5
JOURNAL OF RESE ARCH ot the National Bur eau of Standards- C. Engine er ing and Instr umenta tion Vol. 64C, N o. 4, Odobe r- D ecember 1960 Automatic Precise Recording of Temperature Gaylon S. Ross and Herbert D. Dixon (April 15, 1960) An apparatu s is described which automat i ca ll y and co nti nuou sly record s s mall tempera- t ur e changes. The principal componen ts are a pl at inum resistance thermom et er , a modified G- 2 Mue ll er vVheatston e bridge, it direct c urr ent amp lifi er, and a potentio me tric , strip-ch art recorder. Frequen t zero checking is unnece ss ary because the syste m is extre mely sta bl e. In systems where the genera l dependence of tempemture on ti me is known, a near ly uniform cha nge of 0.00001 °C per minut e is easily discernible over a rerio? of minutes or more. However, the meas ur ement of tempe rature at any giv en lIls tant IS IInllted by a n inherent; electro nic noise band of 0.00004 ° C. A simil ar ar range ment , using a t hermocouple pair a nd a pot e ntiom e ter instead of the pl ittinum ther mometer and the vVheat s tone bridge, is also described. 1. Introduction Th e results of man y l aboratory operation s arc mor e val u able if there is a co ntinuou s and highly pr ecise record of temperature. One of the mo st pre- cise temperature m easuring systems in general l ab- oratory usc consists of a platinum resistan ce ther- mometer, a · Wh eatst on e brid ge, a sensitive suspension galvanometer, alld a competent operator. T emp erat ure differences of 0.0002 °e can b e d etecte d, but the manual op erations arc te dious, boring, and e}" -p en sive. A system for automatically recording temperature is desirable, provided it can be achieved without a sacrifice in accuracy or pr ecision . Armstrong and co work ers [1]1 describe the usc of a dir ect C UlTent amplifier and recorder to balan ce a Muell er resis tan ce brid ge . The y recorded tempera- ture with a precision of 0.0001 °e, while maintainin g a response time of approximately 5 sec. The auto - mati c temperature recording sys tem described in this pap er wa s designed specifically for use in ob- servi ng time -temperature cooling curves of very nearl y pur e sub st ances [2]. In this sytem tempera - ture is recorded with a precision of 0.00002 °e, but the res pon se time is approximate ly 40 sec. In ord er to maintain su ch a high precision , the most essenti al requirement is long-term bridge stability, sin ce fre- qu ent bridge zeros cannot be taken. The a ppa ratus a pp ears to be generally useful in experim enta l systems wherein the maximum temper- at ur e range to be recorded is less than 1 deg an d the gr eatest r ate of temperat ur e ch ange is 0.002 °e per minute while recording at maximum sensi tivity. Th e allowable temperature s pan ftnd the rate may be in creased with a correspondin g decrease in sensi tivity. 2. Equipment and Techniques In this automatic system the gal vanometer i re pla ced by a high- gain amplifier. Th e operator is rep laced by mechanical co ntrol s and a strip- ch art, recording-po ten ti om e ter . In general practice, the bridge dials are set fo r a particular experim ent, a nd this setting is no t changed excep t to make a sensiti vi ty check at the end of the experimen t. Th e off-balance curr en t fr om the brid ge is feel into an amplifier. Th e amplified signal is atten uat ed, filtered, a nd reco rd cd . A block di agram of the system is shown in fi g ur e 1. Th e specifi c components and th e modificaLions and adap tations of these, as used in this au tomatic recording system, are describ ed in the following sections. Z ERO TI Irl ING SW ITCH FIGURE 1 TYPE G-l BRIDGE FI GURE 1 d- c BREAm AMPLI FIER NOFICU RE A TH NUA TOR FILTERS BIA$ Io1 ECHANISM FIGURE 5 PO TENTIOMETRIC RE COROER NO FIGURE FIG U RE 1. Block diagram oI the automatic temp erature Te- l Fi g ur es ill brackets incli cate the litera tur e references at th e end of this paper. cording system. 271

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JOURNAL OF RESEARCH ot the National Bureau of Standards- C. Engineering and Instrumenta tion Vol. 64C, No. 4, Odober-December 1960

Automatic Precise Recording of Temperature Gaylon S. Ross and Herbert D. Dixon

(April 15, 1960)

An apparatus is described which a uto matically and con tinuously records small tempera­t ure changes. The principal co mponents are a platinum resistance t hermometer, a modified G- 2 Muell er vVheatstone bridge, it direct current amplifi er , and a potentiometric, strip-chart recorder. Frequen t zero checking is unnecessary because t h e system is extremely stable. In systems where t he general depe ndence of tempemture on ti me is known, a nearly uniform cha nge of 0.00001 °C per minute is easily discernib le over a re~ordil~g r erio? of ~O minutes or mo re. However, the measurement of t emp erature at any given lIlstant I S IInll ted by a n inherent; electro nic noise band of 0.00004 ° C. A similar a rrangement, using a t hermocouple pair a nd a potentiometer in stead of t he plittinum t hermometer and t he vVheatstone bridge, is also described .

