*
Operating a Petroleum-Research Analytical laboratory W. C. SCHAEFERMEYER and E. S. S M I T H Research and Process Department, Union Oil Co. of California,
Analytical expenses represent a substantial part of petroleum research costs; therefore, all analytical laboratory operations should be examined carefully. Frequently, laboratories which would not consider using inferior testing methods or equipment depend upon accounting and communication procedures that are not consistent with good office practice. Any system of handling samples, keeping records, and preparing reports depends upon the philosophy of the organization using it. This paper describes some of the procedures used by the research analytical group of the Union Oil Co. of California and the general policies that influenced their development. Sample handling from the time a client fills a sample bottle until the sample is returned or discarded is discussed and the advantages of printed forms and special equipment are described. The preparation and application of weekly and monthly reports for the aid of supervisory personnel in the conduct of laboratory operations are elucidatedI
T
HE criterion of the efficiency of an analytical laboratory to
those seeking its services is the accuracy of the result and the speed with which it is obtained; the measure used by the analyst is the degree to which his technical training is utilized: and in addition, research management is concerned with whether the services needed are supplied at reasonable cost. It is the function of analytical supervision to reconcile these somewhat divergent viewpoints and to provide services that as nearly as possible satisfy everyone. T o accomplish this, considerable information must be collected, correlated, and made available where and when needed, and all operational procedures in the laboratory must be well coordinated. The information needed by the one submitting the request, hereinafter designated as the client, is how to submit a sample and request sheet and how the answer will be returned. Analytical personnel need to know the accuracy required, approximate composition, contaminating substances, possible hazards, priority of work, whether or not the analysis is a specification test, and, in general, as much background as possible on the sample source and the use to which the data are to be applied. Supervisory personnel, from the lowest level in the analytical laboratory to the head of the department, must know how well the services are being provided, whether the laboratory is being operated efficiently, what the work is costing, and the present and anticipated work load. The basic information for these purposes is procured from specially designed work request forms and monthly work load estimates submitted by the client and from time sheets submitted by analytical personnel. The operational procedures that must be coordinated are the handling of work requests and samples, the recording of analytical data, the selection of the proper method for unusual samples, and the preparation of statistical reports. The handling of requests and samples is expedited by mechanical duplication of request forms and by the use of special tags and storage facilities. The recording of analytical data is simplified by printed work sheets. A centralized punched-card file system makes possible the rapid selection of the proper method. The preparation of statistical reports for supervision is aided by the use of punched cards and IBhl equipment. This paper is restricted to describing the operational techniques that the analytical group of the research and process department
&ea, Calif.
of the Union Oil Co. of California has found effective. The techniques described are the result of a study of the procedures of similar laboratories in the industry and several years’ experimentation in this laboratory. Several interesting papers on laboratory operations have appeared recently in the literature (1-5). The analytical group of 65 persons located a t the Brea Research Center is composed of three sections which are subdivided into eleven laboratory units. This group provides the complete line of testing required by petroleum research investigations and, in addition, furnishes consulting services and performs analytical research. During 1953 some 42.000 samples were processed, 29,000 by the chemical section and 13,000 by the other two sections. The number of tests performed on chemical section samples ranged from 1 to 35 and averaged about 2. The samples analyzed by the instrumental sections were counted as one test per sample per instrument regardless of the number of components reported. This analytical group has developed an organization that facilitates coordination of operations and distribution of supervisory responsibilities to the analytical chemists. This group is composed of a supervisor, a secretary, two clerks, 22 chemists, and 39 technicians. A11 of the chemists in the group have a t least a bachelor’s degree or its equivalent and many of the technicians have had college training in science. Reporting to the supervisor are three administrative section leaders and two coordinators. The coordinators assist in bringing the operations of the group together into a harmonious relationship: one to coordinate sample handling, records, and statistical reports: and one to develop and maintain a readily accessible up-to-date file of analytical methods. Reporting to the section leaders are unit leaders who are charged with direct supervision of laboratory work and personnel. The procedures used in any laboratory and the facilities provided will be influenced by the philosophy, policies, and rules of the organization of which it is a part. T o aid in understanding why some of the techniques described were adopted, the pertinent policie- that guide the analytical group are enumerated. 