A look at the electronic analytical balance - Analytical Chemistry (ACS

A look at the electronic analytical balance. Randall M. Schoonover. Anal. Chem. , 1982, 54 (8), pp 973A–980A. DOI: 10.1021/ac00245a003. Publication ...
0 downloads 0 Views 6MB Size
Randall M. Schoonover National Bureau of Siandards Washington, D.C. 20234

ALookat the

Electronic Analytical Balance Today, if we were to wander around the nation's industrial facilities and laboratories, we would find electronic balances being used for everything from counting batches of resistors to adjusting the component ratio of epoxy mixtures. Many of these halances are suitable for the most demanding analytical work, while others are less precise hut serve many purposes well. In the following discussion the analytical balance is defined as an instrument with capacities ranging from 1g to a few kilograms and with a precision of at least one part in 105 of maximum capacity. Many modern electronic balances have a precision of one part in lo' a t full capacity, and the.accuracy is usually comparable. The inspiration for the modern analytical balance came from a weighing method change suggested by Borda (1 1. To overcome the difficulties of unequal arm lengths inherent with the two-pan, equal-arm balance, Borda suggested a method known as suhstitution weighing to be used in place of transposition weighing. In 1886 a balance was designed and built specifically for substitution weighing, although the modern one-pan substitution halance did not become commonplace until the 1950s.Although these halances are completely mechanical in operation, the optical readout system was usually assisted with a light bulb.

The Analytical Balance and the Mass Unit Before looking in detail a t the electronic balances, it is worthwhile to consider how mass is determined from a balance weighing and to briefly look a t the inner workings of a modern mechanical substitution balance. The reader should keep in mind that of the many forces the balance can respond to, we are only interested in the gravitational and buoyant forces and would like to exclude all others. First, we must recognize that the This micie not subject to US. Copyright

Published IS82 American Chemical Society

Optical System Lamp

FulcNm

Scale

Built-in

Weights

Counterweigh Beam Dashpot

Weigh Pan

I

I

Flgure 1. A modern one-pan mechanical analytical balance

balance reading is not the mass of the sample being weighed and therefore is not the desired result. The balance manufacturer has built the balance to indicate so-called apparent mass of the material being weighed. In essence, if the material being weighed has a density of 8.0 g/cm3 a t 20 "C and the air density is 0.0012 gIcm3, then and only then does the balance indicate the mass of the object being weighed. Obviously, these conditions are rarely met, and the balance reading must he corrected t o get the desired massJ2). The important point of the above discussion is that all analytical balances are calibrated by the manufacturers to indicate what is known as "apparent mass vs. 8.0 g/cm3." In some instances the balance may actually contain a single weight or a set of weights, or a weight may he supplied

separately by the balance manufacturer for calihration of the balance. It is from this inilial calihration and subsequent recalihrations that the user is lied to the mass unit, directly for standard conditions and tis computation for all other conditions. For many years another apparent mass wale hased on this principle had heen in use. The hasis of this scale was a brass weight whose density was specified tn be 8.3909 g/cm? at 20 "C with an air density of O.UO12 glcm?. This scale is generally referred to as the "apparent mass vs. hrass" scale.

Balance Princlples Today there are two dominant lypes of electronic balances in use the hybrid and the electromagnetic force balance. The hybrid balance uses a mix of merhanical and electronically generated forres, whereas the electro-

ANALYTICAL CHEMISTRY, VOL. 54, NO. 8. JULY 1982

973 A

Null

Detector /

Error ' f Signal

L I

--

/J

Servomotor

Correction Current

Figure 2. Simplified electromagnetic servo system

I

4

-

Null

Detector

k

Servomotor

I I

Flgure 3. The analytical hybrid balance magnetic force balance uses electronically generated forces entirely. A brief review of mechanical balance principles is worthwhile before the hybrid and electromagnetic force balances are discussed. In all cases, a null indicator is used to determine when the internal force balances the gravitational force on the sample. The Mechanical Balance. The modern mechanical balance is a onepan, two-knife balance with the apd i e d eravitational force on the Dan hear1;counterbalanced hy a fixed weight built into the balance beam.

