Marine Particles: Analysis and Characterization

Marine Particles:analysis And Characterization\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0......Page 5
Copyright\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0......Page 6
Contents\r......Page 7
Workshop Format......Page 9
1.1. Bottle Filtration Methods......Page 13
1.2. In Situ Filtration Methods......Page 15
1.4. Preservation Procedures For Sediment Trap Samples......Page 16
1.6. Procedures For Samples From ReducingEnvironments......Page 17
2. The Workshop Report by Members of the Working Group \"Particle Sampling and Preservation\"......Page 18
2.1.2. Organics.......Page 19
2.2.1. Sieve filters......Page 20
2.2.2. Depth filters.......Page 22
2.3.1. Inorganics.......Page 23
2.4. In Situ Filtration Versus Bottle Samples......Page 24
2.5.2.Organics.......Page 26
2.6. Sample Preservation: Sediment Traps......Page 27
2.6.2. The swimmer problem.......Page 28
References......Page 29
1. Introduction......Page 31
2.1. Pore Size Separations......Page 32
23. Ultracentrifugation......Page 34
2.10. Electrophoresis......Page 35
3. \"Selective\" Chemical and Analytical Methods......Page 36
5. Summary......Page 38
References......Page 39
2.1. Methods Using SCUBA......Page 42
3. Laboratory Handling and Chemical Analysis of Marine Snow and Fecal Pellets......Page 43
3.6. Interstitial Nutrients......Page 44
References......Page 45
2. Water Column Sampling and Sample Handling......Page 46
2.4. Carbonate......Page 47
2.7. Biogenic Particulate Silicate Opal......Page 48
3.2. Preparation of the Collector Cups......Page 49
3.4. Sample Handling Prior to Splitting......Page 50
3.6. Losses of Particulate Matter During Deployment......Page 51
References......Page 54
2.1. Apparatus......Page 56
2.3. Procedures......Page 57
3.1. Sample Acquisition and Preparation......Page 59
3.2 Instrumental Procedures.......Page 60
References......Page 62
2.3. Equipment and Reagents......Page 63
2.6. Sensitivity, Precision, Recovery Efficiency......Page 64
References......Page 65
3. Particulate Organic Phosphorus......Page 66
References......Page 67
3. Definitions and Caveats......Page 68
5.2. Processing......Page 69
6.3. Processing: Total Mass......Page 70
8.2. Analysis......Page 71
9.3. Sinking Particles: PC, PN and PP......Page 72
References......Page 73
2.2. Preparation......Page 75
4. Post Recovery Preparation, Shipboard......Page 76
5.3. Determination of Mass, Total Carbon, OrganicCarbon and Organic Nitrogen......Page 77
References......Page 78
2.3. Sample Collection and Handling......Page 79
2.6. Calibration Procedures......Page 80
References......Page 81
3.2. Procedure......Page 82
4.5. Alternate Method......Page 83
5.4. Comments......Page 84
References......Page 85
2. Particulate Carbon and Nitrogen......Page 86
2.3. Analytical Notes......Page 87
3. Particulate Phosphorus......Page 88
3.1. Procedure For Dried Ground Materials/Filters......Page 89
3.2. Analytical Notes......Page 90
References......Page 91
3.1. Thy Weight......Page 92
4.2. Variances Between Replicate Sediment Traps and Subsamples......Page 93
References......Page 94
1. Introduction......Page 95
2.1.1. Particle type inventories.......Page 97
2.1.2. Organic elemental inventories.......Page 98
2.1.4. Molecular-level inventories......Page 99
2.2.1. Standards and standard reference materials.......Page 100
2.2.3. Chemical modification and instrumental analysis.......Page 102
2.2.4. Recommendations.......Page 103
2.3.1. Adsorption/desorption.......Page 104
2.3.2. Aggregation and disaggregation of particles......Page 106
2.3.4. Recommendations......Page 107
2.4. Optimization of Sampling and Analytical Strategies......Page 108
References......Page 109
5. HPLC Pigment Separations......Page 112
8. Quality Assurance Procedures......Page 113
References......Page 115
3. High Pressure Liquid Chromatography......Page 117
4. Mass Spectral Analysis......Page 118
5. Nuclear Magnetic Resonance Spectrometry NMR......Page 119
References......Page 120
2.1. Published Analytical Method......Page 121
2.2. Procedural Changes......Page 122
3. Cutin Analysis......Page 123
4. Amino Acid Analysis......Page 125
5.1. The Aldose Method......Page 126
References......Page 128
2. Filtration......Page 130
4.1. Hydrolysis......Page 132
4.2. Gas Chromatography......Page 133
4.3.1. Seawater, DFAA.......Page 134
5.2. MBTH Method......Page 136
6. Flow Cytometry......Page 137
References......Page 138
1.2. Polysaccharide Hydrolysis and Depolymerization Techniques......Page 141
1.5. Liquid Chromatography......Page 143
