Aridus3 Desolvating Nebulizer System

Transcription

1 Aridus3 Desolvating Nebulizer System Operator s Manual Manual Part Number Rev 0

2 COPYRIGHT Teledyne Technologies Incorporated. All rights reserved Rev 0, October 25, 2017 Teledyne CETAC Technologies authorizes its customers to reproduce, transmit, or store this document in its entirety, including this page, for the express purpose of installing, operating, or maintaining the product described herein. TRADEMARK ACKNOWLEDGEMENTS Windows is a registered trademark of Microsoft Corporation in the United States and other countries. All other marks are the property of their respective owners. Teledyne CETAC Technologies Customer Service & Support Industrial Road Omaha, Nebraska 68144, USA Phone (800) (USA only) Phone (402) Fax (402) cetacservice@teledyne.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 improve products described herein at any time without notice or obligation.

3 Contents 1 Introduction...7 About This Book... 8 Aridus3 System Overview... 8 Aridus3 Specifications... 9 Sample Compatibility...10 Where to Go for More Information Preparing for Installation Choosing a Location...11 Space Requirements...11 Power Requirements...11 Environmental Requirements...12 ICP-MS Requirements...12 Gas Requirements...13 Unpacking the Aridus Aridus3 Packaging Installing the Aridus Installing the Membrane Desolvator Module...15 Establishing External Connections...17 Connecting the Aridus3 to the Power Source...17 Connecting the Aridus3 to the ICP-MS...18 Connecting the Aridus3 Drain Tubing...22 Installing the Spray Chamber in the Aridus Connecting the Nebulizer to the Aridus Connecting the Aridus3 to the Host Computer...26 Using a USB To Serial Adapter...27 Setting Up the 4-Liter Trap Bottle...28 Summary View of Connections to the Back Panel of the Aridus Using the ASX-112FR Autosampler With the Aridus Connecting the Aridus3 C-Flow PFA Nebulizer to an ASX-112R Autosampler Verifying Installation Installing the Aridus Link Software...33 Initial Operating Procedure...37 Temperature and Gas Flow Ranges...39 Range of Conditions (Gas Flows and Temperatures)...39 Allowed Ranges of Aridus3 Gas Flows and Temperatures...39 ICP-MS Operation...40 System Optimization...40 Aridus3 Optimization Procedure Using the Aridus3 Desolvating Nebulizer System Establishing Optimal Operating Conditions...43 Establishing the Lab Environment...43 Replacing Aridus3 Components

4 Contents Sample Transfer Line: FEP-Lined PVC Tubing Peristaltic Pump Tubing of the Host ICP-MS Instrument Startup Procedure...44 Shutdown Procedure...45 Monitoring the Temperature and Gas Flows...45 Switching from Organic Samples to Aqueous Samples and Aqueous Samples to Organic Samples...46 Moving the Aridus Using the Aridus Link Software...49 Initial Startup of Aridus Link Software...49 Using the ICP Ignition Tool...51 Adjusting the Aridus3 Gas Flows and Temperatures...52 Saving an Aridus3 Parameter Setting...53 Aridus Link Software Tools Collapse Screen...54 Aridus Link Software Tools Pressure Units...55 FlowSaver Software Tool Installing the QuickWash3 Fast Washout Accessory...59 Why Spray Chamber Cleaning Is Needed How the QuickWash3 Accessory Works How the QuickWash3 Accessor Is Controlled Equipment Supplied With the QuickWash3 Accessory...61 Installing the QuickWash3Accessory...61 Summary of QuickWash3 Liquid Flows...65 Controlling the QuickWash3 Through the Aridus Link Software (Manual Control)...66 Controlling the QuickWash3 Via the ASX-112FR Autosampler (Automated Control)...67 Connecting the Control Cable Operating the QuickWash3 Automatically Important Notes for Operation of the QuickWash QuickWash3 Specifications Maintaining the Aridus Cleaning the Aridus External Cleaning Internal Cleaning Maintaining the Nebulizer and Spray Chamber...74 Cleaning the Nebulizer Removing the PFA Spray Chamber Disassembling the PFA Spray Chamber Backflushing the C-Flow PFA Nebulizer...76 Main Fuse Replacement...77 Spray Chamber and Desolvator Fuse Replacement...78 Rinse Procedure for the Membrane Desolvator...79 Removing and Rinsing the Membrane Desolvator...80 Rinsing the Membrane Desolvator Module and PFA Spray Chamber Installed in Aridus Removing the Top Cover Troubleshooting the Aridus Communication Problems

5 Contents Temperature Control Problems...90 The PFA spray chamber does not heat up...90 The membrane desolvator oven does not heat up...91 Mass Flow Controller Problems...93 There is no control or intermittent control via the Aridus Link software of the Ar sweep gas flow and/or the N 2 addition gas flow...93 Argon sweep gas mass flow controller (MFC) will not provide a reading of at least 4.00 L/min Ar or reading is unstable...94 Nitrogen addition gas mass flow controller (MFC) will not provide a reading of at least 10.0 ml/min of N 2 flow or flow is unstable...94 Nebulizer / Plasma Problems...94 Poor and/or unstable aerosol generation...94 Sample flow rate problems...95 Poor precision...95 High elemental oxide levels...96 Excessive nitrogen-containing polyatomic ion interferences...96 Nebulizer self-aspiration stops...96 Plasma Problems...96 Plasma flickers excessively or is unstable...96 Autosampler Communications Interface Problems...96 RS-232 Serial Cable Problems...97 ASX-112FR Firmware Setting...97 Returning the Product to CETAC for Service...97 Shipping the Product...97 Product Warranty Statement...98 Returned Product Procedures...99 Returned Product Warranty Determination Safety and Regulatory Information Safety Characteristics Environmental Characteristics Electrical Characteristics Safety Notices Power Cord Set Requirements and Maintenance Mains Disconnect Operating Environment Explanation of Caution and Warning Notices Electromagnetic Interference Explanation of Regulatory Marks Glossary

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7 1 Introduction The Aridus3 desolvating nebulizer system is designed primarily for ICP mass spectrometry. The Aridus3 incorporates a C-Flow PFA (perfluoroalkoxy) microconcentric nebulizer, which provides low sample flow rates (approximately 50, 100, or 200 microliters/min.). The nebulizer is constructed entirely of inert materials and is suited for use with acidic and alkaline solutions. Solutions may contain nitric acid (HNO 3), hydrochloric acid (HCl), hydrofluoric acid (HF), or ammonium hydroxide (NH 4OH). Sensitivity is improved with the Aridus3 system by enhancing analyte transport efficiency and reducing solvent loading to the plasma. With conventional pneumatic nebulization, injected water vapor causes oxide and hydride polyatomic ion interferences in ICP-MS; organic solvent vapor loading causes carbide polyatomic ion interferences as well as plasma instability and carbon deposition on ICP-MS sampling cones. Using the Aridus3 system for sample introduction greatly reduces these problems. It is strongly noted that the degree of sensitivity enhancement is dependent on the type of ICP-MS used and the area of application. Functionally, liquid sample is nebulized into a PFA spray chamber using a C-Flow PFA microconcentric nebulizer operating at a sample uptake rate of approximately 100 µl/min and an argon nebulizer gas flow rate of 0.7 to 1.1 L/min. The spray chamber is heated to help reduce the formation of solvent droplets inside the spray chamber. The spray chamber is also drained by the host ICP-MS peristaltic pump. The nebulizer gas flow then transports the aerosol from the spray chamber to a heated inert fluoropolymer tubular membrane. Solvent vapor passes through the membrane and is removed by an exterior flow of Ar gas (sweep gas). Analyte continues through the middle of the membrane tube to the ICP-MS instrument. An external view of the Aridus3 desolvating nebulizer system is shown in FIGURE

8 About This Book This document describes the procedures for installing, using, and maintaining the nebulizer system. This manual covers the following products: Teledyne CETAC Aridus3 desolvating nebulizer system WARNING CHEMICAL INJURY HAZARD The Aridus3 desolvating nebulizer system 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. Aridus3 System Overview FIGURE 1-1. Aridus3 Desolvating Nebulizer System. 8

9 Chapter 1: Introduction The following standard components/accessories are included with each Aridus3 system: ICP-MS interface kit: All parts to interface to the operator s ICP-MS, including torch adapter, fittings, and tubing. Aridus3 completion kit: Includes tubing for Ar and N 2 gas supply, 4 L trap bottle, serial cable, USB-to-serial adapter, and software CD. Rinse kit: Contains membrane rinse accessories and a tubing kit that connects to the necessary ports. Spare fuse kit: Contains replacement fuses for the Aridus3. Gas-line tubing kit: Contains all the necessary tubing to interface the argon sweep gas and nitrogen addition gas to the Aridus3. C-Flow PFA nebulizer: One low-flow microconcentric nebulizer. A 100 microliter/min nebulizer is standard. A 50 microliter/min or a 200 microliter/min nebulizer are also available. NOTE: Contact Teledyne CETAC Technologies if you need additional accessories or added features to integrate the Aridus3 with your analytical system or if your laboratory has unique requirements. Research and development of new features and accessories for the Aridus3, often inspired by customer requests, is a continuing activity of Teledyne CETAC Technologies. Aridus3 Specifications Nebulizer: C-Flow PFA; 50, 100 or 200 µl/min Inert Desolvating Membrane: Ar Sweep Gas: 0 to L/min Nitrogen Gas: 0 to 50.0 ml/min Input Pressure (Ar and N 2): 75 to 125 psi (5.2 to 8.6 bar) Membrane Oven Temperature: 140 C (factory default setting), adjustable 80 C to 180 C Spray Chamber: PFA with pumped drain Spray Chamber Temperature: 110 C Voltage (Switch-Selectable): 120 VAC +/- 10%, 50/60 Hz, 6A 220 VAC +/- 10%, 50/60 Hz, 3A Dimensions (Without Autosampler): 33.7 cm W x 19.2 cm H x 52.0 cm D (13.3 in W x 7.6 in H x 20.5 in D) Weight: 11.8 kg (26 lbs) 9

10 Computer Requirements: Microsoft Windows 7 or Windows 10 operating system (32-bit or 64-bit) Microsoft.NET Framework 4.6 (included on CD or with Windows 10) 2 GB RAM (minimum) 1 available serial or USB port Sample Compatibility The Aridus3 may be used with aqueous or organic samples. Analysis of samples containing less than 1% of dissolved solids is recommended. Best performance will be achieved with 0.1% to 0.5% dissolved solids. Solvents should have a boiling point below 160 C. If solvents are analyzed which have a boiling point greater than 160 C, the solvents will not be efficiently removed from the membrane and will require that the membrane be rinsed and the Aridus3 re-optimized. 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 on Teledyne CETAC s website: Teledyne CETAC Technologies Customer Service and Support: Phone: 1 (800) (USA only) 1 (402) Fax: 1 (402) cetacservice@teledyne.com The software and hardware manuals for the ICP-MS instrument you are using. 10

