1 /2-hour method

TWA DAAMS monitoring may be performed using a 12-hour method. 

Jones, D. L., Braiisford, M. A., and Drocourt, J.-L. Solid phase, laser-scanning cytometry a new two-hour method for the enumeration of microorganisms in pharmaceutical water. Pharm. Forum 25 7626—7645,1999. 

D Haese E, Dumon I, Werbrouck H, Dejonghe V, Herman L (2005) Improved detection of Mycobacterium paratuberculosis in mfik. J Dairy Res 72 125-128 Guyomard S (1997) Vahdation of a scanning laser system for microbiological quality control (QC) analysis. Pharm Technol Fur (September) 50-54 Jones DL, Brailsford MA, Drocourt JL (1999) Solid-phase, laser-scanning cytometry a new two-hour method for the enumeration of microorganisms in pharmaceutical water. Pharmacopeia Forum 25 7626-7645... 

Soil, nonexchangeable (fixed) ammonium Pretreat soil with KOBr-KOH, shake with 5 N HF-1N HCI for 24 hours Method 84-7, steam distillation with KOH, titration Not reported Not reported Bremner 1965... 

In manufacturing, time study and predetermined motion time data are the major sources for obtaining standard data. In construction and white-collm environments, work sampling and man-hour reports are the principal means of information. Likewise, in certain government agencies, such as the post office and the military depots, work sampling and man-hour methods are used. 

Vajda and Kovacs described three methods labeled A, B, and C, for the direct amination of the pyridine with alkyl amines in the presence of sodium amide or finely divided potassium or sodium metal. An example of method A was the preparation of 2-M-butylaminopyridine from a mixture of n-butylamine, pyridine, and sodium amide in boiling toluene (60 hours). In method B, powdered sodium (or potassium) metal was used instead of sodium amide and the reflux time was 20 hours. Method C employed sodium metal, a bath temperature of 120°, boiling under reflux with stirring for 3 hours and an additional 7 hours of boiling without stirring. The yields of 2-n-butylamino-pyridine in the above three methods were 38%, 50%, and 33%, respectively. These authors claimed that the reaction proceeded via a radical rather than an ionic (nucleophilic) pathway because dipyridyls were also formed. When a pyridine is heated with a three- to fourfold excess of a primary aliphatic amine in the presence of finely divided sodium metal, 70 to 80% yields of 2-alkylaminopyridines are obtained. ... 

Step 1 A quick and cheap action for testing the peak homogeneity the J/2 hour method ... 

Lamp Method the sample is burned in a closed system in an atmosphere of 70% CO2 and 30% oxygen in order to avoid formation of nitrogen oxides. This method was to have been abandoned as it takes three hours to carry out, but remains officially required for jet fuel sulfur analysis. 

The suggested method is appropriately implemented at the practice. The cost and working hours of unit measurement of it is less than of any alternative method of destructive test and with respect to the authenticity inspection of Stress-Deformation the given method is inferior only to destructive testing. The method was successfully implemented while evaluation of service life of main pipe-lines sections and pressure vessels as well. Data of method and instrument are used as official data equally with ultrasonic, radiation, magnetic particles methods, adding them by the previously non available information about " fatigue " metalwork structure. 

The system allows the inspeetion of all the blade roots of the whole engine within less than one hour. This is a very fast method which fulfils all the customer requirements concerning reliability, inspeetion speed and the inspeetion on the wings". 

Since the drop volume method involves creation of surface, it is frequently used as a dynamic technique to study adsorption processes occurring over intervals of seconds to minutes. A commercial instrument delivers computer-controlled drops over intervals from 0.5 sec to several hours [38, 39]. Accurate determination of the surface tension is limited to drop times of a second or greater due to hydrodynamic instabilities on the liquid bridge between the detaching and residing drops [40],... 

The procedure is computationally efficient. For example, for the catalytic subunit of the mammalian cAMP-dependent protein kinase and its inhibitor, with 370 residues and 131 titratable groups, an entire calculation requires 10 hours on an SGI 02 workstation with a 175 MHz MIPS RIOOOO processor. The bulk of the computer time is spent on the FDPB calculations. The speed of the procedure is important, because it makes it possible to collect results on many systems and with many different sets of parameters in a reasonable amount of time. Thus, improvements to the method can be made based on a broad sampling of systems. 

