Prodigy / Prodigy XP Operations Manual操作手册（英文版）

仪器资料 · 发表于 2017-6-29 20:24:52

Prodigy / Prodigy XP Operations Manual操作手册

1 TABLE OF CONTENTS

1 TABLE OF CONTENTS 3
2 PRODIGY/PRODIGY XP SAFETY NOTES 9
2.1 PRODIGY/PRODIGY XP SAFETY LABELS 9
3 CONVENTIONS 10
3.1 TRADEMARKS 10
4 PRODIGY/PRODIGY XP QUICK START TUTORIAL 11
4.1 PRODIGY/PRISM/PRODIGY-H OVERVIEW 11
4.2 SALSA OVERVIEW 12
4.3 CREATING A METHOD 14
4.3.1 Method Setup 14
4.3.1.1 Naming the Method 14
4.3.1.2 Entering Elements and Wavelengths 15
4.3.1.3 Entering Standard Concentrations 16
4.3.1.4 Setting Analytical Parameters 17
4.4 IGNITING THE PLASMA 18
4.5 POSITIONING THE PLASMA 19
4.6 SPECTROMETER REFERENCE ALIGNMENT 20
4.6.1 Manual Alignment Method 20
4.6.2 Autoalign Method 21
4.7 CREATING A CUSTOM LINE LIBRARY 21
4.8 WAVELENGTH ALIGNMENT 24
4.8.1 Manual Alignment Method 24
4.8.2 Autoalign Method 25
4.9 COLLECTING WAVELENGTH SPECTRA 25
4.9.1 Collecting Spectral Information for Standards 25
4.9.2 Collecting Spectral Information for Samples 26
4.9.3 Examining Wavelength Scans 26
4.9.3.1 Background Correction 27
4.10 CALIBRATION 27
4.10.1 Reviewing the Calibration Data 28
4.11 SAMPLE ANALYSIS 29
4.12 CREATING SEQUENCES 30
4.12.1 Adding Quality Control Checks 30
4.12.2 Setting up the QC Automation 31
4.12.3 Setting up Sequences 33
4.13 REPORTING RESULTS 34
4.13.1 Paper reports 34
4.13.2 LIMS interfacing 34
5 SAMPLE INTRODUCTION 35
5.1 SELECTING SAMPLE INTRODUCTION SYSTEMS 35
5.1.1 Torch Configuration 35
5.1.1.1 Torches 35
5.1.2 Spray Chambers 36
5.1.2.1 The Cyclonic Spray Chamber 36
5.1.2.2 The Scott Double Pass Spray Chamber 37
5.1.2.3 The HF Resistant Spray Chamber 38
5.1.3 Nebulizers 38
5.1.3.1 The Concentric Nebulizer 38
5.1.3.2 The V-groove Nebulizer 39
5.1.3.3 The Hildebrand Nebulizer 40
5.1.3.4 HF Resistant Nebulizers 40
5.1.3.5 Laser Ablation 41
5.1.4 Tubing Choices 41
5.2 SAMPLE INTRODUCTION SETUP 42
5.2.1 Overview 42
5.2.1.1 Axial Systems 42
5.2.1.2 Radial Systems 43
5.2.2 Installing the Torch 43
5.2.3 Installing the Nebulizer 45
5.2.4 Installing the Spray Chamber 45
5.2.5 Optimizing Sample Introduction 45
6 METHOD DEVELOPMENT 48
6.1 METHODS AND ANALYSIS CHAPTERS 48
6.1.1 Element and Wavelength Selection 48
6.1.1.1 Sensitivity 52
6.1.1.2 Linear Dynamic Range 53
6.1.1.3 Freedom from Interferences 53
6.1.1.4 Atomic vs. Ionic Lines 54
6.1.2 Integrations 54
6.1.3 Rinse Time 55
6.1.4 Uptake Time 55
6.1.5 Peaking Line 55
6.2 PLASMA PARAMETERS 56
6.2.1 RF Power 56
6.2.2 Nebulizer Pressure 57
6.2.3 Coolant Flow 58
6.2.4 Auxiliary Flow 58
6.2.5 Sample Uptake Rate 58
6.2.6 Compromise Operating Conditions 59
6.3 SPECTRAL INTERFERENCES 59
6.3.1 Background Correction 60
6.3.1.1 Simple Background Shift 62
6.3.1.2 Sloping Background 62
6.3.1.3 Curved Background 62
6.3.1.4 Complex Background 62
6.3.2 Spectral Overlap and Interfering Element Correction 63
6.3.2.1 Partial And Direct Spectral Overlap 64
6.3.2.2 Interfering Element Correction Factors 66
