M-6000A Mercury Analyzer Software Manual COPYRIGHT Copyright CETAC Technologies Inc., 1998 480034 Version 1.5, October, 1998 For use with M-6000A Software REPRODUCTION All rights reserved. Reproduction or transmission of this document in whole or in part, and by any means without the express written consent of the copyright owner or authorized agent is prohibited. Requests for additional copies of this, or any other CETAC publication, can be filled by contacting an authorized distributor or CETAC Technologies Inc. Customer Service & Support 5600 South 42nd Street Omaha, Nebraska 68107, USA Phone (800) 369-2822 (USA only) Phone (402) 733-2829 Fax (402) 733-5292 E-mail custserv@cetac.com DISCLOSURE This document contains CETAC proprietary data and is provided solely to its customers for their express benefit of safe, efficient operation and maintenance of the product described herein. Use or disclosure of CETAC proprietary data for the purpose of manufacture or reproduction of the item described herein, or any similar item, is prohibited, and delivery of this document shall not constitute any license or implied authorization to do so. REVISIONS 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. WARNING Under all conditions the user must use safe laboratory procedures during the use of this product. 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. SAFETY Instruments, accessories, components or other associated materials may not be returned to CETAC Technologies if contaminated with biohazard or radioactive materials, infectious agents, or any other materials and/or conditions that could constitute a health or injury hazard to CETAC employees. Call Customer Service and Support if there is any question or doubt relative to decontamination requirements. CAUTION and WARNING statements, as applied in this document, shall be interpreted consistent with the following context: CAUTION applies only to potential property damage conditions; WARNING applies to potential personal injury conditions, in combination with or exclusive of potential property damage. All user-serviceable components are specifically identified in this document as such; the balance shall be assumed to require the expertise of a factory service technician/engineer for adjustment, repair, replacement, modification, etc. Others not so qualified and performing these actions shall do so at their own risk. Furthermore, never operate the instrument without first reading and understanding both the M6000A Mercury Analyzer Operator’s Manual and M-6000A Mercury Analyzer Software Manual and ensuring the instrument is operated safely and properly. Notices and Compliance Declarations FEDERAL COMMUNICATIONS COMMISSION (FCC) NOTICE This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to Part 15 of the FCC Rules. These limits are designed to provide reasonable protection against harmful interference in a commercial installation. This equipment generates, uses, and can radiate radio frequency energy and, if not installed and used in accordance with the instructions, may cause harmful interference to radio communications. Operation of this equipment in a residential environment is likely to cause harmful interference, in which case the user will be required to correct the interference at his own expense. CANADIAN NOTICE This digital apparatus does not exceed the Class A limits for radio noise emissions from digital apparatus as set out in the interference-causing equipment standard entitled "Digital Apparatus." ICES-003 of the Department of Communications. AVIS CANADIEN Cet appareil numerique respecte les limites de bruits radioelectriques applicables aux appareils numeriques de Classe A prescrites dans la norme sur le materiel brouilleur: "Appareils Numeriques," NMB-003 edictee par le ministre des Communications. MODIFICATIONS The FCC requires the user to be notified that any changes or modifications made to this device that are not expressly approved by CETAC Technologies, Inc. may void the user's authority to operate the equipment. CABLES Connections to this device must be made with shielded cables with metallic RFI/EMI connector hoods to maintain compliance with FCC Rules and Regulations. AD-1 Notices and Compliance Declarations POWER CORD SET REQUIREMENTS The power cord set supplied with your instrument meets the requirements of the country where you purchased the instrument. WARNING CAUTION If you use the instrument in another country, you must use a power cord set that meets the requirements of that country. This equipment is designed for connection to a grounded (earthed) outlet. The grounding type plug is an important safety feature. To reduce the risk of electrical shock or damage to the instrument, do not disable this feature. To reduce the risk of fire hazard and electrical shock, do not expose the unit to rain or humidity. To reduce the risk of electrical shock, do not open the cabinet. All maintenance is to be performed by an Authorized CETAC Service Provider. Protection provided by the equipment may be impaired if the equipment is used in a manner not specified by the manufacturer. CLEANING INSTRUCTIONS To clean the exterior surfaces of the instrument, complete the following steps: 1 Shut down and unplug the instrument. 2 Wipe the instrument exterior surfaces only using a towel dampened with a lab-grade cleaning agent. WARNING 3 Repeat step 2, using a towel dampened with clear water. 4 Dry the instrument exterior using a dry towel. Do not allow any liquid to enter the instrument cabinet, or come into contact with any electrical components. The instrument must be thoroughly dry before you reconnect power, or turn the instrument on. COOLING FAN OBSTRUCTION The instrument cooling fan(s) shall remain unobstructed at all times. Do not operate the instrument if the cooling fan(s) are blocked or obstructed in any manner. ENVIRONMENTAL Operating Temperature: Relative Humidity AD-2 10° to 30°C 0% to 95% Notices and Compliance Declarations AVERTISSEMENT AVERTISSEMENT POUR UNE PROTECTION CONTINUÉ CONTRE LES RISQUES D’INCENDIE, REMPLACER UNIQUEMENT PAR DES FUSIBLES DE MÊME TYPE ET AMPÈRAGE. TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN RÉPARATEUR QUALIFIÉ. AVERTISSEMENT NE PAS GLISSER LA MAIN SOUS OU DERIERE LES ECRANS THERMIQUES DU FOUR. GARDER LA PORTE D'ACCES AU DEVANT DU BOITIER BIEN FERMEE POUR ASSURER LA PROTECTION CONTRE LES BRULURES AVERTISSEMENT TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN RÉPARATEUR QUALIFIÉ. AVERTISSEMENT TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN RÉPARATEUR QUALIFIÉ. Notices and Compliance Declarations AVERTISSEMENT AVERTISSEMENT TOUT CONTACT AVEC LES HAUTES TENSIONS PEUT ENTRAINER LA MORT OU DES BLESSURES SÉVÈRES. CE PANNEAU NE DOIT ÊTRE ENLEVE QUE PAR UN RÉPARATEUR QUALIFIÉ. WARNING SURFACES CHAUDES, LAISSER LE COUVERCLE HERMÉTIQUEMENT FERMÉ. POUR ACCÉDER, METTRE LA TEMPÉRATURE DU FOUR À ZÉRO, OUVRIR LE COUVERCLE ET LAISSER REFROIDIR 5 MINUTES AVANT DE TOUCHER LA VERRERIE OU TOUTE SURFACE MÉTALLIQUE INTÉRIEURE. HIGH LEAKAGE CURRENT ENSURE PROPER GROUNDING AVERTISSEMENT COURANT DE FUITE ÉLEVÉ — FORNIR UNE MISE À LA TERRE EFFICACE. AVERTISSEMENT POUR LA PROTECTION PERMANENTE CONTRE UN CHOC ÉLECTRIQUE, UNE BRÛLURE DES YEUX (RADIATION UV) OU DE LA PEAU, LAISSER LE COUVERCLE HERMÉTIQUEMENT FERMÉ LORSQUE L’APPAREIL EST SOUS TENSION. LAISSER REFROIDIR 5 MINUTES (APPAREIL ÉTEINT) AVANT D’ENLEVER LE COUVERCLE. AD-4 Contents M-6000A Mercury Analyzer Software Manual Contents Contents Preface viii 0.1 Who Should Read This Book viii 0.2 How to Use This Book viii 0.3 Conventions Used in This Book 0.3.1 Where to Go for More Information 1 Introduction ix xi 1-2 1.1 The Hardware 1-2 1.1.1 ASX-500 or ASX-500 Model 510 Auto Sampler 1-2 1.1.2 M-6000 Mercury Analyzer 1-2 1.1.3 ADX-500, Auto Dilutor Accessory 1-3 1.2 Absorbance Signal 1-3 1.3 Template 1-3 1.4 Worksheet 1-4 1.4.1 1.4.2 1.4.3 1.4.4 Standards and Samples Time Profile Zero the M-6000A Calibration 1.5 Analysis of Samples, Step by Step ii 1-6 1-6 1-7 1-8 1-8 M-6000A Mercury Analyzer Software Manual Contents 2 Preparing for the Software Installation 2.1 M-6000A Software System Requirements 3 Installing the M-6000A Software 2-2 2-2 3-2 3.1 Installing the Hardware 3-2 3.2 Installing the Software 3-2 3.2.1 The Borland Database Engine 3.2.2 CETAC M-6000A Mercury Analyzer Software 3-2 3-3 3.3 Microsoft Windows 3.1 3-3 4 Verifying the Installation 4-2 4.1 Software Selftests 4-2 4.2 Verifying Hardware/Software Requirements 4-2 4.3 Verifying the Installation 4-3 4.4 Testing the Interface 4-3 4.5 System Check in the Software 4-3 4.6 Verify The Software Configuration of COM Ports Manually 4-4 4.6.1 Using Windows’ Terminal Program 4-4 iii M-6000A Mercury Analyzer Software Manual Contents 5 Using the M-6000A Software 5.1 Part I: Software Reference 5.1.1 5.1.2 5.1.3 5.1.4 Worksheet Options: Report Options: Administration Options Exit 5.2 Worksheet Options 5.2.1 Load Worksheet Dialog Box 5-2 5-2 5-3 5-3 5-3 5-3 5-4 5-4 5.3 Filing Tab 5-6 5.4 Develop Tab 5-7 5.4.1 5.4.2 5.4.3 5.4.4 Measurement Sub-Tab Standards Sub-Tab QC Sub-Tab Notes Sub-Tab 5.5 Labels Tab 5.5.1 Load Samples From Disk 5.5.2 Setup Auto Dilutor and ASX-500 Racks 5.5.21 Auto Diluter Setup 5.5.3 Autofill 5.5.4 Clear 5.5.5 Common Sample Parameters 5.5.6 The Labels Grid Popup Menu 5.6 Analysis Tab 5.6.1 Start 5.6.2 Stop 5.6.3 Read 5.6.4 Sample Label 5.6.5 Concentration 5.6.6 %RSD 5.6.7 Mean ABS 5.6.8 Tube # 5.6.9 Sample Label 5.6.10 g/L 5.6.11 Signal Profile Chart 5.6.12 Changing Worksheet Parameters with the Signal Profile Chart iv 5-8 5-18 5-21 5-24 5-24 5-25 