Apparatus pumps

Apparatus Pumping systems used in these studies for high-performance columns were a Varian 8500 syringe pump and a Varian 5000 isocratic pump. An Altex IlOA was employed for the con-trolled-pore glass (CPG) columns. Waters Associates model 401 refractometers were used on all instruments. Stagnant mobile phase was kept in the reference side of the refractometer. Samples were injected with a Rheodyne 70-10 injection valve using a 20yl loop (lOOyl for CPG columns). 

Waters High Pressure Liquid Chromatography apparatus (pump 6000 A, injector U6K, UV detector 440, u-styragel columns set 10 - 10 - 10 - 500 A), =254 nm, flow rate ... 

The same appHes to the formwork plans from which the details of the concrete components are derived. Here, the foundations of the apparatuses, pump sumps, ramps, floor ducts etc. are in the focus of the process engineer. 

These limitations have recently been eliminated using solid-state sources of femtosecond pulses. Most of the femtosecond dye laser teclmology that was in wide use in the late 1980s [11] has been rendered obsolete by tliree teclmical developments the self-mode-locked Ti-sapphire oscillator [23, 24, 25, 26 and 27], the chirped-pulse, solid-state amplifier (CPA) [28, 29, 30 and 31], and the non-collinearly pumped optical parametric amplifier (OPA) [32, 33 and 34]- Moreover, although a number of investigators still construct home-built systems with narrowly chosen capabilities, it is now possible to obtain versatile, nearly state-of-the-art apparatus of the type described below Ifom commercial sources. Just as home-built NMR spectrometers capable of multidimensional or solid-state spectroscopies were still being home built in the late 1970s and now are almost exclusively based on commercially prepared apparatus, it is reasonable to expect that ultrafast spectroscopy in the next decade will be conducted almost exclusively with apparatus ifom conmiercial sources based around entirely solid-state systems. 

An interferometric method was first used by Porter and Topp [1, 92] to perfonn a time-resolved absorption experiment with a -switched ruby laser in the 1960s. The nonlinear crystal in the autocorrelation apparatus shown in figure B2.T2 is replaced by an absorbing sample, and then tlie transmission of the variably delayed pulse of light is measured as a fiinction of the delay This approach is known today as a pump-probe experiment the first pulse to arrive at the sample transfers (pumps) molecules to an excited energy level and the delayed pulse probes the population (and, possibly, the coherence) so prepared as a fiinction of time. 

Figure B2.3.3. Crossed-moleciilar beam apparatus employed for die study of the F + D2 —> DF + D reaetion. Indieated in the figure are (1) the effusive F atom soiiree (2) slotted-disk veloeity seleetor (3) liquid-nitrogen-eooled trap (4) D2 beam souree (7) skimmer (8) ehopper (9) eross-eorrelation ehopper for produet veloeity analysis and (11) rotatable, ultralrigh-vaeuum, triply differentially pumped, mass speetrometer deteetor ehamber. Reprinted with pemrission from Lee [29], Copyright 1987 Ameriean Assoeiation for the Advaneement of Seienee.

The example above of tire stopped-flow apparatus demonstrates some of tire requirements important for all fonns of transient spectroscopy. These are tire ability to provide a perturbation (pump) to tire physicochemical system under study on a time scale tliat is as fast or faster tlian tire time evolution of tire process to be studied, the ability to synclironize application of tire pump and tire probe on tliis time scale and tire ability of tire detection system to time resolve tire changes of interest. 

Figure C3.1.8. Schematic diagram of a transient kinetic apparatus using iaser-induced fluorescence (LIF) as a probe and a CO2 iaser as a pump source. (From Steinfeid J I, Francisco J S and Fiase W L i989 Chemical Kinetics and. Dynamics (Engiewood Ciiffs, NJ Prentice-Fiaii).)...

Figure C3.1.11. Apparatus for pump-probe time-resolved resonance Raman spectroscopy. (From Varotsis C and Babcock G T 1993 K4ethods Enzymol. 226 409-31.)...

Ultrafast TRCD has also been measured in chemical systems by incoriDorating a PEM into the probe beam optics of a picosecond laser pump-probe absorjDtion apparatus [35]. The PEM resonant frequency is very low (1 kHz) in these experiments, compared with the characteristic frequencies of ultrafast processes and so does not interfere with the detection of ultrafast CD changes. 

Schematic diagrams of modem experimental apparatus used for IR pump-probe by Payer and co-workers [50] and for IR-Raman experiments by Dlott and co-workers [39] are shown in figure C3.5.3. Ultrafast mid-IR pulse generation by optical parametric amplification (OPA) [71] will not discussed here. Single-colour IR pump-probe or vibrational echo experiments have been perfonned with OP As or free-electron lasers. Free-electron lasers use...

