Report

REVOLUTION
chemistry is an ancient
science (1-6). For more than a
Analytical
hundred years, it has played an
important role in chemical education. The
curriculum used to teach analytical chem-
istry has, of course, changed dramatically
over time, from the use of books that
described the use of gravimetry, flame
tests, and bead tests to computer simula-
tion of actual analytical Instruments and
experiments. Understanding the origins
of the analytical curriculum is essential as
educators debate how it should change to
meet the needs of today’s students. In this
Report, the evolution of analytical chemis-
try into the 20th century is briefly traced
to lay the foundation for discussing the
evolution of the modern curriculum and
where it might be headed.

In the beginning
The tools and basic chemical measure-
ments of analytical chemistry date back to
early recorded history. The chemical bal-
ance is of such early origin that it was as-
cribed to the gods in the earliest docu-
ments found. The use of standard weights
is traced to the Babylonians in 2600 BC,
who considered them so important that us-
ers were supervised by their priests. Met-
als and alloys were also used in ancient
times, and the perceived value of gold and

To determine in what direction the analytical
chemistry curriculum should go, it’s
important to look back at its origins
silver was probably a major incentive for
acquiring analytical knowledge. In the
fourth century BC, the purity of gold
was determined from the extent of the yel-
low marks it made on a touchstone.
Gary D. Christian
University of Washington

532 A Analytical Chemistry, September 1, 1995 0003 2700/95/0367 -532A/$09.00/0

-

1995 American Chemical Society

©
IN QUANTITATIVE ANALYSIS
The first wet test appears to have been
described by Pliny the Elder (AD 23-79),
who noted that if copper sulfate was adul-
terated with iron sulfate, the extract of gall-
nuts turned black. During the Middle
Ages [ca. 470-1470), alchemists began to
assemble the body of knowledge that be-
came analytical chemistry, and growth
continued during the phlogiston era (to ca.
1700) as quantitative chemical relation-
ships were sought.
Robert Boyle coined the term “analyst”
in his 1661 book The Sceptical Chymist, so
he could be considered the creator of
this branch of chemistry as well as the
founder of chemistry as an independent
science. Gravimetric analysis was proba-
bly invented by the German physician-
chemist Friedrich Hoffmann in the 17th
century when he precipitated chlorides
with silver nitrate and sulfates with lime. In
the 18th century, Jons Jakob Berzelius in-
troduced stoichiometric concepts, and
Antoine Lavoisier used the balance to dis-
prove the phlogiston theory by perform-
ing quantitative experiments to demon-
strate the law of conservation of mass,
which earned him the title “father of quan-
titative analysis.” The 18th century also
saw development of chemical microscopy,
flame tests, the blowpipe, bead tests, and
titrimetry.
Joseph Gay-Lussac, Robert Bunsen,
and Karl Friedrich Mohr developed titri-
metric analysis in the 19th century. In fact,
Gay-Lussac developed a titrimetric meth-
od for silver that was accurate to better
than 0.05% and has not been improved
upon since (5). The only major advance in
titrimetry in the 20th century was the in-
troduction of complexometric techniques.
In the first 40 years of the 20th century,
the emphasis on a scientific, rather than an
empirical, approach increased, as did the
emphasis on instrumental measurements to
supplement traditional wet chemistry mea-
surements (2). During this period, several
academic centers of analytical chemistry
emerged, and such notable academic analyt-
ical chemists as C. P. Baxter (Harvard),
E. M. Chamot (Cornell), C. W. Faulk (Ohio
State), N. H. Furman (Princeton), V. W.
Meloche (Wisconsin), M. G. Mellon (Pur-
due), E. H. Swift (Caltech), G. F. Smith (Illi-
nois), H. H. Willard (Michigan), J. H. Yoe
(Virginia), and I. M. Kolthoff (Minnesota)
began to develop analytical chemistry as
we know it today.
