Laboratory operation

Analysis of Process hazards. The proposed operation must be thoroughly analyzed for hazards before the project is undertaken. After the 

Cleaning for fluorine service. It is important that materials that may contact elemental fluorine be thoroughly cleaned to remove any traces of grease or other substance that may ignite on contact with fluorine. Furthermore, it is important to passivate all surfaces that may contact fluorine. Refer to the manufacture s fluorine material safety data sheet for more information. The assembled anodes used in the laboratory were degreased by refluxing overnight with trichlorotrifluoroethane in an oversized Soxhlet extractor. 

Materials compatibility. We use scrupulously clean and scratch-free FEP (FEP is the acronym for the copolymer of tetrafluoroethylene and hexafluoropropylene) tubing for handling our mixtures of fluorine and nitrogen at ambient temperature. Corrugated FEP tubing is convenient for making strain-free assemblies. We have found that Monel is excellent for use with dry molten KF-2HF. Mild steel corrodes slowly and stainless steels corrode rapidly. Kel-F polychlorotrifluoroethylene is satisfactory for use with HF and with KF-2HF polypropylene and polymethylpentene are not satisfactory. 

Preparation ofKF-2HF. This is prepared by carefully adding hydrogen fluoride vapor mixed with nitrogen to solid potassium bifluoride.13 Potassium bifluoride is available in convenient quantities from some supply houses (Aldrich 23,928-3, for example). The addition of hydrogen fluoride vapor to potassium fluoride is extremely exothermic and is best not attempted. The addition of liquid hydrogen fluoride to potassium bifluoride is also extremely exothermic and is best not attempted. 

Bauer and W. V. Childs, paper 933 presented at die 1997 Montreal meeting of The Electrochemical Society. 

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PRELIMINARY LABORATORY OPERATIONS III.l. DETERMINATION OF MELTING POINTS... 

The safety review technique is also usehil for small laboratory operations and small changes in existing processes. In these cases, the committee often consists of two or three people and any changes are often less formally recommended. 

SPC on manufactured products SQC on laboratory operations communicate with corporate CIM system improved QA/QC on products reduced testing costs correlate laboratory analyses and process measurements faster solutions to production problems tested in laboratory faster notification of backlog problems improved electronic data interchange capabiUties automated communication with inventory, ordering, and materials planning systems... 

Another step in laboratory automation to be achieved is the conversion of standard chemical procedures such as titrations or thermal gravimetric analysis, into unit laboratory operations. A procedure could then be selected from these laboratory operations by an expert system and translated by the system to produce a set of iastmctions for a robot. The robot should be able to obey specific iastmctions, such as taking a specified sample aliquot and titrating it using a specified reagent. 

Analytical and Laboratory Operations. Sulfamic acid has been recommended as a reference standard in acidimetry (55). It can be purified by recrystaUization to give a stable product that is 99.95 wt % pure. The reaction with nitrite as used in the sulfamic acid analytical method has also been adapted for determination of nitrites with the acid as the reagent. This reaction is used commercially in other systems for removal of nitrous acid impurities, eg, in sulfuric and hydrochloric acid purification operations. 

Until the early 1960s, laboratory iavestigators rehed on dialysis for the separation, concentration, and purification of a wide variety of biologic fluids. Examples iaclude removal of a buffer from a proteia solution or concentrating a polypeptide with hyperosmotic dialysate. Speciali2ed fixtures were sometimes employed alternatively, dialysis tubes, ie, cylinders of membrane about the si2e of a test tube and sealed at both ends, were simply suspended ia a dialysate bath. In recent years, dialysis as a laboratory operation has been replaced largely by ultrafiltration and diafiltration. 

All processes except laboratory operations. A laboratory operation is defined as any work with substances m which the containers used for reactions, transfers and other handling of substances are designed to be easily manipulated by one person. This does not include operations whose function IS to produce commercial quantities of material. 

Operating costs are best done in-house, because company personnel are familiar with corporate philosophies of staffing, maintenance, control laboratory operations. administrative requirements, and many other support aspects of running the business. If adequately staffed, the in-house study group should handle operating costs rather than try to teach a contractor company requirements. 

Buildings. Company philosophies on operating and maintenance as well as control and satellite laboratory operations and administrative requirements will set building requirements. The licensor will make suggestions, but the operating company will have to take the lead in setting up these requirements. 

For many laboratory operations it is necessary to weigh objects or materials which are far heavier than the upper weight limit of a macro analytical balance, or small amounts of material for which it is not necessary to weigh to the limit of sensitivity of such a balance this type of weighing is often referred to as a rough weighing . A wide range of electronic balances is available for such purposes with characteristics such as, for example,... 

The study of reactions with rates that He outside the time frame of ordinary laboratory operations requires specialized instrumentation and techniques. This chapter presents the wide range of methods currently in use for very fast reactions. Extraordinarily slow reactions, on the other hand, have received very little attention. For them, one may resort to measuring a tiny concentration of product over normal times, as in the method of initial rates. 

A third source of aquatic plutonium is liquid effluent discharged from laboratory operations into ponds and streams. An example of this is a former waste pond at Oak Ridge National Laboratory, Pond 3513, that received liquid wastes with low concentrations of transuranic elements before it was retired. This impoundment has water quality similar to high pH natural ponds. 

