Process and reaction monitoring with medium field NMR spectroscopy:
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Abschlussarbeit Buch |
| Sprache: | English |
| Veröffentlicht: |
Kaiserslautern
Laboratory of Engineering Thermodynamics (LTD), University of Kaiserslautern
2020
|
| Schriftenreihe: | Scientific report series / Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics
volume 32 |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis Inhaltsverzeichnis |
| Beschreibung: | XXII, 137 Seiten Illustrationen, Diagramme |
| ISBN: | 9783944433318 |
Internformat
MARC
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| 016 | 7 | |a 1219080764 |2 DE-101 | |
| 020 | |a 9783944433318 |c Broschur |9 978-3-944433-31-8 | ||
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| 084 | |8 1\p |a 540 |2 sdnb | ||
| 100 | 1 | |a Friebel, Anne |d 1989- |e Verfasser |0 (DE-588)1216428816 |4 aut | |
| 245 | 1 | 0 | |a Process and reaction monitoring with medium field NMR spectroscopy |c Anne Friebel |
| 264 | 1 | |a Kaiserslautern |b Laboratory of Engineering Thermodynamics (LTD), University of Kaiserslautern |c 2020 | |
| 300 | |a XXII, 137 Seiten |b Illustrationen, Diagramme | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 490 | 1 | |a Scientific report series / Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics |v volume 32 | |
| 502 | |b Dissertation |c Technische Universität Kaiserslautern |d 2020 | ||
| 650 | 0 | 7 | |a Prozessüberwachung |0 (DE-588)4133922-8 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Reaktionstechnik |0 (DE-588)4136173-8 |2 gnd |9 rswk-swf |
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| 689 | 0 | 2 | |a NMR-Spektroskopie |0 (DE-588)4075421-2 |D s |
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| 810 | 2 | |a Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics |t Scientific report series |v volume 32 |w (DE-604)BV040983565 |9 32 | |
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Datensatz im Suchindex
| _version_ | 1804181942250242048 |
|---|---|
| adam_text | CONTENTS
XV
CONTENTS
1
INTRODUCTION
1
2
LIQUID-LIQUID
EQUILIBRIA
5
2.1
INTRODUCTION
...................................................................................................
5
2.2
EXPERIMENTS
...................................................................................................
7
2.2.1
CHEMICALS
...........................................................................................
7
2.2.2
EXPERIMENTAL
SETUP
AND
PROCEDURE
..................................................
8
2.2.2.1
NON-REACTIVE
SYSTEMS
.......................................................
8
2.2.2.2
REACTIVE
SYSTEM
...............................................................
9
2.2.3
NMR
INSTRUMENT
AND
METHODS
.......................................................
10
2.2.4
PEAK
ASSIGNMENT
AND
QUANTIFICATION
...............................................
10
2.2.5
CORRELATION
........................................................................................
12
2.3
RESULTS
AND
DISCUSSION
..................................................................................
13
2.3.1
SYSTEM
TOLUENE
+
ACETONE
+
WATER
..................................................
13
2.3.2
SYSTEM
DIETHYL
ETHER
+
ACETONE
+
WATER
.......................................
13
2.3.3
SYSTEM
DIETHYL
ETHER
+
METHANOL
+
WATER
....................................
14
2.3.4
SYSTEM
ACETONITRILE
+
ETHANOL
+
CYCLOHEXANE
.................................
15
2.3.5
REACTIVE
SYSTEM
WATER
+
ACETIC
ACID
+
ACETIC
ANHYDRIDE
..............
16
2.4
CONCLUSIONS
...................................................................................................
17
3
BATCH
DISTILLATION
21
3.1
INTRODUCTION
...................................................................................................
21
3.2
EXPERIMENTS
...................................................................................................
22
3.2.1
CHEMICALS
...........................................................................................
22
3.2.2
EXPERIMENTAL
SETUP
..........................................................................
22
3.2.3
PROCEDURE
...........................................................................................
24
3.2.4
ANALYSIS
.............................................................................................