6.4 MATRIX INTERFERENCES 70
6.4.1 Sample Introduction System Matrix Effects 70
6.4.2 Plasma Matrix Effects. 71
6.4.3 Determining if Matrix Effects are a Problem 71
6.4.4 Coping with Matrix Effects 74
6.4.4.1 Matrix-Matching 74
6.4.4.2 Method of Standard Addition (MSA) 74
6.4.4.3 Internal Standard 76
6.5 ESTIMATING ANALYTE CONCENTRATIONS IN SAMPLES 78
7 ROUTINE MAINTENANCE AND INSTALLATION 80
7.1 MAINTENANCE SCHEDULE 81
7.1.1 Attention Items 81
7.1.2 Prior to start up 82
7.1.3 At end of day 83
7.1.4 Every Day 83
7.1.5 Every week 83
7.1.6 Every Month 83
7.1.7 Every 2 Months 84
7.1.8 Every 6 Months 84
7.1.9 Annually 84
7.2 MAINTENANCE PROCEDURES 84
7.2.1 Powering off Instrument before Servicing 84
7.2.2 Camera Purge Gas Dehydrator Replacement 86
7.2.3 Changing Argon Gas Cylinders 88
7.2.4 Changing Plasma Viewing Windows in Torch Box 88
7.2.4.1 Axial view window 89
7.2.4.2 Radial view window on Dual-View Prodigy/Prodigy XP 89
7.2.4.3 Radial view window on Radial Prodigy/Prodigy XP 89
7.2.5 Nebulizer 90
7.2.5.1 Concentric Nebulizer 90
7.2.5.2 Hildebrand Grid Nebulizer 90
7.2.6 Cleaning Nebulizer 90
7.2.7 Peristaltic Pump and Tubing 92
7.2.7.1 Setting Tension 92
7.2.7.2 Oiling the Pump 92
7.2.8 Sample Introduction Assembly 92
7.2.8.1 Cleaning the Torch 93
7.2.8.2 Cleaning the Spray Chamber 93
7.2.9 Autosampler Maintenance 93
7.2.10 Camera Water Cooling System 93
7.2.10.1 External Camera Water Cooling System 93
7.2.10.2 Internal Camera Water Cooling System 93
7.2.11 Water Recirculation System 94
7.2.11.1 Chemical Wash 94
7.2.11.2 Cleaning Water Recirculator Filter 95
7.2.12 Cleaning Air Filters 95
7.2.13 Ventilation Requirements 95
7.3 TROUBLESHOOTING 95
7.3.1 Mechanical Problems 96
7.3.1.1 Plasma will not ignite 96
7.3.1.2 Interlocks On Monitor: 97
7.3.2 Camera Full Echellegram Shows Unusual Shapes in Continuum: 99
7.3.3 Instability (High RSDs) 100
7.3.3.1 Sample Introduction System 100
7.3.3.2 Nebulizer 100
7.3.3.3 Parameters 101
7.3.3.4 Conditions 101
7.3.3.5 Leaks 101
7.3.3.6 Chemistry and Labware 101
7.3.3.7 Water System 102
7.3.4 Check Standard Failures 103
7.4 DIAGNOSTICS 104
7.4.1 System Test 104
7.4.2 Autosampler Calibration 104
7.4.3 Resetting Source Mirror 105
7.4.4 Fuse Replacement 105
7.5 CONSUMABLES AND SPARE PARTS 105
7.5.1 Consumables All Plasma Configurations 105
7.5.2 Consumables Axial and Dual View 106
7.5.3 Consumables Radial View 107
7.5.4 Spare Parts All Plasma Configurations 107
7.5.5 Spare Parts Axial and Dual View 108
7.5.6 Spare Parts Radial View 108
7.6 INSTRUMENT SET-UP 108
7.6.1 Installation Short Procedure 108
7.6.2 Reducing Power and Gas Consumption 110
8 SALSA SOFTWARE OVERVIEW 112
8.1 STARTUP LOGIN 114
8.2 MENU BAR 115
8.3 THE TOOL BAR 116
8.4 INSTRUMENT CONTROL BAR 117
8.5 SCHEDULED MAINTENANCE 119
8.6 NAVIGATION PANEL 121
8.7 DETAIL PANEL 122
8.8 STATUS PANEL 123
8.9 COMPUTATION MATHEMATICS 124
8.9.1 Concentration and Calibration Calculations 124
