Some history of LAOS

Detailed historical account of LAOS rheometry can be found else where. I add here only my own interest in obsolete instrument designs.

DAQ from a Weissenberg rheogoniometer R16

DAQ from a Weissenberg rheogoniometer R16 (Bogie 1966)

The history of LAOS as a test condition is as old as that of oscillatory shearing rheometry. The use of Lissajous figure was first proposed as early as 1944.  K. Weissenberg first proposed a harmonic analysis of LAOS data in 1964. In fact it was not easy for early experimentalists to maintain or measure small deformation esp. for complex fluids before necessary technology break through in actuators and transducers (e.g. linear voltage differential transformer, LVDT). LAOS was therefore more frequently reached in the past than in today whenever an oscillatory shearing was performed.

Harmonic decomposition of the LAOS data was done in various way before the age of computer. One way was fitting the data with a Volterra intergral equation of a limited number of orders to find the corresponding high order kernels (which was not a real decomposition).

Solartron advertisement

Solartron transfer function analyser (TFA) advertised on Sci. Am. (1959)

The commercial success of Weissenberg rheogoniometer series evoke the desire to extract higher harmonics from the electric signals. One noticeable idea by Harris and Bogie was using the once-called ‘dynamic analysis’ system, product of Solartron Electronic Groups Ltd. It was in essence a cross-correlation method to obtain higher harmonic information on an analog circuit design. The system consisted of a resolved component indicator (or transfer function analyser, as it was more frequently called) excited by a pair of in-phase / quadratic signals from a mechanical reference generator.

The transfer function analyser technique lasted for as long as one decade on Weissenberg rheogoniometer as its model upgraded from R16 to R18, but bolder try on a computer using FFT was performed in as early as 1971. The analog signal was sampled and input in a signal averager to raise the S/N ratio. From then on, the later development was not hard to imagine: smaller and faster computers coupled with more sensitive and accurate measurement systems.

A major transition occurred, though, from Weissenberg rheogoniometer to the Rheometrics mechanic spectrometer (RMS) series during the 1970s, which also shift the LAOS and harmonic analysis to the new device. The device had a few of new feature compared to the Weissenberg counterpart. First, it directly gave the result of G’ and G”, otherwise the earlier rheologists had to manually calculated from the Lissajous curves. Second, it provided an oven chamber to perform high temperature experiment, a feature not easily achievable with old rheogoniometers. And third, it upgrade the driving system from gears-based to electronic motor††. These features gained a wide acceptance very fast, and ARES soon became a standard of rheometer as well as the platform for LAOS, as the Weissenberg rheogoniometer once had been.

† Interested readers may refer to a technical report of the former Royal Aircraft Establishment in 1964 about a measurement system for amplitude and phase available here, which may give a brief description of the technical status at that time.

†† Interested readers are referred to Rev. Sci. Instrum. 1984, 55, 1675.

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Book review: Principles of measurement systems


Principles of Measurement Systems (Paperback)

By (author) John P. Bentley

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The principles of measurement should have been much more frequently involved than only when we need to customize an instrument. At present, the measuring techniques have completely digitized. The principles we learnt in undergraduate physics experiment class may not applicable now. Before the electronic age, most measuring instruments convert the physical quantity into a pointer-scale indicator where human eyes are required to determine the quantity. For example the thermometer converts the temperature into the height of the liquid in a tube. Even the reflective index, if measured by an classic Abbe reflectometer, was converted into the sharpness of the edge between two blocks of color, also requiring human eyes. Students are trained to read as accurately as possible by eyes in the labs during undergraduate study, but after they enter their PhD projects they practically encounter only modern instruments which display digits on a screen or export ascii text files in a computer. Therefore they easily lost the caution of measurement non-ideality, or they lack the knowledge to care about this.

The modern measuring system starts almost inevitably from sensors, a large class of electronic components, rather than the human eyes. Digits on the screen can of course be consistently read by all people including the physically challenged provided additional techniques. This is the triumph of the electronic age indeed. But the problems do not disappear; they are instead hidden inside the instrument between lines of the electronic circuits. What was once understood in an undergraduate class becomes too technical to explain now. Therefore although we have long entered the electronic age we still skip this part in the undergraduate education. And most graduate students trust the instrument companies very much in their PhD project until the problem becomes explicit. Problems become explicit when we need to design a measurement system customized for a research purpose.

In China there is such a class called like “Principles of Electronic Measurement”. But it is limited in the departments of electronics, electrics, industrial control, automation, etc., out of the sight of the students of physical sciences. But my feeling becomes stronger and stronger that experimental physical research must based on full knowledge about the general measurement principles as well as emerging measuring techniques. Otherwise, the perspectives of scientific research is limited by instrument company instead of pioneered by scientists. I am interested in how widely students in other countries can access this course.

That’s why I, different from the reviewers on its item page on Amazon.com, think this book useful. Indeed as one of the reviewer commented:

If you hope to use this book to get a general overview of measurement systems, then you may be alright, but if you want to be able to perform actual calculations, you should look elsewhere.

This may be insufficient for a text book for professional fields e.g. applied electronics or industrial control, but the practical case for physical sciences is that students need informed in the first place what they need to care about, in a systematic way rather than tips and tricks. I also compared this book with several Chinese textbooks of electronic measurement, and I found the selection of content is the best in Bentley’s book for informing electronic non-experts the necessity to care about what. It becomes rather easy task for one to find more literature for special cases after informed, whereas being completely uninformed or knowing only random, incomplete tips will mislead a researcher quite far.

† I am, of course, talking about the situation in China only.

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Visiting KIT

I am visiting Prof. M. Whilhelm’s lab here in Karlsruhe Institute of Technology since May 15 until May 22 to be trained of FT-rheology technique. The information of the first two days was rich and I just had time to write a summary in Chinese.

I feel quite at home in Germany. The food here is very similar to what I can eat in a typical western restaurant in Guangzhou. Nowadays the food culture is quite globalized among big cities I guess. And I get on well with the group members.

In the first two days several students there introduced what they did to me whenever they had time. And the most helpful discussion was with Kathrin who is researching rheology. I also had a much deeper discussion with another student Deepak who is currently focus on the rheology of polymer/carbon nanotubes composite. We found common interest in the relationship of percolation threshold with the LAOS phenomena. And I also learned useful way of thinking when it comes to developing new measuring parameters. It is somewhat unexpected that I even found common interest with students doing synthesis. Alicia is now working with PS-PLLA copolymers, and I worked on PEO-PLLA copolymer during master years too (see my introduction page). So we went into very detailed discussion in the experimental tricks and problems.

I hope I did not expose too much above… I just want to thank them for sharing. But this is exactly the problem I want to talk about here: where should we draw the line between the secret and the share-able?

After a submission of a manuscript to a journal but before it’s accepted, it is a common practice that the manuscript be classified. This mean there is indeed a stage when the finding is secret to others. But what about cooperation? If I am asked about cooperation in future project, it of course means that we have to share ideas that is not published. What is the guideline here? And if there is not a clear deal whether we are going to cooperate or not, as a visiting student should I still share as much as possible? Otherwise why am I visiting?

Maybe the answer is not straight forward and delicate but I would like to know your experience, if any.

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