Sample preparation techniques in analytical chemistry:
Gespeichert in:
| Format: | Buch |
|---|---|
| Sprache: | English |
| Veröffentlicht: |
Hoboken, NJ
Wiley-Interscience
2003
|
| Schriftenreihe: | Chemical analysis
162 |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis Klappentext |
| Beschreibung: | XX, 458 S. Ill., graph. Darst. |
| ISBN: | 0471328456 |
Internformat
MARC
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| 245 | 1 | 0 | |a Sample preparation techniques in analytical chemistry |c ed. by Somenath Mitra |
| 264 | 1 | |a Hoboken, NJ |b Wiley-Interscience |c 2003 | |
| 300 | |a XX, 458 S. |b Ill., graph. Darst. | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 490 | 1 | |a Chemical analysis |v 162 | |
| 650 | 4 | |a Sampling | |
| 650 | 4 | |a Chemistry, Analytic |x Methodology | |
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| 689 | 1 | 1 | |a Probenahme |0 (DE-588)4047319-3 |D s |
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| 830 | 0 | |a Chemical analysis |v 162 |w (DE-604)BV000008780 |9 162 | |
| 856 | 4 | 2 | |m Digitalisierung UB Bayreuth - ADAM Catalogue Enrichment |q application/pdf |u http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000003&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |3 Inhaltsverzeichnis |
| 856 | 4 | 2 | |m Digitalisierung UB Bayreuth - ADAM Catalogue Enrichment |q application/pdf |u http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000004&line_number=0002&func_code=DB_RECORDS&service_type=MEDIA |3 Klappentext |
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Datensatz im Suchindex
| _version_ | 1804129819480293376 |
|---|---|
| adam_text | CONTENTS
CONTRIBUTORS
PREFACE
CHAPTER
1
SAMPLE PREPARATION: AN
ANALYTICAL PERSPECTIVE
Somenath
Mitra
and Roman Brukh
1.1.
1.2.
1.3.
1.4.
xvu
xix
The Measurement Process
1
1.1.1.
Qualitative and Quantitative
Analysis
3
1.1.2.
Methods of
Quantita
ti
on
4
Errors in Quantitative Analysis: Accuracy
and Precision
6
1.2.1.
Accuracy
6
1.2.2.
Precision
6
1.2.3.
Statistical Aspects of Sample
Preparation
10
Method Performance and Method
Validation
12
1.3.1.
Sensitivity
13
1.3.2.
Detection Limit
14
1.3.3.
Range of Quantitation
15
1.3.4.
Other Important Parameters
15
1.3.5.
Method Validation
16
Preservation of Samples
17
1.4.
1
.
Volatilization
19
1,4.2.
Choice of Proper Containers
19
1.4.3.
Absorption of Gases from the
Atmosphere
20
1.4.4.
Chemical Changes
20
1.4.5.
Preservation of Unstable Solids
20
vu
VIH
CONTENTS
SECTION A
1.5.
Postextraction
Procedures
1.5.1.
Concentration of Sample Extracts
1.5.2.
Sample Cleanup
1.6.
Quality Assurance and Quality Control
during Sample Preparation
1.6.1.
Determination of Accuracy and
Precision
1.6.2.
Statistical Control
1.6.3.
Matrix Control
1.6.4.
Contamination Control
References
EXTRACTION AND ENRICHMENT IN
SAMPLE PREPARATION
21
21
22
25
28
29
31
32
35
CHAPTER
2
PRINCIPLES OF EXTRACTION AND THE
EXTRACTION OF SEMIVOLATILE
ORGANICS FROM LIQUIDS
Martha J. M. Wells
37
2.1.
Principles of Extraction
37
2.1.1.
Volatilization
38
2.1.2.
Hydrophobicity
43
2.1.3.
Acid-Base Equilibria
50
2,1.4.
Distribution of
Hydrophobie
Ionogenic Organic Compounds
57
2.2.
Liquid-Liquid Extraction
57
2.2.1.
Recovery
60
2,2.2.
Methodology
66
2.2.3.
Procedures
68
2.2.4.
Recent Advances in Techniques
72
2.3.
Liquid
l-Solid Extraction
74
2.3.1.
Sorption
75
2.4.
Solid-Phase Extraction
78
2.4.1.
Sorbente in
SPE
81
2,4.2.
Sorbent
Selection
96
2.4.3.
Recovery
99
2.4.4.
Methodology
108
CONTENTS
ІХ
2.4.5.
Procedures
111
2.4.6.
