Application Engineering in Laboratory and Process ... - ACS Publications

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REPORT FOR ANALYTICAL

CHEMISTS

Application Engineering in Laboratory and Process Instruments

While basic physical or chemical principles are the same in laboratory, research scale, and process monitoring a n d control instruments, each application has its own problems of design, engineering, installation, and operation. To meet these needs, analytical instrument manufacturers have established application engineering units. A p p l i c a tion engineering in the case of process instruments is o b vious to the user; with laboratory instruments, contributions of application engineering, being "behind-thescenes," are not as obvious. This month's Report for Analytical Chemists outlines the application engineering approaches taken by some analytical instrument manufacturers to meet instrument needs in the laboratory and in the plant.

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monitoring and control of chemical processes has placed a major responsibility on the analytical instrument manufacturer. Equipment to provide automatic, direct concentration readout, for example, in a production scale operation is quite different from instrumentation developed for research and laboratory-scale use. Since process analyzer requirements cannot be met satisfactorily by simply plugging in laboratory t y p e instruments, new approaches have had to be used. T h e problems are diverse and t h e approaches to solving t h e m are equally diverse. E a c h of the major analytical instrument manufacturers is approaching the need for process analytical instrumentation a little differently. T h e approaches used by several of these are illust r a t e d in this article. Even though the same physical principles might be involved, entirely new concepts of design, manufacturing, and m a r -

keting became necessary to satisfy the process industries. This, in turn, has led m a n y major instrument manufacturers to establish application engineering units. I n s t r u m e n t manufacturers generally have applied the technique of application engineering to their laboratory instruments, although, to the user, results often are less a p p a r e n t than in the case of process instruments. W i t h process instruments, the application engineeringis obvious and often dramatic. T h e laboratory instrument, on the other hand, is the product of almost continuous application engineering which begins during development of the instrument and which continues behind the scenes as long as the instrument is produced. Chemists, physicists, and other technical personnel study changing requirements of the customers and, in turn, refine the product on subsequent m a n u facturing runs and develop accessories or new models to meet the changing needs.

Conventional laboratory instruments are standard units in t h a t all instruments having the same model number are exact duplicates and are manufactured on a mass production basis. Except for complex units, they are generally distributed by laboratory a p p a r a t u s dealers. These instruments are used by technically trained people who are familiar with their operation, application, and general use. All they need are an operation m a n u a l and application d a t a sheets. T h e y seldom need technical assistance from the manufacturer. Only in the case of very complex or complicated research-type or laboratory-type instruments do these scientists need technical assistance from the instrument manufacturer. The instrument manufacturer's responsibility in such cases, therefore, is to supply a well-designed and proven instrument a t the lowest possible cost. Application engineering responsibilities in this area consist of improving performance of the instruments, developing new uses, and new attachments for standard instruments to increase their versatility. T h e application engineer is also responsible for suggesting and helping design new instruments. Need for a new instrumental method is sometimes indicated in the literature. These developments often originate from extensive laboratory studies and as a result of consultations with instrument users. Information concerning applications of these instruments is disseminated in the form of application d a t a sheets, technical reports, papers published in technical journals, and books. E a c h of these steps is essential if the manufacturer is to promote wide usage and sales. I n the case of expensive laboratory instruments, the application engineer acts as liaison between the VOL. 33, NO. 10, SEPTEMBER 1961



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REPORT FOR ANALYTICAL CHEMISTS customer and the instrument company's sales department to ensure t h a t the right instrument is recommended to solve the customer's problems. One ill-advised purchase can hamper the adoption of other instrumental methods by a customer for many years. The application engineering group in the analytical instrumentation field is responsible for providing technical support of the marketing operations. Process Analysis Instrumentation In all but the more complicated units, and except for his continued improvement of subsequent models, the instrument manufacturer's responsibility as to the use of laboratory instruments usually ceases when the instrument leaves the shipping platform. This is not the case with process analyzers. Process instruments are usually sold on a plant stream performance basis. The instrument manufacturer's responsibility for a unit purchased on a performance basis is not completely discharged

until the unit is installed on the plant stream, is running and performing to the purchased specifications, and preferably starting to show the justification payout. Process instruments are designed to function continuously ; hence, are required to be rugged, reliable, simple in operation, and to have a very low order of maintenance and operator attention factor. Unlike laboratory analyzers, process analyzers are standard only to a certain point in manufacture. Beyond this, they are highly customized by the addition of special accessory equipment, and application engineered to handle a specific and usually unique analytical problem in the customer's plant stream. Just as few streams are identical as to composition, physical conditions, and environment in different plants, so few complete process analyzers are identical in their over-all form. W h a t may be considered to be minor stream differences, such as pressure, temperature, dew point, dirt load, trace impurities, etc., can require very different instrument configurations, sampling systems,

response times, accuracies, and maintenance schedules. As a consequence, few analysis instruments such as industrial gas chromatographs and process infrared analyzers are sold on a strictly hardware basis; most are purchased as complete process analysis systems. These are sold directly to the user or his contracting engineer and guaranteed to perform to definite mutually acceptable specifications at a specific point in a specific process stream of a specific plant. Application Engineering of Process Instruments The decision to employ process analyzers should be made only after careful guidance by those who are technically familiar with the requirements for instrumentation. A process should be engineered, from an instrument point of view, in exactly the same manner as it is operated on a manpower basis ; t h a t is, it should be neither under nor over instrumented. Expected yield and quality improvements, lower operating costs, lower capital ex-

Control room operator checks readings on process gas chromatograph

Photos courtesy of Beckman Instruments, Inc.