The early textbooks
Textbooks on analytical chemistry began
appearing in the 19th century. Karl Frese-
nius published a book on qualitative anal-
ysis (Anletung zur quatitativen chemischen
Analyse) in 1841, followed by a volume on
quantitative analysis (Anletung zur quanti-
tativen chemischen Analyse) a few years
later. In 1894, Wilhelm Ostwald published
an influential text on the scientific funda-
mentals of analytical chemistry entitled
Die wissenschaflichen Grundagen der an-
alytischen Chemie. He was the first to rec-
ognize the role of analytical chemistry in
the development of chemistry as a sci-
ence, and he put forth theoretical explana-
tions of analytical phenomena, including
equilibrium constants. He stated that “An-
alytical chemistry is doomed to continue
occupying a position subordinate to other
branches if analytical chemists do not
stop teaching and practicing analysis
solely as an empirical technique and art.”
Analytical Chemistry, September
WISSENSCIIAFTL1CIIEN GRUNDLAGEN
ANALYT1SCHEN CHEMIE.
M.F-MLSTiUv DAJM1KSTELLT
W. OSTWALD.
LEIPZIG
VERLAG VON WILHELM ENGELMANN
Title page from Die wissenschaflichen
Grundagen der analytischen Chemie.
Frances Sutton wrote A Systematic
Handbook of Volumetric Analysis (or The
Quantitative Determination of Chemical
Substances by Measure, Applied to Liquids,
Solids, and Gases) in 1863. By 1911, the
book had gone through 10 editions (7),
which indicates the rapid changes in volu-
metric techniques during that time. (Re-
member, this was in the days before books
were revised frequently.) The 621-page
10th edition is filled with details on volu-
metric apparatus, specific techniques for
given substances, and titrimetric methods
such as alkalimetry and acidimetry, oxi-
dation and reduction, and precipitation.
The first edition of Stephen Popoff s
Quantitative Analysis lists three reasons
for its publication: “First, to incorporate in
1, 1995 533 A
 Report^
a single book the theory, laboratory in-
structions, problems, and explanations for
the calculations of these problems; sec-
ond, to emphasize the law of mass action
and the theory of equilibrium to quantita-
tive reactions; third, to incorporate some
of the more recent advances in analytical
chemistry.”The second edition, published
in 1927 (8), includes chapters on errors
and compilation rules, electroanalysis,
conductomeric titrations, and colorimetric
methods. Recognizing the importance of
acquiring an understanding of the basis of
a measurement, Popoff states, “The ob-
ject of teaching chemistry in a college or
university is not to turn out mere routine
analytical chemists.”
In their classic 1929 book Applied Inor-
ganic Analysis, W. F. Hillebrand and
G. E. F. Lundell of the National Bureau of
Standards (now the National Institute of
Standards and Technology), stated that
“... there is a great need for the develop-
ment of quantitative procedures that can
be applied to the separation or determi-
nation of substances in complex mix-
..They were referring, however,
tures.
primarily to precipitation procedures.
Colorimetric methods for inorganic
analysis were sufficiently mature by 1921
that F. D. Snell devoted a book to that sub-
ject. The second edition, published in
1936 with C. T. Snell, was expanded to two
volumes and also included organic and
biological methods (9). It contained nu-
merous designs of Duboscq and similar
BALANCING METHOD
Plate of photoelectric colorimeter from
Colorimetric Methods of Analysis.
534 A Analytical Chemistry, September
colorimeters, including a “universal colo-
rimeter” for nephelometric as well as colo-
rimetric measurements, and a Yoe de-
sign for a photoelectric colorimeter.
A classic
The person who unknowingly laid the
foundation for much of the renaissance of
analytical chemistry in the United States
was Nicholaas Schoorl, a professor in the
School of Pharmacy at the University of
Utrecht (The Netherlands), who taught
analytical chemistry and studied the char-
acteristics of acid-base indicators and
derivatives of dilute acids and bases. One
of Schoorl’s students was Izaac Maurits
Kolthoff, who majored in pharmacy rather
than chemistry to avoid the Latin and
Greek requirements of the chemistry de-
partment.