8.9.2 Concentration of Unknown Samples Calculation 125
8.9.3 Update Intercept and Update Slope Calculations 125
8.9.4 Internal Standard Calculations 126
8.9.5 IEC Calculations 127
8.9.6 Duplicate Sample Calculations 128
8.9.7 Spike Recovery and Percent Recovery Calculations 128
8.9.8 Concentration Ratio Calculations 129
8.9.9 Concentration Ratios and Updates 130
8.9.10 Concentration Ratios and Sample Calculations 133
8.9.11 Calculation Sequence and Protocol 134
9 METHOD 135
9.1 OPEN AND CREATING A METHOD 135
9.2 INSTRUMENT CONTROL 137
9.2.1 Autosampler Controls 138
9.2.2 Diagnostics 139
9.2.3 Optimize Sample Intro 141
9.2.4 Plasma controls 142
9.2.5 Pump Controls 143
9.2.6 Spectrometer 144
9.2.7 Torch Gas Controls 145
9.3 ELEMENT SELECTION 146
9.4 LINE SPECIFIC INFORMATION 148
9.4.1 Overview of Line Info 148
9.4.2 General line info 149
9.4.3 Calibration 151
9.4.4 Align Wavelength 152
9.4.4.1 Automatic Alignment of Wavelengths 154
9.4.5 Inter-element Corrections 156
9.4.5.1 How to Apply an IEC 156
9.4.5.2 IEC Example 157
9.5 STANDARDS 159
9.5.1 Update Standards 161
9.5.2 Method of Standard Additions 164
9.6 INTERNAL STANDARDS 165
9.7 CONCENTRATION RATIO 167
9.8 QUALITY CONTROL CHECKS 169
9.9 QC AUTOMATION 171
9.10 ANALYTICAL PARAMETERS 174
9.11 GENERAL 177
10 SEQUENCE 178
10.1 SEQUENCE OVERVIEW 178
10.1.1 Sample Weights and Volumes 179
10.1.2 Autosamplers Available 180
10.1.3 Editing Rack While Running Sequence 182
10.2 CUP MACROS (FLEXIBLE QC AUTOMATION) 184
10.3 SYNCHRONIZING EXTERNAL HARDWARE TO A SAMPLE SEQUENCE 187
10.3.1 SampSync Special Characters or String Commands 188
11 ANALYSIS 189
11.1 ANALYSIS OVERVIEW 189
11.2 RESULTS 190
11.2.1 Hiding Samples and Analysis items 191
11.2.2 Renaming Samples and Analysis items 192
11.3 SCANS 194
11.3.1 Full Scans (Method Development) 195
11.4 PROFILES 196
11.5 RAW DATA 197
11.5.1 TRA Calculation Validation 197
11.6 IMAGE 199
11.6.1 Fingerprint Spectra (QA mode) 200
11.7 CONTROL CHART 203
11.8 REPORT 205
11.8.1 Report Formats 206
11.8.2 Report Limits and Averaging 210
11.8.3 Report Control and Filtration 211
11.8.4 Report Precision Customization 212
11.8.5 Blank Subtraction 213
11.9 QUICK REPORT 215
11.10 RECALCULATE 216
11.11 TIME RESOLVED ANALYSIS (TRA) 218
11.12 RUNNING STANDARDS 223
11.13 RUNNING SAMPLES 225
11.14 RUNNING QC CHECKS 226
11.15 RUNNING MSA ADDITIONS 227
11.16 COLLECTING ECHELLOGRAMS 229
12 GETTING STARTED 231
12.1 CREATING A NEW METHOD 231
12.1.1 Semi-Quantitative Method 231
12.2 ADD QC DIALOG 235
12.3 DISPLAYER (NOT AVAILABLE ON PRODIGY XP) 237
12.4 ECHELLOGRAMS 238
12.5 IDENTIFIER (NOT AVAILABLE ON PRODIGY XP) 241
12.6 METHOD LINES 242
12.7 MODIFY QC DIALOG 243
12.8 NEW RACK 244
12.9 OPEN SAMPLE RACK FILE 245
12.10 SAVE RACK FILE 246
12.11 SPECTRAL IMAGES (NOT AVAILABLE ON PRODIGY XP) 247
12.12 UPDATE INTERCEPT 248
12.13 UPDATE SLOPE 249
12.14 USER LOGIN ADMINISTRATION 250
12.15 DATABASE MANAGEMENT 253