What are the principles & the procedures involved in on-line, in-line and non-invasive process analysis

These are sample chemistry coursework questions

What are the principles & the procedures involved in on-line, in-line and non-invasive process analysis. Compare between them (advantages & dis-advantages). commenting on any sampling issues.

(300 word)

References:

  1. Process Analytical Chemistry

Edited by F. McLennan and B.R. Kowalski

Blackie Academic and Professional, an Imprint of Chapman and Hall

Wester Cleddens Road, Bishopbriggs, Glasgow

  1. J.B. Callis, D.L. Illman and B.R. Kowalski

Anal. Chem., 1987, 62, 624A

  1. Raman Spectroscopy for on-line, real-time, multi-point industrial

chemical analysis

M.J. Roberts, A.A. Garrison, S.W. Kercel and E.C. Muly

Process Control and Quality, 1991, 1, 281-291

  1. K. J. Clevett

Indust. Perspect. Control Instrumentation

1994, 29, 26(3)

  1. K. J. Clevett

Process Analyser Technology

John Wiley and Sons, New York, 1986

  1. D.J. Huskins

Quality Measuring Instruments in On-line Process Analysis

Halstead Press, New York, 1982

  1. P. E. Mix

The Design and Application of Process Analyser Systems

Wiley Interscience, New York, 1984

  1. Process Analytical Chemistry

Anal. Chem. 1993, 65, 199R

  1. Why is the sampling system crucial for on-line analysis?
  2. What are the key features to consider when designing a sampling system?
  3. Describe the general stages of a sampling system including the need for conditioning.

(300 word)

References:

  1. Process Analyser Technology
    J. Clevett
    John Wiley & Sons, New York, 1986
  2. Sampling Systems for Process Analysers
    C. Cornish, G. Jepson and M.J. Smurthwaite
    Butterworth, London, 1981
  3. Chemical Engineering Handbook
    H. Perry
    McGraw-Hill Chemical Engineering Services
  4. Principles of Sample Handling System Design for Process Analysis
    A. Houser
    Proc. ISA Symp., Pittsburgh, PA, 1977
  5. Process Analyser Sampling Systems
    G. Nichols
    Analytical Chemistry, 1981, 53, 489A.
  6. Process Analytical Chemistry
    McLennan and B.R. Kowalski (Editors)
    Blackie Academic and Professional, Glasgow, 1995, Chapter 2.
  7. Considerations for the selection and design of sampling systems for heterogeneos processes in a stirred tank reactor
    Diez-Lazoro, M.L. Hitchman and D. Littlejohn
    Chemical Engineering and Design, 83(A4), 344
  8. Sampling and Sample Preparation in Process Analysis
    E. Creasy and T.W. Francisco
    Encyclopedia of Analytical Chemistry, R.A. Meyers (Ed.), John Wiley and Sons Ltd.
  • Be able to describe laser diffraction, FBRM and dynamic image analysis for measurement of particle size.

(300 word)

References

  1. Application of continuous crystallisation in an integrated continuous pharmaceutical pilot plant, Zhang, H., Lakerveld, R., Heider, P.L., Tao, M., Su, M., Testa C.J., D’Antonio, A.N., Barton, P.I., Braatz, R.D., Trout, B.L., Myerson, A.S., Jensen, K.F., Evans, J.M.B, Crystal Growth and Design, 2014, 14(5), 2148
  2. Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman Spectrometry, Hamilton, P., Littlejohn, D., Nordon, A., Sefcik, J., Slavin, P., Andrews, J., Dallin, P., Chemical Engineering Science, 2013, 101, 878
  3. Studies of particle drying using non-invasive Raman spectrometry and particle size analysis, Hamilton, P., Littlejohn, D., Nordon, A., Sefcik, J., Slavin, P., Dallin, P., Andrews, J., Analyst, 2011, 136 (10), 2168
  4. Different modes of dynamic image analysis in monitoring of pharmaceutical dry milling process, Nalluri, V.R., Schirg, P., Gao, X., Virdis, A., Imanidis, G., Kuentz, M., International Journal of Pharmaceutics, 2010, 391(1-2), 107
  5. Estimation of particle size distributions from focused beam reflectance measurements based on an optical model, Kail, N., Marquardt, W., Briesen, H., Chemical Engineering Science, 2009, 64(5), 984
  6. Evaluation of dynamic image analysis for characterizing pharmaceutical excipient particles, Yu, W.L., Hancock, B.C., International Journal of Pharmaceutics, 2008, 361(1-2), 150
  7. Laser diffraction and image analysis as a supportive analytical tool in the pharmaceuticaldevelopment of immediate release direct compression formulations, Tinke, A.P., Vanhoutte, K,. Vanhoutte, F., De Smet A., De Winter, H., International Journal of Pharmaceutics, 2005, 297(1-2), 80
  8. Sympatec, http://www.sympatec.com/EN/ImageAnalysis/Fundamentals.html, Nov. 2014.

