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The NIR Spectrum - Vol. 1 No. 4 (2003) Page

New Applications for NIR Exist All Around You

Bruce Campbell, President CNIRS

Are you thinking of de-veloping a new application for NIR? Perhaps you are not at all sure if there would be a correlation that would permit a decent calibration to be derived? Don’t worry. Try it anyway. If you knew beforehand that the appli-cation would not work, you would have to know ALL there is about the relation-ships. I don’t know about you, but I have yet to meet anyone who knew all about the spectro-chemical prop-erties of a sample set. Therefore, unless you are that rare breed, there is a good probability that some sample attribute will have some effect on the spectra. And when anything affects the spectra, it is fair game for development of an application. There is one parameter that doesn’t directly affect individual spectra. I am thinking here of time. Nu-merous applications exist where time is important. Consider, for example, curing paint. Is curing time impor-tant? Many paint companies think so. Some even adver-tise “fast curing paints.” In addition, a major challenge for paint companies is to de-crease the amount and type of volatile organic com-pounds, VOC. Wouldn’t

scans of paint samples show the degree of curing? But you ask, “How can a thin film of paint have enough of a path length to enable a significant sig-nal-to-noise level to be achieved?” Well, why not have the light beam impinge at a decided angle to

the surface of the paint, only a few degrees from zero, with the detector also at the same angle but al-most 180 degrees different? This may increase the path length through the paint while giving a longer path length for the space imme-diately above the paint. This latter path length may enable the detection and quantification of the gases coming off the paint - sort of a remote sensing ar-rangement. If this specula-

tion really would works, as I think it would, a new application would be garnered. The usage would

complement present methods of testing and may even sup-plant them. Would such an approach be feasible? There are prob-lems that would have to be overcome, such as how to en-sure a long enough path length for the gases when there could be appreciable scattering of the light beam from the paint layer. The method of applying the paint layer may introduce variables. The thickness of the paint layer could be very important. And on and on. But consider the rewards of overcoming Cont’d Page 7 — President’s

http://www.pharm.uky.edu/asrg/cnirs/cnirs.html http:/www.idrc-chambersburg.org

Your Personal Source of Information Vol. 1 No. 4 — 2003

Contents

Presidents Message ................................ 1 Editorial Board ......................................... 2 Governing Board/Committees .................. 3 Lab-Process Monitoring .......................... 4 Chambersburg Meeting .......................... 8 Spotlighting Italy ...................................... 9 Computer Tips ....................................... 11 Member Activities .................................. 12 Remembering ........................................ 13 Bibliography ........................................... 14 Membership Guidelines ......................... 15 CNIRS Awards ....................................... 16 FOSS NIR Systems ................................ 17

http://www.pharm.uky.edu/asrg/cnirs/cnirs.html

http://www.idrc-chambersburg.org

The NIR Spectrum - Vol. 1 No. 4 (2003)

Editors Fred McClure, Editor-in-Chief [email protected] NC State University USA Kerry Walsh, Editor [email protected] Central Queensland University Australia Jing An, Editor [email protected] Saskatchewan Wheat Pool, Canada North America David Funk, Editor [email protected] Szent Istvan University, Hungary Europe Yuki Ozaki, Editor [email protected] Kwansai Gakuin University, Japan Asia Celio Pasquini, Editor [email protected] State University of Campinas, Brazil South America

Associate Editors Nils Berding [email protected] Bureau of Sugarcane Exp. Stations Australia Darrell Donahue [email protected] University of Maine USA Roberto Giangiacomo [email protected] Istituto Sperimentale Lattiero Caseario Italy John Guthrie [email protected] Centre for Food Technology Australia Andy Hale [email protected] NC State University USA Charles Hurburgh [email protected] Iowa State University USA

Beverly Jacobson [email protected] American Crystal Sugar Co. USA Michael Rode [email protected] Zeiss, Ltd. Germany Gary Ritchie [email protected] US Pharmacopoeia USA David Semmes [email protected] Proctor and Gamble USA Theo van Kempen [email protected] NC State University USA Lois Weyer [email protected] ATK Elkton, LLC USA Qian Wang [email protected] Bruker Optics USA Hong Yang, [email protected] A & T University USA

Editorial Advisors Woody Barton [email protected] USDA/ARS USA Bruce Campbell [email protected] Avian, Inc. USA Emil Ciurczak [email protected] NIR Consultant USA Jim Drennen [email protected] Duquesne University USA Bill Fateley [email protected] Kansas State University USA Deborah Habernicht [email protected] Montana State University USA Susan Foulk [email protected] Guided Wave, Inc. USA

Rob Lodder [email protected] University of Kentucky USA

From the Editors

We are continually looking for ways to improve The NIR Spec-trum. This issue contains some changes that have been taken from the comments of members. Boundaries of text boxes, which in the past have been a little gaudy, have been reduced in size in hopes that they enhance, rather than de-tract from, the content (or text). You will note that the boundary lines in this issue are thinner and there are fewer of them. The font of the articles have changed, making the text more readable on a screen. Susan Foulk, Editorial Advisor, pulled together information on “fonts for web-pages.” Font research suggest that the font you use should be (1) in keeping with objectives, (2) easy to read on a computer screen and (3) be widely available. Basically, there are only two types of fonts — serif and sans serifs. Serif fonts are those that have fine cross-lines at the extremities of the letter. San serif (“san” is French for “without”) are fonts that don’t have serifs. Times New Roman is a common serif font. Arial is typi-cal of sans serif. The author of this font data (Mario Sanchez in The Internet Digest) talks about four fonts: Arial, Times New Roman, Verdana and Georgia. Of the five, Sanchez says that only Georgia and Ver-dana qualify for on-screen reading. He ranked Verdana exceptional “because its wide body makes it the clearest font for on-screen reading, even at small sizes.” En-joy.

