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Fully automated Pensky-Martens Flashpoint Tester

acc. to ISO 2719 (Method A and B) ASTM D 93 (Method A and B) IP 34 (Method A and B)

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Grafik 12-0770W

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TABLE OF CONTENTS
Grafik 12-0770W _________________________________________________________________________________ 3

1.
1.1 1.2 1.3 1.4

Description of the device________________________________________________________7


Introduction _______________________________________________________________________7 Connection values of the PMA-4 and device properties _______________________________8 Weight and dimensions of the PMA-4________________________________________________8 Components_______________________________________________________________________9

Graphic: 12-0770 B _____________________________________________________________________________ 10

2.
2.1 2.2

Operation ___________________________________________________________________12
Location _________________________________________________________________________12 Bringing into service ______________________________________________________________12

2.2.1 Mounting ______________________________________________________________________________ 12 2.2.1.1 Mounting of the Multi-function-head ___________________________________________________ 12 Grafik: 12-0770 A_______________________________________________________________________________ 13 2.2.1.2 Mounting of the test cup holder _______________________________________________________ 14 2.2.2. Switch -on _____________________________________________________________________________ 15 2.2.3 Clean the test insert ____________________________________________________________________ 16

2.3

Menu Guidance ___________________________________________________________________17

2.3.1 Status display __________________________________________________________________________ 17 2.3.2 Programs______________________________________________________________________________ 25 2.3.3 Sample-ID _____________________________________________________________________________ 26 2.3.4 Choice of the ignition-system to be used ___________________________________________________ 27 Graphic 12-0770 X _____________________________________________________________________________ 31 2.3.5 Expected flashpoint _____________________________________________________________________ 34 2.3.6 Temperature of the block ________________________________________________________________ 35 2.3.7 Setting date and time ___________________________________________________________________ 37 2.3.8 Setting barometric pressure correction ____________________________________________________ 37 2.3.9 Setting LCD brightness__________________________________________________________________ 38

3.
3.1.

Test conduct_________________________________________________________________39
Program selection_______________________________________________________________39
Search-Programs (SEARCH-hiVis, SEARCH-LoVis) ________________________________________ 39 RAPID-Programs (RAPID-loVisc, RAPID-hiVisc)____________________________________________ 39 USER-Programs (USERPROGRAM1. USERPROGRAM2) __________________________________ 40 Programs for Method B (EN-B-lowVisc, D93-B-loVisc, EN-B-highVis, D93-B-hiVisc) ____________ 40 Programs for Method A (EN-A-lowVisc, D93-A-loVisc, EN-A-highVis, D93-A-hiVisc) ____________ 40 Flashpoint determination of bitumen samples_______________________________________________ 41 Flash point trial with the little cup pPM 12-1777 _____________________________________________ 42 3.1.1 3.1.2 3.1.3 3.1.4 3.1.5 3.1.6 3.1.7

3.2 3.3

Program start _____________________________________________________________________46 Program tables ___________________________________________________________________52

3.3.1 Program table __________________________________________________________________________ 52 C 3.3.2 Program table __________________________________________________________________________ 53 F 3.3.3 Programmparameter in __________________________________________________________________ 54 C 3.3.4 Programmparameter in __________________________________________________________________ 56 F

3.4

Barometric Correction_____________________________________________________________58
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3.5 3.6

Printer Protocol of a Test Run______________________________________________________59 Validity of found flashpoints _______________________________________________________60

4.
4.1 4.2 4.3

Parameters__________________________________________________________________62
Program parameter _______________________________________________________________62 Device parameter _________________________________________________________________70 Changing of Parameters ___________________________________________________________74
Changing the program parameters ________________________________________________________ 74 Changing of device parameters __________________________________________________________ 75 Printing of Program parameters __________________________________________________________ 77 Printing of device parameters ____________________________________________________________ 78

4.3.1 4.3.2

4.4

Printing of Parameters ____________________________________________________________77

4.4.1 4.4.2

5. DISPLAY HISTORY and PRINT HISTORY _________________________________________79 6. 7.


8.1

Safety mode _________________________________________________________________81 Maintenance ________________________________________________________________82


Calibration _______________________________________________________________________84

8. Trouble shooting ________________________________________________________________84


8.1.1 Calibration of the Pt100-sensor ___________________________________________________________ 84 Drawing 12-0770D______________________________________________________________________________ 84 8.1.2 Calibration of the PMA-4 with Reference-Materials __________________________________________ 88

8.2

Trouble Shooting _________________________________________________________________90

* Display does not work when switched on _________________________________________________________ 90 * Display does not show any symbol ______________________________________________________________ 90 * Gas Ignition does not work _____________________________________________________________________ 90 * Gas flame is unstable__________________________________________________________________________ 90 * Electric Ignition does not work __________________________________________________________________ 90 * No indication of sample temperature _____________________________________________________________ 90 * PMA-4 does not start after pressing RUN-Key ____________________________________________________ 91 * Stirrer does not work __________________________________________________________________________ 91 * Hose-coupling is to tight to the stirrer and the lid sticks? ____________________________________________ 91 * Opening mechanics of Lid and Shutter does not work ______________________________________________ 91 * Aging problems of the Electric Ignitor ____________________________________________________________ 91 * Opening mechanics for shutter does not slide freely. _______________________________________________ 91 Drawing 12-0770C______________________________________________________________________________ 92 * Results of Reference material s do not comply with the certificate____________________________________ 94 * Cleaning the thermocouple of the multisensor _____________________________________________________ 94

8.3

Replacing the electric ignition _____________________________________________________95

9.

Spare Parts _________________________________________________________________97

GENERAL SAFETY RECOMMENDATIONS _________________________________________98

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Introduction

Thank you for purchasing the new PMA 4 which with its unique features offers a completely new dimension of sample changes. Traditional devices require ignition, moving of the lid and indication all as separate time consuming steps, whereas the PMA-4 does all this for you in one go- all it takes is a gentle push of the Multifunctions- head and you have done everything at once! The advantages are obvious: In most cases more than one test insert can be filled ready for change at the same time, covered with lids and multifunction detectors- all set for change. The actual sample change after a completed test is thus not only faster but also requires less of the users attention since this is all done practically as the device goes along. This of course means less errors- (is the stirrer set properly? ignition connected? sensor inserted? etc.) and the user can direct all his or her attention to the important tasks. But the improvements dont stop just here. The new electric ignition system offers another surprise: Despite the compact size of the device it contains an intelligent ignition control. You will be reminded if the ignition needs changing; the ignition itself is operated at its optimum and therefore lasts much longer- protected from unnecessary wear and tear. Especially the voltage fluctuations common to the industry in 24 hour operations are now perfectly absorbed. Of course you can run your PMA-4 with a gas ignition as well. The electric ignition is here used as an aid to ignition. This comes in handy when doing reference tests and for general assumptions. The electric ignition controls and ignites the gas flame at start of test or reignites it automatically in case of extinction. Please ensure a low pressure gas supply to avoid problems at setting.

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1.2

Connection values of the PMA-4 and device properties : 230 V 10%, 50/60 Hz or: 115 V 10%, 50/60 Hz (alternating) : 10 A m 1 1/4` for 110/115V 4 A m 1 1/4` for 220/230V : 900W : about +40 to 350 C C (without external sample precooling) from about +20 (with external precooling) C : error +/- 0.3% full scale : 0-400 C 400 C 200 C 100 C (0.1+ 0.0017 * T(K)) 0.8 C 0.5 C 0.3 C

Mains voltage

Fuse

Power Flashpoint range

Barometric Pressure Sensor Temperature sensor

Stirrer speed Gas Data

: 60 to 250 rpm ( 1rpm) : Propan/Butan or Natural Gas, max. 0,05 bar serial RS 232 for Printer (Option 25-0282) serial RS 232 for PC a) for service to update program without having to open control unit. (Download-interface) b) for PC control/ evaluation

Transportation conditions:

temperature: -50 to +50 C relative air humidity: 90% vibrations: 8 - 120 Hz at 30m/s2 max

1.3

Weight and dimensions of the PMA-4

WxHxD = 230 x 460 x 390, Weight: 8 kg

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1.4

Components

Front of the PMA-4 1 2 3 4 5 6 7 8 9 10 11 Multifunction head Multi-Detector for flashpoint and temperature Flexible stirrer coupling (12-0780) Stirrer Test insert with lid (12-0777) Ignition (Gas -or electric ignition) Display Cursor-keys STOP-key RUN (START)-key ENTER-key

Rear of the PMA-4 12 13 14 15 16 17 18 On/Off- switch Gas connection (for external gas supply) Connecting cable for Multi-Sensor Control cable for stepper motor Printer - Interface (RS 232) PC-Interface (RS 232) Alternating switch 230V/115V

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Graphic: 12-0770 B

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2. 2.1

Operation

Location

Please make sure that the PMA-4 stands freely because of heat emission (flashpoint range up to 350 C). The device should not be submitted to draft. Draft can bias the measured flashpoint and influence the control of the gas flame function. If you place more than one PMA 4 next to each other you should separate them with an appropriate screen since their ventilation in the case of temperature increase and flashpoint can influence their performance. 2.2 Bringing into service

2.2.1 Mounting 2.2.1.1 Mounting of the Multi-function-head To ensure safe transportation the PMA-4 is divided into bottom part (control device) and upper part (Multi-Function-Head). Mount the column on the bottom part (acc. to drawing 12-0770A) which holds the MultiFunction-Head later on. The column is screwed onto the bottom part as shown in drawing 12-0770A with the partition pointing to the left. Mount the Multi-Function-Head on the bottom part by inserting the bolt into the guide of the column. Make sure that the pin clicks into place. Turn the Multi-Function-Head aside to the right and click it into place. Connect plug for step motor control and the Multi-Detector at the back of the device. The ignitor is mounted according to 2.3.4
Choice of the ignition-system to be used.

