1593626 en DuMaster D-480 Operation Manual
Imprint Product Identification: Operation Manual, DuMaster D-480 11593626 en BÜCHI Labortechnik AG Meierseggstrasse 40 Postfach CH-9230 Flawil 1 E-Mail: quality@buchi.
Copyright Note 3 Copyright © BÜCHI Labortechnik AG All rights reserved This document contains proprietary information of BÜCHI Labortechnik AG. Reprint is prohibited. Due to continued product development this information may change without notice. The information and intellectual property contained herein is confidential between BÜCHI Labortechnik AG and the client and remains the exclusive property of BÜCHI Labortechnik AG.
Contents 5 Contents CHAPTER 1 General 13 Revision history ........................................................................................................................................... 14 About this document.................................................................................................................................... 15 Display conventions ....................................................................................................................................
Contents 6 Understanding the operating software......................................................................................................... 59 Basic functions of the operating software......................................................................................... 60 Software user interface .................................................................................................................... 61 Sample view.................................................................
Contents 7 Start-up .......................................................................................................................................... 109 Connecting peripherals .................................................................................................................. 110 Connecting supply lines and waste gas lines ................................................................................. 111 Removing the transport protection .........................................
Contents 8 Setting the size of the graph .......................................................................................................... 156 Configure report ............................................................................................................................. 157 Display print preview ...................................................................................................................... 157 Data backup and printing .........................................
Contents 9 Filling, removing and installing the absorption and drying tubes ............................................................... 233 Filling the drying tubes ................................................................................................................... 234 Removing and installing the drying tubes....................................................................................... 236 CHAPTER 9 Repairing the instrument 239 Interpreting PC error messages ................
Contents 10 Column properties (Dialog) ............................................................................................................ 283 Save views (Dialog) ....................................................................................................................... 284 Load views (Dialog)........................................................................................................................ 285 Delete views (Dialog) ................................................
Contents 11 Statistics > Clear statistic (Command) ........................................................................................... 332 Statistics > Include/Exclude sample (Command) ........................................................................... 333 Statistics > Include/Exclude value (Command) .............................................................................. 333 Calibration menu ............................................................................................
CHAPTER 1 General Purpose This chapter contains general topics of the document. In this chapter Revision history .............................................................................................................................14 About this document ......................................................................................................................15 Display conventions.............................................................................................................
1 - General 14 Revision history List of modifications in this document up to now Date Operation Manual D-480 Modification ©BÜCH Labortechnik AG
1 - General 15 About this document Status of the operating instructions The status of the operating instructions is: 27.08.2013. Identification number The operating instructions identification number is: 11593626. Validity The operating instructions are valid for all instruments as from serial number: 16091001. Analyzer The operating instructions describe the basis type of the instrument D-480 in N operation mode.
1 - General 16 Display conventions Before you start using this guide, it is important to understand the terms and typographical conventions used in the documentation. The following kinds of formatting in the text identify special information. Formatting convention Type of information Triangular bullet () Step by step procedure. You can follow these instructions to complete a specific task. Special bold Items you must select, such as menu options (e. g. File > New), command buttons (e. g.
CHAPTER 2 Basic security settings Target group Personnel working with the instrument. Purpose This section describes basic safety rules required to avoid risks for the user of the analyzer. In this chapter Working with the operating instructions .........................................................................................18 Representation of safety instructions.............................................................................................
2 - Basic security settings 18 Working with the operating instructions Operating the analyzer Read the operating instructions thoroughly before performing work with the analyzer. Storing the operating instructions Store the operating instructions carefully and make sure the instructions are accessible for all relevant personnel. Passing on the operating instructions If you pass on the analyzer, always pass on the operating instructions, too.
2 - Basic security settings 19 Read the instructions on the individual chemicals in the safety data sheets. The risk notes for individual chemicals can be found in the R-Phrases. Safety advice can be found in the SPhrases. Intended use of the instrument Intended use This section describes what the instrument is suitable for and what substances may be analyzed with it. Description of the instrument The elementary analyzer is an instrument for fully automatic and quantitative analysis of the element N.
2 - Basic security settings 20 Contact with the substances may lead to chemical burns or poisoning. Combustion analysis of larger quantities of the substance may lead to explosions.
2 - Basic security settings Front door Left side door Rear wall Instrument cover. 21 The casing separates hot, live parts from the surroundings. Protective earth conductor The electrical components of the analyzer are grounded by a protective earth conductor: The first protective earth conductor is located on the rear wall of the analyzer. The second protective earth conductor is located outside the cover of the electrical area (arrow).
2 - Basic security settings 22 Warning signs on the analyzer Warning sign furnace The following picture shows the warning sign on the furnace heat protection cladding: Warning sign electrical area The following picture shows the warning sign on the electrical section cover: Meaning of the warning signs The following table explains the meaning of the warning signs: Warning sign Meaning Warning: hot surfaces Electric current hazard Note You are obliged to keep the warning signs on the instrument comple
2 - Basic security settings 23 Warning: changes to the instrument Safe instrument The analyzer is designed and delivered in such a way to ensure safe working if you observe the instructions in the operating instructions. Warning: Changes to the instrument If you make any changes to the instrument, you risk rendering the instrument unsafe. The consequences would be: Injuries to the operating personnel Damages to the instrument loss of warranty.
2 - Basic security settings 24 Required personal safety equipment Protective glasses You require protective glasses for many activities. Make sure that protective glasses are always available nearby the analyzer. Protective gloves BÜCHI two kinds of protective gloves with the instrument: The protective leather gloves for protection against cuts on broken glass from cold quartz components. The heat protection gloves for protection against burns on hot components.
2 - Basic security settings 25 Damaged base panel Please observe the following instruction: Caution Damaged base panel! Damage to the base panel will impair proper functioning of the carousel. Before starting maintenance work, always remove all samples from the carousel. When dismantling and cleaning the carousel: Never use pointed objects to dismantle the carousel. Never use sharp or aggressive cleaners.
2 - Basic security settings 26 Removing reaction tubes Please observe the following instructions: Warning Hot reaction tubes! Risk of burning due to hot instrument parts. When replacing the reaction tubes: Warning Wear protective glasses. Wear the enclosed heat protection gloves. Place the hot tubes in a tube rack on a level, non-combustible surface. Protect the hot tubes from unauthorized access. Never leave the instrument unattended when the furnace has been pulled out.
2 - Basic security settings Warning 27 Harmful substances when glass is broken! When filled quartz or glass components break there is a risk that harmful substances may be released. Wear a dust mask when handling cold quartz and glass parts. Replacing fuses Please observe the following instructions: Risk Live parts! When replacing fuses there is a risk of electrocution. Before replacing fuses: Risk Allow the furnaces to cool down. Disconnect the power supply plug.
2 - Basic security settings 28 Overheating of tube fillings Please observe the following instruction: Caution Overheating if tube fillings are not appropriate for the operating mode! Overheated tube fillings melt, run into the furnace area and destroy the furnace. Make sure that the tube fillings correspond to the selected operating mode.
CHAPTER 3 Product description Target group Personnel working with the instrument. Purpose This section provides general information about the instrument. In this chapter Analytical characteristics and technical specifications ...................................................................30 Instrument design ..........................................................................................................................
3 - Product description 30 Analytical characteristics and technical specifications Target group Personnel working with the instrument. Purpose This section lists the analytical characteristics and technical specifications. In this section Analytical characteristics ...............................................................................................................31 Technical specifications........................................................................................................
3 - Product description 31 Analytical characteristics Analytical characteristics The following table explains the analytical characteristics: Analytical characteristic Comments Analysis method Nitrogen determination from a sample according to Dumas. Combustion of the samples, transfer to N2, separation of foreign gases, thermal conductivity detection. Standards Analysis method according to: AOAC 99.03, AOAC 993.13, AOAC 968.06, AOAC 992.15, AOAC 992.
3 - Product description Interfaces 32 USB, RS232 /V24, Safety low voltage as per DIN IEC 380/VDE 0806/08.
3 - Product description 33 Instrument design Target group Personnel involved with the instrument. Purpose This section describes the design of the instrument. In this section Front view ......................................................................................................................................34 Furnace section .............................................................................................................................35 Rear view ...............................
3 - Product description 34 Front view Front view, closed The following picture shows the front view of the instrument with the front door closed: Front view, open The following picture shows the front view of the instrument with the front door opened: Legend: 1 Ball valve 2 Drying tubes 3 Furnace with heat protection cladding Operation Manual D-480 ©BÜCH Labortechnik AG
3 - Product description 35 Furnace section Location of the furnace section The furnace section is located behind the front door of the instrument. The front door is held by a magnet, thus it can be opened easily. What is inside the furnace section? The furnace section contains a furnace with three independent heaters. The temperatures of the heaters are pre-selected from the PC. All heaters are temperature-monitored by the software and can be shut down in the event of a malfunction.
3 - Product description 36 Top view furnace The following picture shows a top view of the furnace pulled out: Legend: 1 Post combustion tube plug 2 Post combustion tube 3 Combustion tube connection 4 Combustion tube 5 Reduction tube plug 6 Reduction tube Rear view Rear view The following picture shows the rear view of the analyzer: Legend: 1 Rear wall 2 Air baffle 3 "PC" PC connector (USB) 4 "Reserve" reserve 5 "~" mains connector 6 "CO2 IN" CO2 gas inlet 7 "O2 IN" O2 gas inlet 8 "REF" reference gas ou
3 - Product description 37 Right side view Right side view, closed The following picture shows the right side of the analyzer with the side door closed, as seen from the front: Legend: 1 Right side door 2 Main switch Right side view, open The following picture shows the right side of the analyzer with the side door open, as seen from the front: Legend: 1 Mainboard 2 Furnace 3 Main switch Operation Manual D-480 ©BÜCH Labortechnik AG
3 - Product description 38 Left side view Left side view, closed The following picture shows the left side of the analyzer with the side door closed, as seen from the front: Legend: 1 Left side door Left side view, open The following picture shows the left side of the analyzer with the side door open, as seen from the front: Legend: 1 Thermal conductivity detector (TCD) 2 Water condenser Operation Manual D-480 ©BÜCH Labortechnik AG
3 - Product description 39 Top view Top view of the instrument The following picture shows the top view of the instrument: Legend: 1 Carousel cover 2 Carousel, sample magazine and cover ring 3 Instrument cover Peripherals and their function Types of peripherals The following picture shows the analyzer and its peripherals Legend: 1 Instrument 2 Balance 3 Printer 4 PC Functions of the peripherals The following table lists the functions of peripherals: Peripheral Function PC Operation of the instrumen
CHAPTER 4 Understanding the instrument and planning its use Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose This section helps you to assess the applications of the instrument and subsequently plan the use of the instrument. In this chapter Layout and mode of functioning ....................................................................................................42 Processes in the instrument during a measurement...........................................
4 - Understanding the instrument and planning its use 42 Layout and mode of functioning Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose This section describes what the instrument does, what the analysis parameters mean, and what happens in the instrument during an analysis. In this section Functional units .............................................................................................................................
4 - Understanding the instrument and planning its use 43 Functional units Introduction The following section describes what units comprise the instrument and what functions the individual units perform in the analysis procedure. Functional diagram The following diagram shows the basic setup of the instrument and its division into functional units.
4 - Understanding the instrument and planning its use 44 I Mechanical sample insertion and O2 dosing system II Furnace area and reaction zone III Gas drying IV Detector Symbols The following list names the functional and basic symbols: Two-way valve Pressure sensor Gas separation Three-way valve Loop Measuring cell Check valve Heated tube Sensor Throttle Drying Hose line Flow controller Combustion Copper tube Flow sensor Post combustion Reduction Pressure contoller Actuator Mec
4 - Understanding the instrument and planning its use 45 6 Post combustion tube with tube filling Oxidation of the combustion products at the CuO/Pt catalyst 7 Reduction tube with tube filling Binds excess oxygen. Reduces NOX to N2. Binds volatile halogen compounds and sulfurous compounds. For details on the processes in the furnace area, cf. Substance digestion and preparation of the reaction gas mixture (on page 47).
4 - Understanding the instrument and planning its use 46 Processes in the instrument during a measurement Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose The following section is designed to help you understand the processes that take place during a measurement. In this section Sample insertion and initiation of measurement ............................................................................
4 - Understanding the instrument and planning its use 47 Sample insertion and initiation of measurement Introduction The following section explains how to insert the analysis samples into the combustion tube and how to initiate measurement of the reaction products. Note The bracketed numbers used below refer to the part numbers listed in Functional units (on page 43).
4 - Understanding the instrument and planning its use 48 Volatile halogen compounds are bound on silver wool. The gas stream is predried in the water condenser (8). In the downstream drying tube (8) the residual moisture is removed by Sicapent®. In the reduction tube (7), nitrogen oxides are quantitatively transferred at the tungsten contact to form molecular nitrogen. Excess oxygen is bound. Sulfur absorption takes place in the reduction tube (7) at the tungsten.
4 - Understanding the instrument and planning its use 49 Basic facts about working with the instrument Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose The following section provides basic facts about working rationally and appropriately with the instrument. In this section Setting device parameters .............................................................................................................50 Instrument equipment ................................
4 - Understanding the instrument and planning its use 50 Setting device parameters About instrument parameters You need to know the following about instrument parameters: The instrument parameters listed here are average values. The optimized instrument parameters from initial start-up are stored on the enclosed installation CD. The user can optimize them for special applications or extraordinary demands.
