CETAC ASX-112FR Autosampler - Operator's Manual
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COPYRIGHT TRADEMARK ACKNOWLEDGEMENTS © 2008-2014 Teledyne Technologies Windows is a registered trademark of Incorporated. All rights reserved. Microsoft Corporation in the United States and other countries. 480159 Rev 4 , January, 2014 PharMed and Tygon are registered Teledyne CETAC Technologies authorizes its trademarks of Saint-Gobain Performance customers to reproduce, transmit, or store Plastics. this document in its entirety, including this page, for the express purpose of installing, All other marks are the property of their operating, or maintaining the product respective owners. described herein. Teledyne CETAC Technologies Customer Service & Support 14306 Industrial Road Omaha, Nebraska 68144, USA Phone (800) 369-2822 (USA only) Phone (402) 733-2829 Fax (402) 733-1932 E-mail custserv@cetac.com REVISIONS Teledyne CETAC Technologies strives to provide the scientific community with an unparalleled combination of effective technology and continuing value. Modular upgrades for existing instruments will continue to be a prime consideration as designs progress. Teledyne CETAC Technologies reserves the right to revise this document and/or improve products described herein at any time without notice or obligation. Warranty registration entitles the named owner exclusively to manual change pages/new editions as they are published.
Contents 1 Introduction .............................................................................................................. 7 Overview.................................................................................................................................... 7 About This Book ..................................................................................................................... 7 Who Should Read This Book ...................................................................................... 7 Autosampler Configuration Options ............................................................................. 8 Autosampler Standard Components ............................................................................. 9 Additional Equipment Required ...................................................................................12 Optional Accessories ..........................................................................................................12 Chemical Compatibility .....................................................................................................14 Where to Go for More Information ..............................................................................14 2 Preparing for Installation ................................................................................. 15 Choosing a Location ............................................................................................................15 Space Requirements.................................................................................................... 15 Work Surface Requirements .................................................................................... 16 Rinse Solution Requirements................................................................................... 16 Liquid Waste Routing Requirements ................................................................... 16 Power Requirements................................................................................................... 16 Unpacking the Autosampler ...........................................................................................17 3 Installing the Autosampler ............................................................................... 19 Overview .......................................................................................................................... 19 Mounting the Sample Probe Assembly ......................................................................20 Connecting the Rinse Station..........................................................................................22 Peristaltic Pump Configuration.............................................................................. 23 Gas Displacement Pump Configuration .............................................................. 25 Argon Gas Supply for Gas Displacement Pump ................................................ 26 Assemble and Place the Sample Rack and Vials .....................................................31 Short Rack Configuration ......................................................................................... 31 Tall Rack Configuration ............................................................................................ 32 Connecting the Autosampler to the Power Supply ...............................................34 Connecting the Autosampler to an Analytical Instrument ................................35 Connect the ASX-112FR Autosampler to the Host Computer ..........................35 Establishing an RS-232 Serial Communications Interface ................................36 Establishing a USB Communications Interface ......................................................37 Establishing an IEEE Communications Interface ..................................................41 ASX-112FR Tray Files ........................................................................................................41 4 Verifying Installation .......................................................................................... 43 Testing the Communications Interface ......................................................................43 Checking the Autosampler Components ...................................................................44 Testing the Sample Probe ................................................................................................44 3
