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aboniaboniaboniaboniFMXFMXFMXFMX

HydroTracerHydroTracerHydroTracerHydroTracer

Operation Manual

aboni GmbH für Mess- und Automatsierungstechnik

Zeche Ernestine 10D-45145 EssenGermany

Tel. +49 700 abonifon; +49 201 74 70 631+49 700 22664 366;

Fax +49 700 abonifax +49 201 74 70 633+49.700 22664 329

email [email protected]

Operation Manual FMX HydroTracer E2-1 1

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


Measuring Principle

The patented method of the HydroTracer determines the absolute water content. The mass of thewater is measured within the reactor. The percentage of moisture of the sample is calculated bydivision with the sample weight.

The sample is weighed and filled into the sample tray. The sample tray is shifted into theHydroTracer, being a part of the reactor. A heater warms the sample to a temperature chosen by theoperator. The water within the sample material evaporates. The volatile water rises to the upper partof the reactor. Two pipes connect the heated sample tray with the cooled upper part where thereagent 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 thefollowing 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 bynatural convection, created by a special configuration of the vertical pipes. By this method evenhygroscopic materials are completely dried. The final concentration of hydrogen in the reactor isproportional 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 isnecessary to determine the air humidity and the air density. Integrated sensors measure the humidityof the ambient air, the temperature and the air pressure. With this data the software determines thewater 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 thanneeded 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 whichwould be set free by the reaction of hydrogen with the oxygen of the air) is about 0.1 kJ andtherefore harmless.

sensor

sample tray

pipes

reagent bed withreagent

reactor lidCutaway view ofthe reaktor

heated area

cooled area

Evaporated waterreacts to Hydrogen.The concentrationof hydrogen is ameasure of thesample humidity.


The reagent

Calcium hydride reacts with water to calcium hydroxide (hydrated lime, agricultural hydrate), which isa weak base and quite harmless. Nonetheless, take care calcium hydride does not get into contactdirectly with (liquid) water. The reaction heat together with the oxygen of the air could ignite thedeveloping 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. Avoidthe contact with inflammeable, especially wet materials and leave the used reagent exposed to theair, where it can react slowly with the air humidity. An ideal container is an open tin can. After a fewhours calcium hydride is completely transformed to calcium hydroxide. If left even longer exposed tothe air, calcium hydroxide reacts to calcium carbonate ( CaCO3, chalk) with the carbon dioxide of theair 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 PCsoftware. 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 beinstalled 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 fanruns 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 itsoperation temperature.


Operation

Take care the accessories are within reach. Do not leave your sample material exposed to the ambientair 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 notstart but cancel the program by clicking on the CANCEL–button or pressing the key F5. Repeat thesesteps 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 amessage „initalizing, wait“ is blinking.


Input mask 1 appears:

Input mask 1 withintegrated name list andmaterial list

Fill in a name for the operator and the material data or select it out of the tables on the left. The newdata 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 ortype ENTER on the keyboard to finish.

NoteIntegrate the table of materials into the input mask 1

A selection of plastics with proposed data concerning materials, heating temperature and density isincluded within the file „Materialliste“. To integrate this data into the input mask 1 (see pictureabove), copy the file <CD>\:data\Materialliste from the CD into the directory C:\FMX. The next timethe program FMXE02 is called it will automatically integrate this list in the mask. New entries will beadded by the new input arrays on the right. If you want to delete data out of the materials table (orthe name table) call the file with the program WORDPAD and delete the appropriate line. Store thefile Materiallist without extension then.

If the operation system of the PC uses a comma as decimal point, use the file Materialliste in thedirectory <CD>\:comma\Materialliste


Input mask 2 appears:

Put in the sample weight. The error caused by the weight measurement is linear, therefore in manycauses a balance with a resolution of 0.1 g is sufficient. ( Example: Sample weight 20 g, measuredmoisture 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 tothe balance accuracy).

