substance ''consumed'' in the course of a chemical reaction. ''Solvents'', though involved in the reaction mechanism, are usually not called reactants. Similarly, ''catalysts'' are not consumed by the reaction, so they are not reactants. In biochemistry, especially in connection with enzyme-catalyzed reactions, the reactants are commonly called substrates. Definitions Organic chemistry In organic chemistry, the term "reagent" denotes a chemical ingredient (a compound or mixture, typically of inorganic or small organic molecules) introduced to cause the desired transformation of an organic substance. Examples include the Collins reagent, Fenton's reagent, and Grignard reagents. Analytical chemistry In analytical chemistry, a reage ...
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Degasification
Degassing, also known as degasification, is the removal of dissolved gases from liquids, especially water or aqueous solutions. There are numerous methods for removing gases from liquids. Gases are removed for various reasons. Chemists remove gases from solvents when the compounds they are working on are possibly air- or oxygen-sensitive (air-free technique), or when bubble formation at solid-liquid interfaces becomes a problem. The formation of gas bubbles when a liquid is frozen can also be undesirable, necessitating degassing beforehand. Pressure reduction The solubility of gas obeys Henry's law, that is, the amount of a dissolved gas in a liquid is proportional to its partial pressure. Therefore, placing a solution under reduced pressure makes the dissolved gas less soluble. Sonication and stirring under reduced pressure can usually enhance the efficiency. This technique is often referred to as ''vacuum degasification''. Specialized vacuum chambers, called vacuum degassers, ar ...
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Schlenk Flask
A Schlenk flask, or Schlenk tube, is a reaction vessel typically used in air-sensitive chemistry, invented by Wilhelm Schlenk. It has a side arm fitted with a PTFE or ground glass stopcock, which allows the vessel to be evacuated or filled with gases (usually inert gases like nitrogen or argon). These flasks are often connected to Schlenk lines, which allow both operations to be done easily. Schlenk flasks and Schlenk tubes, like most laboratory glassware, are made from borosilicate glass such as Pyrex. Schlenk flasks are round-bottomed, while Schlenk tubes are elongated. They may be purchased off-the-shelf from laboratory suppliers or made from round-bottom flasks or glass tubing by a skilled glassblower. Evacuating a Schlenk flask Typically, before solvent or reagents are introduced into a Schlenk flask, the flask is dried and the atmosphere of the flask is exchanged with an inert gas. A common method of exchanging the atmosphere of the flask is to flush the flask out with ...
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Winchester (bottle)
Winchester (, ) is a City status in the United Kingdom, cathedral city in Hampshire, England. The city lies at the heart of the wider City of Winchester, a local government Districts of England, district, at the western end of the South Downs National Park, on the River Itchen, Hampshire, River Itchen. It is south-west of London and from Southampton, its nearest major city. At the 2021 census, the built-up area of Winchester had a population of 48,478. The wider City of Winchester district includes towns such as New Alresford, Alresford and Bishop's Waltham and had a population of 127,439 in 2021. Winchester is the county town of Hampshire and contains the head offices of Hampshire County Council. Winchester developed from the Roman Britain, Roman town of Venta Belgarum, which in turn developed from an Iron Age ''oppidum''. Winchester was one of if not the most important cities in England until the Norman Conquest in the eleventh century. It now has become one of the most expe ...
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Phosphorus Pentoxide
Phosphorus pentoxide is a chemical compound with molecular formula Phosphorus, P4Oxygen, O10 (with its common name derived from its empirical formula, P2O5). This white crystalline solid is the anhydride of phosphoric acid. It is a powerful desiccant and dehydration reaction, dehydrating agent. Structure Phosphorus pentoxide crystallizes in at least four forms or polymorphism (materials science), polymorphs. The most familiar one, a metastable form (shown in the figure), comprises molecules of P4O10. Weak van der Waals forces hold these molecules together in a hexagonal lattice (However, in spite of the high symmetry of the molecules, the crystal packing is not a close packing). The structure of the P4O10 cage is reminiscent of adamantane with ''T''d symmetry point group. It is closely related to the corresponding anhydride of phosphorous acid, phosphorus trioxide, P4O6. The latter lacks terminal oxo groups. Its density is 2.30 g/cm3. It boils at 423 °C under atmospheric pre ...