Explosive proof and non-explosive proof infrared stream analyzers, flow colorimeters, and specially-designed infrared automobile exhaust analyzer in the Process Infrared Laboratory, Application Engineering Department 28 A

•·

ANALYTICAL CHEMISTRY

REPORT FOR ANALYTICAL CHEMISTS

penditures on equipment and installation, increased safety and, of course, higher return on investment are the most important economic factors. In the case of high volume, multimillion dollar per year processes, an increase in yield of even a few tenths of a percent resulting from use of process analysis equipment might easily justify the cost of such equipment. The financial return resulting from properly used instruments illustrates this point. $2,000 to $5,000 per month is common, with $10,000 to $25,000 per month becoming more commonplace. In several instances, savings on complete plants have exceeded the $50,000 per month level. Of course, it can be argued that previously the plants had not been operated properly; nevertheless, before the processes were instrumented these savings were simply not known to exist. Before these gains can be physically accomplished in most cases, several technical problems must be overcome. It is here that the user must place his full confidence in

those who are vvell versed in the proper application of process analyzers and have the required experience in application engineering the complete unit into the plant stream. Regardless of the anticipated savings, the matter of the cost of the instrumentation is still of foremost interest to those who are relatively unfamiliar with analysis instrumentation. In these instances it is not unusual for the potential customer, whose familiarity with instrumentation stems from timehonored temperature, pressure, flow, or liquid level instrument hardware, to question the quoted price of the application engineering necessary to tailor the analysis instrument to his plant stream. It is not unusual in situations of this type for the customer to purchase the hardware only and handle the application engineering himself. This, as it turns out, is the most effective manner in which the value of application engineering can be demonstrated. The next order, 95% of the time, will cover complete application engineering. Relatively few companies have a tech-

nical staff experienced in handling problems in this area. Even when they have an experienced staff, many of these purchase application engineering since the over-all expense has been demonstrated to be as low or lower than their costs, plus the fact that their engineers are usually busy in other areas. Another very important aspect is that the instrument manufacturer assumes the complete responsibility for making the instrumentation operate to specifications. Of all the problems that have to be overcome in application engineering an analysis instrument into a process stream, sample handling is probably of paramount importance. The best instrument built is no better than the sampling system ahead of it. A properly designed sample system must take a representative sample from the stream, transport it to the analyzer, and act upon it either physically or chemically to put it into a form ready for analysis. The design of sample systems is an engineering science of its own and can at times involve as much cost as the analysis instru-

Field operator is shown adjusting bypass rotometer in process gas chromatograph

Several industrial gas chromatographs are being checked out in the Application Check-Out Laboratory in Application Engineering Department VOL. 33, NO. 10, SEPTEMBER 1961



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ANALYTICAL CHEMISTRY

ment that it serves. The general design criteria involve locating a proper sampling point, preventing composition changes in the system, drawing a sample flow rate consis­ tent with sample economy and process controllabilit}'·, maintaining constant pressure and temperature, and pretreating the sample to re­ move interfering components or contaminants. The more or less standard cus­ tomer-application engineering rela­ tionship is listed chronologically as follows: (1) Upon customer inquiry, con­ sult with customer on the feasibility of instrumenting and the type of instrument needed. (2) Work with customer or his contracting designer to ob­ tain the required data. (The proper time to instrument is when the plant is being de­ signed.) After the project has been approved and the approach decided upon, the literature is searched in the company library. Pertinent previous work done by the department is also reviewed for added information. If laboratory analysis is re­ quired, samples are obtained from the customer and the analysis completed. The limitations, sensitivity, ac­ curacy, and complete recom­ mended method is then sup­ plied to the customer for his evaluation. (3) Work up design calculations, performance specifications, and application engineering quotation covering sample handling and accessory equipment involved, includ­ ing control equipment if re­ quired. (4) Upon receipt of customer purchase order, application engineer the more or less standard production hard­ ware unit by modification and addition of critical com­ ponents and accessory equip­ ment, check performance specification of the final ver­ sion against the guaranteed performance specifications with respect to range, ac­

curacy, response time, and general operability. Run the unit continuously for several days on samples made up to the analysis of the cus­ tomer's stream, calibrate, re­ cord critical set points, and write up special installation instructions. (5) Work with customer through the instrument company's Service Department on in­ stallation, calibration, and start-up. Application Engineering and Return on Investment

Industry is interested in increas­ ing production, improving quality, and lowering costs. A most effec­ tive means is to adapt modern anal­ ysis instrumentation and control methods. The difference between notable success or dismal failure in choosing and installing this instru­ mentation rests with the technical competence of the application engi­ neering involved. Again, benefits of application en­ gineering in the field of laboratory instruments sometimes are not readily apparent to the buyer. The extensive research and experimenta­ tion conducted by some of the in­ strument manufacturers is not wit­ nessed by the customer. But the benefits are reflected in the wider applicability of the instruments produced. Many analyses, once considered too costly or too timeconsuming to conduct through standard wet chemical methods, have become rapid, routine pro­ cedures with new laboratory instru­ mentation. In the case of process instru­ ments, performance can, and sav­ ings usually can, be calculated prior to installation, by the customer's engineering group, with the assist­ ance of the instrument manufac­ turer's application engineering de­ partment. Instrumentation in general aver­ ages slightly better than 10% of plant investment. The analysis in­ strumentation portion is approxi­ mately 10% of this, or 1% of plant investment. On this basis, large companies might well have several million dollars worth of process analysis instrumentation.