ASX-112FR Autosampler Operator’s Manual Contents 5 Using the Autosampler ....................................................................................... 47 Establishing Optimal Operating Conditions ............................................................ 47 Creating the Lab Environment ............................................................................... 47 Replacing Auto Sampler Components ................................................................. 48 Purchasing Supplies ................................................................................................... 48 Arranging the Sample Vial Racks ................................................................................. 49 Starting the Autosampler................................................................................................. 49 Shutting Down the Autosampler .................................................................................. 50 Flushing the Rinse Station and Flow Path ................................................................ 50 Reconfiguring the Autosampler Sample Height .................................................... 51 Reconfiguring the Autosampler ICP-MS Personality........................................... 52 6 Maintaining the Autosampler .......................................................................... 53 Cleaning the Autosampler ............................................................................................... 53 Routine External Cleaning ....................................................................................... 53 Thorough Cleaning ..................................................................................................... 54 Checking for Leaks .............................................................................................................. 55 Replacing the Rotary Tray ............................................................................................... 55 Replacing the Rinse Station ............................................................................................ 56 Replacing Peristaltic Pump Tubing ............................................................................. 58 Replacing the Sample Probe ........................................................................................... 58 Replacing the Rinse Tubing ............................................................................................ 59 Spare Parts ............................................................................................................................. 60 Peristaltic Pump Tubing ........................................................................................... 60 Sample Probes............................................................................................................... 60 C-Flow PFA Nebulizers .............................................................................................. 60 Vials................................................................................................................................... 60 7 Troubleshooting the Autosampler ................................................................. 61 Power System Problems .................................................................................................. 61 Communications Interface Problems ......................................................................... 62 RS-232 Serial Cable Problems ................................................................................ 62 USB Cable Problems.................................................................................................... 62 Software Configuration Problems ........................................................................ 63 Alignment Problems .......................................................................................................... 63 Returning the Product to CETAC for Service .......................................................... 64 Shipping the Product.................................................................................................. 64 Product Warranty Statement ................................................................................. 64 Returned Product Procedures ................................................................................ 65 Returned Product Warranty Determination .................................................... 66 8 Operating a CETAC Autosampler Using a Terminal Program .............. 67 Using C-Term™ ..................................................................................................................... 67 Starting C-Term ........................................................................................................... 67 Overview of the C-Term Window ........................................................................... 68 Configuring C-Term .................................................................................................... 69 Setting Preferences ..................................................................................................... 70 Using HyperTerminal ........................................................................................................ 70 Autosampler Commands .................................................................................................. 74 9 Safety and Regulatory Information................................................................ 75 Characteristics ...................................................................................................................... 75 Environmental Characteristics .............................................................................. 75 4
ASX-112FR Autosamplers Operator’s Manual Contents Electrical Characteristics.......................................................................................... 76 Safety Notices ........................................................................................................................77 Power Cord Set Requirements ................................................................................ 77 Power Cord Safety Maintenance ............................................................................ 77 Mains Disconnect ......................................................................................................... 77 Cleaning Instructions ................................................................................................. 78 Mechanical Hazards ................................................................................................... 78 Operating Environment............................................................................................. 79 Explanation of Caution and Warning Notices .................................................. 80 Avertissements en Français ............................................................................................81 Electromagnetic Interference ........................................................................................82 Explanation of Regulatory Marks .................................................................................82 10 Glossary ................................................................................................................... 83 5