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Grafik: 12-0770 A

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2.2.1.2

Mounting of the test cup holder

The test cup holder is mounted on the left of PMA4 rear side. The 2 screws at the left of the rear panel are loosened and fixed again together with the holder.

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2.2.2. Switch -on Please ensure before connecting the device to the mains that the stated voltage on the back matches the mains or adjust accordingly if necessary. The respective voltage has to be set at both switches at the back of the PMA-4. Connect printer (if existent) to the printer interface at the back of the PMA-4. Printer must be switched on prior to switching on the PMA-4 to ensure that the head line with actual date etc. will be properly printed. When using a gas ignition connect external gas supply to the back of the device. Insert the Multi-Detector into the test insert (cup and lid). Position test insert into the PMA-4 and turn the Multi-Function-Head towards you so that the connection between Multi-Detector and stirrer is made. Now you can switch on the PMA-4. After a brief self test the device gives a quadruple signal to indicate readiness. Following introduction menu is displayed:

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actual sample temperature

status

actual program

sample name temperature of the heater block selected igniter (E=electric, g=gas)

expected flash point

If PMA-4 is switched on without the test insert and the indicator and sensor being assembled you will be given the following display: (Test temperature cannot be indicated.)

2.2.3 Clean the test insert The crucible and its lid are protected against corrosion through wax coating. The wax layer can lead to a wrong flash point. Clean the entire testing apparatus with a dry cloth before using the first time.

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2.3

Menu Guidance

Pressing <ENTER> key will position the blinking cursor on the display at the decimal digit of the flashpoint preselection. With the keys < Arrow right> and <Arrow left> you can get from one menu point to the other. With the keys <Arrow up> and <Arrow down> you select within the respective menu and confirm with <Enter>. If you move the cursor keys to a menu point and confirm with <ENTER> without having made a choice yet the display will explain the respective menu points. If you dont put anything in while being in a submenu within 10 sec the device will automatically return to the initial position. Pressing the <ENTER>key will prompt the following display

The flashing cursor is on the decimal digit of the flashpoint preselection.

2.3.1 Status display Following status displays are possible: The respective explanation is given on display when moving the cursor keys to the menu point status display and once again pressed <ENTER>.

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STOP: The device is in the STOP-modus, no heating

When in STOP- mode the <STOP>key switches the stirring motor on or off.

STOPhead: Safety feature If the Multifunctions- Head is moved out during the running test the device aborts the program immediately.

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STOPgas: Safety feature If the magnetic valve for gas ignition is opened and the indicator for ignition flame control is not given a signal for an ignition flame after 50 sec the magnetic valve automatically turns off again and the program is at STOP. This prevents the emission of too much gas. Additionally the test is stopped after the gasflame was switched on and detected by the gasflame detector, for example when during the test cycle no gasflame is detected for 50sec. The electric ignitor always glows during the test cycle for faster switching on the gasflame when it was blown out.

STOPsen: The sensor is not connected or the heating sensor is defective. STOPign: The electric ignition is not connected.

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STOPgrad: A shortcut of the sample Pt100 during a running test is detected.

ATTENTION: The functions STOPgas, STOPhead, STOPign, STOPsen, STOPgrad are printed out. On the display you will only see STOP. You can call up the explanations by moving the cursor to STOP and <ENTER>. RUNNING: A program was started. The device heats up.

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TESTING:

The program was started. The PMA-4 is in its test phase. Flashpoint tests are conducted.

BURN:

The device registered a flashpoint outside the pot. The program is automatically terminated. The test has to be started again with a lower flashpoint preselection.

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FPok:

The device detected a flashpoint. Only if the flashpoint was detected in accordance to the preselected standard, the following message will be given:

FPinval: FPlow: FPhigh:

A flashpoint was detected but it was not within the standard requirements and is either to high or to low with respect to the preselected flashpoint-temperature. FPlow and FPhigh are printed out. On the display appears FPlow or FPhigh.

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A flashpoint found at first immersion or during safety mode (see chapter 6) is invalid (FPinval).

OVERFLO: 20 above the put in temperature of the a nticipated flashpoint the program is C automatically aborted for safety reasons.

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When <RUN> is pressed without a test insert in PMA4 or with turned off head the following error message will be displayed

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2.3.2 Programs Following programs can be chosen: D93-A-loVisc D93-A-hiVisc D93-B-loVisc D93-B-hiVisc EN-A-lowVisc EN-A-highVis EN-B-lowVisc EN-B-highVis RAPID-LoVisc RAPID-HiVisc SEARCH-LoVis SEARCH-HiVis USERPROGRAM1 USERPROGRAM2 Program ASTM D 93 Method A for low viscous samples Program ASTM D 93 Method A for high viscous samples Program ASTM D 93 Method B for low viscous samples Program ASTM D 93 Method B for high viscous samples Program ISO 2719 Method A for low viscous samples Program ISO 2719 Method A for high viscous samples Program ISO 2719 Method B for low viscous samples Program ISO 2719 Method B for high viscous samples Program Rapid (Fast heat- up) for low viscous samples Program Rapid (Fast heat- up) for high viscous samples Search program for low viscous samples Search program for high viscous samples infinitely programmable user program infinitely programmable user program

Details in chapter 3.1 If flashing cursor is positioned on a program and no new program has been selected by the arrow keys you can call up a detailed explanation of the program with <ENTER>.

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Scrolling with the cursor keys will prompt the bottom line: DISPLAY HISTORY PRINT HISTORY PRINT PARAMETER CHANGE PARAMETER PRINT MANUAL : the last 99 results are shown on the display : the last 99 results are printed out : prints the current program parameters : jumps to the SETUP-Menu for the program parameters : a brief manual is printed out

When you press <ENTER>-you will call up the respective function.

2.3.3 Sample-ID You can put in sample-ID and user-ID in this sample-ID menu.

For sample-and user-ID you are given 7 digits which can be used for alphabetical (A to Z) or numerical (0 to 9) signs. If a new user name is put in the header is automatically printed out anew. The four latest used sample names are saved together with all parameters (used program, expected flashpoint) and can be called up again by way of the cursor keys. If the last 3 digits of the sample name are numeric, the sample number is automatically counted up. To activate this function however the device parameter 29 has to be set at 0001. (chapter 4.2). This parameter is set to 0000 by the manufacturer. Example: OEL0001 at 1. test OEL0002 at 2. test and so on.

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2.3.4 Choice of the ignition-system to be used The PMA-4 allows use of an electrical as well as gas ignition. For selection of the ignition please move the cursor to the ignition symbol.

Press <ENTER>-to get to the submenu

Select the used ignition with the arrow keys:

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confirm with <ENTER>.

The selection can be checked with the symbol appearing on display:

Electric igniter

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Gas ignitor

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ELECTRIC IGNITION The electric ignition is put into the ignition holder and fixed with a knurled head screw. Both the ignition plugs are connected into the sockets at the upper surface of the device. NOTE: Before plugging in the ignition makes sure that your knurled head screw is nearly loose since otherwise the ignition coils could be damaged.

Menupoint ELECTRIC IGNITOR contains a submenu for the exchange of the electric ignition after ageing or short circuit. Please see for details: 8.3 Replacing the electric ignition . GAS IGNITION If you use the gas ignition, the electric ignitor has to be used as an auxiliary ignitor in a special position at the right side of the Multi-Function-Head. The electric ignitor works to ignite the gas ignition in the first place later on. Attention: Make sure that the ignitor cables and the tubing will not interfere each other when moving the Multi-Function-Head.

Before starting a test conduct a manual immersion test before turning on the gas ignition. Therefore press <arrow up> and keep it pressed until the escaping gas is ignited by the electric ignition. (The opening of the magnetic valve is indicated by a cracking sound.)

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Graphic 12-0770 X

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This ensures that the gas has been in all hoses before the test. The gas valve can simultaneously be set so, that the flame reaches an average of 4mm according to standard by aid of a screw driver. To shorten the initial ignition process the valve can be carefully opened a tiny bit for a very short period of time. SAFETY FUNCTION: If the flame indicator registered no ignition flame within 55 sec the magnetic valve automatically switches off.

ATTENTION: PLEASE USE FOR GAS-CONNECTION ONLY TUBES WHICH ARE ADMITTED FOR GAS-OPERATION!

ATTENTION:

If the device realizes that there is no electric ignition connected after a program was started the program returns to STOP and following malfunction note is given:

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2.3.5 Expected flashpoint With the PMA-4 it is possible to detect flashpoints up to 350 C. To change the preselection move the cursor to the flashpoint preselection, set the requested value with the arrow keys and confirm with <ENTER>. If you press <ENTER>-without changing the flashpoint preselection an explanation is given on display:

The expected flashpoint can be altered even while the program is running. Just press the <ENTER>-key in the running program and the cursor will flash at the ten digit of the flashpoint preselection. You can now alter your preselection and confirm with <ENTER>. If the program has already proceeded however to the test range (ignition started) and you altered the preselection to a point below the test range the ignition is turned off again.