Any residual inequality of forces causes an angular displacement of the beam. Equilibrium is reestablished hy adding or subtracting internal weights. Figure 1is a schematic of a typical one-pan mechanical balance. The halance readout is attained by summing the weight dial indications with a beam displacement indicator such as a projected optical scale. Whatever means are used to indicate the angular disdacement of the balance beam, the haiance is manufactured and calihrated LO indicate the same apparent mass

9 7 4 A * ANALYTICAL CHEMISTRY, VOL. 54, NO. 8. JULY 1982

scale as that of the built-in weights. The prominent features are the built-in weights (i.e., mass standards) and beam damping. However, of significance is the constant loading of the balance beam regardless of the sample weight on the pan. This feature provides a constant balance sensitivity; that is, the angular beam displacement in response to a small force change remains constant regardless of pan loading, a characteristic not found in equal-arm halances. The Hybrid. The hybrid balance is identical to the mechanical balance just described except the balance beam is never allowed to swing through large angular displacements when the applied loading changes. Instead the motion is very limited and when in equilibrium the beam is always restored to a predetermined reference position by a servo-controlled electromagnetic force applied to the beam. The Electromagnetic Force Balance. The more recent development of the electromagnetic force balance is a radical departure from the past in several ways. First, a magnetic force balances the entire load either by direct levitation or through a fixed-ratio lever system. Second, the loading on the electromechanical mechanism that constitutes the balance is not constant, hut varies directly with applied load. Finally, the sensitivity and response are no longer dominated by the dynamics of the balance beam but are largely controlled by the servo system characteristics. The Servo System Servo systems differ in classification and design, hut a simple explanation of how a balance servo works in principle is given here. The details of the circuitry are omitted since there are many different means to achieve the desired result. There are two distinct electronic approaches to the servo system. In one method a continuous current is driven through the servomotor coil and in the other method the current is pulsed. The latter technique has the advantage of simpler coupling to digital readout indicators, although both systems work well and, from the user's standpoint, there are many advantages available from the electronic nature of the cell regardless of its internal operation. In an electromagnetic servo system (Figure Z), the force associated with the sample being weighed is mechanically coupled to a servomotor that generates the opposing magnetic force. When the two forces are in equilibrium the error detector is a t the reference position and the average electric current in the servomotor coil is proportional to the resultant force

The CHROMATOPAC C-R2A is an advanced microcomputer data processorwith graphic printer. Its BASIC language program lets you expand and change your program freely, with simple key operation.

It has 2 channel processing and 2 channel recording capability. Above all, the C-R2A is not just a data processor. It's an invaluable host computer which lets you boost the capability of your Shimadzu computerized GC and LC.

Wfite today for more Informatlon on these and other Shlmadzu Instruments. SHIMADZU SCIENTIFIC INSTRUMENTS, INC. 9147-H Red Branch Rood. ColumQia.Md. 21C45. U S.A. Phone: (3011997-1227 Telex: 87959

SHIMADZU (EUROPA) GmbH

4 M a D U s J d d o l f l . J o ~ n nWeyerSrr. ~ 1.F.R.GBrmmy Phone: (W11)314081 TeIex:08586839

SHIMADZU CORPORATION INTERNATIONAL MARKETING DIV. Shinjuku-Mitrui Building. 1-1. NiShishiniuXu 2-chome. Sniniuru-hu. Tokyo 180, Japan. Ph0ne:Tohyo 03-248-5341 Telex:Dp2-3291 SHMDTJ.

CIRCLt 194 ON READER SERVICE CARD

Elecbom neiic ForceTeil

Weigh Pan

\

Flgure 4. The force balance cell in a classical enclosure

that is holding the mechanism a t the reference position. When the applied load changes, a slight motion occurs between the fixed and moving portions of the error-detector components, resulting in a very rapid change in current through the coil. The direction and magnitude of this current change are such as to restore the equilibrium condition. The reference or “null” position is usually not arbitrarily chosen, but is selected to allow the flexure pivots to remain in a relaxed state with the beam parallel to the gravitational horizon. A Closer Look ai Electronic Balances The Hybrid. When the mechanical balance is modified by the addition of servo control and other electronics, as shown in Figure 3, several beneficial things happen. Functionally, the most important change OCCUIB when the balance beam is servoed to a reference or null position. Doing this not only results in an electronic output hut also makes knife adjustments and edge quality less critical. Furthermore, other forms of pivots, such as flexural pivots, taut fibers, etc., which are more rugged and economical to manu976A

f

facture, can then be used in place of knife edges. Like the purely mechanical balance, the balance output from a hybrid halance is the summation of the built-in weights being used for a particular weighing and the restoring force required to hold the beam at the null position. In some balances the output reading indicates hotb of these in a single digital display, the necessary summing having taken place electronically. The most salient features that distinguish the electronic hybrid from the electromagnetic force cell balance are the still-recognizable balance beam and the built-in weights. Equilibrium is closely approximated by the selected built-in weights so that the forces generated by the servomotor are small. If industry trends continue, the hybrid balance will eventually disappear a t capacities much above 1g, hut will probably survive for some time to come a t the lower capacities. At these small capacities there is a t present a problem of balance precision surpassing the expressed uncertainty of the built-in weights and any external weight sets that may be required in the use of a balance. Normally the manufacturer will calibrate or adjust