Recent
Advances
in SPE
11
3
2.5,
Solid-Phase Microextraction
113
2.5.1.
Sorbents
116
2.5.2.
Sorbent
Selection
118
2.5.3.
Methodology
119
2.5.4.
Recent Advances in Techniques
124
2.6,
Stir Bar Sorptive Extraction
125
2.6.1.
Sorbent
and Analyte Recovery
125
2.6.2.
Methodology
127
2.6.3.
Recent Advances in Techniques
129
2.7,
Method Comparison
130
References
131
CHAPTER
3
EXTRACTION OF SEMIVOLATILE
ORGANIC COMPOUNDS FROM SOLID
MATRICES
139
Dawen
Kou
and Somenath
Mitra
3.1,
Introduction
139
3.1.1.
Extraction Mechanism
140
3.1.2.
Preextraction Procedures
141
3.1.3.
Postextraction
Procedures
141
3.2,
Soxhlet and Automated Soxhlet
142
3.2.1.
Soxhlet Extraction
142
3.2.2.
Automated Soxhlet Extraction
143
3.2.3.
Comparison between Soxtec and
Soxhlet
145
3.3,
Ultrasonic Extraction
145
3.3.1.
Selected Applications and
Comparison with Soxhlet
147
3.4,
Supercritical Fluid Extraction
148
3.4.1.
Theoretical Considerations
148
3.4.2.
Instrumentation
152
3.4.3.
Operational Procedures
153
3.4.4.
Advantages/Disadvantages and
Applications of SFE
154
3.5,
Accelerated Solvent Extraction
155
CONTENTS
3.6.
3.7.
3.5Л.
Theoretical Considerations
155
3.5.2.
Instrumentation
156
3.5.3.
Operational Procedures
158
3.5.4.
Process Parameters
159
3.5.5.
Advantages and Applications of
ASE
161
Microwave-Assisted Extraction
163
3.6.1.
Theoretical Considerations
163
3.6.2.
Instrumentation
164
3.6.3.
Procedures and Advantages/
Disadvantages
170
3.6.4.
Process Parameters
170
3.6.5.
Applications of MAE
173
Comparison of the Various Extraction
Techniques
173
References
178
CHAPTER
4
EXTRACTION OF VOLATILE ORGANIC
COMPOUNDS FROM SOLIDS AND
LIQUIDS
183
Gregory C. Stack, Nicholas H. Snow, and
Danen
Кои
4.1.
Volatile Organics and Their Analysis
183
4.2.
Static Headspace Extraction
184
4.2.1.
Sample Preparation for Static
Headspace Extraction
186
4.2.2.
Optimizing Static Headspace
Extraction Efficiency and
Quantitation
187
4.2.3.
Quantitative Techniques in Static
Headspace Extraction
190
4.3.
Dynamic Headspace Extraction or Purge
and Trap
194
4.3.1.
Instrumentation
194
4.3.2.
Operational Procedures in Purge
and Trap
199
4.3.3.
Interfacing Purge and Trap with
GC
199
4.4.
Solid-Phase
Microextraction
200
CONTENTS
XI
4.5.
4.6.
4.4.1.
SPME Method Development for
Volatile Organics
201
4.4.2.
Choosing an SPME Fiber Coating
204
4.4.3.
Optimizing Extraction Conditions
206
4.4.4.
Optimizing SPME-GC Injection
207
Liquid-Liquid Extraction with Large-
Volume Injection
208
4.5.1.
Large-Volume GC Injection
Techniques
208
4.5.2.
Liquid-Liquid Extraction for
Large-Volume Injection
211
Membrane Extraction
212
4.6.1.
Membranes and Membrane
Modules
215
4.6.2.
Membrane Introduction Mass
Spectrometry
217
4.6.3.
Membrane Extraction with Gas
Chromatography
218
4.6.4.
Optimization of Membrane
Extraction
222
Conclusions
223
References
223
4.7.
CHAPTER
5
PREPARATION OF SAMPLES FOR
METALS ANALYSIS
227
Barbara B. Kebbekus
5.1.
Introduction
227
5.2.
Wet Digestion Methods
230
5.2.1.
Acid Digestion
—
Wet Ashing
231
5.2.2.
Microwave Digestion
234
5.2.3.
Comparison of Digestion Methods
235
5.2.4.
Pressure Ashing
237
5.2.5.
Wet Ashing for Soil Samples
237
5.3.
Dry Ashing
240
5.3.1.
Organic Extraction of Metals
241
5.3.2.