25
3.2.5
MODELING
AND
SIMULATION
..................................................................
25
3.3
RESULTS
AND
DISCUSSION
..................................................................................
27
3.3.1
SYSTEM:
DIMETHYL
SULFOXIDE
+
ACETONITRILE
+
ETHYL
FORMATE
....
27
3.3.2
SYSTEM:
ETHYL
ACETATE
+
ACETONE
+
DIETHYL
ETHER
...........................
27
3.3.3
SYSTEM:
ACETIC
ACID
+
PYRIDINE
.......................................................
29
XVI
CONTENTS
3.3.4
SYSTEM:
METHANOL
+
DIETHYLAMINE
..................................................
29
3.4
CONCLUSIONS
...................................................................................................
32
4
REACTION
MONITORING
35
4.1
INTRODUCTION
...................................................................................................
35
4.2
REACTION
SYSTEMS
AND
KINETIC
MODEL
...........................................................
36
4.3
REACTOR
MODELS
..............................................................................................
37
4.4
EXPERIMENTS
...................................................................................................
38
4.4.1
CHEMICALS
...........................................................................................
38
4.4.2
EXPERIMENTAL
SETUP
AND
PROCEDURE
..................................................
38
4.4.3
NMR
INSTRUMENT
AND
METHODS
.........................................................
39
4.4.4
PREMAGNETIZATION
IN
FLOW
..................................................................
41
4.4.5
RTD
MEASUREMENTS
..........................................................................
42
4.4.6
PEAK
ASSIGNMENT
AND
DATA
ANALYSIS
..................................................
43
4.5
RESULTS
AND
DISCUSSION
...................................................................................
45
4.5.1
KINETIC
MEASUREMENTS
.....................................................................
45
4.5.2
2D
NMR
MEASUREMENTS
..................................................................
48
4.6
CONCLUSIONS
...................................................................................................
49
5
MODELING
OF
MAGNETIZATION
53
5.1
INTRODUCTION
...................................................................................................
53
5.2
EXPERIMENTS
...................................................................................................
55
5.2.1
CHEMICALS
...........................................................................................
55
5.2.2
EXPERIMENTAL
SETUP
..........................................................................
55
5.2.3
PROCEDURE
...........................................................................................
57
5.2.3.1
PHYSICAL
PROPERTIES
...............................................................
57
5.2.3.2
RELATIVE
MAGNETIZATION
.........................................................
57
5.3
MODELLING
AND
SIMULATION
......................................................................
58
5.3.1
TRANSPORT
MODEL
FOR
MAGNETIZATION
...................................................
58
5.3.2
SIMULATION
........................................................................................
59
5.4
RESULTS
AND
DISCUSSION
..................................................................................
61
5.4.1
PURE
WATER
........................................................................................
61
5.4.2
MIXTURES
OF
WATER
+
ACETONITRILE
......................................................
64
5.5
CONCLUSIONS
...................................................................................................
67
6
CONCLUSIONS
71
LITERATURE
74
APPENDIX
87
CONTENTS
XVII
A
LIQUID-LIQUID
EQUILIBRIUM
87
A.
L
SYSTEM
ACN
+
ETOH
+
CH
-
ALTERNATIVE
MEASUREMENT
METHODS
...........
87
A.
1.1
SAMPLE
SHIFTING
METHOD
IN
COMBINATION
WITH
CARBON
MEDIUM
FIELD
SPECTROSCOPY
.........................................................................
87
A.
1.1.1
EXPERIMENTAL
SETUP
AND
PROCEDURE
.............................
87
A.
1.1.2
NMR
INSTRUMENT
AND
METHODS
..................................
87
A.
1.1.3
PEAK
ASSIGNMENT
AND
QUANTIFICATION
.............................
88
A.
1.1.4
RESULTS
AND
DISCUSSION
...................................................
88
A.
1.2
SLICING
METHOD
IN
COMBINATION
WITH
PROTON
HIGH
FIELD
SPECTROSCOPY
89
A.