Fred McClure –EIC

Editorial Board


Governing Board Executive Committee Bruce Campbell, President [email protected] Howard Mark, Secretary [email protected] Susan Foulk, Treasurer [email protected] Fred McClure, Past President [email protected]

Members at Large Darrell Donahue [email protected] David Hopkins [email protected] Beverly Jacobson [email protected] Emil Ciurczak [email protected] Don Dahm [email protected] Gary Ritchie [email protected]

Committees Awards Dave Hopkins, Chr. [email protected] Bibliography Fred McClure, Chr. [email protected] Gary Ritchie, Hong Yang and David Semmes Conference (IDRC) Lois Weyer, Chr. [email protected] Sandra Kays, Phil Williams, Emil Ciurczak, Roumiana Tsenkova and Qian Wang Constitution and Bylaws Dave Ryan, Chr. Woody Barton, Don Dahm, Susan Foulk and Howard Mark Inter-Society Program Development Woody Barton, Chr [email protected]. Yuki Ozaki, Richard Streamer, Qian Wang Celio Pasquini, Howard Mark and Christian Paul Membership Darrell Donahue, Chr. [email protected] Susan Foulk, Howard Mark, Fred McClure and Brian Osborne

Governing Board/Committees

International Diffuse Reflectance Conference — 2004 Attendance is limited to the first 150 regular conferees. To reserve your place, with no obligation,

and to receive a copy of the subsequent circulars, Email: [email protected] To retain your place, registration must be received by July 1, 2004.

Further information is on the web at: www.IDRC-Chambersburg.org


NEAR INFRARED SPECTROSCOPY for

LABORATORY PROCESS MONITORING

Celio

Pasquini

Instituto de Química Universidade Estadual de Campi-

nas (UNICAMP) Caixa Postal: 6154, CEP: 13084-

971 – Campinas – SP – Brazil Near infrared (NIR) spectros-copy is an analytical technique that surpasses requirements for monitoring most industrial proc-esses. It is used to monitor many of the critical quality parameters in the petroleum, paper, textile, brewing, and polymer industries — not to mention the numerous documented applications in the field agriculture where NIR spec-troscopy continues to help achieve the highest standards in production, including supplying rationale for making objective de-cision in precision agriculture. However, the number of ap-plications where NIR spectroscopy is implemented for monitoring of laboratory processes is compara-tively low. By laboratory proc-esses, we mean processes occur-ring in chemistry laboratories as part of research or processes in-volved in the development of a product or industrial process, all still at the bench stage. Numerous physical-chemistry processes can be documented, such as reaction monitoring[1-7], distillations[8], lyophilization[9] or even more complex separation processes, such as thin layer chromatography[10,11] and molecular self-assembling[12].

All these processes, commonly carried on in a chemistry labora-tory, have been monitored by NIR spectroscopy with the inherent advantages shown by that spectral region, namely: almost universal capability for the detection of C-H, N-H, S-H and O-H containing com-pounds, fast and reliable spectrum acquisition (enabling a multivari-ate approach to be applied to process monitoring), remote sens-ing through optical fibers and probes, reduced requirements for sampling and sample conditioning, including solid, liquid and gaseous samples, not to mention the econ-omy of NIR equipment. The use of NIR spectroscopy for monitoring reactions in real time in the laboratory is frequently described in the literature. Some-times, perhaps by chance, selec-tivity for a given product or re-agent is achieved and a single clear and unique spectral feature can be used to follow the reaction. However, this is not the case for most applications and, perhaps, this fact led to the sub-utilization of NIR to tackle the laboratory re-action-monitoring problem. Char-acteristics of the NIR spectra, all bursting with information, are such that, many times, the spec-tral set obtained can not be ana-lyzed without the use of chemom-etrics. The use of already common chemometric multivariate data treatments can help to correlate the total spectra to concentration or property changes taking place inside a reaction flask. The ap-proach has become even more attractive by the introduction of rapid-scan Fourier Transform (FT) and Acousto-optic Tunable Filter (AOTF) instruments. Both tech-nologies can acquire NIR spectra over a wide spectral range in a matter of seconds, even when co-addition is implemented to im-prove the signal-to-noise ratio. An

AOTF spectrometer can, for in-stance, record a full NIR transmit-tance spectrum from 1100-2500 nm in about 50 ms. Therefore, real time monitoring by NIR of fast-changing laboratory proc-esses, including fast chemical re-actions, has become a reality. The very fact that NIR spec-troscopy does not destroy the sample is another attractive fea-ture, permitting the monitoring of small quantities of (sometimes very expensive) products and/or reagents employed in specialized chemical reactions. Micro-reactors can be designed and reactions can be easily monitored, achieving a low cost/benefits ratio in the de-velopment of synthetic routes. Arriving at a suitable NIR sys-tem for laboratory process moni-toring is often simpler than with other quantitative analytical meth-ods. This comes from the fact that the system under study in the laboratory presents some well de-fined characteristics, mainly re-lated to its composition and ex-pected composition changes. This facilitates the production of stan-dards for qualitative and/or quan-titative purposes, when necessary. The example below illustrates the use of fast scanning instru-ments along with chemometrics to enhance the extraction of infor-mation from laboratory processes. Based on the results of a re-cently published paper, the poten-tial of NIR spectroscopy for moni-toring laboratory processes can be evaluated[8]. Two aspects are relevant, namely: the fast scan-ning speed of modern instruments and the use of chemometrics to simplify the qualitative and quan-titative interpretation of the huge amount of spectral data obtained. The feature that allowed the continuous monitoring of the com-position of a condensate in a dis-tillation device was very simple.

