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SP1202 116-120 Wilks Thomsen Guest Editorial Infrared Solves Some Unusual Problems for the Film Industry Paul A. Wilks aving recounted in in a while there is a mix-up We happened to have a my previous guest in the shop and we lose Thunder Dome ATR attachment editorials some of the track of the film orienta- supplied by Thermo Spectra- past history of the tion, which could lead to a Tech (Madison, WI), which was HHevolution of infrared disaster if film with the being evaluated for another instrumentation and how it has wrong orientation is used purpose. We found that there begun to move out of the labo- in further processing. was such a concentration of IR ratory into the real world of ma- “Can you provide us energy at the upper surface of terials analysis (1, 2), I thought with some sort of equip- the spherical element in the it might be interesting to de- ment that will quickly tell Thunder Dome that one needed scribe three analytical problems us which side is which?” only to press a piece of the film ” . Our extruder was functioning erratically, and we have produced Paul A. Wilks several hundred rolls of film that may or may not have the correct is president of Wilks Enterprise (140 Water Street, South Norwalk, thickness moisture barrier. How can we check these rolls to determine CT 06854) and a member of which has the correct barrier thickness and which doesn’t?” Spectroscopy’s editorial advisory board. He can be contacted by phone that came to us from the plastic Although each material had on the spherical surface with at (203) 855-9136 and film industry and discuss how characteristic infrared absorp- one’s thumb and there would be by e-mail at pwilks@ infrared techniques solved tion bands, taking transmission a strong positive reading from wilksir.com. them. spectra would obviously not the infrared filtometer if the Wilks Enterprise was ap- help in film orientation. Attenu- sealant surface was down, and a proached several months ago by ated total reflectance (ATR) much weaker reading from the a manufacturer of plastic films sampling would, however. The other side. A reading takes less for packaging with the following trouble was that the one usable than 30 s. The film orientation problem: band in the sealant spectrum problem was solved and the in- was rather weak and conven- frared filtometer, with spherical “We manufacture a film tional horizontal ATR sampling ATR surface on the “thumb that is basically polyethyl- methods, even with the clamp sampler” is now in use in the ene with a sealant layer on set at fairly high pressures, did film processing plant. one side. Trouble is, you not show significantly different A short time later, another can’t tell which side is absorption at the wavelength of film maker approached us with which by just looking at the the characteristic sealant band. another problem: film. Although we take (We managed to break a ZnSe great care in our processing ATR plate in the evaluation to make sure we know process!) “Guest Editorial” which side is up, every once continued on page 120 116 Spectroscopy 17(12) December 2002 www.spectroscopyonline.com TUTORIAL Walther Gerlach and the Foundations of Modern Spectrochemical Analysis Volker Thomsen The author discusses the life and sometimes-overlooked work of German scientist Walther Gerlach. Volker Thomsen many compilations of scientific thereof are generally conceded is senior biographies. to begin with the work of Bun- applications For most scientists, the name sen and Kirchhof (1). Their 1860 scientist at Gerlach brings to mind only the publication (3) showed that NITON classic Stern–Gerlach experiment qualitative chemical analysis was Corporation, 900 Middlesex of atomic physics. It is not gener- feasible. One year later, the au- Turnpike, ally appreciated that Gerlach, a thors proved this rather conclu- Building 8, first-rate experimental physicist, sively by discovering two new el- Billerica, MA transformed the spectrographic ements — cesium and rubidium 01821, and an technique from a qualitative or — by spectroscopic analysis. adjunct faculty member in semiquantitative tool into a quan- Attempts to produce quanti- physics at Mount titative method of instrumental tative analyses using photo- Wachusett chemical analysis. He did this by graphic film (spectrograph) Community introducing the internal standard rather than the human eye College, Gardner, method, which remains central to (spectroscope) ran into grave MA 01440. He can be reached modern spectrometric analysis, problems, caused by the number via e-mail at whether the excitation is by of variables associated with the vthomsen@ niton.com. lmost without excep- tion, all precision It is not generally appreciated that Gerlach, quantitative analysis AA using emission spectra a first-rate experimental physicist, transformed is based on some variant of the internal-standard