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Instrument Division Fisher Scientific Company 71 1 Forbes Ave.

Pittsburgh, Pennsylvania 15219

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Y ~ L Gl 75672
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FISHER Surface Tensiometer
Model 20
CQNTENTS

THE INSTRUMENT
UNPACKING
ASSEMBLY
CALIBRATION
OPERATION
Measuring Surface Tension
Measuring Interfacial Tension
Converting Scale Readings
MAINTENANCE
Annual Application of Oil
Replacement of T o r s i o n Wire
REPLACEMENT PARTS

ILLUSTRATIONS

Figure

1 Mechanical S y s t e m
2 Measuring Surface Tension
3 Measuring Interfacial Tension
4 Correction Factor Chart
THE INSTRUMENT
The FISHER Surface Tensiometer, Model 20, i s used to
d e t e r m i n e the apparent s u r f a c e tension and interfacial tension
of liquids. Employing the ring method to achieve speed and
accuracy, the i n s t r u m e n t i s applicable to many educational,
biological, medical and industrial determinations i n connec-
tion with water, petroleum products, detergents, pharmaceu-
tical m a t e r i a l s and other substances.

The Model 20 utilizes the principles of operation originally


devised by Dr. P i e r r e Lecomte du Nouy, the noted biochemist,
f o r studies of blood s e r u m and other biological fluids. E s s e n -
tially a torsion-type balance, it i s the kind of instrument
c u r r e n t l y specified by the American Society for Testing M a t e r i a l s
in Methods D-971 (interfacial tension of oil against w a t e r ) and
D-1331 ( s u r f a c e and interfacial tensions of detergents).

In the du Nouy method, a platinum-iridium ring of p r e c i s e l y


known dimensions i s suspended f r o m a counter-balanced
l e v e r a r m . The a r m i s held horizontal by torsion applied
t o a taut s t a i n l e s s s t e e l w i r e , to which it i s clamped. Increasing
the t o r s i o n in the w i r e r a i s e s the a r m and the ring, which
c a r r i e s with i t a film of the liquid in which i t i s i m m e r s e d .
The f o r c e n e c e s s a r y to pull the t e s t ring f r e e f r o m this s u r f a c e
film i s m e a s u r e d .

The Surface T e n s i o m e t e r shows this "apparent" s u r f a c e o r


interfacial tension (the l a t t e r m e a s u r e d a t the interface between
two i m m i s c i b l e liquids) on a calibrated dial. The dial readings
c a n be used d i r e c t l y for comparative studies o r converted to
"true1' values by using a c o r r e c t i o n factor chart.

UNPACKING
The FISHER Surface T e n s i o m e t e r i s shipped in a single carton.
Carefully unpack the contents, and check each i t e m against the
packing l i s t below. If any i t e m s a r e damaged, save a l l packing
m a t e r i a l and file c l a i m with the c a r r i e r ; i f any i t e m s a r e
m i s s i n g , notify your n e a r e s t F i s h e r Branch.

Quantity Item Number

1 Surface T e n s i o m e t e r 14-812
1 Platinum -Iridium Ring 14-812-5
2 T o r s i o n Wire Assembly 12208
1 Instruction Manual 15041

ASSEMBLY
The Surface T e n s i o m e t e r c o n s i s t s of a t o r s i o n w i r e balance with
a dial calibrated in dynes p e r centimeter, a weighed platinum-
iridium ring, and a movable table. The t o r s i o n w i r e balance
and movable table a r e mounted on the stand within the case.
The ring i s shipped i n a wooden container which i s s e c u r e d t o
the m a i n pedestal of the stand.

P r i o r to u s e , the i n s t r u m e n t should b e placed on a solid support


(table o r bench) and leveled. To do this, simply open the door
and, using the two knobs n e a r the left edge of the base, adjust
the feet until the s p i r i t l e v e l indicates that the cabinet i s level.

