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Summary of Contents for Bruker BioSpin minispec mq60
- Page 1 minispec ● minispec mq-Series User Manual Version 001 Innovation with Integrity...
- Page 2 Copyright © by Bruker Corporation All rights reserved. No part of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form, or by any means without the prior consent of the publisher. Product names used are trademarks or registered trademarks of their re- spective holders.
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Page 3: Table Of Contents
Contents Contents About This Manual .......................... 5 Policy Statement ......................... 5 Symbols and Conventions .................... 5 Safety.............................. 7 Intended Use........................ 7 Qualified Personnel...................... 7 Correct Usage........................ 7 Electrical Safety ........................ 8 Lifting Safety ........................ 9 Personal Safety........................ 9 2.6.1 Safety for Persons Wearing Pacemakers ................ 9 2.6.2 Safety During Cryogen Refilling.................. 10 2.6.3 Safety When Working with VT Probe Systems.............. 11 2.6.4... - Page 4 Contents 6.2.1 Direct Cable Connection .................... 34 6.2.2 Connection to a Network.................... 35 Wake-up State of the minispec.exe Software .............. 35 Configuration of the Software, the Welcome Box ............. 35 6.4.1 Selecting Applications and Connections................ 36 6.4.2 Changing Analyser Type and Calibration Permission............ 36 General Measurement Handling .................. 36 List of Standard Applications .................... 37 The minispec Standard Windows .................... 39 The Signal Window ...................... 39...
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Page 5: About This Manual
About This Manual About This Manual This manual enables safe and efficient handling of the device. This manual is an integral part of the device, and must be kept in close proximity to the device where it is permanently accessible to personnel. In addition, instructions concerning labor protection laws, operator regulations tools and supplies must be available and adhered Before starting any work, personnel must read the manual thoroughly and understand its contents. - Page 6 About This Manual WARNING WARNING indicates a hazardous situation, which, if not avoided, could result in death or serious injury. This is the consequence of not following the warning. 1. This is the safety condition. u This is the safety instruction. CAUTION CAUTION indicates a hazardous situation, which, if not avoided, may result in minor or moderate injury or severe material or property damage.
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Page 7: Safety
Safety Safety This manual contains notices which should be observed to ensure your own personal safety as well as to protect the spectrometer and the connected equipment. Intended Use The minispec is a pulsed time-domain NMR analyzer used for the monitoring of NMR receptive nuclei, particularly hydrogen, fluorine and phosphorus, but sometimes other nuclei. -
Page 8: Electrical Safety
Safety Electrical Safety There is no danger of electrical shock during routine operation of the spectrometer, however the following precautions must be followed to assure user safety and protection of the instrument. WARNING Electrical hazard from electrical shock A life threatening shock may result when maintenance is performed. u Place the mains power switch in the OFF position (direction labeled "0"... -
Page 9: Lifting Safety
Safety Lifting Safety The standard magnet unit may weigh up to 150 kg depending on the type of the minispec Analyzer, to ensure safety the follow safety instructions must be followed: CAUTION Risk of injury from lifting heavy objects. The unit is very heavy and may lead to injury when lifting. u Do not attempt to lift the unit over the edge of the carton, remove the carton first. -
Page 10: Safety During Cryogen Refilling
Safety Example of a Stray Field Plot for a Typical 0.47T / 20 MHz Magnet The above figure is an example of a stray filed plot for a typical 0.47T/20 MHz magnet, plots for other frequencies are available in the Pre-installation Manual (included on the minispec software CD or memory stick). -
Page 11: Safety When Working With Vt Probe Systems
Safety 2.6.3 Safety When Working with VT Probe Systems WARNING Danger of injury due to burns (hot/cold) when working with VT probe systems The operator may burn their hands or fingers when touching a very hot or cold sample, or the top of the VT probe. - Page 12 Safety E1400011_1_001...
