aboni FMX HydroTracer Operation Manual aboni GmbH für Mess- und Automatsierungstechnik Zeche Ernestine 10 D-45145 Essen Germany Tel. +49 700 abonifon; +49 700 22664 366; +49 201 74 70 631 Fax +49 700 abonifax +49.700 22664 329 +49 201 74 70 633 email [email protected] Table of Contents Page Measuring principle 2 Reagent 3 Setting into operation 3 Installation of the software 3 Connecting the HydroTracer 3 Operation 4 The operation step by step 4 Selection of temperature 6 Determination of the sample size 6 Loading of the HydroTracer 7 Measuring period 12 End of measurement 12 Saving the results 12 Dry run 13 LEDs 13 Errors 13 Communication problems 13 Using the USB-port 13 Appendix: Installation manual of the program Declaration of Conformity Material safety data sheet calcium hydride Operation Manual FMX HydroTracer E2-1 1 Measuring Principle The patented method of the HydroTracer determines the absolute water content. The mass of the water is measured within the reactor. The percentage of moisture of the sample is calculated by division with the sample weight. Cutaway view of the reaktor Evaporated water reacts to Hydrogen. The concentration of hydrogen is a measure of the sample humidity. reactor lid sensor reagent bed with reagent pipes cooled area heated area sample tray The sample is weighed and filled into the sample tray. The sample tray is shifted into the HydroTracer, being a part of the reactor. A heater warms the sample to a temperature chosen by the operator. The water within the sample material evaporates. The volatile water rises to the upper part of the reactor. Two pipes connect the heated sample tray with the cooled upper part where the reagent is placed. The reagent bed is a small flat tray, filled with approximately 0.1 g calcium hydride. When the humid air flows over the reagent, gaseous water reacts with calcium hydride according the following equation: CaH2 + 2 H2O → Ca(OH)2 + 2 H2 The cooled, dried gas enters again the lower part of the reactor. The gas circulation is supported by natural convection, created by a special configuration of the vertical pipes. By this method even hygroscopic materials are completely dried. The final concentration of hydrogen in the reactor is proportional to the water content of the sample before the measurement. The ambient air also contributes water to the reactor atmosphere. To achieve accurate results it is necessary to determine the air humidity and the air density. Integrated sensors measure the humidity of the ambient air, the temperature and the air pressure. With this data the software determines the water of the air humidity which is deduced off the final result. The concentration of hydrogen is measured by a sensor detecting the thermal conductivity of the gas. The air-hydrogen atmosphere does not react chemically, because the temperature is much lower than needed to supply the activation energy of the oxyhydrogen gas reaction. Even if it would react, the theoretic maximum of the reaction enthalpy (the amount of energy which would be set free by the reaction of hydrogen with the oxygen of the air) is about 0.1 kJ and therefore harmless. Operation Manual FMX HydroTracer E2-1 2 The reagent Calcium hydride reacts with water to calcium hydroxide (hydrated lime, agricultural hydrate), which is a weak base and quite harmless. Nonetheless, take care calcium hydride does not get into contact directly with (liquid) water. The reaction heat together with the oxygen of the air could ignite the developing gas. The small amount of reagent which is needed per measurement averts this danger. Always close the reagent bottle directly after use. Because the reagent is always added in surplus, it will be still reactive after the measurement. Avoid the contact with inflammeable, especially wet materials and leave the used reagent exposed to the air, where it can react slowly with the air humidity. An ideal container is an open tin can. After a few hours calcium hydride is completely transformed to calcium hydroxide. If left even longer exposed to the air, calcium hydroxide reacts to calcium carbonate ( CaCO3, chalk) with the carbon dioxide of the air and can be disposed without any problems. Setting into operation The HydroTracer is controlled by a PC and the data from the intrument is analysed by the PC software. The data is transferred by a serial interface RS 232 (COM port). Before the HydroTracer can be run the first time, the program and the necessary driver have to be installed on the PC. Installation of the software 1. Place the CD into the CD-drive of your computer. 