F o r shipping purposes, the tension h a s been relieved f r o m the


t o r s i o n wire. In o r d e r to r e s t o r e the tension, back off the
s c r e w which i s a c c e s s i b l e through the s m a l l hole i n the upper
c e n t e r portion of the r e a r of the cabinet. Loosening this
s c r e w allows the tension spring (Item 4 of F i g u r e 1 ) to e x e r t
p r e s s u r e against t h e bar (Item 2), thus r e s t o r i n g t h e tension
on the wire. The packing m a t e r i a l which supports the junction
of the t o r s i o n w i r e and level a r m should be removed, a s should
the packing m a t e r i a l on the level a r m n e a r the index m i r r o r
and a r r e s t m e c h a n i s m ( I t e m s 12 and 23 of F i g u r e 1). The
Surface T e n s i o m e t e r i s now ready f o r calibration.

CALIBRATION

The calibration of the t o r s i o n w i r e and hence of the Surface


T e n s i o m e t e r h a s been carefully t e s t e d a t t h e factory but should
be checked before u s e and adjusted i f necessary. The calibration
i s c a r r i e d out s o that the dial will r e a d directly in dynes p e r
centimeter.

Make s u r e that the t o r s i o n a r m a r r e s t mechanism (Item 23)


i s holding t h e a r m . Hang t h e platinum-iridium ring on the
hook a t the left end of the lever. Cut a s m a l l s t r i p of paper
and fit i t onto t h e ring to a c t a s a platform f o r a weight which
will be u s e d f o r t h e calibration. R e l e a s e the t o r s i o n a r m ,
a n d adjust t h e knob on t h e right side of the c a s e until the index
(Item 11) and i t s i m a g e a r e exactly i n line with the r e f e r e n c e line
of the m i r r o r (Item 12). Turn the knob beneath the main dial
on the front of the i n s t r u m e n t until t h e v e r n i e r r e a d s z e r o on
the outer s c a l e of the dial. A r r e s t the t o r s i o n a r m .

P l a c e a known m a s s f o r calibration on the paper platform (600


m i l l i g r a m s i s quite suitable and simplifies calculations). R e l e a s e
the t o r s i o n a r m . T u r n t h e knob on the right side of the c a s e in a
counterclockwise direction until the index and i t s i m a g e a r e again
exactly in line with t h e r e f e r e n c e line of the m i r r o r . Record
the dial reading to the n e a r e s t 1 / 10 s c a l e division (by u s e of
the v e r n i e r ) .
It i s now n e c e s s a r y t o determine t h e accuracy of the calibration
f r o m the reading obtained. The apparent surface tension, S,
i s given a s follows:

where:

M = the weight expressed in g r a m s


g = acceleration of gravity expressed in
cm/sec2
L = m e a n circumference of the ring in
centimeters
?
,S = dial reading = apparent s u r f a c e tension
\
in dynes p e r c m

F o r example, suppose that a 600 milligram weight was used.


The circumference of t h e ring i s 6. 00 cm, and the value for
g i s 980 c m / s e c.2
Then we find that

If the dial reading differs f r o m the calculated value, then t h e


effective length of the t o r s i o n a r m m u s t be adjusted until these
two values do agree. This adjustment i s accomplished by
turning the knurled knob a t the left end of the l e v e r a r m (Item
10) s o a s t o move the hanger hook. If the recorded dial reading
i s g r e a t e r than the calculated value, move the hook to shorten
the effective length of t h e a r m . Conversely, i f the dial reading
i s l e s s than the calculated value, move the hook to lengthen the
effective length of the a r m . Repeat the calibration procedure
until the dial reading and calculated value agree. The dial
will r e a d directly in dynes per centimeter.

The m e a n c i r c u m f e r e n c e of rings i s 6. 00 c m in general. Slight


deviations may be found, and the circumference of each ring i s
noted on i t s container. In the preceding example, 600 milli-
g r a m s w e r e used to simplify calculations.

The value of g, the acceleration of gravity, v a r i e s slightly f r o m


place to place on the surface of the earth. F o r p r e c i s e work,
the u s e of the exact value of g for the locality i s recommended.
F o r c e r t a i n localities, this value m a y be listed in various hand-
books; o r i t may be determined experimentally.