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Page 13: Transport, Packaging And Storage
Transport, Packaging and Storage Transport, Packaging and Storage Installation, initial commissioning, retrofitting, repairs, adjustments or dismantling of the device must only be carried out by Bruker Service or personnel authorized by Bruker. Damage due to servicing that is not authorized by Bruker is not covered by your warranty. Symbols on the Packaging The following symbols are affixed to the packaging material. -
Page 14: Inspection At Delivery
Transport, Packaging and Storage Do not Damage Air-tight The packaging is air-tight. Damage to the Packaging barrier layer may render the contents unusable. Do not pierce. Do not use sharp objects to open. Component Sensitive to The packaging contains components which Electrostatic Charge are sensitive to an electrostatic charge. -
Page 15: Storage
Transport, Packaging and Storage Storage Storage of the Packages Store the packages under the following conditions: • Do not store outdoors. • Store in dry and dust-free conditions. • Do not expose to aggressive media. • Protect against direct sunlight. •... - Page 16 Transport, Packaging and Storage E1400011_1_001...
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Page 17: Technical Data
Technical Data Technical Data General Information Series Type Weight Length Width Heigth (kg) (cm) (cm) (cm) mq-Series mq60 mq-Series mq40 mq-Series mq20 Airgap 33 mm* mq-Series mq20 Airgap 25 mm* mq-Series mq20 Toothpaste Analyzer mq-Series mq10 mq-Series mq7.5 mq-Series mq20 Airgap 33 mm with PGU* mq-Series mq20 Airgap 25 mm with PGU* mq-Series... -
Page 18: Connection Values
Technical Data Connection Values Electrical Series Type ND/NE/ Voltage/ Apparent Circuit Frequency Power Protection Consumption Maximum/VA mq60 100-240 300/250 3.15 AT 50-60 Series (2 pieces) mq40 100-240 300/250 3.15 AT 50-60 Series (2 pieces) mq20 Airgap 33 100-240 300/250 3.15 AT 50-60 Series (2 pieces) -
Page 19: Operating Conditions
Technical Data Operating Conditions Environment No. Series Type Temperature Temperature Relative Decreasing Range Range Humidity Linear Till Safety Maximum/°C Ideal/°C at 31°C, Relative Class Maximum/ Humidity < 50% at 40°C, Maximum/% mq60 18-28 22-25 80 (non- < 50% IP20 Series condensing) mq40 18-28... -
Page 20: Rating Plate
Technical Data NormaI environmental conditions (CAN/CSA 61010-1-12; IEC 61010-1: 2010; ANSI/UL 61010-1) • Indoor use only. • Maximum operation altitude: 2000 m. • Ideal operating temperature: 22-25 °C. Minimum operating temperature: 18°C maximum operating temperature: 28°C humidity (non-condensing): 20-80%. • Maximum relative humidity 80% for temperatures up to 31 or decreasing linearly to 50% relative humidity at 40 °C. -
Page 21: Introduction
Introduction Introduction The minispec is a benchtop Nuclear Magnetic Resonance (NMR) analyzer for detection of hydrogen ( H), fluorine ( F), and other abundant NMR-active nuclei. Its common application is in polymer, chemical and agrifood industry quality control and quality assurance (QC/QA), where it is routinely used for fast, reproducible and non-destructive analysis. -
Page 22: Improvements
Introduction • minispec Plus Classic • minispec Plus Chemometrics • minispec Plus NoCalibration • minispec Plus Tempering Improvements The minispec mq-Series is the fifth generation of benchtop pulsed NMR analyzers produced by BRUKER. Since the first BRUKER minispec series was introduced in the early 1970’s, there have been many improvements in hardware and software. -
Page 23: Environmental Considerations