4 - Understanding the instrument and planning its use 51 Instrument equipment Combustion tube filling The following picture shows the fillings and filling heights of the combustion tube: Legend: 1 Ash crucible 2 Corundum balls (3 mm) 3 80 g CuO + 20 g Corundum balls (110 mm) 4 Corundum balls (10 mm) 5 Wire mesh ronde (22 mm) 6 Spacer Working temperature 950 °C Reduction tube filling The following picture shows the fillings and filling heights of the reduction tube: Legend: 1 Silver wool 2 Copper (20 m
4 - Understanding the instrument and planning its use 52 Filling the post combustion tube The following picture shows the fillings and filling heights of the post combustion tube: Legend: 1 Silver wool 2 Corundum balls (76 mm) 3 200 g CuO + 15 g Pt catalyst (180 mm) 4 Corundum balls (50 mm) 5 Wire mesh ronde (22 mm) 6 Spacer Working temperature 800 °C Background knowledge required for calibration Important calibration principles Perfect calibration of the instrument is a key condition for achieving cor
4 - Understanding the instrument and planning its use 53 The daily factor for a measuring component is clearly outside of the range of 0.9 to 1.1. Also, it displays fast changes in time from day to day. Calibration formulae The formulae used for calibration can be found in Calibration formulae (on page 55). Calibration curve calculation method For details on the various calibration curve calculation methods and when to use them, see Calibration curve computation method criteria (on page 53).
4 - Understanding the instrument and planning its use 54 Linear calculation over the whole range The following picture shows an example in which a linear calculation over the whole range achieves acceptable calibration curve quality. Linear calculation over two ranges The following picture shows an example in which a linear calculation over two ranges achieves acceptable calibration curve quality.
4 - Understanding the instrument and planning its use 55 Polynomial calculation over the whole range The following picture shows an example in which a polynomial calculation over the whole range achieves acceptable calibration curve quality. Achievable calibration curve quality Process standard deviation "Proc-SD" and quality factor "r" serve as a measure of achievable calibration curve quality.
4 - Understanding the instrument and planning its use 56 Computing calibration coefficients Once the absolute element contents have been computed and the peak areas have been measured for the respective sample, the pairs of values (absolute content / peak area) are transferred into a coordinate system where they form the calibration curve. By means of an algorithm, the calibration coefficients a - e are computed which, entered in a polynomial, constitute the calibration curve.
4 - Understanding the instrument and planning its use 57 Routine measuring work is performed at set intervals or on defined occasions before, during or after a series of measurements with real samples. Instrument blank values Determination of the instrument blank value depends on your needs. The following overview shows the type and purpose of the individual determinations.
4 - Understanding the instrument and planning its use 58 Blank value determination In blank value determination, the peak area values of the blank samples are averaged.
4 - Understanding the instrument and planning its use 59 Understanding the operating software Target group Personnel with basic chemical knowledge and basic computer knowledge.
4 - Understanding the instrument and planning its use 60 Basic functions of the operating software Introduction The following section describes the functions of the operating software and what instrument control and data processing operations are possible.
4 - Understanding the instrument and planning its use 61 Software user interface The main window of the operating software The following screenshot shows the main window of the operating software and designates the various areas and bars: Title bar The title bar displays the name of the file that you are currently processing. The title bar has the usual functions for displaying the system menu and for minimizing, maximizing and closing the window.
4 - Understanding the instrument and planning its use 62 ... display the online help. Details on the various buttons on the toolbar can be found at Toolbar (on page 296) and in the online help. Sample view The sample view displays a table of input, measuring and computed analysis data of all samples in a particular series. If an error occurs while measuring a sample, the table contains an appropriate message. For details on the sample view, see The sample view (on page 62).
4 - Understanding the instrument and planning its use 63 View The sample view looks like a familiar calculation sheet in a spreadsheet program. Sample view input functions In the sample view you define the sequence of your analysis samples. The sequence must match the sequence in which you arrange your samples on the carousel.
4 - Understanding the instrument and planning its use 64 Sample not yet analyzed, but a sample name has been set and a method does not yet exist. Sample analyzed error-free with valid date information. Sample analyzed error-free with valid date information. The measured peak area is below the specified calibration range. The result was interpolated. Sample without valid date information. Sample which caused a non-critical error during measurement or which exceeded a calibration range.
4 - Understanding the instrument and planning its use 65 Progression view (graph view) Progression view displays a graph of the development over time of important instrument parameters and measured values during measurement of the sample selected in the sample view. You can recognize the current sample by the green border around the graph display.
4 - Understanding the instrument and planning its use 66 Statistics view The statistics view displays the element content percentages of all samples in a series, grouped by sample name.
4 - Understanding the instrument and planning its use 67 If your series includes samples previously defined as calibration samples, you can use them to calculate calibration coefficients. You can define and determine up to two calibration ranges according to which polynomial degree you want to determine the calibration curve.
4 - Understanding the instrument and planning its use 68 The areas of the status view and what they mean The following table lists the individual areas of the status view and the information they contain: Area Meaning Process Displays a list of individual processes during the analysis procedure. The current process is highlighted with a colored background so that you can see the progress of the analysis of the current sample straight away. Displays "Standby" when the instrument is in idle mode.
Copyright Note 69 Copyright © BÜCHI Labortechnik AG All rights reserved This document contains proprietary information of BÜCHI Labortechnik AG. Reprint is prohibited. Due to continued product development this information may change without notice. The information and intellectual property contained herein is confidential between BÜCHI Labortechnik AG and the client and remains the exclusive property of BÜCHI Labortechnik AG.
Copyright Note 70 In dialogs In dialogs you can also press the right mouse button to display certain commands. In the "Configure view" dialog, right click to display the Properties command, that opens the "Column properties" dialog. See Configure view (on page 282). Further functions In the "Specify upper and lower calibration range" dialog you can right-click to set the dividing line between the upper and lower calibration range.
Copyright Note 71 Data administration and data security Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose This section describes what options the system offers with regard to data administration and data security. In this section Laboratory information and management system (LIMS) ..............................................................72 Conditions for operating the LIMS ......................................................................................
Copyright Note 72 Laboratory information and management system (LIMS) What does LIMS do? The Laboratory Information and Management System (LIMS) collects and manages data from different systems and thereby facilitates laboratory operation and documentation. Interaction between the software and LIMS The following features characterise the interaction between the analyzer software and LIMS: The flow of data is unidirectional, i. e. it only goes in one direction, from the analyzer to LIMS.
Copyright Note 73 21 CFR Part 11 functionality What is 21 CFR Part 11? 21 CFR Part 11 is a regulation that was published by the American Food and Drug Administration (FDA), under number 21 CFR part 11, at the end of the 1990s and that has legal force in the USA. It governs technical and organizational requirements to be fulfilled in order to use electronic data and documents instead of paper for development, approval and production.
Copyright Note 74 Restricted access to menu functions The software restricts access to the menu functions on the basis of three user groups: The lowest user group may only perform actions required in routine operation. The middle user group may also perform actions requiring experience, e.g. calibration. The top user group may also perform actions requiring a great deal of experience, e. g. changes to the system configuration.
CHAPTER 5 Work performed by the system administrator Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to perform typical system administrator tasks. In this chapter Installing and updating the software ..............................................................................................76 Configure analyzer ...............................................................................................................
5 - Work performed by the system administrator 76 Installing and updating the software Conditions for installation In order to install the software correctly, administrator rights for the PC must be available. Requirements for operation Do the following to be able to operate the software without any problems: On the PC where the software is installed, check power management settings under Control Panel > Power Management or under Control Panel > Power Options.
5 - Work performed by the system administrator 77 Configure analyzer Target group Personnel with basic chemical knowledge and basic computer knowledge. Purpose This section describes what the instrument does, what the analysis parameters mean, and what happens in the instrument during an analysis. In this section What can you modify in the configuration? ....................................................................................78 Defining logon timeout .........................................
5 - Work performed by the system administrator 78 What can you modify in the configuration? Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). What can you set? You can set the following in the configuration: Interface properties Weighing data properties Signature program properties Device parameter See Configure analyzer (on page 77).
5 - Work performed by the system administrator 79 Creating new sections Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). Creating new sections Proceed as follows: Open the "Device configuration" dialog by selecting Options > Configuration. Select the tab for which you want to create a new section. Enter the name of the new section in the "Section" dropdown listbox and click New Section to the right of it.
5 - Work performed by the system administrator 80 Defining LIMS export settings Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to define export settings for LIMS as system administrator. In this section LIMS export settings ......................................................................................................................
5 - Work performed by the system administrator 81 LIMS export settings What is set? The following are set for LIMS: What data to send. Whether the data is transferred via interface or network. The interface settings. What instrument the data belong to. See LIMS settings (on page 311).
5 - Work performed by the system administrator 82 Setting up user administration Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to set up the user administration as system administrator. In this section User administration........................................................................................................................83 Recommendations for user administration .........................................
5 - Work performed by the system administrator 83 User administration User groups Access to menu functions is restricted on the basis of three user groups in the operating software. These groups are automatically set up when you install the software under Windows: The user group "DuMaster user" with the lowest authorizations. The user group "DuMaster superuser" with more authorizations. The user group "DuMaster administrator" with most authorizations.
5 - Work performed by the system administrator 84 Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). Granting authorizations Proceed as follows: Open the "Device configuration" dialog by selecting Options > Configuration. Select the "DEVICE.INI" tab. Select the "Menu" section by clicking the arrow next to the "Section" dropdown listbox. In the field "Items" all menu commands are listed.
5 - Work performed by the system administrator 85 Defining interfaces Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to define various interfaces as system administrator. In this section Defining the analyzer / PC interface ..............................................................................................86 Defining the LIMS / PC interface ........................................................................
5 - Work performed by the system administrator 86 Defining the analyzer / PC interface Note The operating software can only be operated in combination with the analyzer if the serial number of the instrument matches the software licence number. This ensures that the analyzer is always operated together with the same software and the settings recorded in the logbook. Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24).
5 - Work performed by the system administrator 87 Defining the balance / PC interface Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). Defining the balance / PC interface Proceed as follows: Open the "Device configuration" dialog by selecting Options > Configuration. Select the "DEVICE.INI" tab. Then select the "Balance Port" section by clicking the arrow next to the "Section" dropdown listbox.
5 - Work performed by the system administrator 88 Editing analysis data Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section describes when it makes sense to edit analysis data and to what extent this is possible. In this section When does it make sense to edit analysis data?...........................................................................89 Limits for modifying analysis data .......................................................
5 - Work performed by the system administrator 89 When does it make sense to edit analysis data? Reasons for modifying analysis data The following reasons exist to edit analysis data: If old calibration coefficients only exist as a hardcopy and you want to load them, you can manually input the calibration coefficients. If you have created a template of the sample data for the measurements and you need to enter the samples still to be measured in the template.
5 - Work performed by the system administrator 90 Performing checks Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to perform various checks as system administrator. In this section Checking documents for authenticity .............................................................................................91 Signing documents ..............................................................................................
5 - Work performed by the system administrator 91 Checking documents for authenticity What signature is checked? Only those signatures can be checked that are enabled in the "Verify digital signature" dialog and if their radio button is checked; for example the "created" signature. If the document already has multiple signatures, the user must select one to check. Note Note the following: The signature program must be installed.
5 - Work performed by the system administrator 92 Viewing the logbook Viewing the logbook Proceed as follows: Open the logbook by selecting Options > Logbook. Select the period for which to view the logbook. Open the "Select period" dialog by selecting File > Load. In the "Select period" dialog, use the arrows of the corresponding fields to set the year and month and then click OK. The desired period - if available - is displayed in the logbook.
5 - Work performed by the system administrator 93 Working with the database Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to perform various database tasks as system administrator. In this section Database .......................................................................................................................................94 Administrative work on the database .............................................
5 - Work performed by the system administrator 94 Database What is a database? A database is characterized by the following: A database is an organized collection of data managed by a data management system. Different users can access shared data in a database. Databases allow the user to input, edit and delete data. Databases permit searching and selecting data with the aid of filters. Databases allow the user to create evaluations and statistics.
5 - Work performed by the system administrator 95 Defining the autoexport directory Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). Selecting a directory Proceed as follows: Open the "Device configuration" dialog by selecting Options > Configuration. Select the "DEVICE.INI" tab. Select the "AutoExport" section by clicking the arrow next to the "Section" dropdown listbox.
5 - Work performed by the system administrator 96 Autoexport Autoexport creates a backup of the current document as an mdb file after every save or sub-save process. The advantage of this is that you do not always have to save the whole database. However, autoexport is only performed if you have defined a directory for saving backups. You can set this directory in the Configuration menu. The file name is as follows: xxxxx.YYMMDDhhmmss.mdb.
5 - Work performed by the system administrator 97 Reorganize database Proceed as follows: Open the "Clean database" dialog by selecting File > Backup/Restore > Database > Clean up. Click Backup now. You cannot reorganize the database without backing up. This displays the "Select backup file name" dialog: Enter a file name in the "File name" field and click Save. The database is saved. Click Reorganize in the "Reorganize database" dialog.
5 - Work performed by the system administrator 98 Ways of optimizing the use of the analyzer Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section gives an overview of the ways in which you can optimize the use of the analyzer for your own particular application. In this section Optimizing basic instrument settings .............................................................................................99 Optimizing sample data editing .