11 2 Preparing for Installation Before you install the Aridus3 desolvating nebulizer system, you should evaluate the physical arrangement of the laboratory to choose a suitable location. Once you choose a location, you must carefully unpack the system prior to beginning the installation. Choosing a Location Choosing a location for the Aridus3 involves evaluating the laboratory environment for the availability of space and power. For the Aridus3 to function optimally, the location you select must meet specific requirements associated with each of these items. The following sections discuss space and power requirements. Space Requirements Most analytical applications benefit from the shortest sample flow path. A one meter length of FEP lined PVC tubing is provided to connect the Aridus3 to the ICP-MS torch. Place the Aridus3 sample out port less than one meter from the ICP-MS torch. The system without the ASX-112FR autosampler is 33.7 cm x 19.2 cm x 52.0 cm (W x H x D). Adequate space should be allowed for proper ventilation. Power Requirements Place the Aridus3 within 1.2 meters of the power outlet. The Aridus3 is provided with a voltage selection switch on the back panel. The voltage may be selected as either VAC ± 10%, 50/60 Hz, 6A or VAC ± 10%, 50/60 Hz, 3A. See FIGURE

12 FIGURE 2-1. Voltage Selection Switch WARNING SHOCK AND FIRE HAZARD The system must be plugged into an outlet which has a protective ground connection. Ensure that you position the system so that the power cord connector is easily accessible (is not blocked), so the cord can be quickly disconnected if needed. In case of hazard, the system should be disconnected from the power source. Do not apply power until ready to operate the system. Environmental Requirements To create satisfactory operating conditions in your lab environment, follow these guidelines: Operate the Aridus3 in a conventional lab environment where the temperature is F (10 30 C); the humidity is 20 70% non-condensing; and the unit is not exposed to excessive flammable or corrosive materials. Avoid rough handling. Do not expose the Aridus3 to vibration or shock. Protect the Aridus3 from long-term exposure to condensation, corrosive materials, solvent vapor, standing liquids, or liquid spills into the electronics. Observe the same general electrostatic discharge precautions as with any other integrated circuit electronic devices. Low humidity environments, especially when combined with static-generating materials, require maximum care. ICP-MS Requirements To achieve optimum performance with the Aridus3, the ICP-MS system must meet factory specifications from your vendor and be in good operating condition. Check the ICP-MS performance using the standard sample 12

13 Chapter 2: Preparing for Installation introduction system before Aridus3 installation. If the sensitivity, oxide ratios and overall performance do not meet instrument specifications, consult the ICP-MS Operator s Manual. If ICP-MS performance specifications are met, then begin installation of the Aridus3 system. In order for the C-Flow PFA nebulizer to properly self-aspirate, a minimum argon gas pressure of 520 kpa (75 psig, 5.2 bar) is recommended in the nebulizer gas line. Ensure that the Ar gas supply for the C-Flow PFA nebulizer is from a known, good supply. The argon nebulizer gas supply from the host ICP-MS is typically used for the C-Flow nebulizer. Gas Requirements The argon gas supply for the Aridus3 sweep gas may be teed in from the main ICP-MS instrument argon gas supply. Nitrogen gas must be supplied from an external source at a pressure of at least 520 kpa (75 psig, 5.2 bar). Nitrogen with a minimum purity of % should be used. The gas pressure for both the argon and nitrogen should be in a range of 520 kpa to 860 kpa (75 to 125 psi, 5.2 to 8.6 bar). Unpacking the Aridus3 Inspect external packaging upon receipt for signs of physical damage from rough handling or abuse during shipment. Inspect all items during unpacking and notify the carrier immediately of any visible or concealed damage. Remove packing checklist from the shipping container, and check off items against it. Leave accessories in the packing until you are ready to install them on the Aridus3. Aridus3 Packaging The Aridus3 system may be shipped in several containers: One container holds the Aridus3 desolvating nebulizer system, the membrane desolvator module (oven), the 4 L trap bottle, the ICP-MS interface kit, and the Aridus3 completion kit. A separate container holds the ASX-112FR autosampler, if ordered. A separate container holds the QuickWash3 fast washout accessory, if ordered. 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. 13

14 NOTICE EQUIPMENT DAMAGE FROM CONDENSATION If condensation forms on or inside the Aridus3, allow it to dry thoroughly before connecting it to a power source and operating it. Failure to do so may cause equipment damage. NOTE Keep the factory packaging in case the product ever needs to be returned or shipped to another location. 14

15 3 Installing the Aridus3 To install the Aridus3, you must complete the tasks described in this chapter. WARNING Ensure that the AC power is off (0 showing at the bottom edge of the power switch) on the back of the Aridus3 before proceeding with installation. Installing the Membrane Desolvator Module The membrane desolvator module (often called the oven ) is shipped as a separate item with the Aridus3. 1 Locate the module and remove the protective packaging. FIGURE 3-1. Membrane Desolvator Module. 15

16 2 The module is designed to insert directly into the large rectangular port on the back panel of the Aridus3. Position the module as shown in FIGURE 3-2. FIGURE 3-2. Position of Membrane Desolvator Module. 3 Insert the module into the Aridus3 chassis and press it in past the first resistance. Note that there are two O-rings which help seal two connection stems. FIGURE 3-3. Inserting Membrane Desolvator Module Into Aridus3. 16

17 Chapter 3: Installing the Aridus3 4 The support panel of the membrane desolvator module should be flush (even) with the back panel of the Aridus3. The 5/32 hex wrench can be used to lock the module in place. FIGURE 3-4. Locking Membrane Desolvator Module In Place. Establishing External Connections The first step in the installation process involves connecting the Aridus3 to the power source and to the ICP-MS instrument. The following sections explain how to establish these connections. Connecting the Aridus3 to the Power Source Voltage-specified power cords are supplied with each Aridus3. If you need a different power cord, contact Teledyne CETAC Technologies. WARNING Use only the provided power cord or an exact replacement. NOTICE Ensure that the Aridus3 voltage selection switches are set to the correct voltage. If the wrong voltage is selected, damage to the Aridus3 may occur. See FIGURE 2-1 on page 12. To connect the Aridus3 to a power source, plug the cord into the power module located on the back panel of the Aridus3. Then plug the cord into an appropriate AC outlet (110 or 220 VAC ± 10%, 50/60 Hz depending on the voltage selection). See FIGURE

18 FIGURE 3-5. Connecting the Power Cord. Connecting the Aridus3 to the ICP-MS Depending on the ICP-MS model, a torch adapter is supplied for interfacing the Aridus3 sample out tubing to the ICP-MS torch. Adapters are available for all ICP-MS instruments. 1 A length of ¼" O.D. FEP (fluorinated ethylene propylene)-lined PVC tubing is connected to the torch adapter. Connect the other end of this tubing onto to the SAMPLE OUT port located on the back panel of the Aridus3. This tubing end will be equipped with a threaded nut and ferrules for attachment to the threaded SAMPLE OUT port. The threaded nut with ferrules should only be finger-tightened onto the SAMPLE OUT port. See FIGURE 3-6. FIGURE 3-6. Connecting the SAMPLE OUT Line. 18

19 Chapter 3: Installing the Aridus3 NOTICE Make certain that the FEP lining in the sample out tubing is not blocking the sample aerosol path to the ICP-MS torch. This can result in instability and loss of analyte signal from the ICP-MS instrument. 2 Attach the other end of the sample out tubing, containing the torch adapter, to the ICP-MS torch/injector (FIGURE 3-7). Note that FIGURE 3-7 depicts the attachment of the standard 12/5 glass joint. While this is a common type of interface, the interface for the operator s specific ICP-MS torch may be different. FIGURE 3-7. Connecting a Torch Adapter to the ICP-MS Torch. 3 The rinse port on the back panel of the Aridus3 is supplied with a threaded plug fitting installed. The rinse port should remain plugged except during cleaning / rinsing of the membrane desolvator. 4 Place the 4 liter trap bottle on the floor, below the level of the Aridus3. If possible, place the bottle against a metal post so that the attached magnets help hold the bottle in place. NOTICE Do not add any liquid to the trap bottle, as the bottle is designed to condense solvent vapor from the Ar sweep gas. 5 Screw the 3/8 inch threaded adapter end of the insulated PFA tubing to the corresponding 3/8 inch threaded fitting for the sweep gas out port on the back of the Aridus3. Attach the 3/8 inch adapter of the other end of this tubing to the corresponding 3/8 inch threaded fitting on the lid of the 4 liter trap bottle. See FIGURE 3-8 and FIGURE Note the sweep gas out port is on the far upper right area on the back panel of the Aridus3 (see the callout in FIGURE 3-10 on page 21). If space is tight, you may use the included elbow fitting. When using the elbow fitting, ensure that flow is always directed downward, never upward. 19

20 FIGURE 3-8. Attachment of Insulated Sweep Gas Out Line to 4-Liter Trap Bottle. 6 Connect the trap bottle exhaust tubing to the remaining port on the lid of the 4-liter trap bottle. This tubing will conduct solvent vapors to the exhaust vent. The exhaust should be vented at atmospheric pressure into an appropriate laboratory fume exhaust system. The trap bottle exhaust tubing is composed of rigid material to prevent bending and blocking the flow of exhaust vapors. The exhaust tubing may be cut to an appropriate length, depending on the distance to the fume exhaust system. See FIGURE 3-9. Additional tubing may be attached to the rigid exhaust tubing, but ensure that the tubing is not kinked or blocked. FIGURE 3-9. Attachment of Rigid Exhaust Tubing to Lid of 4-Liter Trap Bottle. 7 A minimum argon and nitrogen supply pressure of 75 psi (520 kpa, 5.2 bar ) is required to operate the Aridus3. The argon may be teed in from the ICP-MS instrument argon supply using the ¼ inch union tee. Connect the ¼ inch O.D. 20

21 Chapter 3: Installing the Aridus3 tubing, labeled ARGON and NITROGEN to the respective supply ports on the back panel of the Aridus3. The ¼" O.D. tubing for each is simply inserted into the corresponding press fit connectors. Simply push the tubing into its respective connector until it is fully secure. See FIGURE Note that the ARGON supply is for the Aridus3 sweep gas. NOTICE The insulated gas out line should curve downward (FIGURE 3-10) so that any condensed solvent vapor flows into the floor-mounted 4 L trap bottle. Sweep Gas Out Port FIGURE Connection of Argon and Nitrogen Supply Tubing to Aridus3. 8 Connect the nebulizer gas supply line (4 mm O.D.) to the nebulizer gas inlet port on the side of the C-Flow PFA nebulizer. This supply line is part of the interface kit; the supply line connects between the host ICP-MS nebulizer gas port and the gas inlet of the C-Flow PFA nebulizer. See FIGURE FIGURE Attachment of 4 mm O.D. Nebulizer Gas Tubing to C-Flow PFA Nebulizer. 21