Introduction CAUTION Accident or material damage hazard from falling or tilting instrument Instrument may fall down or tilt during installation, retrofitting, dismantling, or while moving on a cart. u Use the carrying handles during lifting. u When a table or cart is used, it should meet the requirements in the site planning guide. u The instrument should be secured to the cart or table. -
Page 24: Installation Of The Minispec Mq-Series
Introduction WARNING Risk to life due to high magnetic fields A magnetic field of more than 0.5 mT (5 Gauss) is life-threatening for people with pacemakers or active metal implants. Exposure to more than 8 T can cause damage to health. Duration of exposure (8 h/day) above the limit of 200 mT can cause damage to health. -
Page 25: Unpacking The System
Introduction Figure 5.2: The minispec Magnet Unit (left) and Electronic Control Unit (right). A number of optional accessories can be added and adapted for use: Gradient Unit (for pulsed field gradient experiments), electronic balances, auto sampler, temperature control baths and variable temperature control units, etc. 5.3.1 Unpacking the System When unpacking the instrument ensure that all components listed in the packing list are part... -
Page 26: Figure 5.3: Handles On The Side Of The Magnet Unit
Introduction CAUTION Risk of injury from lifting heavy objects. The unit is very heavy and may lead to injury when lifting. u Do not attempt to lift the unit over the edge of the carton, remove the carton first. u Do not attempt to lift the unit on your own or without necessary precaution against injury. -
Page 27: Electronic Control And The Magnet Unit Connections
Introduction 8. Remove and retain the clear plastic dust covers from each component of the minispec and inspect them for damage. 9. If either unit appears to be damaged, contact your BRUKER representative immediately. Due to accessories, consumables or optional units packaging may vary. Bruker will make every effort to deliver the instrument damage free. -
Page 28: Electronic Control, Magnet And Gradient Unit Connections
Introduction 5.3.3 Electronic Control, Magnet and Gradient Unit Connections The recommended placement of the Gradient Unit in regards to the minispec is with the Gradient Unit between Magnet and Electronic Control Unit. Cable connections have been constructed with this layout in mind. The sketch and the photo of the back plane of the Gradient Unit below indicate the cable connections between the units. -
Page 29: Specifications Mq-Series
Introduction Specifications mq-Series 5.4.1 Weights and Dimensions Electronic Control Magnet Unit Gradient Unit Unit (optional) Dimensions (W x H x 25 x 33 x 65 47 x 33 x 65 25 x 33 x 65 D) in cm Weight (kg) depends on magnet 5.4.2 Electrical Specifications... -
Page 30: Interpretation Of The Leds
Introduction Interpretation of the LEDs Users receive continuous indication of the status of the different units in the form of light emitting diodes (LEDs), which are built into the front panel of the units. 5.5.1 mq-Series Systems Electronic Control Unit Right LED, connection status indicator: •... -
Page 31: Calibration Samples Hatch And Probe Exchange
Introduction Calibration Samples Hatch and Probe Exchange The Magnet Unit cover has two outer hatches or doors. • The first one is on the front panel of the unit and can be used to contain the calibration samples. Pressing on the upper part of the hatch will unlock and open it. •... - Page 32 Introduction Replace the assembly by following the instructions in reversed order. Intelligent probes were developed for the minispec mq-Series. When you exchange a probe, the software will read the most important parameters (pulse length, resonance frequency) from the probe itself. The software will prompt the user to confirm the settings. After temperature stabilization it is recommended to run the Daily Check procedure.