“The main
emphasis should
he on the
fundamental
chemical aspect
Kolthoff became interested in the the-
ory of acid-base indicators (4) and was
greatly influenced by a 1909 paper by
S.P.L. Sorenson on the colorimetric and
potentiometric determination of pH.
Schoorl, a modest man, insisted that Kolt-
hoff publish his early papers under his
own name, and Kolthoff published his first
paper, entitled “Phosphoric acid as mono-
and dibasic acid,” in 1915 (10). He pre-
sented his thesis in 1918 on “Fundamen-
tals of Iodimetry,” a subject he would re-
turn to often. He spent 10 years on the
faculty in the Pharmaceutical Institute at
the University of Utrecht, publishing 270
papers and 3 books before joining the fac-
ulty of the University of Minnesota in
1927. Although Kolthoff officially retired in
1962, he remained active in analytical
chemistry for another 30 years. Kolthoff
himself felt that the transformation of ana-
lytical chemistry into a scientific discipline
came about because of physical and bio-
physical chemistry (4).
1, 1995
The teaching of analytical cnemistiy in
the United States was markedly influ-
enced by the publication of Kolthoff and
Sandell's Textbook of Quantitative Inor-
ganic Analysis in 1936, which did much to
establish analytical chemistry as a sepa-
rate discipline. In the preface, Kolthoff and
Sandell note that “It does not seem to be
generally realized that analytical chemis-
try is one of the fundamental branches of
science.” Their goal was to offer a bal-
anced outline of the theoretical aspects of
inorganic quantitative analysis, noting that
“There appears to be a tendency to exag-
gerate the significance of ‘theory’ at the
expense of practical work in chemical
analysis.” (Kolthoff, of course, is known
for his maxim that “theory guides, experi-
ment decides.” One wonders if he might
have borrowed this from Robert Boyle,
who stated in The Sceptical Chymist that
‘Theories must be supported by experi-
ments.”)
In their first edition, Kolthoff and Sand-
ell emphasized classical procedures, but
"highly specialized" methods (conducto-
metric and potentiometric titrations, gas
analysis, nephelometry, spectrography,
etc.) based on physicochemical properties
were detailed enough to enable the stu-
dent to “appreciate the advantages of such
methods,” The third edition in 1952 still
emphasized the classical techniques (IT).
The authors note that “It might seem
that because of the development of self-
registering instruments and automatic
apparatus, classical analytical chemistry is
becoming outdated. If this idea were cor-
rect, the subject matter of our courses in
quantitative analysis would require dras-
tic revision. In our opinion such a change
is neither necessary nor desirable.... The
main emphasis in beginning courses in
quantitative analysis should be on the fun-
damental chemical aspect.”
Moving into the modern era
There have been several surveys in the
past decade that have summarized the re-
cent evolution of analytical chemistry
and what is covered in modern analytical
chemistry texts (12,13). In preparation for
a symposium on teaching analytical chem-
istry organized by Royce Murray in 1980,
I surveyed 25 major institutions to deter-
mine what was being taught at the under-
graduate level and when.
 In my survey, about 40% of the schools
taught analytical chemistry in the fresh-
man year. The quality ranged from desir-
able, in which analytical faculty taught a
lecture/lab course using a quantitative
analysis test, to undesirable, in which non-
analytical faculty taught a lab only, with
no connection to the freshman lecture
course. Typical freshman or sophomore
analytical courses used texts that cov-
ered gravimetric and volumetric methods,
acid-base equilibria, spectrophotometry
(UV-vis, atomic, IR), potentiometry, and
separations (solvent extraction, basic chro-
matography). Lectures typically covered
these topics, and occasionally ion ex-
change, GC, ion-selective electrodes,
nonaqueous acid-base chemistry, electro-
gravimetry, and fluorescence were dis-
cussed as well.
