INSTRUCTION MANUAL KL-04

Transcription

1 INSTRUCTION MANUAL LIGHT OBSCURATION PARTICLE COUNTER KL Higashimotomachi, Kokubunji, Tokyo , Japan

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3 Organization of this manual This manual describes the features and operation principles of the Light Obscuration Particle Counter KL-04. For information regarding the operation of other equipment in the case of incorporating the KL-04 into a measurement system with other equipment, always make sure to refer to the documentation of the other equipment. The following pages contain important information on safety. Be sure to read this part. This manual contains the following sections. Outline Describes the features of the unit. Controls and Features Briefly identifies and explains the buttons, lamps, connectors and all other parts of the unit on the front, left side and rear panel. Preparation Describes how to connect the sampling tube, drain tube, power cord and other parts of the unit. Window Operation Describes the basic operation of the windows. Start Up Describes how to start / stop the unit. Operator Management Describes how to register operators and how to set / change their access authorizations. Measurements Provides a basic explanation of measurement. Performance-Test Provides a basic explanation of Performance-Tests. Calibration Provides a basic explanation of calibration. Print Provides a basic explanation of printing. i

4 Export the measured data Describes how to export the measured data by using the built-in floppy disk drive. Back Up Describes how to back up / restore measurement data by using the built-in tape drive. System Setting Provides a basic explanation of how to set the clock and how to connect with a network. Useful Tools Describes how to use the virtual keyboard and how to take a snapshot of the screen. Audit Trail Describes the audit trail function. Maintenance Describes the inspection and maintenance of the unit and how to change the syringe. Troubleshooting Describes checking procedures and countermeasures in case there is a problem during start up and operation. Specifi cations Lists the technical specifications of the unit. * All company names and product names mentioned in this manual are trademarks or registered trademarks of their respective owners. ii

5 FOR SAFETY In this manual, important safety instructions are specially marked as shown below. To prevent the risk of death or injury to persons and severe damage to the unit or peripheral equipment, make sure that all instructions are fully understood and observed. WARNING Disregarding instructions printed here incurs the risk of death or severe injury to persons. Caution Disregarding instructions printed here incurs the risk of injury to persons and/or damage to peripheral equipment. Important Disregarding instructions printed here incurs the risk of damage to the product. Mentioned about the tips to use this unit properly. (This messages do not have to do with safety.) iii

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7 Caution Types of sample fluids The unit is designed for measuring liquid-borne particles. Never use the unit with the liquid types listed below, to prevent false measurement and the possibility of accidents and damage to the unit. - Explosive liquid or mixtures containing explosive fluid - Hydrofluoric acid or other fluid which can cause corrosion of parts in contact with the fluid or mixtures containing such fluid - Liquid with a temperature of less than +15 C or more than +30 C When using different types of sample fluid where mixing can lead to reactions such as thermal build-up, hardening, or particle generation, always perform thorough cleaning to ensure complete replacement. Weight The weight of the unit is about 14 kg. When transporting or otherwise moving the unit, use a suitable trolley or other implement and ensure safety to prevent the risk of injury. When setting the unit, hold the handle tight with one hand and with the other hand hold the cut-out on the opposite side panel. v

8 WARNING Sample fluid danger prevention When toxic sample fluid comes into contact with any part of the human body or when toxic gases generated by the sample fluid are breathed, there is a danger of severe injury or death. Sample fluid also involves the risk of fire, explosion, corrosion, deformation and other effects when other objects are in the surrounding area. Observe the following points closely to prevent leakage and adherence of sample fluid. Do not pass hydrofluoric acid or other sample fluids which can cause corrosion of fluid-contacting parts (their materials are described in the specifications) through the system. Observe the following points when setting up or dismantling a measurement system. - Check the sample fluid for any risks due to toxicity or other harmful properties. - Make sure that sample fluid cannot leak from the system and come into contact with body parts, clothing etc. - When attaching or detaching tubes, connectors etc., always use appropriate protective tools and wear dual-layer gloves. - Double-check all connections before starting the sample fluid flow. When using sample fluid which may produce harmful gases, provide adequate ventilation as prescribed by applicable laws and regulations. Before and after measurement, clean the entire sample fluid system thoroughly to remove any remnants. Otherwise unwanted effects such as thermal build-up, hardening, particle accumulation etc., can occur. This is especially important to prevent the possibility of serious accidents when using the unit to measure different types of sample fluids. Before starting to prepare the system for storage, complete the cleaning process with pure water and verify neutrality (ph7). Dispose of waste sample fluid only as prescribed by applicable laws and regulations. Never mix waste sample fluid with other substances unless absolute safety has been established. vi

9 WARNING The unit uses a laser source This unit is designated as a class 1 laser product according to IEC (2001). The internal particle detector mechanism uses a laser, but it is fully shielded so that the beam cannot exit from the enclosure. The identification label shown at right is affixed to the rear of the unit. "Caution - use of controls or adjustments or performance of procedures other than those specified herein may result in hazardous radiation exposure." vii

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11 Precautions Operate the unit only as described in this manual. Use the unit in locations within the prescribed temperatures and humidity ranges (+15 C to +30 C, 20% to 80% RH). Store the unit in locations within the prescribed temperatures and humidity ranges (-10ºC to +50 C, 90% RH and less). Do not use or store the unit in locations which - may be subject to condensation by sudden changes in temperature, or - may be subject to freezing inside the piping, or - may be subject to splashes of water or other fluids, or to direct sunlight, or - may be subject to air with high salt or sulfur content, to corrosive chemicals, or to gases, or - may be unstable or inclined, or - may be subject to vibrations or shock. Before using the unit, make sure that all cord, cable and tube connections are correctly and safely established. Do not subject the cords, cables and tubes to excessive bending or other force. When disconnecting the cords, cables and tubes, disconnect while holding onto the end of the plug, connector or tube. Use stable power with minimum excessive electrical noise or voltage fluctuation, which meets the conditions in the specifications. Excessive electrical noise, voltage fluctuation or external noise can cause the unit to operate abnormally or malfunction. Ground the unit securely by using a grounded AC outlet. Ungrounded operation incurs the risk of electric shock and damage to the unit. Do not disassemble the unit or attempt internal alterations. If a malfunction should happen to occur, do not try to solve the problem on your own, but rather note the condition of the unit clearly and contact the supplier. The end plugs are required to seal the unit when returning it for maintenance or servicing. Store the plugs in a safe location for later use. The sample fluid system of the unit must always be filled with sample fluid (during measurement, storage, and transport). If the sample fluid system dries up, particle detector problems can occur. Before returning the unit for maintenance or servicing, thoroughly purge the piping with pure water. Then fill the piping with ethyl alcohol and install the end plugs. In addition, use the special packaging box so as to prevent the unit from being subjected to vibrations and shock. ix

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13 Contents FOR SAFETY...iii Outline... 1 Relationship between Calibration, Performance-Test and Measurement... 2 Light Source... 5 Particle Size Detection... 5 Controls and Features... 6 Front Panel... 6 Left Side Panel... 7 Rear Panel... 8 Preparation... 9 Installing the Sample Container Plate... 9 Connecting Sampling Tube Connecting the Drain Tube Connecting the Keyboard and Mouse Connecting Power Cord Connecting the Printer (Local Printer) Connecting to a Network (LAN Cable) Connecting the External Display Electromagnetic Stirrer (Option) Controls and features How to install How to use Window Operation Virtual Desktop Window Menu Pop-up Window Changing the Overlap Order of the Windows Moving a Window Changing the Window Size Selecting Window Closing Windows Start Up Power ON Login Workspace Menu KL-04 - Start New Window Change Displayed Language xi

14 Password Registration and Change Completion (Logout) Method Operator Management Operator Operator Registration Add Operator Change of Operator Registration Details KL-04 - Operator Management Window Measurements Basic Operations Measuring Sequence The Measurement Result To Display Previously Measured Data Measurement - Data Selector window Measurement Parameter Setting Change Measurement Parameters Measurement Parameters Performance-Test Performance-Test Sequence The Performance-Test Result Performance-Test Parameter Setting Changing the Performance-Test Parameters Performance-Test Parameters Calibration Calibration Sequence The Calibration Result Display Calibration Data Calibration Parameter Setting Change Calibration Parameter Calibration Parameter Print PS Files Print Samples Export the measured data Export the measured data Back Up Backup Restore xii

15 System Setting Set Clock KL-04 - Set Clock Window Network Settings Settings for a Printer Connected to the Network Useful Tools Virtual Keyboard TkSnapshot TkSnapshot (Version 0.31) Window The TkSnapshot - Save Window Audit Trail Operations recording in the audit trail Format for recorded items Searching and Viewing the Audit Trail File Audit Trail Backup and Restore When Clock Setting Was Changed Maintenance Syringe Replacement Handling the Syringe Cleaning main unit Noise Level Check and Flow Cell Cleaning Cleaning Using a Cell Cleaning Brush Periodic Maintenance The Standardization of Units by the Regional Pharmacopeia Transport Troubleshooting When the Letters / Figures on the KL-04 Controller Window appear in Red When the Letters / Figures are Displayed in Orange on the KL-04 Controller When the Performance-Test Fails When Message Window Appears When KL-04 Does Not Start Up Normally Cannot Perform Backup/Restore Syringe Response Problem Specifications xiii

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17 Outline The Light Obscuration Particle Counter KL-04 detects particles suspended in a fluid and measures their size and numbers using the light-obscuration method. The unit is an automatic particle measurement system specially designed for process step control and quality management for example at medical production. The light-obscuration principle is optimal for performing insoluble particulate matter tests for injections as prescribed by the Japanese Pharmacopeia (JP), United States Pharmacopeia (USP), and European Pharmacopeia (EP). The unit also provides compliance with regulations for electronic records and signatures, such as 21 CFR Part 11: Electronic Records; Electronic Signatures by the American FDA. However, signature support is provided for handwritten signatures only. The features of the unit are as follows. - Measurable particle size range of 1.3 to 100 µm. - Rated sample fluid flow of 25 ml / min. - Built-in syringe pump enables measurement without connecting to other flow control systems. - Able to set 20 channels of measurable particle size range. - Built-in hard disk can save several years of measurement data. - Built-in tape drive enables backups and restoration of data saved on the hard disk. - Measurement data can be transferred by connecting to networks. Also the measurement data can be exported in TSV (Tab Separated Values) format by using the built-in floppy disk drive. - A printer (Post Script Level 2 and above) can be connected to print out the measurement results. - Conformance with the Instrument Standardization (Calibration, Performance-Test) of the Japanese Pharmacopeia (JP) and the United States Pharmacopeia (USP). RION Co., Ltd. carries out a standardized system test (Calibration, Performance- Test) as a factory option. - Whether the measurement result is acceptable or not can be decided. - An external display can be connected. - All major operations affecting electronic records such as measurement data creation, modification, and deletion are recorded as audit trail information which can be viewed and printed. - Access control for functions such as measurement data modification and deletion can be set for individual operators. 1

18 Outline Relationship between Calibration, Performance-Test and Measurement When the unit is shipped from the factory, a maximum of 4 optional Calibrations, including options, is supplied as well as the Performance-Test, used to confirm that the measurement system is appropriate (based on the methods decided by RION Co., Ltd. (Basic measurement) and each Pharmacopeia). The Calibration data is the data used on each calibration method when the unit is shipped from the factory. By applying one of these calibration settings, the unit can be set to the same condition as the time when it was initially calibrated. The tests confirming whether the system condition is appropriate or not are called Performance-Tests and their results are called Performance-Test data. The Calibration data applied to each unit and the results of Performance-Test are recorded in the Performance-Test data. Passing the Performance-Test indicates that the unit is in the same condition as at the time when it was calibrated. The relationship between Calibration, Performance-Test and measurement is shown on the chart below. Quality control method Basic measurement JP USP EP Calibration data KL-04_Basic JPxx (Particle size calibration) USPxx (Particle size calibration) JPxx or USPxx (Particle size calibration) Performance-Test data KL-04_Basic JPxx (Unit test) USPxx (Unit test) JPxx or USPxx (Unit test) Measurement parameter For basic measurement For JP For USP For EP * The basic measurement means that the unit is calibrated based on the method decided by RION Co., Ltd. Calibration and Performance-Test for JP, USP and EP will be registered only to the customers who has requested this option. EP has no regulations about Calibration and Performance-Test, so will be applied JP or USP. In the chart, when the quality control method is a basic measurement, the unit is calibrated based on the method decided by RION Co., Ltd. upon shipment. The data used there is the Calibration data KL-04_Basic. The results obtained when confirming that the condition of the unit is appropriate, by applying the Calibration data KL-04_Basic, are the Performance-Test data KL-04_Basic. Also, before a measurement can be done the Performance-Test data must be selected in the measurement parameters. Which calibration data apply to the unit is decided by selecting the Performance-Test data. 2

19 Outline In other words, if the Performance-Test data KL-04_Basic is selected, the Calibration data KL-04_Basic is applied to the unit and the unit is in the calibrated condition based on the method decided by RION Co., Ltd. Important The Performance-Test data complying with the purpose of the quality control test must be selected. An accurate measurement cannot be performed when wrong Performance-Test data are selected. Multiple Performance-Test parameters (condition of test, condition of acceptance or rejection) can be registered to the same Calibration data. This is useful when carrying out the Performance-Test as an inspection before starting any measurement. A formal Performance-Test must be implemented to judge if the condition of the unit is appropriate. However, it is possible to confirm the condition of the unit by setting up a Performance-Test parameter with a name different from the formal Performance-Test, such Calibration as the chart on the right, and implement the Performance-Test when needed, such as at an inspection before commencement. In other words, multiple Performance-Test parameters, such as formal Performance-Test and simple Performance-Test, can be set to the same Calibration Performance-Test Performance-Test 1 Simple Performance-Test data and used appropriately. Measurement parameter Important Performance-Test data obtained with appropriate or equivalent (to a chosen pharmacopeia) Performance-Test parameters must be selected for a measurement. The measurement cannot be carried out properly if the Performance-Test data is obtained with inappropriate Performance-Test parameters. 3

20 Outline Procedure from preparation to measurement The flow chart below shows the general procedure from preparation to measurement. Detailed information on each procedure is described in the page number referenced in the chart. Preparation (Refer to page 9) Start Up (Refer to page 32) When the unit is started for the first time after being shipped from the factory Login (Refer to page 34) Password Registration and Change (Refer to page 38) Operator Registration (Refer to page 40), System Setting (Refer to page 110) When calibration is to be carried out Logout (Refer to page 39) Calibration (Refer to page 77) Do you want to check the performance of the unit before starting a measurement? Yes No Performance-Test (Refer to page 63) Measurements (Refer to page 47) *Password registration and change are carried out by operators after they log-in, if necessary. 4

21 Outline Light Source The life expectancy of a laser diode such as used in the KL-04 is shorter than that of other semiconductor devices. When the laser diode nears the end of its service life, the optical power falls below the rated level. There are considerable differences in service life between individual diodes. Some may fail already after several thousand operation hours. Particle Size Detection The unit is calibrated at the factory, using particles of known diameter and refractive index (monodisperse polystyrene latex (PSL) spheres with a refractive index of 1.6) in pure water. Since the amount of light obscured by a particles is used as reference to determine the particle size, the measured size corresponds to the light-obscuring size of polystyrene latex spheres. 5

