0.1 0.1 Operation Manual H - 500 · Copyright Ó 2005 by ELTRA GmbH Germany – August 2005 –...

Copyright 2005 by ELTRA GmbH Germany – August 2005 – Operation Manual H-500 0.1-1

0.1 0.1

Operation Manual H - 500

1 INSTALLATION 1.1 Setting up 1.2 Front panel illustration 1.3 Mains power connections 1.4 Data Interfaces 1.5 Gas connections 1.6 Adjusting the gas flow 1.7 Adjusting the furnace temperature

2 ANALYSIS 2.1 Working procedure 2.2 Collecting samples of melted steel 2.3 Calibration of the analyser using gas dosing device 2.4 Work breaks

3 MAINTENANCE 3.1 General information 3.2 Installing and removing the reagent tubes 3.3 Filling the reagent tubes 3.4 Replacing the O-rings 3.5 Replacing the combustion tube

4 DESCRIPTION OF FUNCTION 4.1 Measuring principle 4.2 Gas flow system 4.3 Thermoconductivity cell 4.4 Micro controller 4.5 Furnace

5 MISCELLANOUS 5.1 Ordering numbers 5.2 Packing 5.3 Software 5.4 Pre-installation guide


1 INSTALLATION

1.1 Setting up As the device is rather light, ca. 40 kg, there are no strong recommendations concerning the stability of where it is set up. Due to the balance, the platform should be placed to be as free of vibration as possible. Placing the furnace to the right of the analyser is generally recommended. The position of the balance is optional. Generally, placing it on the right is recommended. The size of a desktop is sufficient for the entire set-up. Below is an example of installation:

��The environment of the device must not necessarily be air-conditioned, although it is

best if the room temperature remains between 18°C and 25°C. Under no conditions the device should be placed in direct sunlight ! Avoid places exposed to the wind of air conditioners or to the wind blowing through open windows or doors.

Serial No.:

5 0-60

75

2 30 +/- 10%

XXXXXXXXXX

Mo del No.:

0 ,33

H 500

Volts AC:

Amps :

Watts :

Hz :

E LTRA G mbHMai nstr . 85B lock20 D- 41469 Neuss Ger ma ny

Phone: ( 49)213 712822 Fax:( 49) 2137 12513

2-1-1 H500

230 V AC 50 0W ma x

for bal an ce, pr in ter

and comp uter o nl y

Nitr og en I npu t2- 4 b ar ( 30 - 60 p si )

9 9, 9% p u re

Furnace i n Gas out let

F urnace out

4 A Fu se slow b low 4A

0, 33 A 75 Wa tts2 30V AC +/-10 % 50/60 Hz


1.2 Front panel illustration

1 Set point / Furnace temperature display 2 Set point / Furnace temperature switch 3 Temperature adjustment 4 Cock for gas dosing device 5 Flow display 15l/h 6 Adjustable restrictor 7 CO � CO2 conversion (Schutze reagent), CO2 trap, H2O trap 8 Carrier gas purification 9 Flow display 15l/h (furnace inlet) 10 Flow display 130l/h (analytical, actuated by the gas pump) 11 Adjustable restrictor for furnace inlet gas flow adjustment 12 Pressure gauge 1,5 bar / 22 psi 13 Mains power switch 14 Furnace

1,5

2

1

2, 5

0 ,5

4 0 0

2 0 0

6 0 0

3 0 0

2 0 0

1 0 0

0

1-3-1H500

Set Point

Fu rnace Tempera tu re

°C1 00 0

H 500H yd rogen D ete rmina to rPC con tro l led

1

23

4

5

6

7 8

9

10

13

12

11

14


1.3 Mains power connections As the TC-cell requires about 1 hour to reach a stable operating temperature, it is advisable to connect the analyser to the mains power first and switch on, before further installation work is carried out. This waiting time is only necessary when installing the analyser, because normally it is not switched off and therefore always in operating temperature.

1 Analyser 2 Computer 3 Monitor 4 Printer 5 Balance 6 Triple power outlet 7 Analyser mains plug

At first only the analyser (1) is plugged in and switched on. Turn the main switch to position 1 (stand-by condition). See 1.2. All the mains cables should be connected as shown in the schematic above. The computer (2), the printer (4) and the balance (5) should be plugged into the triple power outlets (6) on the rear side of the analysis device.