5 - Work performed by the system administrator 99 Optimizing basic instrument settings Analyzer configuration You can optimize the following by means of configuration: Interface properties Signature program properties Device parameter See Configure analyzer (on page 77). Reacting to irregularities If irregularities occur during the analysis, it is important for the user to quickly identify any errors. In the "Error handling" dialog the user defines how the analyzer is to react to incidents.
5 - Work performed by the system administrator 100 Prioritizing urgent samples Via Edit > Swap you can prioritize urgent samples and analyze them earlier than scheduled. However, in the solids modes the samples are only swapped in sample memory, and you have to swap the samples on the carousel by hand. If multiple determination is activated you always should swap all samples from one vial to all samples from the other vial instead of swapping only single samples. See Swap samples (on page 277).
5 - Work performed by the system administrator 101 The following import options are available: Import into an empty sample memory. Import into a sample memory that is not empty. Importing into an empty sample memory After importing into an empty sample memory, the weighing data and any sample names are now in the sample memory. The weighing data are input starting from sample No. 1.
5 - Work performed by the system administrator 102 Performing other administrator tasks Target group Personnel with good knowledge of the operating system and administrative settings. Purpose This section enables you to perform various tasks as system administrator. In this section Modifying the registration ............................................................................................................103 Printer setup ........................................................................
5 - Work performed by the system administrator 103 Modifying the registration Dialog: "Product registration" When you start the operating software for the first time, the "Product Registration" dialog is displayed. Once you have registered, the dialog is no longer displayed when you launch the program. Changing the registration You must have administrator rights to modify the registration. Modifying Proceed as follows: Launch the operating software.
CHAPTER 6 Starting up and shutting down the instrument Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to start up or shut down the instrument according to instructions. In this chapter Setting up and starting up the instrument ....................................................................................106 Shutting down the instrument .........................................................................................
6 - Starting up and shutting down the instrument 106 Setting up and starting up the instrument Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to set up and commission the instrument according to instructions. In this section Rules for first-time start-up ..........................................................................................................107 Instructions for operating the furnace ............................
6 - Starting up and shutting down the instrument 107 Rules for first-time start-up First-time start-up Observe the following rules for first-time start-up. First-time start-up is performed by a trained service technician. Only the service technician may open the transport packaging. If the customer opens the transport packaging, this results in loss of warranty. Make sure that the user is completely available for instruction and hand-over of the equipment at the time of first-time start-up.
6 - Starting up and shutting down the instrument 108 Room temperature should be constant. Analyzer and peripherals must be protected from drafts and direct heat. An air-conditioned room is advantageous as the analyzer emits heat. Take suitable action to avoid electrostatic discharge. Electrical discharges can lead to malfunctions of the instrument.
6 - Starting up and shutting down the instrument 109 Category Type Part of initial equipment Carrier gas CO2: No Combustion gas Purity: 99.995 % Consumption approx. 725 ml/min Adjust the intake pressure at the delivery point until the PC pressure display "Input" reads 1300 mbar. Oxygen: Purity: 99.995 % Intake pressure 2.5 bar Consumption approx. 0.
6 - Starting up and shutting down the instrument Filling the drying tube (on page 234). Filling the combustion tube (on page 222). Filling the post combustion tube (on page 223). Filling the reduction tube (on page 224). 110 Install the required glass and quartz components. Leave the tube outlets open for subsequent conditioning. Used tubes also need to be conditioned. See Installing reaction tubes in the furnace and conditioning (on page 229).
6 - Starting up and shutting down the instrument 111 Peripherals A PC must be connected. It is essential for operation. A printer should be connected so that you can print out measuring results. A balance should be connected, so you do not need to enter the sample weight by hand.
6 - Starting up and shutting down the instrument 112 Detail of the rear The following picture shows a detail of the rear of the analyzer with the associated gas connections: Legend: 1 "CO2 IN" CO2 gas inlet 2 "WASTE" measuring gas outlet 3 "REF" reference gas outlet 4 "O2 IN" O2 gas inlet Connecting supply lines Safety instruction Strictly observe the safety instruction "Mixing up gas inlets" under Warning notes during operation (on page 24).
6 - Starting up and shutting down the instrument 113 Removing the furnace transport protection Proceed as follows: Open the front door of the instrument. Push the right side door open from inside (magnetic lock). The transport protection is now visible in the form of a bracket (1). Unscrew the screws and remove the bracket. Fasten the bracket on the rear casing angle (1). It should be stored there so that it does not get lost.
6 - Starting up and shutting down the instrument 114 Push the left side door open from inside (magnetic lock). The water trap (1) and the transport protection (5) are now visible. Loosen the ground-in clamp (3) which connects the glass tube with the water trap and unscrew the cap with the pan connector (4). Also unscrew the cap with the hose (2). Remove the transport protection (5). Tighten both caps (2 & 4) again.
6 - Starting up and shutting down the instrument 115 CO2 intake pressure CO2 intake pressure is set at the delivery point so that the following values are displayed on screen: The "Input" display shows approx. 1300 mbar. The "MFC CO2" display shows approx. 650 ml/min. The "Flow CO2" display shows approx. 650 ml/min. Flow rate The following flow rate settings are typical: The "MFC CO2" display shows approx. 650 ml/min for the measuring gas outlet.
6 - Starting up and shutting down the instrument 116 Shutting down the instrument Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to shut down the instrument according to instructions. In this section Shutting the instrument down for short measuring breaks (standby) ...........................................117 Shutting the instrument down for long measuring breaks (switching off) .....................................
6 - Starting up and shutting down the instrument 117 Shutting the instrument down for short measuring breaks (standby) What are short measuring breaks? Short measuring breaks are breaks that last overnight or for 2-5 days. Procedure The analyzer and the PC stay online during short measuring breaks. Only the sleep function is activated for the instrument. Setting the analyzer sleep function.
6 - Heating up the furnace / checking parameters 118 In case the analyzer has to be transported, mount the corresponding transport protection(s) again. Heating up the furnace / checking parameters Note Note the following: The following section is part of initial start-up. All steps described in initial start-up before "Heating up the furnaces / checking parameters" must have already been performed. See Start-up (on page 109).
CHAPTER 7 Using the instrument Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to perform measurements with the instrument. In this chapter Measurement settings .................................................................................................................120 Preparing samples...................................................................................................
7 - Using the instrument 120 Measurement settings Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to define the necessary settings for measurements. In this section Defining keywords for blank and conditioning samples ...............................................................121 Viewing list of defined factor, monitor and standard samples ...............................................
7 - Using the instrument 121 Defining keywords for blank and conditioning samples Keywords Names of blank samples and conditioning samples must be defined as keywords so that the software recognizes and handles the samples as blank or conditioning samples.
7 - Using the instrument 122 Click Close to close the dialog. Required substances Different amino acids like e.g. aspartic acid, glutamic acid or uric acid have been proven to be advantageous. Theoretical element contents of standard substances The following tables lists the theoretical nitrogen contents of the standard substances used in the calibration tables: Standard substance Ntheor[%] Aspartic acid 10.52 Glutamic acid 9.52 Uric acid 33.
7 - Using the instrument 123 Specifying the computation method for blank value and daily factor Defining the blank value calculation method Proceed as follows: Open the "Configure Calculations" dialog in the operating software by selecting Options > Settings > Calculation. In section "Blank value determination" define the calculation method: If you... ...
7 - Using the instrument 124 ... switch off a signal, uncheck the appropriate checkbox. Click OK. This closes the dialog and saves the settings. Configuring error handling Reacting to irregularities If irregularities occur during the analysis, it is important for the user to quickly identify any errors. In the "Error handling" dialog the user defines how the analyzer is to react to incidents. Incident Consequences During analysis, the computed element contents exceed the defined tolerances.
7 - Using the instrument 125 Preparing samples Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to prepare samples properly. In this section Sample preparation instructions ..................................................................................................126 Determining sample weight .............................................................................................
7 - Using the instrument 126 Sample preparation instructions Samples with potential risks Various sample substances can pose a risk to the user during the analysis: Contact with the substances may lead to chemical burns or poisoning. Combustion analysis of larger quantities of the substance may lead to explosions.
7 - Using the instrument 127 The result will be that the nitrogen content is well measurable and you will achieve an optimum in catalyst consumption as well as in maintenance effort. Generally, you should prefer to carry out multiple measurements with lower weights instead of fewer measurments with higher weights. Determining sample weight with unknown substances Proceed as follows: Start with a sample weight at approx. 300 mg.
7 - Using the instrument 128 Packing fatty, humid and non-pelletizeable solid samples - packing with tin film and/or tin boats Examples of solid samples of this matrix include sausage, cheese, meat, yeast (fat and humid), dry yeast, soil, oily samples which release oil when pressed and small sample weights (calibration standards). Proceed as follows: Tare the tin film or tin boat to zero. Fill in the sample.
7 - Using the instrument 129 Preparing measurement work Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to prepare measurement work. In this section Software usage rules ...................................................................................................................130 Starting the operating software ........................................................................
7 - Using the instrument 130 Software usage rules Software usage rules Observe th following rules in order to avoid disruptions during analysis: The control PC must not be used simultaneously as an office workstation as this may lead to software instability. Observe the following if using the operating software and other software at the same time: Programs that require a lot of computer processing capacity or access disk drives for long periods (e.g. disk formatting) may cause disruptions.
7 - Using the instrument 131 The carrier gas is reactivated and the furnaces are heated up to their working temperatures. Selecting the operating mode Essential condition Before switching operating modes, you must have performed all refitting work required for the new operating mode. Safety instruction Strictly observe the safety instruction "Changing mode" under Warning notes during operation (on page 24).
7 - Using the instrument 132 Open the "Methods" dialog in the operating software by selecting Options > Settings > Methods. In the left field, select the appropriate method. In the fields at the right side the parameters of the selected method are now displayed. Click Close to close the dialog again. Defining custom methods Proceed as follows: Open the "Methods" dialog in the operating software by selecting Options > Settings > Methods. Click New.
7 - Using the instrument 133 Copy methods Defining custom methods The existing method can be copied with the option "Copy methods" and subsequently the parameters of the corresponding requirements can be changed accordingy. In a lot of cases this is more efficient than creating a new method and entering all parameters. Copy methods Proceed as follows: Open the "Methods" dialog in the operating software by selecting Options > Settings > Methods.
7 - Using the instrument 134 ... "Auto-decrement the number in the sample name": Works the same way as autoincrement, only the figure in the name is decremented. ... "Increment/decrement interval": Defines the amount the number in the sample name is increased/decreased.
7 - Using the instrument 135 This closes the dialog and the samples are swapped in the sample memory. Manually swap samples in the carousel. Optimizing sleep and wake-up behavior What can you optimize? You can set sleep/wake-up behavior so that conditioning samples in a series are measured before the first user starts work on the instrument in the morning.
7 - Using the instrument 136 Performing measurement work Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to perform all measurement work. In this section Values for oxygen dosing ............................................................................................................137 Performing measurements ..............................................................................
7 - Using the instrument 137 Values for oxygen dosing Meaning of oxygen dosing The following illustrate the meaning of oxygen dosing: If oxygen supply is insufficient, the catalysts are reduced and thus limited in their effect and durability. The unburnt sample substance remains in the ash finger and distorts the results of analysis of subsequent samples.
7 - Using the instrument 138 Animal feed, approx. 500 mg medium fat content 50 mgFeed 250 ml/min, 100 sec Cheese, sausage, appr. 500 mg high fat content 500fatCheeseSausage 300 ml/min, 150 sec Blank value with O2 Blank with O2 80 ml/min, 60 sec Blank value without O2 Blank without O2 50 ml/min, 1 sec Beer, milk, soil, appr. 500 mg medium fat content 500mgBeerMilkSoil 120 ml/min, 60 sec Starch, approx. 400 mg 400mgStarch 250 ml/min, 150 sec Soil, approx.
7 - Using the instrument 139 When is routine measuring work necessary? You must perform routine measuring work before measuring real samples: if you have not performed any routine measuring work today if measuring breaks exceed a duration of 2 hours.
7 - Using the instrument 140 Save the data or print them out. See Data backup and printing (on page 158). When can routine measuring work be omitted? You can measure real samples without preceding routine measuring work: if you have already performed routine measuring work today if measuring breaks last less than 2 hours.
7 - Using the instrument 141 Definitions Routine measuring work comprises the following activities: Determination of instrument blank values. Instrument conditioning with conditioning samples. Determination of daily factors. Routine measuring work is performed at set intervals or on defined occasions before, during or after a series of measurements with real samples. Instrument blank values Determination of the instrument blank value depends on your needs.
7 - Using the instrument 142 Measure a maximum of 50 real samples. At the end of the series, measure the following daily factor sample four times and check the daily factor: 250 mg glutamic acid with method "Standard". Checklist for blank value / conditioning and daily factor measurements Purpose The checklist helps you to check whether the instrument is ready to measure blank value, conditioning and daily factor samples.
7 - Using the instrument 143 Checklist Go through the following list: Were the results of a blank value determination OK? Were the results of the conditioning sample measurement OK? Have you processed a series of measurements with daily factor samples? Are the operating gases on? Are the furnaces at setpoint temperature? Combustion tube: 950 °C Post combustion tube: 800 °C Reduction tube: 815 °C Is pressure OK? Display on the PC "Press.
7 - Using the instrument 144 The N integral values should be between 10 and 50 after stabilization. If your N integral values are significantly higher than 50, repeat the blank value determination with methods which is associated with an oxygen dosing time of 1second (e.g. "Blank without O2"). If the N integral values are then normal, the oxygen was contaminated. Otherwise, the system has probably a leak.