Lab-Process Monitoring


It consisted of a glass flow cell molded as a small funnel and a siphon (inner volume of 150 mi-croliters) adapted at the end of the condenser. Two optical bun-dles were implemented to carry the monochromatic radiation from an AOTF crystal to the flow cell and from there to the detector (transmission mode). The scan speed of the AOTF-based instru-ment allowed for 50 spectra in the region from 800 to 1800 nm (nominal resolution of 2 nm) to be obtained in about 4 s. Thus, the condensate was monitored in real time at 4 s intervals. Figure 1A shows spectra of the distillation of a mixture of hexane and toluene. Although many chemometrics tools could be em-ployed to access the information in the data set, Principal Compo-nent Analysis (PCA) revealed a substantial amount of information about the characteristics of the distillation process. Figure 1B, for instance, shows the scores for the first and second principal compo-nents of the data set shown in Fig-ure 1A. Spectra of pure sub-stances present in the binary sys-tem and of some mixtures in dif-ferent proportions have been added to the spectra of the con-densate before the whole set was submitted to PCA. Therefore, the bi-dimensional graph of scores allows one to observe the compo-sition of the condensate during distillation. This type of data can be used to control the optimiza-tion of the distillation process. Ob-serve that the changes in the spectral features in the NIR spec-tral region (though possible to be identified in the original spectra set of Fig. 1A) can not be directly associated with condensate levels. Therefore, chemometrics plays an invaluable and important role in making NIR spectroscopy feasible for monitoring laboratory proc-esses.

The contribution of chemomet-rics is more evident where com-plex systems are under investiga-tion and composition information is scarce. That is the case with the distillation of gasoline, a complex mixture of hydrocarbons, which in Brazil, must contain about 25% of ethanol. Figure 2 shows the scores for the first and second PCs ob-

tained by monitoring the conden-sate coming from the distillation of 10 samples of regular and 2 sam-ples of adulterated gasoline. Spec-tral differences between regular and adulterated gasoline are ob-served in the spectra of the origi-nal samples (without distillation). However, the information obtained by monitoring the distillation by

Figure 1. A, Collection of spectra obtained during real time monitor-ing of a distillation of a mixture of toluene and hexane (50:50%, v/v). B, scores obtained by PCA of the distillation data of the mixture in A. The PCA was carried out after five spectra of mixtures of toluene and hexane and the pure substances, obtained directly in the flow cell, were incorporated into the distillation spectra set shown in A. The bold symbols in B represents the scores values for the five spec-tra obtained: a, pure hexane; b, binary mixture containing 70% (v/v) of hexane; c, a 50:50% mixture; d, mixture containing 70% (v/v) toluene and, e, pure toluene.

a

b

c

d

e



NIR is far more effective in distin-guishing between the two adulter-ated samples and in locating the fractions of condensate responsi-ble for the greatest differentia-tion. Additionally, the information obtained can help in the identifica-tion of the adulterant employed. Furthermore, since distillation is a common practice in laboratories

dealing with petroleum deriva-tives, the simple adaptation of commercial distillation devices to NIR spectroscopy increases the quality and quantity of information the process can generate. The examples above help to illustrate the potentials of NIR spectroscopy for monitoring small-scale laboratory processes. The same approach could be used to follow synthesis reactions, devel-opment and optimization of indus-trial process at the bench stage as well as other physical processes carried out in the laboratory. An important question is: What are the steps involved in convert-ing a laboratory-bench NIR spec-trophotometer to a useful full- scale laboratory process monitor-ing system? First of all, it would

be necessary to establish the real-time requirements for monitoring any given process. Fast processes, such as distillations, may require the use of fast instruments, like FT- and AOTF-based technologies. On the other hand, the use of very simple instruments based on NIR-LEDs, diode arrays or optical inter-fering filters may be put into prac-

tice for dedicated applications if some expertise in the design of optical instrumentation is avail-able. The next step is to adapt the spectrophotometer by selecting the correct approach to probe the process. Reflectance and transmit-tance measurements may be util-ized. Usually, optical fibers consti-tute the best way to look at the process, allowing the spectropho-tometer to be placed far away from the reaction, thus, avoiding possible damage to the instru-ment. Sometimes, the process apparatus can be assembled in the optical path of the NIR instru-ment. It may become necessary to construct a suitable cell, the interior of which contains the process activity being observed.

Once the hardware has been set, the system is ready to gener-ate data. At this point, another question becomes relevant: Does the software supplied along with the spectrophotometer allow for the acquisition of data dictated by the process? The software must allow the user to set the time in-terval and frequency of data ac-quisition. Ideally, an external (hardware) trigger must be pre-sent to synchronize spectral data acquisition with the beginning of the process, thus, improving the versatility of the monitoring sys-tem. High storage capacity on per-manent media should be available in the controlling computer. Most spectrometer-control pro-grams do not allow the user to develop auxiliary software, caus-ing the user to resort to external software for further analysis. This limits the potential for real-time (or automatic) control of the process by utilizing feedback volt-ages based on recorded spectral data. Teamwork between the technical supporters of the spec-trophotometer manufacturer can be extremely helpful to overcome problems encountered. Instrument manufacturers could assure many more success stories if they would simply supply more details of pos-sible control signals and software source code. Last, but a no less relevant step, is the extraction of informa-tion from the acquired spectra. Sometimes the process can be fol-low by looking only at specific wavelengths that present the rele-vant information. However, in most cases encountered in near infrared spectroscopy, the infor-mation will be distributed in tiny spectral variations present throughout the spectrum. This is where chemometrics comes into play. Chemometrics can be used for extracting subtle information useful for determining the process

Figure 2. Scores distribution for the first two PCs for ten regular sam-ples of gasoline (black circles) and for two adulterated samples (open triangles and circles). The arrows indicate the direction of tempera-ture/time increase during the distillation of regular gasoline.