2. Follow the instructions of the installation manual (see appendix). Note: The program FMXE2-1.exe will create a subdirectory C:\FMX on the harddrive C. If necessary, take care this harddrive is accessible, otherwise the software will not run. Connecting the HydroTracer Connect the power supply cable on the rear side of the HydroTracer. Connect the HydroTracer with the data cable to the serial port of your PC. Switch on the power. If the HydroTracer is properly connected to the power supply, the system fan runs and the green LED glows. Switch on your PC (if not done already). The HydroTracer is now ready for the measurement. Note: The gas sensor of the Hydrotracer needs approximately 90 sec. after power supply to reach its operation temperature. Operation Manual FMX HydroTracer E2-1 3 Operation Take care the accessories are within reach. Do not leave your sample material exposed to the ambient air over a longer period, especially if it is hydroscopic. Note: It is recommended to acquaint oneself with the operation before doing a „serious“ measurement. Therefore run the program and follow the menu until you have reached the step START / F10. Do not start but cancel the program by clicking on the CANCEL–button or pressing the key F5. Repeat these steps until you are aware of the procedure. The operation step by step Open the program FMXE02.exe. The following screen is displayed: Run the program by clicking the arrow key on the screen (menu bar up left) or by using the keys Ctrl + R simultanously. Now some calibration data is transferred from the Hydrotracer. This may last some seconds while a message „initalizing, wait“ is blinking. Operation Manual FMX HydroTracer E2-1 4 Input mask 1 appears: Input mask 1 with integrated name list and material list Fill in a name for the operator and the material data or select it out of the tables on the left. The new data will occur in the tables the next time the program is called. You can jump from one input to another with the tabulator keys. Click on CONTINUE on the screen or type ENTER on the keyboard to finish. Note Integrate the table of materials into the input mask 1 A selection of plastics with proposed data concerning materials, heating temperature and density is included within the file „Materialliste“. To integrate this data into the input mask 1 (see picture above), copy the file <CD>\:data\Materialliste from the CD into the directory C:\FMX. The next time the program FMXE02 is called it will automatically integrate this list in the mask. New entries will be added by the new input arrays on the right. If you want to delete data out of the materials table (or the name table) call the file with the program WORDPAD and delete the appropriate line. Store the file Materiallist without extension then. If the operation system of the PC uses a comma as decimal point, use the file Materialliste in the directory <CD>\:comma\Materialliste Operation Manual FMX HydroTracer E2-1 5 Input mask 2 appears: Put in the sample weight. The error caused by the weight measurement is linear, therefore in many causes a balance with a resolution of 0.1 g is sufficient. ( Example: Sample weight 20 g, measured moisture content 0.1000 %; resolution of the balance is 0.1 g, error caused by balance resolution: 0.1g / 20 g = 0.005 = 0.5 %. The measured result of 0.1000% has deviates about ±0.0005 % due to the balance accuracy). Selection of temperature The temperatures given in the materials table are proposals, which might not fit always for each member of a group of materials. Generally a temperature is chosen which is as high as possible to accelerate the evaporation of water but low enough to avoid thermal decomposion. Usually the melting of the sample should be avoided to allow easier cleaning of the sample tray. If you are not shure which temperature is appropriate, try lower temperatures first. In some cases the melting of the sample might be necessary (e.g. to investigate the behaviour of compound fillers), then a (dry!) aluminum film can be inserted into the tray before the measurement. If the heating temperature and the density of a single sample deviates from the usual characteristic, it can be added in the input mask 2 without changing the material table. Determination of the sample size The sample filled in the sample tray should not touch the upper part of the reactor. The rim of the tray is also the seal face of the O-ring integrated in the reactor and has to be kept clean. The sample amount depends on the moisture