Selection of temperature

The temperatures given in the materials table are proposals, which might not fit always for eachmember of a group of materials. Generally a temperature is chosen which is as high as possible toaccelerate the evaporation of water but low enough to avoid thermal decomposion. Usually themelting of the sample should be avoided to allow easier cleaning of the sample tray. If you are notshure which temperature is appropriate, try lower temperatures first. In some cases the melting of thesample 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, itcan 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 thetray 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 asmall amount. A water content of 5 mg to 10 mg is recommended. The diagrams indicate theoptimum input depending on the (supposed) moisture.

Recom. sample weight (density 1 g/cm³ )

0

1

2

3

4

5

6

7

8

9

10

0,0001 0,001 0,01 0,1 1 10 moisture in %

wat

er c

onte

nt in

mg

Recom. sample weight (density 1 g/cm³ )

0,110

10

20

30

40

50

60

0,0001 0,001 0,01 0,1 1 10

moisture in %

sam

ple

wei

ght i

n g


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. Thetime schedule should be maintained rather accurate. Leaving the reactor open too long as well as tooshort can reduce the accuracy.On the right panel the steps are listed which have occured before, so the menu can be followed evenif a step was missed according the time schedule.

Open the reactor by liftingthe lateral handlessimultaneously. Thesystem fan will stop.

Open reactor by lifting thelid forward into thedirection of the smallsemispherical outcut.


Lift the reagent bed withthe pincers and removethe used reagent

Take out the sample trayby lifting it slightly andpull it out off the front.Remove old samplematerial.

Take a 1/3 of a spoonwith the spatula and fill itinto the reagent bed.


Spread the reagent on thereagent bed.

Close the reagent glassthorougly.

Fill in the sample material.Spread the samplematerial so the bottom ofthe tray in evenlycovered. Clean the rimwith the brush.The seal face is indicatedin red on the screen.


Insert the sample tray.Take care that the lowerrim of the tray is properlyplaced over the heatingplate.

Insert the reagent bedwith the pincers.

Clean O-ring and seal faceof with the brush. Thesealing surfaces areindicated in red on thescreen.


Close reactor lid.Take care the clasp isproperly locked.

Push down simultaneouslythe lateral handles. Thesystem fan must runagain.

After 95 seconds theCONTINUE buttonappears.Click on or press Key F10to start the measurement.No further action isrequired by the operator.


Measuring period

The sample is heated up to the selected temperature. The heating temperature is shown in the upperleft diagram. The diagram below displays the actual total water content in mg. The measuring timedepends on the kind of sample and the water content. Usually a measurement is finished within 15 to45 minutes.The display of the estimated water content occurs after a while, showing the mass percentage. Untilthe measurement is finished, this is only a prognosis, which interpolates the mathematic function ofthe water increase versus time. When the program has finished the measurement the final result isshown.

End of measurement

A menu occurs after the measurement is finished which enables the choice between saving the resultor trash it. If no selection is done within 60 seconds, the results are automatically saved and theprogram stopps. The heater is switched off and the main fan cools the reactor to athe defaulttemperature of 50 °C. When the main fan has stopped, the Hydrotracer is ready for the nextmeasurement.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 graphdo 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 .html-file containing the data and the diagrams as shown on the screen.


The measurement data saved in Data-table.txt is appended as new line to the table, containing all thedata as indicated in the window ´Final Results` on the screen. The .txt-file can be easily read bytabulation programs as Microsoft Excel.

The .html-file is saved as shown in theillustration opposite, if no other selectionis done. The name of the file is createdas FMXdate-time. Time is the start-uptime of the measurement program. Thusthe .html- file can be assigned to ameasurement saved in Data-table.txt,where the first two columns indicate thedate 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 longerperiod or if the water content of a previous measurement exceeded 80 mg. It is also recommended ifthe instrument was not in use for a few days and very low water contents shall be detected. Alwaysleave 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 maxiumheating temperature of 210 °C.

LEDs

There are three light-emitting diodes below the blue plastic sheet on the top of the HydroTracer.