7 - Using the instrument Name: Blnk Weight: 1 mg 145 Click Method in the line of the appropriate sample. An arrow is displayed with which you can open a dropdown list with various methods. Select the appropriate method for the blank value sample. Cf. Types of blank value determination and their settings (on page 143). Start the blank value determination via System > Auto run. Once the measurements are finished you can compute the blank value.
7 - Using the instrument 146 Allocate the daily factor to the real samples in the sample view (text view). Enter the daily factor in the corresponding factor column. How to selectively trigger the daily factor Proceed as follows: Define the type of factor calculation. For that purpose, open the "Configure Calculations" dialog in the operating software by selecting Options > Settings > Calculation. Define the mode of factor determination: If you in section "Factor determination"... ...
7 - Using the instrument 147 Click OK. "Standard tolerance monitoring" is now enabled. Stopping continuous analysis When do I stop continuous analysis? It makes sense to stop a continuous analysis in the following cases: If the result of the blank value indicates that the instrument is leaky. If the results of the conditioning sample indicate that parts of the instrument are defective or that gas pressure and flow behaviors are not OK.
7 - Using the instrument 148 Preparing measuring data for evaluation Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to prepare measuring data for evaluation. In this section Configuring the sample view .......................................................................................................149 Determine measuring units and number of decimal places. ...........................
7 - Using the instrument 149 Configuring the sample view Configuring the sample view Proceed as follows: Select cells in the sample view. Specify what you want to have displayed in the view. Open the "Configure view" dialog by selecting View > Gridview > Configure. Decide: If you want to... ... show a column: Select the entry in the "Hide" column and click <<<. The entry is moved to the "Show" column. ... hide a column: Select the entry in the "Show" column and click >>>.
7 - Using the instrument 150 Saving the sample view Saving the sample view Proceed as follows: Open the "View configuration" dialog by selecting View > Gridview > Save configuration. Enter the name of the view in the text box at the top and click Save. The view is saved and can be loaded at a later point. Loading a sample view Loading a sample view Proceed as follows: Open the "View configuration" dialog by selecting View > Gridview > Load configuration.
7 - Using the instrument 151 You can generate statistical data manually. In this case, the user combines any samples in groups. Statistical data are then automatically generated for these groups. Generating statistical data fully automated Proceed as follows: Click Statistics > By names. A warning appears which has to be confirmed. Respond to the warning note: If statistics memory... ... may be deleted: Click Yes. ... must not be deleted: Click No and safe your data.
7 - Using the instrument 152 Mean value The mean value of "n" element concentrations is computed with this formula: whereas: /c = Mean value of concentrations ci = Individual concentrations in the group n = Number of group members i = index from 1 to n Absolute standard deviation Absolute standard deviation is computed according to this formula: whereas: s = Absolute standard deviation ci = Individual concentrations in the group n = Number of group members i = index from 1 to n Relative standard deviati
7 - Using the instrument 153 Single peaks In general a single peak looks as follows: Superimposed peaks These are two peaks where one superimposes the other. Peak 1 is designated as "socket" and peak 2 is designated as "superimposed". The following picture shows such a run. Melted peaks These are two consecutive peaks where the second peak already starts although the first is not yet finished.
7 - Using the instrument 154 Manual integratability Regarding the integratability there are certain differences between the individual peak types. Well integrable are: Sinple peaks with clear beginning and tailing. This peak type normally is integrated without any problem from the firmware implemented in the algorithm. However, a reintegration may be necessary, in particular if the peak is very small and therefore the end mark was set too early.
7 - Using the instrument 155 Click and mark the peak end in the same way as described in the previous step for the peak start. As soon as peak start and end are marked, a baseline is drawn automatically and the integration result is displayed below the peak graphic. Furthermore, the area content appears in light blue. Click to adjust the height of the baseline.
7 - Using the instrument 156 The peak area was entered in the corresponding cell in the sample view and the new concentration value was calculated. Furthermore, the date for the corresponding sample was deleted and the text "ManInt" was entered in the info column. Now the process of the manual integration of superimposed peak is completed.
7 - Using the instrument 157 Setting the size of the graph with the mouse Proceed as follows: Drag a rectangle in graph view using the mouse. The selected area is displayed larger. Setting the zoom factor back to 1 By clicking the button at the upper left corner of the graphic filed you can set the zoom factor from any value back to 1. Configure report Configure report Proceed as follows: Open the "Configure Report" dialog by selecting File > Report configuration.
7 - Using the instrument 158 Data backup and printing Why backup and print data? The measuring data of a sample are displayed on screen and saved to a temporary file after every analysis. In order to save the data permanently, it is necessary to save them separately or print them out. Graph view All graphical information (pressure, peaks, etc.) of a sample are saved. This allows you to view and print various measuring variables in a graph.
7 - Using the instrument 159 Overview of export and import file formats Export and import The analysis data are managed in a database, so it is not possible to load and save them as files in the usual way. However, by using the File > Export/Import > Export and File > Export/Import > Import menu functions it is possible to transport documents "out of" the database and to transport external documents "into" the database.
7 - Using the instrument 160 Edit the imported data as required and save them when you are finished. Exporting LIMS data Selecting data to send Proceed as follows: Open the "LIMS settings" dialog by selecting Options > Settings > LIMS. Open the "LIMS data" tab. Decide: If you want to... ... send data: Check the appropriate checkbox in the "Data to send" section. ... not send data: Uncheck the appropriate checkbox in the "Data to send" section.
7 - Using the instrument 161 Working with documents Target group Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers. Purpose This section enables you to work with database documents. In this section Creating new documents .............................................................................................................162 Editing documents ..........................................................................................
7 - Using the instrument 162 Creating new documents Usual procedure Usually, one document is created per day. The data are separated and evaluated by customer at the end of the day. Document capacity A document can store sample data from a maximum of 5 carousels. Creating new documents Proceed as follows: Select File > New to create a new document. Save the new document by selecting File > Save. The "Save document" dialog appears.
7 - Using the instrument 163 Swap samples Proceed as follows: Open the "Swap samples" dialog via Edit > Swap. Enter the sample numbers to be swapped and confirm with OK. Editing finished samples Finished samples are only edited in special cases. See Editing analysis data (on page 88). Deleting documents Who is allowed to delete? Deleting documents is reserved for the Administrator level. What is deleted? The document itself is deleted along with all previous versions of the document.
7 - Using the instrument 164 A message appears which informs that the coefficients included in the document are different and the current coefficients will be overwritten during the document is loaded. This message must be confirmed by you. Click Yes to continue. The document is displayed. Finding previous versions Note: This function is only accessible if 21 CFR Part 11 functionality is enabled. Proceed as follows: Open the "Open document" dialog in the operating software by selecting File > Open.
7 - Using the instrument 165 Importing documents Importing documents Proceed as follows: Open the "Open" dialog by selecting File > Export/Import > Import. From the "Look in" dropdown listbox select the directory containing the document. Select the document file and click Open. Decide: If the coefficients of the selected document... ... match the current coefficients: The document is imported immediately. Herewith, the import is finished. ...
7 - Using the instrument 166 Checking documents for authenticity What signature is checked? Only those signatures can be checked that are enabled in the "Verify digital signature" dialog and if their radio button is checked; for example the "created" signature. If the document already has multiple signatures, the user must select one to check. Note Note the following: The signature program must be installed. Signatures can only be checked or created if 21 CFR Part 11 functionality is enabled.
CHAPTER 8 Maintaining the instrument Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section is designed to maintain proper working order of the instrument. In this chapter Important information about maintenance ...................................................................................168 Performing the calibration............................................................................................................
8 - Maintaining the instrument 168 Important information about maintenance Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section provides important information about maintenance. In this section Maintenance work to be performed by the customer ...................................................................169 Viewing the status of maintenance intervals................................................................................
8 - Maintaining the instrument 169 Maintenance work to be performed by the customer Note Observe that the maintenance or replacement times indicated here are greatly dependent on the respective sample matrix. All intervals and figures indicated are only examples and by no means guarantee service life of consumables or wear and tear parts.
8 - Maintaining the instrument 170 Viewing the status of maintenance intervals Viewing maintenance intervals Proceed as follows: Open the "Maintenance intervals" dialog in the operating software by selecting Options > Maintenance > Intervals. In the overview field on the left all maintenance events are displayed, i.e. the corresponding assignment as well as the percentaged count as a highlighted bar. Click the respective event in the overview field.
8 - Maintaining the instrument 171 Status view message If the maximum number of measurements is reached for a maintenance event: the due maintenance event is displayed in the status view in the "Maintenance" field the background of the "Maintenance" field turns red a wrench flashes. The following screenshot shows the status view message: To be observed after maintenance If you have performed the due maintenance you must manually reset the "Status" field to zero for the respective event.
8 - Maintaining the instrument 172 Safety instruction Strictly observe the safety instruction "Gas pressure" under Warning notes during operation (on page 24). "Preparing the instrument: Gas pressure" Proceed as follows: Shut off gas supply. Open the "Replace part" dialog in the operating software by selecting Options > Maintenance > Replace Part. Wait for pressure drop without pressing any buttons until the message "Part can now be replaced." is displayed and the Finish button becomes accessible.
8 - Maintaining the instrument 173 Baking out tubes to remove moisture and contaminations from the tube fillings. The following are baked out: Combustion tube. Reduction tube. Post combustion tube. Flushing tubes Requirements: A new tube has been installed. The analyzer is in "Replace part" status. The tube ends are closed. Safety instruction Strictly observe the safety instruction "Gas pressure" under Warning notes during operation (on page 24).
8 - Maintaining the instrument 174 Safety instruction Strictly observe the safety instruction "Baking out combustion/reduction tube" under Warning notes during operation (on page 24). Proceed as follows: Close the "Replace part" dialog in the operating software. To do so, click Finish in the "Replace part" dialog. This automatically switches on the gas again and the atmospheric nitrogen is removed by flushing with carrier gas for five minutes.
8 - Maintaining the instrument 175 Performing the calibration Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section provides facts about calibration and also enables you to perform calibration. In this section Viewing list of defined factor, monitor and standard samples ......................................................176 Defining standard substances .............................................................................................
8 - Maintaining the instrument 176 Viewing list of defined factor, monitor and standard samples Viewing the list Proceed as follows: Open the "Standard samples" dialog in the operating software by selecting Options > Settings > Standards. The list box displays all currently defined standards. By checking the requested standard sample the settings are displayed in the right area of the dialog.
8 - Maintaining the instrument 177 Viewing calibration coefficients Viewing calibration coefficients Proceed as follows: Open the "Calibration coefficients" dialog in the operating software by selecting Calibration > Coefficients. Highlight the name of a coefficient set in the listbox. The calibration coefficients of the coefficient set and the limits the calibration is valid within are displayed.
8 - Maintaining the instrument 178 Process The section is divided into the following phases: Prepare samples and perform measurement Ascertaining appropriate calculation methods Set calculation methods, perform calculation Optimizing calibration curves and apply calibration Requirements: Before starting work, the following requirements must be met: Read Background knowledge required for calibration (on page 52) and Assessing the calibration curves (on page 182).
8 - Maintaining the instrument 179 Set oxygen dosing parameters (method) for conditioning and calibration samples according to the following list: Weight 2 - 20 mg: O2 dosing time 110 sec. O2 flow = 50 ml/min. O2 cut-off threshold = 30 %. Weight 20 - 100 mg: O2 dosing time 110 sec. O2 flow = 100 ml/min. O2 cut-off threshold = 30 %. Weight 100 - 200 mg: O2 dosing time 120 sec. O2 flow = 150 ml/min. O2 cut-off threshold = 30 %.
8 - Maintaining the instrument 180 Click OK to save your settings and close the dialog. The "Specify lower and upper calibration range" dialog appears. It displays a graph generated from the absolute contents of the samples and their peak areas in a linear calculation. The graph displays deviations of the measuring points from these lines.
8 - Maintaining the instrument 181 If deleting has not had the desired effect, you can undo it. To do so, select the deleted sample and click the "Include/Exclude" button again. The sample is now included again. Once you have excluded all samples with significant deviations from the calibration curve, click the "Next" button. The next calibration curve appears in the calibration view.
8 - Maintaining the instrument 182 Assessing the calibration curves Calibration curve display in the calibration view After the calibration curves have been computed, the calibration points and the calibration curve for the respective element are displayed in the calibration view. The individual calibration points are displayed as circles. The following picture shows an example of a calibration curve for the nitrogen element.
8 - Maintaining the instrument 183 The following table explains the characteristics relating to the sample, as displayed in the above picture: Characteristic Description Sample No. Shows the analysis number of the sample selected at the cursor. Area Integral of the selected sample. slope Slope of the curve at the calibration point of the selected sample.
8 - Maintaining the instrument Operation Manual D-480 184 ©BÜCH Labortechnik AG
8 - Maintaining the instrument 185 Calibration tables Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section contains specific rules for the calibration. If you want to use these rules, you must define the standard substances used there as calibration samples. Of course, you can also use different substances but then you must develop the calibration rule yourself. In this section Calibration table for nitrogen calibration ..........................
8 - Maintaining the instrument 186 Calibration table for nitrogen calibration Suggestion The following table is a recommendation for a calibration. The user can customize settings to the specific analytical task.
8 - Maintaining the instrument 187 Replacing the ash crucible Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to replace the ash crucible. In this section Purpose and frequency of crucible replacement .........................................................................188 Removing the ash crucible ..........................................................................................................
