Operation and Service Manual MPA120 EZ-Melt Automated Melting Point Apparatus Stanford Research Systems Revision 1.4 (11/05) Certification Stanford Research Systems certifies that this product met its published specifications at the time of shipment. Warranty This Stanford Research Systems product is warranted against defects in materials and workmanship for a period of one (1) year from the date of shipment. Service For warranty service or repair, this product must be returned to a Stanford Research Systems authorized service facility. Contact Stanford Research Systems or an authorized representative before returning this product for repair. Information in this document is subject to change without notice. Copyright © Stanford Research Systems, Inc., 2005. All rights reserved. Stanford Research Systems, Inc. 1290-C Reamwood Avenue Sunnyvale, California 94089 www.thinksrs.com Printed in U.S.A. EZ-Melt Automated Melting Point Apparatus Safety and Preparation For Use i Safety and Preparation for Use CAREFULLY READ THE IMPORTANT SAFETY INSTRUCTIONS AND NOTES INCLUDED IN THIS SECTION BEFORE USING THE EZ-MELT AUTOMATED MELTING POINT APPARATUS AND ANY OF ITS ACCESSORIES. Within this section, the word 'product' specifically refers to the EZ-Melt Automated Melting Point Apparatus and any of its accessories. This product is designed and built for use in synthetic and analytical chemistry laboratories. It is intended to be used to determine melting temperatures and melting ranges between ambient and 400°C temperatures. Safety risks are associated with all research and production activities. Though long experience has proven melting point instrumentation to be remarkably safe, hazards are always associated with analytical equipment. The most effective way to minimize risk to yourself and others is to read, and strictly follow, all safety instructions and warnings during the installation, operation and maintenance of all equipment used in your laboratory. The intent of this section is to collect, in a single place, the most common risks associated to the installation, operation and maintenance of this product. The instructions are also repeated, with additional information, at the appropriate points throughout this manual. This product has been designed with user safety as a priority and has been proven to show reasonably safe operation provided it is installed, operated and serviced in strict accordance with all the safety instructions included in its manual Safety Instructions and Warnings • SAFETY PAYS! Safety instructions must be strictly followed during all stages of installation, operation and service of this product. Failure to comply with these precautions and warnings violates the safety standards expected of users of this product. • This Operations Manual is a component of the product and must remain readily available to all laboratory personnel with access to the EZ-Melt Melting Point Apparatus. • If you have any doubts about how to use this product safely, contact Stanford Research Systems using the contact information provided in this manual. • Do not use this product for any purpose other than its intended usage. • Retain these safety and operating instructions for future reference. • Identify and adhere to all warnings posted on the product and throughout this manual. • Failure to comply with these instructions may result in serious personal injury, including death, as well as significant property damage. EZ-Melt Automated Melting Point Apparatus ii Safety and Preparation For Use • This instruction manual should form the basis of any training requiring the use of this product. • Wear protective garments such as lab coat and goggles at all times. • Refer servicing to qualified personnel only. Product Placement Requirements • Place this product on a stable, clean, level and even surface. • Place the product away from water sources - faucets, safety showers, eyewashes, rain, etc. Do not allow the product to become wet. • No containers, chemicals or other appliances should be placed behind the product. • Always operate the unit in its proper upright orientation. Do not operate the unit on its side. • To prevent damage to the product and ensure sufficient cooling in the electronic compartment, place the sidewalls of the unit at least 10 cm away from walls or other objects. • Your EZ-Melt may produce some smoke the first time it is heated. The smoke is caused by residual oils coating the metal surfaces of the heater and surrounding areas. Once the oils burn away, the smoke will permanently cease. Electrical Shock Risks The most common risk associated with the operation of chemical instrumentation equipment is electrical shock. • It is your responsibility to install and operate this product in full conformance with local electrical codes. Consult an experienced electrician if necessary. • If the power cord becomes damaged, replace it immediately. • Dangerous voltages capable of causing injury are present during the operation of this product. Do not remove the covers while the unit is plugged into a live outlet. • Do not use this product if it has unauthorized modifications. Unauthorized modifications may result in fire, electric shock and other hazards. • Do not install substitute parts or perform any unauthorized modifications to this instrument. • The line fuse is internal to the