Operation Manual - gut-stuttgart.de · The polymer sample is radiated with infrared light and the...

36
sIRoGran Stationary Infrared-Spectrometer For Granulate Measurement Operation Manual

Transcript of Operation Manual - gut-stuttgart.de · The polymer sample is radiated with infrared light and the...

Page 1: Operation Manual - gut-stuttgart.de · The polymer sample is radiated with infrared light and the reflected light of the measuring spot is transmitted into the spectrometer optics

sIRoGran

Stationary Infrared-Spectrometer For Granulate Measurement

Operation Manual

Page 2: Operation Manual - gut-stuttgart.de · The polymer sample is radiated with infrared light and the reflected light of the measuring spot is transmitted into the spectrometer optics

Manual: sIRoGran - 1 - Copyright by IoSys/G.U.T.

Table of contents

1 Setup of the stationary Infra-Red optic for Granulates- sIRoGran .......................................... 3

1.1 X/Y-table ................................................................................................................................................... 3

1.2 The Measuring Rod ................................................................................................................................. 3

1.3 The Computer with Control and Measurement Electronics ............................................................... 3

1.4 The Spectrometer Optic ......................................................................................................................... 4

2 Hints and Instructions ................................................................................................................ 4

2.1 Warnings and Safety Instructions ......................................................................................................... 4

2.2 Technical Data ......................................................................................................................................... 4

3 Operating instructions ................................................................................................................ 5

3.1 Starting the Manual Operation ............................................................................................................... 5

3.2 Measuring ................................................................................................................................................ 5

3.3 Integrated Mini-Plotter ............................................................................................................................ 6

3.4 Starting the Automatic Operation ......................................................................................................... 7

3.4.1 Adjusting and Recalibrating ............................................................................................................... 7 3.4.2 Using the Micro-Plate with Micro-Plate Mode .................................................................................... 8 3.4.3 Using the Open-Frame with Open-Frame Mode ............................................................................... 9 3.4.4 Using the Open-Frame with Micro-Plate Mode + Result Control .................................................... 10

3.5 New Names, Abbreviations and Functions in the 2013 Software .................................................... 11

3.6 Transporting the sIRoGran Unit .......................................................................................................... 12

4 Enter new Password ................................................................................................................. 12

5 Time and Date Setting .............................................................................................................. 12

6 The sIRoGran-program ............................................................................................................. 12

6.1 Conventions in this Manual ................................................................................................................. 12

6.2 Operating Elements in the Start-Display ............................................................................................ 13

6.3 Operating Elements in the Result-Display ......................................................................................... 14

6.4 Operating Elements in the Teach-In Menu ......................................................................................... 16

6.5 Operating Elements in the Keys-Display ............................................................................................ 17

6.6 Operating Elements in the Step-Motor Mode ..................................................................................... 18

6.6.1 The Micro-Plate Mode ..................................................................................................................... 18 6.6.2 The Open-Frame Mode ................................................................................................................... 19 6.6.3 Step-Motor Operating Elements while Scanning ............................................................................. 20

6.7 New Functions and Hotkeys ................................................................................................................ 21

6.8 Polymer Type Identification by Neuronal Networks .......................................................................... 22

6.8.1 The Min-Pxl statement ..................................................................................................................... 22 6.8.2 Standard Model (All, for coloured, natural or milky-like plastic parts): ............................................ 23 6.8.3 Clear Type Model (clrT, for clear, transparent plastic parts): .......................................................... 23 6.8.4 New Extra Model: ............................................................................................................................ 23

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Manual: sIRoGran - 2 - Copyright by IoSys/G.U.T.

6.8.5 Gray Type Model (gryT, for gray-coloured plastic parts):): .............................................................. 24 6.8.6 Foil Model (Foil, for thin materials): ................................................................................................. 24 6.8.7 DSD Model (for household and packaging plastics):....................................................................... 24 6.8.8 Composition of Styrene-containing Polymers .................................................................................. 25

6.9 Polymer Type Identification by PLS .................................................................................................... 25

6.10 Recalibration of sIRoGran .................................................................................................................... 26

6.11 Operating Elements in the Spc-Mode ................................................................................................. 27

6.11.1 The Main Menu ................................................................................................................................ 27 6.11.2 The Shift Menu................................................................................................................................. 28 6.11.3 The Bottom Menu ............................................................................................................................ 29 6.11.4 Additional Operating Elements ........................................................................................................ 29 6.11.5 Step-Motor Operating Elements in the Spc-Mode ........................................................................... 30

6.11.5.1 The Micro-Plate Mode .............................................................................................................. 30 6.11.5.2 The Open-Frame Mode ............................................................................................................ 31 6.11.5.3 Step-Motor Operating Elements while Scanning...................................................................... 32

7 The System Files for sIRoGran ................................................................................................ 33

7.1 The Initialization File ............................................................................................................................. 33

7.2 The Plate-File ......................................................................................................................................... 33

7.3 The Teach-In File ................................................................................................................................... 34

7.4 The Dat-Files .......................................................................................................................................... 34

8 Data Exchange .......................................................................................................................... 35

8.1 Using PC-Link cable ............................................................................................................................. 35

8.2 Using the USB-Stick ............................................................................................................................. 35

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Manual: sIRoGran - 3 - Copyright by IoSys/G.U.T.

1 Setup of the stationary Infra-Red optic for Granulates- sIRoGran

The device mainly consists of four function groups

X/Y-compound table combined with two linear guides

Measuring rod with Near Infrared light source (NIR)

NIR-spectrometer optic

Computer with control and measurement electronics 1.1 X/Y-table The X/Y-table consists of two linear guides that are connected in a rectangular way by an angle profile. The linear guides have a travel range of max. 150 mm. The individual axes are driven by a stepping motor which is controlled by an stepping-motor interface circuit board. The minimum step width is about 0,15mm. The reference switches accuracy is < 0.1 mm for each linear guides (drive module). 1.2 The Measuring Rod The measuring rod is connected to the housing with a 80 cm long metallic protective hose jacketed in PVC. The measuring head is attached onto the sample and the measurement is triggered by pressing one of the red start buttons. Inside the measuring head a NIR-light-source is integrated. The polymer sample is radiated with infrared light and the reflected light of the measuring spot is transmitted into the spectrometer optics by a fiber optic. The end of the measuring head is protected against contamination with a NIR-filter window. The NIR-light-source is switched on by a relay and turned off when the pressing is stopped. A yellow LED signal indicates that the device is operating. 1.3 The Computer with Control and Measurement Electronics The functional tasks of the computer (PC/104 technology) are to transmit the parameters to the spectrometer electronics and to further process and evaluate the signals received before displaying them on the LCD screen. Direct operating of the software is made possible with an integrated touch panel. The user enters the parameters via the menu-guided sIRoGran software. To ease handling further, the industrial PC supports the simultaneous connection of an external keyboard with a PS/2 plug. A serial interface (9 pole SUB-D plug) and an USB socket is provided for the transmission of data or to connect an external TFT-touchscreen (optional feature).

Start Trigger

Mini-Plotter

TFT-touchscreen

Switch for Mini-Plotter

X/Y-table

Measuring rod

ScanStop-Trigger (aside)

touch pens

four revolving fixation clamps

computer connections

X-linear guide

Y-linear guide

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Manual: sIRoGran - 4 - Copyright by IoSys/G.U.T.

1.4 The Spectrometer Optic The basic principle of the method is the diffuse near infrared reflection spectroscopy whereby characteristic absorption behaviors of different polymer types are used in the NIR wavelength region.

The diffuse near infrared reflected radiation is transported via the optical fiber to the slit of the multi-channel spectrometer to be scattered into its different wavelengths. From the end of the optical fiber the beam of light falls on an imaging diffraction grating. The light reflected by the grating falls on a sensor array. This photo-detector converts the light into electric analog signals. 32 pixels of the optical spectrum are scanned simultaneously, whereby an almost complete overview spectrum in the observed spectral range is recorded.

The signals are read opto-electronically after each scan. The analog signals are digitized on an interface board. The 12 bit digitized data then are transferred to the evaluation computer. To improve the signal/noise (S/N) ratio, the signals are accumulated by the software after each individual scan (runs) and then arithmetically averaged by the number of measuring cycles that has been set to give the spectral representation following. The dynamic range extends from 0 to 4096 arbitrary counts for a scan (12 bit intensity resolution). For a improved scaling the dynamic range is rounded to 4100.

2 Hints and Instructions

2.1 Warnings and Safety Instructions

In order to ensure that the device can operate properly, set it up in a manner so that it cannot slip and will not be subject to vibrations. Do not shake the device!

Ensure that there is an adequate circulation of air for the device. The slits are for ventilation purposes and may not be covered over or otherwise blocked. The openings are designed to ensure that the device can function properly.

Take care that no liquid (water, rain etc) gets into the device or inside the measuring head. This can lead to internal components being damaged or to a short-circuit.

To avoid short-cuts, do not use the device near water or in moist ambient surroundings.

Ensure that the protective hose of the measuring rod is not subjected to stress when being coiled up for transportation (damage of the fiber optic). Clamp the hose into the clip mounted on the sIRoGran device.

This measuring device consists of sensitive electronic components. Use not in accordance with the instruction may result in their destructions. Electrostatic discharges, induces voltage peaks and balance currents between different voltage potential are particularly harmful.

Ensure that the movement of the measuring rod fixed in the clips on the carriage is no way blocked or obstructed.

2.2 Technical Data Rated voltage: 100-240 VAC (external AC power supply) Rated current: 2.5 A max.

Protection class: Type of protection: IP 20 Dimensions (WxHxD): 480 x 290 x 390 mm (with XY-table) Weight: 8 kg Ambient temperature: 15...35°C Max. relative air humidity: Operating: 10%...90%

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Manual: sIRoGran - 5 - Copyright by IoSys/G.U.T.

3 Operating instructions

3.1 Starting the Manual Operation 1. Check the protection window at the rod measuring head and clean it with a soft tissue in case it is dirty. Do not scratch the protection window. 2. Power on the device at the main power switch. The device starts booting and loads the main program for the plastic identification. At first the sIRoGran starts with the message: First do Recalibration then the readiness of the device is signaled with the message: sIRoGran.

3. At first, recalibrate the system by pressing the <F4> key (for PS/2-keyboard) or <CAL> icon (for touchscreen), resp.. Then attach the measuring rod against the white ceramic plate and keep pressing the one of the both triggers until the last message Stop triggering! appears. It signals the end of the recalibration procedure. If an error message appears, repeat the recalibration (see: Recalibration of sIRoGran). For the recalibration either the

reference mounted on the housing or the small ceramic plate for the finger or the big tile can be used.

3.2 Measuring 1. Activate the restriction of the plastic identification to polymer types (All-,

gryT-, clrT-, DSD- or Foil functions) either to the most probable ones due to colour (All, gray Type) or property (Foil, clear Type) or origins (DSD) which appears most plausibly due their polymer similarity. The activation of these functions are signaled in red in the Result display.