At the symposium, Murray summa-
rized five major factors that had affected
the teaching of analytical chemistry over
the past decade: employment opportuni-
ties, because the number and complex-
ity of analyses had grown as a result of in-
creased government regulation; in-
creased student interest; increased faculty
appointments; continued grant support
for fundamental research in analytical
chemistry, even though the pressure to
fund applied science had increased; and
the knowledge explosion in fields such as
chromatography and data handling.
The knowledge explosion is the big-
gest problem with which analytical chem-
istry educators must contend, with too
little lecture and laboratory time available
to teach properly. Murray noted that
textbooks have grown more in size and
number of chapters than they have in
terms of conveying knowledge. He pro-
posed that we move a greater portion of
what we customarily call “instrumental
methods" to the sophomore year and re-
move material on the less-relevant titri-
metric and gravimetric methods. There
are those who argue, however, that we
must be careful not to displace a thorough
coverage of conventional equilibrium and
related topics, and that the increased inter-
est in biological and pharmaceutical sci-
ences and the importance of being able to
apply equilibrium methodologies to ex-
periments in these areas underlines the
need for students to receive a firm grasp of
these methodologies.
Table 1. Subjects taught in quantitative analysis lecture
> 90% Significant figures, confidence limits, Q-test, concentration units,
neutralization titrations, buffers, polyprotic acids, primary standards,
complexometric titrations, Ksp. redox titrations, Nernst equation, cell
voltages, potentiometry, pH electrodes, Beer's law
80-89% t-Test, ionic strength, activity coefficient, gravimetry, back titrations,
acid-base theory, salt hydrolysis, a-values, standard solutions, K„
solubility, charge balance, redox equations, reference and other
electrodes, spectrometry
70-79% Error propagation, Debye-Huckel, diverse ion effect, normality,
precipitation titrations, mass balance, formal potential, ion-selective
electrodes, standard buffers, mixture calculations in spectrophotometry
60-69% Sampling, sample preparation, least squares, permanganate and
dichromate titrations, junction potentials, standard addition, atomic
spectrometry, chromatography, ion exchange, GC
50-59% Glassware calibration, iodimetry, derivative titrations, electrogravimetry,
coulometry, solvent extraction, LC, theoretical plates, resolution
40-49% f-Test, Kjeldahl, cerate titrations, polarography and voltammetry, van
Deempter equations
30-39% Correlation coefficients, amperometry, IR, fluorescence, chelate
extractions, capacity factor, TLC, planar chromatography
< 30% Control charts, Gan's plots, anodic stripping voltammetry, spectral
interpretation, ICP spectroscopy, ion chromatography, computer
programming
In 1984,1 conducted a survey (sent to books, the distribution of pages among
175 schools, 95 responses received) to other topics generally was not too differ-
help in revising an ACS exam in analytical ent from that in contemporary texts. How-
chemistry. Respondents were asked to ever, although the earlier texts reflected
check which of a list of 100 topics they what analytical chemists did, current texts
taught in their quantitative analysis course. do less so and seem to have evolved di-
A partial summary of the results is given in rectly from their predecessors with ex-
Table Interestingly, not a single topic was
1. panded coverage of statistical methods
checked 100% of the time. The top 30% of and addition of some instrumental tech-
topics were generally classical methods, niques. Traditional determinations con-
statistics, potentiometry, and spectropho- tinue to be the mainstays of the labora-
tometry. Atomic spectrometry and chro- tory part of the course.
matography were in the next 10%, and more Murray has also documented the con-
specialized electrochemistry and chroma- tent of undergraduate analytical chemistry
tography in the following 10%. The lower courses from the 1950s, when rapid
50% included some higher level instru- changes began as a result of what he calls
mental methods such as voltammetry and “chemical transducers,” devices and
IR spectroscopy. means to convert chemical structure and
Locke and Grossman conducted a sur- composition information into electrical
vey of the curriculum in quantitative analy- and optical phenomena such as spectra,
sis in 1987 and compared their results voltammograms, and chromatograms
with the 1982 ACS exam in analytical (15). He asserts that an appreciation of
chemistry (14). They noted that all the chemical transducers is perhaps the most
popular texts included virtually the same lasting contribution that analytical chem-
topics and that all the schools offered ei- istry plays in undergraduate education.
