Time-Based Injection Procedures

Common for the time-based injection procedures is that the sample volume is metered as a function of time, the most important feature of this 

Riley et al. [394] in 1983 introduced an injection technique that they termed controlled-dispersion flow analysis. In this, a computer-con- 

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The same statistical procedures were used here to evaluate the effects of humics on batch and continuous LLE. A base extraction procedure (19) was required for processing methylene chloride extracts prior to GC injection in order to protect the GC column from contamination by humics. This process led to losses of 2,4-dichlorophenol and the chlorinated biphenyls. Therefore, these compounds were not used in the evaluation of the CLLE in the presence of humics. All other compounds were not affected by the base extraction procedure. The ANOV procedure tested each compound for changes in concentration by comparing early batch extraction recoveries (from freshly prepared solution) to later ones (after the 12.5-L extraction). This process was done separately for Parts 1 and 2. It was therefore possible to test each compound for time-dependent decreasing concentration with and without the presence of humics. 

In flow-based analytical procedures where the chemical reactions involved and/or the steps of analyte separation/concentration are relatively slow, the analytical signal can be attenuated by reducing the mean available time for the development of these physico-chemical processes. From a practical point of view, the result is equivalent to in-line analyte dilution. This possibility has been exploited in the spectrophotometric determination of hydrogen peroxide in contact lens care solutions using a sequential injection lab-on-valve system [60]. In view of the high sensitivity of the reaction between the analyte and 2,2,-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) in the presence of the enzyme... 

Several instrument manufacturers supply flame photometers designed specifically for the determination of sodium, potassium, lithium, and sometimes calcium in blood serum, urine, and other biological fluids. Single-channel and multichannel (two to four channels) instruments are available for these determinations. In the multichannel instruments, each channel can be used to determine a separate element without an internal standard, or one of the channels can be reserved for an internal standard such as lithium. The ratios of the signals from the other channels to the signal of the lithium channel are then taken to compensate for flame noise and noise from fluctuations in reagent flow rate. Flame photometers such as these have been coupled with flow injection systems to automate the sample-introduction process (see Section 33B-3). Typical precisions for flow-injection-analysis-based flame photometric determinations of lithium, sodium, and potassium in serum are on the order of a few percent or less. Automated flow injection procedures require l/KIO the amount of sample and 1/10 the time of batch procedures. -... 

Wahl and Deck were able to obtain an estimate of an assumed second-order rate coefficient ( 10 l.mole" .sec at 4°C) using a separation procedure based on the extraction of Fe(CN)e by a chloroform solution of Ph AsCl, in the presence of the ions Co(CN)g and Ru(CN)6, to reduce the exchange between the iron species in the two liquid phases. A similar estimate was obtained using a precipitation method in the presence of the carrier Ru(CN)6. A direct injection technique was used as short reaction times were necessary. Wahl has reviewed the large induced exchanges occurring in the chemical separation methods. The extraction procedure when the carriers Co(CN)6 and Ru(CN) are present provides the most satisfactory method of separation. ... 

The outline of this paper is as follows. First, a theoretical model of unsteady motions in a combustion chamber with feedback control is constructed. The formulation is based on a generalized wave equation which accommodates all influences of acoustic wave motions and combustion responses. Control actions are achieved by injecting secondary fuel into the chamber, with its instantaneous mass flow rate determined by a robust controller. Physically, the reaction of the injected fuel with the primary combustion flow produces a modulated distribution of external forcing to the oscillatory flowfield, and it can be modeled conveniently by an assembly of point actuators. After a procedure equivalent to the Galerkin method, the governing wave equation reduces to a system of ordinary differential equations with time-delayed inputs for the amplitude of each acoustic mode, serving as the basis for the controller design. 

Determination of CholesteroL For meat extraction, the procedures for determining the cholesterol of extracted lipid samples were described Chao et al. (2i). For edible beef tallow extraction, the preparation of samples for cholesterol content was based on the AOAC (22) method Section 28.110. The prepared sample was then injected into a Supelco SPB-1 fused silica capillary column of 30 meters x 032 mm i.d. in a Varian Model 3700 gas chromatograph equipped with dual flame ionization detectors. The initial holdup time was 4 min at 270°C and then programmed to a temperature of 300°C at a ramp rate of 10°C/min. Helium flow rate and split ratio were 13 ml and 50 1, respectively, while the injector/detector temperature was 310°C. 

Calibration and quantification procedures are easier in LA-ICP-MS compared to other solid-state mass spectrometric techniques because the laser ablation and the ICP ion source operate at normal pressure and the laser ablation of solid samples and ionization of analytes are separated in space and time. Therefore the advantage of solution calibration in ICP-MS can be applied in this solid-state analytical technique. The introduction of solution based calibration, which is only possible in LA-ICP-MS, was an innovative step in the development of this sensitive mass spectrometric technique. A number of different calibration approaches using aqueous standard solutions in the dual gas flow technique have been discussed by various authors.74 75 In the dual gas flow injection technique , the nebulized standard solution and the laser ablated sample material are mixed in the -piece and the two gas flows from the nebulizer (e.g. ultrasonic nebulizer) and laser ablation chamber are added. Using solution based calibration with the addition of a standard solution, Leach et alP determined minor elements in steel reference materials with a relative accuracy of a few %. In comparison to the so-called dual gas flow technique proposed in the literature, where the argon flow rates through the nebulizer and ablation cell add up to 11 min-1 (e.g. 0.451 min-1 and... 

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