Ser ial No. :

50- 60

75

230+ /- 10%

XXX XXXXX XX

Model No. :

0,33

H500

Vol tsA C:

Am ps:

W att s:

Hz:

E L TR A Gm b HM a ins tr. 85 Bl oc k2 0D -4 14 69 N eu ss Ge rm an yP h on e:( 49 )21 37 1 28 22 F ax :(4 9)2 13 7 12 51 3

2 30 V A C5 0 0W max

f o r ba l an ce , pri n t er

a nd co mp ut e r on l y

Nit ro ge n In pu t2 -4 b a r (3 0 -6 0p s i)

9 9,9 % p ure

Furna ce i n Ga s outl et

Furna ce ou t

4A Fu se s lo w bl ow 4A

0 ,3 3A 7 5 Wa tts23 0V AC +/-1 0% 5 0/6 0Hz

2

3

4

5

2-2-1 H500

1

6

7


1.4 Data Interfaces

Rear side of UNI 1.4 board:

1 Balance connection (serial) 2 PC connection (serial interface (COM-port)) 3 Analog input/output signals 4 Digital input/output signals 5 Autoloader connection

When all the units are connected to the mains power, then data connections can be made. The plugs are all different from each other, so that they cannot be interchanged. The required data cables are included if the additional units are supplied. These are adapted to the interfaces when the analysers are put into operation in our company. As the balance transfers the weight to the analyser, its serial interface must be programmed. The computer is already provided with an operating system and software for controlling the analyser. NOTE: For all instructions on operating the PC software refer to the Help-function of the software.

2

3 45

1

2-3-1

Analog I/O Digital I/O

Loade

rMicrocontrollerboard UNI 1.4Part No.18467

PC

Balance


1.5 Gas connections For the operation of the analyser nitrogen supply is necessary. The necessary tube is shipped together with the device.

The tube connects the device through the fitting (1) with the nitrogen bottle, or nitrogen supply, through a pressure regulator. This connection must be very secure, given that the operating pressure in the tube is 2 to 4 bar (30 to 60 psi). The tube connection (2) is the exhaust for the gas flow system. If desired, the exhaust can be channelled through a tube into the open air. NOTE: If the gas dosing device is used for calibration of the analyser, the pure helium gas supply must be connected to the analyser. The fittings for connection are situated on the rear side of the analyser and marked as “He in” and “He out”. The pressure on the input is 1 to 2 bar (15 to 30 psi).

Ser ial No.:

50- 60

75

230 +/- 10%

XXXXXXXXXX

M odel No.:

0,33

H 500

Volts AC:

Amp s :

Wa tts :

Hz :

E LTRA G mb HM ainst r .85 Bl ock20 D- 41469 N eussG er ma ny

Pho ne:( 49) 2137 1282 2 Fax: (4 9)21 371 2513

2-4-1 H500

2 30 V AC 50 0W ma x

for b a la nc e, p ri nt era nd co mpu ter on l y

Ni tro ge n In pu t2- 4 bar (30- 60psi )

99,9% pur e

Fu rn ace i n G as ou tl et

Furnace out

4A Fuse slow b low 4A

0, 33A 75Watt s230V AC +/-10% 50/60Hz

2

1


1.6 Adjusting the gas flow

Before adjusting the furnace input flow assure the following: ��The analyser is connected to the nitrogen supply. See 1.5. ��Adjust 2 to 4 bar (30 to 60 psi) on the pressure regulator of the Nitrogen supply (nitrogen

cylinder). ��Set the main power switch (1) of the analyser to position 2. ��Read 1,5 bar on the pressure gauge (2). Adjust the restrictor (3) to read about 50 l/h on the flow meter (4) The pump in the analyser is now in operation and the flow of about 10 l/h is displayed on the upper flow meter (5). This flow is electronically regulated. An external adjustment is neither necessary nor possible.

1, 5

2

1

2, 5

0 ,5

4 0 0

2 0 0

6 0 0

3 0 0

2 0 0

1 0 0

0

1-3-1H500

Set Point

Furnace Tem peratur e

°C1000

H 500Hydrogen Det ermi nat o rPC cont rol led

1

2

3

4

5


1.7 Adjusting the furnace temperature

��Set the mains power switch (1) to position 1 or 2.

��Set the switch (3) to position "Set point".

��Set 1000°C on the display (4) by turning the potentiometer (2).