Mercury is extensively used in various pieces of scientific apparatus, such as thermometers, barometers, high vacuum pumps, mercury lamps, standard cells (for example the Weston cell), and so on. The metal is used as the cathode in the Kellner-Solvay cell (p. 130). 

When constructing a manometer of the type shown in Fig. 12(c), it is impor tant to apply a very high vacuum (e.g., with a Hy-Vac pump) to the manometer while the mercury in the left-hand (sealed) limb is heated until it boils unless this is done, traces of air will remain in this limb and cause inaccurate readings. During a distillation, the tap I should be kept closed except when a pressure reading is being taken if it is left open indefinitely, a sudden default by the distillation apparatus or by the pump may cause the mercury in the sealed limb of G to fly back and fracture the top of the limb. 

The complete filtration apparatus is shown in Fig. 5, p. 11. A simpler and cheaper apparatus is shown in Fig. 45. This consists of a boiling-tube A having a side-arm for connection to the pump the tube A is conveniently held in a wooden or cork block B or in a clamp. The funnel F may be fitted into A through a pliable rubber disc D the latter is more useful than a cork since it covers tubes of various diameters. The filtrate is collected in the centrifuge-tube T. 

Chill the concentrated solution of the amine hydrochloride in ice-water, and then cautiously with stirring add an excess of 20% aqueous sodium hydroxide solution to liberate the amine. Pour the mixture into a separating-funnel, and rinse out the flask or basin with ether into the funnel. Extract the mixture twice with ether (2 X25 ml.). Dry the united ether extracts over flake or powdered sodium hydroxide, preferably overnight. Distil the dry filtered extract from an apparatus similar to that used for the oxime when the ether has been removed, distil the amine slowly under water-pump pressure, using a capillary tube having a soda-lime guard - tube to ensure that only dry air free from carbon dioxide passes through the liquid. Collect the amine, b.p. 59-61°/12 mm. at atmospheric pressure it has b.p. 163-164°. Yield, 18 g. 

Assemble in a fume-cupboard the apparatus shown in Fig. 67(A). Place 15 g. of 3,5-dinitrobenzoic acid and 17 g. of phosphorus pentachloride in the flask C, and heat the mixture in an oil-bath for hours. Then reverse the condenser as shown in Fig. 67(B), but replace the calcium chloride tube by a tube leading to a water-pump, the neck of the reaction-flask C being closed with a rubber stopper. Now distil off the phosphorus oxychloride under reduced pressure by heating the flask C in an oil-bath initially at 25-30, increasing this temperature ultimately to 110°. Then cool the flask, when the crude 3,5-dinitro-benzoyl chloride will solidify to a brown crystalline mass. Yield, 16 g., i.e,y almost theoretical. Recrystallise from caibon tetrachloride. The chloride is obtained as colourless crystals, m.p. 66-68°, Yield, 13 g Further recrystallisation of small quantities can be performed using petrol (b.p. 40-60°). The chloride is stable almost indefinitely if kept in a calcium chloride desiccator. 

Dissolve 1 g. of anthracene in 10 ml. of glacial acetic acid and place in 50 ml. bolt head flask fitted with a reflux water-condenser. Dissolve 2 g. of chromium trioxide in 2 ml. of water and add 5 ml. of glacial acetic acid. Pour this solution down the condenser, shake the contents of the flask and boil gently for 10 minutes. Cool and pour the contents of the flask into about 20 ml. of cold water. Filter off the crude anthraquinone at the pump, wash with water, drain well and dry. Yield, 1 g. Purify by re crystallisation from glacial acetic acid or by sublimation using the semi-micro sublimation apparatus (Fig. 35, p. 62, or Fig. 50, p. 70). 

Assemble an apparatus similar to that used in the prenous experiment, i.e., a 500 ml. conical flask fitted at the neck with a freshly-charged calcium chloride tube, a dropping-funnel, and in addition an outlet-tube joined to the water-pump so that dry air can be drawn through the calcium chloride tube and thence through the conical flask. The purpose of the air-stream is to remove as much as possible of the excess of hydrogen chloride. 

Meanwhile set up the ether distillation apparatus as used in the preparation of triethyl phosphite (p. 308). Distil off the ether and then fractionally distil the residue at water-pump pressure. The di-isopropyl hydrogen phosphite distils at 79Vi4 mm. other b.ps. are 8o°/i5 mm., 82-5°/i7 mm. Yield, 25 g., 89%. 

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