In procedure

An interesting example of a large specific surface which is wholly external in nature is provided by a dispersed aerosol composed of fine particles free of cracks and fissures. As soon as the aerosol settles out, of course, its particles come into contact with one another and form aggregates but if the particles are spherical, more particularly if the material is hard, the particle-to-particle contacts will be very small in area the interparticulate junctions will then be so weak that many of them will become broken apart during mechanical handling, or be prized open by the film of adsorbate during an adsorption experiment. In favourable cases the flocculated specimen may have so open a structure that it behaves, as far as its adsorptive properties are concerned, as a completely non-porous material. Solids of this kind are of importance because of their relevance to standard adsorption isotherms (cf. Section 2.12) which play a fundamental role in procedures for the evaluation of specific surface area and pore size distribution by adsorption methods. 

The earliest examples of analytical methods based on chemical kinetics, which date from the late nineteenth century, took advantage of the catalytic activity of enzymes. Typically, the enzyme was added to a solution containing a suitable substrate, and the reaction between the two was monitored for a fixed time. The enzyme s activity was determined by measuring the amount of substrate that had reacted. Enzymes also were used in procedures for the quantitative analysis of hydrogen peroxide and carbohydrates. The application of catalytic reactions continued in the first half of the twentieth century, and developments included the use of nonenzymatic catalysts, noncatalytic reactions, and differences in reaction rates when analyzing samples with several analytes. 

Other uses of oxyacetylene flames in mill operations are in building up or hardfacing metal, lancing (piercing a hole in a metal mass), and a variety of metal cleaning procedures. A minor but interesting fuel use of acetylene is in flame spectrophotometry where oxygen and nitrous oxide are used as oxidants in procedures for a wide variety of the elements. 

Analytical and Test Methods. Many of the procedures for technical analyses of magnesium hydroxide are readily available from the principal producers. These procedures should be carefully reviewed. Site-specific variations in procedure steps and mechanics, especially for chemical activity, can bias results and inadvertantiy disqualify an otherwise acceptable product. 

Polymerization Processes. Vinyl acetate has been polymerized industrially by bulk, solution, suspension, and emulsion processes (34). Perhaps 90% of the material identified as poly(vinyl acetate) or copolymers that are predominantly vinyl acetate are made by emulsion techniques. Detailed information is in patent and scientific Hterature and in procedures available in the brochures from monomer producing companies (15,34). 

What are the equipment manufacturer s recommendations for use of the equipment and is it reflected in procedures ... 

The numbers in parentheses following the name of the eompound refer to the volume and page of Organic S5mtheses. New methods or changes in procedure have not been checked unless otherwise noted.)... 

Accounting for staff can be difficult hence tlie advantage of site logging-in procedures. Instructions... 

It may have been possible to implement very obvious waste-reduction measures already, before embarking on obtaining a material balance (even as early as at the end of Phase I). You should now consider the material balance information in conjunction with visual observations made during the data-collection period, to pinpoint areas or operations where simple adjustments in procedure could greatly improve the efficiency of the process by reducing unnecessary losses. 

Process operators may take limited action in danger areas if they (1) have informed the incident command structure of the emergency. (2) have adequate PPE. (3) have adequate training in procedures they are to perform, and (4) employ the buddy system... 

Site D lacked a sufficient CRZ and also lacked access/egress control for the exclusion zone. The site control plan did not accurately identify the function of the CRZ as a buffer zone between the exclusion zone and the support zone, and there was no buffer area between the decontamination pad and the road that runs adjacent to the pad, marked as a support zone. Also, an exclusion zone log-in procedure for tracking personnel who enter and exit this zone was not used on site as called for in the SSAHP. 

No technicians participation in procedures development, hence, no sense of ownership. 

Techniques for quantifying Techniques used were basically from NUREG/CR-1278 or PRA Procedun s Guide, Chapter 4. (l)THERP (1980 version NUREG/CR-1278 with appropriate factors for a tree was used in procedure defined events. (2) A time dependent modeling approach was used to quantify operator actions during a sequence. THERPmethixlr. were ii ,cd as described in WASH- Id ... 

Whether you have one procedure or twenty to address this requirement you need to cover all types of equipment as well as test software if you use it. Some of the requirements of this section may need to be addressed in procedures developed for other purposes, such as the requirement for determination of measurements. 

There is only a requirement for a record of changes in procedures and not changes in plans, specifications, and drawings, which are clearly not procedures, but whether it be procedures, work instructions, or other types of instructions, you will need to be able to demonstrate that you have a system for preventing the recurrence of nonconformities. 

A carbonyl group cannot be protected as its ethylene ketal during the Birch reduction of an aromatic phenolic ether if one desires to regenerate the ketone and to retain the 1,4-dihydroaromatic system, since an enol ether is hydrolyzed by acid more rapidly than is an ethylene ketal. 1,4-Dihydro-estrone 3-methyl ether is usually prepared by the Birch reduction of estradiol 3-methyl ether followed by Oppenauer oxidation to reform the C-17 carbonyl function. However, the C-17 carbonyl group may be protected as its diethyl ketal and, following a Birch reduction of the A-ring, this ketal function may be hydrolyzed in preference to the 3-enol ether, provided carefully controlled conditions are employed. Conditions for such a selective hydrolysis are illustrated in Procedure 4. 