-0,08 -0,06 -0,04 -0,02 0,00 0,02 0,04

-0,04

-0,03

-0,02

-0,01

0,00

0,01

0,02

0,03

0,04

PC2

PC1



variables of interest. Data collected during a proc-ess usually will generate three-way data sets (time x wavelength x absorbance/reflectance) contain-ing the information about the process evolution. Depending on the type of information required for evaluating the process, the chosen data treatment should ex-tract both qualitative or quantita-tive information from the spectral data. Chemometric software pack-ages can be purchased that will supply the more usual procedures of multivariate regression and data analysis. PCA, as shown in the example above, is an impor-tant multivariate technique pro-ducing qualitative and even quan-titative information about labora-tory processes. This last step, not surprisingly, constitutes a major bottle neck for the use of NIR spectroscopy in laboratory process monitoring. These drawbacks can not be at-tributed to the lack of chemomet-rics software packages but, per-haps, to a culture where univari-ate-based process monitoring is still predominate. Processes carried on by a re-search or development laboratory can make impressive use of the new NIR instrumentation that is now capable of generating real-time data even for fast processes. When the capacity of NIR spec-troscopy for gathering information from the progress of a laboratory process is combined with the in-terpretative capacity of modern multivariate data treatments, cer-tainly a powerful tool is created whose full potential is still waiting to be explored by scientists re-sponsible for developing chemis-try in many of their specialties. Neither NIR spectroscopy nor chemometrics can be ignored when facing these issues.

REFERENCES 1. Bjorsvik, H.R., Appl. Spectrosc., 50, 1541-1544 (1996). 2. Lachenal, G., Pierre, A. and Poisson, N., Micron, 27, 329-334 (1996). 3. Hammond, J., Kellam, B., Mof-fat, A.C. and Jee, R.D., Anal. Comm., 36, 127-129(1999). 4. Geladi, P. and Aberg, P., J. Near Infrared. Spectrosc., 9, 1-9 (2001). 5. Geladi, P. and Forsstrom, J., J. Chemom., 16, 329-338 (2002). 6. Blanco, M. and Serrano, D., Analyst, 125, 2059-2064 (2000). 7. Dupuy, J. Maazouz, A. and Benali, S., E-Polymers, 018 (2003). 8. Pasquini, C. and Scafi, S.H.F., Anal. Chem., 75, 2270-2275 (2003). 9. Brulls, M., Folestad, S., Sparen, A. and Rasmuson, A., Pharm. Res., 20, 494-499 (2003). 10. Ciurczak, E.W. and Murphy, W.R., Spectrosc. Int., 3, 39-44 (1991). 11. Yamamoto, H., Yoshikawa, O., Nakatani, M. and Maeda, T, Appl. Spectrosc., 45, 1166-1170 (1991). 12. Iwahashi, M., Suzuki, M., Katayama, N., Matsuzawa, H., Czarnecki, M.A., Ozaki, Y. and Wakisaka, A., Appl. Spectrosc., 54, 268-276 (2000).


President’s—Cont’d from Page 1

those limitations. Other measure-ments of the effect of time could be envisioned. Many calibrations have been developed for various aspects of fruit. Have any been have been developed that incorpo-rate the effect of time and storage conditions? And wouldn’t it be nice to take your spectrometer to a restaurant to test the freshness of the fish you ordered? (Actually, the restaurant owner may want to have such a test run on the fish delivered to the restaurant.) And if you want to try a really, really far out one, what about analyzing the near infrared spec-tra from stars? Not to find out what the stars composition is, but to discover the types of material that is absorbing some of the en-ergy transmitted through space. One would have to work with vari-able light-source intensities, but possibly with only seven types of stars, the variations in source may not constitute an insurmountable problem. In any new application, let your imagination free. I think you would be surprised at what appli-cations you can develop. If you do, this newsletter would be a good place to let others know about it, sort of a prepublication tool.

FOSS NIR Systems, Inc. Sponsors Vol 1 No 4

We thank FOSS NIR Systems for sponsor-ing this issue of The NIR Spectrum. Their inter-est, cooperation and support of The Council for Near Infrared Spectroscopy over many years has enabled CNIRS to offer technical education and training in NIR technology throughout the world. The team spirit exhibited by all our spon-sors is deeply appreciated. We in CNIRS look forward to exciting times ahead for NIRS.

POSTNOTE Dr. Celio Pasquini is Full Professor in the Chemistry Institute of the State Uni-versity of Campinas (UNICAMP), SP, Brazil, where he has taught and con-ducted research in analytical chemistry since 1982. He is coordinator of an “Instrumentation and Automation Group” whose research goals include: Lab automation, development of analyti-cal instrumentation, development of optrodes, flow analysis and NIR spec-troscopy. He and his wife, Dulcineia, have two children, Aline and Diego.


12th International Diffuse Reflectance Conference (IDRC)

Wilson College, Chambersburg, Pennsylvania, USA August 8-13, 2004

First Circular

Attendance is limited to the first 150 regular confer-ees. To reserve your place, with no obligation, and to receive a copy of the subsequent circulars Email: [email protected] To retain your place, registration must be received by July 1, 2004. For further information visit the CNIRS/IDRC websites—addresses are on the front of this newsletter. As an exciting first, the IDRC will sponsor a Joint USP/FDA Symposium/Workshop on PAT, August 7-9. The Aug 9 (Monday) session of the conference will be part of the Sympo-sium. Scheduled Plenary Sessions:

Sun Aug 8: Opening of Conference (7:00 PM) Mon Aug 9: NIR in the Pharmaceutical Industry (8:00 AM & 7:00 PM) Tue Aug 10: NIR in the Food and Agricultural Industry (8:00 AM & 7:00 PM) Wed Aug 11: Medical Applications of Diffuse Re- flectance Spectroscopy (8:00 AM & 7:00 PM) Thu Aug 12: Emerging Uses of and Recent Ad- vances in Diffuse Reflectance (8:00 AM) Banquet (6:00 PM) Fri Aug 13: Attacking Typical Chemometric Problems in NIR Spectroscopy (8:00 AM) Adjourn (noon)

Poster Sessions: Each Conferee will have the oppor-tunity to present a poster. The setting will include a 10 minute oral presentation, as well as the more traditional poster format. Certain posters will be selected for 15 minute presentations at the plenary sessions. Software Shootout: There will be an opportunity to work on a sample set prior to the conference. The shootout is contest designed to help new NIR users know if their approach is “state of the art” and for experienced people to show off a bit. Prizes will be awarded. Vendor presentations: Vendors who support the conference are entitled to give brief technical (non-commercial) presentations. For details see above web site.