1.2.1
EXPERIMENTAL
SETUP
AND
PROCEDURE
.................................
89
A.
1.2.2
NMR
INSTRUMENT
AND
METHODS
.......................................
90
A.
1.2.3
PEAK
ASSIGNMENT
AND
QUANTIFICATION
.................................
91
A.
1.2.4
RESULTS
AND
DISCUSSION
.......................................................
91
A.
2
POSITIONING
OF
THE
SAMPLE
TUBE
...................................................................
91
A.
3
PEAK
ASSIGNMENT
.........................................................................................
92
A.
4
INTEGRATION
METHODS
....................................................................................
92
A.
5
DETAILS
ON
CORRELATION
.................................................................................
95
A.5.1
NRTL
AND
UNIQU
AC
MODEL
..........................................................
95
A.
5.2
SLOPE
CURVE
METHOD
..........................................................................
96
A.
6
EXPERIMENTAL
PHASE
COMPOSITION
..................................................................
97
B
BATCH
DISTILLATION
104
B.
L
RTD
MEASUREMENT
BYPASS
............................................................................
104
B.
2
QUANTITATIVE
FLOW
MEASUREMENTS
....................................................................
104
B.
3
ACCURACY
OF
NMR
ANALYSIS
............................................................................
105
B.
4
GC
METHOD
AND
CALIBRATION
.........................................................................
105
B.
5
ANTOINE
AND
NRTL
PARAMETERS
....................................................................
106
B.
6
RESIDUE
CURVES
...............................................................................................
107
C
REACTION
MONITORING
112
C.
L
PREMAGNETIZATION
IN
FLOW
...............................................................................
112
C.
2
RTD
MEASUREMENTS
.......................................................................................
112
C.
2.1
PROCEDURE
..............................................................................................
112
C.
2.
2
PARAMETRIZATION
OF
TSR
MODEL
..........................................................
114
C.
2.
3
SENSITIVITY
STUDY
PER
........................................................................
115
C.
3
EXPERIMENTAL
DATA
..........................................................................................
116
C.3.1
KINETIC
DATA
........................................................................................
116
D
MODELING
OF
MAGNETIZATION
123
D.
L
MAGNETIC
FIELD
STRENGTH
..................................................................................
123
XVIII
CONTENTS
0.2
TEMPERATURE
DEPENDENCE
OF
RELAXATION
TIME
.................................................
123
0.3
NUMERICAL
DIMENSIONS
OF
THE
FLOW
CELLS
.........................................................
123
0.4
PEAK
ASSIGNMENT
.............................................................................................
124
0.5
LAMINAR
AND
TURBULENT
SIMULATION
IN
FLOW
CELL
III
..........................................
124
0.6
WEIGHING
FUNCTION
OF
NON-UNIFORM
EXCITATION
PROFILE
....................................
125
0.7
OPTIMIZATION
OF
SOLVER
OPTIONS
AND
MESHING
.................................................
126
0.8
SENSITIVITY
ANALYSIS
-
SELF-DIFFUSION
COEFFICIENT
..............................................
127
0.9
SOURCE
CODE
BLOCHFOAM
SOLVER
.......................................................................
128
0.10
EXPERIMENTAL
AND
SIMULATION
DATA
..................................................................
128
|
| adam_txt |
CONTENTS
XV
CONTENTS
1
INTRODUCTION
1
2
LIQUID-LIQUID
EQUILIBRIA
5
2.1
INTRODUCTION
.
5
2.2
EXPERIMENTS
.
7
2.2.1
CHEMICALS
.
7
2.2.2
EXPERIMENTAL
SETUP
AND
PROCEDURE
.
8
2.2.2.1
NON-REACTIVE
SYSTEMS
.
8
2.2.2.2
REACTIVE
SYSTEM
.
9
2.2.3
NMR
INSTRUMENT
AND
METHODS
.
10
2.2.4
PEAK
ASSIGNMENT
AND
QUANTIFICATION
.
10
2.2.5
CORRELATION
.
12
2.3
RESULTS
AND
DISCUSSION
.