22 Connecting the Aridus3 Drain Tubing There is one liquid drain tube from the PFA spray chamber of the Aridus3 unit. To set up this drain tube, follow the steps below. 1 Obtain the peristaltic-pump drain tubing kit from the Aridus3 completion kit. The kit will contain a 4 foot (122 cm) length of 1/16 inch OD ETFE tubing with an attached ¼-28 PEEK (tan-colored) nut with ferrule. 2 Install the PEEK nut with ferrule into the threaded drain port on the front of the Aridus3 PFA spray chamber. See FIGURE FIGURE Connection of Spray Chamber Drain Tubing to PFA Spray Chamber. 3 Connect the open end of the FEP tubing to a length of peristaltic pump tubing. 4 Install the peristaltic pump tubing onto a peristaltic pump, usually the pump of the host ICP-MS instrument. Note that liquid from the spray chamber drain port should flow to the inlet of the peristaltic pump and then to a suitable waste container. The direction of flow is typically shown by flow arrows on the pump. See FIGURE FIGURE Connecting the Drain Line to a Peristaltic Pump. 22

23 Chapter 3: Installing the Aridus3 Installing the Spray Chamber in the Aridus3 The PFA spray chamber for the Aridus3 is shipped as part of the completion kit. To install the spray chamber, follow the steps below. 1 Open the transparent front door of the Aridus3 by pulling downward. 2 Position the PFA spray chamber in front of the opening to the spray chamber heater. NOTE The tan colored extraction post should be at the top (12 o'clock position), as shown in FIGURE FIGURE PFA Spray Chamber In Position. 3 Insert the PFA spray chamber into the spray chamber heater. There will be some resistance as the spray chamber nears the end of the heater assembly. Push the spray chamber all the way into the heater assembly until the chamber is fully seated and connected to the membrane desolvator. FIGURE PFA Spray Chamber Installed. 23

24 Connecting the Nebulizer to the Aridus3 1 Open the front door of the Aridus3 by pulling downward. 2 Note the position of the spray chamber. The tan colored extraction post should be at the top position (12 O'clock) and the drain line should be at the bottom. 3 If you have not already done so, attach the other end of the drain line to a length of the peristaltic pump tubing as described in Connecting the Aridus3 Drain Tubing on page If you have not already done so, connect one end of the 4 mm O.D. nebulizer gas tubing to the side gas port of the C-Flow PFA nebulizer. Insert the tubing into the PFA nut and finger-tighten the nut. See FIGURE 3-11 on page Place the free end of the nebulizer gas tubing and the spray chamber drain tubing along the left side of the Aridus3 cabinet. Note that the free end of this tubing may or may not have an adapter fitting, depending on the brand and model of the host ICP-MS. 6 (Optional) Install the two holder loops onto the side of the Aridus3. To do this, remove the two screws, insert the screws through the loops, then reinstall the screws. The tubing can then be secured with the two holder loops. FIGURE Secure Placement of Nebulizer Gas Tube and Spray Chamber Drain Tube. 7 Attach the free end of the nebulizer gas tubing to the nebulizer gas port of the host ICP-MS. See the example in FIGURE

25 Chapter 3: Installing the Aridus3 FIGURE Example Nebulizer Gas Line Connection to Host ICP-MS Instrument. 8 Insert the C-Flow PFA nebulizer into the spray chamber port. See FIGURE Ensure that the nebulizer is fully inserted through both O-rings of the port. FIGURE Insertion of C-Flow PFA Nebulizer into Spray Chamber Nebulizer Gas Port. 9 Carefully set the C-Flow uptake line through the sample inlet notch in the upper left side of the Aridus3 cabinet. See FIGURE If the ASX-112FR autosampler is to be used, attach the sample probe assembly to the ASX-112FR probe holder. (Refer to the ASX-112FR Operator s Manual for further instructions.) 25

26 FIGURE Placement of the C-Flow Nebulizer Probe. Connecting the Aridus3 to the Host Computer Use the provided serial cable or your own serial cable with two male DB-9 connectors. The Aridus3 may be connected to the host ICP-MS computer or to a dedicated computer such as a laptop. 1 Plug one end of the cable into the host computer s serial (COM) port. If the computer has more than one serial port, make sure to use the same port which is selected in the instrument control software. 2 Finger-tighten both screws of the connector. 3 Connect the other end of the cable to the Aridus3 COM port. 4 Finger-tighten both screws of the connector. FIGURE Connection of DB-9F Serial Cable to Aridus3 COM Port. 26

27 Chapter 3: Installing the Aridus3 NOTES If a host computer serial port with a DB-9F, a DB-25M, or a DB-25F connector (9 pin D-subminiature receptacle or 25 pin D-subminiature plug or receptacle) must be used, use an adapter to convert the serial port to a DB-9M. Do not use a null modem adapter. When interconnecting any computing devices, keep the communications cables away from sources of electromagnetic or radio frequency (RF) interference, such as electric motors, transformers, fluorescent light ballasts, or RF energy sources. Limit cable runs for RS-232C to less than 16 meters. If these conditions cannot be satisfied, use low-impedance, fully shielded cables to provide satisfactory operation. The cables are available from many sources, but you will need to specify the correct mating connectors and straightthrough (DTE-DCE) wiring. Using a USB To Serial Adapter If an open serial COM port is not available on the host computer, a USB to serial adapter can be connected so a USB port can be used for communications to the Aridus3. One adapter is provided in the Aridus3 completion kit and is shown below in FIGURE Note that the USB to serial driver software will automatically be loaded upon installation of the Aridus Link software; no additional software download is required. FIGURE USB to Serial Adapter. 27

28 Setting Up the 4-Liter Trap Bottle The 4-liter trap bottle is supplied with two encapsulated magnets, which are secured to one side of the bottle. The magnets can be used to secure the bottle against a metal surface, such as the support leg of a laboratory table or cabinet. See FIGURE FIGURE Encapsulated Magnets Attached to 4-Liter Trap Bottle. 28

29 Chapter 3: Installing the Aridus3 Summary View of Connections to the Back Panel of the Aridus3 Electrical, communications, and gas connections to the back panel of the Aridus3 are summarized in FIGURE Note the downward slope of the insulated sweep gas out line to the 4-liter trap bottle which rests on the laboratory floor. This slope helps ensure drainage of any condensed liquid from the sweep gas out flow to the 4-liter trap bottle. FIGURE Summary View of Connections to Back Panel of Aridus3. 29

30 Using the ASX-112FR Autosampler With the Aridus3 The Teledyne CETAC ASX-112FR autosampler may be used for automated sample introduction to the Aridus3. The integrated sample probe of the C-Flow PFA nebulizer may be attached to the sample probe holder of the ASX- 112FR and directed via host computer control to blanks, standards, and samples. The footprint of the ASX-112FR is designed for placement on the top cover of the Aridus3, conserving valuable laboratory benchtop space. See FIGURE FIGURE Aridus3 With Teledyne CETAC ASX-112FR Autosampler. Connecting the Aridus3 C-Flow PFA Nebulizer to an ASX-112R Autosampler 1 Insert the C-Flow PFA nebulizer uptake line through the Z-axis sample probe assembly on the ASX-112FR autosampler. Insert the sample probe through the cylindrical support collar, then finger tighten the thumbscrew on the side of the collar to secure the probe. (Refer to the ASX-112FR Operator s Manual for further instructions.) See FIGURE 3-25 for probe setup. 30

31 Chapter 3: Installing the Aridus3 FIGURE Installing the Sample Probe on the ASX-112FR Autosampler. 31

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33 4 Verifying Installation Once installation of the Aridus3 is complete, it is important to verify that you have installed the system correctly. Attempting to use the Aridus3 before ensuring that it is installed correctly may result in damage to the system. Verifying installation of the Aridus3 consists of five parts: Software installation Initial operating procedure ICP-MS operation under normal conditions System optimization Aridus3 optimization This chapter explains initial operation of the Aridus3, ICP-MS operation, and the optimization of the Aridus3. Installing the Aridus Link Software The Aridus Link software requires the Microsoft Windows 7 or later operating system and is compatible with both 32-bit and 64-bit versions. It will automatically install the required versions of the Microsoft.NET Framework if missing as well as the USB-RS 232 drivers. 1 Locate the Aridus3 CD in the completion kit and load the CD into the host computer (this may be the ICP-MS computer or a separate computer such as a laptop). 33

34 2 Open the drive for the CD and browse the contents as shown below: FIGURE 4-1. Files on Aridus3 CD. 3 Select InstallMenu.exe and begin to follow the screen prompts. The screen below will appear: FIGURE 4-2. Aridus Link Setup Wizard. 4 Click Next and the following screen will appear: FIGURE 4-3. Aridus3 Release Notes. 34

35 Chapter 4: Verifying Installation 5 Read the Aridus3 Release Notes and click Next. The following screen will appear: FIGURE 4-4. Aridus Link Software License Agreement. 6 Read the Aridus Link software license agreement and then choose to accept the agreement and click Next. The following screen will appear: FIGURE 4-5. Aridus Link Ready to Install Screen. 35

36 7 Installation of the Aridus Link software may now begin; click Install to start this process. The following screens will appear. FIGURE 4-6. Aridus Link Installation Status. FIGURE 4-7. Aridus Link Installation Status. FIGURE 4-8. Aridus Link Installation Status. 36

37 Chapter 4: Verifying Installation FIGURE 4-9. Completion of Aridus Link Installation. 8 Click Finish. The Aridus Link software is now installed and an Aridus Link icon will appear on the host computer main screen. The icon appears as below: FIGURE Aridus Link Icon. Initial Operating Procedure 1 Plug the supplied power cord into the Aridus3 and then into the AC supply outlet. NOTICE Check that that the Aridus3 voltage selection switches are set to the correct voltage (115 V or 230 V). If the wrong voltage is selected, damage to the Aridus3 may occur. See FIGURE 2-1 on page Turn on the Aridus3 power switch, located on the back panel of the unit. 3 Click on the Aridus Link icon to open the Aridus Link software. 4 Open the supply valves for the argon and nitrogen gas flows to the Aridus3. The status light in the front of the Aridus3 cabinet will cycle from yellow to red color during the warmup period. Please see the pictures in FIGURE