Optional Sessions: A variety of tech-nical sessions will be during the

afternoons

Recreational Opportuni-ties: The facilities of the college campus and lo-cal golf courses are available. A well-developed recreational

program is always impor-tant because this confer-

ence attempts to meet the needs of the total person. The

facilities of the college campus and local golf courses are available for use in

the free/non-session afternoons." Dining and Lodging: Meals at the college cafeteria and accommodations in the college dormitories (non-air conditioned) are included for a regular con-feree.

Costs: The conference attempts to keep costs down to make atten-dance attractive for those paying their own way. The cost for a regular attendee will generally be less than $500.

Don Dahm, Chr. 12th IDRC

Chambersburg Meeting — www.idrc-chambersburg.org

Don Dahm


The Dairy Science Institute (DSI) was established in 1871 by a Royal decree to integrate sci-ence and cheese making. It is lo-cated in Lodi, 36 km from Milan, toward the Southeast in the Padana plane. In 1923, the Insti-tute bought a farm to carry out research on products from milk to cheese. Today the Insti-tute is organized in four departments (Applied Techniques, Chemistry, Microbiology & Enzy-mology, and Technology) in a cen-tral unit of 800 m2, a 40 ha farm with 55 milk cows and a 600 m2

processing pilot plant. The Institute has a large library, open to the public, containing major national and international journals and magazines of in-terest for the entire dairy field. There are 2250 books, FIL-IDF Standards and Docu-ments, Bulletins and Symposia Proceed-ings. In addition, the archive contains docu-mentation of historical interest. Nineteen perma-nent staff with the aid of 27 support units, including contract per-sonnel, scholarship recipients, ser-vices, etc, conduct research at the DSI. The Institute cooperates with various universities and hosts stu-dents doing graduate research, including both Masters and PhDs. The Institute, under the lead-ership of Roberto Giangiacomo since 1998, is mainly funded by the Ministry of Agriculture and Forestry under research programs approved by the national Council of Agriculture. Sources for addi-tional funding include special pro-jects financed by the Ministry of

Agriculture, the National Council of Research and/or The Ministry of Scientific Research. The Institute also receives funding from the European Union. Proceeds derived from selling farm products, offi-cially contracted analyses, certifi-

cates, etc. are an important source of financing as are re-search contracts with private in-dustries, protection Consortia, Re-gions, Mountain Communities, etc. Roberto began his NIR studies in

1976 working on fruits, vegetables and cheese. Through his studies of captured preservation processes and product quality and other the nondestructive attribute of NIRS technology, Dr. Giangiacomo be-gan to push the research enve-lope. He quickly became infatu-ated with the water matrix in bio-materials; he became keenly in-terested in the changes that take place when sugar and salt absorb moisture. In the early beginnings, Roberto closely cooperated with American NIR teams to expand his

knowledge and develop a focus for his future efforts. Since 1985, when Roberto started his work at the Dairy Sci-ence Institute as Director of the Applied Techniques Department (ATD), the development of fast

reliable procedures and analytical techniques in response to Italian pro-ducers and consumers needs became the driv-

ing force for his research. It is im-portant to note that, due to the Italian industrial structure, a sys-tem that involves a lot of small and medium enterprises, the use of NIRS technology within dairy

sector, particularly at the industrial level, is still rather limited. This situation seems to be changing as noted by increased requests to develop NIRS applications. The Applied Tech-niques Department has a the expertise to develop NIRS applica-tions that are easy to apply, that produce accurate results, and offer the intrinsic ad-vantages of being nondestructive and fast. The department is also working to-

wards standardizing procedures through collaborative studies for the optimization and validation of analytical methods at national and international levels, participating in FIL-IDF (International Dairy Federation) activities. The Applied Techniques Lab now has three fulltime specialists, two scientists employed on multi-annual contracts, one part-time graduate student and several un-dergraduate students from Food Science and Technology. For a long time, the only in-

Spotlighting Italy

The Institute of Dairy Science Lodi, ITALY

Back Row (L-R): Michele Curti, Nicoletta Sinelli, Stefania Bar-zaghi, Roberto Giangiacomo, Katia Cremonesi Front Row (L-R): Tiziana M.P. Cattaneo and Claudia Giardina


Spotlighting Italy strument available in the labora-tory was a dispersive spectrome-ter (InfraAlyzer 500, Bran+ Luebbe), an instrument that was primarily operated in the reflection mode. Results from early studies helped to convince the dairy sec-

tor of the benefits of NIRS, result-ing in additional investments in NIR research for improving tech-niques, instrumentation and chemometrics. New instrumenta-tion, derived from active coopera-tion with instrument manufactur-ers for realizing common research goals, has greatly increased the labs output. The lab currently has three NIR spectrometers, ranging from the original disper-sive unit (see above) to a modern FT-NIR spectrometer. One o f more interesting challenges con-fronting researchers in the ATD is: How can milk coagulation be monitored in real time using NIR spectroscopy. Over the last four years, several collaboration stud-ies were carried out in order to identify the influence of substrate, temperature, pH and rennet on spectral data of whole milk. Data were optimized using multiple chemometrics. The feasibility of models was verified by transfer-ring lab results to pilot scale in-volving an FT-NIR spectrometer

optically coupled to the sample stream using fiber optics. Roberto and his staff regularly attend international events, such as International Diffuse Reflec-tance Conference (USA) and the International Conference on Near

Infrared Spectroscopy (ICNIRS). Dr. Giangiacomo, along with his team and cooperators, were host to the 9th ICNIRS held in Verona in 1999. Next year the Dairy NIR team will promote an Italian event, NIR-Italia 2004, in coop-eration with the Chemical Depart-ment of the University of Ferrara, in order to further stimulate Ital-ian NIR users to actively exchange experiences.