22 Controls and Features Front Panel INLET START button FLUSH button Liquid crystal display Locking screw 1 Sample stand Floppy disk drive Tape drive Locking screw 2 START button Press the button to start the measurement. FLUSH button Press the button to start cleaning. Liquid crystal display Shows operation screen. Floppy disk drive To transfer measurement data to other computers on a floppy disk. Tape drive Used to backup / restore measurement data using a tape cartridge. Locking screw 2 Fixes the position of the sample stand. Useful to set a large sample container. Sample stand To hold the sample container at adjustable height. Locking screw 1 Fixes the position of the sample stand. Useful to set a small sample container, such as an ampoule. INLET Sample fluid inlet. Connects to the sampling tube. 6

23 Controls and Features Left Side Panel Valve Tube guide Syringe cover Handle Syringe Syringe cover Clear plastic cover protecting the syringe. The unit will not operate when the cover is open. Tube guide Fixes the drain tube to protect it from being crushed. Valve The INLET opens when drawing in sample fluid and the OUTLET opens when discharging it during draining. Syringe A pump which draws up and discharges sample fluids. Provision for accurate capacity, precision and measurement flow rate is provided through controlling the speed of the plunger in the syringe. The syringe also controls the discharge flow rate of sample fluids. Handle Used when setting the unit. Important When setting the unit, hold the handle tight with one hand and with the other hand hold the cut-out on the opposite side panel. 7

24 Controls and Features Rear Panel POWER switch POWER connector PRINTER connector KEYBOARD connector MOUSE connector LCD switch ETHERNET connector DISPLAY connector POWER switch Turns the power supply ON or OFF. POWER connector Connects to the unit s power supply. PRINTER connector Connects to a printer. KEYBOARD connector Connects to the keyboard provided. LCD switch Turns the backlight of the built-in liquid crystal display ON or OFF. DISPLAY connector Connects to a display. Connects to the built-in display when shipped from factory. ETHERNET connector Connects to a network. MOUSE connector Connects to the mouse provided. 8

25 Preparation Installing the Sample Container Plate Push the sample container plate into the sample stand to secure as per the diagram below. Sample container plate Sample stand 9

26 Preparation Connecting Sampling Tube The PFA sampling tube set provided contains a sampling tube (2 4 dia. length 100 mm) and nut. They need to be connected according to the following procedure. 1. Remove the end plug from the INLET connector by turning the end plug counterclockwise. INLET End plug 2. Loosen the nut of the sampling tube by turning it counterclockwise, and remove the plug from the sampling tube. Nut Plug Sampling tube Plug Nut Sampling tube Important Store the end plug and plug together in a safe place. The end plug will be needed when the unit is sent to the supplier for servicing and maintenance. The plugs will be needed again when removing the sampling tube for storage. 10

27 Preparation 3. Slide the tip of the sampling tube onto the INLET connector and turn the nut clockwise to secure it. INLET Nut Sampling tube SUS sampling tube set (Option) The SUS sampling tube set provided contains a sampling tube (2 3 dia. length 100 mm), nut and packing (total 2 pieces). They need to be connected according to the following procedure. Insert the sampling tube into the nut and insert the packing (1 piece) into the end of the sampling tube. Slide the tip of the sampling tube onto the INLET connector and turn the nut clockwise to secure it. Packing INLET Sampling tube Nut Nut Sampling tube Important Please do not over-tighten the nut. The INLET can be damaged if the nut is over-tightened. Store the end plug in a safe place. The end plug will be required when the unit is shipped to the supplier for service and maintenance. Packing is provided in both the SUS sampling tube set and the drain tube set and each one has a distinctive size. The packing in the sampling tube set is smaller than in the drain tube set. 11

28 Preparation Connecting the Drain Tube The drain tube set provided contains the drain tube (2 3 dia. length 1500 mm) and a packing. They need to be mounted according to the following procedure. 1. Open the syringe-cover and insert the packing in the valve OUTLET. The packing is provided in both the sampling tube set and the drain tube set and each one has a distinctive size. The packing in the drain tube set is larger than in the sampling set. Packing (large) OUTLET Valve 12

29 Preparation 2. Connect the drain tube to the valve OUTLET and lightly fasten the connector to secure it. Connector OUTLET Valve Drain tube Important Please do not over-tighten the connector. The valve can be damaged if the connector is over-tightened. 3. Push the drain tube into the tube guide to secure it. Tube guide Drain tube Valve 13

30 Preparation Connecting the Keyboard and Mouse 1. Connect the keyboard lead provided to the KEYBOARD connector on the rear panel of the unit. KEYBOARD connector Connector Keyboard 2. Connect the mouse lead provided to the MOUSE connector on the rear panel of the unit. MOUSE connector Connector Mouse Important The keyboard and the mouse must be connected before turning on the power of the unit. If the power is turned on before connecting the keyboard and the mouse, problems may occur on the system, for example you may not be able to log in. 14

31 Preparation Connecting Power Cord 1. Turn the power switch to OFF. 2. Insert the connector of the power cord provided to the POWER connector on the unit and insert the plug into the AC outlet. POWER connector Connector AC outlet Plug WARNING To reduce risk of electrical shock, connect the power cord to a grounded AC outlet. Before connecting the power cord ensure that the AC outlet meets the conditions in the specifi cations and has minimum excessive electrical noise or voltage fl uctuation. A malfunction can be caused to the unit if the power supply does not meet the conditions specifi ed. 15

32 Preparation Connecting the Printer (Local Printer) 1. Connect the printer cable to the PRINTER connector on the rear panel of the unit. Only printers supporting Post Script Level 2 and above can be used. Basic set up is completed when the unit is shipped from the factory. Simply connecting to a printer allows printouts to be made. A network printer can also be connected with the unit. However, an enquiry must be made to the system administrator, as the environment will be different depending on the network installed. Refer to Settings for a Printer Connected to the Network on page 116 for basic set-up. PRINTER connector Printer 16

33 Preparation Connecting to a Network (LAN Cable) 1. Connect a LAN cable to the ETHERNET connector on the rear panel of the unit. Make sure the ETHERNET connector correspondents to 10BASE-T. To network ETHERNET connector 17

34 Preparation Connecting the External Display 1. Remove the cable of the built-in display from the DISPLAY connector on the rear panel. DISPLAY connector 2. Connect the cable of the external display to the DISPLAY connector on the rear panel. LCD switch DISPLAY connector 3. Turn the LCD switch OFF on the rear panel. LCD OFF ON 18

35 Preparation Electromagnetic Stirrer (Option) When measuring particles suspended in a fluid, the sample fluid must not be contaminated and particles suspended in the sample fluid must be equally dispersed to obtain a reliable result. The electromagnetic stirrer (option) can equally disperse particles suspended in the sample fluid by turning a stirring bar in the sample fluid using external electromagnetic induction. A remote micro type VARIOMAG HP40107 (Produced by H+P Labortechnik) is used as an electromagnetic stirrer. Controls and features Electromagnetic stirrer Power cord Volume dial Controller Plug Control cable Control cable connector Electromagnetic stirrer Installed in the sample stand of the KL-04. Control cable The plug connects to the control cable connector on the controller with. Controller Turns the power supply ON or OFF and adjusts the revolution speed of the stirring bar by rotating the volume dial. Volume dial Turns the power supply ON or OFF and adjusts the turning frequency of the stirring bar. Turn the volume dial to the right for a higher revolution speed of the stirring bar. Turn the volume dial all the way to the left to cut the power supply off. Control cable connector Connects to the control cable plug of the electromagnetic stirrer. Power cord Connects to the AC outlet. 19

36 Preparation How to install 1. Put the control cable downward through the hole of the sample stand and set the electromagnetic stirrer in the sample stand. 2. Push the sample container plate down on the sample stand to secure it. 20

37 Preparation 3. Connect the control cable plug of the electromagnetic stirrer to the control cable connector of the controller. Controller Control cable Plug Control cable connector Caution The controller must not come into contact with any fl uid. If the controller is in contact with fl uid, an electric shock as well as malfunction of the unit can occur. 21

38 Preparation How to use 1. Ensure that the volume dial on the controller is turned OFF. Completely turn the volume dial to the left until it stops as per the diagram on the right. 2. Connect the power cord to the AC outlet. 3. Put a stirring bar into the sample container and set the sample container on the sample stand. off speed Caution The sample container must be set on the sample stand after ensuring the volume dial on the controller is OFF. If the sample container is set when the volume dial is ON, the stirring bar may jump around, which can cause splashing of the fl uid and damage to the sample container. Also the level of fl uid in the sample container must be controlled to prevent it from overfl owing when the stirring bar is revolving at high speed. The standard level of sample fl uid is 80% of the displayed capacity of the sample container. The surface material of the provided stirring bar is glass. Some sample fluids can cause corrosion, dissolving and other chemical reactions to the stirring bar. Ingredients of sample fl uids must be checked before they are put in the sample container. If the stirring bar is not cleaned adequately contamination of sample fl uids and chemical reactions can occur. The cleanness of the stirring bar must be ensured before putting into the sample container. 22

39 Preparation The correct sample container size appropriate to the volume of the sample fluid must be used. A container with less internal diameter and a flat bottom is preferred. A container with less internal diameter is more efficient in agitation, when the capacity is the same. 4. Turn the volume dial to the right to start the stirring bar revolving. Turn the volume dial to OFF to cut the power supply of the controller and stop the stirring bar revolving. speed off Important When revolving a stirring bar at high speed, bubbles can form in the sample fl uid, which can affect measurement results. Also, if the magnetic coupling between the electromagnetic stirrer and the stirring bar is not strong or fails, the stirring bar will not revolve properly. The revolution speed must be adjusted according to the condition of the stirring bar and the sample fl uid. The stirring bar is magnetic. The unit is also magnetic when the power is ON. Objects which can be affected by magnetism, such as fl oppy disks and watches, must be kept away from the stirring bar and the unit. When revolving the stirring bar at low speed, at first the speed must be set slightly higher to stabilise the revolution and then changed back to the lower speed. 23

40 Window Operation Virtual Desktop Virtual Desktop The unit contains multiple virtual screens but only one of them appears on the actual display, as per the diagram on the right. When displaying multiple windows on a screen, the windows overlap each another and it may become confusing to use. It is convenient to divide and arrange the windows on separate screens. The Virtual Desktop controls how windows are arranged on the screen and which screen appears on the display. Display How to move windows The Virtual Desktop shows which window is open. Drag the relevant window to the screen to which you want to move it. 24

41 Window Operation How to select a screen appearing on a display A screen appearing on a display can be selected by the following three methods. Drag the frame on the Virtual Desktop up to the screen you want to display. Double-click the screen on the Virtual Desktop you want to display. The OLVWM 4.1 window will appear by clicking the right button on the Virtual Desktop (where the window is not displayed). Click the arrow or the home ( ) button. (The left button click is described as click in this instruction manual.) The screen will be moved in the direction of the clicked arrow based on the screen displayed. The left top screen will appear by clicking the home button. How to change the number of screens in the Virtual Desktop The number of screens in the Virtual Desktop can be changed by putting the cursor on the corner of the Virtual Desktop and dragging it to increase or decrease the number of screens. 25

42 Window Operation Window Menu The window menu can be displayed by clicking the left or right button on the window menu button ( ), which is on the header of window. The window menu displays the window s possible operations. The window menu can also be displayed by clicking with the right mouse button on the header or the frame of window. Right-click on the frames of windows without a header. The window menu contains the following commands. (example) Close: Displays the window as an icon. Full Size: Maximizes the window size. Move: Moves the window by dragging to the new position you want. Resize: Enlarges or reduces the window size by dragging it to the position you want. Back: Takes the focus away from the current window and moves the window to the back. Refresh: Refreshes the display of the window if it crashes. Stick: Freezes the display of the window when the virtual screen is switched over on the Virtual Desktop. Quit: Closes the window. 26

43 Window Operation Pop-up Window The base window opens when you log on. Sometimes the pop-up window opens as well as the base window, depending on the user s operation or the operational condition of the unit. The pop-up window is dependent on the base window. Therefore, if the base window is closed when the pop-up window is open, the pop-up window will also be closed. The pop-up window contains the following commands. (example) Dismiss: Closes the pop-up window. Move: Moves the window by dragging it to the position you want. Resize: Enlarges or reduces the window size by dragging to the position you want. Back: Takes the focus away from the current window and moves the window to the back. Refresh: Refreshes the display of the window if it crashes. Owner?: Returns to the base window. 27

44 Window Operation Changing the Overlap Order of the Windows As windows can overlap each other it is usual that a part or the whole of a window will be hidden by other windows. When part of window is hidden by another window, click on the header or the frame of that window. The hidden window moves to the front and the whole window appears. Also, the window hiding the other window can be moved to the back to display the hidden part by selecting Back on the window menu. Most windows can overlap in any order. However, some of the pop-up windows displayed by certain operations on a window will not be hidden by the other windows. In this case, the pop-up window needs to be closed or the other windows need to be moved. Moving a Window A window can be moved by dragging its header or frame to the desired place by holding down the left mouse button, and then releasing it. 28

45 Window Operation Changing the Window Size The size of window can be changed by dragging its resize corners (the L-shaped marks on the corner) to the size you want by holding down the left mouse button and then releasing it. If a window does not have resize corners, the size of the window cannot be changed. Also, some of the window sizes cannot be changed even though it has resize corners. Selecting Window A window can be selected by clicking the left mouse button on the header or the frame. The window in this condition is called the active window. Only the active window can receive input data from the keyboard. The header of the active window appears as below. 29

46 Window Operation Closing Windows Quitting window If the window has buttons such as Quit and Dismiss, the window can be closed by clicking these buttons. If the window does not have these buttons, selecting Quit from the window menu can close the window. Some windows open a pop-up window when closing and require confirmation. The quitting operation on windows can be refused by the unit depending on its operational condition. In this case, appropriate steps must be taken after confirming the operational condition. Displaying a window as an icon A window can be displayed as an icon by selecting Close on the window menu. Also, the icon can be displayed as a window by opening the window menu of the icon and selecting Open. The window displayed as an icon maintains its operational condition. When the window is not needed, it has to be completely closed (refer to the quitting window section). 30

47 Window Operation Quitting pop-up windows Most of the pop-up windows of the KL-04 have a Dismiss button on the bottom and the pop-up window can be closed by clicking the button. Some windows have a Cancel button instead of a Dismiss button, which has almost the same function. Some pop-up windows have only a button with a label such as OK. If so, the pop-up window can be closed by clicking the button. If the pop-up window does not have any buttons to close it, click the right button on the header or the frame to open another pop-up window and then select Dismiss to close the window. If the pop-up window is fixed by a push-pin, click on the push-pin to release it and then click on the released push-pin to close the pop-up window. Push-pin (when fi xed) Push-pin (when released) 31

48 Start Up Power ON 1. Turn the POWER switch at the back of the unit ON. The Start Up screen appears, scrolling across the front crystal display. After a while, the LOGIN screen appears. Session menu: This menu is used for maintenance. Login by selecting Failsafe from the menu, which starts the unit in maintenance mode. In general, it is set to Default login from the moment the power is turned on. If you have logged in using Failsafe mode, restart (i.e., turn the power switch OFF, and then ON again) without touching anything else. Resetting the unit will enable the Session selection to return to Default even if you have logged on in Failsafe mode previously. 32