1. Introduction

The results of many laboratory operations arc more valuable if there is a continuous and highly precise record of temperature. One of the most pre­cise temperature measurin g systems in general lab­oratory usc consists of a platinum resistan ce ther­mometer, a ~!(ueller ·Wheatstone bridge, a sensitive suspension galvanometer, alld a competen t operator. T emperature differences of 0.0002 °e can b e detected , but the manual operations ar c tedious, boring, and e}"-pensive. A system for automatically r ecording temperature is desirable, provided i t can be ach ieved without a sacrifice in accuracy or precision .

Armstrong and coworkers [1]1 describe the usc of a direct CUlTent amplifier and recorder to balance a Mueller resistance bridge . They recorded tempera­ture with a precision of 0.0001 °e, while maintainin g a response time of approximately 5 sec. The auto­matic temperature recording system described in this paper was designed specifically for use in ob­serving time-temperature cooling curves of very nearly pure substances [2]. In this sytem tempera­ture is recorded with a precision of 0.00002 °e, but the response time is approximately 40 sec. In order to maintain su ch a high precision , the most essential requirement is long-term bridge stability, sin ce fre­quent bridge zeros cannot be taken.

The apparatus appears to be generally useful in experimental systems wherein th e maximum temper­ature range to be recorded is less than 1 deg and the greatest r ate of temperature change is 0.002 °e per minute while recording at maximum sensi tivi ty.

The allowable temperature span ftnd the rate may be increased with a corresponding decrease in sensi tivity.

2. Equipment and Techniques

In this automatic system the galvanometer i replaced by a high-gain amplifier. The operator is replaced by mechanical controls and a strip-chart, r ecording-po ten ti om e ter .

In gen eral practice, the bridge dials are set for a particular experim ent, and this setting is no t ch a nged excep t to make a sensitivity check at the end of the experimen t. The off-balance curren t from the bridge is feel into a n amplifier. The amplified sign al is attenuated, filtered, and r ecord cd . A block di agram of the system is shown in figure 1.

The specific components and the modificaLions and adap tations of these, as used in this au tomatic recording system, ar e described in the following sections.

ZERO TI Irl ING SWITCH

FIGURE 1

TYPE G-l ~UEl l ER

BRIDGE FI GURE 1

d- c BREAm

AMPLI FIER NOFICURE

ATH NUATOR FILTERS

BIA$ Io1 ECHANIS M FIGURE 5

POTE NTIO METRIC RECOROER NO FIGURE

FIG U RE 1. Block diagram oI the automatic temperature Te-l Figures ill brackets inclicate the literature references at the end of this paper. cording system.

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2.1 . Wheatstone Bridge

Leeds~and1Northrup , Type G- 2, Mueller Bridge. Mea suring Arm-O to _11 1. 11 10 Ohms G raduated in Steps of 0. 000 1 Ohms [3]

The following lTlOdifications were niitde to the bridge in order to eliminate electricitl and thermitl disturbances:

The galvanometer switches and damping resistance, not essen ti itl in this work, were cliscon­nected . The binding posts used for connecting the bridge to the amplifier and a swi tch for taking the bridge-zero au tomatically were installed . These changes are shown in figure 2, IV hich was taken in part from the manufac turer 's catalog [3], which con­tains a detailed description of the drawing .

MERCURY

fl:l L::r

S2 MOTOR· DRiVEN TIMING SWITCH

TRIPLE POLE DOUBLE THROW COMMUTATOR

F lO n u: 2. G- 21IIuelleT Wheatstone bl'idge with modifications [3].

'rhe portion of t he bridge II' hich was disco nnected is enclosed by dashed li nes.

2. The thermostated n,luminum case, \\'hich con­t ains the principal bridge resistors, was connected directly , to ear th ground. This earth ground was ob tained by means of a heavy copper wire connected to an iron stake driven firmly in to the ground. (This connection was used wher e earth grounds ar e indi­cated ; all other grounds were the usual waterpipe connections.) The true ear th ground was necessary to avoid the introduction of ground currents into the amplifier .