8 - Maintaining the instrument 188 Purpose and frequency of crucible replacement Why replace the ash crucible? It is necessary to replace the ash crucible because combustion residue in the ash crucible can distort readings. When to replace the ash crucible? The intervals at which to replace the ash crucible depend very much on what substanmces you are analyzing. Generally speaking, it has to be replaced after 80 analyzed samples.
8 - Maintaining the instrument 189 Furnace area The following picture shows the details of the furnace area: Legend: 1 Handle 2 Bayonet catch 3 Reduction tube connection 4 Post combustion tube connection Phase 2: Removing the ash crucible Proceed as follows: Open the front door. Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (1) slowly to the right. Remove the ground-in clamp on the reduction tube (3).
8 - Maintaining the instrument 190 Press the post combustion tube plug (1) and the combustion tube connection (3) down lightly and pull the furnace out of the instrument to the front. Pull the combustion tube connection (3) out of the combustion tube (4) with careful jiggling motions. Place the combustion tube connection (3) on the tube rack. Insert the tube extractor into the combustion tube (4). After clamping the crucible tongs in the ash crucible, pull the ash crucible out.
8 - Maintaining the instrument 191 Place the ash crucible in the tube rack into the vent or else on a heat-resistant surface until it has completely cooled down. Protect the hot ash crucible from unauthorized access. If there are any corundum balls sticking on the bottom of the ash crucible, top up some balls in the combustion tube. Installing the ash crucible Note The following section is a continuation of Removing the ash crucible (on page 188).
8 - Maintaining the instrument 192 Insert the new ash crucible into the combustion tube (4). Place the combustion tube connection (3) onto the combustion tube (4). The lance must extend into the ash crucible approx. 5 - 10 mm. Place the ungreased seal on the combustion tube connection (3) at the top.
8 - Maintaining the instrument 193 Replacing sealing elements Target group Personnel authorized by BÜCHI Labortechnik AG. Purpose Replacing sealing elements prevents leaks. As a result of chemical corrosion, mechanical and thermal stress, sealing elements in various components of the instrument can become leaky over time. In this section When to replace sealing elements...............................................................................................
8 - Maintaining the instrument 194 When to replace sealing elements What sealing elements are used? The following sealing elements are used: Half shells O-rings Quad rings Ferrules When to replace sealing elements The following table gives an overview of what instrument components contain which sealing elements and when to replace these sealing elements: Instrument component What to replace To be replaced when... Ball valve Half shells ...
8 - Maintaining the instrument 195 Visual o-ring/quad ring check You can tell when o-rings or quad rings need to be replaced if they no longer protrude round out of the grooves of the respective component. The following picture shows o-rings in a closing plug as an example: Removing sealing elements from grooves Note Please observe the following instruction: Caution Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules).
8 - Maintaining the instrument 196 Ball valve maintenance Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to maintain the ball valve. In this section Removing and dismantling the ball valve ....................................................................................197 Cleaning, assembling and installing the ball valve. .....................................................................
8 - Maintaining the instrument 197 Removing and dismantling the ball valve Note The following section describes the first part of "Ball valve maintenance". The topic is continued in Cleaning, assembling and installing the ball valve. Purpose of maintenance Maintenance of the ball valve serves to avoid ball valve leaks. For this purpose, it is necessary to remove particles such as dust or sample abrasion that sticks between the ball and the Teflon half shells.
8 - Maintaining the instrument 198 Furnace area The following picture shows the details of the furnace area: Legend: 1 Handle 2 Bayonet catch 3 Reduction tube connection 4 Post combustion tube connection Phase 2: Pulling the furnace out of the instrument Proceed as follows: Open the front door. Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (1) to the right. Remove the ground-in clamp on the reduction tube (3).
8 - Maintaining the instrument 199 Furnace area The following picture shows the details of the furnace area: Legend: 1 Ground-in clamp 3 Ball valve fastening Phase 3: Removing the ball valve Proceed as follows: Open the ground-in ball-and-socket joints of the tube (1) leading to the ball valve. Push the right side door open from inside (magnetic lock). From the right, unscrew the ball valve (3) locking screws using an 8mm open jawed wrench.
8 - Maintaining the instrument 200 Phase 4: Dismantling the ball valve Please observe the following instruction: Caution Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules). When cutting sealing elements apart/out with a knife you may damage sealing surfaces. Never remove sealing elements with a knife but rather with tweezers. Proceed as follows: Unscrew and remove the wheel flange of the half shells using the hook wrench.
8 - Maintaining the instrument 201 Remove the ball and top half shell by means of the "knock-out". Loosen and remove the bayonet catch. Press the lower half shells out of the ball valve casing by means of the "knock-out". Cleaning, assembling and installing the ball valve. Note The following section is a continuation of Removing and dismantling the ball valve (on page 197). All steps described there must already have been performed.
8 - Maintaining the instrument 202 Process The section is divided into the following phases: Cleaning the half shells and ball Assembling the ball valve Mounting the ball balve Preparing the Instrument for measurements Requirements Before starting work, the following requirements must be met: Keep the following tools ready: Hook wrench Phillips screwdriver / Allen wrench 3 mm 8 mm open jaw wrench. Keep acetone ready to clean components.
8 - Maintaining the instrument 203 Phase 2: Assembling the ball valve Proceed as follows: Slighly grease the sealing surface of the half shells and the surface of the ball (contact surface of the ball). Insert the bottom half shell (2) and observe the recess for the drive bearing. Insert the ball (3) and observe the position of the recess for the drive bearing. Insert the drive bearing (6).
8 - Maintaining the instrument 204 Furnace area The following picture shows the details of the furnace area: Legend: 1 Handle 2 Bayonet catch 3 Reduction tube connection 4 Post combustion tube connection Phase 4: Bringing the instrument to a "ready to measure" state Proceed as follows: Close the right side door (magnetic lock). Replace the carousel. Push the furnace back: Lift the bayonet catch (2) slightly so as not to damage the seal on the combustion tube connection.
8 - Maintaining the instrument 205 Maintaining the Ni flap and the O2 lance Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to maintain the Ni flap and the O2 lance. In this section Purpose and frequency of maintaining the Ni flap and O2 lance .................................................206 Removing and cleaning the Ni flap ..............................................................................................
8 - Maintaining the instrument 206 Purpose and frequency of maintaining the Ni flap and O2 lance Why maintain the Ni flap and the O2 lance? Maintaining the Ni flap is necessary because the side facing to the combustion chamber will soil which can result in an unsafe working of the Ni flap. The O2 lance will also be slightly soiled by soot which should be removed.
8 - Maintaining the instrument 207 Furnace area The following picture shows the details of the furnace area: Legend: 1 Handle 2 Bayonet catch 3 Reduction tube connection 4 Post combustion tube connection Phase 2: Removing the Ni flap Proceed as follows: Open the front door. Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (1) to the right. Remove the ground-in clamp on the reduction tube (3). Remove the ground-in clamp on the post combustion tube (4).
8 - Maintaining the instrument 208 Phase 2: Removing the Ni flap (continued) Proceed as follows: Press the reduction tube plug (5), the combustion tube connection (3) and the post combustion tube connector (1) down lightly and pull the furnace out of the instrument to the front. Caution: Tilting and jamming the combustion tube connection can damage the combustion tube. Pull the combustion tube connection (3) out of the combustion tube with careful jiggling motions.
8 - Maintaining the instrument 209 Installing the Ni flap Note The following section is a continuation of "Removing the Ni flap". All steps described in "Removing the Ni flap" must already have been performed. See: Removing and cleaning the Ni flap (on page 206).
8 - Maintaining the instrument 210 Place the ungreased seal on the combustion tube connection (3) at the top. Furnace area The following picture shows the details of the furnace area: Legend: 1 Handle 2 Bayonet catch 3 Reduction tube connection 4 Post combustion tube connection Phase 2: Installing the Ni flap (continued) Proceed as follows: Push the furnace back: Lift the bayonet catch (2) slightly so as not to damage the seal on the combustion tube connection.
8 - Maintaining the instrument 211 Process This maintenance work is always carried out together with the maintenance of the Ni flap. The steps in Removing and cleaning the Ni flap (on page 206) are presumed for maintenance and removal of the O2 lance. Safety instruction Strictly observe the safety instruction "Hot instrument parts" under Warning notes during operation (on page 24). Removing the O2 lance Proceed as follows: Place the combustion tube connection upside-down on the tube rack.
8 - Maintaining the instrument 212 Installing the O2 lance Proceed as follows: Pull on the lance connector (2) at the end of the O2 lance (3). Insert the O2 lance with the connector into the 3 mm bore (1) located across from the flap with hinge up to the stop. Avoid breakage of the lance by slight rotary motions while inserting. After insertion the sealing hose must be set in completely into the bore and must not stick out.
8 - Maintaining the instrument 213 Removing, cleaning and installing the quartz glass bridge Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to remove, clean and install the quartz glass bridge. In this section Removing the quartz glass bridge ...............................................................................................214 Cleaning and installing the quartz glass bridge ..........................................
8 - Maintaining the instrument 214 Removing the quartz glass bridge Process The section is divided into the following phases: Preparing the instrument, gas pressure Removing the quartz glass bridge Furnace area The following picture shows the furnace area in detail: Legend: 1 Quartz glass bridge Phase 1, Preparing the instrument, gas pressure Safety instruction Strictly observe the safety instruction "Gas pressure" under Warning notes during operation (on page 24).
8 - Maintaining the instrument 215 When to clean the quartz glass bridge The quartz glass bridge must be checked for soiling after every tube change and, if necessary, cleaned.
8 - Maintaining the instrument 216 Note: When you close a ground-in ball-and-socket joint, you must be able to feel an elastic resistance when you press-in the o-ring, otherwise you must replace the o-ring. Close the front door. Phase 3: Follow-up work, gas pressure/ tightness After completing all maintenance work, put the instrument back into a state ready for measurement. See Start-up (on page 109).
8 - Maintaining the instrument 217 Removing, cleaning and installing the carousel Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to remove, clean and install the carousel. In this section Removing, cleaning and installing the carousel...........................................................................
8 - Maintaining the instrument 218 Removing, cleaning and installing the carousel Purpose of cleaning Dust accumulations or damaged sample packings may soil the carousel in the course of time. Cleaning the carousel prevents these foreign substances from entering the apparatus when you introduce the sample and cause errors. Requirements: Keep the following ready: a soft cloth or bottle brush. some water with a mild laboratory cleaner.
8 - Maintaining the instrument Lift off the ring at the pilots. Clean the plastic top section and ring with a soft cloth or bottle brush and some water with a mild laboratory cleaner. 219 Allow the carousel to dry. If necessary, remove the last traces of moisture with warm air. Replace the ring on the plastic top section and use a wrench to turn the hexagon head screws so that the tips of the screws prevent you from lifting off the ring (tighten the screws only slightly).
8 - Maintaining the instrument 220 Emptying and filling reaction tubes Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to empty and refill reaction tubes. In this section Emptying reaction tubes ..............................................................................................................221 Filling the combustion tube ................................................................................................
8 - Maintaining the instrument 221 Emptying reaction tubes Requirements: Before starting work, the following requirements must be met: The reaction tubes have been removed from the furnace. The reaction tubes have cooled down. Keep a tube extractor ready. Safety instruction Strictly observe the safety instruction "Emptying the reaction tubes" under Warning notes during operation (on page 24).
8 - Maintaining the instrument 222 Filling the combustion tube Note Note the following rules: Observe the filling heights indicated as exactly as possible. The tube filling must not have any cavities. Therefore, tap the tube wall with a piece of wood or cork when filling the tubes. Filling the combustion tube requires the use of the provided plastic tube with dimension data.
8 - Maintaining the instrument 223 Pour the recommended amounts of copper oxide (CuO) and corundum balls into two small beakers; then simultaneously pour from the two beakers into the combustion tube, so that a good mixture is developed. Fill in the corundum balls. Insert the ash crucible. Apply the cleaned Ni flap flange with O2 lance. Notes regarding further operation Please observe the following instruction: Working temperature: 950 °C.
8 - Maintaining the instrument 224 Insert the wire mesh ronde. Fill the chemicals through the plastic tube into the post combustion tube: Fill in the corundum balls. Pour the copper oxide (CuO) and Pt catalyst into two separate beakers - simultaneously pour from the two beakers, so that a good mixture is developed. Fill in the corundum balls. Insert the silver wool. Insert the plug at the top.
8 - Maintaining the instrument 225 Filling the reduction tube Proceed as follows: Furnish both plugs with 2 o-rings of Viton (green) each. Insert the bottom plug. Place the tube in the tube rack. Insert the wire mesh ronde. Fill in the corundum balls. The tungsten will be filled in portions by means of wire mesh spacers. Set the forming tool on the reduction tube and insert the flat spacer into the recess of the tool. Press the spacer into the tube with the filling rod.
8 - Maintaining the instrument 226 Removing/installing and conditioning the reaction tubes In this section Removing the reaction tubes from the furnace ............................................................................227 Installing reaction tubes in the furnace and conditioning .............................................................
8 - Maintaining the instrument 227 Removing the reaction tubes from the furnace Process The section is divided into the following phases: Preparing the instrument, gas pressure Removing reaction tubes Safety instruction Strictly observe the safety instruction "Removing reaction tubes" under Warning notes during operation (on page 24). Requirements Before starting work, the following requirements must be met: Keep a tube rack ready to hold hot components.