5-26 5-27 5-28 5-28 5-28 5-29 5-31 5-31 5-31 5-32 5-32 5-32 5-33 5-33 5-33 5-33 5-33 5-34 5-35 M-6000A Mercury Analyzer Software Manual Contents 5.6.13 Calibration Data Chart 5.6.14 Inspecting the Calibration Data 5.6.15 Anaysis Grid Popup Menu 5.7 Menu Options 5-37 5-38 5-39 5-39 5.7.1 File 5.7.2 Instrument 5-39 5-43 5.8 Report Options 5-49 5.8.1 5.8.2 5.8.3 5.8.4 Settings Tab Data Tab Report Tab Significant Figures and Rounding 5-50 5-53 5-56 5-57 5.9 M-6000A as a DDE Server 5-57 5.10 Part II: M-6000A Software Operation 5-58 5.10.1 5.10.2 5.10.3 5.10.4 5.10.5 5.10.6 5.10.7 5.10.8 5.10.9 A. Creating a Worksheet B. Auto Sampler Labels C. Automatic Attenuation (Zero the Instrument) D. Instrument Calibration E. M-6000A Controls F. Printing Reports G. Automated Detection Limit Function H. Saving Worksheet as a Template I. Recall a Stored Template 6 Maintaining the M-6000A Software 5-59 5-63 5-63 5-64 5-64 5-65 5-66 5-66 5-67 6-2 6.1 Overview 6-2 6.2 Deleting Old Templates and Worksheets 6-3 6.3 Security 6-3 6.3.1 Password Protection 6.3.2 Access Levels 7 Troubleshooting the M-6000A Software 7.1 Hardware Problems 6-3 6-4 7-2 7-2 v M-6000A Mercury Analyzer Software Manual Contents 7.1.1 Verify All Connections 7.1.2 Verify the COM Port Configuration 7-2 7-2 7.2 Software Problems 7-3 7.3 Printing and Windows 7-7 7.4 When All Else Fails 7-9 8 Glossary 9 Index vi G-2 I-2 Preface Preface The M-6000A Mercury Analyzer Software Manual provides an overview and explains the theory of operation of the CETAC M-6000A Mercury Analyzer and its custom software. 0.1 Who Should Read This Book The primary audience for the M-6000A Mercury Analyzer Software Manual consists of laboratory managers, chemists, technicians, fieldservice engineers and owners of the M-6000A. To use this manual safely and effectively, at least a general knowledge of chemistry, electronic or laboratory equipment, and basic chemical handling procedures are required. WARNING Before operating the M-6000A or the ASX-500 or ASX-500 Model 510, it is important to read the M-6000A Mercury Analyzer Operator’s Manual and the ASX-500 or ASX-500 Model 510 Auto Sampler Operator’s Manual. 0.2 How to Use This Book The M-6000A Mercury Analyzer Software Manual contains 7 chapters. Read the chapters sequentially the first time. Thereafter, refer to the chapters separately as needed. The first chapter provides an introduction to the Mercury Analyzer. Subsequent chapters detail the design, replaceable components, and troubleshooting procedures associated with the M-6000A software. These 7 chapters are followed by a glossary of related terms and an index. M-6000A Mercury Analyzer Software Manual Preface 0.3 Conventions Used in This Book This book uses certain conventions to distinguish different types of information easily. This section describes these conventions. Instructions All step-by-step instructions are numbered and in bold, as in the following example. 1 Open the M-6000A Mercury Analyzer Software. Many numbered instructions are followed by more detailed explanations. Menu Items This book uses the following format for referring to menu items: Settings»Communication The text before the arrow symbol is the name of the menu; the text after the arrow symbol is the menu choice. Notes Notes contain a reminder about the effect of particular actions. They are indicated as follows: ix M-6000A Mercury Analyzer Software Manual Preface Note: This example shows how a note is displayed. Cautions Cautions indicate situations that require immediate attention to prevent harm to the M-6000A Mercury Analyzer. Cautions are indicated as follows: CAUTION This example shows how a caution is displayed. Warnings Warnings indicate situations that could cause bodily harm. Warnings are indicated as follows: WARNING This example shows how a warning is displayed. x M-6000A Mercury Analyzer Software Manual Preface 0.3.1 Where to Go for More Information In addition to the M-6000A Mercury Analyzer Software Manual refer to the following resources: The M-6000A Mercury Analyzer Operator's Manual The ASX-500 or ASX-500 Model 510 Auto Sampler Operator’s Manual EPA Method 245.1; method for Hg determination in drinking water. SW846 Method 7470A; Mercury in Liquid Waste (Cold-Vapor Technique) SW846 Method 7471A; Mercury in Solid or Semisolid Waste (ColdVapor Technique) ASTM D3223-91; Standard Test Method for Total Mercury in Water CETAC Technologies Customer Service and Support: Tel: 1 (800) 369-2822 (USA only) Tel: 1 (402) 733-2829 Fax: 1 (402) 733-5292 eMail: custserv@cetac.com xi M-6000A Mercury Analyzer Software Manual Preface xii 1 Introduction 1. Introduction The M-6000A software is designed to assist the user in the mercury analysis of large numbers of samples. The software allows for the manipulation of many different settings. To get the most out of the software, it is necessary to understand how some of these settings interact. 1.1 The Hardware The M-6000A Mercury Analyzer System consists of an Auto Sampler (an ASX-500 or ASX-500 Model 510), the M-6000A Mercury Analyzer, and the host PC. An ADX-500 Auto Dilutor Accessory may also be added to automatically dilute and reanalyze samples. The Auto Sampler and the M-6000A Mercury Analyzer are connected to the host PC’s COM ports allowing communication of data and commands to and from the software. 1.1.1 ASX-500 or ASX-500 Model 510 Auto Sampler The Auto Sampler takes instructions from the PC host and moves the sipper to the samples, rinse, and standards. 1.1.2 M-6000A Mercury Analyzer The M-6000A sends a stream of absorbance values and times to the PC host. Absorbance values are optically calibrated micro-absorbance units (µAbs or 10-6 A) that, when processed through a pre-established, mathematically fitted, calibration curve (of mercury concentration vs. µAbs), will determine the final Hg concentration of a sample. When pre-defining a calibration curve, the micro-absorbance units (µAbs) are mathematically correlated with 0concentrations of known standards. M-6000A Mercury Analyzer Software Manual Introduction 1.1.3 ADX-500 Auto Dilutor Accessory An ADX-500 Auto Dilutor Accessory must be attached to the ASX-500 Model 510. It is designed to also work in conjunction with the M-6000A Mercury Analyzer. It adds the ability to automatically dilute and reanalyze samples which are over the calibration range. It supplies on-line dilution of the sample controlled by user programmable software. Samples are diluted by a factor of 1:10, with sequential dilutions available as a software option. The user can configure the software to dilute samples (1) upon over-range of the calibration curve, where the intensity is above the high standard or (2) upon saturation of the detector. For further information, see the ADX-500 Auto Dilutor Accessory Operator's Manual and sections 5.5.2 and 5.7.2.4 of this manual. 1.2 Absorbance Signal The Absorbance Signal refers to the graph of Abs vs. time created by recording the absorbance values sent from the M-6000A to the software over a period of time. Using the Time Profile defined by the analyst, the Absorbance Signal is converted, through the software, into data for a sample (1st and 2nd Baseline Correction points, replicates, and finally a Concentration and %RSD). 1.3 Template A Template is a predefined configuration that can be used to quickly create a Worksheet (see below) using common parameters for the type of analysis to be done. 1-3 M-6000A Mercury Analyzer Software Manual Introduction For example, a lab may have different levels of detection sensitivity needed for different tasks. This lab may have two Templates. The lab may have one “High Throughput” Template that will record data for high concentration samples at a rate of 1 sample per minute. The lab may also have a “High Sensitivity” Template to analyze low concentration samples at a rate of 1 sample every 3 minutes. To make a Template, it is only necessary to create a Worksheet with the desired parameters, and then save it as a Template. See Section 5.1. 1.4 Worksheet A Worksheet is the “document” consisting of a complete set of saved operating parameters. The Worksheet tells the Auto Sampler and the M-6000A how to analyze samples. Worksheets allow the user to conveniently use the instrument repeatedly under a fixed set of operating conditions without having to re-enter the parameters each time. Different worksheets may be employed to optimally handle different tasks. Worksheets can easily be modified, locked against further modification, replicated, or created from an already defined template. There are several settings in the Worksheet that determine how the system will operate. Table 1-1 shows different worksheet settings to provide several different DL ranges. Following Table 1-1 is a brief description of these settings. 1-4 M-6000A Mercury Analyzer Software Manual Introduction Throughput vs. sensitivity: RANGE #1: HIGHEST SENSITIVITY MODE Application: Very Low Concentration Range Gas Flow Sample Time (for Liquid Uptake or Autosampler "Sip") Rinse Time Baseline Correction Method Expected Results: Detection Limit(nominal): Sample Throughput Rate (minutes/sample) Approximate Drying Agent Life RANGE #2: GOOD SENSITIVITY MODE Application: Medium Throughput Range Gas Flow Sample Time (for Liquid Uptake or Autosampler "Sip") Rinse Time Baseline Correction Expected Results: Detection Limit: (nominal) Sample Throughput (Rate minutes/sample) Approximate Drying Agent Life RANGE #3: HIGH THROUGHPUT MODE Application: High Throughput Range Gas Flow Sample Time (for Liquid Uptake or Autosampler "Sip") Rinse Time Baseline Correction Method Expected Results: Detection Limit: (nominal) Sample Throughput Rate (minutes/sample) Approximate Drying Agent Life 0.002 - 0.5 PPB 40 mL/min 60 s 120 s 2 point 0.001 ppb 3 min/sample 1 week 0.05 - 12.0 PPB 100 mL/min 30 s 30-45 s 1 point 0.015 ppb 1 min/sample 1 week 0.2 - 30 PPB 300-350 mL/min 20 s 20 s 1 point 0.050 ppb 40 sec/sample 1 day Table 1-1. Instrument Parameters to Optimize Throughput vs. Sensitivity. 