ANALYTICAL CHEMISTRY, VOL. 54, NO. 8 . JULY 1982

these weights to a tolerance comparable to the balance precision. When this is not possible these weights are sometimes viewed merely as tare weights. The Force Balance. While the toploading electronic balance is a familiar sight in many situations, its principle of operation is least understood hy most operators. In recent years the force balance principle has also been incorporated into classical enclosures, like those used for the early mechanical balances, as shown in Figure 4. For this reason it is convenient to refer to the electromechanical heart of the balance as the electromagnetic force-halance cell, or simply, the cell. The logic behind having two distinct instrument configurations will become apparent later in the discussion. Like the hybrid balance, one of the cell’s outstanding features is the principle of servoing the mechanical mechanism to a null position. In either configuration the forces generated by the servo motor are much larger than those required for an equivalent-capacity hybrid balance. Of course, the balance beam, if any, no longer resembles its predecessor, and it is always tethered by a parallelogram loading constraint (guides). Unlike the mechanical and hybrid balances that have a counterweight and therefore a compensating buoyant force, the higher precision cells are more reflective of air density changes and may require frequent calibration. Looking first a t the top-loading configuration of the weighing cell (Figure 5), we see that the sample to be weighed is loaded on a weight pan and the loading guides prevent torsional forces, caused hy off-center loading, from perturbing the alignment of the balance mechanism. These same guides may serve to stahilize the moving portion of the servo motor, or as shown in Figure 5 , an additional restraint may perform this task. As previously described, an electromagnetic force is generated to oppose the net gravitational and buoyant force imposed by the mass being weighed. The balance readout is proportional to the amount of current passing through the coil when the equilibrium position is established. The constant of proportionality provides the conversion from current units to apparent mass units. Calibration is performed by the application of a calibrating weight and adjusting the circuitry to indicate the apparent mass of the calibrating weight. Higher precision can be ohtained if the weighing pan is placed below the cell rather than above it, as shown in Figure 4. This is due to better axial alignment a t the pan hook (minimum off-center loading) and a reduction in

Open this door to CAMECA'S exciting new world of microanalysis The CAMEBAX X-Ray Microanalyzer-featuring CAMECA'S exclusive Microbeam System-sets the standard for the industry with: VERSATILITY A Wide Range of Accessories REXIBIUTY Superior Software Architecture PROOUCTIVITY Rapid Analysis with High Sample Throughput 0 CONMNIENCE: Microprocessor Operations And Rapid System Status Assessment 0 SERVICE: A Fully-Trained Nationwide Organization for Complete After-Soles Support 0 0 0

Don't let the door to the future close on you! Write foday for a brochure fo: CAMECA INSTRUMENTS, INC. 2001 West Main Street Stamford, Connecticut 06902 or phone (203) 348-5252

A Subdiary of Thomvrn Corporation of America

CIRCLE 35 ON READER SERVICE CARD

11111111111111111111111111111111

EASY WEIGHS TO SOLVE PROBLEMS. Whatever your weighing problem, there's an Ohausa balance with a simple solution. You can find the one that's right for you by sending for our free catalogs. They'll help,you select from 144 Ohaus models. Everything from mechanical and electronic balances to a large selection of precision weights and masses. And the easiest way to get your free catalog is to send us the coupon.