1.5.3. PAD conditions.......Page 144
1.5.4. Sample preparation for LC analysis.......Page 145
2.6. Blank......Page 146
3. Supercritical Fluid Extraction......Page 147
References......Page 148
2.1. Sodium Dodecyl Sulfate - Polyacglamide Gel Electrophoresis SDS-PAGE......Page 152
2.4. Quantification of Protein on the Gel......Page 153
3. Application of PAGE Techniques......Page 154
4. Problems, Artifacts, and Promise......Page 155
References......Page 156
1. Sampling......Page 159
3.2. TLC-FID......Page 160
4. Molecular Composition......Page 162
5.1. Hydrocarbons......Page 163
5.4. Wax Esters and Triacylglycerols......Page 164
References......Page 165
1.1. Methods......Page 168
2.1. Methods......Page 169
3.1. Methods......Page 170
References......Page 171
1. Introduction......Page 173
2.1. Humic Substance Extraction......Page 174
2.2. Ultrafiltration......Page 175
4. Concentration of Organic Colloids by Hollow Fiber Ultrafiltration......Page 176
5. Recommendations......Page 178
References......Page 179
2. Possible In Situ Method......Page 181
References......Page 184
2. Off-Line Separation of Compounds for Isotopic Analysis......Page 185
3. On-Line Compound-Specific Isotopic Analyses......Page 188
References......Page 190
2.2. Lignin......Page 192
2.9. Future Applications of Pyrolysis......Page 193
5. Spectroscopic Methods......Page 194
References......Page 195
1. Introduction......Page 197
3.1.2. In situ filtration.......Page 199
4. Total Dissolution of Suspended Sediments......Page 200
4.2. Acid Dissolution Techniques......Page 201
5.7. X-Ray Fluorescence XRF......Page 202
References......Page 203
2. Basic Digestion Technique Using 1 to 2 g of Material......Page 204
References......Page 205
3. Instrumental Neutron Activation Analysis......Page 206
4. Radiochemical Analysis and Nuclear Counting......Page 207
5. Other Notes on Sediment-Trap Samples......Page 208
References......Page 209
UPDATED DETERMINATION OF PARTICULATE AND DISSOLVED THORIUM-234......Page 210
References......Page 211
3. Suspended Particulate Matter Mass......Page 212
4. Particulate Organic Matter......Page 214
7. Bibliography......Page 215
References......Page 216
3. Loss of \"Labile Substances\" During Storage and Handling......Page 218
3.1. Losses as a Function of Time......Page 219
3.2. Losses as a Function of \'Washing\"......Page 220
4.2 Sample Analysis......Page 221
6. Intercalibration of AA and INAA Techniques......Page 222
7. Sequential Extraction Procedures......Page 224
References......Page 225
2. General Principles......Page 226
3.1. Matrix Effects......Page 228
3.2. Standardization......Page 229
4.1. Flow Injection......Page 230
References......Page 231
2. Samples Collected From a Hydrowire......Page 233
3. Sample Collection With Sediment Traps......Page 235
4. Laboratory Analyses......Page 236
References......Page 238
1. Particle Electrophoresis......Page 240
2. Organic Coatings on Particles......Page 241
3. Sub-Micron Colloidal Particles......Page 242
References......Page 243
3. Reagents......Page 244
6. Ship-Board Sample Processing......Page 245
7.1. Chemical Leaching Techniques......Page 246
7.3. Blanks......Page 247
8. Particulate Metal Profiles in the Sargasso Sea......Page 248
9. Colloid Collection Using Chromatography Resins......Page 249
References......Page 252
3.2. Thiocyanate Formation and Detection......Page 254
References......Page 255
2. Basic Principle and Experimental Set-Up......Page 256
3. Cross-Flow Filters......Page 257
6. Cross-Flow Filtration Procedure......Page 258
7. Filtration Rate......Page 259
References......Page 260
2. Sampling Methods......Page 262
3. Filtering the Plume Samples......Page 263
References......Page 264
1. Introduction......Page 265
2.2. Power......Page 266
2.5. Electronic Control......Page 267
2.7. Deployment Procedure......Page 268
4. Shipboard Procedures......Page 269
5. Laboratory Filter Handling......Page 270
6. Analytical Procedures......Page 271
References......Page 273
2.1. Cartridge Filtration......Page 275
2.3. Membrane Filtration as Applied to Rare EarthElement Studies......Page 277
4. Analytical Methods......Page 279
References......Page 280
3. Collection of Particulate Matter......Page 282
4. Sample Handling......Page 283
6. Major and Trace Element Analyses......Page 284
9. Particulate Matter in Anoxic Seawater......Page 286
References......Page 288
2. Pre-Cruise Preparations......Page 289
3. Sampling......Page 290
4. Filtration......Page 291
References......Page 292
2. Sample Collection......Page 294
4. Sample Digestion and Analysis......Page 295