2. Press the measuring head against the surface of the sample part. The surface should be smooth and as clean as possible. If not, scratch the surface with the knife to obtain a fresh new material surface. 3. Trigger the start button and keep it pressed until the yellow LED-signal turns off (ca. 1 sec.). During this time a NIR-light-source inside the measuring head is switched on by a relay, the measurement is started and the identification result is displayed until the next measurement is triggered (Single mode). In the Circular-Mode1 the NIR-light-source is continuously powered on while pressing the rod trigger and the display shows the identification results after each measurements. Either the pre-set limit values have not been exceeded (e.g. 1st place less than 70 %, 2nd place greater than 30 % probability) or the minimum of the NetD curve is not in the range of the pre-set Min-/Max-Pixel values. In both cases repeat the measurement until a reliable statement appears. If repeated measurements still are producing this message, the sample might be unknown (not calibrated, see: Polymer Type Identification by Neuronal Networks) or the wrong identification net model was selected for identification or new recalibration is necessary.

1 The Circular Mode is recommended when inhomogeneous small or thin samples (e.g. milled samples, granulates, foils) should be analyzed or polymer identification results seems to be not stable.

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Manual: sIRoGran - 6 - Copyright by IoSys/G.U.T.

4. If the measured light intensity level is low than the message shown is displayed. The Low NIR-Intensity message appears if the measured NIR-light intensity does not exceed the pre-set threshold value for the minimum light intensity (see: The Initialization File). Reasons may be that the sample is too dark2 for the reflection principle or the plastic part is a kind of a diffuse scattering material and thus unsuitable3 for the diffuse near infrared reflection measuring method.

5. For foils and transparent materials a ceramic plate - acting like a mirror -

must be placed behind the parts to reflect back the NIR light into the measuring head for data evaluation. This handling also applies for most of the polymer types which comes up naturally coloured - or milky-like. In general for the identification of transparent thin materials the Foil model should be activated. Due to the variable thickness of foils the absorption characteristic differs in comparison to solid materials. The typical minimum of the measured NIR curve (Min-Pixel) is usually different to solid materials. Thin foils should be folded several times thus a thickness at least 50-100 µm is achieved otherwise the result might not be reliable. Plastic parts thicker than 500 µm should be measured with the Standard or clear Type model.

6. The status of the system should be checked regularly by measuring the reference ceramic plate! If the

message: Changed Condition! Do new Recalibration appears then a new recalibration should be carried out again (see: Adjusting and Recalibrating). The system is heated up causing a sensitivity gain drift of the electronics.

If either incorrect identification results are indicated with known samples or the system condition has been changed after the last recalibration like dis-/connecting an external keyboard or switching on/off the Mini-Plotter a new recalibration is always necessary to ensure the stability of the electronic environment!

3.3 Integrated Mini-Plotter The outside of the paper roll is the side to print on. Use only paper rolls which are coated on the outside with a width of 57.5 mm and a winding diameter of 31 mm. To insert the paper please proceed as following: 1. Open the printer cover by slightly lifting the lever upwards. 2. The paper roll is lifted from the mechanism together with the cover. 3. Unwind a little bit of the paper roll and insert the paper roll in the paper storage. 4. Close the cover by applying sufficient pressure until a clear snap shot can be heart. 5. After printing the paper can be simply ripped off at the tear bar.

2 In general, no dark coloured and black samples or materials filled with soot (carbon-black) can be analyzed using the NIR-technology. Soot absorbs the NIR radiation thus almost no diffuse reflection occurs. 3 Low NIR-light reflection is observed by natural coloured or milky-like Polyamides and Polyolefines (NIR-light scattering). Furthermore it must be stated due to our experience that gray coloured plastics (e.g. PP, PVC) which are containing lot of Talcum (20-40%) as a filling material reduces the NIR light reflection causing non reliable identification results.

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Manual: sIRoGran - 7 - Copyright by IoSys/G.U.T.

3.4 Starting the Automatic Operation 3.4.1 Adjusting and Recalibrating 1. After powering on the device, switch to the Result-Display by pressing

the <F8> key or <NetD> icon, resp.. Then press the <T> key or <SMtr> icon to activate the Step-Motor Mode, resp..

2. Place the clean white ceramic reference reflection plate to its position on the right side on the top of the sIRoGran device. Depending on the application, put either the Open-Frame or the Micro-Plate on top of the ceramic plate and fix them with the four revolving fixation clamps.

3. Carefully fix the measuring rod in the two black clamps mounted at the linear guide carriages. (Do not stress/bend the gray conduit cable and the clamps). In order to avoid the slipping down of the metallic measuring rod within the black clamps, counter/fix the measuring rod with the two rubber O-ring on top of each black clip. 4. Adjust the height of the measuring head (0.5 – 5 mm approx. over the frames) , thus the rod should move comfortably over the Open-Frame or

Micro-Plate not touching also the filled-in samples during the scanning movements.

Do not make the distance larger than necessary, because recalibration procedure might fail due to too low reflected NIR-light intensity. Furthermore the measuring focus may become too large and thus small particles may not be measured!

5. Then recalibrate the system by

pressing the <F4> key or <CAL> icon, resp.. If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod first drives to this position. Longer time pressing of one of both triggers

interrupts the recalibration procedure If an error message appears, repeat the recalibration (see: Recalibration of sIRoGran).

Be aware that the given recalibration place is always empty!

!

!

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Manual: sIRoGran - 8 - Copyright by IoSys/G.U.T.

3.4.2 Using the Micro-Plate with Micro-Plate Mode 1. Select Micro-Plate-Mode by pressing the <F> key or <Frm-Plt> icon

on the touchscreen. The Plate-activation (Plt) is signaled in RED and chessboard-like display is coming up.

2. Using the Micro-Plate fill-in the granulates/pellets/ground materials so

that in almost every of the 625 holes of the Micro-Plate only one particle of similar size is located (except Pos1, A/1, which must be empty for recalibration). Multiple filling with different materials might lead to non-reliable or wrong identification results! Empty holes can be neglected. They will not be evaluated by the statistic software.

They will be marked in white as empty (-). For a better overview four different polymer types can be marked in different colours. This can be done in the Set-Menu by pressing the <F3> key or <Set> icon, resp..

3. First the mechanical reference alignment (X=0, Y=0) of the X/Y-table

should be done by executing the <F5> key or <0/0> icon, resp.. From time to time the re-alignment is advisable. The correct positioning of the measuring head to the Micro-Plate can be checked by using the <F6> / <F7> keys or <Pos1> / <Pos2> icon, resp., because the measuring rod then drives to these respective positions.

4. The scan4 of the Micro-Plate starts by pressing the <F2> key or

<Scan> icon, resp.. The fixed measuring rod at the X/Y-table drives to the position: A/1 and moves step by step (625x) to position: Y/25. Repeated pressing <F2> or <Scan> interrupts the scan and starts again from the beginning and resets all statistic values.

5. The result abbreviation -L- means “LowLight”. The intensity of the diffuse reflected Near Infrared Light (NIR) is less then 5%. Samples might be too dark for measurement. The result abbreviation -H- means High for a “Light OverFlow” signal. The NIR-intensity is higher than the pre-set value for the light intensity range5 (see: The Plate-File). Samples might be too bright/light for measurement or a new recalibration is necessary. 6. The results of the Micro-Plate scan are displayed on chessboard-like screen with each identified plastics shown at their respective positions as well as the non-identifications (---) and empty holes (-). To control individual results, the X/Y-

function can be used by pressing the <F8> key or <X/Y> icon, resp.. The sensor moves to the selected position (see: Using the Open-Frame with Micro-Plate Mode ).

7. A single measurement can be carried out by using one of both triggers6 or pressing the <Space> key or

<Scan> icon, resp.. The NIR-light is automatically switched on and off for the measurement. Be sure that the NIR-light source in the measuring rod is not working unnecessarily (indicated by the yellow LED). If it is accidentally shining, it can be stopped by pressing the metallic main trigger or by quitting the Step-Motor Mode via the <T> key or <Quit> icon, resp..

Any drive errors of the linear guide carriages can be stopped by longer pressing of the main trigger on the left side of the sIRoGran unit until the movement stops and the message: Scan stopped appears.

4 Default scan amount for Micro-Plate-Mode: 1000. The higher the scan number (Runs), the better the resulting average, the more stable is the identification result. However, the measuring time takes longer. On the other hand, the smaller the scan number (1..5000), the more noisy the resulting spectra for evaluation, the less stable is the identification result. On the other hand the measuring time takes shorter. 5 Light Overflow -H- is displayed if the NIR-spectrum of the measurement (in Cts, NirD-view) is higher than the intensities of the actual stored reference spectrum plus the pre-set light level (e.g. 200 Cts). 6 the red trigger on the measuring rod or the metallic ScanStop-trigger at the display housing aside

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Manual: sIRoGran - 9 - Copyright by IoSys/G.U.T.

3.4.3 Using the Open-Frame with Open-Frame Mode 1. Select Open-Frame-Mode by pressing the <F> key or <Frm-Plt>

icon on the touchscreen. The Frame-activation (Frm) is signaled in RED.

2. Using the Open-Frame distribute/fill-in the particles almost in a

single-layer arrangement. Take care that no particles are blocking the free movement of the measuring rod and the placement of the ceramic reference plate. Sweep away any obstructing particles before by using e.g. a brush. The automatic operation mode mainly refers to the surface area of the material, not necessarily to the weight/mass. For best results it is strictly recommended to measure particles of similar thickness, because the used NIR-reflection

technique can measure only the surface percentages, not the masses of the given particles. The step width can be altered as well as the size of the measuring square area.7 within the Set-Menu by pressing the <F3> key or <Set> icon, resp..

3. The positioning of the square measuring area8 of the Open-Frame Mode can be checked by using the <Strt> and <End> icon or <F6> or <F7> keys. The measuring rod then drives to these respective positions. The step width to be chosen (1..10) in the Open-Frame mode within in the Set-Menu should be selected according to the size of the granulates/pellets/ground material. Smaller particles require preferably lower values, bigger particles can be measured with a greater step width to reduce the overall measuring time. The relation between scan time and step width should be evaluated individually depending on the samples under investigation.

4. The scan9 of the Open-Frame starts by pressing the <F2> key or <Scan> icon, resp.. The fixed measuring rod at the X/Y-table drives to the Start-position10 and moves step by step (depending on the pre-set step width) to the calculated End-position. 5. In the Open-Frame mode two times the same identification result must be evaluated successively before it is be counted avoiding interleaving position states. Therefore counting non-reliable results while crossing two pellets/granulates/ ground material is almost avoided. In the Micro-Plate mode each identification result is counted,

because it is required that there must be only one particle in the hole. The non-identified results (---) statistically either can be counted or suppressed by pressing the <N> key or <NoCount> icon, resp.. thus neglecting e.g. the dark-coloured/black materials in the statistic.

6. The end-results of the measuring in both modes can be printed11 by pressing the

<P> key or <Plot> icon, resp.. The intermediate-results while scanning can be printed by pressing the <F7> key or <Plot> icon, resp..

Be sure that the NIR-light source in the measuring rod is not working unnecessarily (indicated by the yellow LED). If it is accidentally shining, it can be stopped by pressing the metallic main trigger or by quitting the Step-Motor Mode with the <T> key or <Quit> icon, resp.