1-5 M-6000A Mercury Analyzer Software Manual Introduction 1.4.1 Standards and Samples In each Worksheet the locations of standards, types of sample trays, and samples in the Auto Sampler must be identified to the software. The standards will be used to calibrate the M-6000A, so that the analysis of the samples will be accurate. These parameters can be saved in a template. 1.4.2 Time Profile To ensure that baseline and sample measurements are taken at the proper time, a preliminary “training session” using a mercury standard must be carried out to create a precisely synchronized Time Profile specific to each Worksheet. The training session should be repeated to update the Time Profile each time the worksheet is used. When choosing a standard to train on, the highest concentration standard will take the longest time to reach its peak and the longest time to rinse out. Using the high standard will ensure that for every other standard or sample taken, the Time Profile will fit appropriately. The Time Profile consists of the times at which the following happen: 1 The Auto Sampler Sipper starts in the rinse station. 2 The Auto Sampler moves to a specified sample tube, drops the sipper into the sample, and the M-6000A begins to send data. This is “Time Zero”. 3 If the 1st Baseline Correction Point has been defined, then during the delay time (before the sample reaches the M-6000A Mercury Analyzer) the M-6000A sends data for the 1st Baseline Correction Point (measured while rinse solution is still in the M-6000A). 4 Once the sample arrives in the sample cell of the M-6000A, the M-6000A sends data for the sample to the host PC. 1-6 M-6000A Mercury Analyzer Software Manual Introduction 5 Once the Auto Sampler has sipped sample for the specified time, it will move back to the rinse station. 6 If the 2nd Baseline Correction Point has been defined, after the sample clears and more rinse solution enters the analyzer, the M-6000A sends data for the 2nd Baseline Correction Point. 7 The system is now ready for the next sample. The Time Profile is defined by the analyst in a worksheet. This is described later in detail in Section 5.1. Training can be done manually by adjusting the values on the Develop Tab of the Worksheet Form, or (preferably) automatically using the mouse and the Signal Profile Chart on the Analysis tab of the Worksheet Form. These parameters can be saved in a Template and will be valid as long as all tubing lengths, diameters, and pressures do not change. Use of the Quality Control (QC) feature will lock a worksheet. Locking a worksheet is permanent. It is possible to duplicate the worksheet by creating a new one and reentering the parameters. 1.4.3 Zero the M-6000A Each time the instrument is set up to run, there will be minute changes in the baseline signal level of the M-6000A. This will be due to changes in temperature, gas flow, etc. It is vital that the M-6000A be sufficiently warmed up before each use, or any data taken from the M6000A will be variable, due to the “baseline drift” of the improperly warmed up system. See the M-6000A Operator’s Manual for information on this topic. In order to account for changes in the signal, the M-6000A can Zero itself mechanically. Mechanical Zeroing is initiated by the analyst with the “Zero” feature under the main menu (Instrument»Zero). This feature is activated prior to analysis (not during analysis). Zeroing should be performed at least daily, to ensure that the M-6000A is operating optimally. 1-7 M-6000A Mercury Analyzer Software Manual Introduction 1.4.4 Calibration Once the Time Profile has been established, a calibration must be run from the Standards of known Hg concentrations. This may be a linear or a quadratic calibration. The calibration process will measure the absorbance of several known standards, and then fit a “curve” to the data collected from the standards. 1.5 Analysis of Samples, Step by Step Briefly, from start to finish, here is the step by step process for an unattended analysis: 1 Open a new worksheet. See Section 5.1. 2 Define the sample gas flow rate, using the Develop tab’s Measurement sub-tab. This parameter, more than any other, will affect the instrumental sensitivity and sample flow rate. See Section 5.4.2. 3 Start defining the Time Profile. Define the number of integrations using the Develop tab’s Measurement sub-tab. The Sample and Baseline Correction Point times are defined later. See Section 5.4.2. 4 Define the location of standards using the Develop tab, Standards sub-tab. See Section 5.4.3. 5 Define the labels of the samples using the Labels tab. Be sure that the sample tray types in the Auto Sampler match the tray types on the software. See Section 5.5. 6 Finish defining the Time Profile by reading a test Absorbance Signal using the Read button on the Analysis tab. 1-8 M-6000A Mercury Analyzer Software Manual Introduction Once this has been done, it will be necessary to set cursors, with the mouse, to mark the Signal Profile Chart for the exact times at which the Baseline Correction Points should be acquired and between which points (start/stop) the sample peak reading should be taken. Whenever running an initial Time Profile, use the highest concentration standard. The concentration of this standard should be greater than that of any sample to be analyzed. Use this standard because the time it takes to reach the peak of the Absorbance Signal will be greater than that of any lower standard or sample. Any Time Profile that fits the Absorbance Signal of the high standard can be presumed to also work for a lower standard or sample. The time parameters may be changed using the mouse to click and drag on the Signal Profile Chart. See Section 5.6. 7 Zero the instrument using the Instrument menu. See Section 5.7.2. 8 Calibrate using the Instrument menu. See Section 5.7.2. 9 Start the overall unattended analysis process using the Start button on the Analysis tab. See Section 5.6.1. The above is an outline of the steps needed to perform an unattended analysis. More detail will be presented in the chapters to follow. 1-9 M-6000A Mercury Analyzer Software Manual Introduction ` 1-10 2 Preparing for the Software Installation 2. Preparing for the Software Installation To install the M-6000A Mercury Analyzer Software, be sure that the PC intended as the host meets the system requirements. 2.1 M-6000A Software System Requirements The M-6000A Software is designed to run with the following PC configuration: IBM Compatible Microcomputer based on an Intel model 486/33 or better. For best results a 486/66 or 586. 8 Megabytes of RAM. For best results at least 12 Meg of RAM and at least 16 Meg for Windows95. Microsoft Windows 3.1, Windows for Workgroups or Windows95 installed. 3 1/2” floppy disk drive. Printer with Windows Driver. 2 Free COM Ports. Local Bus Video running a 800 by 600 resolution monitor. PS/2 or Bus Mouse. It is necessary to have 2 free COM ports available, one each for the Auto Sampler and the M-6000A. A mouse is also required to run the software. 2-2 3 Installing the M-6000A Software 3. Installing the M-6000A Software 3.1 Installing the Hardware Be sure to install the Auto Sampler and the M-6000 Mercury Analyzer instruments before installing the M-6000A software. See the M-6000A Mercury Analyzer Operator’s Manual and the ASX-500 or ASX-500 Model 510 Auto Sampler Operator’s Manual for more information. 3.2 Installing the Software The installation of the M-6000A software is a two step process. First the database engine, and then the instrument control software must be installed. 3.2.1 The Borland Database Engine To make the M-6000A Mercury Analyzer Software responsive and robust, the M-6000A uses Borland International’s Database Engine. To install the database engine: 1 Start Windows. 2 Insert BDE (Borland Database Engine) Disk 1 in A: 3 From the Program Manager, Select File»Run. 4 Type a:\setup and press enter. 5 Follow the on-screen prompts. M-6000A Mercury Analyzer Software Manual Installing the M-6000A Software 3.2.2 CETAC M-6000A Mercury Analyzer Software To install the CETAC M-6000A Mercury Analyzer Software: 1 Start Windows. 2 Be sure the Borland International Database Engine is installed. If it has not been installed, do so now. 3 Insert Mercury Analyzer disk 1 in A: 4 From the Program Manager, Select File»Run. 5 Type a:\install and press enter. 6 Follow the on-screen prompts. 3.3 Microsoft Windows 3.1 If the software is intended to be run in a Windows 3.1 environment, then SHARE.EXE must be loaded before starting Windows. You can load it manually by typing the following command from the DOS prompt: SHARE.EXE /L:50 The easiest way to load SHARE automatically is to add the above line to the computer's AUTOEXEC.BAT file. It will then load each time the computer is turned on. The AUTOEXEC.BAT file is found in the C:\ directory and is a plain ASCII text file. The Notepad program that comes with Windows 3.1 (in the Accessories folder) can be used to edit this file. The line SHARE.EXE /L:50 should be added after the PATH statement in the AUTOEXEC.BAT file. The SHARE command is not necessary if Windows for Workgroups or Windows95 is used. 3-3 M-6000A Mercury Analyzer Software Manual Installing the M-6000A Software 3-4 4 Verifying the Installation 4. Verifying the Installation 4.1 Software Selftests The software will automatically self-test when started, and periodically check the M-6000A and the Auto Sampler to ensure they are still connected and on-line. However, some procedures to verify and troubleshoot installation follow. 