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2.3.6 Temperature of the block The temperature of the heating block is expressed on display via following symbols:

Block has cooled down to the temperature given by the respective parameter.

Program has been started. Block is heating. (A bar means about 5 min until reaching test phase)

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Flashpoint was found, ventilator turned on and the block is cooling down.

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2.3.7 Setting date and time By setting testcode 9993 in program parameter 1 of any program actual date and time can be set:

2.3.8 Setting barometric pressure correction Barometric pressure can be displayed by setting program parameter 1 in any program to 9991.

If there is any correction necessary it has to be inserted into device parameter 4. See chapter 4.3.2 Changing of device parameters

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2.3.9 Setting LCD brightness Brightness can be adjusted by pressing and holding <STOP> for 5sec in the opening menu.

lcd-bright.tif

The brightness can be altered using <arrow up> and <arrow down>. Changes are confirmed with <ENTER>.

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3. 3.1.

Test conduct

Program selection

Select the program according to the sample under test and the standard to be used. Also test with respect to the various test methods of the standards such as e.g. Methods A and B in ISO 2719 and ASTM D93. We also differentiated the samples depending on their viscosity so that the heating control can reach the required gradient of 5-6 C/min or 1-1 .5 C/min in a very short period of time. Example: A low viscous sample shall be measured acc. to ASTM D 93 Method A. Select program D93-A-loVisc (ASTM low viscosity). 3.1.1 Search-Programs (SEARCH-hiVis, SEARCH-LoVis) The Search-Programs are used for preliminary flashpoint detection of unknown samples. Attention: The preselected flashpoint must be 350 in this case C The temperature gradient in this program will be 8.5 C/min, the ignition dips every 5 into C the cup. Test start is preset to EFLP-320 by parameter 16. C This means that expected flashpoint must be set to 350 C. 3.1.2 RAPID-Programs (RAPID-loVisc, RAPID-hiVisc) This program is useful especially when very high flashpoints are to be detected for internal use because this is not a standard method of test. The temperature gradient will initially be 8.5 bu t will be transferred into the standardized C gradient of 5.5 approx. 50 before the expected flashpoint. C C This program safes test time and very often shows good compliance with the long lasting standard method.

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3.1.3 USER-Programs (USERPROGRAM1. USERPROGRAM2) The USER-Programs are the only programs that can permanently be modified by the user. Only when switching from to and reverse also these programs will be initiated. C F USER Programs are preset with Search programs for unknown flash points according to standard requirements. Preselection of expected flash point must be at 350 like in the other search programs. C First dip-in of the ignitor will be at 30 Accord ing to ASTM the first dip-in shall be at 20 C. C (5 above the starting temperature of 15 For t his program parameter 16 has to be set to C C). 3300. In USER1 program the sample is heated at 5-6 C/min, dip-in cycle is 2 stirrer speed C, 120rpm. In USER2 program the sample is heated at 1.3 C/min, dip-in cycle is 2 stirrer speed C, 250rpm.

3.1.4 Programs for Method B (EN-B-lowVisc, D93-B-loVisc, EN-B-highVis, D93-BhiVisc) Method B is requiring stirrer speed of 250 RPM and gradient 1 to1.5 C/min. Programs are divided for high and low viscous samples. 3.1.5 Programs for Method A (EN-A-lowVisc, D93-A-loVisc, EN-A-highVis, D93-AhiVisc) Stirrer speed is 120 RPM. Gradient is 5.5 C. Test conduct according to EN ISO 2719 is the same like in the valid ASTM standard. That is why the EN and ASTM programs at present are identically.

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3.1.6 Flashpoint determination of bitumen samples The special conditions when determining the flashpoint of bitumen samples require a special program. Bitumen samples are inserted only at higher temperatures (softening point of bitumen). The test is usually started at such temperatures as well. After the test is finished the sample has to be removed from the device at higher temperatures. Following parameters are important when conducting tests with bitumen: P03: Initial temperature difference P04: Starting temperature difference P11: Temperature at which fan is switched off P23: Heating to the temperature set in P11 - 0/1

To reach the requested temperature ramp quickly it is necessary to modify the respective starting parameters. Therefore set the parameters 03 and 04 in the parameter set of the used program to a higher value. This value depends on the starting temperature of the sample and the requested gradient. With a sample starting temperature of 200 the P03 : should be at 1700 and the P04 at C 1500. Parameter 11 designates the temperature at which the fan is turned off in a regular program. If parameter 23 is set to 0001 the sample is cooled to the temperature stated in P11. The fan will switch off then and the sample be kept at that temperature. If the test with a bitumen sample is started at room temperature the stirrer will move only 10 prior to the given temperature in P11. C Basically every program can be used as a bitumen program after programming the parameters. If bitumen are tested very often you should consider using one of the USERprograms for it. Since there exist no standards for bitumen you should be certain about the temperature ramp and the stirrer speed to conduct your bitumen test properly. If the low gradient (1.3 C/in ) is chosen the test will take very long and possibly no flashpoint be found. For recommendations regarding your bitumen program see program table. This is a program with a starting temperature of 200 temperature ramp 5,5 stirrer C, C, speed of 120 rpm.

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3.1.7 Flash point trial with the little cup pPM 12-1777 The test insert for little sample quantities 12-1777 consists of: * 12-1785 pPM cup * 12-1786 pPM cover * 12-1787 Multidetector for pPM In the mini cup, very slight sample quantities can be tested. In a sample quantity necessary (in the Pensky-Martens cup by ca. 70 ml) can be reduced here the sample volume (depends on the sample to be tested) on to 2ml. That saves considerable costs in expensive samples (for example perfume oil in the fragrance industry). Also in the disposal of the tested materials is saved. The mini cup does not correspond to the valid standards. Therefore flash points that are determined with this cup cannot be used as a reference. It is however possible to set up company-internal standards and to reduce therewith the largest part of the internal inspection on a least sample quantity. Dependent upon the samples to be tested, it is possible to test sample quantities from 2ml to 15ml. A reduction of the sample quantity leads frequently to an increase of the found flash points. In sample quantities of 5-15 ml, usually similar flash points are found like in the normal cup. A sample quantity of 2 ml can already critically become in certain samples and flash points are found, that are strongly increased in accordance to the normal flash point. The abundance heights designation in the mini cup corresponds to the abundance heights designation in the normal cup and to an abundance quantity of ca. 7 ml. The mini cup is filled also up to this height, the steam room is equally large in both procedures. Pure samples become, therefore no material mixtures, tested, could come it therefore to the determination of very similar flash points. In the test of material mixture, the quantity of the sample to be used is dependent on the share of the volatile substances in the mixture. Before flash points with the mini cup are used as an internal standard, in each case a reference trial with the normal cup should be carried out.

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According to state of the sample to be tested (for example viscosity) and the quantity of the fluid to be tested, it can be necessary to adjust the heating parameters P03 (initial temperature difference) and P04 (start temperature difference). To this purpose, one of the both USER-programs can be used so that the selected parameters remain permanently stored. In all other programs, the program parameters will be set back to the delivery status after turning off / switching on. For highly fluid samples, the inflow parameters P03: 1000 and P04: 0900, for high viscous samples P03: 1200 and P04: 0900 for a temperature increase in the sample of 5-6 C/m in determines. The other parameters should correspond to the attitudes of the program desired (for example stirrer speed, submersion cycle). The correctness of the selected inflow parameters can be controlled in a short (1 minute) print of the temperature increase of the sample, by setting of the program parameter 01 to 0998. The sample name, the sample composition, the found flash point, the air pressure in the flash point test and the corrected flash point will be indicated in the test report. Moreover the sample quantity, the related ignitions (gas / or electric ignition), method A or B and possibly the changed heating parameters, should be indicated. For repeatability and reproducibility no values are available To the security for a sample, always at least two flash points should be determined.

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Setting a flash point correction between mini-cup and standard cup: Precautionary we would like to point out that there is no possibility to set a general or universal correction formula for converting mini cup flash point values into standard cup flash point values. The responsibility for the application of this correction formula and calculated flash points is solely on the user. Sometimes it seems that there are correlations for certain product groups. For safety reasons a correction formula only should be applied after verifying the result on the basis of tests under standard conditions with a standard cup. An automatic correction can be done by using program parameters 24 to 26 with a predetermined correction formula. This correction formula must be determined by doing parallel flash point tests of samples in mini cup and in standard cup. P24: Correction off/on (0/1) P25: Coefficient a (E-3) P26: Coefficient b (E-3)

Correction function is switched on by setting program parameter 24 to 0001. According to the abstract formula: y=a*x + b coefficients a and b are inserted into program parameters 25 and 26, where: y= corrected flash point x= measured flash point Flash point correction is always done from the barometric corrected flash point values. The formula is given into the parameter set as follows:

ATTENTION: This formula is ONLY an EXAMPLE. Formula: corrected value= 1.106*(detected flash point) 2.292 Parameters are set as follows: P24=0001 P25=1106 P26=-2292 Parameter 26 can be set to negative and positive values. A change between (+) and (-) can be done by moving with the cursor into the field in front of the number and changing with <arrow up> or <arrow down>.
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Corrected flash point appears as FPcrd in the printout or on the main display. Another information about the correction is not given, additionally it is only possible to print out the program parameters with the preset correction factors.