Current Projects within the ATD Include:

> Improving chemometrics knowledge > Monitoring the coagulation process > Studying the interaction of water and solids during processing > Evaluating the influence of physical treatment on milk quality > Comparing NIR-MIR spectral information > Applying the 2D-COSS for data interpretation > Verifying the authenticity of products > Using NIRS to predict textural characteristics of cheese for determining shelf life

Contacts: Dr. Roberto Giangiacomo Email: [email protected] Dr. Tiziana Cattaneo Email: [email protected]

POSTNOTE

The Institute of Dairy Science (IDS), located in Lodi, Italy—a town of 45,000 citizens—has a mission comparable to USDA centers, with the exception that IDS operates, unlike USDA, as a non-profit entity that receives partial funding from the Italian Ministry of Agriculture. Dr. Roberton Giangiacomo has lived and worked there for almost 20 years. A man that cannot be separated from his pipe, Roberto enjoys rowing with his children (two sons and one daughter), attending the opera and movies. All three children are equestrians.


Computer Tips

Computer Tips in Issue #3, 2003 talked about backing up. Of the 10 most important rules for successful computer operation, the first three are (1) backup, (2) backup and (3) backup. The other rules are of little consequence if the first three are violated. Computer equipment suppliers have doled out storage media very cleverly—a little bit at a time. First, there was the 3.5” diskette that maxed out at 1.4 megabytes (Mb) of storage. Interestingly, you now have to ask Dell and Gateway to install one if you want it; no longer is it a standard peripheral. Then came the I/Omega disk that would backup 100 Mb of informa-tion. In parallel with the 3.5” disk-ette and the I/O disk was the de-velopment of CD recorders. The CD recorder was boon to storage, allowing you to store about 500 Mb of data, even though you could, in the beginning, use the storage media (the CD/ROM disk) only once. Now the DVD provides backup space in the range of 4 Gb (gigabytes). The problem with DVD technology is that there is more than one standard, making it unreliable as a universal exchange tool. As mentioned in Backing Up . . . Big Time (Vol 1 No 3, The NIR Spectrum, p. 11, 2003), one of the most effective ways to backup lots of data is to implement an ex-ternal hard-disk drive, via. a USB port. This article reported a 40 Mb disk backup system that cost slightly more than $100. It is a self-contained unit, having its own power supply—making it neces-sary to provide two cables: (1) An A/C power cord and (2) a USB to FireWire connection cable. You do not have to carry around an inline

power supply; there is only one little box 2” H x 6” W x 10” D. (You need to read about it to un-derstand how neat it is.) The sys-tem is universally and automati-cally recognized by any computer, with a USB port, running WIN-2000 and WIN-XP. It is truly a plug-and-play device. With a unit like this, you will never need to burn a CD, buy a Zip disk, or use a 3.5” diskette again.

Windows-XP, as well as previ-ous versions of windows, have backup commands—of course. Yet, these tools leave something to be desired—especially when it comes to visualizing the backing up process. In addition, if the challenge is to make a duplicate of a directory or directories, confir-mation of equivalency is difficult at best with WIN commands. Not so with the program call “Beyond Compare (BC),” by a company called Scooter Software (just search for “Beyond Compare” with your favorite Browser. BC is a utility for comparing things, things like text files, fold-ers, zip archives, and FTP sites. It can be used to manage source code, keep folders in sync, com-pare program output and validate CD copies. BC can create a snap-shot of a live (your internal hard drive that you use ever day) direc-tory structure and compare it against a live copy at a later date. It runs under Windows 95 through XP. A salient feature of BC is it visually helps you analyze differ-ences in detail and carefully allows you to reconcile those differences, either manually or automatically. It allows you to do this by display-ing the internal working data and external copies in two side-by-side windows on the screen. Every-

thing is there, right down to the file level. Thus, if you reorganize the working directory the differ-ence from the copy appears clearly color-coded on the screen. You do not need to backup every file each time you do a backup. You back up only the changes. You can download a free trial-version of BC from the internet. If

your experiences are like the one I had, you will own your copy be-fore nightfall. After the parame-ters are fixed, a single click of a button will allow you sync left-to-right, or, if you are bring another computer in sync, a click of an-other button allow you to sync right-to-left. File maintenance and informa-tion display is an area lacking in MS operating systems file-support utilities. For example, why is it that MS does not display the size of directories when it would be so easy to do—just add up the sizes of files and there is. Utilities are available for file maintenance. There are two of which you should take note: (1) Disk Info Utility (DIU) and (2) Bulk Rename Utility (BRU). Both are available for a small donation via the WebSite of Jim Willsher: http://www.jimwillsher.co.uk/Site/Main_Intro.asp These two utilities are easy to learn and very helpful. DIU will give you the size of both Directo-ries and files (shown in the left window)—depending what part of the disk you have open in the left window, plus it will do other things. BRU is very particularly useful for renaming the files from your digital camera. Have Fun Computing!

Fred McClure, EIC

Backing Up . . . Big Time: Part 2

File Syncing

File Maintenance


Member Activities

SPEAKERS BUREAU The Individuals below are available to give presentations and/or training courses.

Speaker: Donald A. Burns, PhD

Title: Basic Near-Infrared Spectroscopy Title: Catch ‘em with NIR Title: Improve Your Presentations with Animated Power Point. Email: [email protected]

Speaker: Bruce Campbell, PhD Title: There is more to chemometrics than NIR: How to decrease the error rate in calibrations Email: [email protected]

Speaker: Robert A. Lodder, Professor

Title: In Situ Spectroscopic Cleaning Validation Title: Theoretical and Experimental Characterization of a Near- Field Scanning Microwave Microscope Title: Remote Hyperspectral Imaging of Endolithic Biofilms Using a Robotic Probe Title: Hyperspectral Techniques in Analysis of Oral Dosage Forms Title: Detection of Lipid Pool, Thin Fibrous Cap, and Inflamma- tory Cells in Human Aortic Atherosclerotic Plaques by Near-Infrared Spectroscopy Email: [email protected]

Speaker: W. F. McClure, Emeritus Professor

Title: Speaking/Writing Technically Title: Electronics for Spectroscopist Title: Fundamentals of NIR Technology Email: [email protected] ============================

*The Speakers Bureau is a service of CNIRS to its members. If you are a member of CNIRS and would like to participate, send picture and titles by Email to Fred McClure, Email: [email protected].