Green indicates: Power supply onYellow indicates: Heater onRed indicates: Error

Errors

If an error occurs during the communication between Hydrotracer and PC, the HydroTracer sends anerror message to the software. In most cases this will interrupt the measurement. Errors of thehardware are indicated by the red LED below the top sheet of the HydroTracer. Shortly break thepower 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, themeasurement is automatically cancelled and the HydroTracer cools down.

Communication problems

In most cases, communication problems are caused by the cabling. Check thoroughly the connectionsbetween PC and HydroTracer. If there are more than two serial ports on the PC, it might be possiblethat the port is not detected automatically by the program (this happens during the initializing at thebeginning). You can select the port manually by using the port-control on the front panel. Select aport 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) theport control in the upper left edge of the screen will show a new port in the scroll-down menu.

Installation Program FMX 2-2 1

Installation of the Software of the FMX HydroTracer

The software has to be installed in 2 steps:A) Installation of the interface driverB) 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 inD:\data\visa301runtime.exe (with D asCD- drive) .

3. The marginal menu appears.Press Setup

4. The marginal menu appears.Press Next.


5. The marginal menu appears.

Click onI accept the License Agreement .

Click on Next.


Click on Next .


Click on Custom.

Click on Next.



Click on PXI.

9. The marginal sub-menu appears.Choose optionDo not install this featureNow this part of the program isdeactivated.

10. Repeat deactivation withwith all submenus butsubmenu Serial, Remote,Enet-Serial, USB, COM-Support.

The menu tree should looklike the marginal picture.

Then click on Next.

11. The marginal menu appears.Click on Next.

The driver configuration is finished.


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 inD:\installer\setup.exe (with D asCD- drive) .

Follow the instructions of the menu. (in local language)The program will be installed into the directory Programs\ FMX 2-2.

SAFETY DATA SHEETin accordance with directives 91/155/EEC, 93/112/EEC and 2001/58/EEC

Calcium hydrideArticle Number 4551XX

Date of first version: 06.03.1994 Date of print: 16.01.2003Revision date: 09.01.2003 Page: 1of 6

1. Identification of the substance/preparationand of the company/undertaking

Identification of the substance or preparationCommercial Product name:

Calcium hydride

Company/undertaking identificationManufacturer / distributor: Chemetall Gesellschaft für chemisch technische Verfahren mbHStreet/POB-No.: Trakehner Straße 3State/city/postal code: D-60441 Frankfurt a. M.Telephone: +49 (0) 69 7165-0Telefax: + 49 (0) 69 7165-2523Dept. responsible for information:

Special Metals Division Telephone: +49 (0) 69 7165-0Additional information: This MSDS pertains to the following products:

455110 Calcium hydride type K455120 Calcium hydride type B455130 Calcium hydride type O455140 Calcium hydride type M

Emergency information:Chemetall GmbH, Langelsheim Telephone: +49 (0) 5326 51-0

2. Composition/information on ingredientsChemical characterization (substance):

CaH2, Calcium hydrideCAS-Number: 7789-78-8EC-Number: 001-004-00-5EINECS-Number: 232-189-2Hazchem-Code: 4 Y

3. Hazard identificationClassification

F

Highly flammable

R 15 Contact with water liberates highly flammable gas.

4. First aid measuresCritical hazard to man and environment:General information: Seek medical treatment when anyone has symptoms apparently due to inhalation or

contact with skin or eyes.after inhalation: Provide fresh air.after skin contact: Take all contaminated clothing off immediately.

After contact with skin, wash immediately with plenty of water.after eye contact: Immediately flush eyes with plenty of flowing water for 10 to 15 minutes holding eyelids

apart. Subsequently seek the immediate attention of an opthalmologist.after swallowing: If swallowed, seek medical advice immediately and show this container or label.

printed by Chemetall GmbH ... with QualiSys SUMDAT




Information to physician: Treat symptomatically.

5. Fire fighting measuresSuitable 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 dioxideParticular 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 measuresPersonal 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:

Cover spilled material with extinguishing powder or pulverized limestone and collect mechanically.Contact experts.

Additional information: 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 storageHandlingInformation for safe handling:

Handle always under inert gas.Precautions against fire and explosion:

Keep away from sources of ignition. No smoking.