PETROTEST INSTRUMENTS DAHLEWITZ PMA4-Version 05.06.2006 Device No 41000000 OPERATOR XXXXXXX


SAMPLE NAME DODECAN PROG NAME D93-A-LoVisc EFP C 083 SAMPLE FPcor C C 082.1 82,0

Tel:033708-56300 Date 06.06.2006

FPcrd BAP C kPa 88,5


101.7

STIR rpm 0120

GRAD C/m 005.7

IGNI G/E E

STATUS TIME H:M FPok 06:14

When the correction formula shall be for permanent use, a USER program should be preset with the correction parameters, as in the other programs the parameters are initialized after switching the unit off/on.

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3.2

Program start

After applying sample to the test cup, putting the lid on and inserting the Multi-Detector the test cup is seated into the PMA-4 and the Multi-Function-Head brought into position. ATTENTION: WORKING WITH GAS IGNITION: Before using the gas ignition for the first time it is recommended to conduct a manual test to make sure that the gas has reached the tip of the ignition jet. Therefore press the key <arrow up> in the <STOP>-Status and keep it pressed until gas is escaping and ignited by the electric ignition. Release key then and let the device conduct an immersion test now. After the first installation of the customers gas supply the tubes are not completely filled with gas. Depending on this the gas can take more or less time to come out of the ignitor. To make this quicker you can increase the flowrate (Attention of coming out the larger flame!!). For this it is practical at first to find with a screw driver carefully clockwise the closed endpoint of the adjustment screw (to adjust the gas flow rate) (see graphic 12-0770X). Then open the flow by about one turn of this screw against clockwise. Press the key <arrow up> in the <STOP>-Status and keep it pressed until gas is escaping and ignited by the electric ignition. Attention: If the flowrate is too high the gas stream cools the electric ignitor. In this case the coil of the electric ignitor looks less lighten depending on the gas cooling: the gas ignitor will never be switched on. After selecting the requested program, the flashpoint preselection and the ignition the <START>-key can be pressed. You can go ahead even if shortly after pushing the Multifunctionshead the sample temperature is not yet displayed. If head has not clicked into place and the contact to the sensor not established following message is given:

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Once the program is started you will have following display:

After program start the ignitor will dip in once (only mechanical test, no active ignitor) By this dip-in a possibly open cover is closed. When the safety function is activated the active ignitor will dip in and a too low flash point (of a wrong sample) will be detected. After this test the ignitor remains glowing for about 30s, for determination of reference voltage for ignitor life time control. When the safety function is activated then in 10 intervals safety flash point tests are carried C out. see also chapter 6. Safety When the safety function is switched off the electric ignitor will only glow for 30s after test start for detection of reference voltage.

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This ignitor movement should close an open lid and prevent an undefined position of the ignitor. Depending on the selected program the instruments gets into the test phase approx.. 20 C before the preselected flashpoint

The cup-symbol will be blinking left from the preselected flashpoint. Independent from the flashpoint preselection it is possible at any time (until 5 C/9 before F test range) to initiate a flashpoint test with the key <arrow up>. If a flashpoint was found the program automatically stops and shows the barometric pressure corrected and rounded flashpoint on display:

The device automatically cools down.

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If the cup is left in the device meanwhile the PMA-4 signals the end of the cooling phase and the ventilator is automatically turned off. The cooling-phase is finished if the set temperature in parameter 11 is reached in heater and sample. When the cup was remaining in the heater section after a test, the PMA-4 will give a short audible signal when it has cooled down to 35 C. If the cup is taken out instead, the ventilator is automatically turned off as soon as the temperatureset in parameter 11 is reached at the heater block. This will be at 35 in all programs. C To speed up readiness for the next test, it is recommendable to remove the warm testcup from the heater section as soon as possible. Compliance or non-compliance with the standards If a flashpoint was found, the PMA-4 is intelligent enough to sort out if this result was within the requirements of the selected standard or not. The following display:

The detected flashpoint was found in accordance with the relevant standard. On the display appears always the corrected and rounded flashpoint.

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It is also possible to call the uncorrected and corrected flashpoint on display. To do this move the cursor to FPok and confirm pressing the <ENTER> key. Following display is given:

The uncorrected, corrected (to barometric pressure) and corrected rounded flashpoints are displayed.

Flash point to high Flash point to low

The detected flashpoint was not detected in accordance with the standard. It was either too high or too low.

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The following information will be at the display when you hit the <ENTER> key and move the cursor to the status position:

If no flashpoint was detected, the PMA-4 will automatically switch off 20 above the C preselected flashpoint.

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3.3

Program tables

3.3.1 Program table C

Program
EN-A_lowVisc EFLP<=110 C EFLP>110 C EN-A-highVis EFLP<=110 C EFLP>110 C EN-B-lowVisc EFLP<=110 C EFLP>110 C EN-B-highVis EFLP<=110 C EFLP>110 C RAPID-loVisc EFLP<=110 C EFLP>110 C RAPID-hiVisc EFLP<=110 C EFLP>110 C SEARCH-loVis SEARCH-hiVis USERPROGRAM1 =SUCH (Norm) USERPROGRAM2 =SUCH (Norm) D93-B-loVisc EFLP<=110 C EFLP>110 C D93-B-hiVisc EFLP<=110 C EFLP>110 C D93-A-loVisc EFLP<=110 C EFLP>110 C D93-A-hiVisc EFLP<=110 C EFLP>110 C

Stirrer speed
120 rpm

Gradient
5.5 C/min

Overflow
EFLP+20 C

Dip-in start
EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22C EFLP-22 C EFLP-22C EFLP-22 C EFLP-22C EFLP-22 C EFLP-22C EFLP-22 C EFLP-22 C EFLP-320 C EFLP-320 C EFLP-320 C EFLP-320 C EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22 C EFLP-22 C

Dip-in cycle
each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C each 5 C each 5 C each 1 C/2 C each 1 C/2 C each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C each 1 C each 2 C

120 rpm

5.5 C/min

EFLP+20 C

250 rpm

1.3 C/min

EFLP+20 C

250 rpm

1.3 C/min

EFLP+20 C

120 rpm

8.5 u.5.5 C/min 8.5 u.5.5 C/min 8.5 u.5.5 C/min 8.5 u.5.5 C/min 8.5 C/min 8.5 C/min 5.5 C/min 1.3 C/min 1.3 C/min

EFLP+20 C

250 rpm

EFLP+20 C

120 rpm 250 rpm 120 rpm 250 rpm 250 rpm

EFLP EFLP EFLP EFLP EFLP+20 C

250 rpm

1.3 C/min

EFLP+20 C

120 rpm

5.5 C/min

EFLP+20 C

120 rpm

5.5 C/min

EFLP+20 C

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3.3.2 Program table F


Programm
EN-A_lowVisc EFLP<=230 F EFLP>230 F EN-A-highVis EFLP<=230 F EFLP>230 F EN-B-lowVisc EFLP<=230 F EFLP>230 F EN-B-highVis EFLP<=230 F EFLP>230 F RAPID-loVisc EFLP<=230 F EFLP>230 F RAPID-hiVisc EFLP<=230 F EFLP>230 F SEARCH-loVis SEARCH-hiVis USERPROGRAM1 =SUCH (Norm) USERPROGRAM2 =SUCH (Norm) D93-B-loVisc EFLP<=230 F EFLP>230 F D93-B-hiVisc EFLP<=230 F EFLP>230 F D93-A-loVisc EFLP<=230 F EFLP>230 F D93-A-hiVisc EFLP<=230 F EFLP>230 F

Stirrer speed
120 rpm

Gradient
10 F/min

Overflow
EFLP+36 F

Dip-in start
EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-576 F EFLP-576 F EFLP-576 F EFLP-576 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F EFLP-40 F

Dip-in cycle
each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F each 5 F each 5 F each 2 F F/5 each 2 F F/5 each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F each 2 F each 5 F

120 rpm

10 F/min

EFLP+36 F

250 rpm

2 F/min

EFLP+36 F

250 rpm

2 F/min

EFLP+36 F

120 rpm

15 &10 F/min 15 &10 F/min 15 &10 F/min 15 &10 F/min 15 F/min 15 F/min 10 F/min 2 F/min 2 F/min

EFLP+36 F

250 rpm

EFLP+36 F

120 rpm 250 rpm 120 rpm 250 rpm 250 rpm

EFLP EFLP EFLP EFLP EFLP+36 F

250 rpm

2 F/min

EFLP+36 F

120 rpm

10 F/min

EFLP+36 F

120 rpm

10 F/min

EFLP+36 F

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3.3.3 Programmparameter in C
Programm/ EN-AlowVisc EN-AhighVis EN-BLowVisc EN-BhighVis D93-ALoVisc D93-AhiVisc D93-BLoVisc D93-BhiVisc

Parameter 01: Test function 02: initial heating % 03: initial heat. diff 1/10 C 04: starttemp diff 1/10 C 05: 1.samplegradient 1/10 C 06: 2.samplegradient 1/10 C 07: grad1-->grad2 1/10 C 08: block nom value 1/10 C 09: overflow 1/10 C 10: stirrer speed rpm 11: threshold fan 1/10 C 12: STOP after flashpoint 13: testcycle a 1/10 C 14: testcycle b 1/10 C 15: EFLP threshold 1/10 C 16: start testcycle 1/10 C 17: FP logic 0/1 18: max. sample temp 1/10 C 19: Safety mode (1/10dgC/F) 20: NT-power % 21: calibration program 22: (0) Unused 23: preheating of bitumen 24: (0/1) Correction off/on 25 : (E-3) Coefficient a 26 : (E-3) Coefficient b 27 : (0) Unused 28: print cycle (sec)

