Professional Documents
Culture Documents
ist in the corrosion tests in the circulation units previously It becomes necessary, therefore, in making the final evslua-
described. Any tendency to foaming should, therefore, mani- tion of a new antifreeze, to employ field tests in a wide variety
fest itself during these tests. Observations are made peri- of automobiles under various conditions of use. Accurate
odically for evidence of foaming. A solution which foams to comparative results cannot be obtained by road testa, it is
any serious extent will foam up into and out of the top of the true, because conditions cannot be controlled, but these tests
reflux condenser which is located on the top reservoir of the do occasionally reveal a fault in an antifreeze which did not
unit. manifest' itself in laboratory tests.
Field Tests Acknowledgrnen t
Sotwithstanding the care which is taken in making labora- Earlier forms of the corrosion-testing equipment described
tory tests, and the effort which is made to duplicate actual herewith were originally developed by the senior author at
conditions of use in a n automobile, it is difficult to simulate The Miner Laboratories in connect,ion m-it'h research fellow-
all conditions. This could probably be accomplished if all ships of the Association of American Soap and Glycerine
automobile cooling systems were constructed exactly alike. Producers, Inc.
Unfortunately, however, they all differ in some way, so that
if the investigator simulates one particular cooling system in Literature Cited
his laboratory tests, then his conditions of test and construc-
[lj Bengouyh, G. D., and May, R.. Engineer, 136,7710 (1923).
tion of equipment will not be wholly applicable to another. 12) Speller, F. N., "Corrosion: Causes and Prevention," 2nd ed..
Cooling systems of various makes of automobiles are likely p. 14, Xew Tork, McGraw-Hill Book Co., 1935.
to differ in one or more of the following characteristics: con- ( 3 ) Ihid., pp. 250-1.
structional design, materials of construction, ,metallic couples, RECEIVED March 28, 1938. Presented before t h e Division of Industrial and
rate of circulation, amount of aeration. and operating tem- Engineering Chemistry a t the 95th Meeting of the American Chemioal So-
perature. ciety, Dallas, Texas, April 18 t o 22, 1938.
Viscosity Measurement
R I . R. CANNON AND &I. R. FENSKE
School of Chemistry and Physics, The Pennsylvania State College, State College. Pa.
Viscosity and viscosity temperature coef- identical boiling points differ in viscosity by several hundred
ficients are valuable identifying properties per cent.
of pure compounds and petroleum frac- It is the purpose of this paper to describe briefly suitable
capillary-type viscometers for measuring viscosity in a simple
tions. This paper discusses the operating but precise manner. In addition, the sources of error and
characteristics of simple modified Ostwald their magnitude will be discussed, together with means of ren-
viscometers that are suitable for covering a dering these negligible.
wide range of viscosity with accuracy. The Figure 1 is a n illustration of a n accurate routine viscometer,
particularly designed for petroleum fractions, which is now in
important sources of error in capillar>- extensive use in the petroleum industry both in this country
viscometers are analyzed briefly and equa- and abroad. A complete description and operating technic
tions for computing the necessary correc- have been recently published by the American Society for
tions are given. Comparisons are made Testing Materials (1).
with other types of capillary viscometers The extra bulb on the capillary side of the instrument is for the
which show that the modified Ostwald is purpose of incorporating an accurate loading device as an integral
part of the viscometer. A glass bridge joins the two legs of the
equal in accuracy to any now- available. viscometer as shown; in addition heavy-walled glass is used
throughout, so that the instrument is not fragile. Practically
any size of working capillary can be used in the viscometer, so
that very viscous fluids such as heavy lubricating oils c m be
The second term on the right side of this equation is the capillary so that kinetic energy corrections may be maintained
kinetic energy correction. In a properly designed instrument below 0.2 per cent. This was verified by testing water a t two
this term should be very small compared with the first term on different temperatures in each of two viscometers with capil-
the same side of the equation. The percentage error or cor- laries of different size.
rection is more important than the absolute figure. The ex-
pression for the percentage correction can be obtained by
dividing the kinetic energy term by the main term and multi-
plying by 100.
;i2
-100
T0
BORE 2.5
L
Kinetic energy correction in per cent = GLASS
STRENGTHENINC
BRIDGE
The velocity in the capillary is given by U. From this
expression it is obvious that kinetic energy corrections ~vill
increase as the square of the velocity in the capillary. 0 ETCHED
LINES
GLASS
STRENGTHENN
BRIDGE
T
1
s
1
BORE 1.5
BOTH BULBS
CAPACITY
= LOCC.