StorageRequirement 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:Contact with water liberates highly flammable gas.

Storage class: 4.3





8. Exposure controls / personal protection

Information on system design and engineering measuresKeep 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: Dust maskHand protection: Leather glovesEye protection: tightly sealed safety glassesBody protection: 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 propertiesAppearanceForm: powderColour: greyOdour: odourless

Safety relevant data

Boiling temperature / boiling range: 600 °CMelting point / melting range: 816 °CIgnition temperature: >= 300 °CExplosive properties: Danger of dust explosion.Density: at 20 °C: 1,9 g/cm³

Additional information

Molecular weight: 42,10Danger of dust explosion.

10. Stability and reactivityCondition to avoid (hazardous reactions):

Keep away from sources of ignition.Avoid friction sparks.Avoid formation of dust/air mixtures because of explosion hazard.

Materials to avoid: Reaction with water or moist air.Hazardous decomposition products:

Calcium, hydrogenThermal decomposition: 600 °C





Additional information: Risk of fire.Selfignition possible at 20°C.Heat development.Development of explosive gas/vapour.

11. Toxicological information

Toxicological TestsAdditional information: Following inhalation: Severe irritant to air passages.

After ingestion: corrosiveFollowing eye contact: corrosiveFollowing 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 effectsAquatoxicity: Toxic to aquatic organisms.Water risk class: 1

Mild water pollutant

Additional ecological informationGeneral remarks: Do not allow to enter ground soil, sewage or drains.

13. Disposal considerationsProductWaste key number (EU): 061399Waste key number (D): 59303Recommendation: 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 packagingWaste key number (EU): 150199Waste key number (D): 35106Recommendation: Handle contaminated packaging in the same way as the substance itself.

Dispose of waste according to applicable local, state, and federal regulations.

14. Transport informationOverland transportWarning board: ADR: Substance number 1404

RID: Kemmler-number X423, Substance number 1404Description of goods: 1404, Calcium hydride

Class 4.3, Code: W2Packaging group ILabel 4.3Limited Quantities LQ0Contaminated packaging: Instructions

P403Special provisions for collective packaging

MP2





Transport by seaUN number: 1404Proper shipping name: Calcium hydride

Class 4.3, Code: -PG: IEmS number: F-G, S-OSpecial provisions 934Limited Quantities NoneContaminated packaging: Instructions

P403Contaminated packaging: Provisions

PP31IBC: Instructions -IBC: Provisions -Tank instructions: IMO -Tank instructions: UN -Tank instructions Provisions

-

Air transportUN/ID number: 1404Proper shipping name: Calcium hydrideICAO/IATA: Class 4.3Hazard 15,0 kgPG: IPassenger Ltd.Qty.: Y- - Maximum quantity: -Passenger: Maximum quantity: ForbiddenCargo: 412 - Maximum quantity: 15 kgERG 4W

15. Regulatory informationClassificationCode letter and hazard symbol:

F Highly flammableR phrase(s): R 15 Contact with water liberates highly flammable gas.S phrase(s): S 7/8 Keep container tightly closed and dry.

S 24/25 Avoid contact with skin and eyes.S 43 In case of fire use extinguishing powder on the basis of NaCl (e.g. Totalit M)

or pulverized limestone. Never use water.

National regulationsNational regulations Germany

Storage class: 4.3Water risk class: 1

Mild water pollutant





Further regulations, limitations and legal requirements:

National regulations Great Britain:Blue Book: Dang. when wet & IMDG-Code $ 4337National regulations Switzerland:Poison Class (Switzerland): 4 = minor strong poisons (EDV-Nr. G-1349)National regulations USA:CFR 49: § 172.102 Dangerous when wetNFPA Hazard Rating:- Health = 3 (high)- Fire = 4- Reactivity = 3 (high)- Other: Water reactive

16. Other information

Further remarksReason of change: Changes in section 14: Changes in the transport declaration ADR/RID 2003, IMDG 2002,

IATA 2003Literature:

Group that issues data sheetContact 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.


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