content of the material. Is this not known, start with a small amount. A water content of 5 mg to 10 mg is recommended. The diagrams indicate the optimum input depending on the (supposed) moisture. Recom. sample weight (density 1 g/cm³ ) Recom. sample weight (density 1 g/cm³ ) 10 60 9 8 water content in mg sample weight in g 50 40 30 20 6 5 4 3 2 10 1 0 0,0001 7 0,001 0,01 0,1 1 moisture in % Operation Manual FMX HydroTracer E2-1 1 0,1 10 0 0,0001 0,001 0,01 0,1 1 10 moisture in % 6 Loading the HydroTracer This chapter describes the steps of the manual operation as shown on the screen. The pictures clarify the action momentarily needed. Below the picture this action is shortly described. The panel counting down the red number on the right indicates the remaining time in seconds. The time schedule should be maintained rather accurate. Leaving the reactor open too long as well as too short can reduce the accuracy. On the right panel the steps are listed which have occured before, so the menu can be followed even if a step was missed according the time schedule. Open the reactor by lifting the lateral handles simultaneously. The system fan will stop. Open reactor by lifting the lid forward into the direction of the small semispherical outcut. Operation Manual FMX HydroTracer E2-1 7 Lift the reagent bed with the pincers and remove the used reagent Take out the sample tray by lifting it slightly and pull it out off the front. Remove old sample material. Take a 1/3 of a spoon with the spatula and fill it into the reagent bed. Operation Manual FMX HydroTracer E2-1 8 Spread the reagent on the reagent bed. Close the reagent glass thorougly. Fill in the sample material. Spread the sample material so the bottom of the tray in evenly covered. Clean the rim with the brush. The seal face is indicated in red on the screen. Operation Manual FMX HydroTracer E2-1 9 Insert the sample tray. Take care that the lower rim of the tray is properly placed over the heating plate. Insert the reagent bed with the pincers. Clean O-ring and seal face of with the brush. The sealing surfaces are indicated in red on the screen. Operation Manual FMX HydroTracer E2-1 10 Close reactor lid. Take care the clasp is properly locked. Push down simultaneously the lateral handles. The system fan must run again. After 95 seconds the CONTINUE button appears. Click on or press Key F10 to start the measurement. No further action is required by the operator. Operation Manual FMX HydroTracer E2-1 11 Measuring period The sample is heated up to the selected temperature. The heating temperature is shown in the upper left diagram. The diagram below displays the actual total water content in mg. The measuring time depends on the kind of sample and the water content. Usually a measurement is finished within 15 to 45 minutes. The display of the estimated water content occurs after a while, showing the mass percentage. Until the measurement is finished, this is only a prognosis, which interpolates the mathematic function of the water increase versus time. When the program has finished the measurement the final result is shown. End of measurement A menu occurs after the measurement is finished which enables the choice between saving the result or trash it. If no selection is done within 60 seconds, the results are automatically saved and the program stopps. The heater is switched off and the main fan cools the reactor to athe default temperature of 50 °C. When the main fan has stopped, the Hydrotracer is ready for the next measurement. Note: Never switch off the power supply before the instrument is cooled and the main fan stops. Note: Within the first minutes the lower graph indicates some fluctuations. These fluctuations of the graph do not influence the latter accuracy of the end result. Saving the results The data is saved in 2 ways: As line of a table in the file C:\FMX\Data\Data-table.txt and as a .htmlfile containing the data and the diagrams as shown on the screen. Operation Manual FMX HydroTracer E2-1 12 The measurement data saved in Data-table.txt is appended as new line to the table, containing all the data as indicated in the window ´Final Results` on the screen. The .txt-file can be easily read by tabulation programs as Microsoft Excel. The .html-file is saved as shown in the illustration opposite, if no other selection is done. The name of the file is created as FMXdate-time. Time is the start-up time of the measurement program. Thus the .html- file can be assigned to a measurement saved in Data-table.txt, where the first two columns