7 The square measuring area is defined around the center of the white ceramic plate which equals the mid position: M/13 in the Micro-Plate. The length of each side is defined in Millimeters (5..150) 8 Start-Position is defined as left-top and End-Position as right-bottom edge. 9 Default scan amount for Open-Frame-Mode: 100 10 If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position. 11 Be sure that the rocker switch of the Mini-Plotter is turned on before. The Mini-Plotter uses the same COM-interface of the computer. If COM should be used for other operations (e.g. data link) then the Mini-Plotter must be switched off.

!

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Manual: sIRoGran - 10 - Copyright by IoSys/G.U.T.

3.4.4 Using the Open-Frame with Micro-Plate Mode + Result Control 1. Select Micro-Plate-Mode by pressing the <F> key or <Frm-Plt> icon

on the touchscreen. The Plate-activation (Plt) is signaled in RED. 2. Using the Open-Frame fill-in the particles almost in a single-layer

arrangement. The automatic operation mode mainly refers to the surface area of the material, not necessarily to the weight/mass12.

Take care that no particles are blocking the free movement of the measuring rod and the placement of the ceramic reference plate and that the given recalibration place (A/1) for the Micro-Plate operation is always empty!!

3. The mechanical reference alignment (X=0, Y=0) of the X/Y-table first

should be done by executing the <F5> key or <0/0> icon, resp.. From time to time the re-alignment to 0/0-Reference position is advisable.

It is strictly recommended before starting a new Micro-Plate scan, always an actual recalibration should be carried out.

4. The scan13 of the Micro-Plate starts by pressing the <F2> key or

<Scan> icon, resp.. The fixed measuring rod at the X/Y-table drives to the position: A/1 and moves step by step (625x) to position: Y/25. Repeated pressing <F2> or <Scan> interrupts the scan and starts again from the beginning and resets all statistic values.

5. The results of the Micro-Plate-Mode measuring are displayed on chessboard-like screen with each identified

plastics shown at their respective positions as well as the non-identifications (---) and empty holes (-).The result abbreviation14 -L- means “LowLight”, -H- means High for a “Light OverFlow” signal.

6. If the actual identification model will be changed (e.g. from Standard/All to DSD) during the automatic scan

then all previous identification results will be deleted and resets all statistic values. 7. To check individual results, the X/Y-function can be used. If keyboard operation <F8> is carried out then the measuring rod goes to the pre-set position which can be defined in the Set-Menu before by using the <F1> or <F2> key/icon. If <X/Y>-icon is pressed via touchscreen then the background of the chessboard-like screen comes up in dashed dark gray. It indicates the activation of the X/Y-field selection. Using now the touch-pen and touching one of the 625 fields then this specific area is shortly marked and the measuring rod moves to this selected position. 8. A single measurement can be

carried out by using one of the triggers or pressing the <Scan> icon, resp.. The NIR-light is automatically switched on and off for the measurement and the result is displayed until the mid area of the touchscreen is slightly pressed again.

9. The end-results of the automatic operation can be printed15 by pressing the <P>

key or <Plot> icon, resp..

Any drive errors of the linear guides can be stopped by longer pressing of the main trigger on the left side of the sIRoGran unit until the movement stops and the message: Scan stopped appears.

12 For best results it is strictly recommended to measure particles of similar thickness, because the used NIR-reflection technology can measure only the surface percentages, not the masses of the given particles. 13 Default scan amount for Open-Frame with Micro-Plate-Mode: 2000. The higher the scan number (Runs), the better the resulting average, the more stable is the identification result. However, the measuring time takes longer. On the other hand, the smaller the scan number the more noisy the resulting spectra for evaluation, the less stable is the identification result., but the measuring time takes shorter. 14 The result “LowLight -L- means the intensity of the diffuse reflected Near Infrared Light (NIR) is less then 5%. Samples might be too dark for measurement. Light OverFlow” –H- signal means that the NIR-intensity is higher than the pre-set value for the light intensity range. 15 Be sure that the rocker switch of the Mini-Plotter is turned on before.

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Manual: sIRoGran - 11 - Copyright by IoSys/G.U.T.

10. When checking the result with the X/Y function there may sometimes occur a different result from the moving mode due to a higher precision of a static measurement (if the parts on the plate have not shifted in the meantime due to the sledge vibrations when moving). There may be e.g. the following result picture (see below left) and on controlling one of these positions there may be the picture below right:

11. You now can choose one of the 4 options by pressing the touchscreen or one of the keys at the

keyboard: NO or <N>: The result of the automatic measuring will be kept --- or <U>: The result will be changed to „unknown“, e.g. with very distorted or “noisy” signals XXX or <X>: The result will not be counted at all. YES or <Y>: The control result will be accepted and will overwrite the original result After a new complete recalculation – made audible by an increasing buzzing tone - the new result will be shown on the screen. 3.5 New Names, Abbreviations and Functions in the 2013 Software New Abbreviations of Polymers in the MicroPlate Display: Within the MicroPlate Mode the polymer abbreviations have been shortened to 3 letters for better visibility: PMMA -> PMA APVC -> APV PA12 -> P12 PA6x -> P6x PCPT -> PCP Styr -> Sty During a MicroPlate-Scan you can change the different detection models in the Standard- and in the Spectra mode. Therefore new Hotkeys are used (always small characters on the keyboard). A -> All / Standard-T C -> clrT D -> DSD E -> Extr G -> gryT S -> Sty4 O -> Overlay M -> Modify P -> PLS-Algorithm Cursor left -> Scan Numbers down during a MicroPlate Scan Cursor right-> Scan Numbers up during a MicroPlate Scan

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Manual: sIRoGran - 12 - Copyright by IoSys/G.U.T.

3.6 Transporting the sIRoGran Unit For transporting the sIRoGran unit the measuring rod should be fixed in the transporting clamps and the X/Y-table should be move to its left-top starting positions like shown in the picture.

Ensure that the gray conduit cable with the NIR-fiber optics and the Y-linear guide are not subjected to any stress .

4 Enter new Password

The system is secured with a password which activates the mIRo-program. In case the message: Program deactivated!… is displayed, please contact [email protected] to obtain the actual password for the device.

To edit once the new password please proceed as following:

1. Connect an external keyboard (PS/2) and a VGA screen to the system. 2. Edit on the DOS-prompt level of the given sub-directory the command line edit ini.dat 3. Replace the 8 stars (*) in the first line of the ini.dat with the new password (8 small

characters!). 4. Save the ini.dat file (ALT+F(ile), ALT+S(ave)) and close the Text-editor (ALT+X(exit)). 5. Edit on the DOS-prompt level miro.exe to start the program.

5 Time and Date Setting

To enter a new Time and/or Date for example for correct Mini-Plotter printouts please do as follows: 1. Connect an external keyboard to the system. 2. Enter on the DOS-prompt level of the given sub-directory the command time or date, resp.. 3. Edit new date or time values and confirm/quit with <ENTER>.

6 The sIRoGran-program

6.1 Conventions in this Manual The device is designed in such a way that it can be operated from the touchscreen and/or from an external keyboard. In general a keyboard permits the menu-guided software to be handled more easily. The following paragraph gives the writing conventions used in these operating instructions: Operations to be carried out via touchscreen are given with the legend on the respective touch field and the word <Icon>. Those to be carried out with the external keyboard with the legend of the keyboard key and the word <Key>. In general only small characters of the keyboard are to be used! A touch field on the display only has to be touched briefly. If a number of keys or, as the case may be, touch fields have to be pressed simultaneously, then this is indicated with a plus sign (+) between the individual key or touch field legends, e.g. <SHIFT>+<F1>. Pressing a key or touching an icon activates or deactivates a mode or function. In general a repeated pressing the same key or touching the same icon again deactivates/activates the operation, respectively.

Unexpected malfunctions of the touchscreen can be stopped by powering on and off the unit again!

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6.2 Operating Elements in the Start-Display

Icon Key Function

Spec F1 Switches to Spc-Mode to view the NIR-Spectra or the transformed Net-Data and to carry out further actions (see: Operating Elements in the Spc-Mode).

Runs F2 Increases (<F2>) or decreases (<F3>) the number of runs16 (scan numbers) to form an average mean spectrum for evaluation.

Cal F4 Starts the routine for the recalibration measurement with the ceramic reference plate (see: Recalibration of sIRoGran).

Keys F5 Displays the assignment of the touchscreen fields and opens further menu options for testing, setting and editing systems files for the sIRoGran (see: Operating Elements in the Keys-Display).

Mode F6 Switching between the Single-Mode and the Circular-Mode. In the Single-Mode the NIR-light-source inside the measuring head is switched on by a relay, the measurement is started and the identification result is displayed until the next measurement is triggered. In the Circular-Mode the NIR-light-source is continuously powered on while pressing the rod trigger and the display shows the identification results after each measurement cycle.

PLS F7 Changes to the PLS model (Partial-Least-Square), where plastic identification is performed using selected Teach-In samples (see: Operating Elements in the Teach-In Menu). The activation of the PLS mode is displayed on the top and the ranking list appears now in blue letters and the icons to select the identification model are disappearing (no function). Pressing again the <PLS> icon switches back to the Neuronal network calculation and the hit list is displayed in red letters.

NetD F8 Switches to the Result-Display. In the NetD (Network Data) mathematically transformed and auto scaled data are displayed. These data are used by neuronal network or PLS processing for plastic identification. On the right bottom side of the screen the Pixel number of the curve minimum is displayed in red letters. The position of the curve minimum (e.g. 12, 15, 20 etc.) is typical17 for a polymer type. On the left side the measured NIR-intensity18 is shown in percentage range. If this intensity level is less then the pre-set limit value for minimum light intensity (e.g. 5%) than the message Low NIR-intensity is shown19.

QUIT ESC Leaves the program and returns back to the DOS prompt level.

16 The higher the scan number (Runs), the better the resulting average spectra (improved signal/noise ratio of the calculated mean), the more stable is the identification result. However, the measuring time takes longer. On the other hand, the smaller the scan number (1..5000), the more noisy the resulting spectra for evaluation, the less stable is the identification result. On the other hand the measuring time takes shorter. 17 Depending on the spectrometer system. 18 The measured NIR intensity is the difference of the left intensity (Pixel number 1) to the right value (Pixel number 32) in %. 19 It means that the diffuse reflected light intensity of the sample is too weak to identify the sample reliably. The pre-set limit value for the minimum light intensity has not been exceeded. This threshold value can be altered in the Ini.net file.

Status window

Main window

Main menu bar

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6.3 Operating Elements in the Result-Display Icon Key Function

USB-Edit Enter Opens the menu to edit the main file name (max. 4 characters) for the automatic spectra saving onto an external USB-stick storage device.

USB-Save BS Activates the automatic USB-saving function (<Backspace>). Spectra are saved with consequent numbers up to –999 behind the main series file name20 in the pre-set subdirectory path of the USB-storage device (see: The Initialization File). Repeated touch deactivates the function.

Plot P Printing out the result as a screen dump by a Mini-Plotter. The rocker switch located at the integrated the plotter must be turned on. Touching the touchscreen or pressing any key on the keyboard stops the actual plotting process.