��Set the switch (3) to "Furnace temperature".

��The display (4) now shows the current furnace temperature.

Normal operation temperature for the H-500 is 1000°C.

1 ,5

2

1

2,5

0,5

4 0 0

2 0 0

6 0 0

3 0 0

2 0 0

1 0 0

0

3-1-1H500

Set Point

Fur nace Temperature

°C

2

1

3

41000

H 500Hydr ogen Dete r mina to rPC con t ro l led


2 ANALYSIS

2.1 Working procedure With the H-500 only steel materials can be analysed. In this chapter the procedure of analysis is described. Before carrying out analyses the following must be assured: ��The temperature of the analyser has to be stable - at least one to two hours with the

mains switch on position 1. ��The moisture trap (5) is checked and, if necessary, it is replaced. See 5.3. ��The incoming nitrogen supply must have a pressure of 2 - 4 bar / 30 to 60 psi. ��The furnace has reached it’s operating temperature. See 1.7. ��The mains switch is set to pos.2 for at least 10 to 15 minutes.

1. The sample must be weighed before carrying out the analysis.

The balance is tared by pressing the TARE button. A pin sample of about 5 grams is placed on the balance. Sample weight must be entered into the software.

NOTE: For all instructions on operating the PC software refer to the Help-function of the software.

1,5

2

1

2,5

0 ,5

4 0 0

2 0 0

6 0 0

30 0

2 00

1 00

0

3-1-1H500

Se t Po in t

Fu rnace Te mpe rature

°C

2

1

3

4

5100 0

H 50 0Hyd ro ge n Deter mina to rP C c on tr ol l ed


Sample weights: The sample weight depends on the H concentration, on the sensitivity of the TC-cell and on the response of the sample inside the furnace. The usual sample size for steel is 50 mm of length and 5 mm in diameter. The weight is around 5 g. The suggested sample size limits are: length = 75 mm and diameter = 6 mm. There is no weight limit, the bigger the sample the higher the peak, which is an advantage. The bigger the diameter, the longer the analysis, more time is needed for the hydrogen to be released from the sample. For this reason, instead of taking bigger samples, it is rather advisable to take more than one sample for an analysis. (two, three or four pins of normal size).

2. The sample is placed into the entrance of the furnace.

Place the furnace in a horizontal position, see drawing A. Insert the sample into the tube of the furnace, about 15 mm from the opening of the tube. Leave the sample in that position for about 10 to 15 seconds

3. Analysis procedure is started.

Press “Start” button in the “Analysis control” window of the software. Analysis procedure is initiated.

4. The sample is entered into the furnace’s hot area.

As soon as the “Analysis” appears in the “Status” window of the software lift the furnace holding it by the handle until the sample slides into the hot area of the furnace, see drawing B. The furnace then is turned back to the horizontal position.

The analysis then runs, and no more handling is necessary. The TC cell signals can be observed and followed on the PC screen. 5. The sample is removed from the furnace after analysis ends.

At the end of the analysis, the handle of the furnace is moved down to enable the sample to drop out of the furnace into a thermally safe pot. See drawing C.

CAUTION: Do not catch the falling sample with your hands! Very hot!

A CB


2.2 Collecting samples of melted steel The specially designed evacuated pin tubes collect melted steel samples. The sample should be stored in liquid nitrogen or dry ice, until the analysis takes place. These pin tubes are made up of a thick section A and a thin section B.

With a special pin tube holder, the pin tube is held and immersed with the thin section B into the melted steel. The heat opens the thin section and the vacuum sucks the steel into the pin tube. CAUTION: Some of the hydrogen contained in the sample is lost at high temperatures. The purpose of the analysis is to establish the true content of hydrogen in the sample. It is therefore necessary to take the sample and to cool it down as fast as possible immersing it in water. During the immersion knock on the sample to brake off the surrounding of the pin tube. Do not leave the sample in the water, because bubbles tend to accumulate on the surface, which reduces the efficiency of cooling, and thus even more hydrogen from the sample will be lost. Preparing the sample for the analysis. To prepare the sample, cut a section of correct dimension. Use an abrasive sawing machine ensuring that plenty of coolant is used. The sample must not exceed a length of 60-70 mm and a diameter of 6-8 mm. Normally there is a layer of heavy oxide on the surface of the sample which needs to be removed. Finally the sample is washed in acetone and then rinsed in ether. A quick blast from a hot air dryer will remove the ether. It is possible to remove the solvent using a vacuum chamber. The vacuum method is most efficient if the sample has a micro porosity and some of the solvent has entered the cracks.