8 - Maintaining the instrument 228 Top view furnace The following picture shows a top view of the furnace pulled out: Legend: 1 Post combustion tube plug 2 Post combustion tube 3 Combustion tube connection 4 Combustion tube 5 Reduction tube plug 6 Reduction tube Phase 2: Removing reaction tubes, continued Proceed as follows: Press the reduction tube plug (5), the combustion tube connection (3) and the post combustion tube connector (1) down lightly and pull the furnace out of the instrument to the fr
8 - Maintaining the instrument 229 Remove the quartz glass bridge. Hold the quartz glass bridge and detach the ground-in clamps. Pull the reduction tube (6), the combustion tube (4) and the post combustion tube (2) out of the furnace and place them in the tube rack. Place the tube rack on a level, non-combustible surface. Protect the hot parts from unauthorized access.
8 - Maintaining the instrument 230 Top view furnace The following picture shows a top view of the furnace pulled out: Legend: 1 Post combustion tube plug 2 Post combustion tube 3 Combustion tube connection 4 Combustion tube 5 Reduction tube plug 6 Reduction tube Phase 1: Installing reaction tubes Proceed as follows: Close the reduction tube (6) with the plug (5). Close the combustion tube (4) with the combustion tube connector (3). Close the post combustion tube (2) with the plug (1).
8 - Maintaining the instrument 231 Note: When you close the ground-in ball-and-socket joints, you must be able to feel an elastic resistance when you press the o-rings into the pans, otherwise you must replace the o-rings. Place the ungreased seal on the combustion tube connection (3) at the top. Check whether the seals are in the pans of the plugs of combustion and post combustion tube.
8 - Maintaining the instrument 232 Close the front door. Phase 2: Conditioning the reaction tube, getting the instrument ready to measure Proceed as follows: Close the "Replace part" dialog in the operating software. To do so, click Finish in the "Replace part" dialog. By doing so, the gas will be automatically turned on. and the atmospheric nitrogen is removed by flushing with CO2 for five minutes.
8 - Maintaining the instrument 233 Filling, removing and installing the absorption and drying tubes Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section enables you to fill, remove and install the drying tubes. In this section Filling the drying tubes.................................................................................................................234 Removing and installing the drying tubes .........................................
8 - Maintaining the instrument 234 Filling the drying tubes Note Note the following rules: Observe the filling heights indicated as exactly as possible. The tube filling must not have any cavities. Therefore, tap the tube wall with a piece of wood or cork when filling the tubes. If the Sicapent® cannot be tapped properly, also a glass rod for slight compacting can be used. Since the life time depends on the amount of Sicapent®, it is recommended to achieve a mean density as high as possible.
8 - Maintaining the instrument 235 Drying tube filling (large) The following picture shows the fillings of the drying tube: Legend: 1 Empty space 2 Cotton (10 mm) 3 Sicapent® (314 mm) Safety instruction Strictly observe the safety instruction "Filling the drying tube" under Warning notes during operation (on page 24). Filling the drying tubes Proceed as follows: Disconnect both tubes. Remove the glass tube. Detach the screw-on caps. Leave approx. 5mm space (1) at the end of the tube.
8 - Maintaining the instrument 236 Notes regarding further operation The drying tube fillings must be replaced regularly in order to ensure correct readings. The drying agent is charged with an indicator which shows the used up zones of the tube. If ¾ of the desiccant is discolored, the filling must be replaced. Removing and installing the drying tubes Function of the drying tubes The drying tubes bind traces of water that would impair both the IR signal (blank value) and the lifetime of the IR detector.
8 - Maintaining the instrument 237 To prepare the instrument for maintenance work follow the instructions in Preparing and following up maintenance work (on page 171). Phase 2: Removing the drying tubes Proceed as follows: Open the front door. Unscrew the small drying tube (1). Loosen the red caps. Remove the small drying tube (1) from the instrument. Unscrew the large drying tube (2). Loosen the red caps. Remove the large drying tube (2) from the instrument.
CHAPTER 9 Repairing the instrument Target group Personnel authorized by BÜCHI Labortechnik AG and having undergone training. Purpose This section is designed to restore proper working order of the instrument. In this chapter Interpreting PC error messages ..................................................................................................240 Performing a system test .............................................................................................................
9 - Repairing the instrument 240 Interpreting PC error messages Software reaction to errors When an error is detected, the software displays its error code on screen and saves it to the "error buffer". If the error is a critical error, the instrument is stopped immediately.
9 - Repairing the instrument 241 Interpreting combustion module error messages and troubleshooting The following table lists combustion module error messages, explaining the causes of the errors and giving tips for troubleshooting: Combustion module error messages Possible causes Corrective action Ambient temperature too high Fan failure. Front door of the instrument was open too long. Release the thermoclick (1) above the furnace again. Then restart the instrument and the software. Cf.
9 - Repairing the instrument 242 Performing a leak test Purpose of the leak test The leak test checks the instrument for leaks. Performing a leak test The instrument software includes two types of leak test: Rough leaktest and fine leaktest. The rough leak test is used to check quickly the system for gas-tightness. The fine leak test checks the gas-tightness of the system by using severer criteria and, in case a leak has been detected, supports you during the leak search procedure.
9 - Repairing the instrument 243 Leak test procedure Process The execution of the leak test takes place in several steps. The leak test always starts with testing of the whole system (Whole leak test). If the program detects a leak during the whole leak test, it will provide additional test stages. The purpose of these test stages is to test only a certain section of the system in sequence. As long as no leak can be detected the next section will be added to the test.
9 - Repairing the instrument F7 + F8 244 Furnace transformer 15 A Process The section is divided into the following phases: Allow instrument to cool down and disconnect from the mains Remove and check fuse Insert fuses Switch the instrument on again Note Please note: If the fuses trip, please always notify your service office as there may be serious reasons for this. Only use fuses matching the indicated type and the indicated voltage on the fuse holder.
9 - Repairing the instrument 245 Phase 2: Remove and check fuse Proceed as follows: If a part of the instrument is no longer working, consult the above table to find out which fuse is resposible for the component. First remove the rear wall. To do that, unscrew the rear wall retaining screws and pull the protective earth conductor connector out of the rear wall. The following picture shows the protective earth conductor connector: Then remove the rear wall.
9 - Repairing the instrument The electrical section is now visible. Pull out the fuse holder of the appropriate fuse. Press the fuse out. Check the fuse: If the fuse wire... ... is visible: Check whether the wire is broken or not. ... is not visible: Measure fuse continuity. 246 Make a decision for the further proceeding: If... ... the fuse wire is broken: Insert a new fuse of the same type. ... no continuity was measured on the fuse: Insert a new fuse of the same type.
9 - Repairing the instrument Plug the protective earth conductor back into the rear wall. Attach the rear wall again. 247 Phase 4: Switch the instrument on again Proceed as follows: Plug the power supply plug of the analyzer into the socket. Switch PC, monitor and printer on. Wait until the boot process is completed. Switch the main instrument switch on. The instrument performs a reference run of the VLS. Launch the operating software.
9 - Repairing the instrument 248 Reacting to a power failure Open document An open document is not lost in the event of a power failure. The temporary document file is automatically loaded when the operating software is restarted.
9 - Repairing the instrument 249 Perform a leak test by selecting Options > Diagnostics > Leak Test.See Performing a leak test (on page 242). If a leak is identified, replace the sealing elements in the furnace area. See Replacing sealing elements. There may still be some residue of the last sample in the combustion section. Perform blank value determinations to remove the residues. See Determining blank values (on page 144). Correct the number of the current sample via Edit > Current sample.
9 - Repairing the instrument 250 Checking air-tightness of instrument Proceed as follows: Perform a leak test to check the air-tightness of the instrument. See Performing a leak test (on page 242). If any leaks are detected, replace all sealing elements in the furnace area. See Replacing sealing elements.
9 - Repairing the instrument 251 Weigh the sample If the weight is not transmitted online, enter the weight by hand in the sample view on the PC. Insert the new sample on the carousel. Open the "Set current weigt" dialog again by selecting Edit > Current weight. Use the arrows to set the number following the number of the last sample. Click OK. This closes the dialog and the cursor moves to the "Weight" column of the selected sample number.
9 - Repairing the instrument 252 Exporting analysis data Proceed as follows: Open the "Export document" dialog in the operating software by selecting File > Export/Import > Export. Select the desired document file and click OK. This displays the "Save file as" dialog. Select the directory to export the document to from the "Save" dropdown listbox. Select the "MS Access Files (*.mdb) file type from the "File type" dropdown listbox and click Save.
CHAPTER 10 Menu and dialog descriptions Target group Personnel involved with the instrument. Purpose This section describes the dialogs and commands in the various menus in the software. Note The order of the menu commands in this document corresponds to the menu structure of the instrument software. If the invokation of a menu command opens a dialog the corresponding dialog wil be described directly instead of describing the menu command. In this chapter Dialog descriptions key.........................
10 - Menu and dialog descriptions 254 Dialog descriptions key Element types The following list provides pictures of element types that feature in the dialog descriptions: Element type Example picture Label Dropdown listbox Checkbox Listbox Radiobutton Button Sliding controller Listbox column Textbox Textbox/label Textbox with checkbox Textbox with buttons Operation Manual D-480 ©BÜCH Labortechnik AG
10 - Menu and dialog descriptions 255 File menu Purpose This section describes commands and dialogs for this menu. In this section File > New (Command)................................................................................................................256 Select document name (Dialog) ..................................................................................................256 Select version (Dialog) ......................................................................................
10 - Menu and dialog descriptions 256 File > New (Command) What is the command used for? This command creates a new document. Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + N Select document name (Dialog) Function The function of this dialog differs depending on how you open it: If it was opened via File > Export/Import > Export, you can select a document to be exported. If it was opened via File > Open you can select a file to load from the database into sample memory.
10 - Menu and dialog descriptions 257 Label Element type Meaning Mode Dropdown listbox Field in which you can select the operating mode as the filter criterion. Only documents in the selected operating mode are displayed. from Textbox with checkbox Field in which you can select a date as the filter criterion. Only documents as from the selected date are displayed if the checkbox next to the date display is checked.
10 - Menu and dialog descriptions 258 Label Element type Meaning Signatures Listbox column Column displaying for what purpose the document was already signed. If the document is unsigned, the column is empty. For the first signature the column displays "created". For the second signature the column displays "checked". For the third signature the column displays "released".
10 - Menu and dialog descriptions 259 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Finding documents (on page 163). Versioning (on page 74). 21 CFR Part 11 functionality (on page 73). Consequences of modifying analysis data (on page 89). Select document name (on page 256).
10 - Menu and dialog descriptions 260 File > Delete (Command) What is the command used for? This command allows you to remove the current open document from the database. Before deleting, the program displays a dialog in which you must confirm that you want to delete the document. Note If 21 CFR Part 11 functionality is enabled, the "Comment change" dialog is displayed after deleting the document from the database. The user must justify deletion of the document in this dialog.
10 - Menu and dialog descriptions 261 Sign (Dialog) Function In the dialog: the user is warned about signing documents that may still need to be edited. After signing, the document is read-only. you can sign a document with an electronic signature. A document may be signed up to three times. Open You can open this dialog, if 21CFR11 functionality is enabled, via File > Sign: Elements The following describes the elements of the dialog.
10 - Menu and dialog descriptions 262 Open You can open this dialog, if 21 CFR Part 11 functionality is enabled, via: File > Verify or via the Signatures button in the "Select document name" dialog. Elements The following describes the elements of the dialog. Label Element type Meaning created Radiobutton verify "created" signature. If the radio button is locked, the signature does not yet exist. checked Radiobutton verify "checked" signature.
10 - Menu and dialog descriptions 263 Label Element type Meaning Cancel Button Aborts the process and discards settings not yet saved. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Exporting LIMS data (on page 160). Laboratory information and management system (LIMS) (on page 72). LIMS export settings (on page 81). Conditions for operating the LIMS. LIMS settings (on page 311).
10 - Menu and dialog descriptions 264 Open Open the dialog via: Menu command Button File > Print Hot key CTRL + P File > Report configuration --- File > Print preview --CTRL + S Elements The following describes the elements of the dialog. In section "Title": Label Element type Meaning Line 1 Textbox Field to input a header. Line 2 Textbox Field to input a header. Line 3 Textbox Field to input a header.
10 - Menu and dialog descriptions 265 Print (Dialog) Function In this dialog you can define print settings. The appearance of this dialog depends on the type of printer installed / activated. It is usually used to define the following: the number of copies to print, the print format, and print quality.
10 - Menu and dialog descriptions 266 Remaining elements: Label Element type Meaning OK Button Starts the printing process according to the settings. Cancel Button Discards settings not yet saved. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Data backup and printing (on page 158). Configure report (on page 157). Display print preview (on page 157). Optimizing data evaluation (on page 101).
10 - Menu and dialog descriptions 267 Printer setup (Dialog) Function In this dialog you can specify the printer and its connection. The appearance of this dialog depends on the type of printer installed / activated. Open Open the dialog by selecting File > Printer Setup. Elements The following describes the elements of the dialog. In section "Printer": Label Element type Meaning Name Dropdown listbox Field displaying a list of printers connected to the computer.
10 - Menu and dialog descriptions 268 Open (Dialog) Function In this dialog you can specify the following for the file to import: Directory containing the file to import, File name of the import file, File type of the import file. Note You can only import files: created with the operating software via File > Export/Import > Export. generated by the "Balance" weighing data capture program. Imported data are stored in sample memory.