4.2 Verifying Hardware/Software Requirements 1 A bus mouse (or PS/2 mouse) is specified for use with the Mercury analyzer to ensure that the mouse cannot conflict with the instrument’s COM port requirements. 2 Initially it is recommended that no FAX/Modem should be installed. 3 It is recommend that the UART controlling the Serial communications should be 16550A (as opposed to the older 8250). This will lead to improved communications under Windows 3.11. This should be almost universal on new computers. Use Ms-DOS 6.2’s MSD.EXE to verify this, if difficulties are encountered. 4 Microsoft Windows for Workgroups 3.11 is optimal (Microsoft Windows 3.1 is also acceptable.) If the software environment is Windows 3.1, be sure that SHARE.EXE is loaded before starting Windows. The line “SHARE /L:50” should be in the computers AUTOEXEC.BAT preceding Windows starting. M-6000A Mercury Analyzer Software Manual Verifying the Installation 4.3 Verifying the Installation Once installation of the M-6000A system is complete, it is important to verify that the system is installed correctly. CAUTION Attempting to use the M-6000A before ensuring that all components are installed correctly may result in damage to the system. 4.4 Testing the Interface If the communications interface between the host computer and the M-6000A system are not established correctly, the system will not function. Before testing the interface, ensure that the port connectors are attached to the M-6000A and the host computer. Be sure that all power switches are on and all R-S232 COM port connections are correct (see Section 3.3, PC Interface). When the software is initializing, it will test the connections to the M-6000A Instrument and the Auto Sampler. 4.5 System Check in the Software The M-6000A software runs a test routine at startup to test the various interfaces throughout the system and give a report on the status of the interface. 4-3 M-6000A Mercury Analyzer Software Manual Verifying the Installation 4.6 Verify The Software Configuration of COM Ports Manually Should the software not find the M-6000A and the Auto Sampler on the correct ports, it may be necessary for the analyst to test them using the M-6000A software and the TERMINAL.EXE program provided with Windows. The standard configuration for the system is to connect the Auto Sampler to COM1 and the M-6000A to COM2. To set the configuration in the M-6000A software; 1 Open the M-6000A software. 2 Click on the “Worksheet” button on the toolbar 3 Choose “open” and pick a worksheet. Press OK. 4 If there is no worksheet to choose from, create a new one. 5 This is the Worksheet View. To bring up the configuration menu, pick “File»Configuration” from the menu and verify the Auto Sampler and the M-6000A are configured/connected to the correct COM ports. If the configuration differs from the standard, reset the M-6000A to COM2 and the Auto Sampler to COM1. 4.6.1 Using Windows’ Terminal Program The Windows’ Terminal program (TERMINAL.EXE in the Windows directory) can be used to manually verify the communication through each serial port. Each device communicates at 9600-8-N-1 (9600 baud, 8 data bits, no parity, 1 stop bit) with no flow control. Both will respond to the command VER (capitalization is important). 4-4 M-6000A Mercury Analyzer Software Manual Verifying the Installation The M6000 will respond ‘CETAC Technologies, Inc. Mercury Analyzer ...’. The Auto Sampler will respond ‘CETAC Technologies ASROM...’. If the responses are not received as expected, or on the expected COM ports, then this will indicate a hardware or Windows configuration problem. Note: This manual assumes the reader and operator of the M-6000A Mercury Analyzer has a working knowledge of how to use standard Windows applications. For more information on how to use Windows, see your computer’s documentation. To check the communication through the COM ports in Windows to the M-6000A and Auto Sampler, do the following: 1 Select “File»Run” from the menu at the top of the Program Manager. 2 Type “TERMINAL” and press enter. 3 Select “Settings»Communications” in the Terminal program. 4 Make the dialog box look like Figure 4-1. The Connector setting in the lower right of the dialog box selects which COM port commands will be sent to. 4-5 M-6000A Mercury Analyzer Software Manual Verifying the Installation Figure 4-1 - Terminal Program, Settings»Communications dialog. 5 In the Connector listbox, select the COM port that the M-6000A instrument is connected to and press OK. The default is COM2. 6 Type “VER” in all caps and press return. If the M-6000A Instrument does not respond ‘CETAC Technologies, Inc. Mercury Analyzer - ...’ then check for loose cables and verify that no other program is using the port (fax software etc.) and cycle the power on the M-6000A. It will return “OK” if connected properly. If this fails, contact your System Administrator for assistance. CETAC Technologies offers an economical PC to work with the M6000A system that is known to have the proper hardware configuration. 7 Select Settings»Communications once again. This time, select the COM port that the Auto Sampler is connected to (the default is COM1) and press return. Type “VER” all in caps and press return. If the Auto Sampler does not respond ‘CETAC Technologies ASROM...’ then there is a cable connection, software configuration, or hardware problem (See step 6 above). 4-6 5 Using the M-6000A Software 5. Using the M-6000A Software This chapter contains two parts. The first part is a detailed reference of the features of the M-6000A Software (Version 1.5). The second will walk the analyst through several everyday functions of the M-6000A Mercury Analyzer System, to familiarize them with the instrument. 5.1 Part I: Software Reference When first opening the M-6000A software, the user will be offered four separate Menu Options on the CETAC M-6000A Toolbar (Fig. 5-1). These Menu Options include: Worksheet, Reports, Administration and Exit. The next few sections cover the operation of the M-6000A through the use of the M-6000A System software menus. Figure 5-1. The CETAC M-6000A Software Toolbar. M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.1.1 Worksheet Options: Briefly the Software Options on the CETAC M-6000A Toolbar allow a user to: Create a new Worksheet from scratch or derive a new Worksheet from a Template. Define Standards and Samples. Zero the M-6000A. Run a Time Profile. Calibrate the M-6000A. Analyze Samples. Define a Template from the current Worksheet. Activate and configure the QC features. 5.1.2 Report Options: Report on a data set from a worksheet. Select data parameters for the report. Preview the printed report. 5.1.3 Administration Options Administration Options are covered in Chapter 6. 5.1.4 Exit Exit will close the software. 5-3 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.2 Worksheet Options Collecting data is done through a conceptual object called a Worksheet. Each worksheet contains information about a M-6000A configuration used to analyze samples; Time Profile to be used, standards and sample locations, etc. The manipulation of Worksheets is done through the Worksheet Options (Fig. 5-2) on the CETAC M-6000A Toolbar. Figure 5-2. The CETAC M-6000A Worksheet Options Menu. 5.2.1 Load Worksheet Dialog Box Once a user clicks on the Worksheet Options, they will be presented the Load Worksheet Dialog Box (Fig. 5-3). From this dialog, users may create new worksheets from scratch, use a predefined template as the basis for a new worksheet, or load existing worksheets. Once a worksheet is loaded/created, the user is taken to (Fig. 5-4) the Worksheet Form. 5-4 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.6.6 %RSD This is the % Relative Standard Deviation that the software has determined using the number of replicates defined. 0.5% - 1.5% is the normal range for the %RSD, unless the concentration of the sample is near the detection limit of the current M-6000A setup. 5.6.7 Mean ABS This is an average of the concentration in micro absorbance units. 5.6.8 Tube # This data grid shows the progress and results of the analysis. This field is the tube number in the ASX-500 or the ASX-500 Model 510. Note that right-clicking on this grid will popup a menu allowing the analyst to clear the grid and to show all the data on a specific sample. 5.6.9 Sample Label This field is the label of the sample tube that was defined in the Labels tab. 5.6.10 µg/L This is the concentration unit of the sample. 5-33 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.6.11 Signal Profile Chart This chart shows an Absorbance Signal, consisting of data points sent to the PC from the M-6000A. It can be used to visually examine and edit the Time Profile. There are several buttons on this chart that are described below: Camera This will copy the data to the clipboard as a graphic (in bitmap format). Scissors This will copy the data to the clipboard as unformatted text (x and y value pairs). Magnifying Glass This will adjust the x-axis scale of the chart. Chart with Eraser This will clear and reset the chart Up arrow This button will toggle the chart between its current size and a fullscreen size. Popup menu Clicking the right mouse button on the Signal Profile Chart will display a popup menu that can toggle the Lockdown and Print the chart, and enable/disable baseline correction. 