0000 0090 1300 1050 0055 0055 0000 0000 0200 0120 0350 0001 0010 0020 1100 0220 0001 3750 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 1600 1000 0055 0055 0000 0000 0200 0120 0350 0001 0010 0020 1100 0220 0001 3750 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0300 0250 0013 0013 0000 0000 0200 0250 0350 0001 0010 0020 1100 0220 0001 3750 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0400 0300 0013 0013 0000 0000 0200 0250 0350 0001 0010 0020 1100 0220 0001 3750 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 1 300 1050 005 5 005 5 0000 0000 0200 0120 0350 0001 0010 0020 1100 0220 0001 375 0 1300 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 1600 1000 0055 0055 0000 0000 0200 0120 0 350 0001 001 0 002 0 11 00 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0300 0250 0013 0013 0000 0000 0 200 0250 0350 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0400 0300 0013 0013 0000 0000 0200 0250 0350 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0000 0060

D93-A-loVisc = EN-A-lowVisc D93-A-hiVisc = EN-A-highVis D93-B-loVisc = EN-B-lowVisc D93-B-hiVisc = EN-B-highVis

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Programm/ Parameter 01: Test function 02: initial heating % 03: init. heat. diff 1/10 C 04: starttemp diff 1/10 C 05: 1.samplegrad. 1/10 C 06: 2.samplegrad. 1/10 C 07: grad1->grad2 1/10 C 08: block nom value 1/10 C 09: overflow 1/10 C 10: stirrer speed rpm 11: threshold fan 1/10 C 12: STOP after flashpoint 13: testcycle a 1/10 C 14: testcycle b 1/10 C 15: EFLP threshold 1/10 C 16: start testcycle 1/10 C 17: FP logic 0/1/2 18: max.sample temp1/10 C 19: Safety mode (1/10dgC/F) 20: NT-power % 22: (0) Unused 23: preheating of bitumen 24: (0/1) Correction off/on 25 : (E-3) Coefficient a 26 : (E-3) Coefficient b 27 : (0) Unused 28: print cycle (sec)

SEARCHLoVis

SEARCHhiVis

RAPIDLoVis

RAPIDhiVis

USER1 SUCH Norm

USER2 SUCH Norm

Bitumen

pPM

Bio Diesel

0000 0090 1800 1500 0085 0085 0000 0000 0000 0120 0350 0001 0050 0050 0000 3200 0000 3750 0000 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 1600 1400 0085 0085 0000 0000 0000 0250 0350 0001 0050 0050 0000 3200 0000 3750 0000 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 1800 1500 0085 0055 0500 0300 0200 0120 0350 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 1600 1400 0085 0055 0500 0300 0200 0250 0350 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 130 0 1050 0055 0055 0000 0000 0000 0120 0350 0001 0010 0020 1100 3200 0000 3750 0000 0040 0000 0000 0000 0000 0000 0000 0060

0000 0050 0300 0250 0 013 0 013 0 000 0000 0000 0250 0 350 0001 001 0 002 0 11 00 3200 0000 3750 0000 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 1700 1500 0055 0055 0000 0000 0 200 0120 2000 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0060

0000 0090 1000 0900 0055 0055 0000 0000 0200 0120 0350 0001 0010 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0060

0000 0065 0800 0700 0030 0030 0000 0000 0200 0250 0350 0001 0020 0020 1100 0220 0001 3750 1300 0040 0000 0000 0000 0000 0000 0000 0060

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3.3.4 Programmparameter in F

Programm/

EN-AlowVisc

EN-AhighVis

EN-BLowVisc

EN-BhighVis

D93-ALoVisc

D93-AhiVisc

D93-BLoVisc

D93-BhiVisc

Parameter 01: Test function 02: initial heating % 03: initial heat. diff 1/10 F 04: starttemp diff 1/10 F 05: 1.samplegradient 1/10 F 06: 2.samplegradient 1/10 F 07: grad1-->grad2 1/10 F 08: block nom value 1/10 F 09: overflow 1/10 F 10: stirrer speed rpm 11: threshold fan 1/10 F 12: STOP after flashpoint 13: testcycle a 1/10 F 14: testcycle b 1/10 F 15: EFLP threshold 1/10 F 16: start testcycle 1/10 F 17: FP logic 18: max. sample temp 1/10 F 19: Safety mode (1/10dgC/F) 20: NT-power % 21: calibration program 22: (0) Unused 23: preheating of bitumen 24: (0/1) Correction off/on 25 : (E-3) Coefficient a 26 : (E-3) Coefficient b 27 : (0) Unused 28: print cycle (sec)

0000 0090 2340 1890 0100 0100 0000 0000 0360 0120 0950 0001 0020 0050 2300 0400 0001 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2880 1800 0100 0100 0000 0000 0360 0120 0950 0001 0020 0050 2300 0400 0001 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0540 0450 0020 0020 0000 0000 0360 0250 0950 0001 0020 0050 2300 0400 0001 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0720 0540 0020 0020 0000 0000 0360 0250 0950 0001 0020 0050 2300 0400 0001 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2 340 1890 010 0 010 0 0000 0000 0360 0120 0950 0001 0020 0050 2300 0400 0001 70 70 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2880 1800 0100 0100 0000 0000 0360 0120 0 950 0001 002 0 005 0 23 00 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0540 0450 0020 0020 0000 0000 0 360 0250 0950 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0720 0540 0020 0020 0000 0000 0360 0250 0950 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

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Programm/ Parameter 01: Test function 02: initial heating % 03: initial heat. diff 1/10 F 04: starttemp diff 1/10 F 05: 1.samplegradient 1/10 F 06: 2.samplegradient 1/10 F 07: grad1-->grad2 1/10 F 08: block nom value 1/10 F 09: overflow 1/10 F 10: stirrer speed rpm 11: threshold fan 1/10 F 12: STOP after flashpoint 13: testcycle a 1/10 F 14: testcycle b 1/10 F 15: EFLP threshold 1/10 F 16: start testcycle 1/10 F 17: FP logic 0/1/2 18: max. sample temp 1/10 F 19: Safety mode (1/10dgC/F) 20: NT-power % 21: calibration program 22: (0) Unused 23: preheating of bitumen 24: (0/1) Correction off/on 25 : (E-3) Coefficient a 26 : (E-3) Coefficient b 27 : (0) Unused 28: print cycle (sec)

SEARCH -LoVis

SEARCH -hiVis

RAPIDLoVis

RAPIDhiVis

USER1 SUCH Norm

USER2 SUCH Norm

Bitumen

pPM

Bio Diesel

0000 0090 3240 2700 0150 0150 0000 0000 0000 0120 0950 0001 0090 0090 0320 5760 0000 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2880 2520 0150 0150 0000 0000 0000 0250 0950 0001 0090 0090 0320 5760 0000 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 3240 2700 0150 0100 0900 0540 0360 0120 0950 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2880 2520 0150 0100 0900 0540 0360 0250 0950 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 2 340 1890 010 0 010 0 0000 0000 0000 0120 0950 0001 0020 0050 2300 5760 0001 70 70 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0050 0540 0450 0020 0020 0000 0000 0000 0250 0 950 0001 002 0 005 0 23 00 5760 0001 7070 0000 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 3060 2700 0100 0100 0000 0000 0 360 0120 3920 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0090 1800 1620 0100 0100 0000 0000 0360 0120 0950 0001 0020 0050 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

0000 0065 1440 1260 0055 0055 0000 0000 0360 0250 0950 0001 0035 0035 2300 0400 0001 7070 2372 0040 0000 0000 0000 0000 0000 0000 0000 0060

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3.4

Barometric Correction

The PMA-4 includes a barometric pressure sensor to enable an automatic barometric correction of the test result. The barometer correction is calculated according to these : korFP = FP + 0,25 ( 101,3 - p) for C korFP = FP + 0,45 ( 101,3 - p) for F On the main display always the barometric pressure corrected and to 0.5 C/1 rounded F flash point is displayed. It is also possible to call the corrected and uncorrected flashpoint on display. To do this move the cursor to FPok and confirm pressing the <ENTER> key. Following display is given:

By setting device parameter 10 to 0001 or 0002 also the uncorrected flash point or the barometric pressure corrected, not rounded flash point can be displayed on main display as a result. In submenu the other values (FPuncor= uncorrected flash point, FPcor, FPcrd) appear accordingly.

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3.5

Printer Protocol of a Test Run Tel:033708-56300 Date 06.06.2006

PETROTEST INSTRUMENTS DAHLEWITZ PMA4-Version 05.06.2006 Device No 41000000 OPERATOR XXXXXXX


SAMPLE NAME DODECAN PROG NAME D93-A-LoVisc EFP C 080 SAMPLE FPcor C C 081.0 80,6 FPcrd BAP C kPa 80,5 102.7 STIR rpm 0120

GRAD IGNI C/m G/E 005.7 E

STATUS TIME H:M FPok 06:14

The head line will be printed when the instrument is switched on and when the operator name was changed. Additionally, the complete head line will be printed out, when the menu for changing operator and sample name will be left with STOP.