indicate the date and the time of a measurement. Dry run A dry run has to be done before the first operation, after the reactor has been left open for a longer period or if the water content of a previous measurement exceeded 80 mg. It is also recommended if the instrument was not in use for a few days and very low water contents shall be detected. Always leave the reagent in the reactor if the HydroTracer is not in use! For a dry run, just do a measurement without any sample material (but with reagent) at maxium heating temperature of 210 °C. LEDs There are three light-emitting diodes below the blue plastic sheet on the top of the HydroTracer. Green indicates: Yellow indicates: Red indicates: Power supply on Heater on Error Errors If an error occurs during the communication between Hydrotracer and PC, the HydroTracer sends an error message to the software. In most cases this will interrupt the measurement. Errors of the hardware are indicated by the red LED below the top sheet of the HydroTracer. Shortly break the power supply. In most cases the error is vanished and the red LED does not glow anymore. If the connection between PC and HydroTracer is interrupted for more than 4 minutes, the measurement is automatically cancelled and the HydroTracer cools down. Communication problems In most cases, communication problems are caused by the cabling. Check thoroughly the connections between PC and HydroTracer. If there are more than two serial ports on the PC, it might be possible that the port is not detected automatically by the program (this happens during the initializing at the beginning). You can select the port manually by using the port-control on the front panel. Select a port before starting the program. The nomenclature is ASRL::1 for COM1, ASRL::2 for COM2 etc. Using the USB-port If there is no serial port available at the PC the USB-port can be used with an USB-to-Serial-Adapter. If the driver is properly installed (this has to be done before the program FMX E2-1.exe is called) the port control in the upper left edge of the screen will show a new port in the scroll-down menu. Operation Manual FMX HydroTracer E2-1 13 Installation of the Software of the FMX HydroTracer The software has to be installed in 2 steps: A) Installation of the interface driver B) Installation of the control program The procedure is explained in detail and can be done without special knowledge. A) Installation of the interface driver 1. Choose option Run from start- menu 2. Run visa301runtime.exe, placed in D:\data\visa301runtime.exe (with D as CD- drive) . 3. The marginal menu appears. Press Setup 4. The marginal menu appears. Press Next. Installation Program FMX 2-2 1 5. The marginal menu appears. Click on I accept the License Agreement . Click on Next. 6. The marginal menu appears. Click on Next . 7. The marginal menu appears. Click on Custom. Click on Next. Installation Program FMX 2-2 2 8. The marginal menu appears. Click on PXI. 9. The marginal sub-menu appears. Choose option Do not install this feature Now this part of the program is deactivated. 10. Repeat deactivation with with all submenus but submenu Serial, Remote, Enet-Serial, USB, COM-Support. The menu tree should look like the marginal picture. Then click on Next. 11. The marginal menu appears. Click on Next. The driver configuration is finished. Installation Program FMX 2-2 3 12. The marginal menu appears. Click on Finish. 13. The marginal menu appears. Click on Yes. The computer will reboot now. B) Installation of the control program of the FMX HydroTracer 1. Choose option Run from start- menu 2. Run setup.exe, situated in D:\installer\setup.exe (with D as CD- drive) . Follow the instructions of the menu. (in local language) The program will be installed into the directory Programs\ FMX 2-2. Installation Program FMX 2-2 4 SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Date of print: Page: 16.01.2003 1of 6 1. Identification of the substance/preparation and of the company/undertaking Identification of the substance or preparation Commercial Product name: Calcium hydride Company/undertaking identification Manufacturer / distributor: Street/POB-No.: State/city/postal code: Telephone: Telefax: Chemetall Gesellschaft für chemisch technische Verfahren mbH Trakehner Straße 3 D-60441 Frankfurt a. M. +49 (0) 69 7165-0 + 49 (0) 69 7165-2523 Dept. responsible for information: Additional information: Special Metals Division This MSDS pertains to the following products: 455110 Calcium hydride type K 455120 Calcium hydride type B 455130 Calcium