Extraction with Supercritical Fluids
244
5.3.3.
Ultrasonic Sample Preparation
245
хи
CONTENTS
SECTION
В
CHAPTER
6
5.4.
Solid-Phase Extraction for Preconcentration
245
5.5.
Sample Preparation for Water Samples
248
5.6.
Precipitation Methods
251
5.7.
Preparation of Sample Slurries for Direct
AAS
Analysis
251
5.8.
Hydride Generation Methods
252
5.9.
Colorimetrie
Methods
254
5.10.
Metal Speciation
255
5.10,
1
.
Types of Speciation
257
5.10.2.
Speciation for Soils and Sediments
258
5.10.3.
Sequential Schemes for Metals in
Soil or Sediment
259
5.10.4.
Speciation for Metals in Plant
Materials
260
5.10.5.
Speciation of Specific Elements
262
5.11.
Contamination during Metal Analysis
263
5.12.
Safe Handling of Acids
264
References
264
SAMPLE PREPARATION FOR NUCLEIC
ACID ANALYSIS
SAMPLE PREPARATION IN
ONA
ANALYSIS
271
Satish Parimoo and Bhama Parimoo
6.1. DNA
and Its Structure
271
6.1.1.
Physical and Chemical Properties of
DNA 274
6.1.2.
Isolation of
DNA 276
6.2.
Isolation of
DNA
from Bacteria
278
6.2.1.
Phenol Extraction and Precipitation
of
DNA 278
6.2.2.
Removal of Contaminants from
DNA 282
6.3.
Isolation of Plasmid
DNA 283
6.3.1.
Plasmid
DNA
Preparation
284
6.3.2.
Purification of Plasmid
DNA 285
6.4.
Genomic
DNA
Isolation from Yeast
287
CONTENTS
ХІІІ
6.5.
DNA
from Mammalian Tissues
288
6.5.1.
Blood
288
6.5.2.
Tissues and Tissue Culture Cells
289
6.6.
DNA
from Plant Tissue
290
6.7.
Isolation of Very High Molecular Weight
DNA
290
6.8.
DNA
Amplification by Polymerase Chain
Reaction
291
6.8.1.
Starting a PCR Reaction
291
6.8.2.
Isolation of
DNA
from Small Real-
World Samples for PCR
294
6.9.
Assessment of Quality and Quantitation of
DNA
296
6.9.1.
Precautions for Preparing
DNA
296
6.9.2.
Assessment of Concentration and
Quality
296
6.9.3.
Storage of
DNA
299
Refere
inces
299
CHAPTER
7
SAMPLE PREPARATION IN
RNA
ANALYSIS
301
Bhama Parimoo and Satish Parimoo
7.1.
RNA:
Structure and Properties
301
7
Л
. 1.
Types and Location of Various
RNAs
303
7.2.
RNA
Isolation: Basic Considerations
306
7.2.1.
Methods of Extraction and
Isolation of
RNA
307
7.3.
Phenol Extraction and
RNA
Recovery:
Bask Principles
309
7.3.1.
Examples of
RNA
Isolation Using
Phenol Extraction
310
7.4.
Guanidinium Salt Method
313
7.4.1.
Examples of
RNA
Isolation Using
Guanidinium Salts
ЗІЗ
7.5.
Isolation of
RNA
from Nuclear and
Cytoplasmic Cellular Fractions
317
XIV CONTENTS
7.6.
Removal of
DNA
Contamination from
RNA
317
7.7.
Fractionation of
RNA
Using
Chromatography Methods
318
7.7.1.
Fractionation of Small
RNA
by
HPLC
318
11.2.
mRNA Isolation by Affinity
Chromatography
319
7.8.
Isolation of
RNA
from Small Numbers of
Cells
323
7.9.
In Vitro Synthesis of
RNA
324
7.10.
Assessment of Quality and Quantitation of
RNA
326
7.11.
Storage of
RNA
328
References
329
CHAPTER
8
TECHNIQUES FOR THE EXTRACTION,
ISOLATION, AND PURIFICATION OF
NUCLEIC ACIDS
331
Afahesh Karwa and Somenath
Mitra
8.1.
Introduction
331
8.2.
Methods of Cell Lysis
333
8.2.1.
Mechanical Methods of Cell Lysis
335
8.2.2.
Nonmechanical Methods of Cell
Lysis
339
8.3.
Isolation of Nucleic Acids
342
8.3.1.
Solvent Extraction and
Precipitation
344
8.3.2.