Two new mass spectrometers Beckman's Application Engineering Department T h e Scientific and Process I n s t r u ments Division of B e c k m a n I n s t r u ments, Inc., located a t the firm's Fullerton, California, p l a n t organized t h e first application engineering group in the field of analytical instrumentation in 1953. T h e A p plication Engineering D e p a r t m e n t , which t o d a y has an annual budget of more t h a n 1/3 million dollars, was created as a result of the firm's awareness of the growing need for application engineering in industry's efforts to solve a wide variety of analytical problems in spectroscopy, electrochemistry, and gas chromatography, and particularly in the area of process instrumentation. Recent developments in food additive legislation, medical research, and computer control of process streams have created a need for advanced forms of instrumentation. T h e application engineering staff is actively working to devise techniques which will solve m a n y of the analytical problems which exist in these fields. L a t e in 1960 this d e p a r t m e n t had grown to such an extent t h a t it moved into larger quarters. R e gional application engineering laboratories have also been set up a t Chicago and Mountainside, N . J. These are staffed with chemists trained a t Fullerton. T h e Application Engineering D e p a r t m e n t functions as instrument consultants and analytical system designers to every conceivable process industry and field. T h e prime prerequisite in staffing this operation is choosing technical people, usually chemical engineers and chemists, with a number of years experience in the various process industries, who are intensely interested in instrumentation. Since analysis instrumentation is essentially a new field, most of the 24 technical people (chemists, chemical engineers, and physicists, and an M. D.) plus 12 technicians in this department have developed their instrumentation background with B e c k m a n over the past six to seven years. T h e y have developed a national reputation in their respective fields.

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31 A

REPORT FOR ANALYTICAL CHEMISTS Beckman's Application Engineering D e p a r t m e n t has two major sections: scientific (laboratory) instrumentation a n d process (industrial) instrumentation. T h e scientific instrument application engineering section includes a staff of 10 chemists a n d physicists with a p propriate technician a n d clerical support. T h e process instrument application engineering group is made u p of 14 chemists and chemical a n d electronic engineers with backgrounds in the various process industries. T h e laboratory instrument section is divided into five groups: infrared spectrophotometry, ultraviolet and visible spectrophotometry, chromatography, electrochemistry, a n d medicine a n d biochemistry. During the past year, members of this section's staff gave 23 technical papers on original work a t major scientific meetings, published eight papers and one book, a n d participated in three university short courses in instrumentation. The process instrument application section is divided into groups corresponding to t h e company's line of process instruments. These are process gas chromatography, nondispersive infrared analyzers, oxygen gas analyzers, a n d electrochemical instruments, a n d sample handling. Each group is headed b y a supervisor, and, in addition t o working on direct customer problems, carries out research and development p r o b lems in areas of specific interest (e.g., sampling problems in t h e metals and ceramic industries, direct control of fractionation with gas chromatography, analog computer control systems for unit operations based on analysis instrumentation, development of applications in t h e food industry, etc.). The department also provides evaluation information on new Beckman products a n d on competitive products. Staff members are active in professional societies a n d travel to all major meetings each year t o present papers on recently developed instrumental applications. Beckman cites many examples to illustrate t h e point t h a t return on

well applied process instruments can be substantial. An American ethylene producer, for example, paid for a $15,000 gas chromatograph instrument system in two days. A similar application in West G e r m a n y paid for itself in eight days. I t is significant to note here, t h a t t h e cost of application engineering w a s $1,150. G a s chrom a t o g r a p h y instrumentation application engineered into critical streams in several synthetic a m monia plants h a s resulted in monthly savings of $5,000. A gas chromatograph in an alkylation operation showed a savings of a p proximately $7,000 per month b y increasing t h e capacity of t h e alkylation unit through product quality improvement. I n another case a polymerization process was instrumented to give a continuous material balance b y means of several analysis instruments. Although savings here cannot be calculated, operating history for one year shows a n e t throughput improvement of more t h a n 2%, with a 5 % increase in yield.

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Beckman's Scientific a n d Process Instruments Division also includes a Custom Products D e p a r t m e n t which modifies s t a n d a r d instruments for individual customers. These modifications m a y include changes both in configuration a n d specifications to meet requirements of a new or extremely complex analytical procedure. Application Engineering a t Perkin-Elmer Corp. The Applications Engineering Section is a group within t h e M a r k e t i n g D e p a r t m e n t of t h e company. I t is made u p of sub-groups of individuals including chemists and engineers of all educational levels, delineated b y a product line such as ultraviolet spectroscopy, infrared spectroscopy, gas chromatography, or process analysis. I t s functions are those which are unified by one characteristic—the Applications Engineer represents the customer viewpoint within the corporation and Perkin-Elmer's technology to the customer. Proceeding from this premise, t h e following functions are logically a s signed t o the Section :