1. Research investigations must not lie delayed because of slowne-s in obtaining analvtical services. 2. Analytical work shall be centralized unlesp definite savings in analysis time dictates otherwiqe. 3. Analvtical time shall he charged to the project or drpartment making the request in order to obtain proper distribution of labor costs and thus to ensure arcurate d s t s on research e\penditures. 4. The analytical group places no restrictions on the ainorint of routine analytical service that may be requested bv the professional men a t the Brea Research Center. Control is maintained by the supervisors of the clients in accordance with their budgets. 5 . 411 regular samples should be completed within 5 worhing d a w , complaint samples within 3 working days, and rush samples within 1 dal-. 6. Requests for rush work are discouraged because granting prioritv to one client usually has an adverse effecton the services that may be rendered to others. Rush samples must be authorized hv a supervisor before acceptance for special service. The analvtical group keeps romplete records on the influx of priority work and watches its influence on the operation of the laboratory. If the situation begins to get out of control, the supervisors are warned that requests of this type must be curtailed if the value of priorities is to be preserved. 7 . Analytical research prohlems are asqigned to the analytical chemists in the group who have the best background for their solution. There is no section for analytical research. 8. Analysts (chemists and technicians) are assigned specific teqtq-for example, infrared absorption analyses or lamp sulfurs.
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Assignments are rotated periodically to maintain flexibility and minimize monotony. 9. All paper work and movement of samples is done by clerks, and all routine and semiroutine tests are oerformed bv technieians, if practical. 10. Time-saving equipment and spccial stationery are used to conserve manpower. COORDINATION O F OPERATIONS
Most requests for analytical work are received from the research and process department and are for the analysis of petroleum products by generally accepted procedures. To help ensure that this work is done rapidly and efficiently and to the satisfaction of clients, special tags and request forms are used. All tags and forms are described in detail in the section on expediting facilities. When submitting samples for analysis, a client must .attach appropriate identification and handling tags to all containers and fill out a work request form. Any reasonable system of numbering or identifying samples is acceptable. Twice daily a delivery man visits all laboratories a t the research center and brings work requests and samples to the analytical sample receiving office. Clients are encouraged to use this delivery service because the resemch center is spread over 22 acres; however, when samples require rush handling or discussion of a special analysis, they may be brought by the clients. The sample-receiving clerk checks a11 incoming requests to see that they are complete, correct, and legible, and that sample identifications on these requests agree with those on the sample tags. Forms which are incorrect are marked and returned t o
..
..
.
Figure 2.
Test card bin
sure that one copy of the request, in addition to the original, is availdde far each test desired. If more copies are needed, they are made on a Themo-Fax duplicator. A single test is cheeked on each copy and the copies with routine tests checked &replaced in pigeonholes by test type. Copies for nonrontine tests are sent to unit or section leaders for assignment; the original copy is given to the card olerk. Upon receiving a request from the sample clerk, the card clerk prepares a deck of cards for each sample listed on this request by selecting appropriate cards for each test from a bin containing prenotched and premarked cards for the most commonly used tests. This bin is shown in Figure 2. The clerk writes the sample number on each card and notches the deck with a groover, according to client, project number, and priority. The cards are placed in an active file by test, and each day that they remain in this tile, up to a total of 10 days, B notch is made in the service portion to indicate the time the sample has been in the laboratory. Analysts obtain requests from the pigeonholes. When ready to start work, they find their samples in the compartments indicated on the requests. After the portion of material needed for the specific test has been withdrawn, the analyst initials the lowest unmarked square on the compartment tag and returns the container to the shelf a t once, so that the sample will be available for other analysts. If the analyst initials the