1 Introduction Overview The CETAC ASX-112FR autosampler is designed to be sturdy, reliable, and easy to use. It provides automated sample introduction that enables you to perform other tasks while the autosampler runs. The ASX-112FR autosampler automatically introduces up to 96 samples when fully loaded. It contains a microprocessor that allows sequential or random sampling, providing flexibility. The autosampler is typically interfaced to and controlled by the ICP-MS instrument host computer using a serial or USB connection. The ASX-112FR offers a small footprint to conserve bench space, a short sample path to preserve valuable sample, and a protective cover to prevent sample contamination. The dual flowing rinse station prevents carry over to ensure sample integrity. The ASX-112FR is both contamination and corrosion resistant and offers a completely inert flow path. The ASX-112FR can be conveniently placed on top of the CETAC Aridus II™ Desolvating Nebulizer System. The Aridus II™ is commonly used for signal enhancement/interference reduction for ICP-MS. Applications include corrosive, limited-volume samples for geology and semiconductors. About This Book This document describes the procedures for installing, using, and maintaining the autosampler. It also provides information about troubleshooting minor problems and describes the design of the autosampler. This manual covers the following products: CETAC ASX-112FR Who Should Read This Book The primary audience for this manual consists of analytical chemists and lab technicians. To use this manual effectively, you should have a basic knowledge 7
ASX-112FR Autosampler Operator’s Manual Chapter 1: Introduction of chemistry, a basic knowledge of electronic sampling equipment, at least a beginning level of computer experience, and working knowledge of the analytical instrument used with the autosampler. CHEMICAL INJURY HAZARD WARNING The autosampler is intended for use only by qualified operators who have been trained in safe laboratory practices. Make sure you know the hazards associated with all of the chemicals you are using, and take the appropriate precautions. Exposure to laboratory chemicals may result in serious injury. Autosampler Configuration Options The ASX-112FR is very configurable making it ideal for use in multiple applications. Three models are available. The standard model comes with a polypropylene rinse station controlled by a peristaltic pump. A second model comes with a polypropylene rinse station controlled by a gas displacement pump, which uses compressed gas to push the rinse solutions through the rinse station. A third model is equipped with a PFA rinse station and a gas displacement pump for ultra-clean applications. All three models have the option to be selected in either a tall or short configuration. The height configuration restricts the choice of racks to be either tall—BelArt half racks (with 7 mL or 14 mL vials) or short—CETAC racks for small samples (with 0.5 mL, 1.0 mL, 1.5 mL or 2 mL vials). The rinse station is also configured in either a tall or short version. Two probe sizes are offered: 0.010” (0.25 mm) ID and 0.035” (0.89 mm) ID. The 0.035” ID is expected to be the standard with the 0.010” ID designed for a low-flow (
ASX-112FR Autosamplers Operator’s Manual Chapter 1: Introduction Autosampler Standard Components Figure 1-1. ASX-112FR Autosampler—Front View Figure 1-2. ASX-112FR Autosampler—Side View. 9
ASX-112FR Autosampler Operator’s Manual Chapter 1: Introduction The following components are located on the front of the autosampler and are shipped with the autosampler. Each lettered item corresponds with a callout in Figure 1-2. A Rotary Tray. The rotary tray has 14 standard positions and a rectangular center cavity, which holds one sample rack in place. B Sample Rack Location. The ASX-112FR includes one sample rack. Rack choices include short or tall rack configurations. A keyed interface plate is required to use the short racks. The tall racks are placed directly in the rotary tray with no interface plate required. The appropriate sample vials must be used for each rack, and the host computer’s software must be configured for that particular rack layout and number of positions. The identification designations are shown in the host computer's software – if the software does not include a specific reference for the ASX-112FR, a reference for the older model ASX-100 may be applicable with the ASX-112FR tray files. Short – CETAC Racks: • 24 position, 1.5 mL or 2.0 mL vials • 48 position, 0.5 mL vials • 96 position, 1.0 mL vials Tall – Bel-Art Half Racks: • 30 position, 14 mL vials • 42 position, 7 mL vials C Standards Vials. Up to 14 standards positions are available with the autosampler: Short Tall 9 – 4 mL vials 9 – 10 mL vials 5 – 20 mL vials 5 – 30 mL vials D Dual Flowing Rinse Station. The dual rinse station is located next to the sample tray. It comes with tubing used to connect the rinse station to two separate rinse sources (deionized water pre-rinse and acid full rinse) and the waste container. The rinse station is provided in either a short or tall version to match the rack choice. E Rinse Alignment Block. F Z-Drive Assembly. G Y-Arm Assembly. The Y-arm is attached to the Z-drive assembly in one of two mounting locations depending upon the choice for short or tall function. H Sample Probe. Sample probes are constructed of fluoropolymer tubing reinforced with a carbon fiber or polyimide tube to provide strength and maintain straightness. Available probe sizes include 0.010” (0.25 mm) ID and 0.035” (0.89 mm) ID. If the ASX-112FR is used with the Aridus II, then the uptake line of the C-Flow PFA nebulizer (equipped with a polyimide support tube) is used as the sample probe. I Power Switch. Rocker switch, single pole-single throw, 16 amp. 10
ASX-112FR Autosamplers Operator’s Manual Chapter 1: Introduction J Power/Status LED. Green light should be lit when the power is on and the autosampler is ready to operate. K Cover. The cover door may be opened (using a bar latch) during operation without interrupting the sampling sequence. The following standard components are located on the back of the ASX-112FR and are shipped with the autosampler. Each lettered item corresponds with a callout in either Figure 1-3 or Figure 1-4. Figure 1-3. ASX-112FR Autosampler-Back View Gas Displacement Pump Model. Figure 1-4. ASX-112FR Autosampler-Back View Peristaltic Pump Model. A On-Board Rinse Pump. The on-board rinse pump may be either a peristaltic pump or a gas displacement pump. In either configuration, the pump is 11