49 Start Up Language Menu: Immediately after registering a new operator, English is set by default as the display language. This menu can be used by any operator to change the display languages. Click to bring up the submenu, then select the appropriate language category, and then click on the required display language. When the display language is changed, a message appears to ask whether the selected language is to be set as default. Click the Yes button to set the selected language from the Language menu as the default language. Click the No button to set the selected language only until the end of the current session, after which the display will automatically return to the previous language. The following notes assume English has been selected from the Language menu. 33

50 Start Up Login Either double-click an Operator icon on the Login screen or type your login name into the Login space, then press the [Return] key. If a password is set, the Login space changes to the Password space. Type in your password, then press the [Return] key. If the screen display returns to the Login screen by showing messages such as Authentication failed, the Login name or the password were entered wrong. Please re-enter the Login name and the password. After the Firmware version number is displayed on the screen, Virtual Desktop, the KL-04 Controller window and the KL-04 - Measurement window appear. Virtual Desktop KL-04 Controller window KL-04 - Measurement window Virtual Desktop : This refers to the interrelationship between this unit s several virtual screens and the screens shown on the display. Please see page 24 for further details. KL-04 Controller window: The current operator s login name, the current time, syringe operating status etc., will be displayed. KL-04 - Measurement window: This window is for measurements. Please refer to Measurements from page 47 onwards for further details. 34

51 Start Up Workspace Menu Click the right mouse button on the display background (where no window is displayed) to show the Workspace menu. The Workspace menu is used to show the KL-04 - Start New Window window or Find Window on the front of the display hidden by overlapping. Start New Window... window: Click to display KL-04 - Start New Window window. Please read the following page 36 for KL-04 - Start New Window. Find Window : Click to show the description list of all currently opened windows. Click on the required title from the list to show it on the front of the display. 35

52 Start Up KL-04 - Start New Window The unit shows a window for the functional settings and commands executed by each button on the KL-04 - Start New Window window. The operation of the unit can be done in this window. Display method The KL-04 - Start New Window window display can be made available by any of the following methods. - On the KL-04 Controller window, click either of mouse buttons to select a Start New Window from the displayed menu. - Press the Show button on the KL-04 - Measurement window etc., then select a Start New Window from the displayed menu. - Select Start New Window from the Workspace, which can be opened by clicking the right mouse button on the areas in which windows are not open. Function Click each button on the KL-04 - Start New Window window to open the following windows. The reference pages indicate functional details and relevant information. Usual Operations: Measurement button: The KL-04 - Measurement window appears. Click when measurement is shall be done. See page 48. Performance Test button: The KL-04 - Performance Test window appears. Click when a Performance-Test is shall be done. See page 63. Calibration button: The KL-04 - Calibration window appears. Click when calibration is shall be done. See page 78. Check Noise Level button: The KL-04 - Check Noise Level window appears. Click when the noise level shall be measured. See page

53 Start Up View/Set Operation Parameters: Measurement Parameter button: The KL-04 - Measurement Parameter window appears. Click to check the measurement parameters or change the settings. See page 53. Performance-Test Parameter button: The KL-04 - Performance-Test Parameter window appears. Click to check the Performance-Test parameters or change the settings. See page 67. Calibration Parameter button: The KL-04 - Calibration Parameter window appears. Click to check the Calibration, Performance-Test parameters or change the settings. See page 85. Management Tasks: Backup/Restore button: The KL-04 - Backup/Restore window appears. Click when data backup or restoration shall be done. See page 108. Operator Management button: The KL-04 - Operator Management window appears. Click to add operator(s) or modify operator registration details. See page 41. Set Clock button: The KL-04 - Set Clock window appears. Click to set the clock. See page 112. System Administration button: The Administration Tasks window appears. Click for network and printer settings. See page 113. Audit Trail button: The KL-04 - Audit Trail window appears. Operators who have the required access privileges can view the audit trail. See page 127. Miscellaneous: Change Password button: The Input pop-up window appears. Click to set or change the password of the Operator who is logged-in. See page 38. System Information button: The System Information pop-up window appears. Click to check the computer s system information. On the System Information popup window are the main computer s Firmware versions, production numbers etc. Unsupported: Virtual Keyboard button: Virtual Keyboard xvkbd - Virtual keyboard appears. Click when using a virtual keyboard. See page 119. Screen Snapshot button: The TkSnapshot (Version 0.31) window appears. Click to file displayed screen images. See page

54 Start Up Change Displayed Language Click the display language button to the right of Language to show a list and select the appropriate language from the list (English, Japanese, German). Each right-click changes the displayed language. After selection of a language, each window will be displayed with its selected language when opened. The setting here is a temporary one. Once logged out, the setting returns to default. To change the default setting, use the Language menu on the login screen. Please refer to Power ON page 32 for the setting. Password Registration and Change To register or change a password, follow the sequence below. 1. Display the KL-04 - Start New Window window. 2. Click the Change Password button in the Miscellaneous menu on the KL-04 - Start New Window window. The Input pop-up window appears. 3. Type in the current password, then press the OK button. The Input pop-up window reappears. When a password is not set, there is no step No. 3. When the password is typed wrongly, the Error pop-up window appears. Click the OK button to close the window, then start the sequence from No. 1 again. 38

55 Start Up 4. Type a new password then press the OK button. The Input pop-up window reappears. Enter between 6 to 22 letters / figures. When a password other than specified or a simple password (i.e., repetition of the same letter) are inserted, the Error pop-up window appears. Click the OK button to close the window and repeat the sequence from No Enter a new password then press the OK button. When a wrong password is entered, an Error pop-up window appears. Click the OK button to close the window and repeat the sequence from No. 4. Completion (Logout) Method 1. Click the Logout button on the KL-04 Controller window. A logout confirmation pop-up window appears. Click the Logout button on the window to return to the Login screen. 2. Turn the system s POWER switch OFF. It is at the rear of the unit. On the display, a logoff screen will move across the screen. After a while, the screen display will disappear and the power will be turned OFF automatically. Important Please be sure not to unplug the power cable prior to the main unit being turned fully OFF. If it is unplugged in too early, damage may occur. 39

56 Operator Management Operator Besides setting measurement parameters and carrying out steps for measurement, the KL-04 also allows a number of administrative tasks, such as performing calibration, checking and ensuring continued performance test compliance, performing data backup, setting the clock, etc. For these tasks, the unit provides an operator management facility that makes it possible to specify access privileges for individual operators (e.g. Measurement is available, but other Management Tasks are not permitted). Authorization of one operator to carry out all management tasks is of course also possible. that the steps for regular measurement can be carried out by all registered operators. Measurement is therefore not included in the list of tasks for which access privileges can be set (see page 45). Operator Registration No Operator icon is registered on the login screen when the unit is dispatched at the factory. Register, an Operator using the following sequences, to set up other operator s registration and access authorization. 1. Input the login name provided by RION in the Login space on the login window. The Login space display will change to a Password space. 2. Input the password provided by RION to the Password space then press [Return] key to login. 3. Display the KL-04 - Start New Window window. See page 36 for the KL-04 - Start New Window window display methods. 4. Click the Operator Management button from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Operator Management window appears. 40

57 Operator Management 5. Click the operator name shown to the right of Operator, then click Add New Operator from the displayed Operators list. Right-click on the operator name to change the display. 6. Type a login ID of not more than 8 letters / figures into the Login name space. 7. If required, input a Full name in up to a maximum of 30 letters / figures. If this is not entered, an assumed Login name will be set. 8. Check the left hand side of the Operator Management from Permitted Management Tasks. For other task items, check when required then set access authorization accordingly. See page 45 for the task item details. 9. Click the Set button. 10. Click the Quit button. The login name and the password provided by RION are common to all KL-04 products. We recommend that you change the password and the login name provided by RION after registering an operator who has the Operator Management access authorization. This is to avoid a login by a third party. See page 38 for the Password Registration and Change. 41

58 Operator Management Add Operator 1. An operator with access privileges to Operator Management must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Operator Management from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Operator Management window appears. 3. Click an operator name shown to the right of Operator. An Operators list will be displayed. Click Add New Operator from the list. Right-click on the operator name to change the display. 4. Enter a login ID with no more than 8 letters / figures into the Login name space. 5. If required, input Full name in no more than 30 letters / figures. If this is not entered, an assumed Login name will be set. 6. If required, check each task item of the Permitted Management Tasks then set the access authorization accordingly. See page 45 for task item details. 7. Click the Set button. 8. Click the Quit button. 42

59 Operator Management Change of Operator Registration Details 1. An operator with access authority for Operator Management must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click on Operator Management from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Operator Management window appears. 3. Click an operator name shown to the right of Operator. An Operators list appears. Select an operator name from the list to change the registered details. Right-click on the operator name to change the display. 4. If necessary, check each task item on the Permitted Management Tasks, then set the required access authorization. See the KL-04 - Operator Management window shown on the following page 45 for task item details. 5. Click the Set button. 6. Click the Quit button. 43

60 Operator Management KL-04 - Operator Management Window The each item description on the KL-04 - Operator Management window is as follows: Operator: Select an operator (displayed with Login name + Full name ) in order to display the setting details on the KL-04 - Operator Management window. The operator name will be displayed on the result screens of the Calibration, Performance-Test or Measurement, or on their printouts. Login name: The operator s Login name is displayed. Full name: The operator s Full name is displayed. When an operator authorized for Management Tasks is logged in, change is permitted within 30 letters / figures. The Full name together with the Login name will be displayed on the result screens of Calibration, Performance-Test or Measurement and the printouts. The Login name is short with less than 8 letters / figures. The Full name entry will enable the easy identification of individual operators. Password: Select the appropriate item(s) from the list shown by clicking on the items displayed on the right hand side. This feature is only accessible to authorized operators with access to Change Other Operator s Password. Right-click on the item names to change the displayed item. Preserve: Select this when no password change is required. Clear: Select this to clear the password, for incidents such as forgetting your password. Disable Login: Select this to forbid logins for specified operators etc. 44

61 Operator Management Permitted Management Tasks The level of authorization to undertake Management Tasks for each individual operator may be set. When setting the access rights (authorization), put check marks in the check boxes. Performance Test: Permit Performance-Test tasks Calibration: Permit Calibration tasks Set Measurement Parameter: Permit the Measurement Parameter setting tasks. Set Performance-Test Parameter: Permit the Performance-Test Parameter setting tasks. Set Calibration Parameter: Permit the Calibration Parameter setting tasks. Modify Measurement Description: Permit making entries in the measurement data modification columns (Sample, No., Memo). Delete Measurement Data: Permit measurement data deletion steps. Backup/Restore: Permit data backup stored on the hard disk and the restore tasks. The built-in tape drive is used for data backup. Operator Management: To permit registration of other operators and set access authorization. 45

62 Operator Management Change Other Operator s Password: Other operator s passwords can be deleted, or they can be prevented from logging in. If Operator Management is permitted, this is accessible. Set Clock: Permit authorization for the setting of the system clock. System Administration: This will permit network setting and printer setting tasks. Audit Trail: Permit viewing of audit trail. Because the steps for regular measurement can be carried out by all registered operators, there is no check box for measurement. 46

63 Measurements Basic Operations The following are this unit s operation samples. START Number of Pre-Measurements : 1 Pre-Suction Pre- Measurement Measurement 1 Measurement 2 Measurement 3 Drain Tare Volume : 2 ml Number of Measurements : 3 Measurement Volume : 5 ml Measuring Operation Drain After Every Measurement? : No When Drain After Every Measurement? is not set, and the combined total of Pre-Suction (i.e., Tare) Volume and total measured volume (total of the measured volume per single measurement Pre-measurement plus the measurement) is smaller than the syringe capacity, the system continues to measure until the syringe capacity is reached, then drains the sample after all measurements are completed. If the combined total volume exceeds the syringe capacity, the system continues up to the measurable number within the syringe capacity level, drains the sample then measures the remainder. On the other hand, when drain after every measurement is set, the sample is drained after each measurement. In the following sample operation example, the total of Pre-Suction Volume (2 ml) plus the total measurement volume (5 ml 4 times = 20 ml) is smaller than the syringe volume (25 ml, Standard product). Pre-Suction, Pre-Measurement and three Measurements can therefore be carried out during in one measuring operation, after which the sample must be drained. After this, the measurement operation is finished. The following operations are carried out for Pre-Suction, Measurement and Drain. Pre-Suction: To flush a sample in the particle sensor or stabilize the flow rate, a number of samples must be purged through to the particle sensor. No particle measurement is done. Pre-Measurement: The particle measurement is done and the result is displayed but is not used for calculation of the average. Measurement: Particle measuring status. Drain: To drain the aspired sample. 47

64 Measurements Measuring Sequence It is necessary to set the Measurement Parameter prior to the actual Measurement. See page 53 for the Measurement Parameter Setting. The following is an example of a measuring sequence. 1. Display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Measurement button from the Usual Operations menu on the KL-04 - Start New Window window. The KL-04 - Measurement window appears. When the KL-04 - Measurement window is displayed immediately after the login, no KL-04 - Measurement window needs to be displayed again. 3. Click the Measurement Parameter name shown to the right of Measurement on the KL-04 - Measurement window. A Measurement Modes list will be displayed. Click the required Measurement Parameter name from the list. 48

65 Measurements 4. Press the Show button on the KL-04 - Measurement window. Select Measurement Parameter from the displayed menu. The KL-04 - Measurement Parameter window appears. Check the contents. After checking, press the Quit button to close the KL-04 - Measurement Parameter window. 5. Set out a sample to clean (normally purified water). 6. Clean by either clicking the Flush button or pressing the FLUSH button on the front of the unit. Important When operating by pressing the FLUSH and START buttons on the unit, ensure that the KL-04 - Measurement window is set in an active window in which the required Measurement Parameter name is displayed. If it is not in an active window, operations may be different from the specifi ed Parameter. 7. Carry out a Blank Measurement. To do this, measure either by clicking the Start button on the display or pressing the START button on the front of the unit. 8. If the Blank Measurement exceeds the target value, return to step 6. If it is less than the target value, set out a measuring sample. 9. Measure the sample. For this, either click the Start button or press the START button on the front of the unit. The measuring operation starts. During this operation, a window indicating the measuring status is displayed. When the measurement is completed, the measurement result will be displayed on the KL-04 - Measurement window. 10. If required, enter a sample name in the Sample space, the sample number in the No. space, and memos in the Memo space. Sample names, sample numbers and Memos can be written-in to the displayed Measurement (accessible during the Measuring operation). The sample number will be incremented for each Measurement startup when the Clear No. Field at Measurement Start? is not checked on the Measurement Parameter and figures are entered. The Memo spaces will be cleared on each Measuring startup. The Measured Data will be stored to the hard disk every time. 49

