More practical problem solving in HPLC:
Saved in:
| Main Author: | |
|---|---|
| Format: | Book |
| Language: | English German |
| Published: |
Weinheim
Wiley-VCH
2005
|
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Item Description: | Aus dem Dt. übers. |
| Physical Description: | XV, 294 S. Ill., graph. Darst. |
| ISBN: | 3527311130 |
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| adam_text | Contents
Preface XV
The Structure of the Book 1
Part 1 (general section) 1
Part 2 (specific questions) 1
In Lieu of an Introduction 3
Chromatography Crossword 4
Across 4
Down 4
An HPLC Quiz 6
An HPLC Tale 9
The Tale of Peaky and Chromy 9
I HPLC Tips 11
1.1 Stationary Phases and Columns 11
Tip No.
01 It improves with age is a rule that applies to port and sometimes
to red wine, but how about your Ci8 column? 11
02 Optimization via column parameters what works best? 14
03 Can selectivity always be put down to chemical interactions
with the stationary phase? 17
04 A matter of perspective ... Or: Selectivity and peak symmetry
of basic compounds using reversed phase packing materials 19
05 Separation of isomers 21
06 When should I use a polar C,8 phase? 23
07 Are polar RP C|g phases more suitable for the separation of polar analytes
than non polar phases? 24
08 What about non endcapped phases are they a thing of the past? 25
09 How can I separate acids using RP C,8? 27
10 The nitrile phase some like it polar 29
I1 The selectivity of RP columns 31
1.2 Buffers, pH Value 33
12 Does it always have to be potassium phosphate? 33
More Practical Problem Solving in HPLC. S. Kromidas JX
Copyright © 2005 WILEY VCH Verlag GmbH Co. KGaA, Weinheim
ISBN: 3 527 31113 0
Tip No.
13 UV cut off of buffer solutions 34
14 Sources of errors when using buffers 35
15 The drawbacks of using buffers 37
16 Why is the pH value so important, and what does it do? 40
17 Why does the pH value shift even though I am using the correct buffer
and the buffer capacity is sufficient? 42
18 Changes to the pH value in the eluent: the extent of the shift
and the reasons behind it 43
19 An unintentional pH shift and its consequences 46
20 RP separations in the alkaline medium 49
21 Separation of basic and acidic compounds contained
in the same sample 51
1.3 Optimization, Peak Homogeneity 53
22 The peaks appear too soon what can be done? 53
23 What can I do if the peaks elute late? 55
24 Quick optimization of an existing gradient method 60
25 Increasing efficiency often the fast track to success 63
26 Additives to the eluent 66
27 Separating the unknown where shall I begin? 69
28 Separation of an unknown sample using a reversed phase C)g column
how do I go about it? 72
29 Developing an RP separation the two day method
Part 1: Choice of column and eluent 74
30 Developing an RP separation the two day method
Part 2: Fine tuning of the separation 78
31 Quick check on peak homogeneity Part 1 80
32 Quick check on peak homogeneity Part 2 82
33 Tied to a standard operating procedure
how can a bad separation be improved further? 84
34 More elaborate measures to check peak homogeneity 86
35 First easily digestible tip 91
36 Second easily digestible tip 94
37 Third easily digestible tip 96
1.4 Troubleshooting 99
38 How to approach problems in a systematic manner 99
39 Spikes in the chromatogram 101
40 Additional peaks in trace analysis separations 103
41 What causes a ghost peak? 105
42 Ghost peaks in a blank gradient 107
43 Strange behaviour of a peak. What could be the cause? 108
44 When could one expect a change in the elution order of the peaks? 110
45 Tailing in RP HPLC Part 1: Fast troubleshooting 114
46 Tailing in RP HPLC Part 2: Further causes and time served cures 116
X
Tip No.
47 Peak deformation and a shift in retention time
due to an unsuitable sample solvent 119
48 Is flushing with water or acetonitrile sufficient? 123
49 Flushing and washing fluids for HPLC apparatus 125
50 When does the peak area change? 127
51 Reasons for a change in either peak height or peak area,
but not in both 129
52 Excesses and their pitfalls 131
53 Algae, fungi and bacteria in HPLC 132
54 Does 40 °C always mean 40 °C? 134
55 The most common reason for a lack of reproducibility
is a lack of methodological robustness 135
Have a break ... 138
Dear Reader 138
Complete the sentences 139
Matching pairs 140
Has Peaky remembered his lessons correctly? 141
1.5 General HPLC Tips 142
56 What changes can you expect when switching from one HPLC system
to another? 142
57 What changes can be expected in a chromatogram if the dead volume
is larger in one isocratic system than in another? 144
58 Contribution of the individual modules of the system
to band broadening 146
59 How to keep retention times constant while reducing the diameter
of the column 148
60 Has 3 |am material been developed sufficiently to be used
in routine separations? 150
61 Miniaturization may be all well and good but when does it really work
and does it make sense in routine separations? 152
62 Why is it that peaks appear later with a new column? 154
63 Column length, flow and retention times in gradient separations 155
64 Column dimensions and gradient separations 159
65 What is the difference between dead time and dead volume on the one hand
and selectivity and resolution on the other? 161
66 Troublesome small peaks 163
67 Lowering the detection limit by optimizing the injection 164
68 Setting the parameters of an HPLC instrument 167
69 The right wavelength old hat to some, a revelation to others 171
70 Characteristics of refraction, fluorescence and conductivity detectors 175
XI
Tip No.