square circled by the sample clerk, he knows that his is the last test, and the color of the sample tag indicates whether the material should be discarded or placed on a separate shelf for return to the client hv the delivery service. Compartment tags from completed samples are returned to the sample clerk, who makes a new tag carrying the same number so that the compartment may be reassigned. Analysts record d l data, calculations, and results on printed work sheets, keeping a carbon copy if they wish. Unit leaders check work sheets daily for completeness of data and possible errors and send them to the card clerk who uses them to keep the punched cards up to date. They are finally filed cbronologically by test in the permanent analytical file. The analyst records results on his copv of the request farm, and, after approval by the unit leader, the copy is returned to the client by the delivery service. Results are reported as soon as they are available rather than being held until all tests requested by the client on a particular sample have been completed; also, because the request form is used as a report sheet, analysts do B minimum amount of writing and transcliption errors are avoided. A flow diagram showing the routing of work requests and samples is shown in Figure 3. All analysts keep time sheets on which they record the number of hours they spend working on various projects. I n addition to indicating the project numbers, they also classify each labor charge according to unit number and labor type its described in the parsgraph on time sheets. At the end of each pay period,
ANALYTICAL CHEMISTRY
1042
these time sheets are processed by the accounting department with IBM equipment. The tabulated information obtained is used for pityroll purposes, to distribute snalytieal labor charges to project accounts, and to prepare monthly operational reports for the analytical group. Requests requiring analytical research such as the evaluation and compxrisan of various methods, improvement of existing procedures, or the development of new techniques may originate anywhere wit.hin the company and, after approval by a responsible authority, are sent to the supervisor of the analytioel group. Special or unusual analyses are requested in a similar manner. To expedite and correlate handling, requests are sent to B oommittee camposcd of the three section leaders and the txiw coor%UPLLS
............
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"NCOUP- BEOININBOFMONI" LETLO END OF U O l r i " TESTS C*ANCE
Figure 5. Portion of monthly report on completed tests, labor, and work load
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vow.
mill0 CLERK
S " LETI -
. . t : . .
IINALITICaIL S"PER",SID*
........ %.MPLE DiSCARD
Figure 3.
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-
:
Routing of work requests, samples, and report*
dinators of the snalytical group. This committee, known as the Committee on Analytical Research and Development, has the following duties: 1. Consider the teohnical soundness of each vequest, decide upon t,he most likely approach to the problem, and assign i t t o the appropriate section within the group. 2. Consider the work load itnd deoide if the job can he completed d h i n n reasonable time with present personnel. If not, notify the client that he must discuss the mioritv of the work vith the analytical supervisor. 3. Kotify the cl ient of the estimated cost of the work, tht estimatcd completion date, and to whom the project was assigned. 4. Watch that work on the research projects does not lag and provide technical a d v i c e when needed 5. Compile a inon t hip. r e p o r t summaname t h e current st&s of each assigned project. ~
T h e committee does not attempt to evaluate the relative importance or justification of clients' requests for research and development work. The research request is reproduced
Figure 4. Active test card file
on the Thermo-Fax duplicator 80 that all membeia of t.lw Committee on Analytiesl Research and Development and i h r analytical chomist to whom the project is assigned may have :L complete description of the assignment. The project is not coilsidered completed until a report has been written, clemed through the committee, and sent to the supervisor fOT distribution 01' transmission to the client. Frequently requests are received from outside the dopartment for analytical services that do not involve research. They arc also processed by the Committee an Analytical Research and Development, itnd the completed work is reported by letter to the client. A weekly reminder is prepared for the supervisor and section leaders listing by title the assignments that. have not been completed. In addition to the progress reports listed, periodic atatistical reports are prepared to assist in the administration of the analytical group. DRTS
The
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is used for daiI3- control mid io Onlv
ureuitre reuorts on the work load of the annlvtical gmuu.
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V O L U M E 27, N O . 7, J U L Y 1 9 5 5 m e of analytical supervisory personnel in determining trends in ivork load, in anticipating personnel requirements and distribution. and in planning for new tests not ordinarily performed by tlic laboratory. Ior. Acid M1. t i t r .