10 - Menu and dialog descriptions 269 Load balance file (Dialog) Function In this dialog you can select whether to insert the weighing data to be imported in an open document or in a new empty document. Open Open the dialog by selecting File > Export/Import > Import. First the "Open" dialog is displayed in which you can select and open the weighing data. Then the "Import balance file" dialog is displayed. Elements The following describes the elements of the dialog.
10 - Menu and dialog descriptions 270 In section "Backup": Label Element type Meaning Select Button Opens the "Find directory" dialog in which you can select the directory to save to. The operating software must have write access to the directory in order to be able to save the backup correctly. --- Label Field displaying the selected directory. Keep max. last n backup files Textbox with buttons Field to input the number of backup files to keep at the same time.
10 - Menu and dialog descriptions 271 Clean database (Dialog) Function In the dialog: the user is warned about reorganizing the database without backing up first. you can start a backup, you can start reorganizing the database. Caution Data loss! Reorganizing the database irrevocably deletes all sample data and the contents of the database logbook. Always backup your data before reorganizing the database.
10 - Menu and dialog descriptions Caution 272 Data loss! Restoring the database via Restore irrevocably overwrites all sample data, the contents of the logbook and the database configfuration parameters. Always backup your data before restoring the database via Restore. Open Open the dialog by selecting File > Backup/Restore > Restore. Elements The following describes the elements of the dialog.
10 - Menu and dialog descriptions 273 Label Element type Meaning Cancel Button Aborts the process or discards the new user data if the operating software is already running. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Starting the operating software (on page 130). User administration. File > Logoff (Command) What is the command used for? The current user will be logged off.
10 - Menu and dialog descriptions 274 Edit menu Purpose This section describes commands and dialogs for this menu. In this section Edit > Redo (Command) ..............................................................................................................275 Edit > Undo (Command) ..............................................................................................................275 Edit > Cut (Command) .....................................................................................
10 - Menu and dialog descriptions 275 Edit > Redo (Command) What is the command used for? This command restores an action that you have previously undone. Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + Y Edit > Undo (Command) What is the command used for? This command undoes a previous action. Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + Z Note You can undo up to five previous actions.
10 - Menu and dialog descriptions 276 Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + C Note You cannot execute this command if no data are selected. Copying data to the clipboard replaces the data previously stored in the clipboard. Edit > Paste (Command) What is the command used for? This command inserts a copy of the clipboard contents at the cursor position.
10 - Menu and dialog descriptions 277 Short cuts Invocation via the toolbar: Note The line to delete must be selected. Executing this command deletes the line and all subsequent lines move up one line. Swap samples (Dialog) Function In this dialog you can swap unprocessed samples in sample memory, e.g. if you want to prioritze urgent samples. Note The samples are only swapped in sample memory. After displaying the dialog, you must swap the appropriate samples on the carousel by hand.
10 - Menu and dialog descriptions 278 If 21 CFR Part 11 functionality is enabled, a new version of the document is created the next time it is saved. Set stop tag (Dialog) Function In this dialog you can specify the sample at which to set the stop marker. Usually, the program automatically moves the stop marker while you input sample data. Therefore it is only necessary to move the stop marker manually in special cases.
10 - Menu and dialog descriptions 279 by clicking the right mouse key to the corresponding sample cell. Select Set current sample... from the popping-up context menu. Elements The following describes the elements of the dialog. Label Element type Meaning Current sample at: Textbox with buttons Field to input a sample number OK Button Saves the setting. Cancel Button Aborts the process. You can also set the sample number in the textbox using the arrows.
10 - Menu and dialog descriptions 280 Note After invoking this command the dialog "Recalculate Hole Postions " opens. Here you can define when the recalculation of the hole positions shall be started. Samples with a low number will not be influenced by the recalculation.
10 - Menu and dialog descriptions 281 View menu Purpose This section describes commands and dialogs for this menu. In this section View > Toggle (Command) ..........................................................................................................282 Zoom in/out (Dialog) ....................................................................................................................282 Configure view (Dialog) ...............................................................................
10 - Menu and dialog descriptions 282 View > Toggle (Command) What is the command used for? This command changes the field in the combi view. Note Execute this command several times to switch to the desired view. The sequence is: Calibration view - progression graph - statistics view - calibration view, etc. Also by clicking on the caption bar of the combi view you can change to the reqested view.
10 - Menu and dialog descriptions 283 Elements The following describes the elements of the dialog. Label Element type Meaning Display column Label All sample data listed in this column are displayed. Hide column Label All sample data listed in this column are not displayed. ^ Button Changes the display sequence of the sample data. Moves selected samples one position to the left in the sample view (text view).
10 - Menu and dialog descriptions 284 Elements The following describes the elements of the dialog. Label Element type Meaning Column Label This field displays the column for which to set the number of decimal places. Decimal places Textbox Field to input the desired number of decimal places. 0 to 7 decimal places are possible. OK Button Saves new settings Cancel Button Discards settings not yet saved.
10 - Menu and dialog descriptions 285 Load views (Dialog) Function In this dialog you can reload saved sample views. However, you can only load a view if the view was saved in the same operating mode as the current mode in which the analyzer is running. Open Open the dialog via View > Gridview > Load configuration. Elements The following describes the elements of the dialog. Label Element type Meaning --- Textbox/label Field displaying the name of the selected view.
10 - Menu and dialog descriptions 286 View > Gridview > Auto align (Command) What is the command used for? This command optimizes the sample view: The individual columns are automatically widened or narrowed to make the headers and entries completely visible. Configure graph view (Dialog) Function In this dialog you can define the appearance of the graph view. Open Open the dialog via View > Graphic > Configure. Progression view (graph view) must be enabled in order to open the dialog.
10 - Menu and dialog descriptions 287 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Data backup and printing (on page 158). Configuring the graph view (on page 156). Right mouse button function (on page 69). View > Gaphic > Auto align (Command) What is the command used for? This command optimizes the graph view: The graph is scaled so that it is completely visible.
10 - Menu and dialog descriptions 288 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Configure statistics view (on page 150). Right mouse button function (on page 69). View > Statistic > Auto align (Command) What is the command used for? This command optimizes the statistics view: The individual columns are automatically widened or narrowed to make the headers and entries completely visible.
10 - Menu and dialog descriptions 289 System menu Purpose This section describes commands and dialogs for this menu. In this section System > Auto run (Command) ...................................................................................................290 System > Single run (Command) ................................................................................................290 System > Stop (Command) ...........................................................................................
10 - Menu and dialog descriptions 290 System > Auto run (Command) What is the command used for? This command starts continuous analysis, i.e. the system processes all samples in sample memory up to the stop marker. Once the system reaches the stop marker, it either goes into idle mode or sleep mode, depending on settings. Short cuts Invocation via the toolbar: Note You can only start the system if the following system conditions exist: System pressure is at least 800 mbar.
10 - Menu and dialog descriptions 291 Note The "Abort analysis" dialog appears. Observe the notes listed therein. Abort analysis only if either the sample has not been thrown in yet or has been already completely combusted. In the latter case, make sure that the column does not retain any element components, i.e. the desorption procedure has been completed. Otherwise, an abortion leads to system contaminations combined with significant damages.
10 - Menu and dialog descriptions 292 Label Element type Meaning Cancel Button Aborts the process. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Stopping continuous analysis (on page 250). Right mouse button function (on page 69). Adjust carousel position (Dialog) Note This function is only available in the solides modes.
10 - Menu and dialog descriptions 293 Label Element type Meaning Position Radiobutton Moves the carousel moves to the desired position. You can set the position number in the textbox to the right. You must input the desired position number minus 1. Reference run Radiobutton The carousel performs reference run, i.e. the carousel first moves to a defined reference position and then to position 0 which has almost the same location.
10 - Menu and dialog descriptions 294 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Selecting the operating mode (on page 131).
10 - Menu and dialog descriptions 295 Windows menu Purpose This section describes commands and dialogs for this menu. In this section Windows > Toolbar / Run-Bar (Command)..................................................................................296 Toolbar ........................................................................................................................................296 Windows > Recent sample (Command) ......................................................................
10 - Menu and dialog descriptions 296 Windows > Toolbar / Run-Bar (Command) What are these commands used for? This command shows or hides the toolbar and the run bar. If the toolbar and/or the run bar is displayed, a check will appear next to the menu item. See Toolbar (on page 296).
10 - Menu and dialog descriptions Icon 297 Command Calibration > Next sample System > Wake-up Help > About ... System > Auto run System > Single run System > Single run (when manual injection is selected) Note The number of the available symbols in the toolbar can be different depending on the instrument type. Windows > Recent sample (Command) What is the command used for? This command shows or hides the enhanced display of the sample analyzed most recently.
10 - Menu and dialog descriptions 298 Label Element type Meaning No. Label Displays the number of the weighed-in sample. The number of the current weighed sample is displayed in a larger font. Wt. [mg] Label Displays the weight of the weighed-in sample. The weight of the current weighted sample is displayed in a larger font. Name Label Displays the name of the weighed-in sample. The name of the current weighed sample is displayed in a larger font.
10 - Menu and dialog descriptions 299 Options menu Purpose This section describes commands and dialogs for this menu. In this section Maintenance intervals (Dialog) ....................................................................................................300 Replace part (Dialog)...................................................................................................................301 Commands for the maintenance of the liquid sampler VLS .............................................
10 - Menu and dialog descriptions 300 Maintenance intervals (Dialog) Function In this dialog, any number of maintenance events can be defined and viewed. Open Open the dialog via Options > Maintenance > Intervals. Elements The following describes the elements of the dialog. Label Element type Meaning --- Listbox In this field the texts of all currently defined events are displayed.
10 - Menu and dialog descriptions 301 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Defining maintenance intervals in the software (on page 170). Viewing the status of maintenance intervals (on page 170). Installing used tubes (on page 171). Maintenance work to be performed by the customer (on page 169).
10 - Menu and dialog descriptions 302 Commands for the maintenance of the liquid sampler VLS Commands for the maintenance of the liquid sampler VLS The commands as well as the procedures for the maintenance of the liquid sampler are described in the VLS operating instructions. Leak test (Dialog) Function This dialog is used to perform a leak test and the leak search: In the display window the tubing diagram of the analysis system is shown.
10 - Menu and dialog descriptions 303 Maintenance work to be performed by the customer (on page 169). Leak test: Test phases (Dialog) Function This dialog displays the current status while performing a leak test. The left half of the dialog displays the individual stages of the test. The current stage of the test is marked with an arrow. The right half of the dialog displays the remaining time of the respective stage of the test and system pressure.
10 - Menu and dialog descriptions 304 In the lower area: Label Element type Meaning Result Label This field displays whether the leak test was successful or not. The following symbols highlight the leak test result: ..... Leak test successful. ..... Leak test failed. Print Button Prints the result after the leak test finishes. Cancel Button Aborts the leak test.
10 - Menu and dialog descriptions 305 Label Element type Meaning Apply Button Heats up the corresponding furnace to a previously entered temperature. The fields display the current temperatures. Placing the cursor in one of these fields "freezes" the temperature displayed there. You can now input a setpoint temperature. By clicking Apply the corresponding furnace will be controlled to the setpoint temperature.
10 - Menu and dialog descriptions 306 Remaining elements: Label Element type Meaning Close Button Closes the dialog. Help Button Opens the description of the dialog in the help. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Performing a system test. Error buffer (Dialog) Function This dialog displays a chronological list of all errors and events detected by the system.
10 - Menu and dialog descriptions 307 Open Open the dialog via: Options > Diagnostics > Error display or by double-clicking the appropriate event line in the "Error buffer" dialog. See Error buffer (on page 306). Elements The following describes the elements of the dialog. Label Element type Meaning Input error code Textbox Field to input the appropriate error code. Once the input box contains a code number, the program displays the decoded result green in the section above it.
10 - Menu and dialog descriptions Label 308 Element type autom. AutoRadiobutton increment the number in the sample name Meaning If a sample name ends with a number (e.g. "Name001"), this figure is automatically incremented by a certain amount and suggested for the next sample (e.g. "Name002"). Exceptions: autom. AutoRadiobutton decrement the number in the sample name If the number of characters is completely used up (e.g.
10 - Menu and dialog descriptions 309 Label Element type Meaning Name Textbox/label Field to input the name of the standard sample. {Element} conc. [%] (or {Element} conc. [ppm]) Textbox/label Field to input the theoretical percentage content of the corresponding element in the respective sample. {Element} tolerance [%] Textbox/label Field to input the tolerance limit of the corresponding element. The tolerance limit is required if standard tolerance monitoring is enabled.
10 - Menu and dialog descriptions 310 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Defining keywords for blank and conditioning samples (on page 121). Acoustic signals (Dialog) Function In the dialog you can enable and disable acoustic signals to be output when certain events occur. The individual signals vary in pitch for easier distinction.
10 - Menu and dialog descriptions 311 Open Open the dialog via Options > Settings > Calculation. Elements The following describes the elements of the dialog. In section "Factor determination": Label Element type Meaning sequentially Radiobutton The daily factor is computed sequentially. total Radiobutton The daily factor is computed as a total. manual input Radiobutton The daily factor can be entered manually, there will be no calculation of the daily factor. autom.
