V O L U M E 26, NO. 4, A P R I L 1 9 5 4 Table I.
Ultraviolet Absorption Maxima for Aureomycin pH 5.4
PH 1 Xa,
mp
231
267 320 368
645
ab 18,200 16,900 6,700
A, Inp
a
228
16,700 14,300
278
pH 1 2
pH 8.4 X, mp 239
277
a 16,200 14,800
8,100 368 7',700 380 15',900 a X = wave lengths of absorption maxima. b a = molar absorptivity.
A, nip
a
247 280
16,600 14,000
385
8,000
...
polarographic behavior if these characteristics are to be obtained for each electrical state of the substance. The electrodes and electrometer used for titrations impose a limitation on the range of dependable p H values. This range may be extended by resort to more accurate but less convenient potentiometer circuits and by use of alternative but likewise less convenient electrode syqtenis. The range of valid pH values is further extended by u-e of smaller sample volumes and higher concentrations of acid or alkali used as titrant. Excellent data
on dissociation beyond this valid p H range can occasionally be obtained by measuring change in ultraviolet or visible light absorption or change in some other physical property as the niolecule dissoriates. Many organic substances exhibit inadequate solubility in n-ater to permit satisfactory titration. I n such cases it may be necessary to titrate the sample in a water-organic solvent mixture. Alcohols, dioxane. and diniethylformamide have proved useful for this purpose. Since pRd values will vary with different solvents, the data jn Figure 7 cannot be used for correlation with structure. LITERATURE CITED
Cohn, E. J., and Edsall, .J. T., "Proteins, Peptides and .Imino Acids," p. 82, Sew Tork, Reinhold Publishing Corp., 1943. (2) Michaelis, L., and lIieutani, AI., 2. p h y s i b . Chem., 116, 185 (1925). (3) Mizutani. H., Ihid., 116, 350 (1925). (4) Simms, H. S., J . Phus. C'hem., 32, 1121 (1928). (1)
R E C E I V Efor D review July 10, 195.3.
Accepted October 9 , I053
Pharmaceutical Control laboratory Record System GEORGE M. NAIMARK and ROBERT F. PRINDLE Strong
Cobb & Co., Inc., Cleveland 4, Ohio
A rapid, efficient pharmaceutical control laboratory record system is described. The system is based on two forms: an analytical "work sheet" and a marginally punched permanent record card, both of which contain the complete product formulation and job-identifying information. The marginal punching permits the coding of analytical and production information which aids in the critical evaluation of production and of laboratory operation.
T
HE authors have developed a record-keeping system for a
pharmaceutical control laboratory Yhich has proved extremely efficient. It evolved from a desire to create a system which xould emphasize ease of recording of analytical control data and simplification of the study of such accumulated data. The system makes use of two forms: a "work sheet" which has the dual function of indicating to the analyst that a specific assay is to be done and serving as the report form after the analysis has been completed; and a marginally punched card which acts as the permanent record of all analytical control data. An industrial analytical laboratory record system also based on a marginally punched card has recently been described ( 2 ) .
of a pharmaceutical product i? initiated by the creation of a manufacturing card which indicates product constituents, concentrations, manufacturing instructions, warnings of dangerous materials, customer's specifications, and all requisite jobidentifying data, such as customer, type of product, and code and lot number. At the time the manufacturing card is made, a duplicate copy is Ditto reproduced on the unprinted side of the control laboratory punched card (Figure 2). Having this complete and accurate copy of each manufacturing card in the control laboratory minimizes routine reference to the master files for the verification of product specifications. In addition, having the complete formula of each product aids the ag-
PUNCHED RECORD CARD
A marginally punched 6 X 8 inch Keysort card manufactured by the McBee Co., Athens, Ohio, serves as the permanent record of analytical control data for each product manufactured by the company. The card, which is printed on one side to minimize clerical preparation time (Figure l ) , is made of card stock which permits duplication on the blank side with a Ditto duplicator. I n this company, production
Figure 1. Punched Card for Permanent Record of Analytical Control Data
646
ANALYTICAL CHEMISTRY product, and any additional informstion which will aid i n the critical evaluation and improvement of the company's production.