SAMPLE NAME PROG NAME EFP ( C) SAMPLE( C)

sample-ID program used expected flashpoint sample temperature at program abort (S TOP or Overflow) uncorrected flash point temperature when flash point found corrected flashpoint, barometric correc tion flash point, barometric pressure corre cted, rounded to the nearest 0,5 C/1 F barometric pressure in kPa stirrer speed rise of temperature in the sample in C/min ignition used (gas / electric) status of a test finished (e.g. FPok, OVFL, STOP) time at test abort

FPcor( C) FPcrd ( C) BAP(kPa) STIR (rpm) GRAD IGN (G/E) STATUS TIME (H:M)

Printer interface: RS 232c, 9600 Baud, 8 bits, 1 Stopbit, no Parity, Connector 25 Pin, Pin no. 2 = ser.-Output, Pin no. 7 = Mass.

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3.6

Validity of found flashpoints

The validity of found flash point always relates to the not (to barometric pressure) corrected, not rounded flash point value, because the temperature of the first dipping in is not (to barometric pressure) corrected, too. In the standards which apply you may find differing statements regarding the validity of found flashpoints. A flashpoint is invalid if it was found upon first immersion.

A flashpoint is too high when it lies more than 28 above the first immersion of the ignition. C

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A flashpoint is too low if it lies 18 or less abo ve the first immersion of the ignition. C

For evaluation program parameter 17 is set: P17=0001 evaluation switched on P17=0000 evaluation off; always FPok

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4.

Parameters

The parameters of the PMA-4 are divided in program parameters and device parameters. Program parameters of all programs except the user programs USER1 and USER2 are initiated at switch-on. Any change undergone in the programs are lost after turn-off. The device parameters are exclusively for service purposes and should at no means be changed.

4.1

Program parameter

Parameter 1: Setting parameter 1 allows various tests and special functions. The values can be printed as follows: Select a program with the cursor in the opening menu and confirm with <ENTER>. Then move the cursor to the program and change with <ENTER> to the sub menu. Select with the cursor keys: DISPLAY HISTORY PRINT HISTORY PRINT PARAMETER CHANGE PARAMETER PRINT MANUAL If PRINT MANUAL is selected and confirmed with >ENTER>, following printout is given:

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PMA4 TEST & SPECIALFUNCTIONS MANUAL


P1 is test & specialfunction parameter For test/special function set parameter value and then press <ENTER> to execute For setup lcd contrast press <STOP> 5 sec. Test/special functions: 0001 1011 1234 2000 4010 4020 4030 9990 9991 9992 9993 9994 0998 0997 0996 0994 0950 flash programming Safety mode on jump to device setup menu print device parameter initialize device parameter initialize userprogram parameter, sample labels & operators name initialize sample labels ignition lifetime test barometer pressure test indicator test setup date/time PT100 adjustment testprint after start, every P25 value & display block / sample temperature display ignition current on test cycle display gasflame indicator on test cycle Display fire indicator Display inspection counter

Parameter 1 will be set to the a.m. value and confirmed with <ENTER>. 0001: A software upgrade can be entered into the PMA-4 from a PC. The Display shows:

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1234: The parameter set of device parameters can be edited. (ONLY FOR SERVICE PURPOSES) 2000: Device parameters are printed out. 4010: Program parameters are initiated, meaning they are reset to delivery mode. 4020: The parameters of the USER program, sample numbers and operator name are initialized. 9991: Test of the barometer pressure display

9993: Setting of date and time

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0998: Test printout of important parameters of the running test Block- and Sample temperature are alternately displayed.

sample temperature

block temperature

The S before the temperature display designates the sample- B the block temperature.

Following values are given on the printer: PROG=ENL EFLP=0080 P1=998 P02=99 P03=1000 P04=0750 P18=0050 P25=0060 nom-BT Block-desired temperature corr-B Correction of heating power act-BTBlock-actual temperature nom-BG Block-desired gradient act-STSample actual temperature nom-SG Sample desired gradient act-SG Sample-actual gradient NT/CT/HP Control values of heating TIME Time of running test

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Parameter 2: Initialheating, % Heating power Heating control parameter The initial heating serves for reaching the standard gradient.

Parameter 3: Initial temperature difference (1/10 C) Heating control parameter The difference between heating block temperature and sample temperature is determined. Example: Parameter 3 is set to 1000. Sample temperature at start is 20 The block heats until 120 C. C with the heating power set in parameter 2.

Parameter 4: Start temperature difference (1/10 C) Heater control parameter The temperature difference between heater block and sample after reaching the initial temperature difference. Once this difference is reached it is switched to "normal" heater control.

Parameter 5: 1. Sample gradient (1/10 C) Desired temperature ramp of the sample

Parameter 6: 2. Sample gradient (1/10 C) Desired temperature ramp of sample Some programs require different desired gradients of sample, for instance the RAPIDPrograms where a temperature ramp of 8,5 (as in S EARCH-Program) is switched to a C ramp of 5,5 (as in STANDARD program). C

Parameter 7: The temperature at which gradient 1 switches to gradient 2 is calculated by subtracting the anticipated flashpoint from the input value. Example: Parameter 7 to 300 (1/10 expected flashpnt: 200 C). C At a sample temperature of 170 gradient 1 is swit ched to gradient 2 and the heating control C adjusted.
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Parameter 8: Desired value of the block when gradient 1 is switched to gradient 2.

Parameter 9: Overflow (1/10 C) Safety function:

When the sample temperature reaches the value which exceeds the anticipated flashpoint in parameter 9 the device aborts and switches to STOP.

Parameter 10: Stirrer speed (rpm) It is possible to set a stirrer speed of 60 to 250 rpm in 10-steps.

Parameter 11: Threshold value in (1/10 for switching ventilato r on and off C) If this temperature of sample is reached in the block the ventilator turns off. If the test cup was taken out of the device only the block temperature is taken into consideration since no sample temperature signal was given.

Parameter 12: STOP after flashpoint 0001/ 0000, yes/ no This parameter is in delivery mode at 0001, meaning STOP after found flashpoint. If parameter is set at 0000 the program continues until overflow (EFLP + 20 This C). parameter allows an observation of the flashpoint by the user. The user can thus decide himor herself when to abort the program by pressing STOP.

Parameter 13: Test cycle (a) in 1/10 if expected flashpoint is smaller or equals parameter 15 C, Example: Parameter 13=0010 Ignition immerses sample in pan at every 1 temp erature increase. C

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Parameter 14: Test cycle (b) in 1/10 if expected flashpoint gr eater than parameter 15 C, Parameter 15: Threshold value in 1/10 for selection of test cyc le (parameter 13 or 14 ) C Parameter 16: Temperature value 1/10 to start test cycle before expected flashpoint when sample C temperature = EFLP - P16 Example: Parameter 16 is set to 0180, expected flashpoint 100 C Testcyle (a) will be started, when Sample temperature = 100 - 18 = 82 C C C

Parameter 17: 0/1 evaluation of flashpoints P17=0001: evaluation on P17=0000: evaluation off; Flashpoint always FPok

Parameter 18: Safety stop at higher sample temperature than P18

Parameter 19: When a flashpoint above 130 is expected, accordin g to ASTM D93-08 it is strongly advised C to dip the ignitor every 10 throughout the test u ntil the test temperature has reached 28 C C before the expected flash point. Therefore, this parameter is preset to 1300 (130 in the ASTM and Rapid-programs. C) The function is switched off by setting the parameter value to 0000.

Parameter 20: Heaterparameter, % of heater capacity This shows the heater capacity that will not be undergone when heater is turned down.

Parameter 21: Parameter 21 can activate the calibration program for comparison of the sensor PT100 with a calibrated thermometer. 0000 = calibration program off 0001 = calibration program for lower temperatures (-5 through + 110 C)
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0002 = calibration program for higher temperatures (+90 through + 370 C)

Parameter 23 (bitumen parameter) Is this parameter set to 0001 the sample is heated to the temperature stated in parameter 11 between tests. This means that a bitumen sample is not completely cooled but left at a temperature equaling the softening temperature, so that indicator and lid can still be removed. As soon as this temperature is reached the fan is switched off and the heating comes on to keep the sample at this temperature. If parameter 23 set to 0002 the stirrer only starts stirring 10 before the temperature giving C in parameter 11.

Parameter 24-26: Correction for flash points with mini-cup Flash point trial with the little cup pPM 12-1777 (see 3.1.7

Parameter 28: Printer interval in sec If parameter 1 is set to 0998, one line is printed each P28 sec.

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4.2 Parameter 1:

Device parameter

Correction of sample-Pt100 sensor in 1/10 C an offset can be set (difference between thermometer and PT100)

Parameter 2: Unused

Parameter 3: Offset for Gasflame indicator in digit (relative temperature)

Parameter 4: Barometric pressure correction in 1/10 kPa

Parameter 5-6: Unused

Parameter 7: Maximum temperature in the heaterblock in 1/10 C Safetyfunction: To avoid overheating of the PMA-4 the maximum achievable temperature of the heater block is limited by this parameter. If this value is achieved, the heater will stabilize the temperature to this value. The heater is not switched off.

