Automated Methods of Analysis One of the major developments in analytical chemistry during the last four decades has

been the appearance of commercial automatic analytical systems, which provide analytical data with a minimum of operator intervention. Initially, these systems were designed to fulfill the needs of clinical laboratories, where perhaps 30 or more species are routinely determined for diagnostic and screening purposes. Domestically, hundreds of millions of clinical analyses are performed annually; the need to keep their cost at a reasonable level is obvious. These two considerations motivated the development of early automatic analytical systems. Now, such instruments find application in fields as diverse as the control of industrial processes and the routine determination of a wide spectrum of species in air, water, soils, and pharmaceutical and agricultural products.

An Overview of Automatic Instruments and Instrumentation At the outset, it should be noted that be International Union of Pure and Applied Chemists recommends that a distinction be made between automatic and automated systems. By IUPAC terminology, automatic devices do not modify their operation as a result of feedback from an analytical transducer. For example, an automatic acid/base titrator adds reagent to a solution and simultaneously records pH as a function of volume of reagent. In contrast, an automated instrument contains one or more feedback systems that control the course of the analysis. Thus, some automated titrators compare the potential of a glass electrode to its theoretical potential at the equivalence point and use the difference to control the rate of addition of acid or base. While this distinction between automatic and automated may be useful, it is not one that is followed by the majority of authors, nor is it followed in this presentation.

Advantages and Disadvantages of Automatic Analysis In the proper context, automated instruments offer a major economic advantage because of their savings in labor costs. For this advantage to be realized, however, it is necessary that be volume of work for the instrument be large enough to offset the original capital investment, which is often large, and the extensive effort that is usually required to put the automatic system in full operation. For laboratories in which large numbers of routine analyses are performed daily, the savings realized by automation can be enormous. With respect to savings in labor

costs, it is worthwhile noting that most automated instruments require less skilled, and thus less expensive, operating personnel; on the other hand, more skilled supervisors may be necessary. A second major advantage of automated instruments is their speed, which is frequently significantly greater than that of manual devices. Indeed, this speed often makes possible the continuous monitoring of the composition of products as they are being manufactured. This information in turn permits alteration of conditions to improve quality or yield. Continuous monitoring is also useful in medicine where analytical results can be used to determine patients current condition and their response to therapy. A third advantage of automation is that a well-designed analyzer can usually produce more reproducible results over a long period of time than can an operator employing a manual instrument. Two reasons can be cited for the higher precision of an automated device. First, machines do not suffer from fatigue, which has been demonstrated to adversely affect the result obtained manually, particularly near the end of a working day. A more important contributing factor to precision is the high reproducibility of the timing sequences of automated instruments-a reproducibility that can seldom be matched in human manual operations. For example, automatic analyzers permit the use of colorimetric reactions that are incomplete or that yield products whose stabilities are inadequate for manual measurement. Similarly, separation techniques, such as solvent extraction or dialysis, where analyte recorveries are incomplete, are still applicable when automated systems are used. In both instances, the high reproducibility of the timing of the operational sequences assures that samples and standards are processed in exactly the same way and for exactly the same length of time.

Unit Operations in Chemical Analysis All analytical methods can be broken down into a series of eight steps, or unit operations, any one of which can be automated. Table 33-1 lists these steps in the order in which they occur in a typical analysis. In some cases, it is possible to dispense with one or more of these operations, but several are required in every analysis. In a totally automatic method, all of the unit operations just listed are performed without human intervention. That is, with a totally automatic instrument, an unmeasured quantity of the untreated sample is introduced into the device, and ultimately an analytical result is produced as a printout or graph. Such instruments are common in clinical laboratories but are less frequently

encountered in industrial and university settings because no totally automatic instrument exists that can accommodate the wide variety of sample matrices and compositions that are encountered in such laboratories.