TeachIn F10 Opens the TeachIn-Menu to teach-in or to select known samples (see: Operating Elements in the Teach-In Menu) for polymer identification using the PLS algorithm. (Partial-Least-Square, “best fitting curve”). The PLS mode is automatically activated and the hit list (ranking) is displayed in blue letters. The advantage of the PLS method is that the user can teach-in own test samples to carry out simple a rapid analysis. The disadvantage is that PLS works for NIR-spectra only which obviously have big spectral differences. Pressing the <PLS> icon brings the display back to the neuronal network calculation (see: Polymer Type Identification by PLS)

Scan TAB Starts a scan without pressing the trigger21. SMtr T Starts and stops the Step-Motor Mode for

scanning granulates, pellets or ground materials. During the Step-Motor operation this mode can also be stopped by pressing the <Quit> touch icon or <Enter> key, resp. (see: ). Be aware that if the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position when starting any movement (see: Operating Elements in the Step-Motor Mode).

In case of any linear guide drive error, press the metallic main trigger on the left side of the unit as long until the movement stops. Unexpected malfunctions of the touchscreen can be stopped by powering on and off the unit again!

20 e.g. main series file name test-1 up to test-999. 21 The NIR-light source is switched on automatically (indicated by the yellow LED at the TFT-touchscreen) in the Step-Motor Mode only, not in the manual operation. For measurement with NIR-light one of both triggers must be pressed.

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Teach-In Menu to save/select own samples for PLS-method

Pixel Number of the curve minimum

Activation of automatic. spectra saving to USB

Displaying amount of NIR-light Overflow measurements

Printing out the result display to a Mini-Plotter

Hit list (ranking) of identification probabilities

Measured NIR-light intensity level

Select identification model

Activation of the Step-Motor function

USB-main series name

Polymer type identified

Editor for USB-file name Scanning without pressing the trigger

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Mdfy M Due to spectra similarity the distinction of some polymer types is sometimes uncertain and could be random-like. To modify the identification result means that the determined probability in the network model (1st ranking in the Hit list) is altered to the main polymer group. The identification will be simplified like

(ABS, PS, PPO Styr). The Modify function can just be activated/deactivated if one of the mentioned polymer types is displayed. A temporary modification of an identification result is then signaled in red.

gryT G This identification model is recommended when gray-coloured plastic parts coming from the electro- and electronic dissembling area (e.g. computer waste) are to be detected, because the amount of polymer types for fine differentiation of the styrene-containing sub-group within this model is extended and other types are neglected to enhance the identification performance. Modified results Modified results (Mdfy) switches

ABS, PS and PPO Styr and PCA, PCPT PC. In this gray-Type model the identification of PA, PP, Styr (ABS, PS, PPO), PC (PCA, PCPT), APVC and PVC is calibrated.

Extra E The Update has the new Extra-Modell (Extr) with a larger polymer variety, to be used as screening

model. Her are plastics from the Standard Model (no PCPT), Foil Model (no PEPA, PPPT and PEPT), Gray Type Model (no PCPT) and Clear type model. PA, PO (PP, PE), Styr (ABS, PS, SAN, PPO), PES (PBT, PET), PC (PCA, PC), PMMA, POM and PVC. PA combines PA6x und PA12. PLA is not included here, but POM.

Foil F This identification model is recommended when thin materials like foils are to be detected. The thin

foils should be folded several times to achieve a thickness of at least 50 - 100 µm, otherwise the result might not be reliable. Materials which are thicker than 500 µm should be measured using the

Standard model (All). Modified results (Mdfy) switches PEPA or PEPT PE and PPPT PP. Identification of PA, PP (PPPT), PE (PEPA, PEPT), PS, PET, PVC, PLA and CLLS foils.

clrT C Restriction of the polymer identification to few clear types which can normally occur also or only as clear, transparent plastic parts (thickness: 0.5 - 6 mm). This identification model is recommended, because the amount of polymer types for fine differentiation of the styrene-containing sub-group is extended within this model and other types are neglected to enhance the identification performance. Modified results (Mdfy) switches

ABS, SAN (AS) and PS Styr. Identification of PO, Styr (ABS, PS, SAN), PET, PC, PMMA and PVC.

DSD D This identification model is recommended when typical plastic parts and foils22 coming from the household and packing area (MWS) are to be detected, because the amount of polymer types is restricted to five polymer types which normally occur as household and packaging plastics (DSD = Duales System Deutschland, Green Dot). Modified results (Mdfy)

switches PP, PE PO. In this DSD-model the identification of PP, PE, PS, PET and PVC is calibrated only.

./. A This Standard identification23 model (no special model activated in red) is recommended when coloured, natural- or milky-like plastic parts (not gray, not black and not transparent) are to be detected. Herein the amount of polymer types for fine differentiation of the styrene-containing sub-group is reduced.

Modified results (Mdfy) switches PA6x, PA12 PA and

PP, PE PO and ABS, PS Styr and PBT, PET PES and

PCA, PCPT PC. Identification of PA24 (PA6x, PA12), PO (PP, PE), Styr (ABS, PS), PES (PBT, PET), PC (PCA, PC, PCPT), PMMA, POM and PVC.

22 No PA-, PEPT- and PLA foils are calibrated and due to the spectra similarity the multilayer foil PEPA was taught in as PE. 23 IoSys uses the following abbreviations: PA=Polyamide, PO=Polyolefine, Styr=Styrene containing polymers, PES=Polyester, PCA=PC+ABS, PCPT=PC+PBT or PC+PET, APVC=ABS+PVC, PLA=Polylactoseacetate-biodegradable, CLLS= Cellulose; Multilayers: PEPA=PE+PA, PEPT=PE+PET, PPPT=PP+PET. 24 Fine differentiation of PA6 and PA66 polymer types is not reliable. Therefore both types are calibrated and combined to PA6x.

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Sample icons (8) to teach-in (save) the spectra or to select

Increasing or decreasing the threshold value for the minimum Hit-Quality for the 1. Ranking in the hit list

Increasing or decreasing the threshold value for the minimum Hit-Difference from the 1. to 2. ranking in the hit list

Keyboard assignment

6.4 Operating Elements in the Teach-In Menu Touch Key Function

1..8 F1..F8 By pressing one of the eight sample icons the actual spectrum will be stored as a Teach-In sample. A gray coloured touch icon indicates that in respective slot no spectrum was stored before or it was deactivated (see <Slct>). The PLS mode must be activated to use the Teach-In spectra for polymer type identification (see: Operating Elements in the Start-Display).

Up 1 Increases the threshold value of the minimum Hit-Quality for the 1st ranking in the hit list25. If the 1st ranking percentage is less than the pre-set Hit-Quality value then the message Low Hit-Quality is shown.

Dwn 3 Decreases (Down) the threshold value of the minimum Hit-Quality for the 1st ranking in the hit list.

Slct 4 Switch to the Select-Bar for activation/deactivation of respective Teach-In samples for the PLS-algorithm (dotted pattern style appears and the <Slct> icon changes to the <Clr> icon). Deactivated or not available storing places are shown in gray letters Pressing the <Clr> icon deletes all stored Teach-In samples (Clear) and renames the referring sample to numbers 1 to 8. Repeated touch of the <Clr> icon confirms the deletion process.

Edit 5 Switch to Edit-Menu for editing of the names of given plastic types. The function is only active if a sample icon has been selected before. Other names with max. 4 characters can be edited by opening the Teach-In File (see: The System Files for sIRoGran).

Up 6 Increases the threshold value for the minimum Hit-Difference from the 1st to the 2nd ranking in the hit list. If percentage difference26 from the 1st to the 2nd ranking is less than the pre-set Hit-Difference then the message Low Hit-Difference is shown.

Dwn 8 Decreases (Down) the threshold value for the minimum Hit-Difference from the 1st to the 2nd ranking in the hit list.

ESC ESC Leaves the Teach-In Menu and returns back to the Result-Window. All settings are automatically saved in the system file Teach-XX.dat which will be loaded when starting the system (see: The Teach-In File).

6.5

25 The Hit-Quality is the first threshold value, which the actual spectrum must exceed (degree of spectral curve similarity in % to the trained-in and stored Teach-In samples) to be indicated. For example: the NetD curve resembles to the Teach-in sample named PE to 91% and to the PP to 41%. If the pre-set Hit-Quality value for the 1st ranking is set higher than 91% (in this example) then the message Low Hit Quality is shown. 26 The Hit-Difference is the difference-threshold value, which must be exceeded (spectra difference of 1. to 2. ranking expressed as percentage ranges). For example: the NetD curve resembles to the Teach-in sample named PVC to 100 and to the PE to 98%. If the pre-set Hit-Difference value for the 1st to the 2nd ranking is set higher than 2% (in this example 100%-98% = 2% Hit-D) then the message Low Hit Difference is shown.

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6.5 Operating Elements in the Keys-Display Icon Key Function27

PlateIni F2 Starts the text editor with automatically loading the initialization file plate-XX.dat or editing the Step-Motor initial X/Y-position data28 (see: The Plate-File).

PC-Link F3 Starts the PC-Link program (intersvr.exe) to enables data exchanges for updates or copying files to another computer (see: Data Exchange).

mIRoNet F6 Opens a further window with a menu bar to select neuronal network calibration files and system files. Pressing an icon/key starts the editor with automatically loading the selected Dat- or Ini-Files (see: The Dat-Files).

mIRoIni F7 Starts the text editor with automatically loading the initialization file ini.dat for the sIRoGran to change e.g. pre-set password or subdirectory path for saving and loading spectra files (see: The Initialization File).

TeachIn F8 Starts the text editor with automatically loading the initialization file teach-XX.dat for the sIRoGran to edit sample names and pre-set threshold values (see: The Teach-In File).

QUIT ESC Leaves the Keys-Display and returns back to the Start-Display.

Do not make any changes to the formatting in the text files. Do not insert a decimal point with integer numbers.

27 To operate the text editor an external keyboard should be connected. In general – if not otherwise noted - quitting the editor resets the loaded text file therefore modifications are directly taken over. 28 In case the linear guides do not find the Position: A1 correctly, please check if the correct values (e.g. 10/10 or 10/15 or 15/10) are set in the first line. It might occur that the original values might be deleted accidentally.

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6.6 Operating Elements in the Step-Motor Mode 6.6.1 The Micro-Plate Mode Icon Key Function

<= F1 Switches to Spc-Mode and back to view the transformed Net-Data or NIR-spectra during the Step-Motor procedure.

Scan F2 Starts the Micro-Plate scan. The fixed measuring rod at the X/Y-table drives to the Start-position: A129 and moves step by step (625x) to the End-position: Y/25. Repeated pressing <F2> interrupts the scan and starts again from the beginning and resets all statistic values.

Set F3 Switches to the Set-Mode to set X/Y-positions and colours for polymer types and to select the identification model for the step-motor operation. Using <F1> and <F2>, the Y- and X-axis position (A..Y, 1..25) for the X/Y-function can be set. Pressing <F3>..<F6> four polymer types can be selected for coloured30 marking. 40 code numbers are listed for given polymer types. <F7>switches to a subpage for defining the non-measured polymers and the “ground noise elimination” mode, see p. 21.

CAL F4 Starts the automatic routine for the recalibration measurement. The step-motor drives to the preset position-1 for the Micro-Plate recalibration.

0/0 F5 The Step-Motor (or <Ins> key) drives both carriages of the linear guides to the upper left reference position to initialize its 0/0-position (X=0, Y=0).