2.3 Calibration of the analyser using gas dosing device The H-500 is equipped with the gas dosing device for gas calibration. The calibration gas is helium.

The gas calibration is carried out as follows: 1. Assure, that the calibration gas supply pressure on the input of the analyser is 1-2 bar. 2. The conditions before starting making analyses has to be met as well. See 2.1. The

furnace temperature is irrelevant for the gas calibration procedure. 3. Pull the knob (4) of the gas dosing cylinder rod. It will move out for app. 5 mm. 4. Rotate the adjustable flow restrictor (6) counter clockwise to purge and fill the calibration

volume of gas dosing device with calibration gas. The flow rate of the gas passing through the calibration volume can be observed on the flow display (5). 10 l/h for several seconds are sufficient for this purpose.

5. Afterwards, stop the calibration gas flow by turning the adjustable flow restrictor (6) clockwise. Wait until the gas flow on the flow display (5) drops completely. Wait another 30 seconds.

6. Enter 1000 mg as a sample weight into the software and start the analysis. As soon as “Analysis” is displayed in the status window of the software, push the knob (4) of the gas dosing cylinder rod. It will move in for app. 5 mm, to initial position.

7. Analysis runs automatically. The analysis results, which will be used for calibration, are displayed on the screen and saved after analysis is finished. The standard value, which has to be entered for the calibration can be found near the gas dosing cylinder, behind the left side panel of the analyser.

NOTE: For all instructions on operating the PC software refer to the Help-function of the software.

1,5

2

1

2, 5

0 ,5

4 0 0

2 0 0

6 0 0

3 0 0

2 0 0

1 0 0

0

1-3-1H500

Set Point

Fu rnace Tempera tu re

°C1 00 0

H 500H yd rogen D ete rmina to rPC con tro l led

1

23

4

5

6

7 8

9

10

13

12

11

14


2.4 Work breaks The mains switch of the H-500 analyser has 3 positions: 0 – Off 1 – Stand by 2 – Operation During work breaks, e.g. lunch breaks, the mains switch remains on position 2. During longer interruptions, e.g. after finishing work for the day, the mains switch is set to position 1 (standby). The analyser's thermostatic control is then still working and no long warm-up time is needed when re-starting the analyser. Energy consumption and wear are negligible on standby. The analyser is designed for long term use, so that no damage results. The mains switch is set to pos.2 for about 10-15 minutes before starting the first analysis. Air and any moisture which has entered the analyser are expelled by the nitrogen flow. The slight influence which the nitrogen flow has on the temperature of the TC-cell, is balanced out. The mains switch is only set to zero for safety reasons or when the analyser is not in use for a long time (more then several days).


3 MAINTENANCE

3.1 General information There are chemicals used in H-500 analyser which become saturated with the time or after certain number of analyses were carried out and must be replaced periodically. The accuracy of the analyses results depends greatly on the quality and condition of the chemicals, therefore their importance should not be underestimated. The periodicity of replacing the chemicals depends on the carrier gas purity, intensity of use of the analyser and the material of analysed samples. The chemicals can be replaced with certain periods or as soon as the saturation signs are visible, i.e. more then half of the chemical is saturated. In common case, the following periods are valid: Every 50 analyses: ��Replace the content of the left glass tube on the front panel of the analyser. See 3.3. Every 100 analyses: ��Replace the content of the right glass tube of the analyser. See 3.3. The chemicals used in the analyser have visual signs of saturation: Chemical Saturation sign Magnesium perchlorate the particles do not move separately, but stick together Sodium hydroxide changes from black to light grey Shutze reagent changes from yellow to brown (red-brown)

NOTE: ��It is not possible to dry the magnesium perchlorate and use it again, as it is chemically

changed after reacting with the moisture. ��Magnesium perchlorate is a very strong oxidative material! The local safety

precautions for handling the chemicals must be followed in any case. ��In order not to miss, but to carry out maintenance in time, the deficiency counters can be

specified in the software (Refer to the help function of the software). IMPORTANT: There are qualities of chemicals such as anhydrone, ascarite, Shutze reagent etc. which have been specially developed for analytical instruments. The commonly available materials serve their specific purposes either inadequately or not at all. The magnesium perchlorate which is commonly available, causes a memory effect and affects repeatability. Another typical effect is that the analysis takes too long and is often not even completed. This effect also occurs with magnesium perchlorate of suitable quality if it is saturated. The commonly available sodium hydroxide binds CO2 very inadequately at room temperature, whereas the special quality not only binds extremely well at room temperature but also contains an indicator.