ther a one-semester or a one-quarter During the period 1930-50, texts cov-
quantitative course. They concluded that, ered basic chemical reactivity and physi-
although lecturers do not feel constrained cal aspects of titrimetry and gravimetry. In
to slavishly follow the emphasis in their the 1960s, spectrophotometry, separa-
assigned texts, the range of topics clearly tions, and electrochemistry were added,
does follow the texts. They compared and coverage of gravimetry decreased.
some earlier texts with modem ones and Although the emphasis on titrimetry has
found that, although there was far greater remained constant over 40 years, cover-
emphasis on gravimetric analysis and ap- age now includes more quantitative
plications of redox titrations in older text- treatment of chemical equilibria, reactiv-
Analytical Chemistry, September 1, 1995 535 A
ity, and use of electrodes as transducers
for detecting end points.
It is clearly pedagogically correct to fur-
ther enhance the emphasis on instrumen-
tal analysis in the introductory-level ana-
lytical course. However, there are road-
blocks to introducing more chemical
transducer materials to the sophomore-
level introductory course: obtaining the
necessary lab equipment, changing the
content of the preceding general chemis-
try course, and deciding what to remove
from the analytical course to make room
for the new material. Therefore, evolution
of the course may rest as much on the
school's (or faculty's) priorities in expendi-
tures as it does on Intellectual progress in
the field or the contents of textbooks. In
addition, the content of the general chem-
istry course must be enhanced to pro-
vide the proper background for introduc-
ing chemical transducer material in the an-
alytical course.
To lead or to follow?
Should standardized exams reflect what is
taught in our curriculum or should they
take the lead in shaping the curriculum?
The Graduate Record Exam (GRE) must
necessarily reflect, to the extent possible,
what is taught, because it is used to test
students' competence for advanced study
based on their knowledge of their under-
graduate curriculum. For several years, I
was a member of the GRE Committee of
Examiners for the Chemistry Test and,
until just recently, there was only one rep-
resentative for analytical chemistry and
two representatives each for organic, in-
organic, and physical chemistry (there are
now two analytical representatives). The
areas emphasized in the exam approxi-
mately reflected the population of the
committee: 15% analytical chemistry, 25%
inorganic chemistry, and 30% each or-
ganic and physical chemistry. The analyt-
ical portion of the exam included the clas-
sical quantitative areas of titrimetry, sepa-
rations (gravimetry and theory and
applications of chromatography), data
handling, statistical tests (t, F, Q, chi-
square). and standards and standardiza-
tion techniques. Instrumentally oriented
topics included basic electronics, electro-
chemical methods, spectroscopic meth-
ods (electromagnetic, mass, NMR), and
radioactivity.
536 A Analytical Chemistry, September
The ACS analytical exam more or less
represents what is taught in quantitative
courses (the topics covered on the 1988
ACS exam reflect the results of my sur-
vey) However, there are those who ar-
. ence in how they approach the problem.
gue that the ACS exam should concen-
trate more on instrumentation to encour-
age instructors and authors to change
their ways.
How should analytical
chemistry be taught?
The question of how to teach analytical
chemistry is a somewhat different one
from what should be included in text-
books or in the curriculum. John Wright
at the University of Wisconsin notes that
the elementary analytical course is proba-
bly pretty good at what it does but Is some-
what outdated. In contrast, the instru-
Itis pedagogically
correct to enhance
the emphasis on
instrumental
analysis in the
introductory-level
analytical course.
mental course has quite a ways to go.
What we need to do is to teach students to
be better problem solvers. Although the
best students can readily handle the tradi-
tional approach of assimilating lecture
notes, doing practice problems, and study-
ing the text, others need to be taught the
skills of thinking scientifically. The prob-
lem is that innovative approaches to de-
velop “mind penetration strategies” re-
quire an increased commitment from both
faculty and students and are inherently
time inefficient.