10 - Menu and dialog descriptions 312 If you are using multiple analyzers with one PC, you must specify one instrument identifier on the "Identifier" tab so that the LIMS data can be allocated to the correct instrument. You can also define user names. Note Note that the LIMS port name must not be identical to the port name between the PC and the analyzer. This could lead to a system crash. Open Open the dialog via Options > Settings > LIMS. Elements The following describes the elements of the dialog.
10 - Menu and dialog descriptions 313 In section "Network": Label Element type Meaning Path name Textbox This field displays the path to store the data. Browse Button Opens the "Find folder" dialog in which you can search the file structure and select a directory. The path must already exist, it cannot be created from the instrument operating software. File extension samples Textbox Field to input the file extension. The file name is automatically generated by the program as follows: dddsssss.
10 - Menu and dialog descriptions 314 Valid for all tabs: Remaining elements: Label Element type Meaning OK Button Saves new settings Cancel Button Discards settings not yet saved. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Exporting LIMS data (on page 160) Defining the LIMS / PC interface (on page 86). Laboratory information and management system (LIMS) (on page 72).
10 - Menu and dialog descriptions 315 Label Element type Meaning Peak anticipation Textbox Field to input a time. Defines the time the system waits for the occurrence of the nitrogen peak. If the system has not detected a peak start after expiration of this peak expectation time, it assumes that the sample does not contain nitrogen. Integrator reset delay Textbox Field to input a time. Defines the time after which the integrator is reset to zero before beginning actual integration. Max.
10 - Menu and dialog descriptions 316 Label Element type Meaning O2 dosing time Textbox Field to input the duration of O2 dosing during the combustion phase. O2 dosing flow Textbox Field to input the duration of oxygen flow during the combustion phase. O2 cut off threshold Textbox Field to input a value which delimits the oxygen excess. If during the oxygen dosing the measured oxygen concentration exceeds this value, then the oxygen supply will be turned off.
10 - Menu and dialog descriptions 317 Elements The following describes the elements of the dialog. Label Element type Meaning Standard tolerance monitoring Checkbox Every finished standard sample is checked as to whether the computed percentage contents are inside the defined tolerance range for theoretical percentage contents. If the tolerance limit is exceeded, continuous analysis is aborted and "Tol" is entered in the info column of the appropriate sample.
10 - Menu and dialog descriptions 318 In section "Sleep": Label Element type Meaning Sleep disabled Radiobutton The sleep/wake-up function is disabled. Sleep after end of sample Radiobutton The analyzer goes into sleep mode after finishing the last sample (indicated by the stop marker). Sleep at sample No. Option field / textbox The analyzer goes into sleep mode when it reaches the specified sample. You can enter the sample number in the adjacent textbox.
10 - Menu and dialog descriptions 319 Monthly logbook (Dialog) Function This dialog contains records of the actions performed by various users in chronological order. You can search for and print out certain information via the dialog menus. The following information is stored for each action: Date and time of the action, Name of the person who performed the action, Type of action, Description of changes, e.g. of parameters, User's justification if the action needed to be justified.
10 - Menu and dialog descriptions 320 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Viewing the logbook (on page 92). 21 CFR Part 11 functionality (on page 73). Select period (Dialog) Function In this dialog you select the period for which to display the logbook. Open Open the "Logbook for month..." dialog via Options > Logbook. Open the "Select period" dialog by selecting File > Load.
10 - Menu and dialog descriptions 321 Safety instruction Strictly observe the safety instruction "Improper changes" under Warning notes during operation (on page 24). Note This section only describes the sections of the tabs in which you can make changes via the "Device configuration" dialog only, as these sections do not have their own settings menu. If 21 CFR Part 11 functionality is enabled, every change to the configuration must be justified in the "Comment modification" dialog.
10 - Menu and dialog descriptions 322 Entry Standard Description Parity N Defines the type of parity check of the serial interface between the PC and the analyzer. N= no parity check E= even parity check O= odd parity check. The following table describes the entries under the "BalancePort" section: Entry Standard Description Name ---- Defines the serial interface between the PC and the balance.
10 - Menu and dialog descriptions 323 The following table describes the entries under the "System" section: Entry Standard Description Logon Timeout 60 Defines the time that must expire before the program displays the login dialog again. User1 --- Specifies the name of the user group which the instrument software regards as level 1 users. User2 Specifies the name of the user group which the instrument software regards as level 2 users.
10 - Menu and dialog descriptions 324 Label Element type Meaning OK Button Saves new settings Cancel Button Discards settings not yet saved. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Granting authorizations (on page 83). Defining logon timeout (on page 78). Creating new sections (on page 79). Defining the analyzer / PC interface (on page 86).
10 - Menu and dialog descriptions 325 Math menu Purpose This section describes commands and dialogs for this menu. In this section Math > Blank values > Calculate (Command) .............................................................................326 Blank values (Dialog)...................................................................................................................326 Math. > Factor (Command) ..........................................................................................
10 - Menu and dialog descriptions 326 Math > Blank values > Calculate (Command) What is the command used for? This command starts a calculation of blank values. The results are entered in the appropriate columns in text view. Note Blank value calculation is only performed if sample memory contains blank samples.
10 - Menu and dialog descriptions 327 Routine measuring work (on page 56) Types of blank value determination and their settings (on page 143) Formulae for blank value determination and compensation (on page 57) Math. > Factor (Command) What is the command used for? This command computes the daily factor of a series of analyses. Define type of peak (Dialog) Function In this dialog the behavior of the manual peak integration will be defined. Open Open the dialog by selecting Math.
10 - Menu and dialog descriptions 328 The dialog The appearance of the dialog depends on the selected peak type. Open Open the dialog by selecting Math. > Manual Peak Integration > Integrate. Elements The following describes the elements of the dialog. Label Element type Meaning Button Allows the setting of the start tag of the single and/or total peak. Button Allows the setting of the end tag of the single and/or total peak. Button Allows the vertical movement of the baseline.
10 - Menu and dialog descriptions 329 Elements The following describes the elements of the dialog. Label Element type Meaning Total Radiobutton Defines that the total area shall be used for the assignment. "Superimposed" peak Radiobutton Defines that the area of the superimposed peak (ligh red color) shall be used for the assignment. (Not available for single peak integration) Socket Radiobutton Defines that the area of the socket (light blue color) shall be used for the assignment.
10 - Menu and dialog descriptions 330 Math. > Recalculate (Command) What is the command used for? This command recomputes the results of all samples in sample memory. This makes sense, for example, if you have analyzed a calibration series and then a measuring series immediately afterwards (e.g. overnight). If you compute the coefficients the next day, you must recompute the appended measuring samples with the newly computed coefficients.
10 - Menu and dialog descriptions 331 Statistics menu Purpose This section describes commands and dialogs for this menu. In this section Statistics > Via names (Command) .............................................................................................332 Statistics > Group (Command) ....................................................................................................332 Statistics > Sort group (Command) ...........................................................................
10 - Menu and dialog descriptions 332 Statistics > Via names (Command) What is the command used for? This command combines samples of the same sample name into a statistical group. The statistical groups are then displayed in the combi view statistics view together with the appropriate results. Statistics > Group (Command) What is the command used for? This command combines two or more selected samples into a statistical group.
10 - Menu and dialog descriptions 333 Statistics > Include/Exclude sample (Command) What is the command used for? This command either includes a sample in the calculation or excludes it. Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + T Note You can execute this command in the following cases: In the statistics view: The selected sample of a statistical group is displayed crossed-out (disabled) and the statistics calculation is performed without this sample.
10 - Menu and dialog descriptions 334 Calibration menu Purpose This section describes commands and dialogs for this menu. In this section Calibration coefficients (Dialog) ...................................................................................................335 Configure calibration (Dialog) ......................................................................................................336 Specify lower and upper calibration range (Dialog) ..............................................
10 - Menu and dialog descriptions 335 Calibration coefficients (Dialog) Function This dialog displays the calibration coefficients on a tab. With suitable permission, you can also manually input the coefficients. Note the following for manual input Observe the following when manually inputting calibration coefficients. Sample memory must be empty, otherwise manual input is not possible. The program interprets the comma as a decimal separator and the * sign as an exponent.
10 - Menu and dialog descriptions 336 Label Element type Meaning Cancel Button Discards calibration coefficients that have just been computed or input. Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Viewing calibration coefficients (on page 177). Defining standard substances as calibration samples (on page 122). Performing calibration. Background knowledge required for calibration (on page 52).
10 - Menu and dialog descriptions 337 Further information Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog: Defining standard substances as calibration samples (on page 122). Background knowledge required for calibration (on page 52). Calibration formulae (on page 55).
10 - Menu and dialog descriptions 338 Calibration > Next sample (Command) What is the command used for? This command moves the sample marker to the next sample in the calibration graph. Short cuts Invocation via the toolbar: Invocation via hot key: CTRL + "+" Calibration > Previous sample (Command) What is the command used for? This command moves the sample marker to the previous sample in the calibration graph.
10 - Menu and dialog descriptions 339 Help menu Purpose This section describes commands and dialogs for this menu. In this section Help > Content (Command).........................................................................................................340 Help > Find (Command) ..............................................................................................................340 Help > BÜCHI Labortechnik AG on the WEB (Command) ..........................................................
10 - Menu and dialog descriptions 340 Help > Content (Command) What is the command used for? This command opens the "Contents" tab of the help window in the foreground. Short cuts Invocation via hot key: F1 Help > Find (Command) What is the command used for? This command opens the "Search" tab of the help window in the foreground.
10 - Menu and dialog descriptions 341 In section "Analyzer": Label Element type Type Dropdown listbox Field displaying the instrument type. Meaning Serial number Textbox Field to input the serial number if it was not automatically sent to the program by the analyzer. The serial number is found on the type plate on the back of the analyzer. This number should match the serial number of the installation CD cover when installing for the first time.
CHAPTER 11 Appendix Target group Personnel involved with the instrument. In this chapter Warranty ......................................................................................................................................344 Accessories, spare parts and consumables ................................................................................
11 - Appendix 344 Warranty Target group Personnel involved with the instrument. In this section Warranty of the overall instrument ...............................................................................................345 Warranty on the furnace ..............................................................................................................
11 - Appendix 345 Warranty of the overall instrument Warranty of the overall instrument Please refer to your order for details on the warranty on the overall instrument. Excluded from the warranty Wear and tear parts and consumables are excluded from the warranty. Warranty on the furnace Warranty on the furnace BÜCHI Labortechnik AG gives a 10-year warranty on the furnace.
11 - Appendix 346 Accessories, spare parts and consumables Target group Personnel involved with the instrument. Purpose This secton contains information about ordering accessories, spare parts and consumables. In this section Smallest workable unit.................................................................................................................347 Required accessories ..................................................................................................................
11 - Appendix 347 Smallest workable unit Condition You can only order the smallest workable unit if you already have all of the necessary accessories. See Required accessories (on page 347). Smallest workable unit D-480 basic instrument with initial set including consumables set for approx. 1000 analyses. Computer with control and application software. Component details Basic instrument: Fully automatic elemental analyzer for quantitative determination nitrogen in solid or liquid samples.
11 - Appendix 348 Computer A computer is essential as the control and evaluation unit. The computer can be ordered together with the software. See Smallest working unit. If you are using your own computer, please observe the following requirements: PC with Pentium III processor 500 MHZ (or equivalent) or faster Operating system Windows XP Professional (SP2 or newer) or a newer version of Windows Professional Available disk space min.
11 - Appendix 349 Consumables set for solid samples Optional Required when the material from the initial set is used up. The following table lists consumables for solid samples: Consumable material set product number Number of analyses 16.00-5013 4000 15.00-5019 2000 Accessories for solid samples The following accessories are required for solid samples: Pelletizer (lever press) Hand driven press for pelletizing of solid samples Includes pressing tool Prod. No. 41.
Index 351 Index 2 21 CFR Part 11 functionality - 73, 94, 259, 260, 261, 262, 320 A About this document - 15 Accessories, spare parts and consumables - 346 Acoustic signals (Dialog) - 310 Adjust carousel position (Dialog) - 292 Administrative work on the database - 94, 268, 270, 271, 272 Analysis mode (Dialog) - 293 Analytical characteristics - 31 Analytical characteristics and technical specifications - 30 Appendix - 343 Area assignment (Dialog) - 328 Assessing the calibration curves - 178, 180, 182 B B
Index Defining the balance / PC interface - 87 Defining the Kjeldahl factor - 132 Defining the LIMS / PC interface - 86, 314 Delete views (Dialog) - 285 Deleting documents - 163 Detection of measuring components and evaluation of the measuring signal - 45, 48 Determine measuring units and number of decimal places.
Index Loading a sample view - 150, 285 Log in as (Dialog) - 272 M Maintaining the instrument - 167 Maintaining the Ni flap and the O2 lance - 205 Maintenance intervals (Dialog) - 300 Maintenance work to be performed by the customer - 169, 301, 303, 304 Manual peak integration - 152, 327, 328, 329 Math > Blank values > Calculate (Command) - 326 Math menu - 325 Math. > Factor (Command) - 327 Math.
Index Selecting the operating mode - 110, 131, 294 Set current weighed sample (Dialog) - 279 Set stop tag (Dialog) - 278 Setting device parameters - 50, 118, 177, 315 Setting the size of the graph - 101, 156, 282 Setting up and starting up the instrument - 106 Setting up user administration - 82 Settings for sample input - 133, 308 Showing or hiding the toolbar - 130 Showing or hiding the weight window - 127 Shutting down the instrument - 116 Shutting the instrument down for long measuring breaks (switchin
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