5-34 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.6.12 Changing Worksheet Parameters with the Signal Profile Chart Refer to Figure 5-14. In order to manipulate the Time Profile using the Signal Profile Chart, the Sample Time Lockdown checkbox on the Develop tab must be clear. Right clicking with the mouse on the chart will popup a menu allowing the analyst to enable or disable the lockdown. Note: Use the Read button to display data for the high standard in the Signal Profile Chart. See all of Section 5.11.1 for details. Figure 5-14. Signal Profile Chart, Maximized. There are three parameters of the worksheet that can be manipulated using this chart. These parameters are: 5-35 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software Sample Time The current sample time on the chart will start at the dark green vertical line and stop at the light red vertical line. Using the mouse, the analyst may define the sample time by clicking on the chart and dragging to the right. The integration times will automatically be recalculated based on the new total sample time. 1st Baseline Correction Point The current 1st Baseline Correction Point on the chart will start at the light blue vertical line and stop at the dark red line. Using the mouse and the shift key, the analyst may change the point times by clicking on the chart and dragging to the right. To do this, press and hold the shift key. Then click, with the left mouse button, on the left limit of the part of the signal to be used as the baseline correction point. A light blue vertical cursor line will appear. Next, without releasing the shift key or the left mouse button, drag the mouse to the right, until the portion of the signal to be used as the baseline correction point is between the light blue and dark red cursor lines. Release the shift and the mouse key, and the chart will update the baseline times in the worksheet. 2nd Baseline Correction Point The current 2nd Baseline Correction Point on the chart will start at the light green vertical line and stop at the purple line. Using the mouse and the control key, the analyst may change the point times by clicking on the chart and dragging to the right. See the description in the 1st Baseline Correction Point section above. 5-36 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.6.13 Calibration Data Chart This chart can be used to visually examine the calibration curve. The green dots are the calibration standard data point markers. Note: Clicking the right mouse button on the Calibration Data Chart will display a popup menu that can turn on and off the data point markers, copy the chart to clipboard, print the chart or allow inspection of the Calibration Data. There are several labels in the lower right-hand corner of the calibration graph (at the top left window of Figure 5-15, see Int., Slope, Correlation) that are described below. These next three fields describe the calibration line/curve. Intercept The Intercept is the value of the constant component of the calibration curve. Slope When a Linear calibration is used, this is the slope of the calibration curve. When a Quadratic calibration curve is used, this is the linear component of calibration curve. Curve When a Quadratic calibration curve is used, this is the quadratic component of the calibration curve. Correlation R2 from regression = correlation. A 0.997 is considered the minimum acceptable correlation coefficient. 5-37 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.6.14 Inspecting the Calibration Data By clicking the right mouse button on the Calibration Data chart you can open the Inspect Calibration Data window. The calibration type (linear/quadratic) being used to fit the calibration data can be changed, a single data point from the calibration standards can be disregarded simply by deselecting the desired standard in the Standards to Include listbox. Slope, Intercept and Correlation are updated on the Calibration Data chart (at the top left window of Figure 5-15) as these changes are made. If the raw scan data was stored, it will be displayed in the Signal Profile chart (at the bottom left window of Figure 5-15). The currently visible plot can be modified with the VCR control on the bottom right of this chart. Figure 5-15. Calibration Data Information. 5-38 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software If any changes made are saved, then the new calibration information goes into effect immediately, and any samples subsequently analyzed with this worksheet will reflect the new calibration curve. 5.6.15 Analysis Grid Popup menu Right clicking on the Analysis grid will display a popup menu that can clear the Analysis grid or display a form that allows inspection of the analysis data on a more detailed level. See Figure 5-21 for this more detailed sample information. 5.7 Menu Options 5.7.1 File The File menu is a complement to the Filing Tab. The main Menu options are: New Worksheet, Open Worksheet, Save Worksheet, Close Worksheet, etc. The following options need further explanation: New Output File causes the current output file to be closed and a new one to be opened. System Configuration brings up a dialog box with 4 tabs. See Figure 5-16 for these options. 5-39 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software Figure 5-16. The System Configuration Menu Dialog Box. The four tabs available in the System Configuration dialog box are: Serial Communications (Tab 1) The Serial Communications tab allows the analyst to specify COM port configurations different than the default for the Auto Sampler and the M-6000A. The default is to use the M-6000A on COM2 and the Auto Sampler on COM1. Calibrate Gas Flow (Tab 2) Should the analyst need to recalibrate the M-6000A software for the current gas configuration, it can be done from this dialog box. The process takes about 5 min. Recalibration should be done whenever the analyst switches between Ar and N2, changes the gas filter on the back of the instrument, changes the drying agent, and as quarterly maintenance. 5-40 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software The analyst will need a gas flow meter to complete the operation. Connect the gas flow meter to the exhaust port on the back of the M-6000A. Initiate the calibration. Input the values as prompted by the software. Directories (Tab 3) This tab displays the directories the M-6000A software uses to store information. They cannot be changed. Preferences (Tab 4) This tab allows the analyst to configure some default preferences of the software. The following System Configuration preferences (Figure 5-16) are available: Display EPA MDL expiry warnings reminds you of the EPA Method Detection Limit Procedure which has an expiration date of 90 days. Autoscale signal profile chart allows the Y-axis scale to automatically adjust to the concentration of a sample. Smart Rinse delays analysis until the signal returns to the baseline. This is useful after a highly concentrated sample has been analyzed. If enabled, the smart rinse will watch for conditions where a very high concentration sample saturated the detector system. If this occurs, then a prolonged rinse will be performed to avoid having memory effects invalidate the measurements on subsequent samples. Smart rinse is only active when a batch of samples is being analyzed. Saturation Error Message on Report By default concentrations are printed on the final report, even if the instrument saturates (as would be indicated by the error flags that appear on the report.) If this behavior is not desired, then this option can be enabled and it will cause a short error message to appear on the report in place of the 5-41 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software concentration for saturated samples. Sipper Depth sets the maximum depth to which the sipper is lowered when sampling. In some circumstances it may be undesirable for the Auto Sampler probe to push all the way to the bottom of the test tube (for example, if sediment is present). The depth to which the sipper is lowered can be customized. Startup Gas Rate - This specifies the gas flow rate that the instrument sets when the M-6000A software is first started up. It can of course later be reset either by a worksheet when samples are analyzed or from the M-6000A controls window. Display Wt./Vol. corrected conc. controls whether concentrations are automatically corrected by the M-6000A software. Calibrate before each batch controls the default behavior of the dialog box, either calibrating before each new batch or not. Print report after each batch controls the default behavior of the dialog box that pops up when the Start button is pushed on the Analysis tab. Zero before each batch controls the default behavior of the dialog box, either invoking AutoZero before each new batch or not. New output file before each batch controls the default behavior of the dialog box, either automatically creating a new output file for each new sample or not. Default Weight and Default Volume control the defaults placed in the weight and volume options on the Labels tab during an Auto Fill operation. Default Tray Type sets the default tray size for the next sample. When a new worksheet is created (and a template is not used) the Auto Sampler tray type will be the one defined here. 5-42 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software 5.7.2 Instrument 5.7.2.1 Zero the M-6000A This will mechanically Zero the M-6000A instrument. Within certain limits, the effect of this process will compensate for baseline offsets due to microscopic dust buildup on the optics of the M-6000, dirty sample windows, and thermal drift. It is vital that this procedure be run at least once a day for proper analysis results. Zeroing should be preceded by an adequate instrument warm-up period (approx. 