Pos1 F6 Drives to the position: A/1 of the Micro-Plate (or <Home> key) While scanning, this function is deactivated.

Pos2 F7 Drives to the position: Y/25 of the Micro-Plate (or <End> key). While scanning, this function is deactivated.

X/Y F8 Goes to the preset X/Y-position. While scanning, this function is deactivated. If keyboard operation <F8> (or <Del> key) is done then the measuring rod goes to the pre-set position which can be defined in the Set-Menu before or with the touchpen. If <X/Y>-icon is pressed via touchscreen then the background of the chessboard-like screen comes up in dashed dark gray. Using now the touch-pen and touching one of the 625 fields then this specific area is shortly marked and the measuring rod goes to this selected position (see: Using the Open-Frame with Micro-Plate Mode ).

Quit Enter Quits Step-Motor Mode31 back to the sIRoGran Start-Display. Frm-Plt F Selects (<F> key) the Open-Frame- (Frm or Plt in red) or Micro-Plate operation for the Step-

Motor Mode. While scanning, this function is deactivated. Plot P Printing out the scanning result by a Mini-Plotter. The rocker switch located closed to the

integrated plotter must be turned on. NoCount N Suppresses the Non-identification results (---) in

the counter list and in the statistical percentage.

29 If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position. 30 Non-identifications (---) are marked in green and empty places (-)are displayed in white. Places are measured as “non-empty” if a NIR-light attenuation of more than e.g. 200 Cts. (see: The Plate-File) had occurred compared to the actual reference spectrum. Besides, “Lowlight“- and “Overflow”-signals are not counted, too. 31 When the Step-Motor Mode is activated again then the last scanning result is displayed again until a new scan is started.

Quit Stepping-Motor mode back to the Start window

Scaling of Micro-Plate X-axis Listing of identified

polymer types with statistic statements

Selecting Open-Frame or Micro-Plate application

Scaling of Micro-Plate Y-axis

Printing out the result to the Mini-Plotter

No counting of Non-identification results

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6.6.2 The Open-Frame Mode Icon Key Function

<= F1 Switches to Spc-Mode and back to view the transformed Net-Data or NIR-Spectra during the Step-Motor procedure (see: Operating Elements in the Spc-Mode).

Scan F2 Starts the Open-Frame scan. The fixed measuring rod at the X/Y-table drives to the Start-position32 and moves step by step (depending on the step width) to the End-position.

Set F3 Switches to the Set-Mode to set positions and sizes and to select the identification model for the Open-Frame operation. Using <F1> and <F2> the Recal-Y- and Recal-X-positions for the recalibration position can be set. With <F3> and <F4> the measuring size for the frame (square size33 in mm, 5..150) and the step width34 (1..10) can be parameterized.

CAL F4 Starts the automatic routine for the recalibration measurement. The step-motor drives to the preset position for the Open-Frame recalibration.

0/0 F5 The Step-Motor (or <Ins> key) drives both carriages of the linear guides to the reference position to initialize its 0/0-position (X=0, Y=0).

Strt F6 Drives to the Start-position of the Open-Frame application (or <Home> key). While scanning, this function is deactivated.

End F7 Drives to the End-position of the Open-Frame application (or <End> key). While scanning, this function is deactivated.

CalP F8 Goes to the Calibration-Position which was set as Recal-X and Recal-Y in the Set-Menu before (or <Del> key). While scanning, this function is deactivated.

Quit Enter Quits Step-Motor Mode35 back to the Start-Display. Frm-Plt F Selects the Open-Frame- or Micro-Plate function (Frm

or Plt in red) for the Step-Motor Mode (or <p> key). While scanning, this function is deactivated.

Plot P Printing out the scanning result by a Mini-Plotter. NoCount N Suppresses the Non-identification results (---) in the

counter list and in the statistical percentage. ./. PgUp Sets the step width higher (max. 10), <Page-Up>. ./. PgDn Sets the step width smaller (min. 1), <Page-Down>. ./. A Sets the scan numbers (scans/runs) in steps of 1 up

to 5000. The scan numbers36 can be changed by pressing the <a> icon repeatedly.

Be aware that the given recalibration place (CalP) for the Open-Frame operation must be empty!

32 If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position. 33 The measuring frame is always arranged around the Center-position M/13 of the scanning area. 34 The smaller the step width, the longer the scan lasts. Step-width:1 equals to 0.15mm (max steps = 1080). The NIR-sensor focus diameter is ca. 2mm. To protect life time of the NIR-light sources it is recommended that scanning should not last longer than 1 hour. 35 When the Step-Motor Mode is activated again then the last scanning result is displayed again until a new scan is started. 36 The default value is 1000 scans, a priori, to obtain a stable average spectrum for evaluation.

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6.6.3 Step-Motor Operating Elements while Scanning Icon Key Function

<= F1 Switches to Spc-Mode and back to view the transformed Net-Data or NIR-Spectra during the Step-Motor procedure.

Scan F2 Starts the Step-Motor scan. Previous results and statistics are deleted before.

Set F3 Switches to the Set-Mode to set parameters. CAL F4 Starts the automatic routine for the recalibration

measurement. The step-motor drives to the preset position for the recalibration. Previous results are deleted. Longer time pressing of one of both triggers interrupts the recalibration procedure.

0/0 F5 The Step-Motor drives both carriages of the linear guides (or <Ins> key) to the reference position again to initialize its 0/0-position (X=0, Y=0).

II F6 Pauses37 the running Step-Motor scan. The scan continues by pressing repeatedly <F6> or the ►-icon. The linear guides stay fixed at their position.

Plot F7 Printing out the actual scanning result by a Mini-Plotter. The rocker switch located at the integrated plotter must be turned on.

Stop F8 Stops the running Step-Motor scan and powers off both step-motors. The actual results will be displayed. Short pressing one of both triggers stops also the scanning.

Quit Enter Quits Step-Motor Mode38 back to Start-Display. NoCount N Suppresses the Non-identification39 results (---) in the counter list and in

the statistical percentage. ./. PgUp Sets the step width40 higher (max. 10), <Page-Up>. ./. PgDn Sets the step width smaller (min. 1), <Page-Down>. ./. A Activates41 the Standard (All) model. ./. G Activates the gray Type (gryT) model. ./. E Activates the Extra Model ./. C Activates the clear Type (clrT) model. ./. F Activates the Foil model. ./. D Activates the DSD model. ./. M Activates the Modify function (Mdfy).

37 Do not use the Pause function for to long time, because the step-motor is still active in this function (motor standby) and sensitivity of the actual reference spectrum might change. 38 When the Stepping-Motor mode is activated again then the last scanning result is displayed again until a new scan is started. 39 In the Open-Frame mode two times the same identification result must be evaluated successively before it is be counted. Therefore counting non-reliable results while crossing two pellets/granulates/ground material is almost avoided. In the Micro-Plate mode each identification result is counted. 40 Changing the step width has no function in Micro-Plate mode. The step width to be chosen in the Open-Frame mode should be selected according to the size of the granulates/pellets/ground material. Smaller particles require preferably lower values, bigger particles can be measured with a greater step width to reduce the overall measuring time. The relation between scan time and step width should be evaluated individually depending on the samples under investigation. 41 Each time when changing the neuronal network identification model all counted values and percentages will be reset to zero.

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6.7 New Functions and Hotkeys Overlay-Function: With the new Overlay-Function (with O oder 0) two Microplate results can be shown above each other to check e.g. the chessboard results with different models or with different scan times. If overlay is activated, then the actual results will be copied to one “layer” “below” and be shown in YELLOW. Now you can make a second scan with another model or scan time in normal colours which are shown above the former results. It is not necessary to make a complete new scan. You simply can change the model after overlay is activated and the system will take all the results of his memory and make a second calculation with the new parameters.The actual measuring model is shown down on the right; the Overlay model for comparison is indicated down on the left in YELLOW. SET-Menu: Within the SET menu you now have the new NoCount function on <F7>. You can choose now up to 6 different polymer types which are not to be counted within the resulting statistic list. They will not show up as names or as percentages. Also the unidentified plastics (---) now must be put in here, if they should not be counted. The not counted polymers are shown in WHITE on the chessboard to show the user which are not counted in the statistics. All the results are counted anew when the SET menu is closed and you will hear the increasing buzzing sound or see a message. Pressing NoCount again shows again all detected polymers in the statistics. When more than 12 plastics are detected, then the middle display will be extinguished and you will see instead of it the additional polymers. <F7> within the No Count menu allows you to change between the normal light attenuation mode and the special signal/noise ratio mode which is used for very small micro particles.With the keys <PgUp> and <PgDn> you can increase or decrease the S/N ratio, depending on the size of the micro particles. If you press the <F> key, you will see the list in bigger display. If pressed again, the former picture will return.

New Key commands: T -> switches the StepMotor function on and off Z -> switches the Modify function on and off F -> switches between MicroPlate and OpenFrame mode O or 0 -> switches Overlay on and off 1 or q -> quits the program 2 or F ->switches between Frame and Plate mode 3 or P -> plots the results 4 or N -> activates/deactivates the NoCount function <Space> or 5 -> switches the FrontView layer when Overlay is ON <Space> -> makes a scan when Overlay is OFF On the touchscreen: The actual position of the measuring head is now marked in a WHITE grid. The four arrows ->, <-, and up and down can move the actual measuring head position in the respective directions for one position per click, as well as with the arrow keys on the keyboard. Pressing the<Space> key when overlay is off or one of the triggers will make an individual measuring at the actual position of the measuring head.

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6.8 Polymer Type Identification by Neuronal Networks The identification of the polymer type using neuronal network is the result of a mathematical model for polymer identification This data processing simply means a comparison with a pre-set pattern recognition42. Different types of plastics are categorized into a main group and into a number of sub-groups for fine differentiation.

Due to this it is very important to select the right identification net model to obtain the correct identification result depending on colour (Standard or gray Types), thickness (Foils) or properties (clear Type) of the plastics to be measured.

After the measurement, the near infrared intensity data (NirD) are mathematically transformed in ratio to the actual reference spectrum of the white ceramic plate and then normalized and scaled into network data (NetD). These values are processed with given weighting factors and special algorithms of the neuronal network model and stored. The pre-set data of the net model have been created, trained and stored by calibration beforehand. The result of the calculation is a ranking list of the most probable polymer types ranging between 0% and 100%. In the top of the Results window the three polymer types with the highest degrees of probability are displayed in red letters. The percentage value expressed the

hit quality determined in the network model. It is not indicating the composition of a polymer blend!. If the results of the measurement for a polymer type exceed the pre-set probability threshold values, then the plastic in the first place in the hit list is additionally displayed in large green letters in the middle of the display. If the pre-set limit values have not been exceeded (e.g. 1st place less than 70 %, 2nd place greater than 30 %), it indicates that the neuronal network was not able to identify the sample reliably. Non-identification is signaled with the No-Result message (---). This is a request to repeat the sample measurement again. If repeated measurements still produce this message, the sample might be unknown (not calibrated) or the wrong net model was selected for identification or new recalibration is necessary. 6.8.1 The Min-Pxl statement The pixel minimum of the NetD curve (Min-Pxl) is very characteristic43 for a polymer type and can alter depending on the thickness44 of the sample. In the file head of a Dat-file the specific Min-Pxl positions of plastics are listed as Minimum- and Maximum ranges. These values were determined during the calibration of the device for each polymer type. In case that the actual pixel minimum of the NetD curve (here: 17) is not in the range of the pre-set Min-/Max-Pixel value of a polymer identified (here: PMMA as the 1st hit list ranking of the identification probability) then the message Min-Pxl is shown (here: pre-set PMMA range 14-15). It indicates a logical restriction of the identification result due to the experiences made during the specific system calibration of the manufacture. The pre-set Min-/Max-Pixel range for a polymer type should be adjusted45 (see: The Dat-Files), if repeated measurements with known samples and correct identification probabilities for the 1st ranking still produce a No-Result message with the Min-Pxl statement.