3. Therm al emf's generated a t junction poin ts were stabilized by insula tion . The emp ty space, in the wooden case which encloses the bridge, was filled wi th glass wool [w d the bridge was surround ed by a 3-in. layer of expanded polys tyr ene. This elimin ated convection currents in side the case. These convec­tion curren ts produced negligible changes in bridge resistances, but large changes in the existing thermal

emf's . Possible accumulation of electrostatic charge was a voided by incorpomting a network of fin e copper wire within the glass wool. This network was grounded to a copper grid placed in the bo ttom of the bridge case . The grid was in turn ear th grounded . The insulated bridge was placed inside a %6 in . thick aluminum box. An addi tion al 3-in . layer of polystyrene was used to cover the outside of this box. The aluminum box was connected to ear th ground .

4 . Bakelite extensions wer e attached to the bridge controls to allow changes in the set tin g of the bridge dials through the in sulation . A diagram of one of these extensions is shown in figure 3.

FI G VRE 3. B1'idge control extension.

5. Sixty cycle alternatin g currcn t interferen cc, generated by the heater current , was eliminated during recordin g operation s by using a 6-v lead storage battery to supply t he hea ter power . vVhen the bridge is no t in use, the heatin g system for the thermostated resistors is main tained by the alter­nating curren t power supply (fig. 4).

HEATER

I I

~~r 1 ~: ~: ~---1

i

6 vd-c ~ 15

IL-____ __. ' ___ • __ _

FIGURE 4. Modified bridge-healer circui ll·Y.

272

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6. Induction peal:s caused by ch anging h eater currents were minimized b~r u sing tIle modified circuitry ShO I\TIl in figure 4 . The salient fe a ture of this modification is the h eater-relay bypass which supplies abou t 85 pereen t of the current ne cessary to keep th e thermostated bridge resistors at a constant temperature. Th e relay , 011 closin g, supplies th e additional 15 percen t through th e shun ted circuit . Since switching of tI le relay does not ch an ge t}1O heater current drasticall.IT , " overshoot" in the h ea tin g cycle is redu ced. Tile Lwo principal r esistall ce decades in the G- 2 bridge arc mounted ill an alu­minum block. Thi s block is separated from the electri cally heated box b~T balsa wood insulation. Thi s serves as a low-pass filter capable of damping out cyclic heatill g-coolin g cffccts if tI le c~' cle is less than 5 mi n. Va riable resistors in the heater con trol network permitted regulation of the heatin g c.\'Ole by regulatin g the heater current . A 4 min heating­cooling cycle, wiLh equal high-low curreJlt periods, was found to be most effe ctive in r educin g overshoot. The usc of a lon ger cycle is not d.esirable , sin ce Lhe tempera t ure of th e resistors would Lhell follow Lhe changin g Lemperature of tIle co ntrolled aluminum case .

7. Shielded, coaxial cable was used. for all brid gr leads. Th ese shield s were ra rLh grounded.

2.2. Amplifier

Liston,Becker Direct,Current Amplifier, Model 14. 8 Cycle Floating Input. Maximum Gain-lX10 ' , With Continuously Variable Gain Controls. Internal Calibration Test Signal From 0.1 to 100 Microvolts

In the aULomatic recording sysLem , Lh e off-balance signal from the bridge was fed directly into tIl e amplifier. Thc shielded , coaxial lead from the bridge to Lhe amplifier was wrapped wi Lh ] iJl. of glass wool , covered wit}1 foil , and the shield and foil earth groulJded.

A peculiarity in the COll truction of the amplifier created an appreciable temperature differen ce be­twee n the inner and th e outer connection of the input plug. Th ermal emf's r esultin g from tl li s differen ce were eliminated by in stalling glass wool around the inner connection and by wrapping the outside connection with glass wool and aluminum foil.

2.3 . Recorder

Minneapolis,Honeywell Regulator Company, Brown Instrument Division-"Electronik," Potentiometric One Millivolt, Extended Range Recorder

'rhe onhr diffi culty eneO ll n Lered with the recorder was the 'problem 'of impedan ce matchill g. The recorder is a low impeda nce input-Lype, a nd the amplifier is a hi gh impeda nce ou tput-t~·pe. The network shown in figure 5 was used to couple these instruments. It is composed of a variable atLenuator, figure 5A, and filterin g-damping circuits, figure 5B. Two alternate low-pass filter systems are shown.

1- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - --j

I 5k A 5k 50 :

I ____ _ J I ' L ____________ _____________ ___ --

- ---- ... • .•.. - - ..• .. ••..•.. -- "'------1

20k !

17l

FIG URE 5. AtlemwtoT, bias mechanism, and filters .

EiLher performs sa ti sfacLorily , altltou gll the RC fil ter }Jas a smaller Lime constant.