90 minutes from “cold start.” See the M-6000A Mercury Analyzer Operator’s Manual for exact warm-up details). It will also be necessary to rezero after any gas flow changes or after any operations involving start/stop of gas flow, any gas tubing disconnect, change of oven temperature, opening the front door, removal of any portion of the instrument case, or change of drying agent. Allow sufficient stabilization time following any such operation before zeroing. 5.7.2.2 Calibration This will run a calibration using the parameters defined in the Develop - Standards subtab. 5-43 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software Note: It is important that the instrument be recalibrated every day to maintain optimum sensitivity and reproducibility. Recalibration is also required upon changing worksheets or following gas flow change, or most any other change. 5.7.2.3 Detection Limit The M-6000A Software allows the analyst to determine several statistics that evaluate the current setup of the M-6000A. These are the Instrument Detection Limit (IDL) and the Method Detection Limit (MDL). Instrument Detection Limit To determine the IDL, the M-6000A software analyzes the blank 5-11 times, as specified by the user, to determine the standard deviation of the blank signal (σ) in micro-absorbance units. It then runs an analysis of a standard described by the user to calibrate the σ value in ppt. Three times this value defines the Instrument Detection Limit. Before an IDL can be run, a Time Profile must be defined. σ = 5-44 ∑ n i=1 (X i − X )2 n − 1 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software σ = ∑ n i=1 (X i − X ) 2 Standard n − 1 3σ Χ or Avg(µA of 5-11 Blanks) IDL 0 ppt Concentration Figure 5-17. Method Detection Limit - EPA IDL. The Method Detection Limit of the M-6000A is calculated as the concentration projected to yield a signal increase equivalent to 3σ of the blank. This 3σ in micro absorbance units is mapped using a preexisting calibration curve into the Method Detection Limit of concentration. The following is an excerpt from USEPA Document Number ILM04.0 describing how to determine the MDL: Before any field samples are analyzed under this contract, the instrument detection limits (µg/L) shall be determined for each instrument used, within 30 days of the start of contract analyses and at least quarterly (i.e., January, April, July, October), and shall meet the levels specified in Exhibit C. The Instrument Detection Limits (in µg/L) shall be determined by multiplying by 3, the average of the standard deviations obtained on three nonconsecutive days (e.g. Monday, Wednesday, and Friday) from the analysis of a standard solution (each analyte in reagent water) at a concentration 3x-5x the instrument manufacturer’s suggested IDL, with seven consecutive measurements per day. Each measurement shall be performed as though it were a separate analytical sample (i.e. each measurement shall be determined and reported for each wavelength used in the analysis of the samples. In addition, IDLs shall be reported on For X-IN for each 5-45 M-6000A Mercury Analyzer Software Manual Using the M-6000A Software instrument used in reporting results for an SDG and shall be submitted with each data package. The analysis of samples too near the Detection Limit, of the current configuration of the M-6000A, will provide questionable data. As with any analytical instrument, accurate quantitative analysis begins at ≥ 5 times the MDL. The Method Detection Limit can be used to determine how well the system is set up, based on the samples being analyzed. This value will ensure enough instrument sensitivity, while minimizing the time it takes to analyze samples. In summary, IDL and MDL are two different methods of determining the limits of accurate analysis for the current configuration of the M-6000A system. IDL MDL Needs Time Profile..............................Yes Yes Needs Existing Calibration................. No Yes Uses Blank .................................... 5-11 times No Uses Low Standard ...................... 1 @ 20+ ppt 7 @ 3 - 5 ppt Based on EPA Spec ............................. No Yes Number of days to determine ...............1 ≥ 5 (Avg. of 3 runs) The DL (IDL/MDL) is related specifically to the method it was determined from. This is because the DL depends on the operating parameters used to create it. Currently the M-6000A software does not require the analyst to rerun the DL after they change the method operating parameters. However, the DL stored with the method may differ from the actual DL if the operating parameters (gas flow, etc.) change, but the analyst does not rerun the DL in the software. 5.7.2.4 M-6000A Controls Using this form, the analyst may manually control the M-6000A and the Auto Sampler without having to employ a Worksheet. Use of 5-46 6 Maintaining the M-6000A Software 6. Maintaining the M-6000A Software 6.1 Overview This chapter covers the features that are available from the Administration Options on the CETAC M-6000A Toolbar of the program (Fig. 6-1). These features include removing old Templates and Worksheets and administering Security Options. Figure 6-1. Administration Options. M-6000A Mercury Analyzer Software Manual Maintaining the M-6000A Software 6.2 Deleting Old Templates and Worksheets To delete a Template or Worksheet, select the respective button from the delete section. The user will be asked for a confirmation and then the data will be deleted permanently. 6.3 Security There are several levels of security available from the software to suit many needs. 6.3.1 Password Protection The simplest security setup is to turn the security features off altogether. This is controlled by the Password Protection checkbox. When this box is off, there is no security enforced by the software. To activate security, check this box. The first user to open the password setting dialog has the opportunity to set him/herself up as a Supervisor/Administrator who can distribute security options to all the other users. Once the Supervisor/Administrator has logged in, these duties and available software features may be shared or transferred to another user. Only someone with Supervisor/Administrator security level can enable/disable system-wide password protection. 6.3.1.1 Password Settings Password settings and access privileges may be modified through the Administration Options by clicking Password Settings. The user will be asked for an ID and password if they have not been asked already and be placed in the User List dialog box (Fig. 6-2). From here, the user may modify the passwords and privileges using the Edit button. Users may be added and deleted using the Add and Delete buttons respectively. 6-3 M-6000A Mercury Analyzer Software Manual Maintaining the M-6000A Software Figure 6-2. User List Dialog Box. 6.3.2 Access Levels Supervisor/Administrator: The first user to activate the security features is given this access level. This user can do anything listed in this software manual. Senior Scientist/Researcher: This user can use any of the features of the instrument and software, except the security features. Experienced Operator: This user can do most, but not all, method configuration. They can not calibrate the gas flow, change the COM port configuration, etc. Beginner: This user can only run samples and batches and can add labels to existing methods. 6-4 7 Troubleshooting the M-6000A Software 7. Troubleshooting the M-6000A Software This chapter covers problems with the software and communication configuration of the instruments. For a complete list of hardware and performance issues, see the M-6000A Mercury Analyzer Operator’s Manual. 7.1 Hardware Problems 7.1.1 Verify All Connections The following connections should be checked if a software problem occurs: The power to the M-6000A The power to the Auto Sampler The COM connection from the computer to the M-6000A The COM connection from the computer to the Auto Sampler The Auxiliary Cable plug on the M-6000A should be connected to the Auxiliary port on Auto Sampler and the 9-pin d-socket on the pump. 7.1.2 Verify The COM Port Configuration See Chapter 4 for a detailed description of how to check the configuration of the COM ports. M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software 7.2 Software Problems Below is a chart of standard Startup software errors that an analyst may encounter, as well as a more general meaning and course of action. Error Message: Probable Cause: Action: Startup 160: Attempt to create COM port control No resources Available was unsuccessful 161: Serial Port is unavailable Not enough RAM. Close other applications. Check system requirements. Serial mouse on one port. Check computer’s hardware and software Only one physical port. configuration. Fax software locking port. 162: The CETAC Instrument controller is No multiple instances of Close all instances of the software and restart already running software are allowed computer. 163: Attempt to create HG_Comm object No resources available was unsuccessful 164: Attempt to create ASX-500 object No resources available was unsuccessful 165: An error occurred while attempting Not enough RAM. Close other applications. Check system requirements. Not enough RAM. Close other applications. Check system requirements. Borland Database Engine Restart Windows. to allocate the WSL database 166: The password table is damaged! Call Tech Support. 