38 FIGURE Status Light During Warm-Up of Aridus3. 5 After approximately 20 minutes, both heaters (spray chamber and membrane desolvator) should be operating at a steady state as indicated by temperature readings of 110 C ± 2 C for the spray chamber and 140 C ± 2 C for the desolvator. The status light in the front of the Aridus3 will turn to a solid blue color when the unit is at Ready status. FIGURE Aridus3 At Ready Status. The main Aridus Link software screen will also display the current temperatures during and at completion of the warm-up period. See FIGURE 4-13 below. 38

39 Chapter 4: Verifying Installation FIGURE Aridus Link Screen At Ready and Connected Status. 6 Set the argon sweep gas flow to 3.00 L/min and the nitrogen addition gas flow to 5.0 ml/min via the Aridus Link screen and click Apply. The gas flows may be typed into the boxes or set via the up and down arrows. Note that after the gas desired gas flow value is entered, it is necessary to click Apply at the bottom right of the screen to set that flow. Allow these flows to purge the Aridus3 for approximately 5 minutes. Temperature and Gas Flow Ranges Range of Conditions (Gas Flows and Temperatures) The following list provides a typical range of conditions for argon gas flows, the nitrogen flow, and the spray chamber and desolvator temperatures: Argon Nebulizer Gas Flow: 0.70 to 1.20 L/min Argon Sweep Gas Flow: 2.00 to 6.00 L/min Nitrogen Addition Gas Flow: 3.00 to L/min Spray Chamber Temperature: factory set at 110 C Desolvator Oven Temperature: factory set at 140 C Allowed Ranges of Aridus3 Gas Flows and Temperatures The allowed ranges of Aridus3 gas flows and temperatures are: Argon Sweep Gas Flow: 0.00 to L/min Nitrogen Addition Gas Flow: 0.0 to 50.0 ml/min Spray Chamber Temperature: 30 C to 130 C Desolvator Oven Temperature: 80 C to 180 C 39

40 NOTE The allowed ranges of the Aridus3 gas flows and temperatures are factory programmed. If a different gas flow and/or temperature range is desired, contact Teledyne CETAC Customer Service. Unauthorized changes in the gas flow and/or temperature ranges settings will immediately terminate the warranty. ICP-MS Operation 1 Using the controls in the Aridus Link software, set the argon sweep gas to 1.00 L/min and the nitrogen gas flow to 0.2 and click Apply. This task can also be done with one click by setting the ICP Ignition control to on status. See the previous FIGURE NOTICE The lower argon and nitrogen gas flows help to ensure a smooth ignition of the ICP-MS plasma. Higher gas flows may cause a rough start of the ICP-MS plasma, including damage to the torch and other torch box components. 2 Ignite the plasma as instructed in the host ICP-MS operating manual. 3 After the plasma has stabilized, use the Aridus Link software to set the argon sweep gas to a value of 2.00 L/min. The nitrogen addition gas flow should remain at a setting of 0.2 ml/min. 4 Prepare and aspirate an appropriate tuning solution through the Aridus3 to the host ICP-MS. An example tuning solution may contain 1 µg/l (ppb) of elements such as indium (In), cerium (Ce), and uranium (U). System Optimization It is necessary to optimize the ICP-MS instrument after installation of the Aridus3. Optimization procedures may include adjustment of gas flows, plasma sampling position, ion lens settings, and other ICP-MS parameters. Typically, the signal to noise or signal to background ratio is the primary criterion for optimization. For detailed instructions on system optimization for aqueous or organic samples, see the Aridus3 Optimization Procedure. After the system has been optimized, the Aridus3 is ready for routine operation. Aridus3 Optimization Procedure 1 After the Aridus3 and the host ICP-MS have reached a stable operating temperature, set the nebulizer gas flow rate to 0.90 L/min and aspirate an appropriate tuning solution that includes elements such as indium (In), cerium (Ce), and uranium (U). 40

41 Chapter 4: Verifying Installation 2 Monitor the signal intensities of the selected set of tuning elements in a time resolved mode and adjust the Ar sweep gas flow to produce the desired signal intensities. The Ar sweep gas flow is one of the most important parameters in determining sensitivity, stability, and interference reduction. Note that the element Ce is often used for this purpose. A typical operating range for the Ar sweep gas is 2.00 to 6.00 L/min, with a maximum setting of L/min. 3 Gradually increase the N 2 addition gas flow to further increase the tuning element(s) signal. Based upon the type of host ICP-MS instrument, only a low flow of nitrogen may need to be used. The operating range of the N 2 mass flow controller is 0.0 to 50.0 ml/min; a typical setting for the N 2 flow is between 3.0 and 10.0 ml/min. 4 After the N 2 addition gas flow has been optimized, the Ar sweep gas can be fine tuned for highest sensitivity and lower oxides (ex. lower % CeO/Ce). Typically the Ar sweep gas is reduced in a range of 0.1 to 1.0 L/min from the first optimized value. NOTE: The addition of N 2 will cause an increase in nitrogen-containing polyatomic ions, such as 40 Ar 14 N + on 54 Fe +. Signal enhancement via nitrogen addition should be considered versus any nitrogen based interferences. 5 Other parameters such as ICP power, ICP sampling position, nebulizer gas flow, and ion lens settings may need to be adjusted to achieve best performance. When properly optimized, the %CeO/Ce should be 0.05% or less. NOTE: Organic solvents (e.g., 2-propanol, toluene, hexane) may be run directly through the Aridus3 to the ICP-MS. To analyze organic solvents, a low flow of oxygen (10 to 30 ml/min) is usually added into the sample out line between the Aridus3 and the ICP-MS torch. The low flow of oxygen helps prevent carbon buildup on the ICP-MS sampler and skimmer cones. The Teledyne CETAC BGX-100 Blend Gas Accessory can be used for oxygen gas addition. Please contact Teledyne CETAC Technologies at (USA only), , or cetacservice@teledyne.com for further information and assistance with regards to gas addition with the BGX

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43 5 Using the Aridus3 Desolvating Nebulizer System It is important to establish sound laboratory practices, analytical environment, and ICP-MS performance before using the Aridus3. The best performance can then be expected when these conditions are met. Establishing Optimal Operating Conditions Malfunction or damage can occur if specific operating conditions are not met. Meeting these conditions requires establishing the proper laboratory environment and replacement of ICP-MS and Aridus3 components that wear out during normal usage. The following sections explain how to meet these conditions. NOTICE Damage or malfunction that results from unsatisfactory operating conditions may constitute misuse and abuse and be excluded from warranty coverage. Establishing the Lab Environment To establish satisfactory operating conditions in your laboratory environment, follow these guidelines: Operate the Aridus3 in a conventional laboratory environment where the temperature is F (10-30 C), the humidity is 20-70% noncondensing; and the unit is not exposed to excessive flammable or corrosive materials. Avoid rough handling of the Aridus3. If possible, do not expose the system to vibration or shock. Protect the Aridus3 from long-term exposure to condensation, corrosive materials, solvent vapor, continual standing liquids, or large spills. Exposures of this type can damage the electronics. 43

44 Observe the same general electrostatic discharge precautions as with any other integrated circuit electronic device. Low humidity environments, especially when combined with static-generating materials require maximum care. NOTICE Discharge static buildup and ground the Aridus3 cabinet before performing any maintenance. Do not touch or short-circuit bare contacts. Avoid using the Aridus3 if strong electromagnetic interference or radio frequency interference is present. In environments with very low humidity, high static charges may affect the stability of the analyte signal, causing a transient drop in intensity within the proximity of the charged object. Replacing Aridus3 Components The following components of the Aridus3 system need to be replaced periodically during normal usage. Failure to replace these components will result in deterioration of analytical performance. Sample Transfer Line: FEP-Lined PVC Tubing The sample transfer line should be replaced when it becomes grossly discolored or when it contains residues/condensation. Peristaltic Pump Tubing of the Host ICP-MS Instrument The peristaltic pump tubing (which is attached to the host ICP-MS peristaltic pump) that drains the Aridus3 PFA spray chamber should be replaced whenever the tubing becomes flat or misshapen due to pump shoe pressure. Please refer to the host ICP-MS operator s manual for instructions on how to replace the peristaltic pump tubing. Startup Procedure 1 If the Aridus3 power has been turned off for an extended period of time, turn on the AC power switch on the back panel of the unit and wait approximately 20 minutes for the Spray Chamber and Desolvator heaters to reach the factory set operating values of 110 C and 140 C, respectively. These temperatures will be displayed in the Aridus Link software screen. 2 Purge the Aridus3 with argon sweep gas (setting of 3.00 L/min) and nitrogen (setting of 5.00 ml/min) for five minutes. Use the Aridus Link software to establish these settings. 3 Decrease the argon sweep gas flow (setting of 1.00 L/min) and the nitrogen flow (setting of 0.2 ml/min). Use the Aridus Link software to establish these settings. Note that the ICP Ignition control on the Aridus Link screen can be used to establish the above gas flow values. 44

45 Chapter 5: Using the Aridus3 Desolvating Nebulizer System 4 Ignite the plasma according to standard operating procedures for the host ICP- MS instrument. Re-adjust Aridus3 operating parameters to the optimized settings. If the system has not been optimized, see pages in the Chapter 4, Verifying Installation. 5 The Aridus3 system is now ready for use. Shutdown Procedure 1 Aqueous Analysis: Aspirate dilute nitric acid (1% v/v) for approximately 5-10 minutes to provide a thorough spray chamber rinse. Follow the acid-rinse by aspirating deionized water for approximately 3-5 minutes. 2 Remove the sample uptake line of the C-Flow PFA nebulizer from the deionized water reservoir and aspirate the solution remaining in the sample line. It is important to dry the sample uptake line before shutting down the Aridus3. 3 Shut down the host ICP-MS instrument using the procedures recommended by the ICP-MS manufacturer. 4 Turn off any separate gas supplies for the Aridus3 argon sweep gas and the nitrogen addition gas. 5 Turn off the power switches on the Aridus3 and (if used) the Teledyne CETAC ASX-112FR autosampler. Monitoring the Temperature and Gas Flows An internal control board enables the setting of the Aridus3 spray chamber and membrane desolvator temperatures. The factory settings of the spray chamber and desolvator temperatures are 110 C and 140 C, respectively. The spray chamber temperature may be set in a range of 30 C to 130 C; the desolvator temperature may be set in a range of 80 C to 180 C. The Ar sweep gas and N 2 addition gas flows are set using dedicated internal mass flow controllers (MFCs). The Ar sweep gas may be set in a range of 0.00 to L/min; the N 2 addition gas may be set in a range of 0.0 to 50.0 ml/min. The mass flow controllers also provide a back pressure value, which can help indicate a restriction in gas flow. A back pressure less than psi indicates normal operation. The actual temperatures and gas flows are displayed in the Aridus Link software screen as shown in FIGURE