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Glass Tubing
Glass tubes are mainly cylindrical hollow-wares. Their special shape combined with the huge variety of glass types (like borosilicate, flint, aluminosilicate, soda lime, lead or quartz glass), allows the use of glass tubing in many applications. For example, laboratory glassware, lighting applications, solar thermal systems and pharmaceutical packaging to name the largest. In the past, scientists constructed their own laboratory apparatus prior to the ubiquity of interchangeable ground glass joints. Today, commercially available parts connected by ground glass joints are preferred; where specialized glassware are required, they are made to measure using commercially available glass tubes by specialist glassblowers. For example, a Schlenk line is made of two large glass tubes, connected by stopcocks and smaller glass tubes, which are further connected to plastic hoses. Industrial Relevance Compared to other materials like plastics the importance of cylindrical half-finished prod ...
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Ground Glass Joint
Ground glass joints are used in laboratories to quickly and easily fit leak-tight apparatus together from interchangeable commonly available parts. For example, a round bottom flask, Liebig condenser, and oil bubbler with ground glass joints may be rapidly fitted together to reflux a reaction mixture. This is a large improvement compared with older methods of custom-made glassware, which was time-consuming and expensive, or the use of less chemical resistant and heat resistant Cork (material), corks or rubber bungs and glass tubes as joints, which took time to prepare as well. One of the glassware items to be joined would have an ''inner'' (or male) ''joint'' with the ground glass surface facing outward and the other would have an ''outer'' (or female) ''joint'' of a correspondingly fitting taper with the ground glass surface facing inward. To connect the hollow inner spaces of the glassware components, ground glass joints are hollow on the inside and open at the ends, except fo ...
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Cannula Transfer
Cannula transfer or cannulation is a set of air-free techniques used with a Schlenk line, in transferring liquid or solution samples between reaction vessels via cannulae, avoiding atmospheric contamination. Syringes are not the same as cannulae, but cannula transfer techniques remain relevant when using them for this purpose. Two methods of cannula transfer are popular: vacuum, and pressure. Both utilize differences in pressures between two vessels to push the fluid through. Often, the main difficulty encountered is slow transfer due to the high viscosity of the fluid. Equipment Septa Septa (: septum) are rubber stoppers which seal flasks or bottles. They give an airtight seal, preventing the ingress of the atmosphere, but are able to be pierced by sharp needles or cannulae. Cannula Cannulae are hollow flexible tubes. Their bore is usually 16-22 gauge thick. They are commonly made of stainless steel or PTFE for their chemical resistance. Stainless steel cannulae are usually 2� ...
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Syringes
A syringe is a simple reciprocating pump consisting of a plunger (though in modern syringes, it is actually a piston) that fits tightly within a cylindrical tube called a barrel. The plunger can be linearly pulled and pushed along the inside of the tube, allowing the syringe to take in and expel liquid or gas through a discharge orifice at the front (open) end of the tube. The open end of the syringe may be fitted with a hypodermic needle, a nozzle or tubing to direct the flow into and out of the barrel. Syringes are frequently used in clinical medicine to administer injections, infuse intravenous therapy into the bloodstream, apply compounds such as glue or lubricant, and draw/measure liquids. There are also prefilled syringes (disposable syringes marketed with liquid inside). The word "syringe" is derived from the Greek σῦριγξ (''syrinx'', meaning "Pan flute", "tube"). Medical syringes Medical syringes include disposable and safety syringes, injection p ...
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Reagent
In chemistry, a reagent ( ) or analytical reagent is a substance or compound added to a system to cause a chemical reaction, or test if one occurs. The terms ''reactant'' and ''reagent'' are often used interchangeably, but reactant specifies a substance ''consumed'' in the course of a chemical reaction. ''Solvents'', though involved in the reaction mechanism, are usually not called reactants. Similarly, ''catalysts'' are not consumed by the reaction, so they are not reactants. In biochemistry, especially in connection with enzyme-catalyzed reactions, the reactants are commonly called substrates. Definitions Organic chemistry In organic chemistry, the term "reagent" denotes a chemical ingredient (a compound or mixture, typically of inorganic or small organic molecules) introduced to cause the desired transformation of an organic substance. Examples include the Collins reagent, Fenton's reagent, and Grignard reagents. Analytical chemistry In analytical chemistry, a reag ...
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