Ohaus Scale Corporation 29 Hanover Road, Florham Park, NJ 07932 (201) 377-9000 Please send my free copy of the new Ohaus catalog I'm interested in n Mechanical balances n Electronic balances

Organization Address

0 1982 Ohaus Scale Corporation. Ohaus is a trademark of Ohaus Scale Corporation.

zip

CIRCLE 157 ON READER SERVICE CARD

Phone 07-82

Weigh Pan

\

I Servomotor Flexure

Fulcrum Load Cwpler Digital Readout

\

Null

1

Detector

\ Control Zero and Tare Ear Figure 5. Top-loading balance servomotor force with a corresponding drop in capacity. Both configurations of the cell require air-draft shielding for high levels of precision. The industry trend is toward the complete elimination of the hybrid balance a t the very highest levels of precision and toward increasing capacity. Benefits and ldiosyncrasles Because the modern analytical balance is electronic in nature it is very often found with a microprocessor as part of the package. The level of sophistication of these instruments may he very high, and there are many halance functions and idiosyncrasies that are unfamiliar to those who are acquainted only with mechanical balances. Let us examine the electronic capabilities that are inherent to the basic balance and those that may be optional. Benefits. I t is assumed that all halances have the digital display to indicate “weieht” and a means to Drovide a zero indication when no load is applied to the weigh pan. Beyond these basic features one is apt to find taring control, dual capacity and precision, selectable sampling period, etc. A brief summary of these features follows: Taring Control. A means to ignore the indication of a weighing constant, such as a weighing boat, by forcing a zero indication when the boat is placed on the balance pan. Most balances permit taring to 100%capacity. Dual Capacity and Precision. This feature allows the balance capacI

-

-

978A

*

ity to he decreased by a predetermined amount with a comparable gain in precision, i.e., a two-for-one balance. The choice of where to place the smaller, more precise range can vary from one balance to another. Selectable Sampling Period. The time required for a balance to obtain a reliable indication under ambient conditions may vary from one location to another; therefore provision is made so the user can vary the integration period by a simple circuit change. As the sampling period is lengthened the overall balance weighing cycle is likewise lengthened. Filters. Some manufacturers provide electronic filters that eliminate certain portions of the noise spectrum from the servo loop. Computer Compatibility. A means to access the balance by an external computer that may range from a simple data transfer such as a BCD output to complete functional control as offered by an RS-232C or IEEE-488 interface bus. Computation. A balance option that does computations such as counting, standard deviation calculations or user-programmable computations. Environmental Weighing Delay. Some balances have a circuit that protects the user from collecting poor data, due to unusually strong air currents or vibrations, by not displaying the weighing results during these periods. Some balances may have an override capability provided by the manufacturer for the acquisition of data during such periods.

ANALYTICAL CHEMISTRY, VOL. 54. NO. 8. JULY lPDo

Idiosyncrasies. Some idosyncrasies of the electronir balance follow. They may present a problem in some applirations: Weighing Ferromagnetic Marerial. Ferromagnetic materials may perturb the magnetic field associated with the servomotor, leading to systematic errors in the weighing. This can he cherked by moving the material in and around the pan area while looking fur large rhanges in the halance zero reading. An easy remedy is to weigh below the balance pan because magnetic forces fall off rapidly with distance. The above effects would be even more pronounred if one had to weigh magnetic materials. Electromagnetic Radiation. Electronic balances may malfunction in the presence of a strong electromagnetic field. This effect may be checked by keyinga hand-held radio transmitter near the balance and looking for a change in balance indication. Dust Susceptibility. Dust migration (from a dirty environment) into the gap between the pole pieces associated with the permanent magnet and moving coil of the servomotor can cause insidious changes in the balance precision and cnlibration. When these particles are ferromagnetir the halance may he rrndered inoperable. Such environments should be avoided. There may also exist a severe explosion potential in this type of environment, mandating the use of an entirely mechanical balance. Black Box Comparison In selecting a particular halance for a task, the following are the familiar specifications to consider along with what has been covered above in detail: capacity, accuracy (agreement with mass scale), precision (reproducibility of a measurement), zero stability, linearity, built-in weight tolerance or calibration accuracy, speed of response, pan size (top-loading balances), temperature coefficient, resolution (least significant figure in the display), and power requirements. Because all balance manufacturers do calibrate their products to the 8.0 apparent mass scale, any potential user can test these specifications with the appropriate 8.0 laboratory weights. One should keep in mind that the manufacturer has tested the product under the best laboratory conditions and if your laboratory is not as conducive to weighing this will be reflected in the test results. The analyst should keep in mind that the balance precision attained in the laboratory will usually dominate the measurement error. However, precision errors must he summed with linearity errors and weight calibration errors in determining the measure-

To Uncover

The Hidden Costs

Of Chromatography Do YOU rezdize how much lower-muitv HPLC salients might be costing you? Consider the frequent consequences.