principle the spectrographic technique from a qualitative first enunciated by Walther Gerlach (1). or semiquantitative tool into a quantitative It seems strange, therefore, that so little is known today method of instrumental chemical analysis. about the founder of modern optical emission spectrochemi- cal (OES) analysis. Aside from arc/spark or the more recent in- intensity of the spectral lines an excellent biography in Ger- ductively coupled plasma (ICP). produced by a given material. man (2), little else is available; These included excitation his name appears in a 110-word Historical Development source instability and variable entry in Encyclopedia Britannica, Although spectroscopy has a photographic film sensitivity. Vol. 5, 15th Edition (1994), but long history going back to New- Several researchers achieved he is not noted in any of the ton, the chemical applications semiquantitative results in the December 2002 17(12) Spectroscopy 117 Tutorial Table I. Improvement in precision using internal standardization. homologous and fixation spectral line pairs. Gerlach was the first to call spec- Spectral line pair Intensity analyte Intensity ratio tral line pairs homologous if they (%RSD) (%RSD) worked well together to compensate for Si(I) 251.6/Fe(I) 281.3 0.82% 0.18% changes in excitation conditions. It is 0.85% 0.22% important to note that not all line pairs Cr(II) 289.8/Fe(II) 273.0 0.44% 0.17% of an analyte and matrix are homolo- 0.95% 0.24% gous. For example, an ionic line of the Mn(II) 293.3/Fe(II) 273.0 0.72% 0.28% matrix element does not couple well 0.98% 0.28% with an atomic analytical spectral line. What defines a pair of homologous late 19th and early 20th centuries. The against the concentration of the stan- spectral lines? No set of necessary and work of W.N. Hartley in Dublin, Ire- dards to produce a working (calibra- sufficient conditions exists, as more re- land, is noted, as his 1882 study appears tion) curve. search in this area is required. We can to have been the first systematic study Two types of internal standard lines state, however, that their excitation po- of the change in spectral line intensity can be used: tentials must be similar; or, in the case with concentration. He also made the ● A weak (nonsensitive) spectral line of of ionic lines, their combined excitation first quantitative spectrographic analy- the major component of the sample. and ionization energies must be similar. sis (determination of beryllium in This approach is most common with Beyond this, we must turn to experi- cerium compounds [1]). arc/spark spectrometry. mentation. Several types of tests may be De Gramont in Paris, France, was a ● A strong (sensitive) line of an ele- performed. driving force for the development of ment such as strontium or yttrium The basic definition of homologous spectrographic methods as a quantita- that is not initially present, but added spectral line pairs, due to Gerlach, is tive technique for chemical analysis (1). to the sample. This approach is that they compensate for changes in the In the United States, Meggers, Kiess, generally used today in ICP excitation energy. The simplest test to and Stimson attempted to bridge the spectrometry. determine if a line pair meets this crite- gap to quantitative analysis in their How does this technique work? Let a rion is to make measurements at differ- 1922 paper (4). However, Meggers and measurement of a spectral line of an ent power levels. ϭ co-workers relied on constant excita- analyte, A, be IA 1000 counts. The in- Homologous spectral line pairs im- tion conditions, extremely difficult to ternal standard spectral line, measured prove the precision of analysis, gener- ϭ produce experimentally at that at the same time, yields ISTD 10,000 ally by a factor of about three or four. ϭ time (5). counts. The intensity ratio is IA/ ISTD Table I shows some examples. A counter In Germany, Gerlach made the real 0.10. Now a second measurement is example is W(I) 400.8/Fe(I) 360.8 in ϭ breakthrough to quantitative analysis. made at some time later: IA 950 tool steel where the %RSD of the ana- ϭ In 1929 Gerlach and co-worker Eugen counts and ISTD 9500 counts. Note lytical spectral line alone was found to Schweitzer introduced the method of that despite the change in measured be 0.75% and that of the intensity ratio internal standards along with the con- values, the intensity ratio remains the 0.70%. This test is simple to perform. cepts of homologous spectral lines and same. This simple yet powerful tech- It has also been found that homolo- fixation pairs (6). Although his name nique compensates for both short and gous line pairs improve the calibration seldom surfaces in today’s spectro- long-term changes in the measuring in- and show less interelement (matrix) ef- chemical literature, it was very promi- strument, the spectrometer.
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