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applicability of this instrument to actual customer situations and problems. The Applications Engineer is expected to understand the potential user's problems from such low levels as, " D o e s the labelling on the knob really tell the customer what it does and does this labelling agree with the information given in the instruction m a n u a l ? , " to such high level judgments as, " I s the resolving power of the device ade-

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quate for the present range of customer needs?" Areas such as aesthetics, suitability of installation and operating instruction, convenience of handling, and other areas not primarily of engineering concern, are t a k e n u p here. Results of this evaluation will be used in recommending continued engineering effort on the devices tested. Specification of Instrumentation. J u s t as instruments produced must be tested to determine their suitability for a customer's needs, needs of the customer for instrumentation not yet produced must be t r a n s ferred from the field to the Development Engineering D e p a r t m e n t . The Applications Engineer stands midway between the field requirements of field use and hardware engineering and it, therefore, falls within the scope of the Section's responsibilities to specify, after suitable field consultations, new instruments and accessories to meet customer requirements. Therefore, prior to the adoption of any new engineering program, a formal specification list is drawn up by the Applications Engineers which, though stated in engineering terms, will be w h a t the customer needs with respect to performance and price. Source of Technical Information. T h e Applications Engineering Section serves as the prime source of technical information for the M a r keting D e p a r t m e n t . As a result of evaluation programs or other a p plications efforts, d a t a are generated which describe the characteristics of both P - E and other equipment and the uses to which they m a y be put. T h e Applications E n gineer will write or aid in the writing of this information in a form suitable for use in reports, brochures, d a t a sheets, bibliographies, and other material. Performance specifications of a new instrument will be shown in terms of spectra or chromatograms and interpreted to show the prime features of the devices in a manner which is meaningful to a customer. A high resolution chromatographic column, for example, m a y be specified as having 40,000 theoretical plates; however, the applications m a n might choose to illustrate this not in such bare and unintelligible terms, but possibly in the application of séparât-

ing two well-known isomers. This illustration may be far more effec­ tive than the word specification in illustrating performance. Applications Engineers are also responsible for orienting Direct Sales personnel in understanding of the company's instruments, their capabilities, and their prime fea­ tures in an absolute sense and, in comparison with competitive prod­ ucts. Technical Representatives. The Applications Engineering Section also represents that group which is best identified by the customer as being representative of the techni­ cal face of the corporation. Appli­ cations Engineers are uniquely qualified to present information on the company's instruments and their use, which is of interest to the technical field. Therefore, a great deal of activity is devoted to field trips and the presentation of techni­ cal papers, participation' as instruc­ tors in college courses on instrumen­ tation, participation in ACS, ISA, and other sponsored lecture tours. The technical public relations func­ tion is also carried through on an individual basis in that customers, or potential customers, who wish to ask about the possible application of P-E instruments to an antici­ pated problem or even problems re­ lated to the manipulation of P - E equipment, will generally come in contact with Applications Engi­ neers as the men who best under­ stand this kind of situation, and who can exploit all of PerkinElmer's resources, Engineering, Special Instrumentation, Manufac­ turing, Training, Demonstration, and Service, in a team effort appro­ priate to each individual problem. Consultants. The Applications Engineering personnel also serve as consultants to other groups within the corporation as well as to the Direct Sales force and their cus­ tomers where specific technical backup is required. New Applications. This group is also responsible for development of new applications. I t is responsible for recognizing potential new gen­ eral areas for application of existing instruments to promote the exten­ sion of product applicability. In the laboratory instrument lines,

those problems are selected which are new and which represent an area of widespread user interest, or are of unique analytical value. For example, the use of analytical in­ struments for insecticide residue analysis is an important new field because of the FDA regulations, and therefore a determined effort would be made to solve general residue problems. On the other hand, a unique problem in the anal­ ysis of space vehicle material or measurement of epitaxial transistor layer thickness, for example, might be of interest, not because of the widespread interest in this analysis, but because of the excellent value of the determination in furthering public goals or specific industrial or scientific requirements. In the process analysis and con­ trol area, Applications Engineeringis performed on a more specific basis. Individual analyzers are fre­ quently sold based on an analysis specification rather than a mere "hardware" specification. Applica­ tions recommends typical analysis systems based as much as possible on standard sampling, instrument, and readout hardware designed to satisfy the customer's analytical problem. Frequently, where neces­ sary, custom designs are undertaken by the Process Engineering Group. This same Engineering Group is also responsible for the fabrication and performance testing of all proc­ ess hardware and systems, both standard and special, with consul­ tation of the Applications Engineer. Thus, the most appropriate profes­ sional and technical abilities are brought to bear on the provision of a process analytical system for the particular case in hand. Both the Process Applications and the De­ velopment and Test Engineers must be oriented along process engineer­ ing lines since they are, in effect, consulting on and specifying part of the plant design for a customer. This area of New Applications is the largest portion of both process and laboratory applications work. At Perkin-Elmer, Applications Engineering does not routinely do actual final assembly and test of process instruments or systems, but rather concentrates on development of new applications. Both standard