Th e outpu t signal from Lhe amplifier was atten­uated ill accordan ce wiLh the manufacLurer's in s tru c­tions, quoted as follows : " IL is desirable to operaLe the amplifier output with a minimum ouLput of 0.5 volts for a full scale deflection so noise origin ating after the gain COli troIs will ]lot cause diffi culty. Wh ere potentiometri c type recorders with full scale ranges of less than 100 millivolts arc employed with the amplifier, a simple resistance a ttenuator should be used between the amplifier and recorder" [4]. The attenuation normallv used was of th e order of 500 to 1, but the variable 'attenu a tor added flexibility to th e usc of the measuri ng system .

2.4. Thermometer

Meyers, Bifilar, Single Layer Helix, Platinum Resistance Thermometer. Resistance-Approximately 25 Ohms at O °C

Thermal amI elect rical interferences ill Lit e thermom­eter were stabilized or elimina ted b l' means of in­sulation and shielding. The thermometer h ead and leads were covered with a braided copper shi~ld , a n in ch thickness of glass wool in sul ation , and a layer of aluminum foil. The shield was elecLri calh' earth grounded. .

2.5. System Zero

The device for obtaining the zero automatically consists of a timing mechanism to activate a solenoid a nd a mercury switch.

A bridge curren t cycle of 8 min is used and it is cu t off for 1 min of each c~' cle . This in telTuption allows the recording of th e zero. The cycle is generated by a motor-driven timin~ switch which operates a direcL current solenoid. The motor-driven timing switch and th e mercury switch used to interrupt brid ge current are depicted schematically in figure 2 as 8 2

and 8), respectively. The solelloid is encased in iron

273

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and mounted on the outside of the aluminum box that contains the bridge. The solenoid rotates a lucite rod that extends through the box and insula­tion. A mercury switch, attached to the rod, inter­rupts the bridge CUlTent at point 8 1 , figure 2, when the solenoid is activated. A mercury s\vitch is used in order to obtain reproducible contacts, and i t is put inside the aluminum box to eliminate thermal disturban ces.

2.6. Procedure

Since resistance changes from contact to contact of thc bridge dials may exceed 5 microhms, it is desirable to set the bridge at a predetermined resist­ance value and not change this setting during the experiment . At the beginning of an experiment the preset bridge resistance value may differ markedly from the thermometer resistance value. The re­corder input voltage must be biased if the bridge dials are not to be changed . This was accomplished by usinO' a 1.5-v mer cury battery , across a shunted voltage b divider , in series with the recorder input (fig.5C) .

In a resistance bridge there are small thermal emf's generated wherever an electrical connection is made. Because of the variety of construction materials and the different temperatures existing in the bridge case, these thermal emf's do no t necessarily cancel one anothcr. One method of taking a zero involves re­versing the polarity of the bridge CUlTen t. This produces an opposite shift in off-balance current , so that the "true" zero is representcd by one-half the differen ce of the two readings. At high amplifica­t ion , the thermal emf's in thc bridgc may make the taking of the zero by the currcn t-reversal method impossible. Since the the~'mal emf's do not change polarity when the current 1S reversed , they represent su ch a sizeable emf that the "forward" and "reverse" current cannot be recorded without changing the bridge setting. Consequently, at hig~est sensitivi~y, zeros were taken by the method of bndge-current lll­terruption. This method consists of shutting off the bridge current and recording the "true" zero or system balance point.

Two separate 6-v lead storage batteries wcre uscd as current sources for the system . One supplied current to the bridge-thermometer assembly and another supplied current to the heater relay-unit and the direct-current solenoid. The batteries are kept fully charged by a t rickle-ch arger during inactive periods.

3. Thermocouple and Potentiometer

The amplifier -recorder assembly has also been used in conjunction with a th?rmocoupl~ and a student­type potentiometer replac~ng the reslstanc~ thermom­eter and the Mueller bndge. A potentIOmeter of higher sensitivity and greater stability would have made the problem of precise temperature recording easier and would have given the value of the tempera­ture interval to a greater degree of accuracy. In this

arrangement the potentiometer was insulated in the same fashion as the Mueller resistance bridge. The box enclosing the potentiometer was constructed of soft iron instead of aluminum, because both electro­static and electromagnetic interferences were more of a problem here than with the bridge. Braided copper shields covered the thermocouple leads and connecting cables to eliminate electrical interference . A water triple-poin t cell was used as the reference temperature for the reference junction. The off­balan ce signal was amplified , attenuated, fil tered , and recorded as previously described for the bridge and thermometer system.