hydride type O 455140 Calcium hydride type M Telephone: +49 (0) 69 7165-0 Telephone: +49 (0) 5326 51-0 Emergency information: Chemetall GmbH, Langelsheim 2. Composition/information on ingredients Chemical characterization (substance): CAS-Number: EC-Number: EINECS-Number: Hazchem-Code: CaH2, Calcium hydride 7789-78-8 001-004-00-5 232-189-2 4Y 3. Hazard identification Classification F Highly flammable R 15 Contact with water liberates highly flammable gas. 4. First aid measures Critical hazard to man and environment: General information: after inhalation: after skin contact: after eye contact: after swallowing: printed by Chemetall GmbH Seek medical treatment when anyone has symptoms apparently due to inhalation or contact with skin or eyes. Provide fresh air. Take all contaminated clothing off immediately. After contact with skin, wash immediately with plenty of water. Immediately flush eyes with plenty of flowing water for 10 to 15 minutes holding eyelids apart. Subsequently seek the immediate attention of an opthalmologist. If swallowed, seek medical advice immediately and show this container or label. ... with QualiSys SUMDAT SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Information to physician: Date of print: Page: 16.01.2003 2of 6 Treat symptomatically. 5. Fire fighting measures Suitable extinguishing media: In case of fire use extinguishing powder on the basis of NaCl (e.g. Totalit M) or pulverized limestone. Never use water. Extinguisher unsuitable on safety grounds: Water, carbon dioxide Particular hazards arising from the substance itself, combustion products or resulting gases: Contact with water liberates highly flammable gas. Particular protective equipment: In case of greater fires: Wear self-contained breathing apparatus. 6. Accidental release measures Personal precautions: Provide adequate ventilation. Avoid generation of dust. Handle always under inert gas. Wear suitable protective clothing, gloves and eye/face protection. Environmental precautions: Do not allow to enter ground soil, sewage or drains. If substance has entered a water course or sewer or has contaminated soil or vegetation, advice police and firefighting department. Methods for cleaning up / spillage removal: Additional information: Cover spilled material with extinguishing powder or pulverized limestone and collect mechanically. Contact experts. Keep away from water. Reacts with water or steam liberating hydrogen and heat. Formation of hydrogen/air mixtures which can ignite on hot surfaces, sparks or open flames instantaneously (explosion). The product is combustible. Never extinguish with a halon or carbon dioxide extinguisher or water. 7. Handling and storage Handling Information for safe handling: Handle always under inert gas. Precautions against fire and explosion: Keep away from sources of ignition. No smoking. Storage Requirement for storerooms and containers: Keep container tightly closed and dry. Provide adequate ventilation. Keep contents under nitrogen (appropriate liquid to be specified by the manufacturer). Information about storage in one common storage facility: Keep away from water. Further information on storage conditions: Storage class: printed by Chemetall GmbH Contact with water liberates highly flammable gas. 4.3 ... with QualiSys SUMDAT SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Date of print: Page: 16.01.2003 3of 6 8. Exposure controls / personal protection Information on system design and engineering measures Keep away from heat. Take precautionary measures against static discharges. Avoid shock and friction. Protect from moisture contamination. See also Information in chapter 7, section storage. Respiratory protection: Hand protection: Eye protection: Body protection: Dust mask Leather gloves tightly sealed safety glasses Wear suitable protective clothing. General protection and hygiene measures: Handle open container with care. Open only when sucking off the air. Use grounding equipment. Keep away from sources of ignition. No smoking. Do not weld. Keep away from water. Avoid contact with skin and eyes. Wash hands when done working with material; at breaks, lunch, shift changes, etc. 9. Physical and chemical properties Appearance powder grey odourless Form: Colour: Odour: Safety relevant data Boiling temperature / boiling range: Melting point / melting range: Ignition temperature: Explosive properties: Density: 600 °C 816 °C >= 300 °C Danger of dust explosion. at 20 °C: 1,9 g/cm³ Additional information Molecular weight: 42,10 Danger of dust explosion. 