66 Measurements The Measurement Result Pre-Measurement Result 1st Measurement Result 2nd Measurement Result 3rd Measurement Result Approval / Rejection judgement Average Measurement Parameter name Channel Bar graph display of the result Management Information Pre-Measurement Result Click the Show button to display the menu and then click Show Pre-Measurement Data? from the menu to display it. Bar graph display of the result Click the Show button to display the menu and then click Show Bar Graph? from the menu to display the pre-measurement data. Differential value(s) from the measured result Click the Show button to display the menu and then click Show Differential Value? from the menu to display it. Management Information Click the Show button to display the menu and then click Show Management Information? from the menu to display it. If measurement data annotation information (Sample, No., Memo) has been changed, the history will also be displayed. 50

67 Measurements To Display Previously Measured Data Follow the sequence below to show the previously measured data. Immediately after the measurement, the latest Measurement Data appears. 1. Press the Show button on the KL-04 - Measurement window to show the menu. Select List of Data from the menu. The Measurement - Data Selector window appears. 2. Select required measured data year and month from the Year & Month list and the date from the Date list. The selected Measurement Data appears on the KL-04 - Measurement window. The time shown for a measurement data file name is the time when measurement that resulted in these data was started. The operators who have the privileges about measurement data modification can edit the measurement data displayed on the KL-04 - measurement window (see page 45). 51

68 Measurements Measurement - Data Selector window The explanation of each item on the Measurement - Data Selector window is as follows; Operator: When a measured result by each operation is required, check the box. With this, the operator name shown on the right hand side becomes effective. Select an operator name from the Operations list which can be displayed by clicking the operator name. Year & Month List: Select the measuring year and month for the Measurement Data. Date List: Select the measuring date for the Measurement Data. Measurement Data List: Select the Measurement Data to display. Delete Data button: Delete the selected Measurement Data. Deletion of the Measurement Data may only be performed by the permitted operator (see page 45). When data is to be deleted, use a Measurement Data list. Several items of data can be selected for deletion at one go by holding down the [Shift] key when clicking on each item, or moving the pointer while holding down the mouse button. Print button: Print the selected Measurement Data. Floppy button: This enables storage of selected Measurement Data on a floppy disk as a TSV (Tab Separated Values) format file. See page 104, Export the measured data for storing method. 52

69 Measurements Measurement Parameter Setting 1. An operator with access privileges to Set Measurement Parameter must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click on Measurement Parameter from View/Set Operating Parameters menu on the KL-04 - Start New Window window. The KL-04 - Measurement Parameter window appears. 3. Click a Measurement Parameter name shown to the right of Measurement to show the Measurement Modes list. Click on Add New Setting from the list. Important The #1 of the Measurement Parameter names has been registered by RION at dispatch from our factory and is used for our inspection. Please do not change the parameter setting. Right-click on the Measurement Parameter names to change the display. Click the Measurement Parameter name to be copied from the Measurement Modes list. Then click on Add New Setting to copy the Parameter. 53

70 Measurements 4. Enter the Measurement Parameter name in the space below Measurement. 5. If required, enter figures or checks in the Measurement Parameter space. See page 56, Measurement Parameter for the explanations of each Measurement Parameter. 6. Click the Register button. 7. When a separate Measurement Parameter is to be set, repeat steps from No. 3 to 6. When the Measurement Parameter Registration is completed, click the Quit button. 54

71 Measurements Change Measurement Parameters Important The #1 of the Measurement Parameter names has been registered by RION at the time of dispatch from the factory and is used for our inspection. Please do not change this parameter setting. 1. An operator with access privileges to Set Measurement Parameters must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Measurement Parameter button from View/Set Operating Parameters menu on the KL-04 - Start New Window window. The KL-04 - Measurement Parameter window appears. 3. Click the Measurement Parameter name shown to the right of Measurement, then click on appropriate Measurement Parameter name(s) from the displayed Measurement Modes list. Right-click on the Measurement Parameter names to change the display. 4. See steps 5 and 6 of Measurement Parameter Setting, above for the method for changing each item. 5. When the changes to the Measurement Parameters are complete, click the Quit button. Click the Register button to increment the revision number. 55

72 Measurements Measurement Parameters See the KL-04 - Measurement Parameter window for the Measurement Parameter. The explanation of each parameter is as follows; Syringe Syringe Volume (ml): This is to set the volume of the syringe which is installed on this unit. The allowable setting range is 5 to 25 ml (1 ml step). The standard syringe volume is 25 ml. Important Please make sure to enter the correct volume of the syringe which is installed on this unit. If set differently, a correct measurement is not be possible. Measurement 56

73 Measurements Aspiration Flow Rate (ml/min): This refers to the syringe suction velocity. This is to set the sample flow rate of the sensor. The standard products are set to 25 ml / min (10 ml / min : Factory option). The allowable setting range is 5 to 100 ml / min (1 ml / min step). Important The aspiration fl ow rate set here must be the same as the aspiration fl ow rate for the Performance Test Data (see page 64) selected by the same parameter setting. If the setting is different, an error message will appear and measurement cannot be carried out (see page 143). Drain Flow Rate (ml/min): This refers to the syringe drain velocity. Set it taking the sample viscosity etc., into consideration. The allowable setting range is 1 to 100 ml / min (1 ml / min step). Tare Volume (ml): To purge the last sample or to stabilize the flow rate, normally set a slightly higher volume than the dead volume (approx. 0.3 ml) inside the sampling tube between the sample and the sensor. In some cases, when the sample in the a sampling tube is changed from stationary to suction condition, particles previously stuck on the walls inside the flow channel will come off and the particle number concentration in the sample may subsequently rise. Take this into consideration when setting the tare volume. The allowable setting range is 0.1 to 10.0 ml (0.1 ml step). The setting value of tare volume is constantly added 0.2 ml, so actual tare volume range is 0.3 (dead volume) to 10.2 ml. Measurement Volume (ml): This sets the volume in which particles are counted. The allowable setting range is [(0.2 ml up to Syringe volume) (Tare Volume ml)] (0.1 ml step). For a standard 25 ml syringe, it will be 0.2 to 24.7 ml. 57

74 Measurements Number of Pre-Measurements (times): Set the number of Pre-Measurements to be carried out prior to the actual Measurement. Usually a Blank Measurement (Blank Check) is carried out after the cleaning prior to a measurement. This enables the inside of the flow channel to become fully clean. However, since the measuring samples are not necessarily in the same condition throughout, it is therefore necessary to set the constant number concentration distribution level inside the flow channel. The Pre-Measurement is, therefore, designed for this purpose. The suction volume etc., will be the same as the one for the Measurement, but the measured results will not be included in the calculation of the average. The allowable setting range is 0 to 10 times. The Blank Measurement is a preliminary measurement in order to check sample(s) and the flow channel condition in situations such as immediately after purging, or when purging a former sample. Number of Measurements (times): This allows setting the Number of Measurements. The allowable setting range is 1 to 100. Drain After Every Measurement?: This is to drain the sample in the syringe after every measurement. Calculate Particles per Unit Volume?: Convert the measured particle numbers to particle number concentration (particle numbers per unit volume). The converted result is only displayed in the Average. The Unit Volume (ml): This is only valid when Calculate Particles per Unit Volume? is checked. This is to set the Unit Volume which allows calculation of the particle number concentration. The allowable setting range is 0.2 to ml (0.1 ml step). When the Unit Volume is not set, the average value for the particles will be related to the measurement unit volume. 58

75 Measurements Dilution Ratio: This is only accessible when Calculate Particles per Unit Volume? is checked. When a sample is measured after dilution for reasons of high number concentration or viscosity, the dilution ratio has to be set. Set the dilution ratio for the sample being actually measured. With that dilution ratio, convert it to the undiluted particle number concentration, then convert it again to the actual volume. The converted result is reflected only in the display of the average. The allowable setting range is 1.0 to (0.1 times step). Clear No. Field at Measurement Start?: Clear the numeric value in the KL-04 - Measurement window at the measurement starting. When this item is not checked, the number (when entered) in the No. filed on the KL-04 - Measurement window increases by one for each new measurement start up. Flush Aspiration Flow Rate (ml/min): This sets the suction velocity of the syringe during cleaning. The allowable setting range is 5 to 100 ml / min (1 ml step). Drain Flow Rate (ml/min): This sets the syringe s drain velocity while cleaning. The allowable setting range is 1 to 100 ml / min (1 ml step). Flush Volume (ml): This sets the suction volume of the syringe to suck each time during cleaning. The allowable setting range is between 0.2 to 25.0 ml (0.1 ml step). Repeat (times): This sets the number of repetitions. The allowable range is between 1 to 100 times. 59

76 Measurements Performance-Test Data Performance-Test Date List: The registered Performance-Test data name list will be displayed. Select the appropriate Performance-Test data to carry out a measurement. Please note that incorrect data selection will not enable you to carry out a correct measurement. The following data are registered at upon shipment of this unit. KL-04_Basic: For use of general measurement JPxx: For measurement in accordance with the Japanese Pharmacopeia (JP) Standards. (Registered only for those who have ordered Option(s)) USPxx: For measurement in accordance with the United States Pharmacopeia (USP) Standards. (Registered only for those who have ordered Option(s)) EPxx: For measurement in accordance with the European Pharmacopeia (EP) Standards. (Registered only for those who have ordered Option(s)) * xx indicates each pharmacopeia s revision number (JP and USP) or version number (EP). View button: This enables checking the selected Performance-Test data. Select the required Performance-Test data name from the list then click this button. The KL-04 - Performance-Test window appears. Effective Period: This sets the validity period for the use of the Performance-Test data. The allowable setting range is between 1 to 9,999 days. Important If the effective period for the set Performance-Test data has expired, an error occurs during the measurement which disables the measurement. 60

77 Measurements Channels Channels List: The set Particle size range will be listed. Add button: This is to add a particle size channel. The allowable channel number is up to 20. Click to show the Add New Channel window. Diameter (µm): This is to add a particle size channel. Set it with the unit s permitted size range of countable particles from 1.3 to 100 µm (0.1 µm step). Set Upper Limit?: This is to set the permitted upper threshold of particle number. Upper Limit (particles): Check to enable the setting of the Set Upper Limit?. The particle counts set here become the acceptance / rejection judgement criteria for the measured data. The judged result will be displayed on the acceptance / rejection result space on the KL-04 - Measurement Data window. Set button: Click this after setting the particle size. The Add New Channel window closes and the added particle size appears on the Channels list. 61

78 Measurements Edit button: Use this to change the particle size or upper limit setting. Select a required particle size channel from the Channels list to edit. Click to display the Edit Channel Setting window. The Edit Channel Setting window setting is the same as the setting on the Add New Channel window. See the previous Add New Channel window for further details of the setting. Delete button: Use this to delete a particle size channel for the test particles. Select the required a particle size channel from the Channels list. Click the group to delete. 62

79 Performance-Test The Performance Test serves to verify if the performance requirements of a given pharmacopeia (particle size resolution etc.) are met by the calibration data of the system. The pharmacopeia defines the requirements both for calibration and testing. If the calibration method is different, the Performance Test content will also differ. A proper Performance-Test should be carried out using a Performance-Test Parameter in order to verify whether the system is operating according to the respective. However, if a simple system check is sufficient, other Performance-Test Parameters can be set in addition to the specified Performance-Test, in order to separate several Performance-Tests. At the time of shipment, the Performance-Test Data is registered with the confirmation of the calibrated result on the unit as satisfactory after carrying out a maximum of four(4) types of Performance-Test, including an Option. Please carry out the Performance-Test regularly in order to check if the system works correctly. The Performance-Test Parameters such as JPxx registered at the time of shipment (only for those who have ordered this option) are in accordance with every Pharmacopeia. When a simple Performance-Test is required, copy the Performance-Test Parameter registered at the time of shipment, then register it is a new Performance-Test Parameter. Performance-Test Sequence The Performance-Test Parameters must be set prior to the Performance-Test. See page 67 onwards for Performance-Test Parameter Setting. The Performance-Test sequence is as follows; 1. An operator with access privileges to Performance Test must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 63

80 Performance-Test 2. Click the Performance Test button from the Usual Operations menu on the KL-04 - Start New Window window. The KL-04 - Performance Test window appears. 3. Click the required Parameter name as shown at the right of Performance Test. A Performance Test Modes list appears. Click a Parameter name to select it from the list. 4. Press the Show button on the KL-04 - Performance Test window. Select the required Performance-Test Parameter name from the displayed menu. The KL-04 - Performance-Test Parameter window appears. Please check the settings. After checking, press the Quit button to close the KL-04 - Performance-Test Parameter window. 5. Select a Performance Test from the displayed list, which can be obtained by clicking on the operation items (Performance-Test data display) shown at the right of Operation. The window display will change to the one for the Performance- Test. 64

81 Performance-Test 6. Set a sample (in general purified water) for cleaning purposes, then click the Flush button on the display or press the FLUSH button on the front of the unit. Important When operating by pressing the FLUSH and START buttons on the unit, ensure that the KL-04 - Performance Test window is set in an active window in which the required Performance-Test Parameter Name is displayed. If it is not in an active window, the operations may be different from the specifi ed Parameter. 7. Carry out the Performance-Test. Prepare the sample(s) then click a button for the required test item (e.g µm) shown on the list. After the test is completed, the test results will be displayed to the right of the items. The test result will be displayed in black if accepted by the system, and in red if rejected. 8. If more test items are required, repeat the sequence from No. 6 to 7 for the number of test items only. After all test items are completed, click the Register button to register the test result. The Registration is not available for rejected test results. 9. Click the Quit button upon completion of the test. The Performance-Test series should be fully completed within 72 hours. If this time limit is exceeded, the test result becomes void. 65

82 Performance-Test The Performance-Test Result Performance-Test Parameter Calibration Data Approval / Rejection Judgement Management Information Management Information Click the Show button to display the menu and then click Show Management Information? from the menu to display it. 66

83 Performance-Test Performance-Test Parameter Setting 1. An operator with access privileges to Set Performance-Test Parameter must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Performance-Test Parameter button from the View/Set Operation Parameters menu on the KL-04 - Start New Window window. The KL-04 - Performance-Test Parameter window appears. 3. Click the Performance-Test Parameter name shown to the right of Performance-Test, then click Add New Setting on the displayed Performance-Test Modes list. Right-click on the Performance-Test Parameter name to change the display. Already registered Parameters can be used by copying them in the following sequence. First, select the Performance-Test Parameter name from the Performance-Test Modes list. Then click Add New Setting to copy the Parameter. 67

84 Performance-Test 4. Input the Performance-Test Parameter name in a space under Performance-Test. 5. If required, input figures or checks in the Performance-Test Parameter. See next page, Performance-Test Parameters for the definition of each Performance-Test Parameter. 6. Click the Register button. 7. Repeat No. 3 to 6 of the sequence for a different Performance-Test Parameter Register. Click the Quit button when the Performance-Test Parameter Register is completed. Changing the Performance-Test Parameters The Performance-Test Parameter name is used for our service inspection purposes and registered at the time of shipment. Please do not change these Parameter setting. 1. An operator with access privileges to Set Performance-Test Parameter must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Performance-Test Parameter button from the View/Set Operation Parameters menu on the KL-04 - Start New Window window. The KL-04 - Performance-Test Parameter window appears. 3. Click a Performance-Test Parameter name shown to the right of Performance- Test. A Performance-Test Modes list appears. Click the Performance-Test Parameter to change items on the list. Right-click on the Performance-Test Parameter name to change the display. 4. See sequence No. 5 to 6 on the Performance-Test Parameter Setting if any modification is required. 5. Click the Quit button when the Performance-Test Parameter setting is completed. 68