ASX-112FR Autosampler Operator’s Manual Chapter 1: Introduction located in the upper right-hand corner on the back of the autosampler. The pump moves the rinse solutions from two rinse sources through the flowing rinse station. B 24VDC Input. The six-pin jack for 24VDC input from the power module. C Auxiliary I/O Port. The auxiliary I/O port detects switch closures or can trigger devices that can be operated from switch closure (TTL) event triggers. It can also be used to control external devices that require +24VDC. An example of such a device is the QuickWash Accessory that can be used with the Aridus II™ Desolvating Nebulizer System. D One RS-232 Serial I/O Port-COM1. The serial port is located in the center of the lower back of the autosampler. The COM1 port is the communications interface between the ASX-112FR and the analytical instrument’s host computer. E USB Option. The ASX-112FR comes standard with a USB port. This port can be used to interface the ASX-112FR with the host computer. F Auxiliary Module Port. The auxiliary module port is included for possible addition of an external device that requires +24VDC. There are two sets of dipswitches located on the bottom of the autosampler. The five-position dipswitch defines normal operating mode or rabbit programming mode. The first three switches of the eight-position dipswitch define the ICP-MS interface and switch #6 controls whether the autosampler functions in the Tall or Short mode: 1 = Tall (Bel-Art racks), 0 = Short (CETAC racks). The following standard components are also shipped with the ASX-112FR: External Desktop Power Supply. The input rating is AC 100V-240V, 1.9 A, with an output of DC 24V, maximum 3.3 A. Serial Interface Kit. The kit includes DB9F port adapters for host computers with normal AT-style DTE serial ports, and a 1.828-meter modular cable. Additional Equipment Required In addition to the provided equipment, you will need: A host computer which has been configured with the ICP-MS software. This computer must have an additional free USB or serial ports beyond the ports required to control the autosampler, spectrometer, and other system components. Optional Accessories If you are doing a specialized type of analysis or are connecting the ASX-112FR to a host computer that uses a non-RS-232 communications protocol, you may need optional accessories in addition to the standard components included with the autosampler. The following accessories are available for the ASX- 112FR: 12
ASX-112FR Autosamplers Operator’s Manual Chapter 1: Introduction IEEE-488 Interface Kit. The kit includes an RS-232/IEEE-488 converter box, an IEEE-488 cable, a power cord, and instructions. It is used to convert an IEEE communications protocol to a serial protocol. C-Flow PFA Nebulizer. The C-Flow Nebulizer is a molded, fixed-capillary style PFA concentric nebulizer for the introduction of low-volume (< 1mL) samples to an ICP-MS. The inert PFA construction allows the introduction of all acids (including hydrofluoric acid), alkalis and organic solvents. It features a standard 6mm diameter tip for easy installation to most spray chambers. QuickWash Fast Washout Accessory. The QuickWash Fast Washout Accessory can be used with the Aridus II™ Desolvating Nebulizer System and the ASX-112FR Autosampler. The ASX-112FR can trigger the QuickWash to begin a rinse cycle for the Aridus II™ PFA spray chamber. Alternate Rinse Height Kit. Alternate rinse kits are available as spares to convert a short configuration into a tall and vice versa. Alternate Sample Rack Kits. Additional rack kits are available as spares to run samples of varying volumes. Alternate Sample Probes. Alternate sample probes are available as spares. NOTE: Contact Teledyne CETAC Technologies if you need additional accessories not listed, need added features to integrate the autosampler into your analytical system, or have unique requirements. Research and development of new features and accessories for the autosampler, often inspired by customer requests, is a continuing activity at Teledyne CETAC Technologies. 13
ASX-112FR Autosampler Operator’s Manual Chapter 1: Introduction Chemical Compatibility Autosampler components are made of Ultra-High Molecular Weight Polyethylene (UHMW-PE) and Polyethylene Terephthalate. The base is made from a high-strength aluminum alloy with an epoxy powder coating finish. The sample racks are made from UHMW-PE or polypropylene and are protected from airborne contaminants and operator interference by a polycarbonate cover. Sample vial choices include PFA and polypropylene. The ASX-112FR operates reliably under a wide variety of conditions. Components in the sample flow path are made of FEP or PFA. When these inert, non-metallic materials are used at temperatures less than 135°C, they can withstand repeated exposure to the following substances: Predominantly aqueous solutions of strong acids (less than 40%) Common organic solvents such as acetone, alcohols, ethyl acetate, Methylethylketone (MEK), petroleum oils and derived fuels, tetrachloroethylene, toluene, kerosene and xylene. CAUTION DAMAGE FROM CHEMICAL EXPOSURE Prolonged or repeated exposure to temperatures greater than 135°C and to the following substances can cause failure of the flow path components: • Solutions of concentrated acids (greater than 40%). • Solutions of concentrated bases (greater than 10% potassium, ammonium, or sodium hydroxides). • Partially halogenated hydrocarbons or extremely aggressive organic solvents (chloroform, methylene dichloride, 1,1,2-trichloroethane). CHEMICAL HAZARD WARNING Do not use the autosampler with substances which could pose a hazard of serious injury to the operator if spilled or injected, such as biological substances or formic acid. Where to Go for More Information In addition to this manual, you can refer to the following resources: New versions of this manual may be available under “Service and Support” on CETAC’s Web site: www.cetac.com ASX-112FR Autosampler Spare Parts Catalog, available on the CD-ROM or under "Parts" on CETAC’s Web site. Teledyne CETAC Technologies Customer Service and Support: Phone: 1 (800) 369-2822 (USA only) 1 (402) 733-2829 Fax: 1 (402) 733-1932 E-mail: custserv@cetac.com The software manual for the ICP-MS instrument you are using. 14
2 Preparing for Installation Installing the autosampler requires preparation. Before you install the autosampler, you should evaluate the physical arrangement of the laboratory to choose a suitable location. Once you choose a location, you must carefully unpack the autosampler prior to beginning the installation. This chapter discusses what requirements must be met when you choose a location. It also describes how to unpack the equipment before installation. Choosing a Location Choosing a location for the autosampler involves evaluating the lab environment for the availability of space, liquid waste routing and power. For the system to function optimally, the location you select must meet specific requirements associated with each of these items. The following sections discuss space, water, and power requirements. Space Requirements Most analytical applications benefit from utilizing the shortest sample flow path. Therefore, you should place the autosampler in close proximity to the analytical instrument. The recommended footprint for the autosampler is shown in the following table. Dimensions Recommended Footprint Height 44 cm (17.3") 55 cm (22") Width 34 cm (13.4") 44 cm (17") Depth 52 cm (20.5") 59 cm (23") Weight 14.1 kg (31 lbs) Table 1: Physical Characteristics – ASX-112FR The weight shown is that of the autosampler itself, without the desktop power supply or other accessories. 15