4 The cost to repeat separation procedures because of solvent artifacts - this wastes analytical labor and valuable instrument time. 4 The cost to regenerate a water deactivated column - thlis causes instrument ”down-time” which requires additional chromatographs to perform the same amount of work. 4 The cost to wash off a residue-laden column - the residue decreases column efficiency. 4 The cost of replacing columns, filters and check valves clogged with particles this can increase cost from $200-800. 4 The cost of isolating residue from preparative peaks - this may cause additional intermediary separations to remove unwan ted cont am i in ants. 4 The cost of maintaining an additional inventory of several “grades” of purity (HPLC, GC, Spectra, etc.) - the quality of high purity solvents deteriorates while on a shelf. 4 The cost to frequently evaluate the less uniform solvents -. this diverts attention away from productilve analytical time. Avoid these “hidden costs” and timeconsuming effects from using lower purity solvents. Switch to B&J Brand High Purity Solvents. Because when it comes to cost and performance, there’s no comparison, B&J Brand is your best value. CIRCLE 27

ON

Sure, less pure solvents might be cheaper. But why jeopardize your chromatography results when you use them? In the long run, lower purity solvents can cost you more because of their inconsistent quality. Compare for yourself. If you’re currently using lower purity HPLC solvents, try the highest purity solvents - B&J Brand. You’ll notice the difference right away. Then do this. Figure out your cost-benefit equation for HPLC chromatography. The answer will be pure and simple. For lower costs and better results, it’s B&J Brand High Purity HPL-C Solvents. Write or call today for a free technical bulletin about B&J Brand High Purity HPLC Solvents. We’ll also send you our distributor listing so you can conveniently order B&J Brand Solvents from a distributor near you.

Avoid he hidden costs. Switch to B&J Brand High Purity Solvents.

-

BURDICK& JACKSON LABORATORIES, INC. 1

1953 South Harvey Street, Muskegon,Michigan U.S.A. 49442 (616) 726-3171

READER SERVICE CARD

ANALYTICAL CHEMISTRY, VOL. 54, NO. 8, JULY 1982

979A

ment uncertainty. Reiterating, if the material being weighed is not close to 8.0 glcm3, there is a buoyancy correction that, when omitted, can he a significant systematic error.

the American Chemical Society serves your information needs! FREE 1982CATALOG 200 pages o f t h e most upto-date information on More than 400 ACS W h s , including 75 new ones listed for the first time 22 magazines and journals. among them the S0ciel)b newjournal ORGANOMtXXLLLICS ACS cassette tapes, including the Science Symposia Series Microform editions for all ACS primaty publications The 1982ACS exhibit schedule

Completely indexed1

Easyto use.

..

more than 25 chemical sub+ categories1

The Future If the past can be used as a guide to the future we can expect improvements in balance structure that will allow for increasing applications. Thus, we can look forward to forcemeasuring transducers that require no moving parts or expensive mechanical adjustments and that are more rugged than present instruments. A few such balances are now beginning to make their appearance in the market. One recent new application is the immersed balance for the density determination of solid objects (3);others will certainly follow. Acknowledgment The author wishes to thank the many colleagues who gave their time and especially James Taylor for the artwork.

References (1) Miller, W. H.”On theConatruetionof the New Imperial Standard Pound; and “On the Commriaon of the lmoerial Standard Poind with the Kilo&mme des Archives,” Phrlosophical Transitions of the Royal Society ofLondon 1856,146,753-946.

(2) Schoonover,Randall M.;Jones, Frank E. “Air Buoyancy Correction in HiehAccuracy W i i hing on Analytical Fiai-

ance.” Anal. $hem. l981,53.900-902. Schoonover, R. M.;Davis. R. S. “Quick’ and Accurate Densitv Determination of

(3)

Laboratory Weights.“ In “Weighing

Technology,” 8th Conference of the IMEKO Technical Committee TC3, Krakow, Poland, Sept. 9-11.1980 (Polish Federation of Engineering Associations).

Request your FREE 1982 Books &JournalsCatalog today!Mail thecoupon beloworcalltollfree(800)424-6747. Need extra copies? Llst names and addresses on a s e p a r a t e s h e e t ofpaper and mail with thls coupon.

-----__-______________________

RUSH MEYOURFREECATALOGI

98OA

-

Randall Schoonouer has been a n employee of the National Bureau of Standards and associated with mass and density metrology for over 20 years. During this time he has nuthored or coauthored nearly 30 related scientific papers and has several inventions to his credit, including a unique high-precision load cell mass comparator and the immersed density balance. ANALYTICAL CHEMISTRY, VOC. 54. NO. 8. JULY 1982