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and custom instrumentation are designed, fabricated, and tested under the cognizance of experienced instrument development engineers in the Perkin-Elmer Engineering Department, allowing the full Applications Engineering effort to be applied to advancing the general status and knowledge of analytical instrumentation and to aiding the users of modern instrumental methods. Other Customer Services. Other user oriented activities at PerkinElmer also provide services to the customers. A Research Department staffed with physicists, physical chemists, chemists, and engineers studies advanced analytical methods and collaborates with certain outside analysts on experimental instrumentation in relatively new fields, e.g., atomic absorption spectroscopy and digital handling of spectroscopic data. A Special Instruments Engineering Group staffed with physicists and engineers designs, fabricates, and tests special modifications of standard laboratory instruments or complete special instrument systems to meet specifications for unique measurements as devoloped between the customer and P-E's Instrument Division's Special Engineering Sales Group. Such advanced instrumentation as the Model 301 double-beam very far infrared spectrophotometers, Model 205 infrared diffuse reflectometer and emissiviometers, and spectrophotofluorimeters, as well as special sampling cells, optics, and detector spectral response measurement equipment are typical of these groups' efforts. Another section, a highly equipped Demonstration Laboratory, offers customer training on the use and manintenance of all standard Perkin-Elmer instruments and accessories with the aid of PerkinElmer's Norwalk Technical Training and Service facilities. These training sessions are scheduled at specific monthly intervals and are offered at no cost to the customer. The Demonstration Laboratory also is available to the customer through his Sales Engineer when consultation or illustrative runs are desired to demonstrate utility of

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his

Application Engineering a t Consolidated Electrodynamics Corp.

The need for comprehensive application engineering services was first recognized by Consolidated Electrodynamics Corp. in 1948, when an Analytical Services group was established to evaluate the feasibility of CEC's analytical instrument product line for specific customer problems. This group was furnished with a laboratory and staffed by experienced laboratory chemists for the actual running of customers' samples in the determination of how compatible these instruments were to the problems. In 1951 the company realized the need for expanding this group from the standpoint of both function and coverage. In this year, the Technical Services group was established to provide adequate technical backup in studying and evaluating customer inquiries and the potential successful performance of the instruments in question. By this time, CEC's product line had been expanded to go beyond the straightforward laboratory type of analyzer and now included instruments suitable for continuous, automatic monitoring for process plant streams. This development was made possible through licensing arrangements with major operating companies to manufacture and market those stream analyzer types they had developed themselves to satisfy pressing control problems. These instruments included infrared, trace oxygen, refractometry, ultraviolet, and nephelometry, including a complete line of sample handling system components. In concept, the Technical Services, or Application Engineering group as it became known, was to fulfill a dual function. The first of these was creative in nature and included the investigation and proving of new applications for the existing product line. Further, another aspect of this creative viewpoint was the writing and dissemination of applicable and worthwhile technical information for the com-

pany's field engineers and for the technical journals. This technical information included the prepara­ tion of information bulletins, sales brochures, operating and mainte­ nance manuals and evaluation re­ ports, along with articles about new, successful applications based upon customer experiences. The second aspect of this work may be termed "bread-and-butter" work and included the evaluation of all customer inquiries from the standpoint of instrument feasibility. Also covered in this aspect was di­ rect correspondence with the field engineers and the customers con­ cerning specific problems and ques­ tions. This thoughtfully conceived basis of operation proved so successful that when the analytical instru­ ment line was accorded its own di­ visional status, a Technical Services group was included in the original plans and was so organized as to function in the way already de­ scribed. In the interim, Consoli­ dated expanded its market in both the laboratory and process stream analyzer field with the accompany­ ing need for an expanded group to provide the type of technical aid that had proved so successful in the past. Each instrument type, whether laboratory or process, is handled by one or more Application Engineers whose backgrounds, training, and experiences best qualify them for these endeavors. It was recognized very early that the best Application Engineer was one who also had the opportunity to actually work on the particular instruments in this area. Accord­ ingly, the Technical Services group has its own laboratories equipped with instruments in the product line. Here, with the help of instru­ ment technicians, each Application Engineer may physically run the study problem in question. A typical routine handling of a customer inquiry begins with the Application Engineer's desk-study of the problem. Similar previous applications are reviewed and all necessary requirements are outlined in the technical specification written by him to completely and compre­ hensively delineate the customer's problem and state the performance characteristics of the instrument in-

A HELPING HAND FOR THE ANALYTICAL CHEMIST

POLYETHYLENE GLOVES (ABOVE) Impervious to practically all cor­ rosive chemicals, lint-free, highly flexible. Inexpensive, expendable.

BORON CARBIDE MORTARS AND PESTLES (LEFT) One of the best materials for hand grinding — almost diamond-hard, inert, resistant to acids and alkalis. Cavity on one or both ends, diameters 1/2" to 3".

SPECIALISTS IN SPECTROSCOPY

s II 1 \\m m II 1 1

Pl*ai« write to us if you wish to receive our news­

INDUSTRIES,

INC.

letter THE SPEX SPEAKER. Scotch Pla ns, N . J .

Circle Νo. 9 on Readers' Service Card

Washing

Glassware's

Quick and Easy with

New, Automatic) Triple-Action

Roto-Rack by Space-saving, economical ROTORACK, with Automatic wash, rinse, HktilleH rinse and extra-high pressure , Owerful, efficient, fastaction washer for almost all glass­ ware. Yet it is built so compactly that it can be used on any laboratory counter top. Its uniquely-designed centerless m t a r v conveyor and s c i e n t i f i c a l l y 1 jet sprays assure that no glass surface can escape the strong and repeated a c t i o n of hot detergent spray, hot water rinse and final dis­ tilled water rinse. Simple and easy to operate, always reliable ROTO-RACK is the low-cost, high-production washer for your labo­ ratory glassware. We'll be happy to send you literature describing it fully. ROTO-RACK is also a v a i l a b l e w i t h f l o o r stand.