ETCHED
,LINES
BORE 2.5
1-
BORE RANGE
0.3 to 2.0
FIGURE3. MICROVISCOMETEB
Dimensions in mm.
length, known as the Couette correction, is a function of the which is placed in the open arm of the viscometer. An ex-
capillary radius. It is included in the viscometer constant perienced operator can load and align the viscometer in the
established by calibration. bath in less than one minute. The viscometer of Figure 1
Drainage errors arise from the fact that all liquids do not has the efflux bulb and lower reservoir directly in line for
drain from a surface with equal ease; hence, the measured eliminating alignment errors. This modification has not
efflux volume for one fluid may be different than for another. been incorporated in the other two viscometers, because they
In a series of experiments performed to measure drainage er- are longer and readily adjusted to the vertical position. The
rors (4) it was shown that these are of negligible magnitude. vertical alignment of bulbs was originated by Gruneisen (2).
In addition t o the possible effect on efflux volume, Fitzsimons The viscometer constant will vary with the temperature,
(6) pointed out that drainage will affect the liquid head. but the magnitude of the change is small and readily com-
The experimental drainage measurements indicate that this puted. This correction arises because of the change of spe-
effect will never change the liquid head by 0.01 per cent in cific volume with temperature. Thus, if the viscometer is
viscometers of the type described here. loaded a t 25" C. and then used a t some higher temperature,
If there is a considerable difference between the surface say 100" C., a correction should be applied. The ther-
tension of the calibrating fluids and the fluids subsequently mal coefficients of cubical expansion of most hydrocarbons do
tested, an error due to capillarity will arise. Although the not differ sufficiently to necessitate an individual correction
familiar capillary-rise equation will not hold rigidly for tubes for each type of compcund. It is therefore possible to give
of large diameter, it may be employed to determine the mag- simply the viscometer constant a t two different tempera-
nitude of this error. It can be readily shown that the change tures, and for other temperatures one can interpolate or
in effective driving head due to surface tension difference is ap- extrapolate. Mathematically the viscometer constant a t a
proximated by the following equation: second temperature may be readily computed from the known
constant a t some other temperature by the following equation :
the working area of the bath is greater than 10 cm. (4 inches). For accurate results it is necessary to employ sensitive
I n most installations their effect mill be small, but if proper and reliable auxiliary equipment. Descriptions of satisfac-
care is not exercised the error so introduced may be of conse- tory units have been published ( 5 ) .
quence.
Comparison with Other Viscometers
TABLE1. MAGNITUDE O F TEhIPERlTURE IXCREiSE I S LIQUIDS Various other modifications of the Ostwald instrument are
CAUSED BY RADIASTENERGY FROM USSHIELDED LIGHTBULBS advocated by some investigators. Ubbelohde's (12) sus-
Distance
of Bulb
pended-level type of instrument differs from the type de-
Surface Temp. scribed here only in eliminating loading errors and reducing
from Temp. of Dif-
Type of 110- Bath of Water fer- surface tension errors I n the design presented here such
Liquid Color Voit Light Bulb Surface Liquid Bath ence errors are of negligible magnitude; hence either type of in-
Cm. C. ' C. C. strument, will yield results of equal accuracy. Zeitfuchs (14)
Lube oil A.S.T.M. 100-watt frosted 1.25 38.41 37.78 0.63 has recently described another modification of the Ostwald
KO. 7 5.00 38 19 37.78 0.41
10.00 38.07 37.78 0.29 instrument.which also reduces loading errors and undoubtedly
-la-watt
_ frosted 1.25 38.06 37.78 0.28 will yield accurate results. Slight modifications of the Ubbe-
5.00 37.92 37.78 0.14
10.00 37.89 37.78 0.11 lohde type have been described by Fitzsiinons (6) and by
50-watt frosted 1.25 37.86 37.78 0.08 Payne and Miller (9).
5.00 37.84 37.78 0.06
10.00 37.81 37.78 0.03 The semimicroviscometer described here is simpler than
Lube oil A.S.T.M. 100-watt frosted 1.25 38.36 37.78 0.58 the falling-sphere type described by Schneider and i\IcCon-
KO.2.5 LOO 38.13 37.78 0 35 riel1 (11) and is more convenient than the type described by
10.00 38.02 37.78 0.24
75-watt frosted 1.25 38.04 37.78 0.26 Levin (7') ivhere surface tension is employed as the driving
5.00 37.94 37.78 0.16 force.