71 Does it always have to be HPLC? 177
72 Methanol versus acetonitrile 180
73 Tale of a foursome pub crawl can peaks elute before the front? 183
References to HPLC Tips 185
2 LC MS Coupling, Micro and Nano LC, Quantification 187
2.1 by Friedrich Mandel, 2.2 by Jiirgen Maier Rosenkranz,
2.3.2 2.3.4 by Hans Joachim Kuss
2.1 LC MS Coupling 187
LC MS The one and only universal tool? 187
Tip No.
74 Choosing the right LC MS interface 189
75 Which mobile phases are compatible with LC MS? 195
76 Phosphate buffers the exception 197
77 Paired ions 198
78 Using additives to enhance API electrospray ionization 200
79 How can I enhance sensitivity of detection? 203
80 No linear response and poor dynamic range? 205
81 How much MS do I need? 208
Need more help? 210
References to LC MS 211
Internet addresses of interest for LC MS coupling 212
2.2 Micro and Nano LC 213
A short introduction 213
Tip No.
82 Lower efficiency plate number too low
Part 1: Effects of dead volume in the connecting parts.
Which column diameter should be used with which capillary
diameter? 214
83 Lower efficiency plate number too low
Part 2: Effects of injection amount and injection volume 215
84 Lower efficiency plate number too low
Part 3: Impact of flow cell (UV, fluorescence, radio detection) 216
85 No gain in sensitivity: flow cell path length S/N 218
86 Fused silica and PEEK capillary connections 219
87 Fast sample loading due to column switching 220
XII
Tip No.
88 Injection system: full loop injection, partial loop fill injection,
timed programmed injection, direct injection 222
89 Protecting the system: cleaning up guard column, saturation column 223
90 Retention time shift: gradient delay volume, mixing chamber volume,
gradient accuracy 224
91 Transferability downscaling: correct gradients 226
References to Micro and Nano LC 228
2.3 Quantification 229
2.3.1 Practical aspects of quantification in HPLC 229
2.3.1.1 Peak area or peak height? 229
2.3.1.2 What factors have an impact on the peak area? 230
2.3.1.3 Formulae and short statements or comments with respect
to the quantification methods 231
2.3.1.4 Examples with actual figures 233
2.3.2 Quantification in Chromatography 236
2.3.2.1 Optimum separation correct peak acquisition 236
2.3.2.2 Understanding the mind of the integration system 240
2.3.2.3 Setting parameters and their effect on peak area and peak height 241
2.3.2.4 Where can mistakes be made? 243
2.3.3 Methods of Quantification 244
2.3.3.1 What is the 100% method? 244
2.3.3.2 What is the external standard method? 244
2.3.3.3 Why use an internal standard? 245
2.3.3.4 In which cases should the additions method be used? 247
2.3.4 Weighted Regression 249
2.3.4.1 What about the F test? What are the other possibilities? 249
2.3.4.2 How do we weight the individual values? 250
2.3.4.3 How to use Excel for weighted regression 250
2.3.5 Solutions to quantification problems 253
References 253
3 Appendix 261
3.1 Solutions to the Problems 261
3.1.1 Crossword the solution 261
3.1.2 An HPLC quiz the solution 261
3.1.3 An HPLC tale with Peaky and Chromy the solution 264
3.1.4 Complete the sentences 265
3.1.5 Matching pairs 266
3.1.6 Did Peaky remember his lessons correctly? 267
XIII
3.2 From Theory to Practice Empirical Formulae, Rules of Thumb
and Simple Correlations in Everyday HPLC 269
3.3 Information Resources for Analysis/HPLC 277
3.4 Analytical Chemistry Today 281
3.5 Trends in HPLC 285
3.6 Thoughts About a Dead Horse 290
Index 291
XIV
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| language | English German |
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| physical | XV, 294 S. Ill., graph. Darst. |
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| spelling | Kromidas, Stavros 1954- Verfasser (DE-588)122124685 aut More practical problem solving in HPLC Stavros Kromidas Weinheim Wiley-VCH 2005 XV, 294 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Aus dem Dt. übers. High performance liquid chromatography Phase partition HPLC (DE-588)4072641-1 gnd rswk-swf Fehlersuche (DE-588)4016615-6 gnd rswk-swf HPLC (DE-588)4072641-1 s Fehlersuche (DE-588)4016615-6 s DE-604 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=012793689&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Kromidas, Stavros 1954- More practical problem solving in HPLC High performance liquid chromatography Phase partition HPLC (DE-588)4072641-1 gnd Fehlersuche (DE-588)4016615-6 gnd |
| subject_GND | (DE-588)4072641-1 (DE-588)4016615-6 |
| title | More practical problem solving in HPLC |
| title_auth | More practical problem solving in HPLC |
| title_exact_search | More practical problem solving in HPLC |
| title_full | More practical problem solving in HPLC Stavros Kromidas |
| title_fullStr | More practical problem solving in HPLC Stavros Kromidas |
| title_full_unstemmed | More practical problem solving in HPLC Stavros Kromidas |
| title_short | More practical problem solving in HPLC |
| title_sort | more practical problem solving in hplc |
| topic | High performance liquid chromatography Phase partition HPLC (DE-588)4072641-1 gnd Fehlersuche (DE-588)4016615-6 gnd |
| topic_facet | High performance liquid chromatography Phase partition HPLC Fehlersuche |
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