This thermocouple system is capable of measuring temperature changes of 0.00005 °C [5, 6]. The abso­lu te temperature is not lmown to this degree of accuracy because of un cer tain ties in reading the potentiometer and of calibrating the thermocouple. The continuous aging of the thermocouple pair necessitates frequent recalibrations and limits its use as a temperature interval sensing element, but for measuring small temperature differences its sensitiv­ity approaches that of the platinum resistance thermometer.

4 . Results and Conclusions

Th e overall capabili ties of the system, when used with the platinum resistance thermometer, are best shown graphically (fig. 6). The graph shows two recordings of the temperature of water at its triple point and a trace of the stability of the amplifier­recorder network with no load.

The triple-point cell was the type used for calibrat­ing thermometers with a thermometer immersion depth of 13 in . [7].

'rrace A, on the graph, shows the temperature of water at its triple point as recorded with the system described in this paper . The background noise band is equivalent to 0.00004 °C and the drift over an hour period is about 0.00002 °C.

O"-----,------,-----,-----~----~,-----~

10

20

30

4 0 )(

~. O.OOOl ll 50 ( O.OO IOC ) O.lfLv

60 1 1 70

/ C

80

6 9 10 II 12

TI ME, r--+ 3 min

FIG U RE 6. 'Temperature of water tTiple point cell (a) reco1'(led with modified equipment; (b) recm'ded with conventional bl'idge and theTmometer; and (c) amplifieT with zel'O load.

274

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The chart was rewound and trace B was recorded. This trace shows the temperature of water at its triple point when recorded with a type G- 2 Mueller Bridge and platinum resistan ce thermometer as supplied by the manufacturer. rrhe background noise is the equivalen t of 0.0003 °C and the drift is approximately 0.0002 0c. Also no ticeable arc the lon g-term c.yelic effects from the temperature changes in the room a nd from the bridge thermal regulator. At best, temperature readings can be made from this trace to ± 0.0005 °C. Again the char t was re­wound and trace C was made. This trace shows the s tability of the amplifier-recorder network. In this case the brid ge and thermometer were disconnected from the system, and the amplifier input leads were shorted . in terms of tempera ture the background noise band is approximately 0.00004 °C and the long-term drif t is about 0.00002 °C, the same as for the t riple-point cell in trace A.

'l'here a rc similarities in the frequency and ampli­t ude of the b ac l-;:ground noi se bands in both traces A and C. This indicates that t be greatest part of the system instabilit y is from Lh e fine stru ctural noise 'origin a ting in the amplifier. Th e ba ndwidth of thi s noi se is 0.00004 °C, and this limi ts tllC preci­sion of an in stantaneous measurement of temper­ature. However , in systems where in the general variation of temperature with time is known , a nearly uniform change of 0.00001 °C/min is casily di scernible for recording periods of 10 min or more. Thi s repre­sents a 10-fold gain in accurac.y and precision over m anual tech niques previousl.v used . Because of the long respon se time of the fiJter , rapid temperature

changes cannot be adequa tely recorded with the present systems. For ra pid temperature changes a different coupling network would have Lo be used .

The specific values of resistance a nd ca pacitance wlei ch are given were dictated by th e characteristics of the recorder and amplifier whi ch were available. Some chan ges would be necessary if in strumen ts with other characteristics were to be used. However, with some modification , thi s arra ngement for record­iu g temperatures can be used for man y purposes.

5. References

[1] G. T . Armstrong, P. K. 'Wong, and L . A. Kriege r, R ev. Sci. Instr. 30, 339 (1959).

[21 A. R . Glasgo w, Jr. , and M . T enenba um, An al. Che m. 28, 1907 (1956).

[31 Leeds a nd Northrup Co mpany Catalog EF22- 33(1) (1955).

[41 Instru ction ma nu al for D C Breaker Amplifier, Model 14, p . 9 (Liston Bec ker Instrument Co ., Inc., Sprin gdale, Conn .).

[5] A. R . Glasgow, J r., G . S. Ross, A. T . Horton, D . Enago ni o, H. D . Dixon , C. P . Saylor, G. T . Fu rukawa, M . L . R eill y, and Jeanette M. I-l ennin g, Anal. Chitn . Acta 17, 54 (1957).

[6] C. P . Saylor, Ana l. Chim. Acta 17, 36 (195 7). [71 Precision resistance t hermometry a nd fi xed points; te m­

peratu re, i ts meas urement a nd co ntrol in scien ce a nd indust ry, Vol. II, p. 141 (Rheinhold Publishin g Corp ., Ne,,· Yo rk, N .Y. ; Chapman a nd Hall , Ltd., London, E ngla nd, 1955) .

(Paper 64C4- 45)

275

l