Inert-atmosphere box

The oils produced in the 6 1 and 3 1 reactions in Et20 appeared to be stable on long-term storage at room temperature in the absence of moisture (e.g., in the inert atmosphere box). However, the waxy product of 1 1 (Et20) reactions and all the coammonolysis products prepared in THF formed gels (i.e., became insoluble) after 3-4 weeks at room temperature, even when stored in a nitrogen-filled dry box. 

As noted, sol-gel syntheses for materials based on water-sensitive reagents, such as titanium isoproproxide, must be carried out under low pH20 conditions, which are typically achieved using either an inert atmosphere box (glove box) or under laboratory conditions using a Schlenk-line.73 The Schlenk-line, shown in Fig. 2.4,71 consists of a dual manifold arrangement with one line... 

Solutions were prepared in an inert atmosphere box. Volumetric measurements based upon density were used. Stock solutions appeared stable for several months in the box. Hypodermic syringes and small volumetric flasks were used to measure and store the solutions. 

The product is a yellow-orange to orange, moisture-sensitive solid. It is stable for a minimum of 4 weeks if stored in a good inert-atmosphere box. It is stable in solution only in liquid ammonia and basic water. The product is soluble, but... 

CiystaHine 100% orthophosphoric acid (40 g, 0.41 mol) and [Et4N][V(CO)6] (6.0 g, 17.2 mmol) were intimately mixed together in an inert-atmosphere box at room temperature in a 500-mL round-bottom flask equipped with a large Teflon-coated magnetic stirring bar. The flask is attached to a connecting tube and a specially adapted Schlenk tube receiver as shown in Fig. 1. 

The sublimation is continued until aU V(CO)e is transferred into the Schlenk receiver. The reaction and collection process requires approximately 1.5 h. The V(CO)g product is transferred in an inert-atmosphere box into a conventional Schlenk tube and stored in a freezer (—30°C or lower) in the dark. Yield 3.25 g... 

The reaction mixture is worked up after 24 h using standard Schlenk or inert atmosphere box techniques. The reaction mixture is filtered with a medium porosity filter and the residue washed with methanol (2 x 10 mL). The filtrate and washes are combined and treated with N(C2H5)4C1 (4.5 g) in... 

In order to produce an aqueous solution which fulfills these criteria, 120 g each of basalt, quartz monzonite, and shale were ground to powders less than 37 m in diameter. Each of the samples was placed in two liters of distilled-deionized water which had been pre-equilibrated with an atmosphere containing 10 percent CO2, 90 percent Ar, and 10 ppm Og. The experiment was carried out in an inert atmosphere box at room temperature (26 + 2°C). Samples of the fluid (10 ml) were extracted at various times over a 35-day period and filtered (O.OSpm). Analyses for Na, K, Mg, Ca, Fe, Al, Si02 (aq). Eh, and pH were made on each sample. The experiment was terminated at the end of 846 hours and analyses for HCO3, SO4, and Cl were made on each of the fluids. 

Procedure. The rock wafers were gently cleaned three successive times with methanol in an ultrasonic bath, dried and placed in the inert atmosphere box. Two wafers of each rock type were inserted horizontally in stainless steel holders and placed in linear polyethylene containers holding 150 ml of the appropriate prepared water. The wafers were allowed to equilibrate with the water for three days and then 5 X of tracer solution was added. The resultant solutions contained V/ 5x10 M of each element. The pH of each solution was measured before and after the addition of the tracer and did not change sign-... 

At the end of the six weeks, the containers were returned to the inert atmosphere box and the wafers removed. 

ProcedureSe One of the rock wafers from each of the containers used in the adsorption experiments was placed in a new polyethylene bottle containing 50 ml of the appropriate aqueous solution. The containers were removed from the inert atmosphere box and gently agitated for six weeks. Tracer concentrations in the solution were measured periodically as described previously. At the end of six weeks, the experiments were terminated, the wafers removed from the containers, and the tracer concentrations of the components of the system determined in the same manner as in the adsorption experiments. 

Comparable or larger errors are introduced by unwanted convective mass transport. Convection is caused by physical motion of the solution, sometimes purposefully introduced for techniques such as rotating electrode voltammetry. When a quiet solution is desired, however, convective errors may arise at longer experiment times (slow scan rates) from mechanical vibrations of the solution. Convection is a particular problem for cells inside inert-atmosphere boxes, on which fans and vacuum pumps may be operative. Convection raises the current... 

The reaction flask was most conveniently charged by the checkers in an inert-atmosphere box. 

Caution. Sodium-potassium alloy reacts vigorously with air and must be handled in a good inert-atmosphere box. Solvents should be dried first over calcium hydride or have a very low water content before one attempts to dry them further over sodium-potassium alloy. 

This complex should be prepared in an inert-atmosphere box or in any system capable of providing a rigorously oxygen- and water-free atmosphere. Solvents should be correspondingly dried and deoxygenated. 

Samples for infrared spectroscopy should be prepared in a dry, inert-atmosphere box. It is best to protect the sample with layers of pressed KBr abovo and below the sample bearing layer. 

An inert atmosphere box used when working with oxygen- or water-sensitive materials. 

Caution. Inasmuch as all operations are to he performed in an inert-atmosphere box, all necessary solutions and apparatus should he placed in the box before starting the preparation. 

Fifteen grams (0.063 mol) of cobalt (II) chloride 6-hydrate is dissolved, with heating, in 15 ml. of water contained in a 150-ml. flask, and the pink solution is boiled for several minutes to expel all air. The flask is quickly stoppered and placed in the inert-atmosphere box. Air is displaced from the box by maintaining a rapid flow of oxygen-free nitrogen through the box for about one hour, with occasional collapse of the gloves. 

Where a reactive lower oxidation state results, a key concern is the necessary protection of the reduced complex from air or other potential oxidants, as they are often readily reoxidized. Usually, this requires their handling in special apparatus such as inert-atmosphere boxes or sealed glassware in the absence of oxygen. Where active metal reducing agents (such as potassium) are employed, special care with choice of solvent is also necessary. The nickel reduction reaction (6.33) can be performed in liquid ammonia as solvent, since the strongly-bound cyanide ions are not substituted by this potential ligand. 

ECL experiments focused on radical ion annihilation are carried out in fairly conventional electrochemical apparatus, but procedures must be modified to allow the electrogeneration of two reactants, rather than one, as is more commonly true. In addition, one must pay scrupulous attention to the purity of the solvent/supporting electrolyte system. Water and oxygen are particularly harmful to these experiments. Thus, apparatus is constructed to allow transfer of solvent and degassing on a high-vacuum line or in an inert-atmosphere box. Other constraints may be imposed by optical equipment used to monitor the light. 

An inert atmosphere box used when working with oxygen- or water-sensitive materiais. The box is fiiied with an inert gas such as nitrogen, and work is done through the ports fitted with large rubber gloves. 

Handling, Storage, and Precaution do not breathe dust avoid contact with eyes, skin, and clothing. Reacts with water, oxygen, and carbon dioxide, and may ignite on exposure to air at elevated temperatures. Handle in an inert atmosphere box or bag and conduct reactions under an inert atmosphere in a fume hood. Store in small lots in sealed containers under nitrogen. 

Eubanks, I. D. Abbott, F. J. Gas purification and pressure control system for inert atmosphere boxes. Anal. Chem. 1969, 41, 1708-1709. 

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