Describe the basis of Raman spectrometry?   (300 word)

References

  1. Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman Spectrometry, Hamilton, P., Littlejohn, D., Nordon, A., Sefcik, J., Slavin, P., Andrews, J., Dallin, P., Chemical Engineering Science, 2013, 101, 878
  2. Studies of particle drying using non-invasive Raman spectrometry and particle size analysis, Hamilton, P., Littlejohn, D., Nordon, A., Sefcik, J., Slavin, P., Dallin, P., Andrews, J., Analyst, 2011, 136 (10), 2168
  3. Monitoring process induced attrition of drug substance particles within formulated blends, Gamble, J.F., Hoffmann, M., Hughes, H., Hutchins, P., Tobyn, M., International Journal of Pharmaceutics, 2014, 470 (1-2), 77
  4. Describe the features and the basis of an attenuated total reflection (ATR) probe, what are the main advantages and limitations of this type of probe and which technique is it used with of in-line analysis?

Comment on the types of optical fiber that are used to connect insertion  or non-invasive measurement probes to spectrometer for process analysis by different molecular spectrometry techniques.  describe how multiplexing can be achieved using fiber optic probes(300 word)

Explain the basis of mid infrared spectrometry (MIR) and near infrared spectrometry ( NIR)?  (200 word )

Describe the basis of transmission and attenuated total reflection ( ATR) probe that are used in the process analysis by UV-visible spectrometry?

(300 word)

Process mass spectrometry is to be used to monitor the concentration of trace levels of toluene in waste water that is to be treated prior to disposal.

(400 word)

  • Describe how the organic analyte can be preferentially sampled from the waste water into the mass spectrometer for on-line analysis. Comment on any precautions that would be required to ensure proper transfer of the sample vapour to the spectrometer.
  • Describe the key features of an interface that would allow one mass spectrometer to monitor several water treatment units. Comment on the aspects of process mass spectrometry that allow such multiplexing.

 

The concentration of several hydrocarbon components needs to be monitored in a gaseous petrochemical process. Process mass spectrometry is being considered for this task.  

(400 word)

  1. i) Comment on the sampling and pre- conditioning steps that would be required for the analysis.
  2. ii) Describe a sampling introduction system for mass spectrometry that would be suitable for this application.

Compare the usefulness of Raman and MIR spectrometries for process

analysis. Include in your answer, comments on: (400 word)

– how flexibe the techniques are for different types of process analysis.

– problems that can affect photon transmission between the

spectrometer and the sample;

– other factors that can adversely affect the use of each technique;

– one process application for each technique, with a comment on why it proved successful for the measurements required.

Describe how an organic analyte, such as toluene, can be preferentially

sampled from an aqueous process stream into a mass spectrometer for on-line

analysis. Comment on any precautions that would be required to ensure proper

transfer of the sample vapour to the spectrometer. (400 word)

 

Quality by Design has been introduced to improve the consistency of medicinal

product manufacturing to a level that is comparable to the automotive and computer industries. Using a single stage or process in a typical tablet manufacturing process, explain how Quality by Design incorporating statistics, process analytical technology and multivariate analysis can be applied within a Good Manufacturing Practice setting. (550 word)

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