85 Performance-Test Performance-Test Parameters The Performance-Test Parameters are displayed on the KL-04 - Performance-Test Parameter window. The definition of each Parameter is as follows; Syringe Syringe Volume (ml): Volume of the syringe installed on this unit can be set. The allowable range is 5 to 25 ml (1 ml step) Important Please be sure to set the installed syringe volume (the syringe volume for the standard installation is 25 ml). If set differently, correct measurement may not be possible. Measurement Aspiration Flow Rate (ml/min): This refers to the Syringe suction velocity and is designed to set the sample flow rate of this sensor. The allowable setting range is 5 to 100 ml / min (1 ml / min step). Important The aspiration fl ow rate set here must be the same as the aspiration fl ow rate for the Calibration Data (see page 79) selected by the same parameter setting. If the setting is different, the Performance Test will not complete normally and registration cannot be carried out (see next page). 69

86 Performance-Test Message KL-04 - Performance Test screen (when the aspiration fl ow rate is mismatch) Drain Flow Rate (ml/min): This refers to a syringe Drain Flow Rate. Set it with account to a sample s viscosity etc. The allowable setting range is 1 to 100 ml / min (1 ml / min step). Tare Volume (ml): In case of a sample s replacement or for the stability of the flow rate, normally set a slightly higher level than the dead volume (approx. 0.3 ml) inside the sampling tube which runs between the sample and the detector. In some cases, when a sample inside a sampling tube is changed from stationary to suction condition, particles previously stuck on the walls inside the flow channel will come off and subsequently the particle number concentration in the sample may rise. Taking these points into consideration, set it to an appropriate level. The allowable setting range is 0.1 to 10.0 ml (0.1 ml step). The setting value of tare volume is constantly added 0.2 ml, so actual tare volume range is 0.3 (dead volume) to 10.2 ml. Measurement Volume (ml) : Set the volume to measure particles. The allowable setting range is [(0.2 to Syringe volume) (Tare volume ml)] (0.1 ml step). With the standard 25 ml syringe, the range is 0.2 to 24.7 ml. 70

87 Performance-Test Number of Pre-Measurements (times): This enables setting of the number of repetitions of the Pre-Measurement prior to the Measurement. As the measuring sample may not necessarily be evenly distributed, It is therefore necessary to set the inside channel to the sample number concentration level. The Pre-Measurement is, therefore, required for this purpose and the suction volume etc., are carried out in the same manner as for the actual Measurement. However, the measurement result will not be included in the calculation of the average. The allowable setting range is between 0 to 10 times. Number of Measurements (times): This refers to setting the Number of Measurements. The allowable setting range is between 1 to 100 times. Drain After Every Measurement?: Drain a sample from the syringe after every measurement. Flush Aspiration Flow Rate (ml/min): This sets the suction velocity of the syringe during cleaning. The allowable setting range is 5 to 100 ml / min (1 ml step). Drain Flow Rate (ml/min): Set the syringe s Drain velocity while cleaning. The allowable setting range is 1 to 100 ml / min (1 ml step). Flush Volume (ml): Set the required volume for the syringe to draw up each time during cleaning. The allowable setting range is between 0.2 to 25.0 ml (0.1 ml step). Repeat (times): Set the number of times the unit carries out cleaning. The allowable range is between 1 to 100 times. 71

88 Performance-Test Calibration Data Calibration Data List: The registered Calibration Data name list will be displayed. Select the appropriate Calibration data to carry out a Performance-Test. Please note that an incorrect data selection will not enable you to carry out a correct Performance-Test. The following data are registered at the dispatch of this unit. KL-04_Basic: Calibrated according to a method in line with RION s specified method. JPxx: Calibrated according to a method in accordance with the Japanese Pharmacopeia (JP). (Registered only for those who have ordered Option(s)) USPxx: Calibrated using a method in accordance with the United States Pharmacopeia (USP). (Registered only for those who have ordered Option(s)) EPxx: Calibrated using a method in accordance with European Pharmacopeia (EP). (Registered only for those who have ordered Option(s)) * xx indicates each pharmacopeia s revision numbers (JP and USP) or version numbers (EP). EP has no regulations about Calibration and Performance-Test, so will be applied JP or USP by customer specification. View button: This enables checking of the selected Calibration Data. Select a required calibration data name from the list then click this button. The KL-04 - Calibration window appears. 72

89 Performance-Test Effective Period: Set the effective period for the application of the calibration data. The allowable setting range is between 1 to 9999 days. Important If the Effective Period for the set Calibrated Data has expired, an error occurs during the measurement which disables the measurement. PSL (General) PSL (General) List: A window for the registered test particle sizes will be displayed. Add button: Click this to add a PSL size for testing. The allowable PSL size channel is up to six (6). Click to display the Add New PSL window. 73

90 Performance-Test Average Diameter (µm): This is to set the PSL size for the test particles to be added. Set it within the system permitted size range of countable particles of 1.3 to 100 µm (0.1 µm step). Subtract CV for the Resolution?: Select this when the CV value(s) of the particles shall be subtracted calculating for resolution calculating CV of the PSL (%): Check Subtract CV for the resolution? to be able to enter values in CV of the PSL (%). Set the CV value of the particles, which shall be subtracted. The allowable setting range is 0.01 to 9.99%. Minimum Concentration (/ml): This sets the minimum number concentration of the count test suspension. The allowable setting range is 100 to 9999 particles / ml (1 particle / ml step). Maximum Concentration (/ml): This sets the maximum number concentration of the count test suspension. The allowable setting range is 101 to particles / ml (1 particle / ml step). Test Method: This selects a test method. JP will carry out tests on sensor resolution, particle counting accuracy, the threshold accuracy stipulated by Japan Pharmacopeia. USP will carry out the Sensor Resolution stipulated by United States Pharmacopeia. Set button: Click after setting the diameter for the test particle(s). An Add New PSL window closes, then a particle group list is added to the PSL (General) list. Edit button: Use this to change the particle diameters or upper threshold setting. Select a required PSL size from the PSL (General) list to edit. Click to display the Edit PSL Parameter window. The setting for the Edit PSL Parameter window is the same as the one for the Add New PSL window. See the explanation of the previous Add New PSL window for further setting details. 74

91 Performance-Test Delete button: Use this to delete the PSL size for the test particles. Select the PSL size from the PSL (General) list to be deleted. Click the PSL size to delete. Permissible Sensor Resolution (%): Set the Permissible Sensor Resolution. The allowable setting range is 1 to 50% (1% step). 100% Cumulative Count Threshold (µm): Set 100% Cumulative Count Threshold. The allowable setting range is 1.0 to µm (0.1 µm step). Permissible Threshold Accuracy (%): Set the Permissible Threshold Accuracy. The allowable setting range is 1 to 50% (1% step). 75

92 Performance-Test Suspension Use Suspension for Performance-Test?: Carry out the Particle Counting Accuracy stipulated by the USP. Select this to use the Suspension. Use Blank Bottle?: Select this to measure and subtract the Blank Bottle counts (which is part of the Performance-Test set of USP). Lower Threshold (µm): Set the lower threshold. The allowable setting range is 1.0 to 99.9 µm (0.1 µm step). Upper Threshold (µm): Set the upper threshold. The allowable setting range is 1.1 to µm (0.1 µm step). Minimum Concentration (/ml): Set the minimum number concentration of the test suspension. The allowable setting range is 100 to 9999 particles / ml (1 particle / ml step). Maximum Concentration (/ml): Set the maximum number concentration of the test suspension. The allowable setting range is 101 to particles / ml (1 particle / ml step). Minimum Ratio: Set the minimum ratio according to USP. The allowable setting range is 1.00 to 4.99 (0.01 step). Maximum Ratio: Set the maximum ratio according to USP. The allowable setting range is 1.01 to 5.00 (0.01 step). ID of the Suspension: Input a Suspension ID with less than 18 letters / figures. 76

93 Calibration When shipped from the factory, a maximum of four possible types of calibration (including options) have been carried out and the results are already registered as Calibration Data. These data serve as reference values that determine the setting (threshold) values for particle classification (size per channel) during measurement. To enable measurement based on calibration data, it is first necessary to carry out the Performance-Test and to register the Performance-Test data. The Calibration Parameters, such as JPxx, registered at the time of shipment (registered only for those who requested this option) are the officially approved ones (in accordance with each Pharmacopeia). When Calibration is required, copy the Calibration Parameter registered at the time of shipment, then copy and modify it and register it as a new Calibration Parameter for use. 77

94 Calibration Calibration Sequence Important The calibration to be carried out after one hour of system ON-time. The Preliminary Calibration Parameter Setting is required for calibration of the unit. See the Calibration Parameter Setting shown from page 85 onwards for this. The Calibration sequence is as follows; 1. An operator with access privileges to Calibration must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Calibration button from the Usual Operations menu on the KL-04 - Start New Window window. The KL-04 - Calibration window appears. 3. Click the Calibration Parameter shown to the right of Calibration then click a test Parameter Name in the displayed Calibration Modes list. 78

95 Calibration 4. Click the Show button from the KL-04 - Calibration window, then select the required Calibration Parameter. The KL-04 - Calibration Parameter window will appear. Check the details. Upon completing the check, press the Quit button to close the window. 5. Select Calibrate from the list by pressing Operation Items (Calibration data display) shown to the right of Operation. The window contents will change to the ones for calibration. 79

96 Calibration 6. Set a sample for cleaning (in general purified water) then either click the Flush button, or the FLUSH button on the front of the unit. Important When operating by pressing the FLUSH and START buttons on the unit, ensure that the KL-04 - Calibration window is set in an active window, in which the required Calibration Parameter Name is displayed. If it is not in an active window, operations may be different from the specifi ed Parameters. 7. Set up pure water for the Blank (Blank is a sample of pure water without any PSL-particles) measurement, then click the Blank button (displayed on the left hand side of the same row) to select the particle size (e.g µm) from the Calibration particle size list. Upon completion of the Blank Measurement, the result will be displayed on the right hand side of the Blank button. 8. Calibrate. Set sample(s) for calibration then select the specific required calibration particle size (e.g µm) from the list. Upon completion of the calibration task, the calibrated particle size will be displayed at the right of the particle size. The calibration result will be displayed in black if it is accepted, and in red if rejected. 80

97 Calibration 9. If other size calibration is required for one after another, repeat the sequence from No. 6 to No. 8 for the number of calibrating particle sizes. Upon completion of the calibration, click the Register button to register the calibration result. If the result is rejected, this means the registration cannot be accessed. 10. Upon completion of the calibration, click the Quit button. 81

98 Calibration The Calibration Result The actual calibration parameters will be displayed. Click on the Show button and select Show Management Information to display management information. The calibration result for an individual particle size The Blank Measurement, and the Calibration result for each calibrated particle size, will be displayed with a graph. Click on the Show button and select Show Management Information to display the management information. 82

99 Calibration Calibration Curve Click on the Show button and select Show Calibration Curve to display the calibration curve. Management Information Click on the Show button and select Show Management Information to display management information. 83

100 Calibration Display Calibration Data 1. An operator with access privileges to Calibration must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Calibration button from the Usual Operations menu on the KL-04 - Start New Window window. The KL-04 - Calibration window will appear. 3. Click the Calibration Parameter name shown to the right of Calibration. The Calibration Modes list will be displayed. Click the required Parameter name from the list. 84

101 Calibration Calibration Parameter Setting 1. An operator with access privileges to Set Calibration Parameter must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Calibration Parameter button from the View/Set Operation Parameters menu on the KL-04 - Start New Window window. The KL-04 - Calibration Parameter window will appear. 3. Click the calibrated Parameter name shown to the right of Calibration. A Calibration Modes list will be displayed. Click Add New Setting from the list. Already registered Parameters can be used by copying them in the following sequence. First, select the Calibration Parameter name from the Calibration Modes list. Then click Add New Setting to copy the Parameter. 4. Enter the Calibration Parameter name in the space underneath Calibration. 85

102 Calibration 5. Enter or check any required setting items. See next page, Calibration Parameter, for the details of each item on the KL-04 - Calibration Parameter window. 6. Click the Register button. 7. Repeat steps 3 to 6 to register a different Calibration Parameter. Click the Quit button when the Calibration Parameter setting is completed. Change Calibration Parameter The Calibration Parameter name which was registered at shipment was used for RION s calibration. Please do not change the parameter detail. 1. An operator with access privileges to Set Calibration Parameter must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Calibration Parameter button from the View/Set Operation Parameters menu on the KL-04 - Start New Window window. The KL-04 - Calibration Parameter window appears. 3. Click the Calibration Parameter name shown to the right of Calibration. A Calibration Modes list appears. Click a required Calibration Parameter from the list. 4. See the sequence No. 5 to 6 of the Calibration Parameter Setting for how to change each item. 5. Click the Quit button when the Calibration Parameter change is completed. 86

103 Calibration Calibration Parameter The Calibration Parameter is displayed on the KL-04 - Calibration Parameter window. The explanations for each parameter are below. Calibration: Rev.: Select a Calibration Parameter to show its setting details. When a new Calibration Parameter Setting is required, enter the calibration parameter in the space below Calibration. The latest Revision Number (the number of changes) will be displayed. The selected setting details for the Revision will be displayed when a number is selected. The number is selected with the + buttons. Syringe Syringe Volume (ml): Set the capacity for the syringe installed on the unit. The allowable range is 5 to 25 ml (1 ml step). Important Please be sure to set the installed syringe volume (the syringe volume for standard installation is 25 ml). If set differently, correct measurement may not be possible. 87

104 Calibration Measurement Aspiration Flow Rate (ml/min): This refers to the syringe s suction rate. This sets the rated flow rate of the unit. The allowable setting range is 5 to 100 ml / min (1 ml / min step). Important The aspiration flow rate set in the Calibration Parameter must be the same as the aspiration fl ow rate for the Performance Test Parameter. In addition, the aspiration fl ow rate for that Performance Test Parameter must be the same as the setting value for the Measurement Parameter that is using it. If the setting is different, the measurement and Performance Test cannot be carried out normally. Drain Flow Rate (ml/min): This refers to the syringe s drain flow rate. Take the sample s viscosity etc., into consideration when setting it. The allowable setting range is between 5 to 100 ml / min (1 ml / min step). Tare Volume (ml): In cases when a sample is replaced, or for the stability of the flow rate, normally set a slightly higher level than the dead volume (approx. 0.3 ml) inside the sampling tube between the sample and the detector. In some cases, when a sample inside a sampling tube is changed from stationary to suction condition, particles previously stuck on the walls inside the flow channel will come off and the particle number concentration in the sample may subsequently rise. Take these points into consideration when setting it to an appropriate level. The allowable setting range is 0.1 to 10.0 ml (0.1 ml step). The setting value of tare volume is constantly added 0.2 ml, so actual tare volume range is 0.3 (dead volume) to 10.2 ml. 88

