The evaluation of a handheld Raman Analyser for the good laboratory practise (glp) compliant identification of paracetamol raw materials, in a pharmaceutical manufacturing environment
- Mavumengwana, Bongeka Nomakhephu
- Authors: Mavumengwana, Bongeka Nomakhephu
- Date: 2015
- Subjects: Raman spectroscopy , Drugs -- Analysis
- Language: English
- Type: Thesis , Masters , MTech
- Identifier: http://hdl.handle.net/10948/4243 , vital:20570
- Description: The use of a handheld Raman analyser for the positive identification of raw materials in a manufacturing pharmaceutical company was evaluated using paracetamol as test raw material to evaluate whether such a system would meet Aspen’s regulatory requirements. The approach involved subjecting the chosen raw material to identification tests under a variety of conditions so as to evaluate robustness, and specificity of the system. Thus, raw material provided by different suppliers, different packages of one manufacturing batch, and raw materials subjected to different storage conditions were evaluated. Specificity was evaluated by deliberately contaminating a sample of paracetamol with either acetanilide, or 4-aminophenol, or both at varying concentration levels. The results obtained from these investigations showed that the handheld Raman analyser can correctly identify the selected raw material (paracetamol) under a wide range of conditions, but could not correctly identify the presence of the selected contaminants at lower concentration levels (< 10 – 20 mass percent). Finally, a cost-benefit analysis was carried out in which a scenario of an existing FTIR-ATR system is used for the analysis of a specific number of raw material samples per year as opposed to a scenario in which a new handheld Raman analyser has to be purchased, set up, and used for the analysis of the same number of raw material samples. This comparison showed that the handheld Raman analyser had a pay-back time of approximately 6 months and gave a return on investment of approximately the same value as the actual purchase cost.
- Full Text:
- Date Issued: 2015
- Authors: Mavumengwana, Bongeka Nomakhephu
- Date: 2015
- Subjects: Raman spectroscopy , Drugs -- Analysis
- Language: English
- Type: Thesis , Masters , MTech
- Identifier: http://hdl.handle.net/10948/4243 , vital:20570
- Description: The use of a handheld Raman analyser for the positive identification of raw materials in a manufacturing pharmaceutical company was evaluated using paracetamol as test raw material to evaluate whether such a system would meet Aspen’s regulatory requirements. The approach involved subjecting the chosen raw material to identification tests under a variety of conditions so as to evaluate robustness, and specificity of the system. Thus, raw material provided by different suppliers, different packages of one manufacturing batch, and raw materials subjected to different storage conditions were evaluated. Specificity was evaluated by deliberately contaminating a sample of paracetamol with either acetanilide, or 4-aminophenol, or both at varying concentration levels. The results obtained from these investigations showed that the handheld Raman analyser can correctly identify the selected raw material (paracetamol) under a wide range of conditions, but could not correctly identify the presence of the selected contaminants at lower concentration levels (< 10 – 20 mass percent). Finally, a cost-benefit analysis was carried out in which a scenario of an existing FTIR-ATR system is used for the analysis of a specific number of raw material samples per year as opposed to a scenario in which a new handheld Raman analyser has to be purchased, set up, and used for the analysis of the same number of raw material samples. This comparison showed that the handheld Raman analyser had a pay-back time of approximately 6 months and gave a return on investment of approximately the same value as the actual purchase cost.