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Page 33: Getting Started
Getting Started Getting Started In general, minispec systems which are delivered with a personal computer already have the minispec software installed. In this case, the user can skip the software installation instructions (see Software Installation [} 33]) and proceed to the instructions on initialization of the PC-to-minispec connection (see Connecting the PC to the minispec for the First Time [} 34]). -
Page 34: Connecting The Pc To The Minispec For The First Time
Getting Started opening the minispec.exe software. However in some cases it might be useful to first run the minispec.exe software to make sure there is a proper network connection from PC to the minispec, then afterwards switch to minispec Plus program. Please note that for proper installation of minispec Plus software further software requirements may apply, refer to the corresponding minispec Plus manual for details. -
Page 35: Connection To A Network
Getting Started 6.2.2 Connection to a Network A direct connection of the PC and minispec using the blue crossed-wire UTP cable is recommended. When a connection to a network is desired, a second network car will help to establish such a connection. The second network card allows the PC to be connected to the network, while the direct connection from the minispec to the PC is still in place. -
Page 36: Selecting Applications And Connections
Getting Started Several symbols, entries and buttons are displayed in the Welcome Box: • Applications to be loaded (path and file name in the white field). • Serial number of the minispec to be connected to (here: ND1428). • Type of analyzer (here: NMR Analyser). •... -
Page 37: List Of Standard Applications
Getting Started The following sequence of actions is generally followed in preparation for measurements: 1. Turn on your minispec and your PC (if they were turned off). ´ Wait until the console CPU/Ethernet process boots, as indicated by the lighting of the left (green) LEDs located on the front edge of the magnet and console. - Page 38 Getting Started • Additive determinations in polymers. • Polybutadiene/polystyrene content in SBR. • Density in polyethylene. • Crystallinity determinations in polymers. • Spin-finish determinations (OPU and WPU) on textile fibers. • Total hydrogen content determinations in hydrocarbons like: – Jet fuel. –...
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Page 39: The Minispec Standard Windows
The minispec Standard Windows The minispec Standard Windows The minispec user interface provides access to all menu functions, parameters, application programs, NMR signal display, and measurement results. In order to provide ready access to commonly needed views of the software operations, the screen is divided into different parts. To facilitate measurement handling and provide easy access to command commands, icon bars have been integrated into the user interface, and windows are available for the control of the measured signal (Signal Window) and the results (Result Window, Statistics Box). -
Page 40: The Spreadsheet Window
The minispec Standard Windows The Spreadsheet Window Spreadsheets have a number of functions in the minispec software: • They allow a clear data input for the preparation of a measurement series. • They give a listed view of the measurement results. •... -
Page 41: The Minispec Menu Functions
The minispec Menu Functions The minispec Menu Functions The minispec software provides many opportunities for data display, data saving, and measurement handling. This chapter describes all functions that are available when the software is configured as NMR-Analyzer . When the minispec is used only for specialized applications (SFC, OIL) many of these functions are unnecessary. -
Page 42: The File Menu
The minispec Menu Functions Figure 8.1: The Default View The arrangement of the different bars supports an intuitive measurement handling. The File Menu The list of items in the Menu Bar depends on the active window. If the Signal Window is active, and an application is loaded, all entries are visible. - Page 43 The minispec Menu Functions The Open Command Shortcuts: Standard Tool Bar: Keys: CTRL+O Use this command to open an existing document in a new window. One can select either: • A complete minispec application (filename extension .app) consisting of maximum four windows: an editor window with ASCII-text in ExpSpel programming language;...
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Page 44: Figure 8.3: The Dialog Box For Data Saving Setup
The minispec Menu Functions Figure 8.3: The Dialog Box for Data Saving Setup Select Default Storing to backup every 100 result box lines of measured data to the file <application>.mdt in the current working directory. When you attempt to exit the minispec application, the system will prompt whether the data should be saved, deleted or copied into another file. -
Page 45: The Edit Menu
The minispec Menu Functions The Print Preview Command Use this command to display the active document as it would appear when printed. The main window will be replaced with a print preview window in which one or two pages will be displayed in their print format. -
Page 46: The Minispec Menu
The minispec Menu Functions The Select All Command Selects the entire content of the Result Window. In the Signal Window this command is only valid in connection with calibrations. Shortcut Keys: CTRL+A The Unselect All Command Unselects the entire content of the Result Window. In the Signal Window this command is only valid in connection with calibrations. -
Page 47: Figure 8.6: The Minispec Settings Table
The minispec Menu Functions The minispec serial number, which is the host name of the minispec, is used to identify the BRUKER minispec, controlled by the minispec software that is running on a PC in a TCP/IP network. Use the command Disconnect from the menu to disconnect from the current minispec (e.g. prior to reconnecting to another minispec). - Page 48 The minispec Menu Functions The Update Settings Command An update may be necessary after the system has been installed, relocated or the probe assembly has been changed. An instrument settings update is also recommended if the Daily Check fails and no other cause of the failure can be localized. One should first check the sample, the cable connections and the sample position inside the probe before running Update Settings.