Bled
%-
ccr. 81 Ne?. Acid
Unit
Figure 9. Analytical work sheet
V O L U M E 27, NO. 7. J U L Y 1 9 5 5
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Vacation, holiday, sick leave, and the time of the coordinators is not charged to laboratory units but to special accounting numbers. This information by type of labor and by laboratory unit within the analytical group has been most helpful in correlating time charges with work completed and may be readily understood by referring to the monthly operational report describe3 in the preceding section. Sample Receiving Office. The sample receiving office is near the center of the analytical building. Two walls of this room are formed by steel cabinets with sliding doors on each side. This arrangement permits the clerk to place samples in compartments from inside the room and the analyst to obtain them from the outside. Shelves in these cabinets are divided into coinpartments by egg easetype separators about 3 inches high, and the individual compartments are numbered an both sides. Adjacent to the storage cabinets are pigeonholes where work requests me filed by test for the analysts. The mom also contains a table for incoming samples, the Thermo-Fax duplicator, the test card bin, and necessary desks and filing cabinets.
1. Issuing information to clients on procedures for making use of analytical services and to analysts on preparation of time
and work sheets. 2. Liaison between clients and analysts on all matters pertaining to the handling, routing, and accounting of samples. 3. Continuous evaluation of methods for sample handling, record keeping, and preparation of statistical reports to ensure that improvements are made whenever possible. 4. Recording and transmitting requests for special analyses and analytical research to the Committee an Analytical Research and Development and providing a list of uncompleted projects for supervisory personnel. 5. Maintaining control on accuracy by obtaining data from analvsis of standard Sam les, cooperative testing, and periodic rerunning of regular sampP,s. 6. Calibration of equipment. Methods. The coordinator of methods is responsible for maintaining an active file of test methods, distributing methods and related general information, and ensuring that the proper format is used for procedures written by analytical group personnel. This includes the distribution of annlytieal methods throuehout
Figure 10.
Duplicator. A Thermo-Fax duplicator, procured from the Minnesota Mining and Manufacturing Co., is used to prepare facsimiles of work requests, so that each analyst assigned t o work on a sample will have a copy. The client supplies up to three copies; therefore, only about 10% of the requests require duplication. The duplicator (Figure l), using the original request as a master, produces a positive, dry copy in about 10 seconds on special infrared-sensitive paper. Room lights need not be subdued and no solutions are required; however, black ink or soft lead pencil must be used in preparing the request. Duplication of request sheets is considered worth while because i t permits several tests on the same sample to be run concurrently, i t provides the analyst with a complete, exact copy of the request, thus avoiding errors in transcription, and i t allows each analyst to use his copj’ to report each test result as soon as it is obtained.
other departments of the company and preparation of memoranda on revisions of these methods. Digests are prepared of all commonly used methods to inform clients of the scope, limitations, analysis time, required sample size, precision, and accuracy. The coordinator of methods also maintainins a file of punched literature reference cards prepared by chemists of the analytical group. All analytical chemists are held responsible for reading and carding literature pertaining to petroleum analysis and specific assignments are made for topics of special importance. All correspondence of the American Petroleum Institute and the American Society for Testing Materials, company reports, and other pertinent unpublished documents are sent to these individuals for carding information on analytical procedures. This reference file is particularly useful for determining what information, related to specified subjects, is in the central research file. The coding and punching system is capable of expanding in size and diversity with the file and greatly increases the accessibility
COORDINATORS
Sample Handling and Records. The coordinator of sample handling and record8 is responsible for preparing the reports discussed in this paper and for all operations of the sample receiving office and is also responsible for:
The techniques and equipment described have proved to be efficient and economical in handling the normal flow of work in
ANALYTICAL CHEMISTRY
1046 the analytical group of the research and process departmelit of the Union Oil Co. of California. Supervisory personnel and management are provided n i t h statistical reports that give a comprehensive survey of the operations of the group and also permit realistic predictions of future requirements for space, equipment, and personnel. The expense of centralizing all paper work and movement of samples is more than compensated by savings in analyst's and client's time. Furthermore, more effective utilization of the training and experience of the analysts is possible. These techniques should be effective in any anslytical laboratory of over 30 persons that is serving a research group. r o t all of the procrduies would necessarily be advantageous, because the basic policies of another laboratory might be sufficiently different to make some procedures inefficient or even unnecessary. These techniques were not all developed in this laborator) , in fact, they are a composite of ideas from many laboratories. This paper is presented with the hope that it will be provocative and stimulate greater interchange of ideas on the subject. S o claim is made that this is the best plan, even for this laboratory,
but it is hoped that it ail1 encourage readers to get i n contwt the authors and exchange ideas foi mutual benefit.