OPERATION

In making a determination of s u r f a c e tension, careful preparation


of the sample and the Surface Tensiometer m u s t precede the
actual manipulation of the instrument.
FIGURE 1 - MECHANICAL SYSTEM

The s a m p l e should b e p l a c e d i n a g l a s s b e a k e r o r c y l i n d r i c a l
v e s s e l with a d i a m e t e r of a t l e a s t 45 m i l l i m e t e r s . F o r testing
oil s a m p l e s a c c o r d i n g to ASTM Method D-971, the g l a s s w a r e
should b e c l e a n e d a c c o r d i n g t o a definite p r o c e d u r e . Any
r e s i d u a l oil f r o m t h e p r e v i o u s s a m p l e i s r e m o v e d with p e t r o -
l e u m naphtha o r benzene followed by s e v e r a l w a s h e s with methyl
ethyl ketone a n d w a t e r , then t h e g l a s s w a r e i s i m m e r s e d i n a
hot cleaning solution of c h r o m i c acid. T h e g l a s s w a r e a l s o should
b e r i n s e d thoroughly with t a p w a t e r , then with d i s t i l l e d w a t e r .
It should b e d r a i n e d i n a n i n v e r t e d position o v e r a c l e a n cloth,
u n l e s s i t is t o b e u s e d immediately.

T h e p l a t i n u m - i r i d i u m r i n g should be c l e a n e d by r i n s i n g i t i n
p e t r o l e u m naphtha o r benzene, then by r i n s i n g i n m e t h y l ethyl
ketone. The r i n g should t h e n b e heated i n t h e oxidizing portion
of a g a s f l a m e .

The p r e c e d i n g i n s t r u c t i o n s apply p a r t i c u l a r y t o p r e p a r a t i o n f o r
d e t e r m i n a t i o n s o n oil s a m p l e s . A c o m p a r a b l e d e g r e e of c l e a n -
l i n e s s should b e sought f o r o t h e r s a m p l e s .
Since s u r f a c e tension i s dependent upon temperature, considera-
tion m u s t be given to this factor. F o r theoretical work, t e m -
p e r a t u r e s m u s t be specified; however, 25OC i s the t e m p e r a t u r e
m o s t commonly used. F o r control work, the operator should
u s e the s a m e t e m p e r a t u r e f o r each type of measurement.

FIGURE 2 - MEASURING SURFACE TENSION


Measuring Surface Tension ( s e e Figure 2):

The cleaned platinum-iridium ring should f i r s t be attached to


the hook a t the end of the l e v e r a r m . The a r r e s t mechanism
should be holding the a r m a t this time.

The liquid to be m e a s u r e d i s t r a n s f e r r e d to the clean glass vessel


and placed on the sample table. The sample table i s moved
around until i t i s directly beneath the platinum-iridium ring.
R a i s e the s a m p l e table until the ring i s i m m e r s e d in the t e s t
liquid. The ring should be in the liquid, beneath the surface
s o that the e n t i r e ring will be wetted. About 118 inch i m m e r -
sion i s generally considered sufficient.

The torsion a r m i s now released and the instrument adjusted to


a z e r o reading. Adjust the knob on the right side of the c a s e
until the index and i t s image a r e exactly i n line with the r e f e r -
ence m a r k on the m i r r o r . Be careful to keep the ring in the
liquid during this manipulation, raising o r lowering the sample
table i f n e c e s s a r y be m e a n s of the knob adjustment underneath
the table. Now t u r n the knob beneath the m a i n dial on the front
of the c a s e until the v e r n i e r r e a d s z e r o on the outer s c a l e of
the dial.
Lower the sample table until the ring i s in the s u r f a c e of the
liquid, adjusting t h e knob on the right side of the c a s e to keep
the index lined up with the reference m a r k on the m i r r o r . The
s u r f a c e of the liquid will become distended, but the index m u s t
be kept on the reference. Continue the two simultaneous adjust-
ments until the distended film a t the s u r f a c e of the liquid breaks.
The s c a l e reading a t the breaking point of the distended film i s
the apparent s u r f a c e tension.

FIGURE 3 - MEASURING INTERFACIAL TENSION


Measuring Interfacial Tension ( s e e F i g u r e 3 ) :

INTERFACIAL TENSION FROM MORE DENSE LIQUID TO LESS


DENSE LIQUID i s made by exerting a n upward f o r c e on the ring.
P r o c e d u r e i s v e r y s i m i l a r to surface tension m e a s u r e m e n t s ;
and cleanliness of ring and sample container i s , of course,
essential.