- Full Text:
- Date Issued: 2015
Photophysical properties of zinc carboxy phthalocyanine-quantum dot conjugates
- Authors: Sekhosana, Kutloano Edward
- Date: 2013 , 2013-03-27
- Subjects: Phthalocyanines , Quantum dots , Zinc , Photochemistry , Atomic force microscopy , Transmission electron microscopy , Raman spectroscopy , Infrared spectroscopy , X-ray photoelectron spectroscopy
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4276 , http://hdl.handle.net/10962/d1001652 , Phthalocyanines , Quantum dots , Zinc , Photochemistry , Atomic force microscopy , Transmission electron microscopy , Raman spectroscopy , Infrared spectroscopy , X-ray photoelectron spectroscopy
- Description: This thesis presents work based on the interactions of water soluble caboxylated zinc phthalocyanines (Pcs) and coreshell quantum dots (QDs). The Pcs are ZnPc(COOH)₈ and ZnPc(COOH)₄ and coreshell QDs are CdTe@ZnS-GSH. GSH = L-glutathione. Characterization and photophysical studies of conjugates were carried out. The approach of coordinating Pcs to QDs was achieved using an organic cross linker, N-N’-dicyclohexylcarbodiimide (DCC) at pH 10 at room temperature. Employing atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman, infrared and X-ray photoelectron spectroscopies, the formation of the conjugates was confirmed. Upon conjugation with Pc derivatives, the fluorescence quantum yield of CdTe@ZnS-GSH decreased due to energy transfer from the QDs to the Pc. The average fluorescence lifetime of the CdTe@ZnS-GSH QD also decreased upon conjugation. The föster resonance energy transfer (FRET) behaviour of CdTe@ZnS-GSH-ZnPc(COOH)₄ conjugates was compared to that of CdTe@ZnS-GSH-ZnPc(COOH)₈. Higher FRET efficiencies were observed for CdTe@ZnS-GSH-ZnPc(COOH)₄-mixed or CdTe@ZnS-GSH-ZnPc(COOH)₄-linked compared to the corresponding CdTe@ZnS-GSH-ZnPc(COOH)₈-mixed or CdTe@ZnS-GSH-ZnPc(COOH)₈-linked. Triplet quantum yield (ΦT) and lifetime (ΤT) of ZnPc(COOH)₈ were found to increase in the presence of coreshell QDs. Though the singlet quantum yield (ΦΔ) value of ZnPc(COOH)8 was lower than ΦT , there was a slight upsurge in the ΦT in the presence of QDs. , Microsoft� Word 2010 , Adobe Acrobat 9.53 Paper Capture Plug-in
- Full Text:
- Date Issued: 2013
- Authors: Sekhosana, Kutloano Edward
- Date: 2013 , 2013-03-27
- Subjects: Phthalocyanines , Quantum dots , Zinc , Photochemistry , Atomic force microscopy , Transmission electron microscopy , Raman spectroscopy , Infrared spectroscopy , X-ray photoelectron spectroscopy
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4276 , http://hdl.handle.net/10962/d1001652 , Phthalocyanines , Quantum dots , Zinc , Photochemistry , Atomic force microscopy , Transmission electron microscopy , Raman spectroscopy , Infrared spectroscopy , X-ray photoelectron spectroscopy
- Description: This thesis presents work based on the interactions of water soluble caboxylated zinc phthalocyanines (Pcs) and coreshell quantum dots (QDs). The Pcs are ZnPc(COOH)₈ and ZnPc(COOH)₄ and coreshell QDs are CdTe@ZnS-GSH. GSH = L-glutathione. Characterization and photophysical studies of conjugates were carried out. The approach of coordinating Pcs to QDs was achieved using an organic cross linker, N-N’-dicyclohexylcarbodiimide (DCC) at pH 10 at room temperature. Employing atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman, infrared and X-ray photoelectron spectroscopies, the formation of the conjugates was confirmed. Upon conjugation with Pc derivatives, the fluorescence quantum yield of CdTe@ZnS-GSH decreased due to energy transfer from the QDs to the Pc. The average fluorescence lifetime of the CdTe@ZnS-GSH QD also decreased upon conjugation. The föster resonance energy transfer (FRET) behaviour of CdTe@ZnS-GSH-ZnPc(COOH)₄ conjugates was compared to that of CdTe@ZnS-GSH-ZnPc(COOH)₈. Higher FRET efficiencies were observed for CdTe@ZnS-GSH-ZnPc(COOH)₄-mixed or CdTe@ZnS-GSH-ZnPc(COOH)₄-linked compared to the corresponding CdTe@ZnS-GSH-ZnPc(COOH)₈-mixed or CdTe@ZnS-GSH-ZnPc(COOH)₈-linked. Triplet quantum yield (ΦT) and lifetime (ΤT) of ZnPc(COOH)₈ were found to increase in the presence of coreshell QDs. Though the singlet quantum yield (ΦΔ) value of ZnPc(COOH)8 was lower than ΦT , there was a slight upsurge in the ΦT in the presence of QDs. , Microsoft� Word 2010 , Adobe Acrobat 9.53 Paper Capture Plug-in