Fig. 1. CPU times (in hours) for 1 ps MD runs for various proteins using three different methods, direct velocity Verlet with a time-step 0.5 fs, r-RESPA with direct evaluation of electrostatic forces and an overall time-step of 4.0 fs, and r-RESPA/TFMM with an overall time-step 4.0 fs (combination of (2,2,2,2) in force breakup).The energy conservation parameter log AE for the three methods are comparable. The CPU time (hours) is for RISC6000 /MODEL 590 computer.

One of the main advantages of the stochastic dynamics methods is that dramatic tirn savings can he achieved, which enables much longer stimulations to he performed. Fc example, Widmalm and Pastor performed 1 ns molecular dynamics and stochastic dynamic simulations of an ethylene glycol molecule in aqueous solution of the solute and 259 vvatc jnolecules [Widmalm and Pastor 1992]. The molecular dynamics simulation require 300 hours whereas the stochastic dynamics simulation of the solute alone required ju 24 minutes. The dramatic reduction in time for the stochastic dynamics calculation is du not only to the very much smaller number of molecules present hut also to the fact the longer time steps can often he used in stochastic dynamics simulations. 

Succinamide. NHoCOCH2 CH2CONH2. (Method 2(a)). Add 5 ml. (5 8 g.) of dimethyl succinate to a mixture of 50 ml. of water and 25 ml. of concentrated [dy o-88o) aqueous ammonia solution in a 150 ml. conical flask. Cork the flask and shake the contents the dimethyl succinate rapidly dissolves to give a clear solution. Allow the solution to stand after about i hour the succinamide starts to crystallise, and then continues to separate for some time. Next day, filter off the succinamide at the pump, wash with cold water, and drain. Recrystallise from water, from which the succinamide separates as colourless crystals the latter soften at 240° and melt at 254 -255° with... 

Reflux 1 ml. of the ether with 5 ml. of freshly distilled, constant boiling point hydriodic acid (Section 11,49,2), b.p. 126-128°, for 2-3 hours. Add 10 ml. of water, distil and collect about 7 ml. of liquid. Decolourise the distillate by the addition of a httle sodium bisulphite, and separate the two layers by means of a dropper pipette (Fig. 11,27,1). Determine the b.p. of the resulting iodide by the Siwoloboff method (Section 11,12) and prepare a crystalline derivative (Section 111,42). 

Preparation of SchlfT s reagent. Method 1. Dissolve 0- 2 g. of pure p.rosaniline hydrochloride in 20 ml. of a cold, freshly-prepared, saturated aqueous solution of sulphur dioxide allow the solution to stand for a few hours until it becomes colourless or pale yellow. Dilute the solution to 200 ml. and keep it in a tightly, stoppered bottle. If the bottle is not adequately stoppered, the reagent will gradually lose sulphur dioxide and the colour wUl return. The solution keeps well if not unnecessarily exposed to light and air. 

Method A. In a 500 ml. round-bottomed flask, fitted with a reflux condenser attached to a gas trap (Fig. II, 13, 8), place 59 g. of succinic acid and 117-5 g. (107-5 ml.) of redistilled acetyl chloride. Reflux the mixture gently upon a water bath until all the acid dissolves (1-2 hours). Allow the solution to cool undisturbed and finally cool in ice. Collect the succinic anhydride, which separates in beautiful crystals, on a Buchner or sintered glass funnel, wash it with two 40 ml. portions of anhydrous ether, and dry in a vacuum desiccator. The yield of succinic anhydride, m.p. 118-119°, is 47 g. 

Method B. In a 500 ml. round-bottomed flask, provided with a reflux condenser protected by a cotton wool (or calcium chloride) drying tube, place 59 g. of succinic acid and 102 g. (94-5 ml.) of redistilled acetic anhydride. Reflux the mixture gently on a water bath with occasional shaking until a clear solution is obtamed ca. 1 hour), and then for a further hour to ensure the completeness of the reaction. Remove the complete assembly from the water bath, allow it to cool (observe the formation of crystals), and finally cool in ice. Collect the succinic anhydride as in Method A. The yield is 45 g., m.p. 119-120°. 