105 Calibration Measurement Volume (ml): Set the volume for the particle measurement. The allowable setting range is [(0.2 to syringe volume) (Tare Volume ml)] (0.1 ml step). For the standard 25 ml syringe, the range is 0.2 to 24.7 ml. Number of Pre-Measurements (times): Set the number of Pre-Measurements prior to the actual measurement. As the measuring sample may not necessarily be evenly distributed, it is therefore necessary to set the inside channel to the sample number concentration level. The Pre-Measurement is, therefore, required for this purpose and the suction volume etc., are carried out in the same manner as for the actual Measurement. However, the measurement result will not be included in the calculation of the mean value. The acceptable setting range is between 0 to 10 times. Number of Measurements (times): Set the number of Measuring Repetitions. The allowable setting range is between 1 to 100 times. Drain After Every Measurement?: Drain a sample from the syringe after every measurement. Flush Aspiration Flow Rate (ml/min): Set the suction velocity of the syringe during the Flush time. The allowable setting range is between 5 to 100 ml / min (1 ml step). Drain Flow Rate (ml/min): Set the syringe s Drain velocity while flushing. The allowable setting range is between 5 to 100 ml / min (1 ml step). Flush Volume (ml): Set the required volume to be drawn up by the syringe each time during flushing. The allowable setting range is between 0.2 to 25.0 ml (0.1 ml step). Repeat (times): Set the number of times for flushing to be repeated. The allowable range is between 1 to 100 times. 89

106 Calibration PSL PSL List: A window for the registered calibration PSL sizes will be displayed. Add button: Click this to add a PSL size for calibration. The allowable PSL size channel is up to twenty (20). Click to display the Add New PSL window. Average Diameter (µm): This is to set the PSL size for the calibration particles to be added. The allowable setting size range is between to µm (0.001 µm step). Minimum Concentration (/ml): This sets the minimum number concentration of the calibration suspension. The allowable setting range is between 100 to 9999 particles / ml (1 particle / ml step). 90

107 Calibration Maximum Concentration (/ml): This sets the maximum number concentration of the calibration suspension. The allowable setting range is between 101 to particles / ml (1 particle / ml step). Half-Count Method: Select the Half-Count Calculation method. JP: This is the calculation method stipulated in the Japanese Pharmacopeia. USP: This is the calculation method stipulated in the United States Pharmacopeia. Adaptive: This is the calculation method stipulated by RION Co., Ltd. Set button: Click after setting the PSL size for the calibration particles. The Add New PSL window closes, then a PSL size list is added to the PSL list. Edit button: Use this to change the particle sizes or Maximum Concentration setting. Select a required PSL size from the PSL list to edit. Click to display the Edit PSL Parameter window. The settings for the Edit PSL Parameter window are the same as the ones for the Add New PSL window. See the explanation of the previous Add New PSL window for further setting details. Delete button: Use this to delete the PSL size for the Calibration. Select the PSL size from the PSL list to be deleted. Click the PSL size to delete. Effective Period: Select the specific Effective Period for the particle data. The allowable setting range is between 1 to 9999 days. 91

108 Print Printouts are available in the following sequence for Measurement Parameter, Performance-Test Parameter, Calibration Parameter, Measured Result, Performance-Test Result, Calibration Result, Operator Setting and Audit Trail. Please ensure the printer is properly connected before printing. See Connecting the Printer (Local Printer) on page 16. Connection to a printer connected to a network is available. However, please contact the system administrator to clarify the status as the particular environment may differ depending on the network. See Settings for a Printer Connected to a Network on Page 116 for the basic setting. 1. An operator with access privileges to each of Management Tasks must log in. 2. This enables display either of the windows for each parameter setting for printing, or individual work windows. 3. Click the Print button on each window. The xxxxxxxxxxxxxxxxx - Print window appears. (The xxxxxxxxxxxxxxxxx indicates the mode window name.) 92

109 Print 4. Click the Paper Size button and select the desired paper size from the list that appears. Click the Destination button and select the destination printer or output to file from the list that appears. To show the Signature Section in the print result (page 96), put a check mark in the Show Signature Section check box. Click the Print button to start printing. Right-click to alter Paper Size and Destination. The selected item changes with each click. If a Specified file is selected to Destination, it will be output as a post script file on /home/login name/temp/directory (see page 95). Click the Status button to display the Print - Status window. Deletion of the print status check or print request is possible in this window. 93

110 Print Error window appearing temporarily after upgrade After the version upgrade process was carried out, an error message will appear when you first attempt to print from any window (see page 143). This is only temporary and does not indicate a problem. Click the Close button in the error window to close the window, and then proceed with printing. The error window will not appear the next time. However, the temporary error window will appear for each operator separately. Printing from KL-04 - Measurement window When you click the Print button in the KL-04 - Measurement window, you can select one of two printing methods: Print... and Print This Data. If you select Print This Data, the window shown on page 92 will not appear, and the previously selected settings for printing data will be used (selected at any previous window after Print... ). 94

111 Print PS Files Postscript (PS) files can be viewed using Adobe Acrobat or other software available for free. When the xxxxxxxxxxxxxxxxx - Print window is called up from any window that allows printing in KL-04, the Destination button gives access to a choice called Specified File. When this is selected, a PS file with the specified name will be created from the print output. The file will be located in the /home/log-in name/temp directory, except for the audit trail, which will be located in the /home/audit Trail/temp directory. The PS file can be retrieved from KL-04 using FTP (File Transfer Protocol). Retrieving a file from KL-04 using FTP (File Transfer Protocol) Procedure This explanation assumes that FTP client software is available and that the operator is familiar with the use of the software. Any FTP client can be used. 1. Connect the KL-04 and the computer where the FTP client is installed. Make the network connection either via a hub using straight cables, or directly, using a cross-wired cable. There are no special requirements regarding power-on sequence and connection sequence. 2. Enter the IP address, log-in name, and password for the KL-04 in the FTP client to connect to the KL Use the FTP client to copy any PS files in the /home/log-in name/temp directory (or in the /home/audit Trail/temp directory for audit trail files) to the computer. 4. Terminate the connection at the FTP client. Important Do not copy, move, or delete any other fi les besides PS fi les in the /home/log-in name/temp or /home/audit Trail/temp directory. If unsuitable network settings (IP address etc.) are selected, the KL-04 may cease to operate normally. For security reasons, you should use the KL-04 only in a safe network environment that uses a standalone confi guration or is protected by a fi rewall. For information on how to check and change the IP address setting of the KL-04, see the section Network Settings on page

112 Print Print Samples Measurement Parameter KL-04 Measurement Parameter Page 1 of 1 Measurement Parameter: #1: KL 04 Basic for RION s Staff Revision: 22 Creation Date: :29:56 Operator: RION s Staffs (rion) Instrument: KL 04 No (kl ) Syringe Syringe Volume: 25 ml Measurement Aspiration Flow Rate: 25 ml/min Drain Flow Rate: 100 ml/min Tare Volume: 0.1 ml Measurement Volume: 10 ml Number of Pre Measurements: 1 times Number of Measurements: 3 times Drain After Every Measurement? No Calculate Particles per Unit Volume? No Clear "No." Field at Measurement Start? No Flush Performance Test Data Aspiration Flow Rate: 100 ml/min Drain Flow Rate: 100 ml/min Flush Volume: 10 ml Repeat: 1 times Performance Test: #1: KL 04_Basic Effective Period: 365 days Channels Diameter 1.3µm 5.0µm Upper Limit Signature Section RION Operator Manager :59:50 setup@kl-04-3 RION :59:50 setup@kl-04-3 No Signature Section Print Sample (under the wavy line) 96

113 Print Performance-Test Parameter KL-04 Performance-Test Parameter Page 1 of 1 Performance Test Parameter: #1: KL 04_Basic Revision: 12 Creation Date: :48:42 Operator: RION s Staffs (rion) Instrument: KL 04 No.ABC (kl ) Syringe Measurement Flush Calibration Data PSL Syringe Volume: 25 ml Aspiration Flow Rate: 25 ml/min Drain Flow Rate: 100 ml/min Tare Volume: 1mL Measurement Volume: 5mL Number of Pre Measurements: 1 times Number of Measurements: 3 times Drain After Every Measurement? No Aspiration Flow Rate: 100 ml/min Drain Flow Rate: 100 ml/min Flush Volume: 10 ml Repeat: 1 times Calibration: #1: KL 04_Basic Effective Period: 365 days Diameter CV Concentration Test Method µm 1.00% /ml JP Permissible Sensor Resolution: 10 % 100% Cumulative Count Threshold: 5µm Permissible Threshold Accuracy: 5% Suspension Use Suspension for Performance Test? Yes Use Blank Bottle? No Lower Threshold: 10 µm Upper Threshold: 15.6 µm Minimum Concentration: 800 /ml Maximum Concentration: 1200 /ml Minimum Ratio: 1.39 Maximum Ratio: 2.61 ID of the Suspension: JSR RION Operator Manager :00:15 setup@kl

114 Print Calibration Parameter KL-04 Calibration Parameter Calibration Parameter: #1: KL 04_Basic Revision: 6 Creation Date: :09:28 Operator: RION s Staffs (rion) Instrument: KL 04 No (kl ) Page1of1 Syringe Measurement Flush PSL Syringe Volume: 25 ml Aspiration Flow Rate: 25 ml/min Drain Flow Rate: 100 ml/min Tare Volume: 0.1 ml Measurement Volume: 5mL Number of Pre Measurements: 1 times Number of Measurements: 3 times Drain After Every Measurement? No Aspiration Flow Rate: 100 ml/min Drain Flow Rate: 100 ml/min Flush Volume: 10 ml Repeat: 1 times Diameter Concentration Half Count Method 1.274µm /ml Adaptive 2.047µm /ml Adaptive 5.125µm /ml JP 7.123µm /ml JP µm /ml JP µm /ml JP µm /ml JP µm /ml JP Effective Period: 365 days RION Operator Manager :22:31 setup@kl

115 Print Measurement Result KL-04 Measurement Data Page 1 of 1 Date: :06:26 Operator: RION s Staffs (rion) Sample: No.: Measurement: #3: USP24 (Rev. 4) Flow Rate: 25 ml/min Measurement Volume: 5mL Unit Volume: 1mL Dilution Ratio: 1 Instrument: KL 04 No (kl 04 2) Channel 2.1µm 5µm 10µm 15µm 20µm 25µm 50µm 1 Cumu. Diff Cumu. Diff Cumu. Diff Cumu. Diff Channel 2.1µm 5µm 10µm 15µm 20µm 25µm 50µm Channel 2.1µm 5µm 10µm 15µm 20µm 25µm 50µm Average (/1 ml) Judgement Cumu. Diff. Limit Result PASS PASS Average (Diff.) Management Information: Measurement Data: File: /home/rion/data/y2001/m10/d16/ Owner: rion / operator Time Stamp: :07:29 Fingerprint: 8742b85dac300b93 Measurement Parameter: Creation Date: :04:30 Operator: RION s Staffs (rion) File: /home/kl04/share/meas/conf/3/4 Fingerprint: bc31d64b b Performance Test Data: Performance Test: #5: USP24 (Rev. 1) Creation Date: :44:32 Operator: RION s Staffs (rion) File: /home/kl04/share/perf/data/5/1 Fingerprint: 358ec94f6f773e41 RION Operator Manager :01:38 setup@kl

116 Print Performance-Test Result KL-04 Performance-Test Data Performance Test: #1: KL 04_Basic Revision: 6 Creation Date: :17:38 Operator: RION s Staffs (rion) Instrument: KL 04 No (kl ) Page1of2 Performance Test Parameter Performance Test: #1: KL 04_Basic (Rev. 12) Aspiration Flow Rate: 25 ml/min Measurement Volume: 5mL Number of Pre Measurements: 1 Number of Measurements: 3 Creation Date: :48:42 Operator: RION s Staffs (rion) Management Information: File: /home/kl04/share/perf/conf/1/12 Owner: rion / kl04 Time Stamp: :48:42 Fingerprint: 4d352d799f09ca19 Calibration Data Calibration Data: #1: KL 04_Basic (Rev. 8) Aspiration Flow Rate: 25 ml/min Creation Date: :09:49 Operator: RION s Staffs (rion) Management Information: File: /home/kl04/share/cal/data/1/8 Owner: rion / kl04 Time Stamp: :09:51 Fingerprint: 2129a70d3b83e7af µm PASS Test Method: JP Average Diameter of the PSL: µm Subtract CV for the Resolution? Yes CV of the PSL: 1% 100% Cumulative Count Threshold: 5µm Date: :12:24 Operator: RION s Staffs (rion) Concentration: 854 /ml [ /ml] Sensor Resolution: 7.9% [max. 10%] Threshold Accuracy: 0.5% [max. 5%] Detail: 84% Cumulative Count Diameter: 9.972µm 50% Cumulative Count Diameter: µm 16% Cumulative Count Diameter: µm Management Information: File: /home/kl04/share/perf/data/raw/10.35/138 Owner: rion / kl04 Time Stamp: :13:38 Fingerprint: 940f8220efb340c2 5.0µm µm 0.000µm µm RION Operator Manager :02:20 setup@kl

117 Print Calibration Result KL-04 Calibration Data Page 1 of 6 Calibration: #1: KL 04_Basic NOT REGISTERED Creation Date: :23:07 Operator: Setup KL 04 (setup) Instrument: Calibration Parameter Calibration: #1: KL 04_Basic (Rev. 6) Aspiration Flow Rate: 25 ml/min Measurement Volume: 5mL Number of Pre Measurements: 1 Number of Measurements: 3 Creation Date: :09:28 Operator: RION s Staffs (rion) Management Information: File: /home/kl04/share/cal/conf/1/6 Owner: rion / kl04 Time Stamp: :09:28 Fingerprint: 1.274µm Blank: 6.6mV Date: :07:48 Operator: RION s Staffs (rion) Calibration: #1: KL 04_Basic (Rev. 5) Management Information: File: /home/kl04/share/cal/data/raw/1.274 blank/53 Owner: rion / kl04 Time Stamp: :08:57 Fingerprint: PSL: 17.2mV Date: :12:28 Operator: RION s Staffs (rion) Calibration: #1: KL 04_Basic (Rev. 5) Half Count Method: Adaptive Window: 10.4mV 25.1mV Concentration: 1065 /ml [ /ml] Management Information: File: /home/kl04/share/cal/data/raw/1.274/54 Owner: rion / kl04 Time Stamp: :13:38 Fingerprint: 6.6mV 17.2mV 0.0mV 39.1mV RION Operator Manager :25:25 setup@kl

118 Print Operator Setting KL-04 Operator List Instrument: KL 04 No.sisaku No.3 (kl 04 3) Page1of1 Operator Password Performance Test Calibration Set Measurement Parameter Set Performance Test Parameter Set Calibration Parameter Backup/Restore Operator Management Change Other Operator s Password Set Clock System Administration #501: rion (RION s Staffs) Normal #502: service (Authorized Service Center) Normal #503: admin (admin) Normal #504: setup (Setup KL 04) Normal #505: kangi (kangi) No password RION Operator Manager :25:47 setup@kl