192: This operation requires a pre- Create a Worksheet. existing worksheet. No worksheets have been defined yet. 384: An unrecognized unit conversion Call Tech Support. has been attempted Table 7-1. Software errors Startup. 7-3 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software Below is a chart of standard Auto Sampler (ASX-500 or ASX-500 Model 510 ) software errors that an analyst may encounter, as well as a more general meaning and course of action. Error Message: Probable Cause: Action: 944: Unable to correctly set the At startup, ASX-500 is not Check serial connection and restart. ASX500''s tray type on-line 945: Error setting ASX-500 pump state Physical ASX-500 Auto Sampler Check serial connection and restart. communication failure 946: Error querying ASX-500 state Physical ASX-500 Check serial connection and restart. communication failure 947: Communication with the ASX-500 Physical ASX-500 pump has failed. Reconfigure your communication failure Check serial connection and restart. system and restart this program. 948: An Error occurred at the ASX-500 Physical ASX-500 Auxiliary I/O communication failure 949: An Error occurred while attempting Physical ASX-500 to park the sipper communication failure 950: An Error occurred while attempting Physical ASX-500 to move the sipper communication failure 951: An Error occurred while attempting Physical ASX-500 to raise the sipper communication failure 952: An Error occurred while attempting Physical ASX-500 to lower the sipper communication failure Check serial connection and restart. Check serial connection and restart. Check serial connection and restart. Check serial connection and restart. Check serial connection and restart. Table 7-2. Software errors for Auto Sampler (ASX-500 or ASX-500 Model 510). 7-4 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software Below is a chart of standard Auto Dilutor (ADX-500) software errors that an analyst may encounter, as well as a more general meaning and course of action. Error Message: Probable Cause: Action: At startup, ADX-500 is not on-line Check power, serial connections and cables and then or connected properly or defective restart. Auto Dilutor 955: Error detecting the ADX-500 cable(s) 956: Error in priming ADX-500 pump 957: Error setting the dilution tube range Physical ADX-500 hardware or Check serial connections and cables and pump and serial communications failure then restart. Serial communications failure or Check serial connections and cables and pump and pump failure (either hardware or then restart. Set dilution tube range again. communications) 958: Error setting the ADX-500's program Serial communications failure rack type 959: Error setting the ADX-500 sipper Check serial connections and cables and then restart. Set rack type again. Serial communications failure speed Check serial connections and cables and then restart. Set sipper speed again. Table 7-3. Software errors for Auto Dilutor (ADX-500). 7-5 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software Below is a chart of standard M-6000A software errors that an analyst may encounter, as well as a more general meaning and course of action. Error Message: Probable Cause: Action: Bad serial connection Check serial connection and restart. 961: A data acquisition failure has Faulty connection ASX- Check connection and restart. occurred. Procedure halted 500 to M-6000A 962: A failure has occurred while setting Bad serial connection Check serial connection and restart. Bad serial connection Check serial connection and restart. Bad serial connection Check serial connection and restart. Bad serial connection Check serial connection and restart. Sample cell dirty Clean Sample cell. Reference cell dirty Clean Reference cell. M-6000A 960: An error occurred initiating data acquisition. Procedure halted the data acquisition parameters 963: The M6000 peristaltic pump has failed to respond correctly 964: A failure has occurred while setting the carrier gas 965: A failure has occurred while attempting to zero the instrument 966: Hardware Zero Upper Limit Reached: Clean the Sample cell 967: Hardware Zero Lower Limit Reached: The reference cell may be dirty 968: The A/D Calibration failed Bad serial connection Check serial connection and restart. 969: The A/D registers -5 Volts. The Hg The Hg lamp is not Turn Lamp On/Replace Lamp. lamp may be switched off working 970: A single point data acquisition failed Bad serial connection Check serial connection and restart. 971: A failure occurred while retrieving At startup, the M-6000 is Check power and communication cables and restart. version information from the M6000 not on-line 972: A failure occurred while attempting Check serial connection and restart. to Calibrate the M6000 A/D 973: A failure occurred while turning on Check serial connection and restart. the Mercury Lamp 974: A failure occurred while attempting to query the Lamp current Table 7-4. Software errors for M-6000A. 7-6 Restart the software and instrument. M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software 7.3 Printing and Windows Windows offers many advanced printing features, not the least of which is the ability to print documents on many different types of printers and have these documents appear very nearly the same. However, the price of these features is a complex system which sometimes needs a little user intervention. From start to finish, here is a brief outline of the steps a document must go through to be printed, as well as some reasons that the document may not print as expected: 1 The user clicks print in the current application. Some of the more subtle “problems” in printing can occur at this point. When you click Print from the file menu, you will print to the default printer specified by the Print Manager. If this is not the intended printer, this can cause a significant problem. Be sure to check which printer you are sending the document to before continuing. 2 The application sends information to Windows, “drawing” the printout. If the document does not make it through this step, it is possibly a problem with the application that printed it. A good way to tell if the application completed this step is to attempt to print to a local printer using the application in question. If you receive a printout (however garbled), or the print manager is running, then you know that the application sent information to the Print Manager and the problem is not in the software trying to print but with Windows’ configuration. 7-7 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software 3 This information is given to the Print Manager in the form of a temporary file. Even if the application printing the document provides the right information to Windows, Windows may not be able to provide this information to the print manager. This may be due to inadequate disk space for temporary files. Check your AUTOEXEC.BAT file for a line like SET TEMP=C:\TEMP. If there is no line like SET TEMP=<directory>, now is a good time to add one. Be sure that the directory specified exists, and has plenty of free space (6-7 Meg is not uncommon for large word processor documents). 4 The Print Manager checks to see if the selected printer is online and ready to go. The Print Manager has a limited ability to check to see if the print will succeed, and can abort if necessary. However, if you are printing to a network printer, the Print Manager may not have this ability. 5 If the printer appears to be on-line, it begins spooling (sending chunks of data at a time as fast as the printer can accept them) through the communications link between the printer and the computer. For the printer to receive and print the document, it must be on, connected to the computer or the network properly, and have paper/ribbon/toner. If you receive a good printout from Microsoft Write, but a garbled printout from the M-6000A software, this may be due to a problem with the printer driver you are using. Windows uses a device independent interface to allow the same document to be printed on many different printers without differences in how an application prints to Windows. If the printer driver you are using is not providing the proper functionality, contact the manufacturer for a printer driver update. This will improve the printing of all your applications. 7-8 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software 6 When the printer has been sent all the document information, the Print Manager then deletes the temporary files and closes itself. At this point, the Print Manager closes, and hopefully the document has printed. However, this is only the end of Window’s part of the printing process. If you are using a network, there may be many more places where a print can be lost even after the Print Manager has sent it properly. If you are in doubt as to whether your computer is printing correctly, connect a printer to the local port. If you receive a printout from this local printer, and not from network printers, then the problem is probably a network/PC configuration. Hopefully, this information can will help fix and avoid problems that occur while printing. 7.4 When All Else Fails If you are having problems with the M-6000A software, when all else fails, close the software, exit windows, turn off both the ASX-500 and the M-6000. Wait a few seconds, turn both back on, and restart the software. If this does not work, call CETAC Technical Support at the number listed in the Preface of this manual. 