Parameter 8: Unused

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Parameter 9: Switch to F by setting parameters to 0000 or 0 001 C/ When switching from to and vice versa the par ameters of all programs including the C F USER programs, device parameters, except offset initiated. Parameter 10: Result display Depending on this parameter flash point value is displayed as uncorrected value (0002), barometric pressure corrected value (0001) or barometric pressure corrected rounded value (0000). Parameter is preset to 0000, display of barometric pressure corrected rounded value Parameter 11: Flash point registration at theoretical test temperature off on (0/1) Flash point is registrated in PMA4 at the temperature when it happens. Depending on the sample gradient this may also be at a temperature value other than full numbers (e.g. 60,2 C) When this parameter is set to 0001 flash point is always registrated at theoretical test temperature (e.g. 60,0 61,0 or 62,0 C; C C) The parameter is preset to 0000. Parameter 12: Unused Parameter 13: PC-control on/off by setting parameter to 0001 or 0000 Parameter 14: Fire extinguisher off/on (0/1)

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Switching from gas to electric ignition by setting parameters to 0000 or 0001 (The option gas or electric ignition is usually set directly in the menu) Parameter 16: maximum permissible deviation of the ignition voltage in mV downwards Reference voltage is checked immediately after test start. Electric ignitor will be switched on the for about 30s. Parameter 17: maximum permissible deviation of the ignition voltage in mV upwards Parameter 18: lower value of ignition current in 1/100 mA Between two ignition tests the ignition current will shortly be reduced to extend the lifecycle of an electric ignition. Parameter 19: higher value of ignition current in 1/100 mA Ignition current at ignition cycle Parameter 20 Threshold for indication of a "run-over" flashpoint in digit for electric ignitor application If after the first ignition test there is an ignition outside of the cup it can be safely assumed that the expected flashpoint was set way too high. The test has to be repeated with a lower flashpoint preselection. If this parameter is set to >4095 this function is turned off. Parameter 21: Unused Parameter 22: Threshold value for Gasflame indication (relative temperature in digit) According to this threshold values it will be detected if the gas ignition flame is on or off. Parameter 23:
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Threshold for indication of a "run-over" flashpoint in digit for gas ignitor application Parameter 24: Unused Parameter 25: 0/1 Autosampler installed no/yes (2=autosampler movement for chilled autosampler) Parameter 26: 0/1 Extended Autosampler menu no/yes Parameter 27: Reserved for autosampler Parameter 28: Unused Parameter 29: If the last 3 digits of the sample names were numeric the sample number is increased by one after each flashpoint test. After switch-on or off it is counted starting from the last digits. Parameter 30-32: Unused

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4.3

Changing of Parameters

4.3.1 Changing the program parameters Only the two programs UserProgram1 and UserProgram2 are ready for permanent changes. In all other programs modifications are accepted, but will be deleted after switch off of the PMA-4. With each new switching on of the PMA-4 all program-parameters are newly initialized. To change parameters move the cursor to the relevant program and press <ENTER>. In the menu appearing the following can be selected. DISPLAY HISTORY PRINT HISTORY PRINT PARAMETER CHANGE PARAMETER PRINT MANUAL Move the cursor to CHANGE PARAMETER and confirm with <ENTER>. You are now in the setup-mode of the program parameters of the selected program:

On the left the number of the parameter is shown (in this case program parameter 1) and on the right the value of the parameter. With the cursor by the left you can select the number of the parameter to change. With the cursor by the right you can select the new value of the parameter and confirm with <ENTER>. Leave the mode with <STOP> If the parameter was changed, but not confirmed with <ENTER> and only left with <STOP>,
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the former value of the parameter will not be changed. 4.3.2 Changing of device parameters The device parameter are set by the manufacturer and should not be changed by the user except device parameter 1 (Offset Pt100), 4 (Barometer correction) and device parameter 29 for counting numerically set sample names. To change a device parameter in any given program change to the program parameter set, for parameter 1 put in value 1234 and confirm with <ENTER>. Display:

As with the program parameters the number of the parameter will be displayed left and the value on the right. Changes are made with the cursor keys and confirmed with <ENTER>.

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Note:: A negative value (- minus) for temperature- and barometric pressure correction (offset) may be activated by moving the cursor at the empty place in front the number. With key <up> or <down> you can select (+) or (-).

Display:

The changes will remain permanent even after switching off the device.

Reset of device parameter to delivery mode: In any given program for program parameter 1 give in value 4010 and confirm with <ENTER>.

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4.4

Printing of Parameters

4.4.1 Printing of Program parameters Select program and use <ENTER> to confirm. Go with the cursor to the program and call up the respective submenu with <ENTER>:

Repeated pressing of <ENTER> key prints out actual program parameter set.

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4.4.2 Printing of device parameters Give in test code 2000 in any program after calling up function CHANGE PARAMETER in parameter 1 and confirm with <ENTER>. The parameter set of the device parameters is printed out. DEVICE PARAMETER 01=0000 02=0000 03=0106 04=-022 05=0000 06=0000 07=0570 08=0000 09=0000 10=0000 11=0000 12=0000 13=0001 14=0000 15=0000 16=0200 17=0200 18=0900 19=1080 20=2000 21=0000 22=1500 23=0300 24=0000 25=0000 26=0000 27=0000 28=0000 29=0000 30=0000 31=0000 32=0000 33=0000 (1/10 Pt100 Sample correction C) (0) Unused (trel) Gasflame indicator correction (1/10kPa) Barometer pressure correction (0) Unused (0) Unused ( Max temperature at heating unit C) (0) Unused (0/1) F C/ (0/1/2) Result display (FPcrd/FPcorr/FPuncorr) (0/1) FP registration at theoretical test temperature (0) Unused (0/1) PC control off/on (0/1) Fire extinguisher off/on (0/1) Gas/Electric ignition (mV) delta U-low (0=function off) (mV) delta U-high (1/100A) Low I-Ign (1/100A) High I-Ign (trel) E-IGN: Threshold overdrive indicator (0) Unused (trel) Threshold gasflame indicator (trel) GAS-IGN: Threshold overdrive indicator (0) Unused (0/1) Autosampler installed no/yes (0/1) Autosampler testcode off/on (0) Reserved for autosampler (0) Unused (0/1) Increment sample label (0) Unused) (0) Unused) (0) Unused)t (0/1) PMP mode off/on

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5. DISPLAY HISTORY and PRINT HISTORY Selecting a program and pressing <ENTER>, the following display will appear:

Pressing <ENTER> again, the results of the last 99 tests on the display will appear by scrolling it with the cursor keys:

The last result is marked with last, the following are counted from 02 till 99. If you have not done 99 tests yet, the not occupied places are named with INVALID.

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With PRINT HISTORY the last 99 results are printed out:

PETROTEST INSTRUMENTS DAHLEWITZ PMA4-Version 05.06.2006 Device No 41000000 OPERATOR XXXXXXX


SAMPLE NAME PROG NAME EFP C SAMPLE FPcor C C FPcrd BAP C kPa STIR rpm

Tel:033708-56300 Date 06.06.2006

GRAD IGN C/m G/E

STATUS TIME H:M

DODECAN INVALID .

D93-A-LoVisc D93-A-LoVisc

0082 0000

083.0 -------

H I S T O R Y H I S T O R Y

FP OK LAST ---------

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6.

Safety mode

In PMA4 a safety mode can be activated, that recognizes a wrong flash point preselection. The safety mode is activated by inserting test code 1011 into program parameter 1 of any program. 1. Immediately after program start - independent from the flash point preselection - one flash point test is carried out. By this dip-in test the correct mechanical function of the shutter mechanism is ensured. A cover that was not fully closed before is shut by this procedure. The test is done with an active electric or gas ignitor. A too low flash point can already be detected here. 2. The active ignitor dips in further at 10 inter vals until the test temperature is reached. C Samples with too high flash point preselection can be detected early enough to prevent any hazard. The flash point is already detected at a lower temperature and the test will be stopped then. Every flashpoint detected during the safety mode is displayed as FPin (invalid flash point).

This safety function can be deactivated by setting device parameter 8 to 0000. When device parameter 8 is set to 0000 only one dip-in takes place at program start (without active ignitor) for ensuring mechanical function of the shutter mechanism.

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7.

Maintenance

We take regularly maintenance of the unit for granted which should be carried out by the user himself or trained personnel at the given time intervals. The given time intervals can be seen as reference to a normal operation of 8 hours every day. Depending on the intensity of use the intervals might have to be extended or shortened. After a certain number of tests on PMA4 display the message

appears. By pressing any key the display returns to the normal start display. If the Inspection message occurs, please contact Petrotest service for further information.

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1 2 3 4 5

object electric ignition electric ignition multi-sensor test inserts gas ignition

function wear & tear test adjustment contacts lid movement even flame?

inspection visual test** visual test visual test function test / cleaning jam test / blowing free spring elasticity, dipping procedure positions normal and during dipping driving force sound test, partly greasing (acc. instructions!) exchange

test interval 1x / month 1x / month 1x / month 1 x / week 1x / year; with gas ignition 1x / year

inspector operator operator operator operator operator/ specialist operator/ specialist operator / specialist operator / specialist operator / specialist operator

instruction

service

MFH (head) rotary slide opening / closing 7 MFH (head) dipping mechanics of ignition 8 MFH (head) stirrer coupling insert stirrer 9 MFH (head) contact set 10 MFH (head) lead

control of rotary slide movement control of ignition positions position and wear & tear contacts MFH movement without hindrance

service

1x / year

service

1x / year

service

1x / year

1x / year position of ignition cable and plug connections 11 MFH (head) column guiding adjustment and wear 1x / year adjustment & tear ** The message Change Ignitor is only displayed at the PMA4 not at the PC

specialist / operator

service contact set service draft 120796A+B service

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8. Trouble shooting 8.1 Calibration

8.1.1 Calibration of the Pt100-sensor Drawing 12-0770D

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The calibration cover combined with a calibrated thermometer makes it possible to examine the precision of the whole measurement system of the sample temperature including the Pt100 dynamically with the used program or at arbitrary points. Errors regarding from calibrations with static precision resistances can be excluded by this way. For this please select the later used flash point program. Linearity deviations from >+-0,2 (0,4 cannot b e accepted. If this cannot be adjusted this C F) causes an defective PT100 or PMA4. In general every program can be used as calibration program. But the program parameter 21 has to be set to 0001 or 0002 in the selected program. P21: 0001 P21: 0002 Calibration program for thermometer 12-0658 (-5 through +110 C C) Calibration program for thermometer 12-0662 (+90 through +370 C C)

Remove the 4 fixing screws at the upper part of the device (multifunctional head) and CAREFULLY lift up the cover. Place the calibration lid on the cup filled with sample and insert the PT100 to be checked into the cup. Choose the thermometer type according to the used temperature range. The small gap between the brass middle plate and the multifunctional head it is now possible to insert the thermometer directly into the lid. The calibration points for thermometer 12-0658 (Temperature range -5 through +110 C C) are 0 35 70 and 105 C; C; C C. The calibration points for thermometer 12-0662 (Temperature range +90 through +370 C C) are 100 200 300 and 370 C; C; C C. Calculate the deviations by aid of the information in the calibration certificate e.g.: deviation acc. to certificate +0.3 at 35 tempe rature, at which you read: 35,3 C C. C.