Membrane Filtration
345
8.4. Chromatographie
Methods for the
Purification of Nucleic Acids
346
8.4.1.
Size-Exclusion Chromatography
347
8.4.2.
Anion-Exchange Chromatography
348
8.4.3.
Solid-Phase Extraction
351
8.4.4.
Affinity Purification
352
8.5.
Automated High-Throughput
DNA
Purification Systems
355
8.6.
Eîectrophoretic
Separation of Nucleic Acids
360
CONTENTS
XV
8.6.1. Gel Electrophoresis
for Nucleic
Acids Purification
360
8.6.2.
Techniques for the Isolation of
DNA
from Gels
362
8.7.
Capillary Electrophoresis for Sequencing
and Sizing
364
8.8. Microfabricated
Devices for Nucleic Acids
Analysis
366
8.8.1.
Sample Preparation on Microchips
370
References
373
SECTION
С
SAMPLE PREPARATION IN MICROSCOPY
AND SPECTROSCOPY
CHAPTER
9
SAMPLE PREPARATION FOR
MICROSCOPIC AND SPECTROSCOPIC
CHARACTERIZATION OF SOLID
SURFACES AND FILMS
377
Sharmtla M. Mukhopadhyay
9.1.
Introduction
377
9.1.1.
Microscopy of Solids
378
9.1.2.
Spectroscopie
Techniques for Solids
381
9.2.
Sample Preparation for Microscopic
Evaluation
382
9.2.
L
Sectioning and Polishing
382
9.2.2.
Chemical and Thermal Etching
385
9.2.3.
Sample Coating Techniques
387
9.3.
Specimen Thinning for
ТЕМ
Analysis
389
9.3.1.
Ion Milling
391
9.3.2.
Reactive Ion Techniques
393
9.3.3.
Chemical Polishing and
Electropolishing
394
9.3.4.
Tripod Polishing
396
9.3.5.
Ultramicrotomy
398
9.3.6.
Special Techniques and Variations
399
Summary: Sample Preparation for
Microscopy
400
9.4.
XVI
CONTENTS
9.5.
Sample Preparation for Surface
Spectroscopy
402
9.5.1.
Ion Bombardment
407
9.5.2.
Sample Heating
408
9.5.3.
In Situ Abrasion and Scraping
408
9.5.4.
In Situ Cleavage or Fracture Stage
408
9.5.5.
Sample Preparation/Treatment
Options for In Situ Reaction
Studies
409
9.6.
Summary: Sample Preparation for Surface
Spectroscopy
409
References
410
CHAPTER
10
SURFACE ENHANCEMENT BY SAMPLE
AND SUBSTRATE PREPARATION
TECHNIQUES
ÏN
RAMAN AND INFRARED
SPECTROSCOPY
413
Zafar Iqbal
10.1.
Introduction
413
10.1.1.
Raman Effect
413
10.1.2.
Fundamentals of Surface-Enhanced
Raman Spectroscopy
415
10.1.3.
Attenuated Total Reflection
Infrared Spectroscopy
420
10.1.4.
Fundamentals of Surface-Enhanced
Infrared Spectroscopy
421
10.2.
Sample Preparation for
SERS
423
10.2.1.
Electrochemical Techniques
423
10.2.2.
Vapor Deposition and Chemical
Preparation Techniques
424
10.2.3.
Colloidal Sol Techniques
425
10.2.4.
Nanoparticle Arrays and Gratings
427
10.3.
Sample Preparation for
SEIRA
431
10.4.
Potential Applications
433
References
436
INDEX
439
A· If
il
groundbreaking guide devoted
entirely to sample preparations
The importance of accurate sample preparation techniques cannot be over¬
stated
—
meticulous sample preparation is essential.
Oken
overlooked, it is
the midway point where the analytes from the sample matrix are transformed
so thev are suitable for analysis. Even the best analytical techniques cannot
Kairy
problems generated by sloppy sample
pretreatment.