11
\\it
ACKNOWLEDGMENT
The authors wish to express their appreciation to G. R. 1,:ibc for his interest and guidance in the preparation of this paper and to the other members of the group for their helpful suggestion-. They are also thankful for the information and inspiration gained from contacts n i t h many other laboratories. Permission of thc Union Oil Co. of California to publish this paper is pxtrfullv acknowledged hi- the authors. LITERATURE CITED
(1) Chapman, It. P., Chem. Inds., 65, 718 (1949). (2) Chem. E?zQ.S e w s , 31, 1919 (1953). (3) Hale, A. H.. and Stillman, J. W., Axai.. CHEX, 23, 678 ( I 9.51 \ .
Ibid.,24, 143 (1952). ( 5 ) Post, B. G., Baker, 31.O., Hiett, T. A . , and Murphy. J. L., I b i d . , 26, 647 (1954). (4)
R E C E I V Efor D rei-iciv May 21i. 1951.
Acrepted Ortoher 2 2 . 1954
X-Ray Photoelectron Spectrometer with Electrostatic Deflection RALPH G. STEINHARDT, J R . ~ ,FREDERICK A. D. GRANADOS, and GLENN I. POW Lehigh University, Bethlehem, Pa.
This communication describes the design and operational characteristics of an improved x-ray photoelectron spectrometer intended for rapid, precise, and convenient chemical analysis of surfaces and subsurface regions of solids. Replacement of the magnetic analyzer by a radial, inverse first-power, electrostatic field analyzer has resulted in considerable improvement in performance. The resolution has been improved by a factor of 5, and the inherent intensity has been increased by a factor of about 20. Variable slit widths make it possible to vary the resolution by a factor of 8, leading to a considerable potentiality for versatiIity. Other refinements decrease the time of a routine determination from 2 to 4 hours to less than 10 minutes.
intensity because the exciting x-ray beam was weakened thimigli operation of the inverse-square law. These geometric consiticwtions also led to the adoption of an end-window countel,. t,hc dead-space characteristics of which ( 1 2 ) further reduced thr measured intensity of the electroh beam. Furthermore t h e height (and consequently the intensity) of the electron beani n x s severely limited by the small pole face separation.
T
HE initial work on the chemical applications of x-ray photo-
electron emission spectra (10, 11) was carried out using a homogeneous-field, 180' deflection, magnetic analyzer for electron dispersion. This type of inst,rument was chosen originalljbecause it appeared unwise t o build a complicated and expensive instrument with which to carry out exploratory work. However, as the need for better precision and greater rapidity grer7 with the analytical potentialities of the method, the limitations of the magnetic deflection instrument became more evident. Objections to the magnetic analyzer stemmed directly from the use of an iron electromagnet. The hysteresis associat'ed with operation a t low magnetic-flux intensities led to considerable difficulty in obtaining accurate electron energy measurements andnecessitated time-consuming operations to minimize its effects. T o avoid fringe effects of the field, it was necessary to extend the pole faces well beyond the limit of the spectrometer chamber and to keep their separation as small as possible. This meant that the x-ray tube had to be placed relat,ively far from the sample, leading to a considerable loss of potential photoelectron Present address, Department of Chemistry, Virginia Polytechnic Institute, Blacksburp, Va. 2 Present address, WePtinghouse Electric Corp., East Pittsbiirpli. Pa. 1
Figure 1.
Schematic diagram of spectrometer chamlwr
The ciiteria n hich \sere established for the characteristics ot new analvzer I\ ere the following: 1. The resolution
$ g 0.005 to 0 025.
I
should be convenientlv variable fiom
2 . The brst accuracy of energy evaluation should be of thrb same order of magnitude as the best resolution-i.e., 0.5%. 3. The inhrrent intensity should be sufficiently great t o nllow rapid determinations with good intensity precision.