ASX-112FR Autosampler Operator’s Manual Chapter 2: Preparing for Installation Allow at least 5 cm behind the autosampler for power cord and communication cable egress. Always position the equipment so that it is easy to disconnect the power cord. Work Surface Requirements The ASX-112FR can be conveniently placed on top of the CETAC Aridus II™ Desolvating Nebulizer System. Otherwise, the autosampler must be placed on a sturdy countertop or table. Do not place the autosampler on a wheeled cart or folding table. During operation, the autosampler produces both vertical and horizontal forces. If the work surface is allowed to shake or wobble, the autosampler may “walk” across the surface, liquids may spill, or data quality may be affected. Rinse Solution Requirements For most applications, 2% nitric acid (HNO3) (v/v) is used as the primary rinse agent and deionized water is used as the pre-rinse agent in the ASX-112FR. Place the rinse agent source(s) within two meters of the ASX-112FR. CHEMICAL INHALATION AND BURN HAZARD WARNING Observe all necessary safety precautions when handling nitric acid (HNO 3 ) solutions. Wear appropriate personal protective equipment, including face shield or goggles, gloves, and a laboratory coat, and ensure that engineering controls (such as ventilation systems) are operating properly. Liquid Waste Routing Requirements Ensure that there is a liquid waste receptacle within two meters of the autosampler. The waste receptacle inlet should be 30 to 60 centimeters lower than the autosampler rinse station outlet and set up so that the rinse drain tubing drops directly into the waste receptacle with no coiling and without being submerged below the liquid level of the waste receptacle. CAUTION SUBMERGED DRAIN TUBING MAY CAUSE EQUIPMENT DAMAGE Ensure that the rinse drain tubing is not submerged in the waste liquid. If the tubing is submerged, waste liquid can back up in the rinse station, flooding the sample tray and potentially damaging the electronics. Power Requirements The autosampler is powered by the supplied external desktop "brick" power supply. Place the autosampler within 1.2 meters of a power outlet. SHOCK AND FIRE HAZARD WARNING Use only the provided power supply. The power supply must be plugged into an outlet which has a protective ground connection. The autosampler is intended to operate from DC power supplied through the provided power supply. The power supply is provided power through an AC power source that will not apply more than 240VAC between the supply conductors and ground. A protective ground connection by way of the grounding connector in the power cord is required for safe operation. 16
ASX-112FR Autosamplers Operator’s Manual Chapter 2: Preparing for Installation Ensure that you position the autosampler so that the location where the power supply cord plugs into it is easily accessible (is not blocked) and it can be quickly disconnected if needed. In case of hazard, the autosampler should be disconnected from the power source. The power supply socket is on the back of the autosampler (see Figure 1-4 on page 11). Connect the power supply to the autosampler first and then connect a line cord to the power supply. Do not apply power to the power supply until ready to operate the autosampler. Unpacking the Autosampler LIFTING HAZARD WARNING The autosampler may be awkward to lift. Incorrect lifting technique may cause personal injury. Use caution when lifting the autosampler. Inspect external packaging upon receipt for signs of shipping damage. Inspect all items during unpacking and notify the carrier immediately of any concealed damage. Check for any kinked or bent tubing. If the system is shipped or removed from storage during cold weather, allow the packaged equipment to equilibrate to room temperature before opening and exposing to warm, humid air. It is usually sufficient to provide four to eight hours for this purpose. CAUTION EQUIPMENT DAMAGE FROM CONDENSATION If condensation forms on or inside the autosampler, allow it to dry thoroughly before connecting it to a power source and operating it. Failure to do so may cause equipment damage. Remove the packing checklist from the shipping container, and check off items against it. Leave accessories in the packing until you are ready to install them. NOTE Keep the factory packaging for use in case the product ever needs to be returned or shipped to another location. 17
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3 Installing the Autosampler The autosampler is designed for easy installation. Installation consists of two parts: assembling the autosampler and connecting it to the host analytical instrument. The autosampler can be installed with minimal effort; no tools are required. You can remove thumbscrews with tools if necessary, but do not tighten them with anything other than your fingers. Overview To install the autosampler, you must complete the following tasks. Each of these tasks will be discussed in detail later in this chapter. Mount the sample probe assembly. Connect the rinse station. Assemble and place the sample racks and standards vials. Establish external connections. Connect the ASX-112FR autosampler to the host computer. Ensure the power switch is off and the power cord is unplugged before WARNING proceeding with installation. If the power is left on, motors may move unexpectedly and cause injury. 19
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Mounting the Sample Probe Assembly Mounting the sample probe assembly on the autosampler is the first task in assembling the ASX-112FR. However, prior to mounting the probe, the installation of the Y-arm should be confirmed to be compatible with the height of the racks intended for use. Figure 3-1 shows three sets of mounting holes provided for height options for the Y-arm. If the autosampler is intended to run with half Bel-Art racks and tall standards in the tall configuration, make sure the Y-arm is mounted in the top most mounting location. If the autosampler is intended to run with the CETAC short racks and short standards in the short configuration, make sure the Y-arm is mounted in the lowest mounting position. The center mounting position may also be used for the desired probe Z-axis travel. Figure 3-1. Y-Arm Mounting Positions. 20
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-2. Sample Probe Assembly Installation. Figure 3-2 illustrates the sample probe assembly installation. The instructions below can be used for the standard probe or the uptake capillary of the C-Flow PFA nebulizer. 1 Insert the probe into the Y-arm assembly and loosely tighten the thumbscrew on the front of the arm, leaving the probe set high until the position is checked. 2 If the C-Flow PFA nebulizer is to be used, secure the uptake line of the nebulizer at the top of the built-in probe. 3 Loosen the thumbscrew of the tubing holder block on the front left of the autosampler. 4 Carefully slide the probe tubing into the holder block groove and gently tighten the thumbscrew. 5 Attach the end of the standard probe to the nebulizer. If using the C-Flow PFA nebulizer, insert the end of the C-Flow into the Aridus II™ PFA spray chamber. See Figure 3-3. 21