42 The relative disadvantage of any neuronal network algorithm is that after the production no other polymer types can be calibrated by the user. The model is only valid for the given main and sub-groups. Modifications must be carried out on demand by the manufacturer. 43 Depending on the spectrometer system. 44 As an example: the Min-Pxl of a thin PE foil is usually at 22 whereby the Min-Pxl of solid PE sample ranges between 20-21. 45 Displacements of the predefined pixel positions in the spectrometer optics can occur as a result of temperature effects.

!

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6.8.2 Standard Model (All, for coloured, natural or milky-like plastic parts): This identification46 model is recommended when coloured, natural- or milky-like plastic parts (not gray, not black and not transparent) are to be detected. Herein the amount of polymer types for fine differentiation of the styrene-containing sub-group is reduced. Modified results (Mdfy) switches PA6x47, PA12 to PA and PP, PE to PO and ABS, PS to Styr and PBT, PET to PES and PCA, PCPT to PC. It means the identification will be simplified. The fine differentiation of the polymer type in the sub-group is modified/altered to the main group. Identification of PA (PA6x, PA12), PO48 (PP, PE), Styr49 (ABS, PS), PES (PBT, PET), PC (PCA, PCPT)50, PMMA, POM and PVC: 6.8.3 Clear Type Model (clrT, for clear, transparent plastic parts): Restriction of the polymer identification to few clear types which can normally occur also or only as clear, transparent plastic parts. This identification model is recommended (thickness: 0.5 – 6 mm), because the amount of polymer types for fine differentiation of the styrene-containing sub-group is extended and other types are neglected to enhance the identification performance. Materials which are thicker than 6 mm the result for clear materials might become not reliable and for materials which are thinner than 0.5 mm the Foil model should be selected. Modified results (Mdfy) switches ABS, SAN (AS), PS to Styr. Identification of PO51 (PE, PP), Styr (ABS52, PS, SAN53), PET, PC, PMMA and PVC: 6.8.4 New Extra Model: The Update has the new Extra-Modell (Extr) with a larger polymer variety, to be used as a screening model. Her are plastics from the Standard Model (no PCPT), Foil Model (no PEPA, PPPT and PEPT), Gray Type Model (no PCPT) and Clear Type model. PA, PO (PP, PE), Styr (ABS, PS, SAN, PPO), PES (PBT, PET), PC (PCA, PC), PMMA, POM and PVC PA combines PA6x und PA12. PLA is not included here, but POM. S -> switches between Sty4 = ABS, PS, SAN, PPO and Sty2 (only ABS, PS). Sty4 is only working with an active Extra-Model. Screening with the new Extra-Model and S4 detection ist he best for a quick screen of unknown samples. The Modify-Function (Mdfy) changes the display to the respective Main Group. All displays in Ready or SPC-Mode are now in GREEN. If modified, then in RED.

46 IoSys uses the following abbreviations: PA=Polyamide, PO=Polyolefine, Styr=Styrene containing polymers, PES=Polyester, PCA=PC+ABS, PCPT=PC+PBT or PC+PET, APVC=ABS+PVC, PLA=Polylactoseacetate-biodegradable, CLLS= Cellulose; Multilayers: PEPA=PE+PA, PEPT=PE+PET, PPPT=PP+PET. 47 Fine differentiation of PA6 and PA66 polymer types is not reliable. Therefore both types are calibrated and combined to PA6x. 48 To distinguish each Polyolefine group for the neuronal network calculation IoSys uses the following abbreviations: PO for Standard (All) and POx for DSD model. 49 To distinguish each styrene-containing group for the neuronal network calculation and editing IoSys uses the following abbreviations: Styr for Standard (All), Styl for clear Type, Strl for gray Type model. 50 Due to their polymer similarity the identification of coloured PC, PCPT and PCA polymer types is sometimes uncertain. Blend ratios from PC/PBT or from PC/PET of 60:40, 50:50 and 40:60 are calibrated as “PCPT”. 51 No fine differentiation of transparent polyolefine is made in ClrT. Fine identification should be done via Standard (ALL) model. Nowadays transparent PO could be a polyethylene with copolymer like Surlyn® of DuPont™ 52 Usually transparent ABS material is a blend which contains PMMA, too. 53 SAN = Styrene-Acryl-Nitril is also named as AS = Acryl-styrene.

PES

PA6x, PA12 PP, PE PBT, PET

POM PO PMMA PA Styr PC PVC

ABS, PS PCA, PCPT

PC PMMA PET Styr PVC

ABS, PS, SAN

PO

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6.8.5 Gray Type Model (gryT, for gray-coloured plastic parts):): This identification model is recommended when gray-coloured plastic parts54 coming from the electro- and electronic dissembling area (e.g. computer waste) are to be detected, because the amount of polymer types for fine differentiation of the styrene-containing sub-group is extended and other types are neglected to enhance the identification performance. The restriction of the polymer identification to gray-coloured materials helps to work out the distinctive marks in the NIR spectra enhancing the NIR-identification performance for these materials. Modified results (Mdfy) switches PPO, PS and ABS to Styr and PCA, PCPT to PC. Identification of PA55, PP, Styr (ABS, PS, PPO), PCA (PC, PCPT)56, APVC and PVC 6.8.6 Foil Model (Foil, for thin materials): This identification model is recommended when transparent thin materials like foils are to be detected. Due to the variable thickness of foils the absorption and reflection characteristic differs in comparison to solid materials. These differences appear in the position number of the NIR-curve minimum for the polymer types (Min-Pixel). The Thin foils should be folded several times thus a thickness at least 50 - 100 µm is achieved, otherwise the result might not be reliable. Materials which are thicker than 500 µm should be measured using the Modified results (Mdfy) switches PEPA, PEPT to PE57 and PPPT to PP. Identification of PA, PP (PPPT), PE (PEPA, PEPT), PS, PET, PVC, PLA58 and CLLS: 6.8.7 DSD Model (for household and packaging plastics): This identification model is recommended when typical plastic parts and foils coming from the household and packing area (MWS) are to be detected, because the amount of polymer types is restricted to few polymer types which normally occur as household and packaging plastics (MWS= DSD =Duales System Deutschland). To enhance the spectral variances, the database of ABS, PS are combined to PS and PBT, PET as PET. In the DSD model no PA-, PEPT-, PLA- and CLLS foils are calibrated and due to the spectra similarity the multilayer foil PEPA was taught in as PE. Modified results (Mdfy) switches PP, PE to PO.

Identification of PO (PP, PE), PS, PET and PVC:

54 Due to the experiences of IoSys it must be stated that gray coloured plastics (e.g. PA, PP, PVC) which are containing lot of Talcum or glass fibers (20-40%) as a filling material reduces the NIR light reflection causing non reliable identification results. 55 Fine differentiation of PA6, PA66 and PA12 polymer types is not reliable. Therefore all types are calibrated and combined to PA. 56 Due to their polymer similarity the identification of gray coloured PC, PCPT and PCA polymer types is sometimes uncertain. 57 Due to the fact that the thickness of the layers are always different, the identification results are sometimes not reliable. 58 PLA=Polylactoseacetate-biodegradable, CLLS= Cellulose (paper, cotton)

PS

PET

PO

PVC

PP, PE

ABS, PS, PPO

PC APVC Styr PP PVC

PCA, PCPT

PA

PET

PVC

PS

PE

PLA PP

PA

PEPA, PEPT

PPPT

CLLS

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6.8.8 Composition of Styrene-containing Polymers In general the differentiation of styrene-containing polymer types like ABS, PS, PPO, SAN (AS), PCA und APVC are difficult with the NIR Technology due to their polymer similarity. Most of them are blends of each other in different concentrations. But restriction of the polymer identification either to their colours (if coloured, natural- or milky-like (Standard) or if gray-coloured (gryT)) and to their material properties (if transparent (clrT) or thin (Foil)) or their characteristic fire retardant compositions helps to work out the distinctive marks enhancing the identification performance for these materials. 6.9 Polymer Type Identification by PLS The identification of the polymer type using the PLS59 method (Partial Least Square) is the result of a comparison of the measured spectrum with the stored Teach-in spectra (best fitting curve). It means that an actual spectrum (here: blue curve) is compared with all teach-in sample data which are activated (here: gray & red curves). The more the blue curve resembles to one of the Teach-in curves, the higher the Hit-Quality percentage. In this case the blue curve has the best fit to the gray one. As an example: the actual curve resembles to the blue curve to 91%.

59 The advantage of the PLS method is that the user can teach-in own test samples to carry out simple rapid analysis. The disadvantage is that PLS works for NIR-spectra only which obviously have big spectral differences.

Teach-In sample-1

Teach-In sample-2

Actual spectra

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6.10 Recalibration of sIRoGran The background to the recalibration routine is that different known types of plastic have been calibrated against a reference standard (white ceramic plate). It means that the near infrared intensity data (NirD) of the known samples were mathematically transformed in ratio to this reference standard, normalized and autoscaled into network data (NetD) for modeling neuronal networks for plastic identification (see:). At that point of time the sIRoGran system was calibrated (the so-called Design state60), this reference spectrum was stored as the “original reference spectrum” (ORG).

Due to temperature effects, deviations in the sensitivity of the scanning electronics are shown up and therefore the resulting intensity data differ. In general, when the device is just powered on or if the system is used in a cold environment (cold state61) the NIR-signals of a measurement are less intense in comparison to the design state. Through the used ratio method, the effect of changes to the state of the system are almost eliminated through the formation of intensity ratios (sample spectrum divided by the current reference spectrum). However, the identification capabilities of the spectrometer can be reduced in the cold state. A priori, the

identification performance is best when the current signal output is similar to the design state. In order to operate the system immediately (no waiting time for warming up), a recalibration routine is used. The recalibration procedure for diffuse reflection measurements automatically adjusts the measurement electronics in a way that the current signal output of the reference standard closely fits to the stored original reference. Proceed as follows to recalibrate the sIRoGran in manual operation62: 1. Press the <CAL> icon to start the recalibration. 2. Attach the measuring head against the white ceramic reference

and keep pressing one of the both triggers (in manual operation mode only) until the last message: Stop triggering indicates the end of the recalibration routine. During the recalibration procedure the following messages will be shown up:

At first, (while pressing the trigger) the message Recalibrating… with a hour-glass appears. This status indicates that the auto-gain-adjustments is running. If the electronic adjustment has adjusted the current signal output similar to the Design state the message Recalibration running... is displayed. At that moment the actual reference measurement with NIR-light is carried out. Afterwards the light is powered down automatically and the message: Dark Measurement now running... is displayed to measure the dark signals (still keep pressing the trigger!). The message: Saved as new Reference signals that the measurement has been accepted.