The glass tubes and the O-rings should be lubricated with high vacuum silicon grease and not with ordinary silicone grease. The user is free to test commonly available materials; the analyser will not be damaged. If problems should arise, however, suitable materials, in proper, unsaturated condition, should be used, before calling technical service. The chemical containers must be closed very tightly, immediately after use, so that they do not become contaminated with air moisture or CO2.


3.2 Installing and removing the reagent tubes

To replace the reagent tubes: The reagent tubes are first lifted, then swung to one side, detached diagonally downwards and emptied. IMPORTANT: The dimensions for filling the glass tubes given in the schematic of 3.3-2 should be respected in all cases. When, for example, there is not enough quartz wool in the bottom of the glass tube, it is possible that dust forming magnesium perchlorate can fall through and block the fitting below. This can damage the analyser and the TC-cell. The components are refitted in reverse order.


3.3 Filling the reagent tubes Chemical Function Magnesium perchlorate (anhydrone) moisture trap Sodium hydroxide CO2 trap Schutze reagent conversion CO to CO2

The reagent tubes are replaced when they are saturated. See 3.1. Please refer to the following schematics to identify the glass tubes on the analyser. In addition to the reagents in the glass tube, fill the bottom end of the tube with annealed glass wool. One should pay attention that the glass wool should be only as thick as necessary, otherwise the flow of gas can be choked. Under no conditions should the amount of glass wool be less than that given in the following schematics, since fine particles of magnesium perchlorate can pass through the wool and collect itself at the bottom of the tube, causing severe damage. At both ends of the glass tube, you should leave sufficient space for the gas connections to be fitted. The free space at the tube ends serve as sealing space. They must be cleaned after filling. The O-rings must be cleaned. Both the O-rings as well as the sealing area of the tube must be greased with high vacuum silicon grease. This eases the assembly as well as the disassembly and further improves the seal. The assembly of the tubes follows in reverse order from the procedure given in 3.2.


Filling quantities ± 20 % 1 Glass wool 90331 2 Magnesium perchlorate (anhydrone) 90200 3 Sodium hydroxide (ascarite) 90210 4 Schutzes reagent 90270 5 Free (empty) 6 Holding device 47200

1 ,5

2

1

2 ,5

0 ,5

0

6-4-2

30

85

30

75

20

15

60

15

15

15

4

3

51

2

1

5

32Se t Point

Furnace Temperature

°C1000

H 500Hydr oge n Det ermi nato rPC co ntr o l le d

6


1 ,5

2

1

2,5

0 ,5

4 0 0

2 0 0

6 0 0

3 0 0

2 0 0

1 0 0

0

1-3-1H500

Set Point

Furnac e Tem pera tu re

°C1 0 00

H 500Hyd rogen De te rmi na to rPC c ont ro l led

70230

70230

70230

70230

3.4 Replacing the O-rings The O-rings (70230) are only replaced when they can no longer adequately seal, due to severe damage or age. When removing the old O-rings, be sure that the sealing area of the fittings is not damaged. The groove in which the old O-rings sat must be cleaned, so that it is completely free of grease. The new O-rings should under no-circumstances be greased before installing, only after installation. Otherwise, the O-rings will turn with the glass tubes when trying to remove it.