The m o r e dense liquid i s t r a n s f e r r e d to the clean g l a s s v e s s e l


and placed on the sample table, and the table moved beneath
the platinum-iridium ring. The sample table i s r a i s e d until
the ring i s i m m e r s e d about 1/ 8 inch and wetted by the heavier
liquid. The torsion a r m i s now r e l e a s e d and the instrument
adjusted to a z e r o reading. Adjust the knob on the right side of
the c a s e until the index and i t s image a r e exactly in line with
the reference m a r k on the m i r r o r . Be careful to keep the ring
i n t h e liquid during t h i s manipulation by r a i s i n g o r lowering t h e
s a m p l e t a b l e (if n e c e s s a r y ) by m e a n s of the knob adjustment
beneath the table. T u r n the knob beneath the m a i n dial on t h e
f r o n t of t h e c a s e until t h e v e r n i e r r e a d s z e r o o n t h e o u t e r s c a l e
of t h e dial.

P o u r t h e l i g h t e r liquid onto the s u r f a c e of the h e a v i e r liquid to


a depth of about 114 t o 1 / 2 inch, depending on the two liquids.
The l a y e r of l i g h t e r liquid should b e deep enough s o that the
ring will not enter. t h e u p p e r s u r f a c e of t h e l i g h t e r liquid before
the interface film ruptures.

B e f o r e proceeding with t h e actual m e a s u r e m e n t , i t m a y be


a d v i s a b l e to allow the i n t e r f a c e t o a g e o r stabilize f o r a time.
F o r example, ASTM D-971 p r e s c r i b e s a n aging p e r i o d of 30
seconds f o r a n i n t e r f a c e between oil and w a t e r .

Lower t h e s a m p l e t a b l e until t h e ring i s i n t h e i n t e r f a c e between


t h e two liquids, adjusting t h e knob on t h e right s i d e of t h e c a s e
to keep t h e index lined up with t h e r e f e r e n c e m a r k on the
m i r r o r . The i n t e r f a c e between t h e two liquids will b e c o m e
distended, but t h e index m u s t be kept on t h e r e f e r e n c e . Con-
tinue t h e two simultaneous a d j u s t m e n t s until t h e distended
f i l m a t t h e i n t e r f a c e r u p t u r e s . The s c a l e reading a t the breaking
point of t h e i n t e r f a c i a l f i l m i s t h e a p p a r e n t i n t e r f a c i a l tension.

INTERFACIAL TENSION FROM LESS DENSE LIQUID TO MORE


DENSE LIQUID i s m a d e by exerting a downward f o r c e on t h e
ring. The r i n g u s e d on the Surface T e n s i o m e t e r i s weighted,
and i n effect e x e r t s i t s own f o r c e , the effective downward f o r c e
being i n c r e a s e d by d e c r e a s i n g t h e upward f o r c e f r o m the t o r s i o n
w i r e a s e x e r t e d through the l e v e r a r m . The p r o c e d u r e differs
only slightly f r o m that employed in the previously d e s c r i b e d
m e a s u r e m e n t of i n t e r f a c i a l tension; and t h e c l e a n l i n e s s of the
r i n g a n d s a m p l e c o n t a i n e r i s , of c o u r s e , e s s e n t i a l .

The m o r e d e n s e liquid i s t r a n s f e r r e d to the c l e a n g l a s s v e s s e l ,


to a depth of 114 t o 112 inch, depending on t h e two liquids.
The l a y e r should b e deep enough s o that t h e ring will not con-
tact t h e bottom of the v e s s e l b e f o r e the i n t e r f a c e f i l m r u p t u r e s .

The l i g h t e r liquid i s now p o u r e d onto the s u r f a c e of t h e h e a v i e r


liquid a l r e a d y in t h e v e s s e l , and the v e s s e l on t h e s a m p l e table
m o v e d beneath t h e platinum-iridium ring. T h e s a m p l e t a b l e
i s then r a i s e d by t h e g r o s s a d j u s t m e n t until t h e ring i s i m m e r s e d
i n the l i g h t e r liquid a n d wetted by it (about 118 inch above t h e
liquid interface). The t o r s i o n a r m i s now r e l e a s e d , and the
i n s t r u m e n t adjusted t o a z e r o reading. Adjust t h e knob on t h e
r i g h t s i d e of t h e c a s e until the index a n d i t s i m a g e a r e exactly
i n line with t h e r e f e r e n c e m a r k on the m i r r o r . Be c a r e f u l to
keep the ring i n t h e l i g h t e r liquid during this manipulation by
raising o r lowering the sample table (if n e c e s s a r y ) by means
of the knob adjustment beneath the table. Turn the knob beneath
the main dial on the front of the c a s e until the v e r n i e r reads
z e r o on the inner s c a l e of the dial.