7-9 M-6000A Mercury Analyzer Software Manual Troubleshooting the M-6000A Software 7-10 Glossary M-6000A Mercury Analyzer Software Manual Glossary Glossary This book frequently uses the following terms: AAS Atomic Absorption Spectrometry Abs Absorbance (-log10 T or 2-LOG10 %T) ADC or A/D Analog-to-digital converter. ASX-500 The ASX-500 or ASX-500 Model 510Auto Sampler. Bar Unit of pressure. 1 bar = 100 kPa ≈ 14.5 psi. Ar Argon carrier gas, chemical formula. CH3HgCl Methyl mercuric chloride (or “methyl mercury”), chemical formula. CLP Contract Laboratory Protocol (analysis protocol of U.S. EPA). Cold Vapor Direct AAS or CVAAS Direct Atomic Absorption Spectrometric analysis (at 245 nm) of “head-space” gas from a stannous chloride or stannous sulfate reactor using neither flame, nor plasma, nor furnace nor any other electro-thermal atomizer. CVAAS works only for the element mercury (Hg). Dia. Diameter. DL Detection limit. Smallest statistically detectable concentration, where the absorbance, Abs (produced by that concentration), equals 3 times the standard deviation σ of the blank. ea. Each. EOFM Electro-Optic Feedback Module; used to stabilize the Hg lamp. EPA U.S. Environmental Protection Agency. EPA-245.1 The standard EPA method of water quality analysis for measuring mercury (Hg). G-2 M-6000A Mercury Analyzer Software Manual Glossary ETFE Ethylenetetrafluoroethylene (Tefzel), a polymeric tubing material. g Gram, unit of mass or “weight”. GCU Gas Control Unit, sets and regulates carrier gas flow rate. GLS Gas-Liquid Separator. HCl Hydrochloric Acid, chemical formula. Hg Mercury, chemical symbol. Hg0 Mercury, elemental (reduced) state. Hg2+ Mercuric ion, mercury in +2 (oxidized) state, typically HgCl2. HgCl2 Mercuric chloride, chemical formula. HNO3 Nitric acid, chemical formula. i.d. Inside diameter. IDL Instrument Detection Limit. DL in ultra-clean, high purity acid media (e.g. 7% HCl, “Ultrex II” grade). IDL is generally measured under “favorable” operating conditions and does not involve sample digestion or preparation steps. IDL indicates what the instrument is capable of doing, if not subjected to contamination, digestion loss, storage loss, or other sample collection/preparation errors or limitations. KMnO4 Potassium permanganate, chemical formula of oxidizing reagent, and Mercury Exhaust Trap agent. L Liter, unit of volume. LED Light-Emitting Diode. M-6000 Specifically the CETAC Mercury Analyzer instrument that sits below the ASX-500 Autosampler. G-3 M-6000A Mercury Analyzer Software Manual Glossary M-6000A Specifically the entire Mercury Analyzer system including the M-6000, ASX-500, Peristaltic Pump, etc. mA Milliamperes (10-3 amperes), electrical current. MDL Method Detection Limit; DL measured under actual reagent purity, sample preparation, and storage conditions for samples, reagents, and containers in question. Calibration standards are generally prepared in the sample media (standard addition) and are carried through all sample digestion/ preparation, storage, transfer, etc. steps, as are blanks. In the presence of significant contamination, small concentration delectability gets worse and the actual MDL should be redefined as 1/3 the contamination, but not less than the statistical MDL! Mg(ClO4)2 Magnesium perchlorate, chemical formula of desiccant (drying agent) “flakes”. mL Milliliter (cubic centimeter, cc, 10-3 L), unit of volume. mm Millimeter (10-3 meter), unit of length. N2 Nitrogen carrier gas, chemical formula. nm Nanometer (10-9 meter), wavelength unit. ng Nanogram (10-9 gram), mass or weight unit. o.d. Outside diameter. P Transmitted radiant power, photon flux at sample detector (after passing through sample). P0 Incident radiant power, photon flux at reference detector (before passing through sample). PC Personal Computer. PEEK Polyetheretherketone; a machined polymeric construction material. G-4 M-6000A Mercury Analyzer Software Manual Glossary pg Picograms (10-12 g), mass or weight unit. PID Proportional Integral Differential. Description of a type of precision heater control device. ppb Parts per billion (ng/mL, 10-9 g/mL, µg/L, 10-6 g/L), concentration unit. ppm Parts per million (µg/mL, 10-6 g/mL, mg/L, 10-3 g/L), concentration unit. ppt Parts per trillion (pg/mL, 10-12 g/mL, ng/L, 10-9 g/L), concentration unit. psi Pounds per square inch. Pressure. 1 psi ≈ 0.068 bar. 1 bar = 100 kPa. psig Pounds per square inch gauge. Gauge reading (above atmosphere reading). PTU Precision-Timed Uptake. Pump or PP Peristaltic Pump. P-P Peak to Peak. A description of how signal noise is measured (One method). RMS Root Mean Square. A description of how signal noise is measured. RMS = 0.707 P-P (Another method). RSD Relative Standard Deviation. A measure of data precision or reproducibility. SCR Stannous Chloride Reactor. Sn Tin, chemical symbol. Typically as SnCl2 reagent. SnCl2 Stannous chloride, chemical formula of reducing agent. T Transmittance (P/P0), often %T or percent transmittance (P/P0 x 100%). TC “To Contain” Designation of a type of volumetric flask calibrated to accurately contain a specified volume of liquid. G-5 M-6000A Mercury Analyzer Software Manual Glossary TD “To Deliver” Designation of a type of volumetric flask or pipet calibrated to accurately deliver a specified volume of liquid. UHP Ultra High Purity. UV Ultraviolet; short wavelength region of spectrum below 370 nm (e.g. 254 nm). VAC Volts Alternating Current. VDC Volts Direct Current. XS A substantial concentration “excess” of one chemical reactant (over another). µg Micro-gram (10-6 g), unit of mass or weight. µL Micro-liter (10-6 L), unit of volume. µAbs Micro-absorbance units. (10-6 Abs). G-6 Index M-6000A Mercury Analyzer Software Manual Index Index A Absorbance Curve Defined 1-3 ADX-500 Auto Dilutor Introduction 1-3 Controls 5-48 Setup 5-27, 5-48 Analysis of Samples Summary and Step by Step 1-8 Analysis Tab 5-31 ASX-500 Hardware 1-2 Racks 5-27 Auto Adjust Integration 5-14 Auto Dilutor Accessory Intro 1-3 Auto Dilutor Accessory 5-49 Auto Dilutor Accessory Setup 5-27,5-49 B Baseline Correction Point 1st 5-8 1st, Changing 5-36 1st, setting 5-15 2nd 5-9 2nd, Changing 5-36 2nd, Setting 5-16 Baseline Correction Point, 1st In Time Profile 1-6 Baseline Correction Point, 2nd In Time Profile 1-7 Baseline Drift Correction 5-15 Baseline Sample Times 5-14 Borland Database Engine 3-2 C Calibrate Gas Flow 5-41 I-2 Calibration 5-44 Algorithm 5-21 Data Chart 5-37 Defined 1-8 Graph 5-53 Linear 5-21 Quadratic 5-21 Changing Worksheet Parameters 5-36 Clear Drain Button 5-57 Common Sample Parameters Default Weight and Default Volume 5-29 Sample Prep Date 5-29 Common Software Operations 5-59 Complete Sample information 5-55 Concentration 5-33 Configuration, system 5-40 Correlation 5-37 Creating Worksheet 5-52 Curve 5-37 D Data tab for reports 5-53 DDE Server 5-58 Default Weight and Default Volume 5-29 Deleting Old Templates and Worksheets 6-3 Detection Limit 5-43 Develop Tab 5-7 F Filing Tab 5-6 Final Volume 5-31 Flow Parameter Guidlines 5-11 Functons Common Software 5-57 M-6000A Mercury Analyzer Software Manual Index G Gas Flow 5-16 H Hardware ADX-500 Auto Dilutor 1-3 ASX-500 Auto Sampler 1-2 I In-line qc tube numbers 5-20 Insert qc standards 5-29 Installing 3-2 Hardware 3-2 Software 3-2 Instrument Control 5-16 Instrument Calibration 5-64 Instrument Detection Limit (IDL) 5-43 Integration 5-13 Intercept 5-37 L Labels Add Row at Current Posn 5-30 Auto Renumber Tubes 5-29 Auto Sampler Labels 5-55 Autofill 5-28 Clear 5-28 Clear Grid 5-30 Delete Current Row 5-30 Sort by Tube No 5-30 Tab 5-24 Linear calibration 5-37 Linear, forced zero intercept 5-21 Liquid flow 5-12 M M-6000A as a DDE Server 5-58 M-6000A Manually Controlling 5-46 M-6000A Mercury Analyzer Hardware 1-2 M-6000A Software Tutorial 5-59 M-6000A Toolbar 5-2 Maintaining the M-6000A Software 6-2 Mean ABS 5-33 Measurement Sub-Tab 5-8 Method Detection Limit 5-44 N Notes Sub-Tab 5-24 P PC requirements 2-2 Printing and Windows 7-5 Printing Reports 5-57 Q QC Activation 5-22 QC Standards 5-23 QC Sub-Tab 5-21 Quality control 5-21 Quadratic calibration 5-37 R Rack Id 5-31 Read Button 5-32 Read Delay 5-13 Real-Time Absorbance Chart 5-8 described 5-34 Recalibration frequencies 5-8 Repeats 5-18 Replicates 5-14 µg/L 5-33 I-3 M-6000A Mercury Analyzer Software Manual Index Report Data 5-53 Options 5-3 Settings 5-50 Tab 5-56 Report Options 5-45 Reslope frequencies 5-8 Rinse Time 5-17 RSD 5-13, 5-33 S Sample Id 5-31 Sample Label 5-33 Sample Matrix 5-18 Sample Time 5-13, 5-36 Sample Time Profile Lockdown 5-14 Sample Trays 1-6 Sample Type 5-31 Sample Weight 5-31 Sampling Times 5-13 Security Password Protection 6-3 Settings Tab 5-50 Setup dilutor & define racks 5-20 Signal profile chart 5-35 Signicant Figures & Rounding 5-57 Sip Duration 5-17 Sipper Depth 5-41 Slope 5-37 Smart Rinse 5-41 Software configuration 5-35 Software Operations 5-51 Software Selftests 4-2 Software Tutorial 5-59 Standards 5-20 Standards Defined 1-6 Standards Sub-Tab 5-19 Standards, concentration and stds tube number 5-20 Start Button 5-31 I-4 Stop Button 5-32 Store raw scan data 5-18 Srip chart recorder 5-49 System configuration menu 5-40 System requirements for PC 2-2 T Template Defined 1-3 Time Profile 1-6, 5-8 Reading a sample to define 5-32 Timing parameters 5-13 Troubleshooting 7-2 Hardware Problems 7-2 Software Problems 7-3 Tube # 5-31, 5-33 Tutorial on Software Operations 5-57 Two-Point Baseline Correct 5-15 U Units 5-21 W Worksheet Close 5-6 Create Template 5-7 Creating 5-52 New 5-4 Options 5-3 Parameters 5-52 Rename 5-7 Save 5-6 Z Zeroing defined 1-7 how to 5-42, 5-64