In case that the intensity data of the actual reference measurement differs

from the last signal curve, error messages like Gain too high! or Gain too low! are shown up. The reason could be that the measuring head was not constantly attached to the ceramic plate causing that non-reproducible spectra. The recalibration procedure has to be repeated.

If the message: Changed Condition! Do new Recalibration appears then the recalibration should be carried out again as described before (gain drifting because electronics are heated up).

60 Design state: For sIRoGran calibration the system was always powered on 2 hours before at a room temperature of 22 C to ensure that the device was in a thermal equilibrium and thus the resulting signals were stable and reproducible. 61 Cold state: When the sIRoGran is just powered on, it is not in a thermal equilibrium. At the beginning the spectra are lower in intensity, drifting towards higher values within 2 hours, i.e. the signal outputs are unstable and non-reproducible. 62 In the automatic operation no one of both triggers must be pressed, however, the messages are also showing up.

Original reference spectrum (ORG)

same measurement in a cold state

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6.11 Operating Elements in the Spc-Mode 6.11.1 The Main Menu Icon Key Function

NirD F1 Switches between the representation views. In the <NirD> mode the raw intensity data are shown and in the slot window the measured NIR-light intensity level and Pixel number of the curve minimum is listed (Min-Pxl). In the <NetD> mode mathematically transformed intensity data are displayed. In the slot window the slot number and the sample file name is listed if stored before.

OnLn F2 Starts the Online-Mode wherein the spectrometer optic is continuously reading out without triggering. The online spectrum is displayed in slot place#1. The Online-Mode allows to display simultaneously other spectra or permits e.g. external light sources held in front of the measuring head to be adjusted for the transmission mode (optional feature). Pressing again the <OnLn> icon stops the online measurement.

??? F3 Activates the polymer type identification (PLS or neuronal network) for all displayed spectra. In the NetD-mode the identification result and the 1st ranking percentage for each spectrum is listed in the corresponding slot window. Pressing again the <???> icon returns back to the statements of NIR-light intensity and Min-Pxl or sample file name.

Cal F4 Starts the same recalibration routine (see: Recalibration of sIRoGran). In the NirD mode the original reference spectrum is automatically loaded in slot place#2 for better comparison and the actual raw intensity data are displayed in slot place#1. If the <Cal> function is unintentionally pressed the recalibration can be stopped touching the <F7> key or <Clr> icon, resp..

AvSp F5 Forms an average spectrum (not auto scaled) from all the spectra which are displayed and plots it in slot place#20 as a brown thick line (see: The Bottom Menu) with a blue coloured slot window. Pressing the icon again cancels arithmetic forming of an average mean.

New F6 Opens the New-Menu to delete the representation of a spectrum at a slot place. The next spectrum

now appears at the slot place marked with „". Clr F7 Deletes all the spectra represented at the slot

places. ESC F8 Leaves the Spc-Mode, back to the Start-Display. 6.11.2

Statement of the selected identification model

Statement of the actual total measuring time

Shift menu bar

Zooms the NirD-curve view

Main menu bar

Number of scans (runs) to calculate a average spectra used for evaluation

Bottom menu bar

Slot window: statement of: -Measured NIR-light intensity level -Min-Pixel -Name of the stored spectrum l

Loading of the original reference spectrum

Starts a scan without triggering

Loading of the current reference spectrum

Pixel Numbers

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6.11.2 The Shift Menu Icon Key Function

Load Sft+F1 Opens the Load-Spectrum Menu to open spectra which were saved in the directory path edited under Dir (max. 22 letters). A temporary change to the pre-set directory (edited in the Initialization File) and path can be carried out under Dir. The files are listed in filtered form in accordance with the characters63 entered. Moving within the window can be done with the <Enter> or <Cursor up> or <Cursor down> key. Loaded spectra are shown in different colours after quitting the menu.

Save Sft+F2 Opens the Save-Spectrum Menu to permit spectra to be stored in the directory path edited under Dir (max. 22 letters). A saved spectrum file gets the file suffix „*.spc“ and is written in a Flat-ASCII text format.

PLS-NNet Sft+F3 Switches between the PLS model (Partial-Least-Square) or the Neuronal Network calculation.

???-OnLn Sft+F4 Starts the Online identification mode64 which continuously displays the identification result with the hit list ranking. The hit list is displayed in red letters for neuronal network and in blue letters for the PLS mode. Pressing the <OnLn> or <Clr> icon stops the online identification measurement.

MS-Dos Sft+F4 Opens the MS-Dos Menu for carrying out given MS-Dos operation commands:

Plot Sft+F6 Prints65 out the actual display as a screen dump to a Mini-Plotter (optional feature). Touching any field of the touchscreen or pressing any key on the Keyboard stops the plotting process.

USB-Load Sft+F7 Opens the USB-Load Menu to load spectra which were saved in an external USB-stick66 in the pre-set subdirectory (e.g. in d:\nir\). Operating elements are the same as described under Load.

Sample Sft+F8 Loads all activated Teach-in samples (max. 8 spectra with the edited file names in the slot #1 up to slot #8. This function gives an overview of the stored Teach-in sample data set.

./. Sft+F9 Starts the recalibration routine without auto-gain-adjustment (not displayed in the Shift menu bar). This procedure is recommended if own application (analysis method) is created whereby the reference spectrum should not have the same intensity level as the stored original reference spectrum (e.g. reference signal as blank signal).

6.11.3

63 A backslash (\) edited at first of the file name activates the loading/saving of a file series. For example, the entry \kal-0 loads/saves all spectra beginning with the file from kal-1; an entry \kal-1 loads/saves all spectra beginning from kal-11. 64 The Online function in the SPC mode operates faster as in the Ready window, because less time is needed for the screen setup. Either the Circular mode while pressing the rod trigger or the Online mode for transmission operation is possible. 65Only active if a the Mini-Plotter is connected and the hardware is activated in the initialization file Ini.dat. 66 The stored NIR-spectra at the USB-Stick have a different file format (in rows/lines), thus these files can not be read and load with the Load-Function (F1).

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6.11.3 The Bottom Menu Icon Key Function

./. 0 Displaying the last NIR-curve (highest Slot-number) as a thick curve (or <t> key). Menu 1 Opens the Menu Bar (also with <ENTER>) to select a net model for polymer type

identification (<F1>..<F5>). Delete 2 Deletes the spectrum with the

highest slot number (also with <Backspace>).

??? 3 Switches to the Result-Display for ca. 2 sec. The spectrum at slot#1 is evaluated (see. Operating Elements in the Result-Display).

Test 4 Starts the Test-Program (sIRoGran.exe) for testing electronic parts on the NIR-interface board and of the X/Y-table device part. In case of hardware operating malfunctions this diagnostic program helps to locate the error. For example: The gain adjustment function of the electronics are checked by using <F3> or <F4> or with the means of the Hotkeys <d> (gain down), <m> (gain mid) and <u> (gain up).

SMtr 5 Starts and stops the Step-Motor Mode for scanning granulates/ pellets or ground materials (see: Operating Elements in the Step-Motor Mode).

6.11.4 Additional Operating Elements Icon Key Function

Scans A Sets the scan numbers67 (scans/runs) in steps of 1, 10, 50, 100, 250, 500, 1000, 2000, 3000, 4000 and 5000. The scan numbers can be changed by pressing the <a> icon repeatedly. The default value is 1000 scans, a priori, to obtain a stable average spectrum for polymer type identification.

Org O Loads the original-reference spectrum into the next vacant slot.

Ref R Loads the current reference spectrum into the next vacant slot.

Scan # Starts a scan without pressing the trigger68.

Zoom Zooms the representation view of the displayed data curves. In the <NetD> mode the intensity percentage ranges then from 0-0.1% which makes it easier to see peak minima (e.g. to detect abnormal curve shapes). In the <NirD> mode the spectra is auto scaled between the first and last Pixel value. Pressing the <Cursor-up> icon again returns back to the full image representation

./. P Activates the polymer type identification (PLS or neuronal network) for all displayed spectra (same as <???> icon).

67 The higher the scan number (Runs), the better is the resulting average spectra (improved signal/noise ratio of the calculated average) and the more stable the identification result. However, the measuring time is longer. On the other hand, the smaller the scan number, the more noisy is the resulting spectrum for evaluation, the less stable is the identification result. However, the measuring time is shorter. 68 The NIR-light source is switched on automatically (indicated by the yellow LED) in the Step-Motor Mode only, not in the manual operation. For measurement with NIR-light one of both triggers (red or metallic one) must be pressed.

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6.11.5 Step-Motor Operating Elements in the Spc-Mode

6.11.5.1 The Micro-Plate Mode Icon Key Function

<= F1 Switches back to the Result-Display with the “chessboard”-view.

Scan F2 Starts the Micro-Plate scan. The fixed measuring rod at the X/Y-table drives to the position-169 (Pos1, A/1) and moves step by step (625x) to position-2 (Pos2, Y/25). Repeated pressing <F2> interrupts the actual scan and starts it again.

Set F3 Switches to the Set-Mode to set X/Y-positions and colours for polymer types and to select the identification model for the step-motor operation. Using <0> and <1> the Y- and X-axis position (A..Y, 1..25) for the X/Y-function can be set. With <2>..<5> four polymer types can be selected for coloured70 marking. 40 code numbers are listed for given polymer types.

CAL F4 Starts the automatic routine for the recalibration measurement. The step-motor drives to the preset position-1 for the Micro-Plate recalibration.

0/0 F5 Step-motor drives (or <Ins>) to the upper left reference position to initialize its 0/0-position (X=0, Y=0).

Pos1 F6 Drives to the position-1 (A/1) of the Micro-Plate (or <Home> key). While scanning, this function is deactivated.

Pos2 F7 Drives to the position-2 (Y/25) of the Micro-Plate (or <End> key). While scanning, this function is deactivated.

X/Y F8 Goes to the preset X/Y-position (or <Del> key). While scanning, this function is deactivated. Frm-Plt P Selects the Open-Frame- (Frm or Plt in red) or Micro-Plate operation for the Step-Motor Mode

(or <e> key). While scanning, this function is deactivated. Plot Sft-F6 Printing out the scanning result by a Mini-Plotter. The rocker switch

located at the integrated plotter must be turned on. NoCount N Suppresses the Non-identification71 results (---) in the counter list and in

the statistical percentage. SMtr 5 Starts and stops the Step-Motor Mode. Stopping the Step-Motor Mode

while scanning e.g. allows to switch from the NetD- to the NirD-View to show the percentages instead of the numbers at the right bottom side.

Be aware that the given recalibration place (A/1) for the Micro-Plate operation is always empty!

69 If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position. 70 Non-identifications (---) are marked in green and empty places (-), where less NIR-light attenuation had occurred compared to the actual reference spectrum, are displayed in white. 71 In the Open-Frame mode the same identification result must be evaluated two times successively before it is counted. Therefore the counting of non-reliable results while crossing two pellets/granulates/ground material is almost avoided. In the Micro-Plate mode each identification result is counted.

!