5. Other Comments on Sampling and Analysis......Page 296
References......Page 297
2. Sample Collection Procedures......Page 298
3. Trace Metal Analysis......Page 299
4. Cross-Flow Filtration......Page 300
References......Page 301
1. Introduction......Page 302
2.1.1. Labile phases: calcium carbonate.......Page 304
2.2. Selective Sampling by Field Equipment......Page 305
3.3. Calcium Carbonate......Page 306
3.4. Filtration as an Analytical Technique: SurfaceProperty Considerations......Page 307
4.2. Mineralogy: Hydrothermal Minerals and the Application of MOssbauer Spectroscopy and Synchrotron X-ray Diffraction......Page 308
4.5. Surface Properties: Dissolution Kinetics of Biogenic Silica......Page 309
4.7. Surface Properties: Metals and Minerals Associated With Bacteria......Page 310
4.9. Surface Properties: Polyfunctional Surface Characteristics......Page 311
4.11. Surface Properties: Interactive Effects of Particles, Colloids and Solutes......Page 312
4.13. Surface Properties: Reaction Rates as a Function of Temperature and Pressure......Page 313
References......Page 314
1. Introduction......Page 320
3.1. Concentration by Fractionation......Page 321
3.4. Conclusions......Page 322
4.2. Specimen Preparation and Specimen Carriers......Page 323
4.3. Internal Standards......Page 325
4.4. Signal and Noise......Page 327
4.4.2. Instrument-sensitive factors:......Page 328
4.5.3. Conditions in the specimen chamber.......Page 330
4.6.4. Peak location and peak intensity.......Page 331
4.7. Quantitative Aspects of XRD Analysis......Page 332
5.1. Opal......Page 333
5.2. Carbonate......Page 334
5.3. Clay Mineral Analysis of Small Amounts of Material......Page 335
References......Page 336
2. Discussion......Page 340
References......Page 343
3. Pre-Cruise Laboratory Preparation......Page 345
4.2. Filtration Procedure......Page 347
6. Discussion......Page 348
References......Page 350
2.1. Sampling of Hydrothermal Plumes......Page 351
2.2. Sample Filtration and Preservation......Page 352
3.1.1. Microprobe system.......Page 353
3.1.2. Standardization.......Page 354
3.2. Synchrotron X-ray Absorption Spectroscopy......Page 357
3.3. Future Applications......Page 359
4. MOssbauer Spectroscopy......Page 360
5. Inductively Coupled Plasma - Mass Spectrometry......Page 362
6. Conclusions......Page 363
References......Page 365
2.4. Large Volume Filtration......Page 367
4.1. Organic Compounds......Page 368
4.2. Mineralogy of Particles......Page 369
4.4. Radioisotopes......Page 370
4.6. Nutrients in the Supernatant......Page 371
References......Page 372
1. Introduction......Page 374
2. Outline of the SPAS......Page 375
3.1. Membrane Filters......Page 376
3.4. Light Microscopy......Page 377
3.5. Binocular Magnifying Glass......Page 380
3.7. Electron Microprobe EDS......Page 381
4. Description of Techniques......Page 382
4.2. Light Microscope Scanning of the Slides......Page 383
4.3. SEM/EMP Mounting......Page 386
4.4. SEM/EMP Study ofthe Filter......Page 387
4.8. LM Stage......Page 388
6. Conclusions......Page 389
References......Page 390
2. Water Sampling Methods......Page 394
3.2. Methods Based on Sample Fraction......Page 395
3.3. Synthesis and Characterization of Synthetic MineralParticles......Page 396
4.1. Sorptive Properties of Particles......Page 397
4.3. Surface Structure of Particles......Page 398
References......Page 400
1.1. Thin Section Material......Page 403
1.1.1. Preparation of samples for micro-analysis by STEM.......Page 404
1.2. Electron Diffraction Analysis......Page 406
2. Time-Series Sediment Traps With Respect toParticle Identification and Micro-analysis......Page 407
3. Marine Snow Collection for Trace Metal Analyses......Page 408
References......Page 409
2. The Evolution of Surface Chemistry as Relevant to Marine Chemistry......Page 411
3. The Surface Complexation Approach......Page 412
3.3. Specific surface area.......Page 413
3.5. Surface Complexation Models of the Particle-Solution Interface......Page 415
5. The Role of Colloidal Material in Marine Chemistry......Page 417
5.1. Evidence For the Importance of Colloids in the Mobility of Trace Elements......Page 418
5.2. Kinetic and Equilibrium Effects of Colloidal Material on Trace Element Behavior......Page 419
References......Page 422
Appendix I. Subject Index\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0\0......Page 426
Appendix II. Author Index......Page 431
APPENDIX III. Glossary of Abbreviations used in Text......Page 442
APPENDIX IV List of trade names and manufacturers referenced in this volume......Page 445