13
2.3.1
SYSTEM
TOLUENE
+
ACETONE
+
WATER
.
13
2.3.2
SYSTEM
DIETHYL
ETHER
+
ACETONE
+
WATER
.
13
2.3.3
SYSTEM
DIETHYL
ETHER
+
METHANOL
+
WATER
.
14
2.3.4
SYSTEM
ACETONITRILE
+
ETHANOL
+
CYCLOHEXANE
.
15
2.3.5
REACTIVE
SYSTEM
WATER
+
ACETIC
ACID
+
ACETIC
ANHYDRIDE
.
16
2.4
CONCLUSIONS
.
17
3
BATCH
DISTILLATION
21
3.1
INTRODUCTION
.
21
3.2
EXPERIMENTS
.
22
3.2.1
CHEMICALS
.
22
3.2.2
EXPERIMENTAL
SETUP
.
22
3.2.3
PROCEDURE
.
24
3.2.4
ANALYSIS
.
25
3.2.5
MODELING
AND
SIMULATION
.
25
3.3
RESULTS
AND
DISCUSSION
.
27
3.3.1
SYSTEM:
DIMETHYL
SULFOXIDE
+
ACETONITRILE
+
ETHYL
FORMATE
.
27
3.3.2
SYSTEM:
ETHYL
ACETATE
+
ACETONE
+
DIETHYL
ETHER
.
27
3.3.3
SYSTEM:
ACETIC
ACID
+
PYRIDINE
.
29
XVI
CONTENTS
3.3.4
SYSTEM:
METHANOL
+
DIETHYLAMINE
.
29
3.4
CONCLUSIONS
.
32
4
REACTION
MONITORING
35
4.1
INTRODUCTION
.
35
4.2
REACTION
SYSTEMS
AND
KINETIC
MODEL
.
36
4.3
REACTOR
MODELS
.
37
4.4
EXPERIMENTS
.
38
4.4.1
CHEMICALS
.
38
4.4.2
EXPERIMENTAL
SETUP
AND
PROCEDURE
.
38
4.4.3
NMR
INSTRUMENT
AND
METHODS
.
39
4.4.4
PREMAGNETIZATION
IN
FLOW
.
41
4.4.5
RTD
MEASUREMENTS
.
42
4.4.6
PEAK
ASSIGNMENT
AND
DATA
ANALYSIS
.
43
4.5
RESULTS
AND
DISCUSSION
.
45
4.5.1
KINETIC
MEASUREMENTS
.
45
4.5.2
2D
NMR
MEASUREMENTS
.
48
4.6
CONCLUSIONS
.
49
5
MODELING
OF
MAGNETIZATION
53
5.1
INTRODUCTION
.
53
5.2
EXPERIMENTS
.
55
5.2.1
CHEMICALS
.
55
5.2.2
EXPERIMENTAL
SETUP
.
55
5.2.3
PROCEDURE
.
57
5.2.3.1
PHYSICAL
PROPERTIES
.
57
5.2.3.2
RELATIVE
MAGNETIZATION
.
57
5.3
MODELLING
AND
SIMULATION
.
58
5.3.1
TRANSPORT
MODEL
FOR
MAGNETIZATION
.
58
5.3.2
SIMULATION
.
59
5.4
RESULTS
AND
DISCUSSION
.
61
5.4.1
PURE
WATER
.
61
5.4.2
MIXTURES
OF
WATER
+
ACETONITRILE
.
64
5.5
CONCLUSIONS
.
67
6
CONCLUSIONS
71
LITERATURE
74
APPENDIX
87
CONTENTS
XVII
A
LIQUID-LIQUID
EQUILIBRIUM
87
A.
L
SYSTEM
ACN
+
ETOH
+
CH
-
ALTERNATIVE
MEASUREMENT
METHODS
.
87
A.
1.1
SAMPLE
SHIFTING
METHOD
IN
COMBINATION
WITH
CARBON
MEDIUM
FIELD
SPECTROSCOPY
.
87
A.