46 FIGURE 5-1. Temperature and Gas Flow Display. NOTE See page 39 for the allowed temperature and gas flow ranges. Switching from Organic Samples to Aqueous Samples and Aqueous Samples to Organic Samples When switching from analyzing organic solvents to aqueous samples, nebulize 2-propanol (isopropyl alcohol, IPA) for 10 minutes before running the aqueous samples. This will condition the spray chamber and membrane desolvator. When returning to organic samples from aqueous samples, nebulize 2- propanol for 10 minutes before running the organic solvents. This will recondition the Aridus3. NOTICE Carefully rinse the Aridus3 spray chamber and membrane desolvator with deionized water when switching between strong acids (e.g. nitric acid) and organic solvents. If heated residue from nitric acid contacts an organic solvent, a charring reaction can occur in the spray chamber and/or membrane desolvation system. Failure to carefully rinse the spray chamber and membrane desolvator between the introduction of strong acids and organic solvents can cause damage to the system and may void warranty conditions. Refer to Rinse Procedure for the Membrane Desolvator on page

47 Chapter 5: Using the Aridus3 Desolvating Nebulizer System Moving the Aridus3 BURN HAZARD FALLING OBJECT HAZARD When moving the Aridus3, do not lift or carry the Aridus3 by the membrane desolvator module handle. The handle is designed to be used only for installing and removing the membrane desolvator module. If the membrane desolvator module is not locked in place, it could slip out and fall. The exposed membrane desolvator module could also cause burns if touched. CAUTION FIGURE 5-2. Incorrect Lifting. Lift the Aridus3 by placing your fingers underneath the chassis. Do not lift using the handle on the back of the unit. 47

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49 6 Using the Aridus Link Software Use the Aridus Link software to control the operation of your Teledyne CETAC Aridus3 desolvating nebulizer system. Initial Startup of Aridus Link Software After the Aridus Link software has been installed as described in Chapter 4, Verifying Installation, follow the steps below: 1 Connect the appropriate power cord to the Aridus3 and ensure that the voltage select switches on the back panel are set to the correct voltage. See Power Requirements on page Connect the serial cable between the host ICP-MS computer and the Aridus3 COM port; if needed, use the USB to serial converter adapter cable to establish communications. See Establishing External Connections on page Ensure that the Ar sweep gas and N 2 addition gas lines are both attached to the back panel of the Aridus3. See Connecting the Aridus3 to the ICP-MS beginning on page Ensure that the sweep gas out line is connected to the 4 L trap bottle and the vent line is placed in an appropriate exhaust; connect the sample out line to the host ICP-MS torch. See Connecting the Aridus3 to the ICP-MS beginning on page

50 5 Click on the Aridus Link icon on the host computer screen to open the software. The screen below will appear: FIGURE 6-1. Aridus Link Software Screen Disconnected. 6 Turn on power to the Aridus3 using the rocker switch on the back panel. Allow the Aridus3 to remain on and wait for the Aridus Link screen below to appear: FIGURE 6-2. Aridus Link Software Screen: Initializing Warming Up. After approximately 10 seconds the Aridus Link software screen will change to connected-warming up status as shown below in FIGURE 6-3. FIGURE 6-3. Aridus Link Software Screen: Connected Warming Up. The Aridus3 will warm up to the preset factory temperatures of 110 C for the spray chamber and 140 C for the membrane desolvator, this warm up process 50

51 Chapter 6: Using the Aridus Link Software takes approximately 20 minutes. Note that the Ar sweep gas and N 2 addition gas flow rates will set to the values that were last entered when using the Aridus Link software. After the warming up time is complete, the Aridus Link software screen below will appear indicating that the Aridus3 is ready for use. See FIGURE 6-4. FIGURE 6-4. Aridus Link Software Screen: Connected-Ready. Using the ICP Ignition Tool The ICP Ignition tool can be turned to the On setting by clicking the control button on the Aridus Link software screen. This tool will reset the Ar sweep gas to 1.00 L/min and the N 2 addition gas to 0.2 ml/min to help ensure a smooth ignition for the ICP-MS plasma. See FIGURE 6-5. FIGURE 6-5. ICP Ignition Tool - On. After the ICP has started and the host ICP-MS is at a ready or analyze status, the ICP ignition tool can be turned off. The Ar sweep gas and the N 2 addition gas will reset to the previous values. Note that the Ar sweep gas flow and the N 2 addition gas flow can be turned down to the ignition values by adjustment via the individual gas controls. See the next section. 51

52 Adjusting the Aridus3 Gas Flows and Temperatures The Aridus3 gas flows and temperatures may be adjusted up or down by the arrow buttons or can be typed in the white box next to each parameter. FIGURE 6-6 shows the adjustment of the Ar sweep gas by the up arrow button. Note that during adjustment the Apply button will change to yellow color. FIGURE 6-6. Adjustment of Ar Sweep Gas. When the Apply button is clicked, the Ar mass flow controller will change the Ar sweep gas flow to 3.20 L/min. The Apply button will change back to a white color. See FIGURE 6-7. FIGURE 6-7. Ar Sweep Gas Set to 3.20 L/min. The spray chamber and desolvator temperatures and the N 2 addition gas can be changed in the same way. Please note the allowed ranges for adjustment of these parameters; these ranges are also shown on the Aridus Link software screen. Parameter Allowed Range Spray Chamber Oven Temperature: 30 C to 130 C Desolvator Oven Temperature: 80 C to 180 C Argon Sweep Gas: 0.00 to L/min N 2 Addition Gas: 0.0 to 50.0 ml/min 52

53 Chapter 6: Using the Aridus Link Software Saving an Aridus3 Parameter Setting The user can save a set of Aridus3 parameter settings (temperatures and gas flows) or open an existing (saved) parameter set. Select File>Save As to save a set of parameters with a definitive name. See FIGURE 6-8. FIGURE 6-8. Saving Aridus3 Temperature and Gas Settings. Selecting Save As opens the screen below; a set of parameters can be given a definitive name for future use or reference. See FIGURE 6-9. FIGURE 6-9. Save As Function for Aridus3 Parameters. The Aridus Link software screen in FIGURE 6-10 shows an example of a parameter set (Aridus3 Parameters 2) that has been opened. When the yellow Apply button is clicked the Aridus3 parameters will change to those settings. 53

54 FIGURE Opened Aridus3 Parameter Set. Aridus Link Software Tools Collapse Screen The Aridus Link software screen can be made smaller by selecting View>Collapse. See FIGURE FIGURE Selecting Collapse Screen Feature. 54

55 Chapter 6: Using the Aridus Link Software After selecting Collapse the software screen will appear as below. See FIGURE FIGURE Collapsed Aridus Link Software Screen. To return the screen to full size, select View>Expand. Aridus Link Software Tools Pressure Units The Aridus3 provides a measurement of gas pressure downstream from the outlet of each mass flow controller (Ar sweep gas and N 2 addition gas). This feature can be useful to detect a possible flow restriction such as a bent or kinked tube. Select View>Pressure Units as shown in FIGURE FIGURE Aridus Link Software Feature Pressure Units. 55

56 When Pressure Units is clicked the screen below will appear. Then select the desired pressure units to display in the main software screen. See FIGURE FIGURE Selection Screen for Pressure Units. The Aridus Link software screen can be secured to the host computer screen by using the Pin feature. This feature keeps the Aridus Link software screen in view while performing other tasks in the ICP-MS software. Select View>Pin as shown in FIGURE FIGURE Aridus Link Software Feature Pin. If the Pin feature is no longer needed, select View>Unpin as shown in FIGURE FIGURE Aridus Link Software Feature Unpin. 56

57 Chapter 6: Using the Aridus Link Software FlowSaver Software Tool The Aridus Link software contains an application to shutoff the Ar sweep gas and the N 2 addition gas after the completion of a long sample run, saving valuable gases. To enable this application, called FlowSaver, select View>FlowSaver. See FIGURE FIGURE Select FlowSaver. After selecting FlowSaver, the screen below will appear. This screen allows a gas shutoff time to be selected based on a 24 hour clock. FIGURE FlowSaver Time Selection. Set the appropriate gas shutoff time and click On. Note that the shutoff time is selected in 15 minute increments. Then click Apply. FIGURE FlowSaver Time Selection. The main Aridus Link control screen will then indicate that the FlowSaver tool is active and will indicate the date and time for gas shutoff. See FIGURE

58 FIGURE Aridus Link screen with FlowSaver On. After the gas flows are shut off, the Aridus3 will be in a Standby mode. This Standby mode is also indicated by the purple color of the status light in the front panel of the Aridus3. To restore the previous gas flows, click the yellow Wakeup button. See FIGURE FIGURE Aridus Link Screen in Standby Mode. 58

59 7 Installing the QuickWash3 Fast Washout Accessory An optional QuickWash3 fast washout accessory may be installed in the Aridus3 cabinet. The QuickWash3 accessory enables in-place rinsing of the PFA spray chamber after the introduction of higher concentration samples. The QuickWash3 may be operated in a manual mode or an automated mode via the ASX-112FR autosampler. See FIGURE 7-21 on page 70 for a picture of the Aridus3 nebulizer system equipped with both the ASX-112FR autosampler and the QuickWash3 accessory. FIGURE 7-1. Teledyne CETAC QuickWash3 Accessory Front View. 59

60 FIGURE 7-2. Teledyne CETAC QuickWash3 Accessory Back View. Why Spray Chamber Cleaning Is Needed Prolonged introduction of higher concentration samples can cause analyte and sample matrix buildup on the inner wall of the heated PFA spray chamber of the Aridus3. This buildup can cause signal spikes and longer sample washout times. Spray chamber rinsing is especially useful if analyte concentrations above 100 μg/l are introduced, such as for isotope ratio measurements performed with multi-collector ICP-MS. This situation can occur, for example, in U-Th dating studies. The QuickWash3 fast washout accessory can be used during the rinse cycle of the Aridus3 to rapidly clean the inner wall of the PFA spray chamber, with significant reduction of washout times. In addition, the QuickWash3 enables PFA spray chamber cleaning without turning off power to the Aridus3, allowing the PFA spray chamber to cool prior to removal, and then spray chamber disassembly and manual rinsing. How the QuickWash3 Accessory Works The QuickWash3 controls a second auxiliary pneumatic nebulizer that is positioned in the left side-front of the PFA spray chamber, generating a tangential aerosol to efficiently clean the chamber. The QuickWash3 controls the flow of rinse solution and argon gas to the secondary nebulizer. The rinse solution is typically recirculated by the host ICP-MS peristaltic pump and is directed to the auxiliary nebulizer via the gas/liquid line from the front of the QuickWash3 accessory. How the QuickWash3 Accessory Is Controlled The QuickWash3 can be operated manually through the Aridus Link software of the Aridus3, or it can be set to run automatically when used with the Teledyne CETAC ASX-112FR MicroAutosampler. Wash times are preset from 10 seconds to 160 seconds, in increments of 1 second, via the Aridus3 control software. 60