Laboratory Service Division

®

Metalwash

MACHINERY CORPORATION r

905 North Avenue / Elizabeth 4, New Jersey

Designer» a n d manufac­ turers of a l l t y p e i of l a b o r a t o r y glassware washers, animal cage ' washers, bottle washers, bottle fillers and dryers.

Circle No. 102 on Readers' Service Card VOL. 3 3 , N O . 1 0 , SEPTEMBER 1 9 6 1



37

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REPORT

DEPENDABLE ACCURACY Wavelength: 5A Photometric: 0.005 at 4A

CRITICAL REPEATABILITY Wavelength: 2A Photometric: 0.003

PRACTICAL WAVELENGTH

How much should you pay for a recording spectrophotometer? $3685, for pinpoint coverage of the visible range. $4285 for visible and UV.

RANGE 200m ; .-700m-.

CONSTANT NARROW BAND PASS Standard: 5A and 50A Special order: 2Aand 50A

You might pay a little less, but at the cost of recording speed, accuracy, repeatability, and range of application. You could pay more than twice as much, but you still wouldn't get such exclusive Spectronic 505® advantages as automatic wavelength speed control and the built-in mercury lamp for checking wavelength calibration.

LOW STRAY LIGHT

The Spectronic 505 provides high-speed, high-precision recording of transmittance, linear absorbance and emission—plus ac­ cessories for reflectance between 400-700 RAPID SCANNING ταμ. The only other instruments that can 6 different speeds, from approach its speed, accuracy and simplicity approximately 1 minute cost from two to four times more. That's to 10 minutes why the Spectronic 505 has become the ' 1 best-selling spectrophotom­ eter of all time. BAUSCH & LOMB INCORPORATED 0 . 1 % at 2 2 0 m ,

60921 Bausch Street, Rochester 2, New York • •

Please send m e Spectronic 505 Catalog D-2009. Send Booklet D-2019, "Fundamentals of Spec­ trophotometry."

BAUSCH & LOMB I

NAME, TITLE PROFESSIONAL ADDRESS | CITY .

Made in America, to the world's highest standards. ZONE

STATE .

I circle No. 54 on Readers' Service Card 38 A



ANALYTICAL CHEMISTRY

volved. In the course of such a study, the all-important sample stream handling components are en­ gineered and a detailed flow sheet sketch of the sample system is pre­ pared. This technical specification, to­ gether with all brochures, technical article reprints, installation recom­ mendations, and drawings, is for­ warded to the group involved in the detailed preparation of the quota­ tion. After the receipt of a pur­ chase order, the Application Engi­ neer again reviews the customer's final requirements and makes any changes in the technical specifica­ tion to reflect these. Each Application Engineer is the "fountain" of all knowledge con­ cerning his specific product line and, as such, performs the very im­ portant function of teaching train­ ing classes for both CEC's own field engineers and the customers' engi­ neers who are sent to the Pasadena plant for such training as is re­ quired. In addition, the Applica­ tion Engineer makes frequent trips both at home and abroad to bring the latest information to the local sales and service offices. With this opportunity, he makes scheduled visits with the field personnel to customer installations for the pur­ pose of discussing existing installa­ tions and determining customers' desires for future analytical instru­ ment needs. He also attends all major technical and professional so­ ciety meetings and exhibits where he may merely be in attendance to monitor the newest developments in his field, or he may actually pre­ sent papers, or staff the company's booth which provides him with an excellent opportunity to meet his public first hand. This type of operation, along with its earlier experiences with continu­ ous plant operation and problems, qualified CEC's application engi­ neers to develop and install the first commercially available chromato­ graphic closed-loop control system utilizing standard control compo­ nents of Taylor Instrument Com­ panies. The company is actively engaged in supplying its stream analyzers (chromatography, p.p.m. moisture detection, p.p.b. sulfur, mass spectrometers) for monitoring

REPORT a n d / o r control based upon single component concentrations, compo­ nent ratios, and computer control. I n summary, then, the Applica­ tion Engineering group performs the important function of being the technical back-up arm of the Ana­ lytical & Control Division's market­ ing endeavor. T h e worthwhileness in this function was recognized long ago a t C E C and continues to serve its two classes of clients; t h e com­ pany's own field engineers and those of their users.

Only $1750! Over $500 less than its closest competitor! But don't let its low cost fool you. In col­ leges all over the country it's a busy teaching tool, with over­ time use in faculty research projects. In industry, it's a basic tool of quality control and new product development.

ttausch & Lomb 1.5 METER STIGMATIC GRATING Spectrograph

A p p l i c a t i o n Engineering a t Philips Electronic Instruments ( N o r e l c o ) Philips Electronic Instruments manufactures standard laboratory equipment in t h e field of x-ray diffraction, x-ray fluorescence, in­ dustrial radiography, electron mi­ croscopy, electron probe micro-ana­ lyzers, automatic x-ray spec­ trometers (Autrometer) and "ons t r e a m " process analyzers. The function of Philips' Application Laboratory is: 1. To provide engineering appli­ cation support to its engineering instrument developments with t h e use and needs of the customer being paramount. 2. To study and evaluate cus­ tomer sampling problems as a direct support to Philips' marketing a c ­ tivities. 3. T o provide follow-up support to users on the application of a n y new materials or analytical prob­ lems with Philips instrumentation. 4. T o maintain a separate proc­ ess control laboratory staffed by personnel with industrial process experience and augmented with in­ strumentation a n d machinery to provide miniature feed conditions t h a t might be experienced in v a r i ­ ous industrial applications. Process instrumentation includes X-ray fluorescent analyzers or other sens­ ing devices to analyze tin coating, zinc coating, and aluminum coating of steel sheets, ores, and slurries t h a t are found in t h e metal beneficiating industries and liquids t h a t are experienced in the chemical and petro-chemical industries.