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-3. Connection of C-Flow PFA Nebulizer to Aridus™ II. See the CETAC Aridus II™ Desolvating Nebulizer System Operator's Manual for more information on connecting the probe and nebulizer. Connecting the Rinse Station The cabinet-mounted rinse station is located at the left-front side of the autosampler within the cover. The ASX-112FR provides the ability to use two separate rinse solutions in a dual flowing rinse station as shown in Figure 3-4. Typically, deionized water is used as a pre-rinse solution and an acid solution, such as 2% HNO3, is used as the primary rinse solution. The dual flowing rinse solutions may be pumped into the rinse station by either an on-board peristaltic pump or with a gas displacement pump. 22
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-4. Dual Flowing Rinse Station. The rinse solutions are pumped into the rinse station through two ports at the bottom of the rinse station and are drained from the top of the rinse station. This up-flow rinsing is the most effective method for decontaminating the sample probe between samples. The waste rinse solutions drain from the top of the rinse station by gravity; it is therefore necessary to ensure the drain tube hangs straight and is unhindered in its path to the waste container. Peristaltic Pump Configuration In the gravity drain arrangement, the rinse solution moves through both channels of the peristaltic pump to the dual inlets at the bottom of the rinse station. It then drains out a single gravity drain at the top of the rinse station. The rinse speed of the peristaltic pump is configurable through ICP-MS command only. If the ICP-MS does not have a command action to alter the pump speed, the speed cannot be changed. Smaller diameter pump tubing is available to enable lower rinse solution flow rates. This tubing (Tygon®) is available in spare part kit SP7296. To connect the rinse station tubing to the rinse station, complete the following steps: 1 Remove the two thumbscrews that secure the rinse station and then remove the rinse station from the autosampler by gently pulling it away from the support guide posts. 2 Use two lengths of approximately 28 inches (72 centimeters) of the 1/8 inch (3-millimeter) I.D. Tygon® tubing provided for the rinse solution uptake. Insert one section of tubing onto each of the two lower fittings for the pre- rinse and main rinse inputs on the back of the rinse station as noted in Figure 3-5. 23
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler 3 Use one length of approximately 72 inches (1.8 meters) of the 3/16 inch (5- millimeter) I.D. Tygon® tubing provided for the rinse station drain. Insert one end into the upper drain fitting on the back of the rinse station as noted in Figure 3-5. Insert the tubing carefully because the rinse station fitting grips the tubing tightly. If you apply too much force, the fitting can break off. The 5-millimeter Tygon® tubing may need to be stretched slightly on the end to allow insertion over the drain fitting. 4 Replace the rinse station on the autosampler. First, thread the tubing through the guide holes on the rinse alignment block out the side of the unit. Then, align the guide posts on the rinse station with the alignment block and carefully push the rinse station into place. Ensure the rinse station is mounted tightly against the alignment block to ensure no rinse misalignment problems. Figure 3-5. Peristaltic Pump Tubing Connections. To connect the rinse station tubing to the peristaltic pump using a gravity drain, complete the following steps: 1 Rinse In – Use two lengths of approximately 72 inches (1.8 meters) each of the 1/8 inch (3-millimeter) I.D. Tygon® tubing. Insert one end of each length of tubing onto the two inlets at the top of the pump. Place the other end of each length of tubing into the two rinse solution sources. Two 2-liter polypropylene bottles with connections, PTFE tubing, and vent ports are provided for the rinse solutions. 2 Rinse Out - Connect the peristaltic pump to the rinse station by completing the following steps: a) Take the free end of the Tygon® tubing protruding through the alignment block from the lower rinse station input and insert it onto the inside channel fitting on the bottom of the peristaltic pump as shown in Figure 3-5. 24
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler b) Take the free end of the Tygon® tubing protruding from middle rinse station input and insert it onto the outside channel fitting on the bottom of the peristaltic pump as shown in Figure 3-5. Insert the tubing carefully because the peristaltic pump fitting grips the tubing tightly. If you apply too much force, the fitting can break off. 3 Drain - Connect the rinse station to the waste container by placing the free end of the 3/16 inch (5-millimeter) I.D. Tygon® tubing protruding from the rinse station outlet (on top) into a waste container. Ensure that the waste container is at least 30 to 60 centimeters lower than the rinse station outlet. Ensure that the tubing outlet is placed in the waste container so that it will not be immersed in the waste solution. Immersion of the drain tube outlet may cause the waste solution to back up and overflow. The drain tubing may be cut to an appropriate length. CAUTION SUBMERGED DRAIN TUBING MAY CAUSE EQUIPMENT DAMAGE Ensure that the rinse drain tubing is not submerged in the waste liquid. If the tubing is submerged, waste liquid can back up in the rinse station, flooding the sample tray and potentially damaging the electronics. Gas Displacement Pump Configuration In the gas displacement pump arrangement, the rinse solutions are pushed by gas pressure through the dual inlets at the bottom of the rinse station. Excess rinse solution drains at the top of the rinse station. The gas displacement pump pressure can be adjusted with the flow adjustment knob on the gas displacement pump panel. Pressure is adjustable from 0 to 5 psi. Higher pressure results in a faster rinse speed. CHEMICAL SPRAY HAZARD WARNING Tighten the fittings "finger-tight." Do not use any tool other than your fingers to tighten the fittings. If the fitting is too loose, the tubing can leak or come out of the fitting. If the fitting is too tight, the tubing and seats will deform and leak. To connect the rinse station tubing to the rinse station, complete the following steps: 1 Remove the two thumbscrews that secure the rinse station and then remove the rinse station from the autosampler by gently pulling it away from the support guide posts. 2 Use two lengths of approximately 28 inches (72 centimeters) of the 0.020 inch (0.5-millimeter) PFA tubing provided for the rinse solution uptake. Insert one section of tubing onto each of the two lower fittings for the pre-rinse and main rinse inputs on the side of the rinse station as noted in Figure 3-4 and Figure 3-6. Nuts and ferrules are supplied to attach the PFA-tubing. Apply gentle pressure to the tubing while tightening the fittings. The fittings should be as tight as you can get them using just your fingers. 25