10.00 37.89 37.78 0.11
The viscometer recently described by Raaschou (10) is also
50-watt hosted 1.25 37.86 37.78 0.08
5.00 37.84 37.78 0.06 a modification of the Ostwald tube and again the main purpose
10.00 37.82 37.78 0.04 is to reduce loading errors. This is accomplished by adjust-
Water .,. 100-watt frosted 1.25 37.83 37.78 0.05 ing the liquid level by visual inspection of the meniscus in a
5.00 37.80 37.78 0.02
10.00 37.79 37.78 0.01 tube of large diameter (17.5 mm.). It is difficult to make
75-katt frosted 1.25 37.80 37.78 0.02 such an adjustment to better than 0.5 mm. An error of this
5.00 37.79 37.78 0.01
10.00 37.78 37.7s 0.00 magnitude would change the driving fluid head by the same
T h e constant-temperature bath was of 36-liter capacity and was filled with amount and introduce a percentage error of 0.5 per cent
water. T h e walls were of Pyrex glass approximately 0.6 cm. thick. T h e (since the total head is approximately 100 mm.). For most
Pyrex teat tube containing t h e sample w&s 5 om. from the inner bath surface,
practical purposes such an error is of little consequence.
Raaschou uses a value of 1.0074 centistokes as the viscosity
The data of Table I were obtained a t 37.23" C. (100" F.) of water a t 20" C., whereas a value of 1.0068 centistokes has
because it is a standard test temperature in the petroleum been recommended by the American Society for Testing
industry. The measurements were made by placing the Materials as the standard for viscosit,y work. While this
fluid under test in a Pyrex test tube and then immersing it difference is slight, it has been included in this report to cover
in a constant-temperature water bath automatically con- completely the many factors involved.
trolled a t 100" F. to within *0.05" F. Temperature meas- It appears, then, that there are available a number of
urements were made by very sensitive Bureau of Standards capillary-type viscometers which will yield accurate results.
calibrated thermometers. I n the experiments where water The prospective user can be guided in his choice by such fac-
was tested, the radiant heat was probably picked up by the tors as cost, simplicity of design and operation, etc.
thermometer bulb rather than by the mater. The magnitude The reproducibility of results with the modified Ostwald
of the actual errors in viscosity caused in this way depend viscometers described in this paper is *0.2 per cent,. The
upon the viscosity temperature coefficient of the fluid a t the accuracy of the results depends upon the accuracy with which
test temperature. Many heavy oils change in viscosity the absolute viscosity of water is known a t 20" C., since water
by 0.2 per cent with a temperature change of 0.1" F. in is used as the ultimate reference basis. This error is prob-
the vicinity of 100" F. At lower temperature levels the ably in the neighborhood of *0.5 per cent. However, rela-
effect would be more pronounced because viscosity tempera- tive viscosities are very accurate and if the reference basis is
ture coefficient increases with decreasing temperature level. clearly defined little confusion will exist and reported values
of viscosities may be readily compared.
Calibration of Viscometers Literature Cited
A nearly ideal reference basis for viscosity work is pure (1) Am. SOC.Testing Materials, "Standards on Petroleum Products
mater. Instruments which are designed t o cover a viscosity and Lubricants," 1936.
range in the neighborhood of water can be calibrated directly (2) Barr, G., "Monograph of Viscometry," London, Oxford Uni-
against water. When an instrument is designed t o cover a versity Press, 1931.
(3) Bingham. E . C., and Thompson, R. T., J. Rheol., 1, 418 (1930).
range far removed from water, such as that found in lubri- (4) Cannon, hf. R., and Fenske, M. R., Oil Gas J.,33, 52 (1935).
cating oils, direct calibration is not possible. However, (5) Ibid., 34, 46 (1938).
water may be retained as the reference basis by standardizing (6) Fitesimons, 0.. ISD. ESG. CHEni., Anal. Ed.. 7, 346 (1935).
a series of oils in suitable master instruments and then em- (7) Levin, H., Ibzd., 9, 147 (1937).
(8) hlikeska, L. A., ISD. ESG. C H E W , 28, 970 (1936).
ploying these oils as calibration standards. This procedure (9) Payne, E. H., and hliller, C. C., Ibid., Anal. Ed., 8, 300 (1936).
has been explained in detail elsewhere (6). As many oils are (10) Raaschou, P. E., Zbid.. 10, 35 (1938).
unstable and increase in viscosity with age as much as 2.0 (11) Schneider, H. F., and McConnell, T. 8., Ibid., 8, 28 (1936).
per cent per year, it is advisable to check the viscosity of (12) Lbbelohde, L., I b i d . , 9, 85 (1937).
(13) Kggins, W. R., J.Inst. Petroleum Tech., 22, 305 (1936).
standardized oils from time to time. Solvent-treated or (14) Zeitfuchs, E. H., E a t [ . Petroleum News, 29, 68 (1937).
aluminum chloride-desludged oils of high viscosity index are
the most stable and some vary only 0.2 per cent per year. RECEIVED
February 8, 1938.