3.5 Replacing the combustion tube

The replacement of the combustion tube is carried out in the following order: 1. Remove the plastic tube (1) together with the copper tube (2) from the combustion tube

inlet (3). 2. Remove the plastic tube (4) together with the copper tube (5) from the outlet of the

combustion tube. 3. Pull the combustion tube (3) out of the front of the furnace. 4. Install a new combustion tube in reverse order. It is advisable to grease the ends of the combustion tube with silicon grease before connecting the plastic tubes. This will enable an easy removal of the plastic tubes for the next replacement

5

4

12

3

6-1-1 H500


4 DESCRIPTION OF FUNCTION

4.1 Measuring principle The measuring method is based on the principle of sample heating, which releases hydrogen and the subsequent analysis through thermal conductivity measurement. The analytical flow amount is held constant through an electronic flow controller at 10 l/h (when not otherwise specially adjusted). The moisture trap along the gas flow system, ensures that a dry gas is supplied to the TC-cell. The TC-cell produces a signal that corresponds to the hydrogen concentration in the gas mixture. This signal is electronically linearized, integrated, divided by the sample weight and the percentages of hydrogen is shown digitally. Since the sample weight is considered, the displayed measurement results are independent of the weight. For this purpose, the sample is weighed before the analysis and its weight is transferred from the balance to the PC software.


4.2 Gas flow system

OUT

I N

13

19

12 10

16

17

18

G a s p um p

Filter

²CO > CO

CO ²H O²

g re e n b l u e

y e l l o w g re y

15T C C E L L

Fi l t e r

11

Controlled1 5 l / h

6

7Controlled

1 3 0 l / h

0. 5

1. 5

2

1

2 . 50

ba r

54

3

1

Pr es su resw i t c h

1 . 5 b a r2 2 p s i 2

Pressureregu la tor

9

CO²

H O²

8

0 . 3 5 b a r / 5 . 3 p s i

14Pressureregulator

CO ²

contr

olle

d

Eic

hg

as

15

l/h

47910Gas flow diagram H-500

²CO > CO Schutzes reagent

CO Trap sodium Hydroxid²H O Trap Magnesium perchlorate²

Pressureregula tor

20

0 . 3 5 b a r

Flo

wse

nso

r

Inject Fill

Eich Volumen0,5Ox150mm

1,5Ox40mm

VitonschlauchVitonschlauch

Vitonschlauch

Vito

nsch

lau

ch

Vitonschlauch Vitonschlauch

Vitonschlauch

Vitonschlauch

Vitonschlauch

PVC Schlauch

PVC Schlauch

PVC Schlauch

PVC Schlauch

PVC Schlauch

PVC Schlauch

1 . 5 b a r

4768047690

PVC Schlauch

A

B

C

Vitonschlauch

47132

47696

Vitonschlauchverbindung

Vitonschlauchverbindung

47697

PVC Schlauchverbindung

21

22

23


1 Carrier gas inlet 13 CO�CO2 conversion, CO2- H2O-trap 2 Pressure regulator 1,5 bar 14 Pressure regulator 0,35 bar 3 Carrier gas stop valve 15 TC-cell 4 Pressure switch 16 Filter 5 Pressure gauge 17 Analytical flow meter (pump) 6 Furnace inlet flow adjustment 18 Filter 7 Furnace inlet flow meter 19 Gas pump 8 Carrier gas purification 20 Pressure regulator (gas calibration) 9 T-piece for TC’s reference flow 21 Adjustable restrictor 10 Furnace input 22 Flow meter 11 Furnace 23 Gas dosing cylinder 12 Furnace output

The nitrogen supply is connected at the inlet (1) of the gas system. Nitrogen of normal technical purity, such as it is available in metal tanks, with a purity of 99.5% is entirely suitable. The nitrogen inlet pressure should be 2 to 4 bar, which is then regulated by the pressure regulator (2) inside the analyser to 1.5 bar, as shown on the pressure gauge (5). Any pressure fluctuation of the external nitrogen supply has no influence on the accuracy of the measurements. The carrier gas stop valve (3) is connected to the mains switch. It is closed (no voltage on the coil) if the mains switch is in pos. 0 or 1 and opened if the mains switch is in pos. 2, thus supplying the carrier gas flow to the analyser only when analyser is in operation. The pressure switch (4) switches the pump on if the carrier gas pressure is more then 1 bar, thus preventing the pump from sucking the atmospheric air, when there is no carrier gas supply. The furnace input flow is adjusted by the restrictor (6) to at least 50 l/h and can be observed on the flow meter (7). This flow is fed into the furnace inlet (10). Impurities in the nitrogen are absorbed into the attached trap (8). The top half of this trap is filled with a CO2 absorber, and the bottom half with a moisture absorber. Magnesium perchlorate (anhydrone) acts as a H2O absorber witch catches any moisture from the gas. Sodium hydroxide acts as a CO2 absorber. At the furnace outlet (12), the hydrogen from the sample, simultaneously with the nitrogen, is sucked by the low pressure created by the pump, and is fed out at a flow rate of 10 l/h. This flow out of the furnace is lower than the flow rate that comes into the (open) inlet. The difference is expelled from the furnace inlet. This prevents air from entering the combustion area. The Schutzes reagent in the glass tube (13) converts CO to CO2, in case any CO is created in the furnace. The CO2 and H2O in the gas mixture are trapped as well by sodium hydroxide and magnesium perchlorate correspondingly. Once the measuring gas is dried up, it is fed through the TC-cell (15). It is here where the gas measurement takes place. Finally, the gas is fed through the upper flow meter (17) on the front side of the analyser. The displayed value must stay at constant 10 l/h. The flow is maintained by a pump (19) and it is electronically controlled. The calibration gas (He) is supplied to the input of the pressure regulator (20). The adjustable flow restrictor (21) and flow meter (22) are used to adjust the flow which will purge and fill the calibration volume of the gas dosing cylinder (23).