1.1.1
EXPERIMENTAL
SETUP
AND
PROCEDURE
.
87
A.
1.1.2
NMR
INSTRUMENT
AND
METHODS
.
87
A.
1.1.3
PEAK
ASSIGNMENT
AND
QUANTIFICATION
.
88
A.
1.1.4
RESULTS
AND
DISCUSSION
.
88
A.
1.2
SLICING
METHOD
IN
COMBINATION
WITH
PROTON
HIGH
FIELD
SPECTROSCOPY
89
A.
1.2.1
EXPERIMENTAL
SETUP
AND
PROCEDURE
.
89
A.
1.2.2
NMR
INSTRUMENT
AND
METHODS
.
90
A.
1.2.3
PEAK
ASSIGNMENT
AND
QUANTIFICATION
.
91
A.
1.2.4
RESULTS
AND
DISCUSSION
.
91
A.
2
POSITIONING
OF
THE
SAMPLE
TUBE
.
91
A.
3
PEAK
ASSIGNMENT
.
92
A.
4
INTEGRATION
METHODS
.
92
A.
5
DETAILS
ON
CORRELATION
.
95
A.5.1
NRTL
AND
UNIQU
AC
MODEL
.
95
A.
5.2
SLOPE
CURVE
METHOD
.
96
A.
6
EXPERIMENTAL
PHASE
COMPOSITION
.
97
B
BATCH
DISTILLATION
104
B.
L
RTD
MEASUREMENT
BYPASS
.
104
B.
2
QUANTITATIVE
FLOW
MEASUREMENTS
.
104
B.
3
ACCURACY
OF
NMR
ANALYSIS
.
105
B.
4
GC
METHOD
AND
CALIBRATION
.
105
B.
5
ANTOINE
AND
NRTL
PARAMETERS
.
106
B.
6
RESIDUE
CURVES
.
107
C
REACTION
MONITORING
112
C.
L
PREMAGNETIZATION
IN
FLOW
.
112
C.
2
RTD
MEASUREMENTS
.
112
C.
2.1
PROCEDURE
.
112
C.
2.
2
PARAMETRIZATION
OF
TSR
MODEL
.
114
C.
2.
3
SENSITIVITY
STUDY
'PER'
.
115
C.
3
EXPERIMENTAL
DATA
.
116
C.3.1
KINETIC
DATA
.
116
D
MODELING
OF
MAGNETIZATION
123
D.
L
MAGNETIC
FIELD
STRENGTH
.
123
XVIII
CONTENTS
0.2
TEMPERATURE
DEPENDENCE
OF
RELAXATION
TIME
.
123
0.3
NUMERICAL
DIMENSIONS
OF
THE
FLOW
CELLS
.
123
0.4
PEAK
ASSIGNMENT
.
124
0.5
LAMINAR
AND
TURBULENT
SIMULATION
IN
FLOW
CELL
III
.
124
0.6
WEIGHING
FUNCTION
OF
NON-UNIFORM
EXCITATION
PROFILE
.
125
0.7
OPTIMIZATION
OF
SOLVER
OPTIONS
AND
MESHING
.
126
0.8
SENSITIVITY
ANALYSIS
-
SELF-DIFFUSION
COEFFICIENT
.
127
0.9
SOURCE
CODE
BLOCHFOAM
SOLVER
.
128
0.10
EXPERIMENTAL
AND
SIMULATION
DATA
.