Devoted entirely to teaching and reinforcing these necessary
pretreatment
steps. Sample Preparation Techniques in Analytical Chemistry addresses diverse
aspects of this important measurement step. These include:
•
State-of-the-art extraction techniques for organic and inorganic analytes
•
Sample preparation in biological measurements
•
Sample
pretreatment
in
microscop)
•
Surface enhancement as a sample preparation tool in Raman and
IR
>pectroscopy
•
Sample concentration and clean-up methods
Quality control steps
Designed to
sene
as a text in an undergraduate or graduate level curriculum,
Sample
Préparation
Techniques in Analytical Chemistry also provides an
invaluable reference tool tor analytical chemists in the chemical, biological,
pharmaceutical, environmental, and materials sciences.
is Professor of Chemistry and Environmental
Science at the New Jersej
institute
of Technology. He is coauthor of the textbook
Environmental Chemical Analysis. In addition, he has published extensiveh
їй
peer-reviewed journals of cbemistr) and analytical sciences.
|
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| author_GND | (DE-588)173187498 |
| building | Verbundindex |
| bvnumber | BV016498293 |
| callnumber-first | Q - Science |
| callnumber-label | QD75 |
| callnumber-raw | QD75.4.S24 |
| callnumber-search | QD75.4.S24 |
| callnumber-sort | QD 275.4 S24 |
| callnumber-subject | QD - Chemistry |
| classification_rvk | VG 5000 VG 5150 |
| classification_tum | CHE 216f |
| ctrlnum | (OCoLC)51518388 (DE-599)BVBBV016498293 |
| dewey-full | 543 |
| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
| dewey-raw | 543 |
| dewey-search | 543 |
| dewey-sort | 3543 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie Chemie |
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| id | DE-604.BV016498293 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T19:11:12Z |
| institution | BVB |
| isbn | 0471328456 |
| language | English |
| lccn | 2003001379 |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-010197205 |
| oclc_num | 51518388 |
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| owner_facet | DE-20 DE-19 DE-BY-UBM DE-91G DE-BY-TUM DE-Er8 DE-526 DE-83 DE-703 |
| physical | XX, 458 S. Ill., graph. Darst. |
| publishDate | 2003 |
| publishDateSearch | 2003 |
| publishDateSort | 2003 |
| publisher | Wiley-Interscience |
| record_format | marc |
| series | Chemical analysis |
| series2 | Chemical analysis |
| spelling | Sample preparation techniques in analytical chemistry ed. by Somenath Mitra Hoboken, NJ Wiley-Interscience 2003 XX, 458 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Chemical analysis 162 Sampling Chemistry, Analytic Methodology Analytische Chemie (DE-588)4129906-1 gnd rswk-swf Probenahme (DE-588)4047319-3 gnd rswk-swf Probenvorbereitung (DE-588)4588977-6 gnd rswk-swf Analytische Chemie (DE-588)4129906-1 s Probenvorbereitung (DE-588)4588977-6 s DE-604 Probenahme (DE-588)4047319-3 s Mitra, Somenath 1959- Sonstige (DE-588)173187498 oth Chemical analysis 162 (DE-604)BV000008780 162 Digitalisierung UB Bayreuth - ADAM Catalogue Enrichment application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000003&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis Digitalisierung UB Bayreuth - ADAM Catalogue Enrichment application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000004&line_number=0002&func_code=DB_RECORDS&service_type=MEDIA Klappentext |
| spellingShingle | Sample preparation techniques in analytical chemistry Chemical analysis Sampling Chemistry, Analytic Methodology Analytische Chemie (DE-588)4129906-1 gnd Probenahme (DE-588)4047319-3 gnd Probenvorbereitung (DE-588)4588977-6 gnd |
| subject_GND | (DE-588)4129906-1 (DE-588)4047319-3 (DE-588)4588977-6 |
| title | Sample preparation techniques in analytical chemistry |
| title_auth | Sample preparation techniques in analytical chemistry |
| title_exact_search | Sample preparation techniques in analytical chemistry |
| title_full | Sample preparation techniques in analytical chemistry ed. by Somenath Mitra |
| title_fullStr | Sample preparation techniques in analytical chemistry ed. by Somenath Mitra |
| title_full_unstemmed | Sample preparation techniques in analytical chemistry ed. by Somenath Mitra |
| title_short | Sample preparation techniques in analytical chemistry |
| title_sort | sample preparation techniques in analytical chemistry |
| topic | Sampling Chemistry, Analytic Methodology Analytische Chemie (DE-588)4129906-1 gnd Probenahme (DE-588)4047319-3 gnd Probenvorbereitung (DE-588)4588977-6 gnd |
| topic_facet | Sampling Chemistry, Analytic Methodology Analytische Chemie Probenahme Probenvorbereitung |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000003&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=010197205&sequence=000004&line_number=0002&func_code=DB_RECORDS&service_type=MEDIA |
| volume_link | (DE-604)BV000008780 |
| work_keys_str_mv | AT mitrasomenath samplepreparationtechniquesinanalyticalchemistry |