CNIRS AWARDS Committee Calls for Nominations

Sponsored by Unity Scientific of Pur-cellville, Virginia, the Gerald S. Birth Award is the most prestigious prize awarded by The Council for Near Infra-red Spectroscopy.

See Page

16 For Details

Dr. Gerald S. Birth


Remembering

Emil Ciurczak

Peter Griffiths Jing An, Canada

Bruce Campbell

Susan Foulk

Jim Drennen Bill Fateley (Mars)

Professor Yanlu Yan, China

USDA, Athens, Ga

The Confederates

Int’l Attndees—IDRC2002

A. Stepniewski (Poland), S. Morimoto (Japan), S. Kawano, (Japan)


THE CNIRS BIBLIOGRAPHY OF

NEAR INFRARED TECHNOLOGY

Introduction The Council for Near Infrared Spectroscopy (CNIRS) maintains a bibliography of near infrared literature (including patents) that covers all forms of NIR technology from 1800 to present. This bibliography, called the CNIRS Bibliography (CNIRS-B), is in three chronologically-ordered libraries (1800-1995, 1996-Present and Patents-(1971-2002). The CNIRS-B contains more than 23,000 citations. It is the single most complete bibliography of NIR technology in existence. The bibliography comes with a licensed copy of End-Note® (for Windows 98/NT, 2000 and XP) that allows the user to do logical searches of any or all fields and recover citations accordingly. Furthermore, the real power of the new NIR bibliography, coupled with EndNote, comes from the fact that user-selected citations can be inserted directly into publi-cations, reports and/or documents prepared with Microsoft Word 97 or higher. Some citations (about 65%) have ab-stracts that will help the user evaluate the references before they are inserted into documents. Some abstracts had to be omitted to avoid copyright violations. As a rule, when the paper discusses technology other than NIR that keyword is included in the keyword list, for example, Raman, photo acoustics, chromatography, pigments & dyes, visible, etc. Sometimes, words (like water and moisture) are used inter-changeably in the abstracts; so, the user may want to search similar words of interest. When doing any search we always encourage users to search title, keywords and abstracts for word(s) of interest. CNIRS-B libraries are furnished on CD only. Potential users of the CNIRS database may want to view the EndNote web page at

http://www.endnote.com/ More than 200,000 researchers, scholarly writers, stu-dents and librarians use EndNote to search online biblio-

graphic databases, organize their references and create bib-liographies instantly and automatically. Instead of spending hours typing bibliographies or using index cards to organize their references, they do it the easy way - by using EndNote! In addition to accessing the CNIRS bibliography, you can search bibliographic databases on the internet, organize ref-erences in databases and create your own personal bibliog-raphies. COST of the Bibliography The CNIRS-B is a product of the Council for Near Infra-red Spectroscopy, a non-profit organization. Monies from the sale of this bibliography are used to promote the advance-ment and practice of near-infrared spectroscopy. CNIRS is an all-volunteer organization. There are no paid staff. Costs of CNIRS-B are as follows: Bibliography complete with EndNote $820.00* Yearly Updates $220.00

======================== *Members of educational institutions get a 50% discount *Members of CNIRS get a 15% discount Copies of the CNIRS Bibliography may be obtained by sending your purchase order along with a check to: W. Fred McClure Emeritus Professor & Chairman Bibliography Committee Council for Near Infrared Spectroscopy North Carolina State University PO Box 7625 Raleigh, NC 27695-7625 TEL: 919-515-6764 FAX: 919-515-7760 Email: [email protected]

*************************************** Please make the check payable to "The Council for Near Infrared Spectroscopy.” Having no paid staff, we are unable to justify an account manager. We have over 67 systems in the hands of satisfied customers, and we have yet to receive a complaint. We stand behind this product and will replace defective disks free of charge. *Effective April 1, 2003. Price subject to change without notice.

CNIRS Bibliography


Membership Classifications & Dues

The Council for Near Infrared Spectroscopy is the only national society solely dedicated to the ad-vancement and practice of near-infrared spectroscopy. The Constitution & Bylaws of the Council stipulates the following member-ship classification (Please NOTE: Dues are per calendar year. All member-discounts are based on payment of dues in full for the

calendar year(s) that apply.) (1) Regular Members — $20/yr: Regular Members shall be persons engaged in the study or use of spectroscopy and/or interested in the objectives and scope of the Coun-cil. (2) Student Members — $5/yr: Student Members shall be full-time undergraduate or graduate students engaged in the study or use of near infrared or related forms of spectroscopy and/or interested in the objectives and scope of the Council. Student members shall not vote or hold office in the Council. (3) Sponsoring Members — $250/yr: Sponsoring Mem-bers of the Council shall be corporate bodies or private companies actively interested in promoting the objectives of the Council on a national and/ or international scale. (4) Honorary Members — Dues Paid for Life by the Council: Honorary Members shall be persons who have made exceptional contributions to near infrared spectros-copy and have been voted into their membership by the Governing Board. No more than two (2) Honorary Mem-bers can be named in any fiscal year. (5) Emeritus Members — Dues Paid for Life by the Council: Emeritus Members shall be persons who have contributed to near infrared spectroscopy and now have retired from active scientific endeavor. Emeritus Members may be proposed by a Local Section, through their Gov-erning Board Delegate, by the Membership Committee, or by the Executive Committee. Upon receiving a simple ma-jority vote at a Governing Board Meeting, the member will be conferred the status of Emeritus Member.