Tautomers are defined as isomers which are readily interconvertible. It is clear that the distinction between tautomerism and ordinary isomerism is very vague indeed, and that it depends on the interpretation of the adverb readily. It is customary to designate as tautomers those isomers whose half-lives (with respect to interconversion) are under ordinary circumstances less than the times required for laboratory operations to be carried out (some minutes or hours), so that the separation of the isomers from the equilibrium mixtures is difficult. The distinction between tautomers and ordinary isomers has no molecular significance whatever, since it is dependent on the accidental ordinary rate of human activity. 

While the calculations in this experiment are difficult, all students can readily perform the laboratory operations. Student teams work together on the challenging aspects of the calculations motivated by the fact that they are able to apply what they have learned in school to a real world substance. 

Throughout the book, the person in charge of day-to-day operations is referred to as the laboratory operator. This is not an administrator or supervisor located in an office down the hall or in another building. The laboratory operator must be heavily involved in all aspects of planning. Only he can estimate space requirements, check a proposed layout for practical and safe operation, and recommend allowances for future expansion. Regardless of the amount of professional assistance available, the laboratory operator can expect to burn much midnight oil. During construction he must be available at all times to take care of those numerous problems nobody had predicted. 

Planning and building a laboratory requires a cooperative effort involving administrators, designers, equipment supply houses, contractors, and the laboratory operator. A laboratory designed for efficient operation can be achieved only if all of them work together with mutual respect and the best possible communication. 

Once it has been decided that a new laboratory should be built, some important basic planning must be done. Whether or not an architect or designer is to be called in later, those in charge of the laboratory operation will need to consider questions such as these ... 

One research laboratory was located on the second floor of a building in which a diaper laundry occupied the first floor. The laundry equipment would periodically send veritable shock waves through the building, making many laboratory operations impossible for a short while. The laboratory workers referred to these annoying incidents as the times when the laundry dropped its load. ... 

In other words, the laboratory operator is still the key person at this stage and should be prepared to burn a considerable amount of midnight oil, even with the best professional assistance. He will be in constant contact with the architect or designer, and the project will sometimes be like a ball that is tossed back and forth. In this game, the building professional will have the... 

At this point of the planning, we are mainly concerned with quantitative estimates of such utilities and the ease, or lack thereof, with which they can be brought to the laboratory area. These considerations have a profound effect on laboratory layout. In laboratories that have been in operation for some time, a lack of needed utilities is a major problem, particularly when new procedures are introduced. Estimates should be made by the laboratory operator in close cooperation with building professionals and should take future needs into consideration. 

From the list of laboratory operations previously prepared, it will now be easy to single out the ones that require power. The manuals for the equipment already on hand and catalog information on items yet to be purchased can provide the power requirements. Compared to what was available some years ago, modern laboratory equipment does not need much power. Exceptions are heating devices and motors, which may be very power hungry. A list of the wattages involved should be made, noting which equipment operates on 110 volts and which on 220. Allowance should be made for future purchases of equipment. This information will help the electrical engineer or contractor determine the number of circuits. 

A good heating and air conditioning system provides more than creature comfort for those working in a laboratory. Conditions of reasonably constant temperature and humidity are important for the proper performance of many laboratory operations. 

A safe laboratory is the result of both good design and proper work rules. The laboratory operator, as the only person fully aware of the work to be performed, must be involved in all safety planning. He will be the one who can supply the safety experts with the information they need. 

Eye protection was rarely practiced in older laboratories except when particularly hazardous work was carried out. Today such protection is mandatory for practically all laboratory operations. 

Older laboratory workers could no doubt add many examples of their own to the list of unsafe practices. Modern laboratory planners and operators, however, are more aware of safety problems, and rules regarding safety have been made much more strict. It is up to the laboratory operator to become throughly familiar with such rules in order to organize and operate a safe laboratory. 

After informing himself on regulations and other safety information, the laboratory operator will be ready to meet and discuss plans with the authorities. To many, this is considered at best a nuisance to be avoided if at all possible. Some think, for instance, that a call to OSHA for information will alert this agency to the fact that a laboratory is there and will be followed up by inspection. Likewise, they fear, a call to the local building department... 

Unfortunately, in the minds of many regulators the word laboratory may conjure up visions of fires, explosions, and highly toxic materials. For that reason, a laboratory planner should be prepared to present the proposed operation in great detail and to answer all questions, even those which may not seem relevant. Any work planned for the future should also be discussed, since the added cost of accommodating for it in the beginning may be just a fraction of what would have to be paid for later modifications. All pertinent facts must be revealed a minor omission could make a big difference in laboratory safety. A laboratory operator who has studied the various rules and regulations with care will have no problem handling such discussions. 

Fume hoods must be of a type suitable for the service they are intended to perform. For many applications, minimum face velocity is specified by regulations. An installer should always check the velocity when a new hood is placed in operation. It should be rechecked whenever any modification is made to the exhaust system. It is up to the laboratory operator to make certain that a hood is not put to new uses for which it was not designed. 

Additional information may be had on storage of chemicals from several sources. Material Safety Data Sheets, for example, have specific instructions with regard to storage. The local fire inspector will have good suggestions, and much can be found in reference books. Above all, the laboratory operator should throughly familiarize himself with all chemicals to be used in order to develop a safe storage system. 

Problems do occur when a laboratory is installed in an existing building on a small scale, often without a building permit, or when an existing laboratory is expanded in a so-called minor way. Such situations are common in industry. A prudent laboratory operator should demand complete compliance with rules in such cases despite cost, w hich could be high, particularly when old mistakes have to be corrected. 

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