119 Print Audit Trail KL-04 Audit Trail Page 1 of 1 Instrument: KL 04 No.003 (kl 04 3) Creation Date: > Operator: ALL Class: ALL Event: ALL :09:17 JST-9:0 root system power-on :09:38 JST-9:0 test operator log-in localhost :10:58 JST-9:0 test operator log-out localhost :11:14 JST-9:0 root system power-off :48:44 JST-9:0 root system power-on :49:06 JST-9:0 test operator log-in localhost :51:03 JST-9:0 test operator log-out localhost :51:21 JST-9:0 RION s Staffs (rion) operator log-in localhost :55:38 JST-9:0 RION s Staffs (rion) file create /home/kl04/share/perf/conf/1/ :06:16 JST-9:0 RION s Staffs (rion) file create /home/kl04/share/perf/data/1/ :07:33 JST-9:0 RION s Staffs (rion) file create /home/higashi/data/y2006/m04/d03/ RION Operator Manager :25:47 setup@kl

120 Export the measured data Export the measured data Measured data can be recorded as TSV (Tab Separated Values) type files on a floppy disk to enable the measured data to work on word processing software or spread sheet software. 1. Insert a floppy disk into the front floppy disk drive. 2. Select the List of Data from the menu displayed when the Show button is pressed on the KL-04 - Measurement window. Measurement - Data Selector window appears. 104

121 Export the measured data 3. When a non-formatted floppy disk is inserted, press the Floppy button to select a disk, then select Format a Floppy Disk from the list of operations. When an already formatted floppy disk is inserted, skip steps 3 to 4 of the process and move on to No. 5. A Confirmation message appears. 4. Click the Yes, Format it button from the confirmation message. Format with a PC-DOS format. Once the message disappears, the formatting is complete. 5. Select the Year & Month of the measured data which you wish to transfer from the Year & Month list, and the measured date from the Date list. Select the measured data from the Measured Data list. Multiple selection is available for measured data obtained on the same day. 6. Press the Floppy button to select Write Selected Data to Floppy Disk from the list of operations. Once the export is completed, a message appears. File names will be automatically allocated to the transferred data according to each measured date and these will be displayed on the message. When multiple data with the same date are to be transferred respectively, please prepare several separate floppy disks to transfer them as all files have the same file names. No extension is allocated to stored files. Particle data will be stored as differential values. 7. Click the Dismiss button. Remove the floppy disk. Data sample See data samples transferred to floppy disks. DATE TAB :06:26 OPERATOR TAB RION s Staffs (rion) INSTRUMENT TAB KL-04 No (kl-04-2) SAMPLE TAB NUMBER TAB MEMO TAB MEASUREMENT TAB #3: USP24 (Rev. 4) SAMPLE-VOLUME TAB 5mL PRE-MEASUREMENT TAB 1 REPEAT TAB 3 105

122 Export the measured data 2.1um TAB 281 TAB 276 TAB 289 TAB 316 5um TAB 61 TAB 46 TAB 60 TAB 54 10um TAB 5 TAB 5 TAB 8 TAB 4 15um TAB 0 TAB 1 TAB 0 TAB 0 20um TAB 0 TAB 0 TAB 0 TAB 0 25um TAB 0 TAB 0 TAB 0 TAB 0 50um TAB 0 TAB 0 TAB 0 TAB 0 * TAB indicates a control code TAB. Data description DATE: Measurement date OPERATOR: Measurement operator name INSTRUMENT: Measurement instrument number SAMPLE: Characters entered in the Sample of KL-04 - Measurement window NUMBER: Number(s) entered in the No. of KL-04 - Measurement window MEMO: Letters input to Memo: of KL-04 - Measurement window MEASUREMENT: Measurement parameter name SAMPLE-VOLUME: Measurement volume PRE-MEASUREMENT: Number of Pre-measurements REPEAT: Number of Repeated Measurements 2.1um TAB 281 TAB 276 TAB 289 TAB 316 5um TAB 61 TAB 46 TAB 60 TAB 54 10um TAB 5 TAB 5 TAB 8 TAB 4 15um TAB 0 TAB 1 TAB 0 TAB 0 20um TAB 0 TAB 0 TAB 0 TAB 0 25um TAB 0 TAB 0 TAB 0 TAB 0 50um TAB 0 TAB 0 TAB 0 TAB 0 : Measurement particle sizes and measured values 106

123 Back Up The built-in tape drive enables data file backup easily without connecting new devices. We recommend regular data file backup to prevent data file damages caused by unexpected incidents such as hard disk damage or power failure etc. When backing up data onto tape cartridges, use one of the data cartridge models indicated on the label affixed to the front of the KL-04. Use Tape Cartridge. denotes the tape cartridge model. Important Before using a tape for the fi rst time or when reusing a tape, perform Retension the Tape on the KL-04 - Backup/Restore window shown on the next page. Data backup will not be successful if other tape cartridge models are used. The tape cartridge models indicated on the label include TR-4 (e.g. the Travan 8 GB data cartridge from Imation Corporation) and TR-5 (e.g. the Travan 20 GB data cartridge from Imation Corporation). Specify one of these models when purchasing tape cartridges. Be sure to use a separate tape cartridge for each KL-04 unit. If you restore backup data from a tape made in one KL-04 in another KL-04, data mismatching and other problems may occur. We recommend to write the serial number of the KL-04 unit onto the tape cartridge to prevent mixups. When the KL-04 version was upgraded from 1.0 to 2.0, do not restore any backups that was taken in version 1.0 and comprise system data. Otherwise the version may revert to 1.0. You can check the KL-04 version on the KL-04 - Start New Window window by clicking the System Information button (see page 36). Backup 1. An operator with access privileges to Backup/Restore must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 107

124 Back Up 2. Click the Backup/Restore button from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Backup/Restore window appears. 3. Insert the tape cartridge into the tape drive located at the front of the unit. 4. Check either one of the following items, or both of them, then select an appropriate backup file type. All Operator s Files: Check this for backups of various parameters or various data files. When not checked, only the measured data of the actual operator will be backed up. System Files: Check this for backing up all of the system information files. 5. Click the Backup to the Tape button. During the back-up, the access lamp on the tape drive at the front of the unit flashes. When the access lamp goes OFF, the backup is complete. 6. Check whether the access lamp is OFF, then remove the tape cartridge. 108

125 Back Up Restore 1. An operator with access privileges to Backup/Restore must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Backup/Restore button from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Backup/Restore window appears. 3. Insert the required backup tape into the tape drive located at the front of the unit. 4. Select an appropriate process if the same file name exists on a required Restore backup tape and the KL-04. Don t Overwrite Existing Files: Select this when you do not want to overwrite a file with the same title on the main computer hard disk. If the content of a measurement data file has changed after a backup was created, restoring the data will overwrite the changes and cause the file to revert to the previous condition. For example, if entries were made in the modification column after the backup, restoring will cause the entries to be lost. To prevent this, put a check mark in the Don t Overwrite Existing Files check box. 5. Click Restore from the Tape button. An access lamp on the tape drive at the front of the unit will go on during the restoring process. Once the access lamp goes OFF, the restoring process is complete. 6. Check whether the access lamp is OFF, then remove the tape cartridge out. 109

126 System Setting Set Clock 1. An operator with access privileges to Set Clock must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Set Clock button from the Management Tasks menu on the KL-04 - Start New Window window. The KL-04 - Set Clock window appears. 3. Input the required settings. See page 112 for more details on each feature of the KL-04 - Set Clock window. 110

127 System Setting 4. Click the Set button. The confirmation message appears. 5. Click the Yes, Set the Clock button. A message appears recommending a logout. 6. Click the Dismiss button to close the message. 7. Log out then log in again. Important After setting the clock, you should quickly log out and then log in again. Otherwise the audit trail information (see page 125 and following) including operation history etc. will continue to be recorded with the previous time information. 111

128 System Setting KL-04 - Set Clock Window The details of the items on the KL-04 - Set Clock window are as follows; Time Zone: Input the appropriate time (i.e., to use this unit) in the designated space. Offset (hours): Input the time difference between the setting region and the UTC. At the time of shipment, the Japanese Time Zone is set as JST, with minus 9 hours for the offset. Date: Time: Input the year in the left space, the month in the middle and the date in the right space. Input the hour in the left space, minutes in the middle and seconds in the right space. 112

129 System Setting Network Settings The following is a brief description of Network settings to connect this unit to the Network. Please contact the system administrator for the detailed settings. 1. An operator with access privileges to System Administration must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the System Administration button from the Management Tasks menu on the KL-04 - Start New Window window. The Administration Tasks window appears. 3. Click the Network Configuration button. The Network Configurator window appears. 113

130 System Setting 4. To change the host name, click the Names button, then change the host name in the Hostname menu. At the time of shipment, KL-04-xxxx (xxxx is the last four digits of the serial number) is set up as the host name. When a change of host name is required, first input all the Network settings then logout. After this, turn the Power switch on the back of the unit OFF. After ensuring the power is fully OFF, turn the POWER switch ON. 5. Click on the Interfaces button to change this unit s previously registered address. 6. Select eth0 from the list then click the Edit button. The Edit Ethernet/Bus Interface window appears. 7. Input an IP address to the IP space and Netmask to the Netmask space then click the Done button. The Edit Ethernet/Bus Interface window closes. At the time of shipment, a random IP address is set up. Please contact a system administrator for an IP address and Netmask. 114

131 System Setting 8. Click the Hosts button then click the Add button. The Edit/etc/hosts window appears. 9. Input the IP address (inputted in step 7) to the IP space, and the host name (inputted in step 4) to the Name space. If required, input a nickname to the Nicknames space then click the Done button. The Edit/etc/hosts window closes. 10. Click on the Save button. 115

132 System Setting Settings for a Printer Connected to the Network The following is a brief description of the settings for connecting the unit to a printer (support PostScript Level 2 and above) connected to a network. Please contact the system administrator for connecting to a different printer on a Network, and its setting. 1. An operator with access privileges to System Administration must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the System Administration button from the Management Tasks menu on the KL-04 - Start New Window window. The Administration Tasks window appears. 3. Click the Printer Setup button. The Red Hat Linux Print System Manager window appears. 116

133 System Setting 4. Click the Add button. The Add a Printer Entry window appears. 5. Select Remote Unix (lpd) Queue from printer types shown on the Printer type then click the OK button. The Edit Remote Unix (lpd) Queue Entry window appears. 6. Input a random printer name to Names (name1[name2]...) space and a host name for the printer to be connected to the Remote Host space, then input a Remote Queue name in the Remote Queue space. The Remote Queue is used to spool printouts requested by this unit. The names vary depending on the printer manufacturers or Os mode. Please contact the system administrator for the printer host name and the Remote Queue name. 117

134 System Setting 7. Click the Select button. The Configure Filter window appears. 8. Select PostScript printer from the Printer Type list then click the OK button. Please do not change the other settings. The Configure Filter window closes and returns to the Edit Remote Unix (lpd) Queue Entry window. 9. Click the OK button. 10. Select Network Configuration from the Administration Tasks window. The Network Configurator window appears. 11. Click the Hosts button then click the Add button. The Edit/etc/hosts window appears. 12. Input the IP address in the IP space, and the host name (inputted in step 6) to the Name space. If required, input a nickname to the Nicknames space then click the Done button. Please contact the system administrator for the IP address. The Edit/etc/hosts window closes. 13. Click the Save button. 118

135 Useful Tools Virtual Keyboard Use the virtual keyboard shown in the window to input characters by using a mouse only. 1. An operator with access privileges to any of the Management Tasks must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Virtual Keyboard button from the Unsupported menu on the KL-04 - Start New Window window. The xvkbd - Virtual Keyboard window appears. 3. Instead of pressing keys on the keyboard, click keys to input letters and figures on the virtual keyboard using the mouse. The operator may only add letters and figures to data measured by the operator him / herself. Entering characters to data measured by other operators is not permitted. 119

136 Useful Tools TkSnapshot Use this to save the window with the displayed image as a file, and to print. 1. An operator with access privileges to any of Management Tasks must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. Click the Screen Snapshot button from Unsupported menu on the KL-04 - Start New Window window. The TkSnapshot (Version 0.31) window appears. 3. Select required settings. See page 122 for the details of each item of the TkSnapshot (Version 0.31) window. 4. Click Snap button. 120

137 Useful Tools 5. Click or drag on areas of the screen, matching the item selected in Snap Type. Window: Click anywhere on the desired window. Region: Drag over the desired region. Screen: Click anywhere on the display. 6. Click the Save button. The TkSnapshot - Save window appears. 7. Enter a name for the image file to Save as, then select a file format from Format, then click the Save button. See the next page for explanation of each item in the TkSnapshot - Save window. The captured image file can be used on other software via a Network using software such as FTP software. Please contact the system administrator for the FTP software application etc. 121

138 Useful Tools TkSnapshot (Version 0.31) Window Load button: Displays stored screen images in the window. Click to show the TkSnapshot - Load window. Select the required file name from the list and click the Load button, then click the View button. Save button: This saves captured window images on the hard disk. Click to show the TkSnapshot - Save window. See the next page for the details of each item in the TkSnapshot - Save window. Print button: To print captured window images. Click to show the TkSnapshot - Print window. Select or click on required items then click the Print button. Snap Type: To capture areas for taking images. Window: To capture only one window. Region: To capture dragged areas. Screen: To capture the whole screen. Snap Delay: To select a delay time from 0, 2, 4, 8, and 16 seconds. This is the time delay from the moment of the Snap button is clicked to the time when the screen image is actually captured. When Region is selected on the Snap Type, Snap Delay is not accessible. Beep During Countdown: This beeps once the Snap button is clicked and until the screen image is captured. 122

139 Useful Tools Hide Window During Capture: This enables the user to hide the TkSnapshot (Version 0.31) window after clicking the Snap button until the screen image is actually captured. The TkSnapshot (Version 0.31) window reappears once the screen image is captured. Snap button: To capture screen images. View button: To view a screen image captured immediately before. The TkSnapshot - Save Window Current Directory: This is to input a screen image store location. The initial entry of the store location is /home/<login Name>/tmp. Save as: This is to input a file name to attach to a screen image. Input the extension for the stored screen image when using a system which recognizes file names with extensions such as Microsoft Windows. 123

140 Useful Tools Format: This is to select a file format for a screen image to be stored. When Automatic is selected, the file format is determined according to the file name extension inputted in Save as. When no extension is entered, it will be stored as a XWD format. When the file format specified in Format is different from the extension of the file name entered under Save as, the file format specified in the Format has priority. Save button: This is to store the screen image. 124

141 Audit Trail The audit trail function complies with the requirements of various electronic recording and electronic signature regulations, such as the 21 CFR Part 11: Electronic Records; Electronic Signatures by the American FDA. The KL-04 continuously records operation history data (when/who/which operation). These data can be displayed, searched (by time period, operator, class, event), and the display contents can be printed. Access to this function can be set for each operator using the Operator Management function (see page 45). This makes it possible to clearly distinguish between administrators and operators, and to transparently manage the production of documents (printouts). 125