5,500
85.5
Unit.
.g.
Vi-
:I
A Stabllimd 550 n t l l i o n u n i t .
0 0
8550 g-
b c o & i o h i d USP Po Ffflrr
WORK SHEET
9.0.
12/32" die omi-doep
0 0 0 0
0
0 0 0
0 0
so0 tableto to f i t 1 1 2 e d r b l a h bottle.
OS.
0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
0 0 0 0 0 0 0 . 0 0
Figure 2. Duplicate of RIanufacturing Card Printed on Reverse Side of Punched Card and on Reverse Side of Work Sheet
gregation and analysis of production and control data. Il7heii a product comes to the control laboratory for analysis this copy of the manufacturing card also obviates the need for clerical entry of customer, code, lot number, and components, in the control laboratory records. This has not only reduced the time required for record keeping but has eliminated the mistakes inevitable in copying. Most of the information printed on the reverse side of the punched card (Figure 1) was formerly transcribed by hand for each job received by the control laboratory. Having the card custom-printed to specifications eliminated this nonconstructive copying of information which is unchanging and independent of the specific job. In addition, printing the names of the constituents most commonly assayed by the laboratory has d s o reduced record-keeping time. Space is provided on the printed portion of the card for the date of receipt of the sample, stage of production. assay data, analysts' initials, customer's label statement for each component, dates of laboratory release for further processing and, finally, data of laboratory release of the finished product. Sufficient space has also been provided for remarks on assay proredures, production problems, or previous experience with the particular product. A t times an additional card is added for more detailed comments on special assav techniques or key points in the handling of the product. Extra cards of this type have even been utilized for the reproduction of memoranda issued by the control laboratory which pertain to the lot. Subsequent reference to such cards helps quickly to clarify the previous history of the product. This punched card system has been found very flexible in this respect and ways of increasing its utility are continually discovered. The marginal punching is conventionally coded ( 1 )for all constituents assayed, manufacturing difficulties encountered, type of
The other form used in the control laboratory record system is a work sheet (Figure 3) which is supplied the analyst for each component to be assayed. The work sheet, which is the same size as the manufacturing and control laboratory punched cards, is made of a paper stock which takes Ditto duplication. A complete copy of the manufacturing card is reproduced on the unprinted side of the work sheet a t the same time the manufacturing and punched cards are Ditto printed. A sufficient number of work sheets are reproduced a t this time to provide one sheet for each component requiring assay a t eveiy stage of production. The printed side of the work sheet makes provision for indicating the stage of production of the sample, date of sample receipt, analyticdl data and remarks, analyst's initials, date of assay, disposition and date of disposition by supervisor, supervisor's initials, remarks by supervisor, and supervisor's instructions to the clerk for entry of assay results :ind comments on the punched card.
Analyticml Data
Initials
Figure 3.
b
Work Sheet for Control Laboratory Record
This form has eliminated the need for extensive clerical preparation of the work sheets before delivery to the analysts. Mistakes made in the recopying of job-identifying information and potencies of components no longer can occur. An appreciable saving of time formerly spent by analysts in verifying data previously copied by the clerk on each work sheet has resulted. The presence of the complete formula on each work sheet also simplifies analytical work by indicating to the analyst the presence of components capable of causing assay interference.