Raise the sample table until the ring i s in the interface between
the two liquids, adjusting the knob on the right side of the c a s e
to keep the index lined up with the reference m a r k on the m i r r o r .
The interface between the two liquids will become distended,
but the index m u s t be kept on the reference. Continue the two
simultaneous adjustments until the distended film a t the inter-
face ruptures. The s c a l e reading a t the breaking point of the
interfacial film i s the apparent interfacial tension.

Converting Scale Readings:

Readings of the Surface Tensiometer give apparent surface


tension and apparent interfacial tension. In o r d e r to obtain the
t r u e surface tension o r t r u e interfacial tension, the relationship

i s used, where S i s the t r u e value, P the apparent value a s


indicated by the dial reading, and F a correction factor. The
correction factor F i s dependent on the s i z e of the ring and the
s i z e of w i r e used in the ring, the-apparent surface o r inter-
facial tension, and the densities of the two phases. The r e -
lationships a r e e x p r e s s e d by the following two f o r m s , either
one of whichmay be used in preparing a correction factor c h a r t
(like the one shown in F i g u r e 4).

where:

F = the correction factor


R = the radius of the ring
r = the radius of t h e wire of the ring ',
P = the apparent value o r dial reading
D = the density of the lower phase
d = the density of the upper phase
K = 0.04534 -
1. 679 r / R
C = the circumference of the ring ,
a = 0.725
b = 0.0009075

The a , b, and the numerical p a r t of K a r e universal constants


for all rings.
In o r d e r to u s e the correction factor chart, the operator must
-
initially calculate the value of the expression P / ( D d) for each
sample, and know the value of R / r . F o r the Surface Tensio-
m e t e r , the circumference of the ring i s 6 centimeters and the
.
radius of the w i r e i s 007 inches. T h e r e may be some slight
variation i n t h e s e dimensions, but the value of R / r i s usually
53. 2. Curves a r e shown for R / r = 50 and R / r = 60, s o that
correction f a c t o r s m a y be found for any value of the r a t i o
between 50 and 60.

Should a ring of different diameter be employed, the u s e r can


p r e p a r e a curve f r o m the above equations. All quantities used
in these equations a r e expressed in the centimeter-gram-
second system, with densities expressed in g r a m s per cubic
centimeter; P (apparent s u r f a c e o r interfacial tension) expressed
in dynes per centimeter; while R, r, and C a r e expressed in
centimeters.

Use of the correction factor i s usually limited to theoretical


work. F o r control purposes, reproducibility within certain
tolerances i s sufficient.

FIGURE 4 - CORRECTION FACTOR CHART


Maintenance on the Surface Tensiometer will normally be limited
to an annual application of oil and occasional replacement of the
torsion wire.

Annual Application of Oil:

The zero adjustment shaft and bearing ( s e e Items 14 and 17 i n


Figure 1 ) should b e oiled once e v e r y twelve months; two drops of
light oil should be sufficient. Putting a drop o r two of oil on the
post and adjusting nut of the sample table i s also advisable once
a year.

Replacement of Torsion Wire:

Replacement of the torsion wire may be n e c e s s a r y f r o m time to


time due to accidental breakage. By referring to Figure 1, the
replacement procedure can be readily visualized. The torsion
a r m (Item 5) should be held by the a r r e s t i n g mechanism (Item 2 3 ) ,
and the clamping block (Item 6) supported by a suitable wood o r
cardboard block between itself and the casting. The cover of the
v e r n i e r pointer on the front of the c a s e should be removed by
loosening the s e t screw. Now the s c r e w a t the back of the c a s e
which controls the tension spring (Item 4) should be turned i n so
a s to r e l e a s e a l l tension on the wire. The front wire holder
(Item 3) should be loosened so a s to r e l e a s e the front end of the
wire. Now the s c r e w s on the clamping block (Item 6 ) of the
torsion a r m should be loosened. The torsion wire should now be
entirely free. If i t i s not broken, i t can be removed by pulling
toward the r e a r of the instrument.