10. Stability and reactivity Condition to avoid (hazardous reactions): Materials to avoid: Keep away from sources of ignition. Avoid friction sparks. Avoid formation of dust/air mixtures because of explosion hazard. Reaction with water or moist air. Hazardous decomposition products: Thermal decomposition: printed by Chemetall GmbH Calcium, hydrogen 600 °C ... with QualiSys SUMDAT SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Additional information: Date of print: Page: 16.01.2003 4of 6 Risk of fire. Selfignition possible at 20°C. Heat development. Development of explosive gas/vapour. 11. Toxicological information Toxicological Tests Additional information: Following inhalation: Severe irritant to air passages. After ingestion: corrosive Following eye contact: corrosive Following skin contact: Reacts slowly with the moisture of the skin causing corrosion. Sensitization: May cause sensitization by inhalation and skin contact. 12. Ecological information Ecotoxicological effects Aquatoxicity: Water risk class: Toxic to aquatic organisms. 1 Mild water pollutant Additional ecological information General remarks: Do not allow to enter ground soil, sewage or drains. 13. Disposal considerations Product Waste key number (EU): Waste key number (D): Recommendation: 061399 59303 Special waste. If Recycling is not possible, disposal is to be done according to valid local laws and regulations on waste disposal (information obligation of authorities). Contaminated packaging Waste key number (EU): Waste key number (D): Recommendation: 150199 35106 Handle contaminated packaging in the same way as the substance itself. Dispose of waste according to applicable local, state, and federal regulations. 14. Transport information Overland transport Warning board: Description of goods: Packaging group Label Limited Quantities ADR: Substance number 1404 RID: Kemmler-number X423, Substance number 1404 1404, Calcium hydride Class 4.3, Code: W2 I 4.3 LQ0 Contaminated packaging: Instructions P403 Special provisions for collective packaging MP2 printed by Chemetall GmbH ... with QualiSys SUMDAT SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Date of print: Page: 16.01.2003 5of 6 Transport by sea UN number: Proper shipping name: PG: EmS number: Special provisions Limited Quantities 1404 Calcium hydride Class 4.3, Code: I F-G, S-O 934 None Contaminated packaging: Instructions P403 Contaminated packaging: Provisions IBC: Instructions IBC: Provisions Tank instructions: IMO PP31 - Tank instructions: UN Tank instructions Provisions - Air transport UN/ID number: Proper shipping name: ICAO/IATA: Hazard PG: Passenger Ltd.Qty.: Passenger: Cargo: ERG 1404 Calcium hydride Class 4.3 15,0 kg I Y- - Maximum quantity: Maximum quantity: Forbidden 412 - Maximum quantity: 15 kg 4W 15. Regulatory information Classification Code letter and hazard symbol: F R phrase(s): R 15 S phrase(s): S 7/8 S 24/25 S 43 Highly flammable Contact with water liberates highly flammable gas. Keep container tightly closed and dry. Avoid contact with skin and eyes. In case of fire use extinguishing powder on the basis of NaCl (e.g. Totalit M) or pulverized limestone. Never use water. National regulations National regulations Germany Storage class: Water risk class: printed by Chemetall GmbH 4.3 1 Mild water pollutant ... with QualiSys SUMDAT SAFETY DATA SHEET in accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC Calcium hydride Article Number 4551XX Date of first version: 06.03.1994 Revision date: 09.01.2003 Date of print: Page: 16.01.2003 6of 6 Further regulations, limitations and legal requirements: National regulations Great Britain: Blue Book: Dang. when wet & IMDG-Code $ 4337 National regulations Switzerland: Poison Class (Switzerland): 4 = minor strong poisons (EDV-Nr. G-1349) National regulations USA: CFR 49: § 172.102 Dangerous when wet NFPA Hazard Rating: - Health = 3 (high) - Fire = 4 - Reactivity = 3 (high) - Other: Water reactive 16. Other information Further remarks Reason of change: Changes in section 14: Changes in the transport declaration ADR/RID 2003, IMDG 2002, IATA 2003 Literature: Group that issues data sheet Contact person: see chapter 1, department responsible for information. The above information describes exclusively the safety requirements of the product and is based on our present-day knowledge.It does not represent a guarantee for the properties of the product described in terms of the legal warranty regulations. printed by Chemetall GmbH ... with QualiSys SUMDAT
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