61 Chapter 7: Installing the QuickWash3 Fast Washout Accessory Equipment Supplied With the QuickWash3 Accessory The following parts are provided: QuickWash3 accessory module Rinse solution tubing kit Cable connection to optional ASX-112FR autosampler Installing the QuickWash3Accessory NOTICE Discharge static buildup and ground to the Aridus3 cabinet before installation. Do not touch or shortcircuit bare contacts. 1 Turn off power to the Aridus3 and disconnect the power cord. 2 If the Aridus3 has been in operation, allow to cool for at least 2 hours. 3 Open the front door of the Aridus3 and remove the cover plate on the front of the Aridus3 cabinet. Perform this task by removing the two thumbscrews that secure the plate; save the thumbscrews for future use. FIGURE 7-3. Removing the Cover Plate. 4 Locate the gas supply line and the power connection cable for the QuickWash3. Both items are inside the cabinet of the Aridus3. 5 Remove the top cover of the Aridus3. See Removing the Top Cover on page 86 for instructions. CAUTION BURN HAZARD The desolvator oven heater block inside the Aridus3 may still be hot. Exercise caution when working near the heater block. 61

62 6 The gas supply line is sealed at its end. Grasp the sealed end with a tool such as a pliers and use a sharp cutting tool or a razor blade to remove approximately 3 to 4 cm of tubing from the end of the supply line. FIGURE 7-4. Cutting the Sealed Gas Supply Line. 7 Connect the open end of the gas supply tubing into the press-fit port on the back panel of the QuickWash3. FIGURE 7-5. Connecting the Sealed Gas Supply Line. 8 Connect the communication/power cable to the corresponding 6 pin port on the back panel of the QuickWash3. FIGURE 7-6. Connecting the Communication/Power Cable. 62

63 Chapter 7: Installing the QuickWash3 Fast Washout Accessory 9 Use the two thumbscrews that were saved from the front panel plate to secure the QuickWash3 to the Aridus3 chassis. 10 (Optional) Temporarily remove the C-Flow PFA nebulizer from the PFA spray chamber. Removing the nebulizer will help ease the connection of the gasliquid line. 11 The tubing mounted in the left front of the QuickWash3 is the gas-liquid line. This line conducts rinse liquid and argon gas to the Aridus3 PFA spray chamber. Remove the ¼-28 plug from the left side of the PFA spray chamber. FIGURE 7-7. Removing the Plug From the PFA Spray Chamber. 12 Remove the protective cap from the end of the gas-liquid line. FIGURE 7-8. Removing the Protective Cap. 13 Connect the gas-liquid line using the attached nut by securing it into the threaded side port of the PFA spray chamber. See FIGURE 7-9 and FIGURE

64 FIGURE 7-9. Connectiing the Gas-Liquid Line to the PFA Spray Chamber. FIGURE Installed Gas-Liquid Line. 14 Locate the QuickWash3 rinse supply kit. Rinse In and Rinse Out lines (0.8 mm ID PFA tubing) are connected to the front of the QuickWash3 via PEEK ¼-28 nuts with ferrules. FIGURE Connecting the Rinse In Supply Line. 64

65 Chapter 7: Installing the QuickWash3 Fast Washout Accessory Summary of QuickWash3 Liquid Flows The completed Rinse in and Rinse Out line connections to the front panel of QuickWash3 are shown in FIGURE FIGURE Completed Connection of Rinse In and Rinse Out lines. The Rinse In line connects to the liquid flow output of the pump tubing from the host ICP-MS peristaltic pump. The Rinse Out line returns rinse solution to the rinse solution bottle when the QuickWash3 is not activated. When the QuickWash3 is activated the rinse liquid is directed to the gas-liquid line connected to the PFA spray chamber. See FIGURE 7-13 for connection to a host peristaltic pump. FIGURE Connections to the Host Peristaltic Pump. A dilute nitric acid solution such a 2% (v/v) nitric acid can be used as the QuickWash3 rinse solution CAUTION CHEMICAL BURN HAZARD Exercise all appropriate safety precautions (safety glasses, gloves, labcoat, etc.) when handling solutions of nitric acid 65

66 Controlling the QuickWash3 Through the Aridus Link Software (Manual Control) When the QuickWash3 is installed, the Aridus Link software will show control features on the bottom of the main software screen. See FIGURE FIGURE Aridus Link Software Screen With QuickWash3 Controls. 1 Set the rinse time and click Apply. The QuickWash3 rinse time can be set in increments of 1 second up to 160 seconds. A rinse time range of 30 to 60 seconds is typically used. The rinse time may be typed in the box or set via the up and down arrows. When a new rinse time is determined, the Apply button will turn yellow and must be clicked to set the new value. The example in FIGURE 7-15 shows a change from a 20 second rinse time to a 30 second rinse time. See Figure FIGURE Aridus Link software screen With Rinse Time Change of 30 Seconds. 66

67 Chapter 7: Installing the QuickWash3 Fast Washout Accessory CAUTION SPILL RISK Ensure that the drain line from the Aridus3 PFA spray chamber is properly connected to the host ICP-MS peristaltic pump so excess rinse solution is pumped to waste. 2 To start rinsing, click QuickWash Start. The QuickWash3 will direct the rinse solution through the gas-liquid line and into the side port of the PFA spray chamber. The status bar will indicate the progress of the rinse cycle. FIGURE Aridus Link Screen with active QuickWash Cycle. Controlling the QuickWash3 Via the ASX-112FR Autosampler (Automated Control) The QuickWash3 can be started via a signal from the ASX-112FR autosampler, specifically when the sample probe moves into the second rinse port of ASX- 112R rinse station. As with manual control, the rinse time is set through the Aridus Link software. To set up the QuickWash3 for automated use via the ASX-112FR, follow the steps below. 67

68 Connecting the Control Cable 1 Locate the RS-232 cable with a 90 degree connector; this is labelled part no FIGURE RS-232 Cable With 90 Degree Connector. 2 Attach the straight end of the cable to the Aux I/O port on the back panel of the ASX-112FR autosampler. FIGURE RS-232 Cable Connection to ASX-112 Aux I/O Port. 3 Attach the other end of the cable (with the 90 degree connector) to the COM port on the front panel of the QuickWash3. See FIGURE 7-19 and FIGURE

69 Chapter 7: Installing the QuickWash3 Fast Washout Accessory FIGURE RS-232 Cable Connection to QuickWash3 COM Port. FIGURE Full View of Connection to Front Panel of QuickWash3. FIGURE 7-21 shows detail of connections between the installed QuickWash3 and a host peristaltic pump. 69

70 FIGURE Full View of Connection Between Installed QuickWash3 and Host Peristaltic Pump. Operating the QuickWash3 Automatically 1 Set the rinse time using the Aridus Link software, as described on page 66. Remember to click Apply. 2 Operate the ASX-112FR as usual. The autosampler will trigger the QuickWash3 whenever the sample probe moves into the second rinse port of ASX-112R rinse station. Important Notes for Operation of the QuickWash3 Typical QuickWash3 rinse times are from 30 to 60 seconds using a dilute nitric acid solution, such a 2% nitric acid (v/v). The pumped rinse solution flow rate to the QuickWash3 is a recommended range of 1.0 to 2.0 ml/min. The argon gas flow rate to the QuickWash3 is factory set via a regulator inside the QuickWash3 at approximately 2.0 L/min. Do not attempt to adjust this setting. Ensure that the drain tubing from the bottom of the PFA spray chamber is connected to the host peristaltic pump and is sending waste rinse liquid to a suitable waste container. Liquid accumulation in the PFA spray chamber can cause signal instability. If using the QuickWash3 in an automated mode, ensure that an appropriate read delay time is set after the QuickWash3 rinse cycle ends. The read delay will allow the Aridus3 and the host ICP-MS to restabilize before collecting data from the next sample. Read delay times may vary depending on the time duration of the QuickWash3 rinse cycle; delay times may be 1 to 3 minutes or longer. 70

71 Chapter 7: Installing the QuickWash3 Fast Washout Accessory QuickWash3 Specifications Power: 24 VDC, 1.0A (via internal connection to Aridus3) Dimensions: 15.8cm (W) x 10.5cm (D) x 4.7cm (H) Argon Gas Flow: 2 L/min (factory setting) Weight: 0.52 kg (1.15 lbs) 71

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73 8 Maintaining the Aridus3 Routine maintenance of the Aridus3 consists of procedures for specific system components and expendable supplies. Maintenance includes checking the Aridus3 system components for leaks or other problems/damage. Some applications may require that certain maintenance procedures be performed more frequently, such as flushing the PFA spray chamber and the membrane desolvation system after prolonged exposure to high dissolved solids. WARNING The Aridus3 must be turned off and the AC power cord unplugged before performing any maintenance on the system. Cleaning the Aridus3 Cleaning the Aridus3 is an important task. Failure to clean the Aridus3 can cause increased wear and reduce the system s operating life. It is especially important to clean up any liquid spills, particularly of acidic solutions. Note that it may be necessary to chemically neutralize spills. The following sections explain external and internal cleaning procedures. WARNING SHOCK HAZARD Do not allow any liquid to enter the instrument cabinet other than as intended through the specified tubing, or come into contact with any electrical components. The instrument must be thoroughly dry before you reconnect power, or turn the instrument on. External Cleaning Use of the Aridus3 can result in spills on the top lid of the unit. To clean any external spills complete the following steps: 73

74 1 Turn the power switch to off (O) and disconnect the power cord to the Aridus3. 2 Wipe the top and sides of the Aridus3 using a towel dampened with a laboratory-grade cleaning agent. 3 Repeat step 2, using a towel dampened with clear water. This process removes any remaining contaminants. 4 Dry the lid of the Aridus3 with a dry towel. The Aridus3 must be thoroughly dry before you turn the Aridus3 power on. Internal Cleaning Use of the Aridus3 can result in spills inside the front door of the unit. To clean any internal spills, complete the following: 1 Turn the power switch to off (O) and disconnect the power cord to the Aridus3. 2 Open the transparent front door by pulling downward. Check the area near the PFA spray chamber for any liquid leaks. 3 Wipe the area inside the front door using a towel dampened with deionized water. 4 Repeat step 3, using a towel dampened with deionized water. This process removes any remaining contaminants. 5 Dry the area inside the front door with a dry towel. The Aridus3 must be thoroughly dry before you turn the Aridus3 power on. 6 Close and secure the transparent front door. Maintaining the Nebulizer and Spray Chamber Cleaning the Nebulizer The C-Flow PFA nebulizer may be removed from the unit while the plasma is on. If droplets collect on the nebulizer tip: 1 Remove the sample uptake tubing from the solution. 2 Allow the nebulizer to aspirate air for 1-2 minutes. 3 Dry the tip of the nebulizer with a lint-free cloth. If the aspiration rate is extremely slow or if the C-Flow PFA nebulizer does not self-aspirate, the capillary may be obstructed. To remedy this condition, the nebulizer may be backflushed with argon gas (see page 76). 74