4.3 Thermoconductivity cell The thermoconductivity cell detects changes of the contents by measuring the thermal conductivity. The thermal conductivity is not absolutely measured, but in relationship to a reference to get a better resolution. This reference is normally the pure carrier gas.

1 Thermo-stabilised cell 2 Measuring channel 3 Reference channel 4 Thermistors 5 Amplifier 6 Electronic unit There are two channels in the cell (1); the measuring channel (2) in which the analysis gas streams, and the reference channel (3) with the pure carrier gas. In each channel there are two thermistors (4) which detect every change of the thermal conductivity of the surrounding with a change of their electric resistance. The thermistors are connected as a Wheatstone-bridge for a measurement with a constant current. The signal of the thermistors is amplified by an amplifier (5) and gets into the micro controller (6). The base line is automatically set to zero, so that no adjustment is necessary. The thermo-stabilisation takes care that the surrounding has no influence on the cell.


4.4 Micro controller The micro-controller module (MCU) contains all components for signal processing and control sequencing. It is working exclusively under the control of the PC software, gathering signals for sending to the PC-software and outputting signals received from the PC-software. The communication between MCU and PC is taking place via serial interface (RS-232). The zero point of the every TC-cell signal is automatically corrected. This correction takes place always, except two cases: ��during analysis, it is freezed, after passing the stability-check before analysis’ start; ��it is disabled during performing the base-line test; The signal from the TC-cell is integrated to calculate the analysis result. The integration starts at the beginning of the analysis and ends after a pre-set minimum time. If the combustion should take longer, the integration is prolonged. In so doing, the detector signal is compared to a comparator level. The integration continues as long as the measurement signal is higher than the comparator level. When it falls below this level, the integration is stopped. Should the measurement signal remain above the comparator level, the analysis is interrupted by a pre-set maximum time. Then the integration is also completed. The integral value is directly proportional to the H content in the combustion gases. The blank value is deducted from the integral value. The signal is then multiplied by the calibration value. By dividing it further by the sample weight, a result is obtained which is not dependent on the weight. If the multipoint calibration is defined, the result will be corrected accordingly to the curvature of the multipoint characteristic. Afterwards result is directly shown as % H on the PC screen. For the instructions on operating the PC-software, please, refer to the Help-function of the Software.


4.5 Furnace The combustion furnace is a resistance furnace. The temperature is adjustable up to 1100°°°°C. The furnace is fully electronically controlled and therefore has no transformer. The set point of the temperature is manually adjustable and is shown on the digital display at a resolution of 1°C. The actual value is measured by a PtRh-Pt- thermocouple. Both signals are fed to the differential input of an extremely sensitive amplifier. The output signals of this amplifier controls the electronic power, so that the actual value (and therefore the temperature) is exactly the same as the temperature setting. A further sensor reads the environmental temperature and corrects the reference point of the thermocouple, so that variations in the environmental temperature have no influence of the furnace temperature. The electronic controlling supplies the heating element with continuous power through phase angle control. This helps to ensure that the temperature is held constant, in contrast to the normal Off / On regulation. Therefore the temperature can be digitally displayed within 1°C, without up or down variations. Through providing a continuos level of power, temperature variations of the heating wire are largely eliminated, so that a maximal operating life of the furnace can be achieved.