Bausch & Lomb DUALGRATING Spectrograph Here's the equiva­ lent of two spectro­ graphs in one! Now you can photograph two different spec­ tral regions . . . in just one ex­ posure . . . on a single 4" χ 10" plate or two 2" χ 10" plates. Highest dispersion and resolu­ tion, for critical edge-to-edge study. So efficient, it reduces hours of analysis to minutes!

How much spectrograph do you really need ? Depends on your work. The more critical, the more you need the high dispersion and resolution of the Dual-Grating. But in more routine use, the simplicity and low cost of the 1.5 Meter make it a popular choice. And there are widely overlapping areas of quality control, education and research in which only your future needs can determine which you should choose. In short, the answer depends on thorough knowledge of your analytical problems and objectives. We'll be glad to survey your requirements—in complete confidence—and recommend the right equipment for your present and future needs. Just call us in for con­ sultation at your conven­ ience. No obligation, of j B A U S C H 4 LOMB INCORPORATED course.

! 81021 Beusch Street, Rochester 2, Ν. Υ.

BAUSCH & LOMB Made in America, to the world's highest standards.

Π Please schedule a consultation at my con­ venience with no obligation to me. Π Please send Spectrograph Catalog D-277. NAME, T1TIE ... PROFESSIONAL ADDRESS

Philips believes t h a t such engiCircle No. 53 on Readers' Service Card VOL. 33, NO. 10, SEPTEMBER 1961



39 A

REPORT FOR ANALYTICAL CHEMISTS

of the manufacturer in determining the variables of a process system from a sample handling position; instrument mounting position; in­ strument housing condition; and useful instrument information out­ put. All these factors have to be evaluated in terms of their eco­ nomic justification to support the use of process instrumentation in an industrial manufacturing stream. Application laboratory support in

neering and customer applications support is necessary to train and in­ form technical people who use their standard laboratory equipment. They feel that this support is neces­ sary to maintain existing customer relationships and to support their growing marketing position in the laboratory field. Applications support in the proc­ ess control field requires a great deal more involvement on the part

the latter category of process con­ trol has proved to be much more of a requirement than previous sup­ port required for standard labora­ tory equipment. The sample handling problems associated with the above de­ scribed materials have been found to be much more pronounced in "onstream" analysis than in static laboratory analysis because human participation is being relieved from the loop. Therefore, it requires a joint participation on the part of the user and the instrument manu­ facturer to work out mutually satis­ factory automatic sample handling methods that will meet the instru­ mental requirements of the sensing device. Such application support as described above is found to be of basic economic necessity for the operation of a successful instrument company.

Application Engineering at Applied Research Laboratories

HIGHLY SELECTIVE FLORISIL? ADSORBENT FOR PRECISE CHROMATOGRAPHIC SEPARATION The hard, porous, white granules of FLORISIL synthetic adsorbent are uniform in size, highly sorptive and stable in either water or organic solvents. FLORISIL is a unique selective adsorbent used in both labora­ tory chromatographic analyses and production separations. For example, FLORISIL is used for chromatographic separations of vitamins, steroids, alkaloids, hormones, antibiotics and pesticide resi­ dues. It also removes color, acids and other contaminants from phar­ maceuticals. And, FLORISIL is useful as a catalyst in cracking partially oxidized hydrocarbons, in gas and gas liquid partition chromatog­ raphy, and for critical finishing of complex hydrocarbon compounds. FLORISIL'S characteristics may suggest further uses to you : Color: White

cr nDicn® Γ LUrtlOl L

Mg 0 Si Ο., Na so

15.5±0.5% 84.0 ±0.5% 5% avg> ( 1 0 % m a x )

* < °-

·

Specific Surface (B.E.T.) : 298mVgm Pore Volume (ml liq. N 2 /gm) : 0.461 Bulk Density: 0.634 p H : Aqueous slurry (1 part solids—Sparts water) =8.5

For free 14-page booklet, or free samples of FLORISIL, write to Floridin Com­ pany, Dept. X, P.O. Box 989, Tallahassee, Fla., or contact nearest sales office.