- Full Text:
- Date Issued: 2013
Raman spectroscopy of ternary III-V semiconducting films
- Authors: Mashigo, Donald
- Date: 2009
- Subjects: Raman spectroscopy , Semiconductor films , Compound semiconductors
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:10522 , http://hdl.handle.net/10948/1011 , Raman spectroscopy , Semiconductor films , Compound semiconductors
- Description: The III-V semiconductor compounds (i.e. In Ga As x 1-x , 1 x x InAs Sb - , In Ga Sb x 1-x and Al Ga As x 1-x ) have been studied using room temperature Raman spectroscopy. X-ray diffraction has been used as a complementary characterization technique. In this study all the III-V semiconductor compounds were grown by metal organic chemical vapour deposition (MOCVD) on GaAs and GaSb substrates. The layers were studied with respect to composition, strain variation and critical thickness. Raman spectroscopy has been employed to assess the composition dependence of optical phonons in the layers. The alloy composition was varied, while the thickness was kept constant in order to investigate compositional effects. A significant frequency shift of the phonon modes were observed as the composition changed. The composition dependence of the phonon frequencies were described by linear and polynomial expressions. The results of this study were compared with previous Raman and infrared work on III-V semiconductor compounds. Strain relaxation in InGaAs and InGaSb has been investigated by Raman and X-ray diffraction. Measurements were performed on several series of layers. For each series, the thickness was varied, while keeping the composition constant. For a given composition, the layer thicknesses were such that some layers should be fully strained, some partially relaxed and some fully relaxed. The Raman peak shifts and XRD confirm that a layer grows up to the critical thickness and then releases the strain as the thickness increases. Critical layer thickness values measured in this study were compared with published data, in which various techniques had been used to estimate the critical thickness.
- Full Text:
- Date Issued: 2009
- Authors: Mashigo, Donald
- Date: 2009
- Subjects: Raman spectroscopy , Semiconductor films , Compound semiconductors
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:10522 , http://hdl.handle.net/10948/1011 , Raman spectroscopy , Semiconductor films , Compound semiconductors
- Description: The III-V semiconductor compounds (i.e. In Ga As x 1-x , 1 x x InAs Sb - , In Ga Sb x 1-x and Al Ga As x 1-x ) have been studied using room temperature Raman spectroscopy. X-ray diffraction has been used as a complementary characterization technique. In this study all the III-V semiconductor compounds were grown by metal organic chemical vapour deposition (MOCVD) on GaAs and GaSb substrates. The layers were studied with respect to composition, strain variation and critical thickness. Raman spectroscopy has been employed to assess the composition dependence of optical phonons in the layers. The alloy composition was varied, while the thickness was kept constant in order to investigate compositional effects. A significant frequency shift of the phonon modes were observed as the composition changed. The composition dependence of the phonon frequencies were described by linear and polynomial expressions. The results of this study were compared with previous Raman and infrared work on III-V semiconductor compounds. Strain relaxation in InGaAs and InGaSb has been investigated by Raman and X-ray diffraction. Measurements were performed on several series of layers. For each series, the thickness was varied, while keeping the composition constant. For a given composition, the layer thicknesses were such that some layers should be fully strained, some partially relaxed and some fully relaxed. The Raman peak shifts and XRD confirm that a layer grows up to the critical thickness and then releases the strain as the thickness increases. Critical layer thickness values measured in this study were compared with published data, in which various techniques had been used to estimate the critical thickness.