128 |
| any_adam_object | 1 |
| any_adam_object_boolean | 1 |
| author | Friebel, Anne 1989- |
| author_GND | (DE-588)1216428816 |
| author_facet | Friebel, Anne 1989- |
| author_role | aut |
| author_sort | Friebel, Anne 1989- |
| author_variant | a f af |
| building | Verbundindex |
| bvnumber | BV046996414 |
| classification_rvk | VG 9507 |
| ctrlnum | (OCoLC)1225974968 (DE-599)DNB1219080764 |
| discipline | Chemie / Pharmazie |
| discipline_str_mv | Chemie / Pharmazie |
| format | Thesis Book |
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| genre | (DE-588)4113937-9 Hochschulschrift gnd-content |
| genre_facet | Hochschulschrift |
| id | DE-604.BV046996414 |
| illustrated | Illustrated |
| index_date | 2024-07-03T15:55:13Z |
| indexdate | 2024-07-10T08:59:40Z |
| institution | BVB |
| isbn | 9783944433318 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-032404166 |
| oclc_num | 1225974968 |
| open_access_boolean | |
| owner | DE-83 DE-706 DE-29T DE-634 |
| owner_facet | DE-83 DE-706 DE-29T DE-634 |
| physical | XXII, 137 Seiten Illustrationen, Diagramme |
| publishDate | 2020 |
| publishDateSearch | 2020 |
| publishDateSort | 2020 |
| publisher | Laboratory of Engineering Thermodynamics (LTD), University of Kaiserslautern |
| record_format | marc |
| series2 | Scientific report series / Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics |
| spelling | Friebel, Anne 1989- Verfasser (DE-588)1216428816 aut Process and reaction monitoring with medium field NMR spectroscopy Anne Friebel Kaiserslautern Laboratory of Engineering Thermodynamics (LTD), University of Kaiserslautern 2020 XXII, 137 Seiten Illustrationen, Diagramme txt rdacontent n rdamedia nc rdacarrier Scientific report series / Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics volume 32 Dissertation Technische Universität Kaiserslautern 2020 Prozessüberwachung (DE-588)4133922-8 gnd rswk-swf Reaktionstechnik (DE-588)4136173-8 gnd rswk-swf NMR-Spektroskopie (DE-588)4075421-2 gnd rswk-swf (DE-588)4113937-9 Hochschulschrift gnd-content Prozessüberwachung (DE-588)4133922-8 s Reaktionstechnik (DE-588)4136173-8 s NMR-Spektroskopie (DE-588)4075421-2 s DE-604 Technische Universität Kaiserslautern, Laboratory of Engineering Thermodynamics Scientific report series volume 32 (DE-604)BV040983565 32 B:DE-101 application/pdf https://d-nb.info/1219080764/04 Inhaltsverzeichnis DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=032404166&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p aepsg 0,98487 20201013 DE-101 https://d-nb.info/provenance/plan#aepsg |
| spellingShingle | Friebel, Anne 1989- Process and reaction monitoring with medium field NMR spectroscopy Prozessüberwachung (DE-588)4133922-8 gnd Reaktionstechnik (DE-588)4136173-8 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd |
| subject_GND | (DE-588)4133922-8 (DE-588)4136173-8 (DE-588)4075421-2 (DE-588)4113937-9 |
| title | Process and reaction monitoring with medium field NMR spectroscopy |
| title_auth | Process and reaction monitoring with medium field NMR spectroscopy |
| title_exact_search | Process and reaction monitoring with medium field NMR spectroscopy |
| title_exact_search_txtP | Process and reaction monitoring with medium field NMR spectroscopy |
| title_full | Process and reaction monitoring with medium field NMR spectroscopy Anne Friebel |
| title_fullStr | Process and reaction monitoring with medium field NMR spectroscopy Anne Friebel |
| title_full_unstemmed | Process and reaction monitoring with medium field NMR spectroscopy Anne Friebel |
| title_short | Process and reaction monitoring with medium field NMR spectroscopy |
| title_sort | process and reaction monitoring with medium field nmr spectroscopy |
| topic | Prozessüberwachung (DE-588)4133922-8 gnd Reaktionstechnik (DE-588)4136173-8 gnd NMR-Spektroskopie (DE-588)4075421-2 gnd |
| topic_facet | Prozessüberwachung Reaktionstechnik NMR-Spektroskopie Hochschulschrift |
| url | https://d-nb.info/1219080764/04 http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=032404166&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| volume_link | (DE-604)BV040983565 |
| work_keys_str_mv | AT friebelanne processandreactionmonitoringwithmediumfieldnmrspectroscopy |
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