V O L U M E 2 6 , NO. 4, A P R I L 1 9 5 4
641
ROUTINE OPERATION
Upon receipt of the sample to be assayed in the control laboratory record office, the clerk removes from the file the punched card and work sheets which had been previously Ditto printed a t the time the manufacturing card was made. Since the lot number, job-identifying information, and complete manufacturing formula are already on the punched card, the only additional data requiring entry on the punched card are the label statements of the constituents to be assayed and the date of receipt of sample. The stage of production involved is merely circled on the punched card. The work sheets also contain the job-identifying data and formula and only require encirclement of the stage of production and entry of date. The component to be assayed is circled on the formula side of the work sheet. One work sheet is prepared for each constituent requiring analysis, and the sheets and sample are delivered to the analysts. The punched card is then numerically filed in the clerk’s “in process” file. Upon completion of the assay the analyst enters the analytical data, results, analytical notes, initials, and date on the work sheet
and in the permanent laboratory notebook, and returns the work sheet to the supervisor. The supervisor indicates disposition of the assay, his initials and date, and, if complete, returns the work sheet to the clerk. The assay results, analyst’s initials and pertinent comments are then entered on the punched card by the clerk. When all of the assay work is completed the job is released for further processing or shipment, and the date of release entered on the punched card. When the laboratory’s analytical work on a particular job is completely finished the punched card is filed serially by lot number in a standard metal file. The work sheets are retained for a short while before being discarded. LITERATURE CITED
(1) Casey, R. S., and Perry, J. W., “Punched Cards,” Yew York, Reinhold Pulilishing Corp., 1951. (2) Hale, -4. H., and Stillman, J. W., ANAL.CHEM.,24, 143 (1952).
RECBIVED for review J u l y 13, 1953. Accepted November 18, 1953.
Visual Control of Analytical Test Scheduling B. G. POST, M. 0. BAKER,T. A. HIETT, and J. Research Laboratory, Houston Refinery,
L. MURPHY
Shell Oil Co.,
Houston,
A visual system has been developed for use in the scheduling of routine analytical tests and for maintaining a daily status report of each sample in process. This system is based upon an application of a Produc-Trol visual order control board. By means of a series of colored plastic pegs which may be placed on the board, i t is possible to visualize the number and type of tests that have been submitted for analysis. Through the use of a color code it is possible to distinguish priority samples, samples which require special techniques or modification of an existing standard procedure, and samples on which the testing is complete but the results have not been reported. combination of a number code with the color code enables the scheduling supervisor to control the relative order in which the requested analyses on a given sample are to be made. Thus, the supervisor has a complete “picture” of the entire work load requested of his section available at all times for planning and assignment of personnel to the various required tasks. The two outstanding advantages of this scheduling system are its presentation in visual form of a summary of the entire work load of the test section and elimination of the necessity of written test assignments to the testers.
I
N RECENT years the scope of analytical chemistry in petroleum refinery laboratories has greatly increased both in variety of analytical functions performed and in the number of analyses required. These increasing demands upon the analytical groups have resulted in a proportionately larger number of routine-type analyses which require detailed technical supervision. Consequently, this trend has increased the amount of time that must be spent in nontechnical work such as sample scheduling, storing, and test reporting. Such housekeeping overhead, while a very necessary function, results in routine, nonskilled use of trained analytical chemists. Further, the inability to visualize readily the exact number and type of tests requested, their relative priorities, and any deviations from speci-
rex.
fied routine analytical procedures have made the problem of test status and scheduling a complex one. Continued studies of these problems during the past three years have been made in an effort to develop a more economical and more efficient procedure for the scheduling of routine analyBes. A review of the chemical literature since 1907 reveals that only three papers discuss this important phase of laboratory operation (a, 4, 5 ) , although a few references to analytical laboratory organization and methods of operation may be found (1, 3). A punch card system similar to that described by Hale and Stillman (4, 5) was developed several years ago, but has been replaced by the system described herein. REQUIREMENTS O F A CONTROL SYSTEM
Economical utilization of the available manpower and facilities of an organization must be based upon a well-planned program. This plan may be a long-range detailed plan of action or it may be a daily program whose details will be filled in as their need arises. Depending upon the scope of the laboratory program and the degree of supervision desired, the supervisor may be required to maintain a daily status report of each sample in process. The maintenance of a daily status report for each sample requires: 1. A means of showing each sample for which an analysis is requested. 2. A method of indicating the exact tests required for each sample. 3. A procedure which indicates priority tests, tests requiring special instructions, and testa that must be run in a predetermined order. 4. A method which indicates when a given test has been satisfactorily completed.
In addition to these basic requirements, the control system selected should: 1. Be simple in operation, easy to maintain and available to all interested personnel during normal working hours. 2. Automatically indicate to each individual his daily work assignment.