Diethyl sebacate. Method A. Reflux a mixture of 100 g. of sebacic acid, 81 g. (102-5 ml.) of absolute ethyl alcohol, 190 ml. of sodium-dried benzene and 20 g. (11 ml.) of concentrated sulphuric acid for 36 hours. Work up as for Diethyl Adipate. B.p. 155-156°/6 mm. Yield 114 g. 

Method B. Reflux a mixture of 101 g. of sebacic acid, 196 g. (248 ml.) of absolute ethjd alcohol and 20 ml. of concentrated sulphuric acid for 12 hours. Distil oft about half of the alcohol on a water bath dilute the residue with 500-750 ml. of water, remove the upper layer of crude ester, and extract the aqueous layer with ether. Wash the combined ethereal extract and crude ester with water, then with saturated sodium bicarbonate solution until effervescence ceases, and finally with water. Dry with anhydrous magnesium or sodium sulphate, remove the ether on a water bath, and distil the residue under reduced pressure. B.p. 155-157°/6 mm. Yield llOg. 

Hydrolysis (or saponification) of n-butyl acetate. Boil 4-5 g. of n-butyl acetate (Section 111,95) with 50 ml. of 10 per cent, sodium hydroxide solution under reflux until the odour of the ester can no longer be detected (about 1 hour). Set the condenser for downward distiUation and coUect the first 10 ml. of distillate. Saturate it with potassium carbonate, aUow to stand for 5 minutes, and withdraw all the Uquid into a small pipette or dropper pipette. AUow the lower layer of carbonate solution to run slowly into a test-tube, and place the upper layer into a small test-tube or weighing bottle. Dry the alcohol with about one quarter of its buUr of anhydrous potassium carbonate. Remove the alcohol with a dropper pipette and divide it into two parts use one portion for the determination of the b.p. by the Siwoloboff method (Section 11,12) and convert the other portion into the 3 5-dinitrobenzoate (Section III, 27) and determine the m.p. 

Boil 2 g. of the ester with 30 ml. of 10 per cent, sodium or potassium hydroxide solution under reflux for at least 1 hour. If the alcohol formed is water (or alkali) soluble, the completion of the hydrolysis will be indicated by the disappearance of the ester layer. Distil ofiF the liquid through the same condenser and collect the first 3-5 ml. of distillate. If a distinct la3 er separates on standing (or upon saturation of half the distillate with potassium carbonate), remove this layer with a capillary dropper, dry it with a little anhydrous potassium carbonate or anhydrous calcium sulphate, and determine the b.p. by the SiwoloboflF method... 

Into a 1500 ml. round-bottomed flask place 97-5 g. of finely-powdered sodium cyanide (1), 125 ml. of water, and a few chips of porous porcelain. Attach a reflux condenser and warm on a water bath until all the sodium cyanide dissolves. Introduce a solution of 250 g. (196 ml.) of n-butyl bromide (Sections 111,35 and 111,37) in 290 ml. of pure methyl alcohol, and reflux gently on a water bath for 28-30 hours. Cool to room temperature and remove the sodium bromide which has separated by filtration through a sintered glass funnel at the pump wash the crystals with about 100 ml. of methyl alcohol. Transfer the filtrate and washings to From n caproamide by SOClj method. 

Method 2. Add gradually 2 -5 ml. of benzoyl chloride to a solution of 0-5 g. of glycerol in 5 ml. of pure pyridine, cooled in ice then reflux for 1 hour. Treat the cold mixture with dilute sulphuric acid this dissolves the pyridine salt and precipitates the glycerol tribenzoate. Wash it with sodium bicarbonate solution, followed by water, and recrystaUise as in Method 1. 

The sulphonanilldes may be prepared by either of the following methods —(i) Reflux the solution of the sulphonyl chloride in benzene obtained as above, with 2 5 g. of aniline for 1 hour. Concentrate the benzene solution to half its volume and cool in ice. Collect the solid which separates on a filter, wash with hot water, and recrystallise from ethanol or dilute ethanol. 

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