instrument and may not be serviced by the user. • Always use an outlet which has a properly connected protective ground. Consult with an experienced electrician if necessary. • GFCI (Ground Fault Circuit Interrupter) protected outlets are often available in laboratory environments, particularly in proximity to water sources. GFCI's are EZ-Melt Automated Melting Point Apparatus Safety and Preparation For Use iii generally regarded as an important defense against electrocution. However, the use of a GFCI in conjunction with the EZ-Melt must NOT be regarded as a substitute for proper grounding and careful connections. GFCI's must also be tested regularly to verify their functionality. Always consult an electrician when in doubt. • Do not use accessories not recommended in this manual as they may be hazardous. • Keep all electrical wiring on your laboratory benches neatly organized and in good working conditions. Label and color-code all high voltage cables. Inspect all HV wires periodically for problems as part of your safety checkups. • Use tie downs and cable channels to hold all electrical wiring in place - no dangling cables. • Keep all electronic instrumentation neatly organized, and remove unconnected cables, power supplies and connectors from your laboratory benches and shelves. • Do not push objects of any kind into this product through openings as they may come in contact with dangerous voltage points or short out parts that could result in a fire or electric shock. • Operation of this product with line voltages other than those accepted by the power supply can cause damage to the instrument and injury to personnel. Burn Risks A common risk associated specifically with the operation of thermal analysis instrumentation equipment is burns. • Observe, and respect, the “HOT LID” warning on the top surface of the product. • Do not touch the heater block while hot. • Check the temperature of the block before opening its compartment. The block may still be hot from previous use even when the unit is off. Turn the unit on to check the block temperature. Explosion Risks Injury due to explosion is another important safety concern during the operation of thermal analysis instrumentation. • This product is not compatible with application environments requiring explosion- proof equipment nor with samples which may explode or ignite by heat, friction or spark. • Do not use this product to analyze samples of unknown composition or contamination. EZ-Melt Automated Melting Point Apparatus iv Safety and Preparation For Use EZ-Melt Automated Melting Point Apparatus Contents v Contents Safety and Preparation for Use i Contents v Front Panel Overview vii Back Panel Overview viii Specifications ix Chapter 1 Getting Started 1 Unpacking 1 Instrument Placement 2 Removable Parts 2 Quick Start Instructions 4 Chapter 2 Using EZ-Melt 7 Principle of Operation 7 Automated Analysis 8 Setup 8 Oven States 10 Recording Visual Observations 12 Reading the Results 12 Chapter 3 Melting Point Determination 15 Introduction 15 Capillary Method 16 Instrument Setup 19 Visual Observations 21 Melting Point Range 25 Melting Point Report 26 Melting Point Depression 27 Chapter 4 Maintenance and Calibration 29 Temperature Offset Calibration 29 Camera Alignment 35 Replacement of Faulty LEDs 36 Broken Capillaries 36 Dirty Window 37 Exterior Cleaning 37 Error Codes 37 EZ-Melt Automated Melting Point Apparatus vi Contents Appendix A Pharmacopeia vs. Thermodynamic Melting Point Determinations 39 Pharmacopeia Melting Point 39 Thermodynamic Melting Point 41 Thermodynamic Correction 42 Thermodynamic Correction with EZ-Melt 43 Appendix B Melting Point Certified Reference Standards 47 What is a Certified Reference Standard? 47 O100MPS CRS Kit 51 EZ-Melt Automated Melting Point Apparatus Front Panel Overview vii Front Panel Overview Figure 1. Front Panel of EZ-Melt. LED Display and Keypad A simple front panel, including a 4 digit LED display with 6 button interface, displays the oven temperature, setup parameters and melting point results, as well as step-by-step status indications throughout the determination process. Observation Window A wide observation window, with a large magnification lens and internal illumination, allows users to observe the samples and determine their melting points visually. Power Indicator The 4 digit LED display and oven illumination is on whenever the unit is turned on. EZ-Melt Automated Melting Point Apparatus viii Back Panel Overview Back Panel Overview Figure 2. Back Panel of EZ-Melt. Ceramic Sample Holder Three sample capillaries may be inserted into the oven via the ceramic insulator visible at the top of the unit. The small metal oven is heated under tight microprocessor temperature control and in strict compliance with modern pharmacopeia methodologies. A precision platinum resistance thermometer provides accurate and reproducible temperature readings with 0.1°C resolution. Glass Capillary Receptacles Two separate glass capillary holders, located on top of the instrument, are available to store empty and discarded capillary tubes. Power Entry Module Connect the EZ-Melt to a properly grounded outlet using the power cord provided with the instrument. Consult an electrician if necessary. EZ-Melt is turned on by flipping the power switch on the Power Entry Module. EZ-Melt Automated Melting Point Apparatus