75 Chapter 8: Maintaining the Aridus3 Removing the PFA Spray Chamber WARNING BURN HAZARD Allow the spray chamber to cool to room temperature before disassembly. If in doubt, wear heat resistant gloves. Take care not to drop the hot spray chamber. To remove the spray chamber: 1 Turn off power to the Aridus3 and allow the unit to cool for minutes. 2 Remove the C-Flow PFA nebulizer. 3 Detach the spray chamber drain line. 4 Grasp the spray chamber extraction post and pull the spray chamber straight out. See FIGURE 8-1. FIGURE 8-1. Removal of the PFA Spray Chamber. Disassembling the PFA Spray Chamber The chamber may be disassembled for cleaning if samples containing high dissolved solids were introduced. 1 Allow the spray chamber to cool before disassembly. 2 Unscrew the end of the spray chamber. See FIGURE

76 FIGURE 8-2. Disassembled PFA Spray Chamber. 3 Rinse the inside of each spray chamber part with a 2% (v/v) nitric acid solution followed by deionized water to help remove deposits from the inner walls. WARNING CHEMICAL BURN HAZARD Wear personal protective equipment (including gloves, safety glasses, and lab coat) and observe all necessary safety precautions when handling solutions of nitric acid or any other acid. Backflushing the C-Flow PFA Nebulizer If an obstruction is suspected in the nebulizer uptake line, follow the steps below: 1 Remove the C-Flow nebulizer from the Aridus3 spray chamber. 2 Start the flow of argon nebulizer gas from the host ICP-MS instrument and set the flow to 1.0 L/min. 3 Place a gloved finger over the end of the nebulizer for a few seconds to backflush argon through the uptake line capillary. This action should remove the obstruction. See FIGURE

77 Chapter 8: Maintaining the Aridus3 FIGURE 8-3. Backflushing the C-Flow Nebulizer. Main Fuse Replacement The main fuses are located in the AC power module fuse drawer located at the left rear of the Aridus3. To replace blown fuses: 1 Turn the AC power switch to off (0) and disconnect the AC power cord. 2 Use a small flat blade screwdriver to unlatch the fuse holder and remove the fuse drawer. See FIGURE Replace the defective fuse with a 5A 250V slow-blow 5x20 mm fuse (T5AL250V). WARNING FIRE AND SHOCK HAZARD Replace only with the specified fuse. Using an incorrect fuse can cause a fire or personal injury. 4 Insert the fuse drawer, replace the power cord, and turn the AC power switch on. If the new fuse blows, do not attempt to operate the unit. Contact your authorized Teledyne CETAC Service Representative or Teledyne CETAC Technologies for assistance. 77

78 FIGURE 8-4. Replacing the Main Fuses. Spray Chamber and Desolvator Fuse Replacement The fuses for the spray chamber and the desolvator are also at the left rear of the Aridus3. To replace blown fuses: 1 Turn the AC power switch off (0) and disconnect the AC power cord. 2 Turn the fuse knob counter-clockwise and pull the fuse holder straight out of the instrument cabinet. See FIGURE Replace the defective spray chamber fuse with a 20mm, 2.5A, 250V slow-blow fuse. 4 Replace the defective desolvator fuse with a 20mm, 5A, 250V slow-blow fuse. 5 Place the new fuse in the fuse holder, reinsert into the respective fuse slot, and turn the fuse holder clockwise to set the fuse in place. WARNING FIRE AND SHOCK HAZARD Replace only with the specified fuse. Using an incorrect fuse can cause a fire or personal injury. 78

79 Chapter 8: Maintaining the Aridus3 6 Replace the power cord and turn the AC power switch on. If the new fuse blows, do not attempt to operate the unit. Contact your authorized Teledyne CETAC Service Representative or Teledyne CETAC Technologies for assistance. FIGURE 8-5. Replacing the Spray Chamber Fuse. Rinse Procedure for the Membrane Desolvator The membrane desolvator may need to be thoroughly rinsed after the analysis of organic samples containing high concentrations of nonvolatile residues or after analysis of aqueous samples containing high concentrations of dissolved solids. The length of time between rinses in a routine operation depends on the types of samples analyzed. Analysis of samples containing less than 1% of dissolved solids is recommended. Best performance will be achieved with 0.1% to 0.5% dissolved solids. When solvent removal efficiency decreases, oxide (e.g., CeO) levels may increase and analyte signal may decrease or become unstable. Analysis of samples with higher dissolved solids may also cause a sample memory effect. The membrane desolvator may then require cleaning. NOTE: If aqueous samples were analyzed, 2% HNO 3 may be used to rinse the membrane. If organic solvents such as toluene or hexane were analyzed, rinse the membrane with 2-propanol. If non-volatile organic samples (e.g., oils diluted in an organic solvent) were analyzed, rinse the membrane with toluene or hexane. After rinsing with such a solvent, perform a second rinse with 2- propanol. 79

80 WARNING CHEMICAL BURN HAZARD Wear personal protective equipment (including gloves, safety glasses, and lab coat) and observe all necessary safety precautions when handling HNO 3 solutions and organic solvents. The membrane desolvator may be rinsed by removing the desolvator module from the Aridus3 or with the module still installed in the Aridus3 chassis. The first procedure describes removal and rinsing of the membrane desolvator. Removing and Rinsing the Membrane Desolvator WARNING BURN HAZARD Wear heat resistant gloves when handling the membrane desolvator. Take care not to drop the hot membrane desolvator. 1 Turn the AC power switch to off (0) and disconnect the power cord from the Aridus3. 2 Allow the Aridus3 to cool for at least 1 hour. 3 Position the Aridus3 so that the membrane desolvator will land on the tabletop should it be dropped. 4 Use the 5/32 hex wrench to open the lock of the membrane desolvator module on the back panel of the Aridus3. FIGURE 8-6. Opening Lock for Membrane Desolvator Module. 80

81 Chapter 8: Maintaining the Aridus3 5 Use heat resistant gloves to pull the membrane desolvator module out of the Ardius3. FIGURE 8-7. Removing the Membrane Desolvator Module Using Heat-Resistant Gloves. 6 Place the membrane desolvator module on a flat surface such as a metal or stone benchtop. Do not place the module on a plastic, wood, or rubber-type surface (unless the module has cooled to room temperature). 7 Locate the Aridus3 rinse kit and obtain the two rinse lines with the PTFE connection blocks. Connect the blocks to the corresponding ports of the desolvator module. 8 Prepare 500 ml of a 2% nitric acid solution, using a high-purity grade of nitric acid. Add this solution to the provided 500 ml rinse bottle of the rinse kit. WARNING CHEMICAL BURN HAZARD Wear personal protective equipment (including gloves, safety glasses, and lab coat) and observe all necessary safety precautions when handling HNO 3 solutions and organic solvents. 9 Attach the rinse bottle to one of the rinse lines; the other rinse line should be placed into a waste container. 10 Raise the rinse bottle above the level of the desolvator module and squeeze the bottle to allow the 2% nitric acid solution to flow into the desolvator module and out to waste. See FIGURE

82 FIGURE 8-8. Rinse Kit Connections to Membrane Desolvator Module. 11 The waste outlet line may be raised above the level of the desolvator module to allow the acid rinse solution to soak (for up to 1 hour) the membrane. A laboratory ring stand may be used to secure the outlet line. See FIGURE 8-9. FIGURE 8-9. Setup for Soaking Membrane Desolvator Module. 82

83 Chapter 8: Maintaining the Aridus3 12 After the rinse and/or soak step is complete, detach the rinse bottle. Rinse and fill the bottle with deionized water. 13 Repeat steps 9 and 10 at least two times with deionized water. As in step 11, deionized water can also be used to soak the membrane desolvator module. 14 Drain the deionized water from the module and detach the rinse kit lines from the module. 15 Reinstall the module into the Aridus3 chassis, ensuring that the contact board (green color) of the module is facing to the bottom. 16 Reconnect the power cord to the Aridus3 and turn on the power switch to on (1). 17 Open the Ardius Link software and set the Ar sweep gas flow to 3.00 L/min. 18 Open the host ICP-MS software and manually set the Ar nebulizer gas flow through the C-Flow PFA nebulizer to 1.00 L/min. Note that the ICP-MS plasma would not be turned on. 19 Allow the Ar gas flows to move through the Aridus3 for at least 8 hours to thoroughly dry the membrane desolvator. 2-Propanol (isopropyl alcohol) may be aspirated through the C-Flow nebulizer to help dry and condition the membrane. Rinsing the Membrane Desolvator Module and PFA Spray Chamber Installed in Aridus3 The membrane desolvator module and the PFA spray chamber may be rinsed as installed in the Aridus3 the module and spray chamber are not removed. To perform this procedure, follow the steps below. 1 Turn the power switch to off (O) and disconnect the power cord to the Aridus3. 2 Allow the Aridus to cool for at least 1 hour. 3 Locate the Aridus3 rinse kit and obtain the two rinse line assemblies with labelled connections. 4 Disconnect the Sample Out line from the back panel of the Aridus3. 5 Remove the threaded plug from the Rinse port on the back panel of the Aridus3. Save the plug for reconnection after the rinse procedure is complete. 6 Disconnect the Sweep Gas Out line from the back panel of the Aridus3. 7 Carefully remove the C-Flow PFA nebulizer from the PFA spray chamber. The PFA spray chamber drain line must be left attached to the peristaltic pump or can be sealed with a ¼-28 plug. 83

84 8 Attach the two labelled rinse line assemblies to the corresponding ports on the back panel of the Aridus3 and to the PFA spray chamber. 9 Prepare 500 ml of a 2% nitric acid solution, using a high-purity grade of nitric acid. Add this solution to the provided 500 ml rinse bottle of the rinse kit. WARNING CHEMICAL BURN HAZARD Wear personal protective equipment (including gloves, safety glasses, and lab coat) and observe all necessary safety precautions when handling HNO 3 solutions and organic solvents. 10 Attach the rinse bottle to the rinse line assembly that connects to the Sweep Gas Out port and to the PFA spray chamber. 11 Place the other rinse line assembly (connects to the Sample Out and Rinse ports) into a waste container. 12 Raise the rinse bottle above the level of the Aridus3 and squeeze the bottle to allow the 2% nitric acid solution to flow into the membrane desolvator module and PFA spray chamber and then out to waste. See FIGURE 8-10 and FIGURE FIGURE Rinse Kit Connections to Aridus3 With Membrane Desolvator Module and PFA Spray Chamber In Place. 84