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler 3 Use one length of approximately 72 inches (1.8 meters) of the 3/16 inch (5- millimeter) I.D. Tygon® tubing provided for the rinse drain. Insert one end into the upper drain fitting on the back of the rinse station as noted in Figure 3-4 and Figure 3-6. Insert the tubing carefully because the rinse station fitting grips the tubing tightly. If you apply too much force, the fittings can break off. The 5-millimeter Tygon® tubing may need to be stretched slightly on the end to allow insertion over the drain fitting. 4 Replace the rinse station on the unit. First, thread the tubing through the guide holes on the rinse alignment block out the side of the unit. Then, align the guide posts on the rinse station with the alignment block and carefully push the rinse station into place. Ensure the rinse station is mounted tightly against the alignment block to ensure no rinse misalignment problems. Finally, reattach the two thumbscrews to secure the rinse station. Argon Gas Supply for Gas Displacement Pump To connect the rinse station tubing to the gas displacement pump using a gravity drain, complete the following steps with reference to Figure 3-6 and Figure 3-7: 1 Two PFA bottles are provided for the rinse solutions. After filling each bottle with the appropriate rinse solution, ensure that the caps for each bottle are secure. A dedicated wrench (green color) is provided to tighten the caps. Label the bottles #1 and #2; fill bottle #1 with pre-rinse solution (ex. deionized water) and bottle #2 with full rinse solution (ex. 2% nitric acid). 2 Rinse Bottle to Rinse In Ports – Use two lengths of approximately 48 inches (1.2 meters) each of 1/8 inch O.D. x 1/16 inch I.D. PTFE tubing. Attach one end of each length of tubing into the two “RINSE IN” ports on the gas displacement pump panel. Use the fittings and ferrules provided. Place the other end of each length of tubing into a fitting on the top of the cap of each PFA bottle. The tubing should extend through the fitting and into the rinse solution. If the tubing will not go through the fitting, then try the other fitting. “RINSE 1 IN” should be connected to bottle#1 with the pre-rinse solution and “RINSE 2 IN” should be connected to bottle#2 with the full rinse solution. Ensure that each fitting is tight. 3 Argon Out to Rinse Bottle – Use two lengths of approximately 48 inches (1.2 meters) each of 1/8 inch O.D. x 1/16 inch I.D. PTFE tubing. Note that this tubing will have pressure relief valves already attached. Attach one end of each length of tubing into the two “Argon Out” ports on the gas displacement pump panel. Use the fittings and ferrules provided. Place the other end of each length of tubing into the other fitting on the top of the cap of each PFA bottle. Note that the tubing should only extend to the bottom of the fitting and not below the level of the liquid in the bottle. The “ARGON OUT” connection below the “RINSE 1 IN” port should be connected to bottle#1 with the pre-rinse solution. The “ARGON OUT” connection below the “RINSE 2 IN” should be connected to bottle#2 with the full rinse solution. Ensure that each fitting is tight. 26
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler 4 Rinse Solution Out – Connect the gas displacement pump to the rinse station by completing the following steps: a) Take the free end of the PFA tubing (0.5 mm I.D.) protruding through the alignment block from the lower rinse station and connect it to the “RINSE 1 OUT” port on the gas displacement pump panel. Use the fittings and ferrules provided. b) Take the free end of the PFA tubing (0.5 mm I.D.) protruding through the alignment block from the middle rinse station and connect it to the “RINSE 2 OUT” port on the gas displacement pump panel. Use the fittings and ferrules provided. 5 Drain- Place the free end of the 3/16 inch (5 mm) I.D. Tygon® tubing protruding from the rinse station outlet (top of rinse station) into an appropriate waste container. Ensure that the waste container is at least 30 to 60 centimeters lower than the rinse station outlet. Ensure that the drain tubing is placed in the waste container so the tubing will not be immersed into the waste solution. Immersion of the drain tubing into the waste solution may cause the solution to back up into the rinse station and overflow. CAUTION SUBMERGED DRAIN TUBING MAY CAUSE EQUIPMENT DAMAGE Ensure that the rinse drain tubing is not submerged in the waste liquid. If the tubing is submerged, waste liquid can back up in the rinse station, flooding the sample tray and potentially damaging the electronics. 6 Argon Gas Supply – Connect the argon gas supply to the “ARGON SUPPLY” inlet on the gas displacement pump panel. The argon gas supply can be from a dedicated argon source or from the ICP-MS argon supply. The recommended argon inlet pressure is 50 psi (350 kPa or 3.44 bar). If the AridusII nebulizer system is being used, the argon can be teed from the AridusII sweep gas supply. See Figure 3-8 for such an argon gas connection. 27
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-6. Gas Displacement Pump Tubing Connections. 28
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-7. Gas Displacement Pump Fitting Connections. 29
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Figure 3-8. Gas Displacement Pump Argon Gas Connection with Aridus II. 30
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Assemble and Place the Sample Rack and Vials Never attempt to load, unload or reposition the sample vial rack or sample WARNING vials while the autosampler is operating. The sample probe may move unexpectedly and cause an injury. Figure 3-9. ASX-112FR Autosampler Rotary Tray The ASX-112FR features a rotary tray, shown in Figure 3-9, which holds both standards and samples. A variety of sample racks can be placed within the center cavity of the rotary tray. Sample racks are classified as short or tall, allowing the ASX-112FR to be configured in either a short or tall configuration. Standards vials also vary between the short and tall configurations. For the short configuration, standard positions 1 through 5 hold 20 mL vials and standard positions 6 through 14 hold 4 mL vials. For the tall configuration, standard positions 1 through 5 hold 30 mL vials and standard positions 6 through 14 hold 10 mL vials. Short Rack Configuration Figure 3-10. CETAC Sample Racks – Short Rack. 31