142 Audit Trail Operations recording in the audit trail For operations listed in the table below, audit trail information is recorded at the point where the operation is completed, or where the file is created in the case of operations that create a file upon completion. For information on Class, Event, and in the table, see the section about the recording format for each item on the next page. Operation Class Event Measurement parameter change Measurement parameter annotation change file create target file name file modified target file name Measurement data deletion file delete target file name Output of measurement data to floppy disk file export floppy Printing and PS file output file print target file name Log-in operator log-in localhost Log-out operator log-out localhost Power-on system power-on Power-off system power-off Add operator operator_mgr create Change operator privileges or password of other operator Operator has opened own password change screen (including no actual change) operator_mgr operator modified Backup tape backup Restore tape restore password_modified newly created operator name name of operator with changed privileges successful or fail, and checked item names successful or fail, and checked item names Date/time change date modified Date/time after it changes *1 Operator has opened network setting screen network modified Operator has opened printer setting screen printer modified Operator has opened audit trail view screen Audit_Trail print print screen search conditions *1 Same for time period and offset, but new log-in is required. 126

143 Audit Trail Format for recorded items The audit trail information comprises the items listed in the table below. Time stamp Operator name Class Event Date/time and time zone Registered operator name Operation category Operation Changed item, measurement data file name, etc. The recording format is as follows. (Example: log-in event) Date Time Time zone :48:44 JST-9:0 Rion's Staffs (rion) operator log-in localhost Time stamp Operator name Class Event For the power-on and power-off events, the operator name is always root. The time stamp for the power-on event is the time when the system of the KL-04 was started. When the operator name was registered as a full name, the log-in name is given in brackets. Audit Trail window 127

144 Audit Trail Searching and Viewing the Audit Trail File 1. Log in as an operator with Audit Trail access privilege, and display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 2. In the KL-04 - Start New Window window, click the Audit Trail button under Administrative Tasks:. The KL-04 - Audit Trail window appears, containing the Audit Trail - Select window. 3. In the Audit Trail - Select window, select the display conditions using the time stamp fields (Start Year/Month/Day and End Year/Month/Day) and the buttons for Operator, Class, and Event. Then click the Display button to show the pertinent information in the KL-04 - Audit Trail window. If you have selected ALL OPERATORS, ALL CLASSES, and ALL EVENTS, the entire audit trail information will be shown. 4. Click the Close button in the Audit Trail - Select window to close the window. By clicking the Print... button in the KL-04 - Audit Trail window, you can print out the currently displayed audit trail information or produce a PS file (see page 92). 128

145 Audit Trail 5. When you click the Conditions... button in the KL-04 - Audit Trail window, the Audit Trail - Select window appears again. 6. To close the KL-04 - Audit Trail window, click the Finish button. Message windows displayed during search When an audit trail search is performed, a window such as shown below may appear. This is shown when the time stamp input for start date and end date is reversed. Repeat the input with correct values. Close the window by clicking the Dismiss button. This is shown when there are more than 2,000 records that match the search conditions. Narrow down the search by specifying more restrictive conditions. Close the window by clicking the Dismiss button. This is shown when there are no records that match the search conditions. Widen the search by specifying less restrictive conditions. Close the window by clicking the Dismiss button. This is shown when the search failed. Turn power to the KL-04 off and then on again. Log in again and repeat the search. Close the window by clicking the Dismiss button. If the same message window appears again, there may be a problem with the system. Please contact the supplier. 129

146 Audit Trail Audit Trail Backup and Restore The audit trail information is always included in a backup. During restore, the audit trail file will not be overwritten. When restore has been performed, an asterisk (*) will be shown to the left of the audit trail item, which indicates that the item pertains to the condition before restore. If restore is carried out multiple times, the audit trail information is also retained in multiple levels. When an item with an asterisk is included, the same recorded content will be shown in the audit trail multiple times. For details on the backup and restore functions, see the section Backup starting on page 107. When Clock Setting Was Changed After changing the set clock, you should certainly log out and then log in again (see page 110 and following). Otherwise the audit trail information will continue to be recorded with the previous time information. 130

147 Maintenance Syringe Replacement Important The syringe may wear out. If foams appear from the sliding piston during suction or when sample liquid is leaking while draining, please replace the syringe. 1. Click the FLUSH button to start the operation. 2. When the plunger has drawn 15 to 20 ml, open the syringe cover then stop the operation (the plunger stops at that position). 3. Turn the POWER switch OFF. 4. Loosen the screw on the clamp. Screw Clamp 131

148 Maintenance 5. While pressing the syringe lightly with one hand, remove the fixing crew on the lower side of the syringe with the other hand. Fixing screw 6. While pressing the syringe lightly with one hand, lower the syringe outer chamber by turning it left with the other hand. The syringe will be removed from the valve. 7. While immersing the end of a new syringe in water, pull the plunger. 132

149 Maintenance 8. Insert the new syringe into the clamp, with the clamp pin on the left hand side and the C-shaped open area to the front. Clamp Syringe 9. Insert the screw area of the new syringe into the syringe fixing hole on the valve. While pressing the syringe lightly with one hand, turn the syringe outer chamber right to install it. 10. Fix the syringe firmly using fixing screw. Fixing screw 133

150 Maintenance 11. Adjust the position by turning the clamp little by little so that the pins make contact with the left hand side of the wall surface in which the syringe is to be fixed. Once it is fixed, tighten the screw while making sure that the pin is in the correct location. Important Please do not over-tighten. This may cause damage. Pin Screw Screwdriver 12. Close the syringe cover. 13. Turn the POWER switch ON. 14. Log in. The plunger returns to the specified location (water inside the syringe will be drained). 134

151 Maintenance Handling the Syringe The sealed piston of the KL-04 Syringe can easily be damaged as it is made of Teflon. Please make sure to follow the instructions below in order to maintain the syringe in optimum condition for as long as possible. - Prior to using the syringe, make sure the sealing area is fully moistened, using pure water such as distilled water or deionized water, etc., to operate the syringe. Never carry out a dry run. - When removing the plunger from the outer syringe, and when re-inserting it, please be sure to handle it in the same manner as above. - After measuring, clean the inside of the syringe thoroughly using pure water such as distilled water or deionized water, etc., (repeat over five full strokes). - Clean the inside of the syringe every one or two weeks using methods A or B shown below. (Select the method depending on the type of measuring sample or the measuring frequency.) A. Cleaning by detergent or bleach 1. Immerse the syringe in diluted detergent or diluted bleach for approx. 30 minutes. 2. Clean it fully using pure water such as distilled water or deionized water etc. B. Cleaning with acid or alkali 1. Immerse the syringe in NaOH (10% concentration) for approx. ten minutes. 2. Clean it fully using pure water such as distilled water or deionized water. 3. Immerse the syringe in HCl (10% concentration) for approx. ten minutes. 4. Clean it fully using pure water such as distilled water or deionized water. - If air bubbles are produced continuously from the piston seal, the syringe needs to be replaced. Please contact the supplier. Cleaning main unit - When cleaning main unit, use neutral detergent and wipe up with soft cloth. Please make sure not to erase the printings, paintings, and markings when cleaning main unit. - The printings, paintings, and marking on the main unit are very important information for safety operation and serious accidents might be caused if operated without them. 135

152 Maintenance Noise Level Check and Flow Cell Cleaning When a sample exceeds the specified maximum particle number concentration, or a sample is mixed with air bubbles, or contamination has occurred, or moisture condensation has formed on the flow cell or the detection system, the letters / figures on the KL-04 Controller window turn to orange. If this occurs during measurement, the Bad Sensing Condition warning message appears after completion of the measurement. Check the noise level and clean the flow cell area in the following way. Noise Level Check 1. Supply pure water to the unit to replace the sample liquid. If the sample liquid undergoes a chemical reaction with water, first replace it with a suitable liquid which does not cause a reaction, then replace that liquid with pure water. 2. Run pure water over the unit to clean it. 3. An operator with access privileges to Calibration must log in and then display the KL-04 - Start New Window window. See page 34 for the login method and see page 36 for the KL-04 - Start New Window window display method. 4. Click the Check Noise Level button from the Usual Operations menu on the KL-04 - Start New Window window. The KL-04 - Check Noise Level window appears. 5. Click the Start button. To check the noise level, clean the flow system thoroughly with purified water, then fill it completely with purified water and carry out the check. The KL-04 Controller - Measurement in Progress window appears. Upon completion of the check, the Noise Level will be displayed. 6. Record the noise level, and then press the Quit button. 136

153 Maintenance 7. Clean the flow cell as described below. If the optional test records document is available, compare the noise level at the time of shipping with the currently recorded noise level. If the noise level has increased, clean the flow cell. If the noise level has decreased, the sensor may be defective. Please contact the supplier. Flow Cell Cleaning 1. Supply pure water to the unit to replace the sample liquid. If the sample liquid undergoes a chemical reaction with water, first replace it with a suitable liquid which does not cause a reaction, then replace that liquid with pure water. 2. Run pure water over the unit to clean it. 3. After cleaning thoroughly, purge the unit with pure water at the sample flow rate (25 ml / min. 10 ml / min for the factory option). When the letters / figures on the KL-04 Controller window change to black, the cleaning is complete. If the letters / figures on the KL-04 Controller window remain orange, repeat the cleaning further (follow the steps from No. 4). 4. Purge the unit with cleaning liquid without contamination. For cleaning liquid, please use detergent used for optical parts or alcohol etc., without any solids. 5. After sufficient purging, replace the cleaning liquid with pure water. 6. Supply pure water at the rated sample flow rate (25 ml / min, 10 ml / min for factory option) to the unit. If the letters / figures on the KL-04 Controller window change to black, cleaning is complete. Check the noise level again according to the procedure on the previous page and confirm the noise level has fallen. 7. If the letters / figures on the KL-04 Controller window remain orange or the noise level is still high, clean using the cell cleaning brushes provided (see next page). 137

154 Maintenance Cleaning Using a Cell Cleaning Brush Use the attached cell cleaning brushes to clean the flow cell. Two cell cleaning brushes are provided in a special case. Cell cleaning brushes - 2 Case Cell cleaning brush portion Important Handle the cell cleaning brushes with care since they are easily bent. To clean the flow cell using a cell cleaning brush, follow the steps described below. 1. Remove the sampling tube from the unit while the sample fluid system is still filled with pure water. Important If a cell cleaning brush is inserted into the fl ow cell while it is dry, there is the risk of the fl ow cell being damaged. Always make sure that the fl ow cell is fi lled with water before cleaning with a cell cleaning brush. 2. Take the cell cleaning brush out of the case and moisten the end of the brush with pure water. 138

155 Maintenance 3. Holding the cell cleaning brush approximately 70 mm away from the end, insert it slowly and carefully, straight into the INLET. Slight resistance may be felt when the cleaning brush reaches the entrance to the flow cell. Continue to slowly and carefully insert the cleaning brush until resistance is no longer felt. Cell cleaning brush Important Applying excess pressure can result in damage to the fl ow cell and cell cleaning brush. If the cell cleaning brush does not enter the fl ow cell, pull out the cell cleaning brush and check for damage or bending of the end of the brush. If the end of the brush is damaged or bent, replace it with another cell cleaning brush. If the cell cleaning brush is inserted with excessive force, it may cause damage to the fl uid system. Please do not insert it by more than approximately 70 mm from the end. 4. Pull out the cell cleaning brush slowly. 5. Repeat steps 3 and 4 several times. 6. Connect the sampling tube to the INLET of this unit, and clean by purging with pure water. 7. Supply pure water to the unit at the rated sample flow rate (25 ml / min, 10 ml / min for factory option). If the letters / figures on the KL-04 Controller window change to black, cleaning is complete. Check the noise level again according to the procedure on page 136 and confirm the noise level has fallen. If the KL-04 Controller window is shown with orange still remaining, there may be excessive contamination or damage of the flow cell area. Please contact the supplier. 139

156 Maintenance Periodic Maintenance In order to maintain continued measurement precision, it is recommended to have the unit checked and serviced once per year. Contact the supplier regarding periodic maintenance. The Standardization of Units by the Regional Pharmacopeia The effective period is set for the standardization of the unit in every region (Calibration, Performance-Test). It is therefore necessary to carry out the standardization (Calibration, Performance-Test) prior to the end of the effective period. If standardization (Calibration, Performance-Test) of units at each region is required from us, please contact the supplier. Transport Before returning the unit for maintenance or servicing, purge the sample fluid system thoroughly with pure water to remove any sample fluid remnants. Then fill the piping with alcohol (ethyl alcohol) and seal it with the end plugs. Wipe the outside of the unit clean so that there are no remnants of chemical substances on the unit. Before transporting or moving the unit, be sure to back up the system and all data. This is to guard against the possibility of data loss and disk failure that can occur if the hard disk drive is exposed to shocks during transit. 140

157 Troubleshooting When the Letters / Figures on the KL-04 Controller Window appear in Red This indicates that the output of the laser diode of the particle sensor has fallen below the specified level. Correct measurement cannot be carried out under these conditions. If this is encountered during the measurement operation, the Sensor Degraded warning message appears after the completion of the measurement. If the red letters / figures on the KL-04 Controller window or the Sensor Degraded warning message appear often, the laser diode may be damaged, or may have some problems. Please contact the supplier. When the Letters / Figures are Displayed in Orange on the KL-04 Controller This indicates a sample exceeding the specified maximum particle number concentration, or a sample mixed with air bubbles, or contamination, or condensation has occurred on the particle detection flow cell area. If this is encountered during measurement, the Bad Sensing Condition warning message appears after the completion of the measurement. Perform Noise Level Check and Flow Cell Cleaning (see page 136) and Cleaning Using a Cell Cleaning Brush (see page 138) then remove any deposits and air bubbles in the flow channel. If this problem persists even after repeated cleaning of the flow cell, the flow cell or detection system may be damaged. Please contact the supplier. When the Performance-Test Fails When the Performance-Test fails, check that there are no problems with the Performance- Test Parameters, the condition of the Test Particles, and no mistakes on the test, then repeat the Performance-Test again. If the failure persists even after several Performance-Tests, there may be problems with the particle detector etc. Please contact the supplier. 141

158 Troubleshooting When Message Window Appears The remaining free space on the hard disk drive in the KL-04 is low, or the hard disk has become full. Erase data that are no longer needed, or contact the supplier. When storing data at a rate of 100 per day, the hard disk of the KL-04 will not become full by measurement and other data alone over a period of 5 to 6 years. However, after several years, performing regular backups is important, because the risk of mechanical failure of the hard disk increases. It may therefore be advisable to replace the hard disk in some instances. Please contact the supplier. Close the window by clicking the Dismiss button. When the internal error message window appears, turn power to the KL-04 off and then on again. If the message window no longer appears, there is no problem. If the message window appears again, there may be a hardware or software fault. the content of the error message and contact the supplier. Close the window by clicking the Dismiss button. 142

159 Troubleshooting This message appears when an attempt is made to perform more than 999 restore operations in a single month. In this case, no more restore operations can be carried out. When the month changes, restore can be carried out again. Close the window by clicking the Dismiss button. This message appears when the aspiration flow rate for the Performance Test Data selected during Measurement Parameter specification is different from the aspiration flow rate specified for measurement. In such a case, measurement cannot be carried out. Change the setting so that the aspiration flow rate values for the Measurement Parameter and Performance Test Data are the same (see page 55). Close the window by clicking the Dismiss button. This message appears when a print operation is performed in any window after performing a version upgrade (see page 92). This is a temporary occurrence and does not indicate a problem. Close the window by clicking the Dismiss button and proceed with the print operation. The message will not appear the next time. However, the temporary error window will appear for each operator separately. 143