- Full Text:
- Date Issued: 2009
A raman spectroscopy study of semiconducting thin films
- Authors: Goosen, William Edward
- Date: 2006
- Subjects: Raman spectroscopy , Semiconductor films , Thin films
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:10514 , http://hdl.handle.net/10948/426 , Raman spectroscopy , Semiconductor films , Thin films
- Description: A home-built Raman system, utilizing a pseudo-backscattering geometry, was built in the Physics Department at the Nelson Mandela Metropolitan University (NMMU). The system was then used to analyse a variety of bulk and thin film semiconducting materials currently being studied in the Physics Department. Silicon wafers were exposed to hydrogen plasma. Raman analysis of hydrogen induced platelets (HIPs), resulting from hydrogen plasma treatment of silicon, is reported. ZnO layers were deposited on glass, GaAs, Si, sapphire and SiC-Si substrates by metalorganic chemical vapour deposition (MOCVD) in the Physics Department at the NMMU. It was found that the ZnO layers grown by MOCVD all exhibited a strong E2 (high) phonon mode that dominated the Raman spectra. Furthermore, the spectra lacked the A1 (LO) phonon mode which is usually associated with the O-vacancy, the Zn-interstitial, or complexes of the two, indicating that the layers were all of good quality. The influence of depositing the ZnO thin film on a 3 mm thick SiC layer was also investigated and compared with the deposition of ZnO on Si substrate, in order to reduce the lattice mismatch between ZnO and the Si substrate. The possible shift of the Raman peaks due to the residual strain in the film, if present, could not be resolved. Characterization of GaN and AlxGa1-xN produced by MOCVD at the CRHEA laboratory of the CNRS in Valbonne, France is reported. A sharp peak at 567 cm-1 corresponding to the E2 (high) mode of GaN broadens and shifts to higher wavenumbers as the aluminium content of the AlxGa1-xN is increased. The shift is accompanied by a decrease in the intensity and a broadening of this peak. The broadening was attributed to a general decrease in the quality of the layers which accompanies increased aluminium content in AlxGa1-xN.
- Full Text:
- Date Issued: 2006
- Authors: Goosen, William Edward
- Date: 2006
- Subjects: Raman spectroscopy , Semiconductor films , Thin films
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:10514 , http://hdl.handle.net/10948/426 , Raman spectroscopy , Semiconductor films , Thin films
- Description: A home-built Raman system, utilizing a pseudo-backscattering geometry, was built in the Physics Department at the Nelson Mandela Metropolitan University (NMMU). The system was then used to analyse a variety of bulk and thin film semiconducting materials currently being studied in the Physics Department. Silicon wafers were exposed to hydrogen plasma. Raman analysis of hydrogen induced platelets (HIPs), resulting from hydrogen plasma treatment of silicon, is reported. ZnO layers were deposited on glass, GaAs, Si, sapphire and SiC-Si substrates by metalorganic chemical vapour deposition (MOCVD) in the Physics Department at the NMMU. It was found that the ZnO layers grown by MOCVD all exhibited a strong E2 (high) phonon mode that dominated the Raman spectra. Furthermore, the spectra lacked the A1 (LO) phonon mode which is usually associated with the O-vacancy, the Zn-interstitial, or complexes of the two, indicating that the layers were all of good quality. The influence of depositing the ZnO thin film on a 3 mm thick SiC layer was also investigated and compared with the deposition of ZnO on Si substrate, in order to reduce the lattice mismatch between ZnO and the Si substrate. The possible shift of the Raman peaks due to the residual strain in the film, if present, could not be resolved. Characterization of GaN and AlxGa1-xN produced by MOCVD at the CRHEA laboratory of the CNRS in Valbonne, France is reported. A sharp peak at 567 cm-1 corresponding to the E2 (high) mode of GaN broadens and shifts to higher wavenumbers as the aluminium content of the AlxGa1-xN is increased. The shift is accompanied by a decrease in the intensity and a broadening of this peak. The broadening was attributed to a general decrease in the quality of the layers which accompanies increased aluminium content in AlxGa1-xN.
- Full Text:
- Date Issued: 2006
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