Main Journal of the American Chemical Society Supercritical Fluid Chromatography with Packed Columns:  Techniques and Applications....

Supercritical Fluid Chromatography with Packed Columns:  Techniques and Applications. Chromatographic Science Series, Vol. 75. By Klaus Anton (Novartis Pharma AG, Basel, Switzerland) and Claire Berger (Ciba Specialty Chemicals, Inc., Basel, Switzerland). Mercel Dekker:  New York. 1998. ISBN 0-8247-0013-9

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Volume:
120
Language:
english
Journal:
Journal of the American Chemical Society
DOI:
10.1021/ja975676h
Date:
November, 1998
File:
PDF, 17 KB
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11542 J. Am. Chem. Soc., Vol. 120, No. 44, 1998

Additions and Corrections

Additions and Corrections
Rules of Stereoselectivity in Tandem Oxidative Polycyclization Reaction with Rhenium(VII) Oxides [J. Am. Chem. Soc.
1998, 120, 9076-9077]. SANTOSH, C. SINHA, EHUD KEINAN,
AND SUBHASH C. SINHA*
Structure 17 in Scheme 5 should be as shown below.

JA985526M
10.1021/ja985526m
Published on Web 10/26/1998

Book ReViews
Supercritical Fluid Chromatography with Packed Columns:
Techniques and Applications. Chromatographic Science Series,
Vol. 75. By Klaus Anton (Novartis Pharma AG, Basel, Switzerland)
and Claire Berger (Ciba Specialty Chemicals, Inc., Basel, Switzerland). Mercel Dekker: New York. 1998. ISBN 0-8247-0013-9.
Klaus Anton and Claire Berger have assembled a gem of papers
from 10 countries and 15 different sets of authors. The book brings
researchers up to date in the area of supercritical fluid chromatography
with packed columns (pSFC, packed column supercritical fluid chromatography). The range of papers in the book provides two thrusts.
These include using pSFC as an analytical and preparative tool and
providing basic information, data, and examples for commercial use.
Further the book should provide a basis for further research and
development.
Each individual chapter (15 chapters) is well written and can stand
alone in addressing a particular facit of pSFC. The book is filled with
the advantages, disadvantages, constraints, comparisons, and limitations
of pSFC. Discussions include the role of pSFC, solubility measurements, packing material, selectivity and retention, variations in stationary and mobile phases, modifiers, detectors, pressure control, and a
number of applications.
Chapters 1-13 focus on analytical and preparative techniques while
Chapters 14 and 15 discuss commercial and industrial applications. In
many cases the discussion of analytical and preparative techniques can
form the basis for commercial applications.
Analytical and Preparative Techniques: The supercritical fluid used
as the mo; bile phase is carbon dioxide in pSFC, and carbon dioxide is
sometimes used in a mixture with methanol as a modifier to increase
solubility of polar hydrocarbons.
Chapter 1 provides a well-documented method for measuring
solubilities. Applications include measurements of vitamin K1, β-carotene, and a series of xanthines. The second chapter provides a
foundation for any researcher wishing to use pSFC as an analytical
technique. It is a combination of literature review and practical
experience. A discussion of analytical and preparative pSFC is
discussed in Chapter 3 along with a discussion of the advantages over
high-pressure liquid chromatography, HPLC. While many applications
of pSFC use ultraviolet detectors, the demonstration of the use of
evaporative light scattering detection is the topic of Chapter 4.
Chapter 5 is a discussion of the use of packed capillary columns in
SFC, allowing for higher column efficiencies in longer columns and
lower mobile phase rates. Diesel fuel samples were examined as one
example of this technique. An interesting discussion of selectivity and
selectivity tuning can be found in Chapter 6. The effect of organic
modifiers on high molecular weight organic compounds is the subject
of Chapter 7. Modifiers include heptane, methylene chloride, tetrahydrofuran, ethanol, propionitrile, acetone, 1-propanol, methanol, acetonitrile, and nitromethane. The transition from a method where density
is the most important factor to a liquid type of behavior depends on

the chemical nature of the modifier extending the range of straight
carbon monoxide pSFC to subcritical fluid chromatography, subFC.
The title of Chapter 8 is Chiral Chromotography using Sub- and
Supercritical Fluids. These fluids are advantageous in providing a
higher resolution of enantiomers in shorter times than HPLC particularly
in applications to pharmaceuticals and other analytes in preparative
separation. Rationally designed chiral stationary phases are discussed
in Chapter 9. These are useful for the separation of enantiometers.
pSFC is used in the development of drugs in Chapter 10 and polymer
additives in Chapter 11. Both chapters provide the advantages of pSFC
to the development process. Chapter 12 provides an application of
pSFC to the fractionation of polymer homologs. The structure and
properties of these uniform polymers can then be determined. The
authors of Chapter 13 demonstrate the role of pSFC in the ever
increasing accuracy of environmental analysis. Examples include
determining the levels of PCB in cod liver oil and soil.
Commercial and Industrial Applications: The last two chapters, 14
and 15, focus on production scale applications of pSFC.
Chapter 14 is titled Preparative Supercritical Fluid Chromatography.
These authors view pSFC as a production tool within preparative pSFC.
They discuss their pilot plant unit separating piperonyl butoxide and
its potential scale-up. Chapter 15 is titled Production of High Purity
n-3 Fatty Acid-Ethyl Esters by Process Scale Supercritical Fluid
Chromatography. This author, Peter Lembke, discusses the scale-up
for production of eicosapentaenoic acid (EPA) from fish oils. After
performing laboratory and pilot scale testing of this separation, he uses
the acquired data to perform a preliminary plant design analysis. The
results of the analysis indicate that, for this high-purity separation of
EPA, the pSFC process is cheapter than a similar HPLC process.
The book can be recommended to those chemical scientists looking
for alternative analytical techniques, particularly environmental scientists
attempting to enlarge their ability to determine trace substances.
Supercritical fluid chromatography provides an analytic technique
intermediate between gas chromatography and high-performance liquid
chromatography. Chemical engineers looking for a new separation
method will find basic information for production of specialty chemicals
using pSFC.
I hope the editors can provide future leadership in this field by
preparing a second monograph dealing with the potential for pSFC in
commercial process applications. A follow-up volume will contribute
to the growth of pSFC in industrial applications.
Harry Knickle, UniVersity of Rhode Island
JA975676H
10.1021/ja975676h