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Page 49: The Measurement Menu
The minispec Menu Functions The I/O Port Settings Command One can connect serial interface devices, such as balances, thermostats or sample changers, to the PC's communication port. To get the port configuration dialog, close all minispec applications, then select I/O Port from the Setup menu. Note: To get the minispec main menu, the R&D level or calibration permission must be given. - Page 50 The minispec Menu Functions Measurement Tool Bar: The command Continue is used to leave an intermediate process in order to continue running the minispec application (e.g. during a waiting time, a data acquisition or a fit display). Shortcuts: Standard Tool Bar: Measurement Tool Bar: Keys: ESC The Calibrate Command...
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Page 51: The Parameter Menu
The minispec Menu Functions A flag in the Info Toolbar indicates a calibrated minispec application. An uncalibrated minispec application is labeled with the following flag: The Detect raw Signal Command In some cases, for example to adjust the acquisition parameters, it might be helpful to detect the signal without data processing. -
Page 52: Figure 8.9: The Acquisition Parameter Table
The minispec Menu Functions If the Save button stays disabled on a connected minispec, customize your minispec software to provide access to the calibrated application. Experiment parameters that can be edited through the Acquisition Parameters menu: Figure 8.9: The Acquisition Parameter Table Scans (1 –... -
Page 53: The Application Configuration Table Command
The minispec Menu Functions Dummy Shots (0 - 32000) Pulses before the measurement can be made prior to the experiments, in order to ensure that the first scan has the same magnetization history as all subsequent scans. Static Gradient (x, y, z, -100…+100) If a Pulse Gradient Unit is attached, this parameter (typically x) is used to control a static gradient generated with a constant current to the gradient coils. -
Page 54: The Acquisition Pre-Delay Time Command
The minispec Menu Functions 8.6.3 The Acquisition Pre-Delay Time command In some cases a defined delay is desired between the time a sample is inserted and the time of measurement start (e.g. if time is needed to allow the temperature of the sample to equilibrate in the magnet). - Page 55 The minispec Menu Functions The Info Views Command This command is subdivided into four parts: 1. minispec Settings: If you choose this item you will get a table of all minispec application relevant instrument settings and parameters. Shortcut: Info Toolbar: The function is disabled (grayed) if no minispec is connected.
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Page 56: Figure 8.11: The Statistics Box
The minispec Menu Functions Figure 8.11: The Statistics Box 4. Fit Info: You can display a window containing all information of a current fit. An active Fit Window is marked with a check mark. The Display Modes Command Different display modes are available for the measurement signal. Possible modes are: Figure 8.12: Display Modes You can activate the desired display mode with a mouse click. - Page 57 The minispec Menu Functions Zoom Scale on / off. To zoom, mark the signal with the rectangle cursor. Using the left mouse button you can toggle between the left/upper and the right/lower limit. The zoom range is defined using the right mouse button. To reset, use the right mouse button or click the Reset button.
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Page 58: The Process Menu
The minispec Menu Functions Note: To ensure a failure-free operation use these options only for diagnostic purposes and not in the background for standard measurements. Unmark Diagnostics View and all diagnostic possibilities when they are not any longer required! The Pulse Ram Diagnostics Command This command is only available if the Editor Window is active. -
Page 59: The Window Menu
The minispec Menu Functions The FFT, Magnitude, Power and Absolute Commands A Fast Fourier Transform of measurement data will be performed using the FFT command. If the NMR signal is observed in complex mode (real and imaginary part of the signal) the Magnitude ([Re2+Im2]1/2) or the power spectrum can be calculated. -
Page 60: The Help Menu
The minispec Menu Functions Shortcut Standard Tool Bar: The 1, 2, 3,... Commands Use the numbers or the mouse to select one of the listed windows at the bottom of the menu to set it into the foreground. 8.10 The Help Menu For a user friendly handling the minispec software includes a detailed help function. -
Page 61: The Experiment Editor Expspel For The Mq-Series
The Experiment Editor ExpSpel for the mq-Series The Experiment Editor ExpSpel for the mq-Series The macro programming language ExpSpel was developed to allow the user to design their own experiments and to modify the BRUKER standard applications. In the mq-series a large variety of new commands have been implemented to enlarge the number of experiments. - Page 62 The Experiment Editor ExpSpel for the mq-Series For a detailed description of ExpSpel refer to the extended Help file where all accessible commands and actions are described in detail. Help Topics can be accessed from the Help pull down menu. When the item About: ExpSpel is selected, an overview of ExpSpel is displayed in the index.