Toluene is a useful co-solvent in metal-ammonia reductions as first reported by Chapman and his colleagues. The author has found that a toluene-tetrahydrofuran-ammonia mixture (1 1 2) is a particularly useful medium for various metal-ammonia reductions. Procedure 8a (section V) describes the reduction of 17-ethyl-19-nortestosterone in such a system. Ethylene dibromide is used to quench excess lithium. Trituration of the total crude reduction product with methanol affords an 85% yield of 4,5a-dihydro-17-ethyl-19-nortestosterone, mp 207-213° (after sintering at 198°), reported mp 212-213°. For the same reduction using Procedure 5 (section V), Bowers et al obtained a 60% yield of crude product, mp, 196-199°, after column chromatography of the total reduction product. A similar reduction of 17-ethynyl-19-nortestosterone is described in Procedure 8b (section V). The steroid concentration in the toluene-tetrahydrofuran-ammonia system is 0.05 M whereas in the ether-dioxane-ammonia system it is 0.029 M. 

The general reaction procedure and apparatus used are exactly as described in Procedure 2. Ammonia (465 ml) is distilled into a 2-liter reaction flask and to this is added 165mlofisopropylalcoholandasolutionof30g(0.195 mole) of 17/ -estradiol 3-methyl ether (mp 118.5-120°) in 180 ml of tetrahydrofuran. The steroid is only partially soluble in the mixture. A 5 g portion of sodium (26 g, 1.13 g-atoms total) is added to the stirred mixture and the solid dissolves in the light blue solution within several min. As additional metal is added, the mixture becomes dark blue and a solid (matted needles) separates. Stirring is inefficient for a few minutes until the mass of crystals breaks down. All of the sodium is consumed after 1 hr and 120 ml of methanol is then added to the mixture with care. The product is isolated as in Procedure 4h 2. After being air-dried, the solid weighs 32.5 g (ca. 100% for a monohydrate). A sample of the material is dried for analysis and analyzed as described in Procedure 2 enol ether, 91% unreduced aromatics, 0.3%. The crude product may be crystallized from acetone-water or preferably from hexane. 

The reduction is carried out much as described in Procedure 2. Ammonia (950 ml) is distilled into a 5-liter reaction flask and 950 ml of /-amyl alcohol and a solution of the ketal in 950 ml of methylcyclohexane are added with good stirring. Sodium (57 g, 2.5 g-atoms) is added in portions. The reaction mixture becomes blue within 30-45 min after the sodium is added and the metal is consumed within about 3 hr after the blue color appears. After the mixture becomes colorless, 200 ml of ethanol is added and the ammonia is allowed to boil off through a mercury trap. Then 500 ml of water and 500 ml 0% potassium bicarbonate solution are added and the organic layer is separated. The organic layer is washed once with 10 % potassium bicarbonate... 

The reduction is effected exactly as in Procedure 8a but using 0.61 g (0.088 g-atom) of lithium. After the crude reaction product has been washed well on the filter with cold water, it is dissolved in ethyl acetate, the solution is filtered through the sintered glass funnel to remove iron compounds from the ammonia, and the filtrate is extracted with saturated salt solution. The organic layer is dried over sodium sulfate and the solvent is removed. The solid residue is crystallized from methanol (120 ml) using Darco. The mixture is cooled in an ice-bath, the solid is collected, rinsed with cold methanol, and then air-dried to give 12.9 g (85%), mp 129-132° reported for the tetrahydropyranyi ether of 3j5-hydroxypregn-5-en-20-one, mp 129-131°. 

The tetrahydropyranyi ether is prepared and reduced exactly as in Procedures 8a and 8c up to the point at which ethylene dibromide would be added. At this point 27 ml (61.5 g, 0.43 mole) of methyl iodide is added instead the addition requires 1-2 min and should be cautious at first. The mixture is stirred for 1 hr and the ammonia is allowed to boil off overnight. The product is isolated as described in Procedures 8a and 8c except that a larger volume of ethyl acetate is required to dissolve the product than in 8c. After removal of the ethyl acetate, the residual material is crystallized from methanol (400 ml). 

This chapter describes some accidents that occurred because operating procedures were poor. It does not include accidents that occurred because of defects in procedures for preparing equipment for maintenance or vessels for entry. These are discussed in Chapters 1 and 11. 

When performing human reliability assessment in CPQRA, a qualitative analysis to specify the various ways in which human error can occur in the situation of interest is necessary as the first stage of the procedure. A comprehensive and systematic method is essential for this. If, for example, an error with critical consequences for the system is not identified, then the analysis may produce a spurious impression that the level of risk is acceptably low. Errors with less serious consequences, but with greater likelihood of occurrence, may also not be considered if the modeling approach is inadequate. In the usual approach to human reliability assessment, there is little assistance for the analyst with regard to searching for potential errors. Often, only omissions of actions in proceduralized task steps are considered. 

The Information Contained in Procedures Is Correct, but It Is Not Cast in a Form Usable by the Individual at His or Her Workplace. 

Check Road Tanker while filling Provide secondary task involving other personnel. Supervisor periodically checks operation Stress importance of regular checks for safety Provide automatic log-in procedure... 

Effects of Improvements in Procedures on Error Probabilities Calculated Using SLIM... 

ORIGINAL ERROR PROBABILITY AFTER IMPROVEMENTS IN PROCEDURES RATIO BEFORE/AFTER IMPROVEMENTS... 

These are defined in MORT as changes in procedures without an associated safety review. 

Training and procedures were not available for blowdown situations. Blowdown was dealt with only briefly in training, and was either ambiguously referred to in procedures or did not appear at all. Workers viewed blowdown... 

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