The replacement wire h a s a b a r (Item 2 ) attached for holding in


the tension spring (Item 4). The wire should be installed by
working the front end forward f r o m the r e a r , being careful not
to bend o r kink the wire. Do not fasten the wire in the clamping
block (Item 6) a t this stage. It should be brought forward through
the sleeve (Item 14) to the front wire holder (Item 3 ) . A scribed
line shows the position i n which the wire should be placed in o r d e r
to center it. Hold the wire taut with p l i e r s and tighten the two
s c r e w s of the front wire holder. Excess wire may now be cut off
and the cover of the v e r n i e r pointer assembly replaced.

Tension should now be applied to the wire by slacking off on the


s c r e w that holds the tension spring. This s c r e w i s accessible
through the r e a r of the case. The procedure i s the s a m e a s when
the instrument was originally unpacked and readied for use.

The torsion a r m m u s t now be attached to the wire. This i s b e s t


accomplished by removing the left s c r e w f r o m the clamping block
(Item 6) and loosening the right screw. The w i r e m u s t r e s t i n
the groove i n the block, and when so fitted, the two s c r e w s a r e
tightened. Upon removing the support f r o m under the clamping
block, check and if n e c e s s a r y adjust the diameter of the new
torsion w i r e a s follows:

1. Level the instrument.

2. Cut a s m a l l s t r i p of paper and place i t on the platinum-iridium


ring to f o r m a platform.

3. P l a c e a 1:000 g r a m weight on the platform.

4. Release the torsion a r m .

5. Adjust knob on right side of instrument c a s e until index


pointer on a r m coincides with reference line on m i r r o r .

6. Turn knob to right of main dial on front of instrument until


v e r n i e r r e a d s z e r o on outer s c a l e of dial.

7. Remove 1.000 g r a m weight f r o m platform.

8. Place a 1.800 g r a m weight on platform.

9. Adjust knob on right side of instrument c a s e until index


pointer on a r m coincides with reference line on m i r r o r .

NOTE: The reading obtained should b e 65.7 to 66.0. If the


reading i s higher, the diameter of the torsion w i r e between the
a r m and the r e a r of the instrument m u s t be reduced. Conversely,
i f the reading i s lower, the diameter of the w i r e between the a r m
and the front of the instrument m u s t b e reduced. In each c a s e ,
Crocus cloth should be used. The w i r e m u s t be kept syrnrnet-
r i c a l and round with uniform diameter along i t s length.

10. Calibrate instrument a s directed on pages 2 and 3 under


CALIBRATION.
REPLACEMENT PARTS

The following i s a l i s t of p a r t s which may need to be replaced


over a period of time. To a s s i s t i n identifying each item, the
tabulation includes c r o s s reference numbers to the mechanical
s y s t e m drawing (Figure 1).

Visual Reference -
Item Number
(Figure 1)

Torsion Wire As.sembly


Clamp B a r
Tension Spring
Torsion A r m
A r m Clamping Block
Index Assembly
Hanger Spring
Hanger Assembly
Knurled Nut
Mirror
Vernier Pointer
Dial Shaft
Worm Gear
Dial Hub
Support Casting
Bushing Assembly
Worm
Worm Gear Shaft
Large Bearing
Small Bearing
Inner Clamp
Outer Clamp
Cam
C a m Support
Lever
Grommet
P e d e s t a l Clamp Assembly
Table
Table Spring
Table Screw
Table Nut
Table Stop
Level
Counter Weight
Grommet
Leveling Foot Assy
Knob, F r o n t Panel
Knob/w Crank
Dial
Large Bevel G e a r
Small Bevel Gear
Handle
Fisher Scientific Co.
Instruments, Apparatus, Furniture and
Chemicals for Laboratories.

Manual No. 15041


Revised and Published 6-73
Effective with Serial No. 1 17
Seventh Issue

073-006
Litho in U.S.A.