A successful method developed by
John Walters at the University of Wiscon-
sin (now at Saint Olaf College) uses a
group or team approach in the laboratory.
At Wisconsin, students form teams of
four and work on specific problems that
might be encountered in developing an
experiment. For example, Kw might be
used to calculate solubility losses in a
1, 1995
gravimetric determination. Although stu-
dents may have encountered these calcula-
tions in the lecture portion of the class,
Lhe change in context makes a big differ-
The group approach creates discussion,
participation, and responsibility to the
team, and role playing allows the stu-
dents to experience different sets of re-
sponsibilities (16).
Walters has been innovator in the
an
way analytical chemistry is taught. By us-
ing role playing in the laboratory, he cre-
ates an atmosphere that encourages a
sense of '‘ownership” of the experiment.
Other educators relate the excitement of
recent discoveries, by their own research
group or others, to the students. Discus-
sions of this sort do more to instill in stu-
dents the character of chemistry than does
learning new factual material.
FIA: Mini analytical chemistry?
There sound pedagogical reasons for
are
keeping much of our time-honored curric-
ulum the way it is. However, I would like
to propose (and I admit my bias up front)
introducing a semiautomated, miniatur-
ized, and highly efficient technique into
the quantitative analysis laboratory: flow
injection analysis (FIA). Conceived in the
mid-1970s, FIA has proved to be a versa-
tile tool for performing wet chemical anal-
yses on a microscale level and in a short
Time
: ^
Figure 1. Single-line FIA manifold.
Analog output is in the form of a peak that
starts recording at the time of injection fQ. T is
the residence time corresponding to the peak
height measurement and fD is the peak width
at the baseline.
time frame (17). Although there are more
than 6000 publications on the topic, an
indication of its popularity in the research
community, FIA is not widely used in the
teaching laboratory'.
Ruzicka and Hansen began to incorpo-
rate FIA into the teaching laboratory
shortly after its development as an analyti-
cal technique (18). Since then, equip-
ment has been improved and made less
expensive, and modern computer technol-
ogy has made it easy to automate. Several
suitable laboratory exercises have been
published (19-27). The potential of FIA
in chemical education has been espoused
by several educators (28,29), and the
University of Kansas has received funding
to introduce FIA into its laboratory
courses and those of surrounding col-
leges.
The basic components of an FIA sys-
tem are a pump, an injector, a reaction coil,
and a detector (Figure 1). A peristaltic
pump is generally suitable. Tube diame-
ters are typically 0.5-0.8 mm, flow rates
are ~
1 mL/min, and injected sample vol-
ume is ~
25-100 pL. The carrier stream
into which the sample is injected is unseg-
mented and may contain a reagent that
reacts with the analyte. As the sample is
propelled by the carrier stream, it under-
goes controlled dispersion and mixing
with the carrier, depending on the mani-
fold design, resulting in a concentration
gradient of the sample. The products of
the reaction are monitored by a detector
with an appropriate flow cell, and a tran-
sient peak is recorded in -30 s. Typi-
cally, the height of the peak is measured
and related to the analyte concentration,
although area or width may be used in-
stead. The FIA manifold can be config-
ured in a variety of ways, from a single
channel to multiple channels, so multiple
reagents can be used.
For those who wish to introduce FIA
into the laboratory, a fairly simple manual
system can be assembled, and inexpen-
sive manual and computer-controlled sys-
tems are commercially available. The
manual FIA system shown in Figure 2 con-
tainsa variable-speed peristaltic pump, an
injection valve, aT-connector for a two-
line system, and a reaction coil, and can be
connected to an appropriate flow cell or
detector to perform a variety of experi-
ments. Such a manually operated system
Figure 2. Manually operated FIA instrument.
is preferred for student experiments be-
cause students can get hands-on experi-
ence in its operation.