Listing of identified polymer types with statistic statements

Selecting Open-Frame or Micro-Plate application

No counting of Non-identification results

X- and Y-axis position of the X/Y-table

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6.11.5.2 The Open-Frame Mode Icon Key Function

<= F1 Switches back to the Result-Display with the listing. Scan F2 Starts the Open-Frame scan. The fixed measuring rod at

the X/Y-table drives to the Start-position72 and moves step by step (depending on the set step width) to the End-position.

Set F3 Switches to the Set-Mode to set positions and sizes and to select the identification model for the Open-Frame operation. Using <6> and <7> the Recal-Y- and Recal-X-positions for the recalibration position can be set. With <8> and <9> the measuring size for the frame (square size73 in mm, 5..150) and the step width74 (1..10) can be parameterized. Code numbers for given polymer types are only listed in the activated Micro-Plate Mode.

CAL F4 Starts the automatic routine for the recalibration measurement. The step-motor drives to the preset position for the Open-Frame recalibration. Longer time pressing of one of both triggers interrupts the recalibration procedure.

0/0 F5 Step-motor drives (or <Ins> key) to the reference position to initialize its 0/0-position (X=0, Y=0).

Strt F6 Drives to the Start-position of the Open-Frame application (or <Home> key). While scanning, this function is deactivated.

End F7 Drives to the End-position of the Open-Frame application (or <End> key). While scanning, this function is deactivated.

CalP F8 Goes to the preset Calibration-Position which was pre-set as Recal-X and Recal-Y in the Set-menu before (or <Del> key). While scanning this function is deactivated.

Frm-Plt P Selects the Open-Frame- or Micro-Plate function (Frm or Plt in red) for the Step-Motor mode (or <e> key). While scanning, this function is deactivated.

Plot Sft-F6 Printing out the scanning result by a Mini-Plotter. The rocker switch located at the integrated plotter must be turned on.

SW PgUp Sets the step width higher in steps of 1 up to max. 10, <Page-Up>. ./. PgDn Sets the step width smaller (<Page-Down>. Scans A Sets the scan numbers (scans/runs) in steps of 1 up to 5000. The scan numbers75 can be

changed by pressing the <a> icon repeatedly. SMtr 5 Starts and stops the Step-Motor Mode. Stopping the Step-Motor Mode while scanning allows

e.g. to load and save spectra or to change parameters.

Be aware that the given recalibration place (CalP) for the Open-Frame operation must be empty!

72 If the X/Y-table has not been initialized to the reference position 0/0 before, then the measuring rod drives firstly to this position. 73 The measuring frame is always arranged around the Center-position M/13 of the scanning area. 74 The smaller the step width, the longer the scan lasts. Step-width:1 equals to 0.15mm (max steps = 1080). The NIR-sensor focus diameter is ca. 2mm. To protect life time of the NIR-light sources it is recommended that scanning should not last longer than 1 hour. 75 The default value is 100 scans, a priori, to obtain a stable average spectrum for evaluation.

!

Listing of identified polymer types with statistic statements

Selecting Open-Frame or Micro-Plate application

Setting of the step width

X- and Y-axis position of the X/Y-table

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6.11.5.3 Step-Motor Operating Elements while Scanning

Icon Key Function

<= F1 Switches to Spc-Mode and back to view the transformed Net-Data or NIR-Spectra during the Step-Motor procedure.

Scan F2 Starts the Step-Motor scan. Previous results are deleted before. Set F3 Switches to the Set-Mode to set parameters. CAL F4 Starts the automatic routine for the recalibration measurement. The step-motor drives to the

preset position for the recalibration. Pressing one of both triggers interrupts the recalibration procedure

0/0 F5 The Step-Motor (or <Ins> key) drives both carriages of the linear guides to the upper left reference position again to initialize its 0/0-position (X=0, Y=0).

II F6 Pauses the running Step-Motor scan. The scan continues by

pressing repeatedly <F6> or the ►-icon. Plot F7 Printing out the actual scanning result by a Mini-Plotter.

The rocker switch located at the integrated plotter must be turned on.

Stop F8 Stops the running Step-Motor scan. The actual results will be displayed. Pressing one of both triggers stops also the running scan.

./. PgUp Sets the step width76 higher (max. 10), <Page-Up>.

./. PgDn Sets the step width smaller (min. 1), <Page-Down>.

./. A Sets the scan numbers77 (scans/runs) in steps of 1, up to 5000.. The scan numbers78 can be changed by pressing the <a> icon repeatedly.

./. S Activates79 the Standard (All) model.

./. G Activates the gray Type (gryT) model.

./. E Activates the Extra-model

./. C Activates the clear Type (clrT) model.

./. F Activates the Foil model.

./. D Activates the DSD model.

./. M Activates the Modify function (Mdfy).

./. S Switches between the S4 and the S2 mode within the Extra model

76 Changing the step width has no function in Micro-Plate mode. The step width to be chosen in the Open-Frame mode should be selected according to the size of the granulates/pellets/ground material. Smaller particles require preferably lower values, bigger particles can be measured with a greater step width to reduce the overall measuring time. The relation between scan time and step width should be evaluated individually depending on the samples under investigation. Experiences have to be gained. 77 To be averaged for the display of the result in steps of 1, 10, 50, 100, 500, 1000, 2000, 3000, 4000 up to 5000. The default value is 1000 scans, a priori, to obtain a stable average spectrum for evaluation. 78 The default value is 1000 scans, a priori, to obtain a stable average spectrum for evaluation. 79 Each time when changing the neuronal network identification model all counted values and percentages will be reset to zero.

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7 The System Files for sIRoGran

7.1 The Initialization File Pre-set parameters like the serial number of the unit, hardware address, directory paths and the activation of optional features are stored in the file: ini.dat. This text file can be opened by pressing the <F7> (mIRoIni) in the Keys-Display (see: Operating Elements in the Keys-Display). As an example a typical initialization file is listed: (data always differ depending on the system!). 7.2 The Plate-File Parameters like the X- and Y-positions80 of the X/Y-table81 for the Micro-Plate- or Open-Frame operation, the threshold values for the NIR-light attenuation and the polymer types for coloured marking are stored in the file: plate-XX.dat. This text file can be opened by pressing the <F2> key or the <PlateIni> icon in the Keys-Display. Four polymer types can be selected for coloured marking. 40 code numbers are listed for given polymer types. As an example a typical PlateIni-file is listed: (data always differ depending on the system!).

80 In case the linear guides do not find the Position: A/1 for the Micro-Plate Mode correctly, please check if the correct values are set in the first line. 81 The X-axis ranges between 1... 25. The Y-axis ranges between A ...Y. For storage the letters are transformed to numbers 1… 25 again.

Password which activates the sIRoLine-program. Overwrite the 8 stars by entering a new password (8 small characters!) supplied by your distributor.

Activation code for optional configurations 0=deactivated, 1= activated .

Preset subdirectory path for saving and loading spectra files.

Position-1 (Pos1, A/1) for the linear guides

X-, Y-positions for Step-Motor operation.

Selection of polymer types by editing the code numbers.

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7.3 The Teach-In File Sample names and pre-set threshold values edited in the Teach-In menu are stored in the file: teach-XX.dat (XX=series number). This text file can be opened by pressing the <F8> (TeachIn) in the Keys-Display. Herein other sample names can edited compare to the given polymer types list. As an example a typical Teach-In file is listed: 7.4 The Dat-Files The Min-/Max-Pixel range of the NetD curve minimum and given values of the neuronal network models (weighting factors) are stored in the Dat-files modelname-XX.dat (XX=series number). These text files can be opened as described before in the Keys-Display by switching into the mIRoNet Menu with <F6> and then pressing the <f>..<u> keys or model name icons. As an example for a typical Dat-file of the Standard (All) model is listed (data always differ depending on the actual individual unit!).

Maximum pixel value. Between these two numbers the peak minimum of the NetD-curve (Min-Pxl) must be positioned to display the 1st hit list ranking in big letters. These values were determined during the calibration of the system before (DESIGN state).

Minimum pixel value

Pre-set threshold values for the Hit-Quality and Hit-Difference statement for the “best fitting algorithm” using the PLS-method.

Individually editing the Teach-In sample with names with max 4 characters (e.g. Test).

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8 Data Exchange

8.1 Using PC-Link cable For communication with other computers and the update of software the MS-DOS communication system Interlink/Interserver can be used for the communication between the device system and other computers (only working for computers equipped with Windows95® or Windows98®) for with the aid of the serial interface, a zero modem cable (Laplink-cable, 9p-SUB-D). Copy the interlnk.exe file (supplied by Floppy-Disk or e-mail) to a directory on the computer (e.g. your Desktop or Laptop computer) where you want to make the communication with the systems. The interlnk.exe file should be placed in the main root c:\ of the external computer and should get an entry in the config.sys file82 as following.

device=c:\interlnk.exe /com /noprinter /auto.

1. Connect a serial zero modem cable to the COM interfaces of the device (acts as Server) and the external

computer (acts as Client). 2. Switch off the integrated Mini-Plotter (optional feature) with the rocker switch locate aside before to avoid

data transfer malfunctions. 3. Press the <PC-Link> icon (or <F3>) in the KEYS-Menu to start

data exchange program (intersvr.exe). 4. Reboot the external computer (e.g. your Laptop or Desktop-PC) to

start the data exchange program. The drives of the measuring device (e.g. A:\, C:\) will appear now as additional drives (e.g. F:\, G:\) at your external computer which you can now access to copy files for updates or to copy stored spectra to your computer.

5. If no computer link could be established then restart the external computer again and press repeatedly <F8> to enter the Microsoft Window 98 Start Menu. Press <5> to select the Dos prompt level.

6. Power down the device to quit the PC-Link-program. 8.2 Using the USB-Stick For data exchange with other computers and software updates an USB stick can be connected to the USB port of the system. Before booting up83. the system the USB-Stick must inserted correctly into the USB slot. Access to the USB-stick can be done by the means of an external keyboard and by editing <d:> usually.

Sometimes there is no access to the USB-Stick at first time and the following German error message84 is shown: Unzulässiger Datenträgertyp beim Lesen von Laufwerk D: Quit the error message by editing <w> like (W)iederholen (repeat) to get access to <d:> again.

Attention: Before putting the USB-stick into an external computer, the <MKSHEET> (Make Sheet) command has to be executed first as a MS-Dos command on the active storage directory of the USB-Stick to convert the *.int files of any measurement series into a file data.txt, which afterwards can be read by table calculation programs like Excel on an external computer. All existing *.int files on this subdirectory will be converted to the new created file data.txt, so that it is advisable to delete eventually remaining older *.int files beforehand.

82 Please recognize that there might be some config.xxx files on your computer in the root directory (usually c:\) depending on the operating system you may have for initial starts or the later change to MS-DOS. In such a case all files named config.xxx should be altered accordingly with the above mentioned line. Please make sure that also the lastdrive command is giving enough figures for the deviated disks on your computer when connecting to the mIRoPort. Always place the new command at the end of the config.xxx files to avoid conflicts with other commands redirecting drives. Then either from the Windows Explorer or alternatively starting the MS-DOS mode, updates for the unit can be easily copied. 83 The USB stick will be recognized by the MS-DOS system at time of booting only ! When the USB stick is disconnected while system operation and connected again then it will not recognize the USB stick again. The unit must be restarted again. 84 German based MS-DOS is used.

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