Membership Benefits Benefit #1: Participate in the only professional member-ship society in the world dedicated to the enhancement, practice and expansion of near-infrared spectroscopy. Benefit #2: Members of CNIRS in good standing (dues paid) for 2003 and 2004 will receive a 15% discount on their registration fee (room and meals excluded) at the International Diffuse Reflectance Conference at Chambers-burg, PA in August, 2004. In addition, they will receive a

15% discount for all short courses taken at the IDRC. Benefit #3: Members of CNIRS in good standing will re-ceive a 15% discount on the CNIRS bibliography, a data-base that contains more than 24,000 citations, plus over 900 patents. This discount is not in addition to the 50% discount awarded to educational institutions and/or their faculty. Benefit #4: Members may join in the planning of short courses, technical sessions and other activities at the In-ternational Diffuse Reflectance Conference, Chambers-burg, PA held biannually in the even numbered years. Benefit #5: Help sponsor and administer awards: Hon-orary Membership and the Gerald S. Birth Award . Benefit #6: Join with other members at social receptions held at selected conferences every year. Benefit #7: Members in good standing will have access to The NIR Spectrum, the CNIRS Web-NewsLetter. CNIRS has two websites:

http://www.pharm.uky.edu/asrg/cnirs/cnirs.html

http://www.idrc-chambersburg.org

Both WebSites have discussion forums accessible from the above home pages.

Membership Dues: Corporate — $250/yr; Regular — $20/yr; Student—$5/yr. The Governing Board of the CNIRS invites you to join with them in the furtherance of NIR technology throughout the world. Your participation is invalu-able to the future of this Society.

Dues Payment Guidelines:

Payment of membership dues to the CNIRS may be made in one of several ways. Bank transfers require an additional $10 US to cover transfer fees charged by banks. We accept payment via check drawn on a US bank or a Canadian bank written in US dollars. We also accept US and International money orders in US dollars. Either form of payment should be mailed to:

Susan Foulk, CNIRS Treasurer 128 N. Deer Run Drive

Lincoln University, PA 19352

Payment by credit card may be made by sending your credit card information either by mail, FAX or by phone to the treasurer. If sending information by FAX or phone the number is (610) 255-5979 between the hours of 7am and 9pm EST. You may use the Membership Form on the next page, indicating card type, card number, cvv2 code (3 digit code on the back), expiration date, name on the card and the zip code where the bill is normally sent.

CNIRS Membership


CNIRS Membership / Awards Membership Form:

Name: _________________________________ Company: ______________________________ Address 1:______________________________ Address 2:______________________________ City: ____________ State/Province: ________ Zip/Post Code: _________________________ Phone: ________________________________ Email Address: _________________________

Credit Card Information:

Card Type: ___ VISA, ___ MasterCard ___ Discover or ___ Amex Card Num _____________________________ CVV2 code (3 digits on back) ____________ Expiration Date (Mo/Day/Year): __________ Name on Card: ________________________ Billing Zip/Post Code ____________________ ————————————————

- Darrell Donahue, Membership Chairman

Email: [email protected]

CNIRS AWARDS:

Call for Nominations The Awards Committee is requesting nominations for three award categories: (1) The Gerald S. Birth Award for outstanding innovation in diffuse reflection or diffuse transmission spectroscopy is con-ferred by the Council for Near-Infrared Spectroscopy (CNIRS) and sponsored by Unity Scientific Corp. in memory of Gerald Birth. The late Dr. Birth was the founder of the International Diffuse Reflectance Conference (IDRC), now sponsored by the CNIRS. He also made many contributions to the instrument technology re-lated to diffuse reflectance. It is fitting that the Unity Scientific Award carry Dr. Birth’s name, to honor him and to recognize his numerous innovations and contributions to the area of diffuse reflection, transmission and interaction instrumentation. This award recognizes a specific accomplishment in advancing the Art and Science of Near Infrared Spectroscopy by a senior research scientist. All scientists performing research in Diffuse Reflection Spectroscopy or in Diffuse Transmission Spectroscopy in the visible, NIR or mid-IR regions are eligible for the award. The award-winning work must have been published between 01-Mar-2002 and 28-Feb-2004. The awardees (practicing or retired) may be (or have been) affiliated with industry, academia, govern-ment, or have another suitable affiliation. Undergraduate stu-dents, graduate students, and post-doctoral researchers are not eligible. The awardees must be alive and able to present the award-winning work at the IDRC, 07- to 13-August-2004. This prestigious award entails an honorarium of $2000.00 as well as expenses for his/her travel to the IDRC meeting and for an ac-companying guest, up to $1500. (2) Honorary Membership in the CNIRS: According to the Constitution and Bylaws of the CNIRS: “Honorary Members shall be persons who have made exceptional contributions to near in-frared spectroscopy and have been voted into their membership by the Governing Board. No more than two (2) Honorary Mem-bers can be named in any fiscal year.” Nominations are to be submitted to the Awards Committee. This committee will collect the nominations and supporting documentation that will be passed on the Governing Board for a vote. (3) IDRC Fellowships: Support for students and scientists, who might otherwise be unable to attend the IDRC meeting with-out additional financial aid, is available from the CNIRS. Fellow-ships will cover meeting registration and travel up to $1000. Ap-plicants should submit a resume and brief statement of how they would benefit from attending the Meeting. In addition, individuals selected for support are expected to submit a poster of their work in the Poster Session of the IDRC. Nominations and supporting material, from within the inter-national spectroscopy community at large, for any of the above three awards should be sent to David Hopkins, Chair of the CNIRS Awards Committee, [email protected]. The deadline for all nomination materials to reach the Awards Committee is 30-Apr-2004.

- David Hopkins Awards Chairman

Email: [email protected]

Please complete this form and mail, FAX or Email to: Ms. Susan Foulk, Treasurer, CNIRS, 128 N. Deer Run Drive, Lincoln Univer-sity, PA 19352. Email: [email protected]. Payment made by check or money order should be mailed to the above address.

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Documents

foss nir systems

made exceptional contributions

diffuse transmission spectroscopy

monitoring laboratory processes

real time monitoring

laboratory process monitoring

emil ciurczak

ddonahue umche