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Three CETAC sample racks are available for the short configuration. These are shown in Figure 3-10. To assemble and place the samples and standards for a short configuration, complete the following steps: 1 Ensure the short sample tray adapter plate is screwed into place in the center of the rotary tray. It should be placed so that the alignment guide is placed nearest the guide dot as shown in Figure 3-9. An ASX-112FR ordered in a short configuration will be shipped with the adapter plate in place. 2 Place the standards vials in the rotary tray as shown in Figure 3-9. 3 Load the sample vials in the sample tray and place the tray in the center of the rotary tray aligning the groove on the bottom of the tray with the alignment guide on the adapter plate. This should also align the two alignment dots on the corner of the sample tray and the rotary tray. A correctly placed sample vial rack will not move more than ± 0.2 millimeters unless lifted. A tilted sample vial rack or vials indicate an improperly placed rack or vials, which must be corrected before you operate the autosampler. 4 Replace the autosampler cover by sliding it into the groove in the rinse alignment block. The cover on the ASX-112FR has a hinged front door, secured by a bar latch, which can be opened and closed during operation without impacting the sampling sequence. The entire cover itself can also be fully removed during operation without impact to the sampling sequence; however, this is not recommended as the removal act could result in an impact to the Y-arm assembly causing an alignment error. In the case of a mechanically induced alignment error, the power to the unit would need to be cycled off and on to realign the Y-arm. Tall Rack Configuration 30 42 Figure 3-11. Bel-Art Sample Racks. 32
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Two half Bel-Art racks are provided for the tall configuration. The tray layouts are shown in Figure 3-11. To assemble and place the samples and standards for a tall configuration, complete the following steps: 1 Assemble the Bel-Art rack by snapping the middle and top sections to the bottom according to the instructions included with the rack. 2 Ensure the short sample tray adapter plate is not screwed into place in the center of the rotary tray. An ASX-112FR ordered in a tall configuration will be shipped without the adapter plate in place. 3 Place the standards in the rotary tray as shown in Figure 3-9. 4 Load the sample vials in the sample tray and place the tray in the center of the rotary tray. A correctly placed sample rack will not move more than ±0.2 millimeters (mm) unless lifted. A tilted sample vial rack or vials indicate an improperly placed rack or vials, which must be corrected before you operate the autosampler. 5 Replace the autosampler cover by sliding it into the groove in the rinse alignment block. The cover on the ASX-112FR has a hinged door, secured by a bar latch, which can be opened and closed during operation without impacting the sampling sequence. The entire cover itself can also be fully removed during operation without impact to the sampling sequence; however, this is not recommended as the removal act could result in an impact to the Y-Arm assembly causing an alignment error. In the case of a mechanically induced alignment error, the power to the unit would need to be cycled off and on to realign the Y-arm. 33
ASX-112FR Autosampler Operator’s Manual Chapter 3: Installing the Autosampler Connecting the Autosampler to the Power Supply The autosampler is powered by the supplied external desktop "brick" power supply. Ensure that you position the autosampler so that the location where the power supply cord plugs into it is easily accessible (is not blocked) and it can be quickly disconnected if needed. In case of hazard, the system should be disconnected from the power source. 1 Turn the power switch on the autosampler OFF. 2 Check the plug on the power cord to verify that it is of the correct type for your country. 3 Plug the power cord into a power outlet. 4 Plug the power cord into the power supply. Power Cord to Grounded AC Power Outlet To POWER Connector on Autosampler Figure 3-12 Desktop "Brick" Power Supply 5 Plug the power supply into the 24V connector on back of the autosampler. 6 Turn the power switch on the front of the autosampler ON. It is important to use the appropriate power cord for your country. See “Power requirements” on page 76. “Power Cord Set Requirements” on page 77. FIRE AND SHOCK HAZARD WARNING Use only the provided desktop power supply. The power supply must be plugged into an outlet which has a protective ground connection. 34
ASX-112FR Autosamplers Operator’s Manual Chapter 3: Installing the Autosampler Connecting the Autosampler to an Analytical Instrument You can connect the autosampler directly to a sample introduction peristaltic pump and then to the ICP-MS or to a sample introduction device, such as the CETAC Aridus II™ Desolvating Nebulizer System. To do so, complete the following steps: 1 Determine the free length of the sample probe tubing you need, add 10 centimeters, and cut the free end of the sample probe to length. Determining the free length includes allowance for movement of the Y-arm in the X, Y, and Z axes. The additional 10 centimeters provides a service loop for unrestricted sample probe motion. Excessively shortened sample probe tubing is not repairable and must be replaced. 2 Connect the free end of the sample transfer tubing to the inlet of the analytical instrument’s peristaltic pump tubing. The free end may be connected directly to the ICP-MS nebulizer. If the CETAC C-Flow PFA nebulizer is used (the free end acting as the sample probe for the ASX-112FR) then the nebulizer may be installed directly into the Aridus II™ PFA spray chamber or the host ICP-MS spray chamber. Connect the ASX-112FR Autosampler to the Host Computer Instrument control software on the ICP-MS host computer controls both the analytical instrument and the autosampler. You cannot operate the autosampler until you establish a communications interface between the autosampler and the host computer. It is through this interface that the host computer directs the operation of the autosampler. The autosampler supports the following communications protocols: The serial (RS-232) protocol is the standard configuration. There are two RS-232 serial ports on the autosampler, and a serial interface kit is shipped with the autosampler. The parallel (IEEE-488) protocol is less common than the serial configuration. An IEEE-488 interface kit is available as an optional accessory to the ASX-112FR. The USB interface is an optional configuration. A virtual COM port is created when using the USB and therefore, the connection looks like a standard RS-232 serial port to the host PC software. NOTE: Although the autosampler supports several communications protocols, the host computer governs which protocol is used. To determine which protocol is 35
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