FLORIDIN COMPANY

Sales Offices: P.O. Box 989, Tallahas­ see, Florida · 375 Park Avenue, New York 22, New York · 8000 Bonhomme Avenue, St. Louis 5, Missouri · 292 Meadows Building, Dallas 6, Texas Circle No. 1 on Readers' Service Card 40 A



ANALYTICAL CHEMISTRY

Applied Research Laboratories, Inc., manufactures both optical emission and x-ray fluorescence in­ strumentation primarily for indus­ trial research and production con­ trol. A recent development is the electron microprobe x-ray analyzer which is used for basic research on extremely small areas. Since only a small percentage of equipment made by Applied Re­ search Laboratories may be cate­ gorized as mass production items, the majority of ARL's products are the result of application engi­ neering. ARL's highly specialized instru­ ments are made to order for each customer's particular analytical ap­ plication. ARL's principal instruments and their applications appear below : In the optical emission field are: production control Quantometers for direct-reading elemental analysis of metals, nonmetals, oils, ores, slags, and all uses where spectrochemical methods are applicable ; the Quantovac which is designed especially for production con­ trol in the iron and steel industry; and the Quantograph, a versatile unit, either spectrographs or direct-reading, which is finding increased applications in space age technology. In the x-ray fluorescence area are: the vacuum x-ray Quantometer and

detect and continually record... * vacuum production x-ray Quantometer, instruments for rapid x-ray analysis of all elements above atomic number 11, and the Quantrol, an "on-stream" con­ tinuous analysis instrument for tin plate and galvanize lines, ores, slurries, etc.

Application Engineering by F&M Application engineering by F & M Scientific Corp. consists largely of custom designing of laboratory in­ struments t o solve a specific anal­ ysis problem. The basic design a p ­ proach is similar to t h a t used in t h e process industry; t h a t is, the cus­ tomer's needs are determined and an instrument constructed specifi­ cally to meet these needs. In some cases, the custom unit becomes the prototype of a new instrument line. Examples of custom instrumenta­ tion and other forms of applica­ tion engineering a t F & M have in­ cluded: New custom instrumentation. A gas chromatograph was needed to analyze nitrogen, carbon monoxide, carbon di­ oxide, and oxygen in human respiratory gases. A standard chromatograph was not suitable since the sensitivity re­ quirement for carbon monoxide was in fractional parts per million and a dual column unit was necessary to achieve separation of all the compo­ nents. In this case, four different basic instrumentation approaches were de­ signed and evaluated before the most suitable one was developed to meet the customer's needs. Custom analytical procedures. A plant laboratory with no previous gas chromatographic experience asked for a complete and detailed analytical pro­ cedure for analyzing a specific plant stream. Although a standard instru­ ment was found to be suitable, the length and composition of the column had to be determined and an exact stepby-step procedure developed starting with handling the sample, operating the instrument, and calculating results. Evaluation of instrumentation. Often a reauest is received to specify one of F&M's standard chromatographs which is best suited to meet the cus­ tomer's needs. In same cases the choice is obvious. In other cases, samples have to be analyzed on two or more instruments to determine the optimum choice. Consultation. F&M scientists are often asked to visit industrial labora­ tories on a paid consultant basis to dis­ cuss specific procedures or instrumenta­ tion. In some cases, specific instru­ mentation is recommended which may be available commercially or which re­ quires custom work in their or F&M's laboratory.

HYDRAZINE

concentration down to 0.005 ppm with the

T E C H N I C O N ®

j/\^^^r\r*al Automatically analyzes or monitors hydrazine content of sample stream A field-proven system... over 2000 AutoAnalyzers are now auto­ mating routine wet-chemistry analyses in plants and laboratories throughout the free world . . . analyzing up to 60 repetitive samples per hour and monitoring on-stream continuously. Φ Detects other trace elements too, e.g.; calcium, potassium, sodium, cycloserine, phenol, sugar, etc. A total of 75 fullyautomated determinations now possible, more are coming. Send for your free abstract method kit and brochure AKf today

T E C H N I C O N CONTROLS, I N C . R E S E A R C H PARK • CHAUNCEY, Ν. Υ. Circle No. 174 on Readers' Service Card

—a new tool for the Chemist—

DRUMMOND "MICROCAPS" (Disposable micro-pipettes) These pipettes consist of short lengths o f precision capillary tubing calibrated to contain a definite volume from end to end. They are accurate to within less than 1 % and are so low in cost that you can afford to use them once and discard them. While they are of great value in general micro-chemical applications, they are especially useful in handling o f dangerous material. N o particular skill is needed in order to obtain accurate results. Operation: The pipette is inserted through the rubber cap on the end of the bulb assembly shown at the left. A hole in the end of the rub­ ber bulb permits filling by capillary attraction. When filled from end to end, the volume is correct—no more, no less. To discharge: hold finger over the hole in end of bulb and squeeze. To rinse, re­ peat the operation wilh the diluent. Microcaps are stocked in the following sizes: 1, 2, 3, 4 , 5, 10, 1 5, 2 0 , 30, 4 0 , 5 0 , 75 and 100 lambda. Other sizes can be made up on short notice. Prices: 1 to 5 0 lambda incl., per vial of 100 (with bulb assembly) $ 4 . 5 0 ; over 50 to 100 lambda, per 100, $5.50. PRECISION CAPILLARY TUBING. W e can also furnish capillary tubing to a tolerance of plus or minus .005 mm, of any diameter up to 1.5 mm O.D., in 12 or 2 4 " lengths. This tubing may be had in standard flint, lead, or boro-silicate glass. Write for further infor­ mation.

DRUMMOND SCIENTIFIC CO.

524-526 N. 61st St. Philadelphia 5 1 , Pa.

Circle No. 206 on Readers' Service Card V O L . 3 3 , N O . 10, SEPTEMBER 1 9 6 1



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