5 MISCELLANOUS

5.1 Ordering numbers Front side:

11064 Reagent tube 11185 Paper filter 11480 Adjustable restrictor 15083 Flow display 15l/h 15085 Flow display 130l/h 35850 Main power switch 47012 Electronic unit 47200 Clamping fixture 70230 O-ring 72010 Pressure gauge

M e nuC LR C al

b l

Enter S TO P START

m g

1 ,5

H- 50 0Hydrogen Determinator

2

1

2 ,5

0,5

N r.

Set Poi nt

Furnace Temperature

°C 4 0 0

2 0 0

6 0 0

3 00

2 0 0

1 0 0

3.86 ppm H

1000

1 2 : 0 1 1 2 3 4 5 6 7 8 0 / 0 1 4 5 2 2 0 . 4 m g

1 20 0

0

1-3-1H500

35850

72010

11480

15085

15083

70230

70230

70230

7023070230

11185

11185

47200

11064

11

06

4


Rear side:

11035 Cooling fan 11492 Pressure regulator

DIGITAL ANALOG

PRINTERS er ial No.:

50-60

75

230 +/-10%

XXX XXXXXXX

Model No.:

0,33

CS 500

Volts AC:

A mps :

Watts :

Hz :

ELTRA Gm bHMai nst r. 85Bl ock20D- 41469NeussGer manyPhone:( 49)213712822 Fax: (49) 2137 12513

BALANCE COMPUTER

Ox yge n In pu t2-4 bar (30 -60ps i )

9 9, 9% pu re

Furnace in Gas out let

Fu rnac e ou t

4A Fuse slow blow 4A

0, 33A 75 Watt s230V A C +/ -10% 50/ 60Hz

230V A C 500W maxf or balance, pri nterand comput er only

1-3-1H500

1 1492

11035


5.2 Packing

Before packing the analyser and the furnace must be wrapped in plastic foil to protect them from moisture and dust, and then to be placed in a wooden case. The wrapped analyser and furnace should be surrounded by a layer of foam (chips) of at least 10cm, in order to avoid any damage due through transport. Especially the foam where the analyser and furnace are put on is very important. It should be neither too hard nor too soft. When the foam is too soft, the analyser will practically touch the wood. Fix the foam on the bottom of the wooden case by gluing. The analyser and furnace should be wrapped in plastic foil, especially when you use chipsor any other kind of material in small pieces. The glass tubes must be empty.

atleast10to15cm

Foam or chips

at least 10 cm at leas t 10 cm

Wooden case

M e nuC LR Cal

bl

E n ter STO P STAR T

m g

1,5

H- 50 0Hydrogen Determinator

2

1

2 ,5

0 ,5

Nr.

Set Point

F ur n ace T em pera tu re

°C 400

200

600

3 00

2 00

1 00

3 .86 p pm H

900

1 2 : 0 1 1 2 3 4 5 6 7 8 0 /0 1 4 5 2 2 0 .4 m g

1 20 0

0

Soft foam Sof t f oam


5.3 Software For the instructions on operating the PC-software, please, refer to the Help-function of the Software.


5.4 Pre-installation guide The following requirements apply when installing the Analyser Eltra H-500: Carrier gas: Nitrogen 99.99% pure; 2 - 4 bar (30 - 60 psi). Main power supply: 230 VAC ±10%, 50/60 Hz; 20 A fuse. Analyser dimension: 75 x 52 x 60 cm. Analyser weight: ca. 40 Kg The balance should rest on a vibration free support. Connections for nitrogen and compressed air; outer diameter = R¼". (The tubes supplied together with the analyser have a connector with G¼" inner diameter).


Inspection and Quality Certificate We herewith confirm that the ELTRA products manufactured according to the quality and quantity you require. Thanks to a thorough inspection before shipment, the instrument, together with its accessories, the consumption materials and spare parts, are free of manufacturing defects and will provide excellent performance. When treated in a proper way for the required application, according to the specifications from our offer, our order acknowledgement and in accordance with our catalogue specifications, the above products will show good results, and therefore will be used to your entire satisfaction. Y. Polemitis 2005-09-07 Name Date Signature

0.1 0.1 Operation Manual H - 500 · Copyright Ó 2005 by ELTRA GmbH Germany – August 2005 –...

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Transcript of 0.1 0.1 Operation Manual H - 500 · Copyright Ó 2005 by ELTRA GmbH Germany – August 2005 –...