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Chemical lnstrumerrtation
Edited by GALEN W. EWING, Seton Hall University, So. Orange, N. J. 07079 feature
XXXVIII. Refractometers
1. E. MALEY, Anacon, Inc., Ashlond. Mass. 0172 1
Types of Refractometers
Two types of refrectometers are com-
mereially avaihhlo, the di&renlial and
the critical-an.& I n the differential
refractometer, a light beam is transmitted
through a partitioned cell which refracts
the beam a t an angle which depends on the
difference in refractive index between the
sample liquid in one part and a standard
liquid in the other. Differential re-
fraetometers can be accurate to 1 X 1 0 '
units of refractive index difference between
the two liquids. In the critical-angle
refractometer the light incident on the
surface of the solntion changes sharply
from reflected lo t,rsnsmitted light a t a
critical angle. Several different versions
of the differential and critical-angle re-
fractometers are commercially available Figure 3. Differential refractometer.
far the laboratory and for continuous
process monitoring.
solution, this instrument may he used for strument, and n calibration curve of com-
A. Critical-Angle Refractometers highly opaque samples and various murky position versus refractometer reading is
solutions and suspensions, as well as plotted. Various rangas and nominal
Critical-anglo refractometers measure transparent samples.
the refractive index of liqoids a t an inter- values of refractive index can be ac-
face with air or, more commonly, with a commodated by the various instruments,
glass prism. As shown in Fig. 2, a light,
8. Differential Refractometers and some of them will provide any range
beam is directed a t the interface a t down to An = 10" a t any nominal value.
Differential refractometers are in- The minimum detectable index dif-
various angles in the vicinity of the critical tended primarily for the analysis of
angle. The critical angle is the angle from ference for sustained periods of operation
liquid mixtnres. They are applicable to is '/la of the range or lo-' units of re-
the perpendicular a t which the beam any mixture whose refractive index is a
changes from light transmit,ted into the fractive index for the best of the new
single-valued function of the composition; instruments. I n the most precise in-
liquid to light totally reflected a t the this includes nearly all simple binary sys-
liquid surface. At angles smnller than the struments sensitivity is limited t o this
tems. In refractive index meltsotwnents. value mainly by mechanical deformation
critical angle the light is transmitted into
the liquid. The critical angle depends not of the instrument caused by changes in
only on the solution composition hut also ambient and sample temperature.
on the prism material. The refractive The principle of the differential re-
recognized and precautions are taken lo fractometer is very simple. First con-
index can he calculated from: minimize the temperatwe effect. sider thepnsgsge of a beam of light through
i, = arc sin (n,/nJ Each of the instmments employs n. a simple right-angled prism of refraotive
sample cell through which :h light beam is index n, and s. second prism of idenlical
where
transmitted. The beam is refracted composition in close proximity to the
i, critical angle in radians within the
= t,hrmgh an angle whose size depends on first but with t,he refracting mrfaces re-
elass t,he refractive index difference between versed (Fig. 3a); the beam will p a s s
n, =index of refraction of the glass the sample and x standard which con- through the combination without net
nr = index of refraction of the liquid stitutes a part of the cell. The angle of
refraction is measured with a photoelectric refraction. If, however, the second prism
The significant fesbure of a crilical is made of material having a very slightly
pickup. different refractive index from the first.,
angle refractometer is that, i t measures the
refract.ive index s t the swface of a soh-
The aoolieabilit~vof a refractometer to n + dn, then the beam will be deflected
tion. Since surface reflection requires no through t,he angle B (Fig. 3h). I f dn is
penetration of the light beam into the (Conlintwd on page A470)
Process Refradometers
Since the early dsys of World War 11,
recording refractometers have been used to
monitor thepurity of butadieneandstyrene
streams. In addition, process refractom-
eters have been used to control the
blending of these two feed components in
the manufacture of GR-S rubber. The
refractive indices of styrene and hutadiene
are approximately 1.5434 and 1.4120,
respectively. A change of 0.1'% is easily
detectable by continuous refractometry.
Applications in the food industry in-
volve materials xnch as soya bean and
cottonseed oils having refractive indices Figure 6. Sulfuric acid, hydmchioris acid.
INLINE REFRACTOMETER
BLOCK DIAGRAM
Figure 8. In-line refroctometer. steel tubing or pipe, the process fluid does
not have t o be removed from the pipeline
t h e pipe. I n operation, a light heam from d.. transmitted t o some remote instru-
a n incandescent light hnlh is directed
through a lens and out the back of t,he (Continued on page A476)
The A b b i Refroctometer
The range of the Abbi: is normally
1.3000 to 1.7000, the maximum pre-
cision attainable being 0.0001. I t reads
the refractive index directly, and requires
only a drop of sample. White light is
used, and to prevent R colored, indistinct
boundary between the light and dark
fields two direct-vision prisms, called
Amici prisms, are placed one above the
other between the objective and eyepiece
of the telescope. These are constructed
of different varieties of glass and are so
designed as not la deviate a ray of light
of the wavelength of the sodiwn D line.
Rays of other wavelengths are, however,
deviated, and by rotaiing the Amici
prisms it is possible to comteraet the
Carbonated Beverages
Figwe 14 ilhtstrates a typical installa-
tion of an in-line refractorneter a t a
carbonated beverage plant. Here the
unit measures the amount of sugar in the
beverage after it has been completely
carbonated and just prior to bot,tling.
~ ~
..
Some other anolications of interest are
measurement of glycerine-water mixtures,
formaldehyde-methanol mixtues, syn-
SWL"
Figure 15. Applerouse control system.
bhetic rubber processes, and a variet,y of well as standard lubricating oils in refin-
instant food products, inclnding coffee eries has been done for many years with
and tea. An extremely important applice- laboratory refractornetem. It was felt
tion is in the hydrogenation of fats and that it would be impossible to analyze
Figure 14. Carbonated beveroge plant
oils. The analysis of these materials as
(Continued on page A484)
PEFRACTOMETER
ha I
RECOVERY
BOILER
ASH GREEN
cracking-unit feed stock, mcaswement of FROM EVAPORATOR )%( LlOVOR
octane numbers of gasoline, and detection
of interfaces in pipelines. I t provides
all immcdiate, simple analysis witho~lta
very elaborate, highly complicated,
sampling system. In :L nnmber of eases Figure 16.
-
Paper mill recovery boilers.
the elimirmtian of s sampling system in
itself mare than justifies installation of the
refractometer.
The field of in-line measurements is simplify the complicated analysis mea- plied to direct in-line measurement,.
becoming more and mare import,ant with surements it is virtually essential in many In summary, refractometers have been
the advent of completely controlled aoto- rases that the unit become a n in-line mea- used fur almost 100 years for the measure-
matic processes. Figwe 15 shows an suring device. By measuring within t.he ment of liquid solutions. Contin~lalim-
automatic control system for applesauce actnal process, many of the problems of provements are being made, particularly
processing and Figure 16 a. monitor for a analysis are eliminated nnd the unreliabil- in the continuous process type refractom-
paper mill recovery bailer. To obtain ity of complicaled sampling systems is re- eters. No significant changes have been
true automatic control in many eases, moved. The in-line measurement pm- made in laboratory refractometers in
analysis must be extremely fast and ex- vides x very high degree of reliability and recent years but the advent of solid state
tremely reliable. The more important s very high speed of response. I t is anti- circuitry probably will ennse some major
factors in analysis instrumentation are cipated ihat in the next few years we will changes in these instrnments in the very
reliability and simplicity. I n order to see more and more analyt,icel devices ap- near futnre. llefractometers are reliable,