What can be done with FIA in the quan-
titative analysis laboratory? Spectrophoto-
metric measurements can be performed
in a fraction of the time required for con-
ventional spectrophotometry. In fact, a
comparison of the two can be revealing
to students. In conventional spectropho-
tometry, each sample must be measured
and added to the reagent (s), diluted to vol-
ume, and allowed to react. An aliquot is
retrieved for the manual spectrophotomet-
ric measurement, is disposed of, and the
cuvette rinsed. In addition, large quanti-
ties of reagents are consumed and must
be disposed of properly. In the FIA experi-
ment, a stock solution of one or more re-
agents is prepared and pumped in the flow
system. The sample is loaded into an in-
jection valve (not requiring careful mea-
surement by the student) and injected into
the flowing carrier stream. The measure-
ment is completed in < 1 min. Multiple in-
jections can be readily performed to ob-
tain precision measurements. Beer’s law
still applies in FIA and can be tested. Al-
though the sample is dispersed, the ex-
tent of the dispersion can be determined
by obtaining a steady-state signal with a
large volume of sample or dye that does
not become diluted and so absorptivity val-
ues can be determined.
Analytical Chemistry. September
auteausa
Many reactions measured by spectro-
photometry', such as those in the molybde-
num blue method for phosphate determi-
nation (30), require a significant amount of
time to occur. Because the measurement
conditions of FIA are very reproducible,
the reaction need not be completed, and
the measurements can be precisely per-
formed with the few seconds of reaction
that occurs as the sample is being trans-
ported to the detector. We have actually
performed measurement of an organic
condensation reaction in a nonaqueous
solvent in 40 s that normally requires up to
3 h using conventional spectrophotome-
try (31). For kinetically slow reactions,
stopped-flow measurements with computer-
controlled timing devices for the pump can
be used to measure the rate of product for-
mation, usually in < 1 min.
Solvent extraction can also be per-
formed by FIA (32) by injecting the sam-
ple into an aqueous carrier that merges
with the extracting solvent. These seg-
ments are carried to a phase separator as
extraction into the organic solvent occurs.
After phase separation, the extracted ana-
lyte is carried to the detector. This proce-
dure greatly reduces the volume of or-
ganic solvent that must be disposed of, and
the extraction and measurement are per-
formed very quickly. In addition, because
a closed system is used, students’ expo-
sure to the solvent is minimal.
1, 1995 537 A
 RjjnnJ^i

FLA “titrations” can also be performed
(32). In this method, the carrier is the ti-
trant and contains an indicator. When the
sample is injected, equivalency occurs on
the rising and falling portions of the re-
corded signal when passed through a
mixing chamber; the width of the signal is
proportional to the logarithm of the ana-
lyte concentration. Although this proce-
dure has poorer precision than does vol-
umetric titrations, a wide range of concen-
trations can be measured. FIA can also
be combined with classical coulometric
generation of titrant (33).
For the more adventuresome, the new
versatile technique of sequential injection
analysis (34, 35) can be introduced to
students. This technique replaces the in-
jection valve with a multiport selection
valve. Solutions are sequentially aspi-
rated, under computer control, into the re-
action coil and then propelled to the de-
tector, This advanced experiment would
be suitable for the instrumental analysis
laboratory.
Order your NEW
Pesticide/
Words of wisdom
The quantitative analysis course will con-
tinue to be important in chemical educa-
tion. As Lord Kelvin said, “Unless our
knowledge can be measured and ex-
pressed in numbers, it does not amount to
much." R. S. MuSliken, 1966 Nobel laure-
ate, said, “I think it was in a course in quan-
titative analysis that an appreciation of
the scientific method and its rigors began
really to take hold of me... There were
no shortcuts to beat dear thinking, careful
technique, and endless patience. Finally,
Popoff observed, “The value of quantita-
tive analysis to a student... comes in the
acquirement of patience, neatness, and ac-
curacy" (S).
References
(1) A History of Analytical Chemistry, Laitinen,
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