85 Chapter 8: Maintaining the Aridus3 FIGURE Rinse Kit Connection to Aridus3 PFA Spray Chamber. 13 The waste outlet line may be raised above the level of the Aridus3 to allow the acid rinse solution to soak (for up to 1 hour) the membrane desolvator and PFA spray chamber. A laboratory ring stand may be used to secure the outlet line. FIGURE Setup for Soaking Membrane Desolvator Module (In Place) and PFA Spray Chamber. 14 After the rinse and/or soak step is complete, detach the rinse bottle. Rinse and fill the bottle with deionized water. 15 Repeat steps 10 through 12 at least two times with deionized water. Step 13 (soaking the membrane desolvator module) may also be repeated using deionized water. 85

86 16 Drain the deionized water from the Aridus3 and detach the rinse kit lines from back panel of the Aridus3 and the PFA spray chamber. 17 Reinstall the threaded plug into the Drain port on the back panel of the Aridus3. 18 Reinstall the C-Flow nebulizer into the PFA spray chamber. 19 Reconnect the power cord to the Aridus3 and turn on the power switch to on (1). 20 Open the Ardius Link software and set the Ar sweep gas flow to 3.00 L/min. 21 Open the host ICP-MS software and manually set the Ar nebulizer gas flow through the C-Flow PFA nebulizer to 1.00 L/min. Note that the ICP-MS plasma would not be turned on. 22 Allow the Ar gas flows to move through the Aridus3 for at least 8 hours to thoroughly dry the membrane desolvator. 2-propanol (isopropyl alcohol) may be aspirated through the C-Flow nebulizer to help dry and condition the membrane. Removing the Top Cover If you need to remove the top cover from the Aridus3 chassis: 1 Turn off power to the Aridus3 and disconnect the power cord. 2 Allow the Aridus3 to cool for at least 2 hours. 3 Remove the six screws that secure the cover to the Aridus3 chassis. FIGURE Location of the Cover Screws. 86

87 Chapter 8: Maintaining the Aridus3 4 Disconnect the cooling fan on the right side of the cover. FIGURE Disconnecting the Fan. 5 Carefully remove the cover. Please exercise caution as the membrane desolvator heater block and spray chamber heater will be very hot! WARNING BURN HAZARD Observe any necessary safety precautions (such as heat resistant gloves) when handling hot objects. Touching the hot membrane desolvator module or spray chamber heater with bare hands may cause burns. 87

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89 9 Troubleshooting the Aridus3 The Aridus3 is both easy to operate and reliable. However, problems with the system may occur. If good performance is not obtained, try to isolate the problem to determine if it originates in the host ICP-MS instrument, sample preparation procedure, or the Aridus3. This chapter explains how to troubleshoot Aridus3 problems. If you cannot solve a problem using the steps given in this chapter, contact Teledyne CETAC Technologies Customer Service and Support. Phone: (800) (USA only) (402) Fax: (402) cetacservice@teledyne.com Communication Problems There is no communication between the host computer and the Aridus3 The screen below may appear via the Aridus Link software: FIGURE 9-1. Communication Error Screen. 89

90 Check that the DB-9F cable is securely connected between the host computer COM port and the Aridus3 COM port If required, check that the USB to serial adapter is securely connected and that the USB to serial driver program has been loaded onto the host computer. Check that both the power and control cables are connected to both mass flow controllers inside the Aridus3 chassis. Refer to Reconnecting the mass flow controllers on page 93. Temperature Control Problems The PFA spray chamber does not heat up The power cord may not be plugged into the AC wall outlet. Plug in the power cord. The spray chamber fuse may be blown. Replace the spray chamber fuse as described on page 79 (see FIGURE 8-5). The inside electrical connection to the spray chamber heater (oven) might not be connected. The error below may appear from the Aridus Link software: FIGURE 9-2. Spray Chamber Heater Error Notification. Reconnecting the spray chamber heater If the error in FIGURE 9-2 appears, follows the steps below: 1 Turn off power to the Aridus3 and disconnect the power cord. 2 Allow the Aridus3 to cool for at least 2 hours. 3 Remove the top cover of the Aridus3. See Removing the Top Cover on page 86 for instructions. 90

91 Chapter 9: Troubleshooting the Aridus3 WARNING BURN HAZARD Observe any necessary safety precautions (such as heat resistant gloves) when handling hot objects. Touching the hot membrane desolvator module or spray chamber heater with bare hands may cause burns. 4 Locate the electrical connection assembly to the spray chamber heater. Spray Chamber Electrical Connection FIGURE 9-3. Electrical Connection for Spray Chamber Heater. 5 Reconnect this connection if disconnected or loose. Then reconnect the cooling fan and replace the Aridus3 cover. The membrane desolvator oven does not heat up The power cord may not be plugged into the AC wall outlet. Plug in power cord. The desolvator fuse may be blown. Replace the desolvator fuse as described on page 79 (see FIGURE 8-5). The inside electrical connection to the membrane desolvator heater (oven) may not be connected. The error below may appear from the Aridus Link software (FIGURE 9-4). 91

92 FIGURE 9-4. Membrane Desolvator Heater Error Notification. Reconnecting the membrane desolvator heater If the error in FIGURE 9-4 appears, follows the steps below: 1 Turn off power to the Aridus3 and disconnect the power cord. 2 Allow the Aridus3 to cool for at least 2 hours. 3 Remove the top cover of the Aridus3. See Removing the Top Cover on page 86 for instructions. WARNING BURN HAZARD Observe any necessary safety precautions (such as heat resistant gloves) when handling hot objects. Touching the hot membrane desolvator module or spray chamber heater with bare hands may cause burns. 4 Locate the electrical connection assembly to the membrane desolvator heater. See FIGURE 9-5. Membrane Desolvator Electrical Connection FIGURE 9-5. Electrical Connection for Membrane Desolvator Heater. 5 Reconnect this connection if disconnected or loose. Then reconnect the cooling fan and replace the Aridus3 cover. 92

93 Chapter 9: Troubleshooting the Aridus3 Mass Flow Controller Problems There is no control or intermittent control via the Aridus Link software of the Ar sweep gas flow and/or the N2 addition gas flow The power cord may not be plugged into the AC wall outlet. Plug in the power cord. Check that the DB-9F cable is securely connected between the host computer COM port and the Aridus3 COM port. If required, check that the USB to serial adapter is securely connected and that the USB to serial driver program has been loaded onto the host computer. There may be a loose connection to one or both of the Aridus3 mass flow controllers (MFCs). Reconnecting the mass flow controllers The MFCs are inside the Aridus3 cabinet. 1 Turn off power to the Aridus3 and disconnect the power cord. 2 Allow the Aridus3 to cool for at least 2 hours. 3 Remove the top cover of the Aridus3. See Removing the Top Cover on page 86 for instructions. WARNING BURN HAZARD Observe any necessary safety precautions (such as heat resistant gloves) when handling hot objects. Touching the hot membrane desolvator module or spray chamber heater with bare hands may cause burns. 4 Locate the two mass flow controllers mounted in the front, right area of the Aridus3. 5 Check that both power and communication cables are securely connected (not loose) to both mass flow controllers. Re-secure any connection if required. See FIGURE

94 Mass Flow Controller Power Cable Mass Flow Controller Communication Cable FIGURE 9-6. Aridus3 Mass Flow Controllers for Ar Sweep Gas and N2 Addition Gas. Argon sweep gas mass flow controller (MFC) will not provide a reading of at least 4.00 L/min Ar or reading is unstable The argon supply is low. Replace the argon supply, or adjust the argon supply pressure to at least 75 psig (520 kpa or 5.2 bar) Nitrogen addition gas mass flow controller (MFC) will not provide a reading of at least 10.0 ml/min of N2 flow or flow is unstable The nitrogen supply is low. Replace the nitrogen supply, or adjust the nitrogen supply pressure to at least 75 psig (520 kpa or 5.2 bar) Nebulizer / Plasma Problems Poor and/or unstable aerosol generation Insufficient nebulizer flow or pressure. The argon nebulizer gas flow should be in a L/min range. If such a flow range cannot be achieved, there may be insufficient nebulizer gas pressure. Increase inlet pressure (not to exceed 860 kpa, 125 psig, 8.6 bar). Normal operating pressure for the Aridus3 is 520 kpa (75 psig, 5.2 bar) argon pressure. If the ICP-MS cannot achieve 75 psig, alternative plumbing may be required. Capillary may be obstructed. Use the C-Flow PFA nebulizer backflush procedure (see page 76). Leak in the nebulizer gas line. Inspect the nebulizer gas line to make certain that all connections are correct and leak-free. If the line is leaking, repair with appropriate tubing. Low or no signal from the ICP-MS. Check the sample out line to make certain the FEP lining is not blocking aerosol flow to the ICP-MS torch. If the lining is in the path, recut the tubing or replace it. 94

95 Chapter 9: Troubleshooting the Aridus3 Check the O-rings in the nebulizer port on the front of the spray chamber. Worn-out O-rings may cause gas to leak out of the spray chamber. Turn off power to the Aridus3 and allow the spray chamber to cool (15-30 minutes). Remove the C-Flow PFA nebulizer and then unscrew the nebulizer port fitting and replace with a new nebulizer port fitting (which has O-rings in place). The port fitting is CETAC part number SP8015. See FIGURE 9-7. FIGURE 9-7. Nebulizer Port with 2 O-Rings. Sample flow rate problems The liquid flow rate is too high. The self-aspired liquid flow rate is determined by the nebulizer gas flow and the inner diameter of the capillary. Decreasing the nebulizer gas flow can decrease the liquid flow rate. Consequently, signal intensity may decrease as a result. Proper nebulizer gas flow rates should be optimized based on each individual application. Normal criteria for assessing performance are signal-tobackground ratios and elemental oxide levels. Liquid accumulation in spray chamber. Replace the host ICP-MS peristaltic pump drain tubing and adjust the pump shoe pressure to be slightly firm. Inspect the pump tubing on a daily basis and replace as required, especially when it becomes worn and flattened. Poor precision Non-optimized gas flows. Poor precision may be caused by non-optimum gas flows. Follow the procedure on page 40 to re-optimize the nebulizer gas, argon sweep gas, and nitrogen gas flows. Concentrated samples. More concentrated samples (>1% dissolved solids) may also cause poor precision. In addition, such samples may require longer rinse-out times. If possible, dilute the sample. Clogged or worn drain tubing. Readjustment or replacement of the host ICP-MS peristaltic pump drain tubing may be necessary to improve precision. Liquid droplets in the exhaust tubing. Check that the exhaust line from the 4 L trap bottle is free of liquid droplets and is not bent. Check that gas flow through the tubing is not obstructed. The exhaust should be vented into an appropriate laboratory fume exhaust system. 95