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Page 63: 10 Basic Nmr Principles
Basic NMR Principles 10 Basic NMR Principles NMR (Nuclear Magnetic Resonance) is made possible by the properties possessed by some atoms that cause their nuclei (part of every atom) to have a magnetic moment. The atom most commonly investigated by NMR is Hydrogen ( H), the nucleus of which is composed of a single proton. -
Page 64: Figure 10.2: Decay Of The Nmr Signal Due To Transverse Relaxation
Basic NMR Principles Figure 10.2: Decay of the NMR Signal Due to Transverse Relaxation Secondly, the system naturally tends to relax back to the thermal equilibrium. This process is equivalent to the polarization process described above and takes place with the time constant . -
Page 65: 11 Maintenance
Maintenance 11 Maintenance 11.1 Cleaning Before Cleaning Disconnect the mains cable from the unit before cleaning. Cleaning the Main Unit Use a clean damp cloth to wipe off any residue from the outside of the unit. Wipe off excess moisture immediately with a dry cloth. For non water soluble marks, wipe using a cloth with a few drops of isopropyl alcohol. - Page 66 Maintenance E1400011_1_001...
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Page 67: 12 Dismantling And Disposal
Dismantling and Disposal 12 Dismantling and Disposal Following the end of its operational life, the unit can be returned to Bruker for safe disposal. If this is impractical, the unit should be disposed of safely as prescribed by local environmental regulations. - Page 68 Dismantling and Disposal E1400011_1_001...
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Page 69: 13 Contact
WEEE DE43181702 Bruker BioSpin Hotlines Contact our Bruker BioSpin service centers. Bruker BioSpin provides dedicated hotlines and service centers, so that our specialists can respond as quickly as possible to all your service requests, applications questions, software or technical needs. - Page 70 Contact E1400011_1_001...
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Page 71: List Of Figures
List of Figures List of Figures Figure 4.1: The minispec MQ-Series Rating Plate................Figure 5.1: The minispec mq Magnet Unit (left) and Electronic Control Unit (right)......Figure 5.2: The minispec Magnet Unit (left) and Electronic Control Unit (right)......Figure 5.3: Handles on the Side of the Magnet Unit ............... - Page 72 List of Figures E1400011_1_001...
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Page 73: Index
Index File menu............ 42 Index Find command.......... 46 Numerics Help menu ............ 34 1, 2, 3, 4, 5 Commands ........ 45 I/O Port Settings command ...... 49 Inspect the delivery .......... 14 Acquisition parameters ........ 51 Installation CD .......... 33 Add applications .......... 36 Instrument Settings command...... 47 Analyzer type............ 35 IP addresses ............ 34 Application Pools .......... 38 Application programs........ 39... - Page 74 Index Remove applications ........ 36 Result Box ............ 43 Result Window .......... 39 RUN.............. 40 Run command .......... 36 Run Repetitive command ......... 51 Run, Stop and Continue commands .... 49 Save command .......... 43 Save Setup Command ........ 43 Saving in ASCII-format ........ 40 Scans (1 – 32000) .......... 52 Select All command.......... 46 Setup program.......... 33 Signal Window.......... 39...
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- Page 76 ● Bruker Corporation info@bruker.com www.bruker.com Order No: E1400011...
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