The program is started in the usual way. According to chosen program following printout is produced:

calibration program low


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Pt100 F C/

Thermometer Sample gradient F C/ C/min F/min

The sample is heated up as stated in the program. About. 5 before the next calibration C point an acoustic signal is given so that the user gets the chance to read the temperature at the thermometer in time. As soon as the temperature which was calculated according to calibration certificate was reached press <Enter> key and the temperature at the PT100 sensor is printed out. The actual temperature ramp is printed out during test as well just for a check. The column "Thermometer F" has to be filled out by user manually. C/ If one reading point was missed the program continues heating normally. The missing value is only not noted on the printout. It is possible to start at a higher value, for instance to leave out the 0 C-point for the lower temperature range. If the comparison proves a constant deviation between thermometer and PT100-sensor the deviation can be set as offset in device parameter 1. If it shows a fluctuating deviation first establish whether this is the result of reading errors at the thermometer. (always read in the same level as your eyes).

ATTENTION: When working with PMA4 autosampler for calibration of multisensor the option Autosampler must be deactivated in PMACON menu Settings or device parameter 18 must be set to 0000 directly in PMA4 menu..

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8.1.2 Calibration of the PMA-4 with Reference-Materials In accordance with the various internal and external requirements for your laboratory it is necessary to recalibrate each and every flashpoint tester in suitable intervals of time. A wide variation of reference materials is available from internal samples to officially certified standard reference materials. As an internal standard we have found n-Dodecane to be very useful. Variations of the flash point value are possible from manufacturer to manufacturer and from batch to batch, but normally it can be found at approx. 82,5 1,5 with good repeatability. C Such an internal standard should not be used for official calibration but as a means of cost saving routine checking of good work of the PMA-4. Standard Reference Materials are officially certified by national bodies (e.g. PTB, Germany) or other approved calibration services. Although the reference material p-Xylol is mentioned in the standards as a means to recalibrate a Pensky-Martens Flashpoint Tester at low temperatures, we suspect that this was a proper selection. As the flash point with 27 is very low and the cr ystallization point of 13 is very close to C C the flashpoint it is nearly impossible to properly control the test conditions. You shouldnt start a test at a temperature which is under the crystallisation point. In this case you will get physical problems of an instable heating ramp. Also to suspect are the flash point values mentioned in manufacturer-catalogues of chemicals. These values are not certified and are mainly used for transport-safety purposes. The mentioned flashpoint values are no guaranteed property of the material. Also these values are normally picked from historical sources of literature and very often 10 lower C than in reality. Purity and cleanliness of modern production of chemical has been very much improved within the last years. This is the main reason for higher actual flashpoints. For safety reasons the historical lower flashpoints from the literature are mentioned. Further is to be mentioned that for reference-tests in several standards the historical manual flashpoint tester with gas-ignition is required.
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Therefore we recommend to use the gas ignition at least for these tests. Although the PMA-4 is controlling the actual lifetime of an electric ignition within close limits, the electric ignition might have slightly been aged.

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8.2

Trouble Shooting

* Display does not work when switched on Check Fuse * Display does not show any symbol
- The LCD contrast is deadjusted. - To get into the contrast menue press STOP button for 5 seconds. Press now the button UP or DOWN to light up the display more or less. Release the menue with STOP, the contrast level will be hold on.

* Gas Ignition does not work - Is gas connected? - Is gas available? - Is air instead of gas in the tube coming from the supply? - Do you use tubes especially for gas? (Silicon is leaky at gas. With that material the PMA4 has an increasing flame within the test period or -when starting the next test period - it needs to long time to switch on the ignitor because of missing flameable gas. After 55 sec. the gas valve has the safety function to switch off the stream). - Is the PMA-4 in the gas-ignition mode? (see ignition symbol at the display) - Does the solenoid click when a manual test is conducted? - Is the electric ignition in its auxiliary position and does it work? - Is the flow rate adjustment of the gas ignitor too low or too high (see 3.2, Graphic 12-0770X)? * Gas flame is unstable Gas valve must be cleaned in regular intervals (see service instruction) Incorrectly silicone tubes were used, which are not gas tight. * Electric Ignition does not work Are the cables properly connected to the sockets? Is the ignition coil defective/damaged? * No indication of sample temperature Is the indicator plug properly connected to the rear? Does the Multi-Function-Head sit in its correct position? Is the glas-body of the Pt-100 temperature sensor defective/broken? Are the contacts of the Multi-Detector dirty?
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For cleaning of the contacts of the Multi-Detector please only use a soft fabric with alcohol on it. * PMA-4 does not start after pressing RUN-Key Please check the error message. SENSOR-ERROR-SAMPLE-SENSOR ------------> PMA-4 started too early / Pt-100 defective SENSOR-ERROR-FLP-SENSOR ------------> Multi-Function-Head not in correct position SENSOR-ERROR-FIRE INDICATOR ------------> Gasflame indicator out of order SENSOR-ERROR-SENSOR HEATING SENSOR ---> Block PT 100 out of order * Stirrer does not work Is the stirrer coupling in its position? Is the stepper motor plug properly connected to the socket at the rear? * Hose-coupling is to tight to the stirrer and the lid sticks? Change hose-coupling 12-0780 Attention: When changing the stirrer coupling, remove the Multi-Function-Head from the basic instrument.

* Opening mechanics of Lid and Shutter does not work Are some sticky or solid residues to be found? Clean the Lid and Shutter Mechanism. Test inserts delivered after 01/01/01 are new designed and can be cleaned easier without using any tools. * Aging problems of the Electric Ignitor Because of sticky residues at the shutter mechanism the movement of the ignitor can be delayed. Depending on this the shutter doesnt open in the right time which causes damaging the ignitor. * Opening mechanics for shutter does not slide freely. Lubricate the sliding curve of the ignition holder with Molycote-Grease. (see graphic 12-0770C)

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Drawing 12-0770C

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* Results of Reference material s do not comply with the certificate Check ignition - immersion depth - flame diameter - electric ignition defective/aged Check temperature gradient (test-code 0998 in parameter 1) Check for residues on the thermion wire ATTENTION: Depending on the samples used for tests it is possible that the residues build up at the wire, which can influence the flashpoint. Please do check the indicator every now and then.

* Cleaning the thermocouple of the multisensor In normal operation it is not necessary to clean the thermocouple. With some samples a formation of precipitation may be possible. Then please dip the thermoelement CAREFULLY into toluene for cleaning.

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8.3

Replacing the electric ignition

Since the ignition in the PMA4 is run with smooth current and the working current between the ignition tests is lowered to a minimum the ignition has a considerably longer life expectancy than conventional ignitions. The quality of the ignition is evaluated by the device according to a number of criteria (voltage rise or drop). If the electric ignition needs changing following message is displayed after the flashpoint test

This message has to be confirmed with <ENTER>. Now the initial menu is displayed (depending as to whether a flashpoint was found, whether the device is OVFL after reaching overflow etc.) The Printout under point IGNITION states: EL-CH for "Change electric ignition".

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Bringing the new ignition into service: Go to the ignition symbol with the cursor in the main menu and confirm with <ENTER>.

In the menu ELECTRIC IGNITION confirm once again with <ENTER> .You are given the following submenu:

Now move the cursor to NEW and confirm with <ENTER>. The changed date signals that a new ignition has been installed.

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9. 12-0787 12-0776 12-0778 12-0779 12-1507 12-0781 12-0785 12-0786 12-0788 12-0787 12-0789

Spare Parts

PMA-4 Indicator PMA-4 Basic Instrument, Multi-Function-Head PMA-4 Electric Ignition PMA-4 Gas Ignition Stirrer Coupling (Pack of 10) Gastubing, Viton (1m) PMA-4 Test-Cup PMA-4 Cover with lid and shutter Flamesensor for control of gas ignition Multidetector with sensor for temperature and flashpoint Multidetector with sensor for temperature and flashpoint in replacement (we send a replacement in exchange for your faulty one) 12-1781 Contact pins for indicator plug (set of 6) 12-0790 Tongs for safe handling of test insert 12-0791 Plug to close thermometer opening 0505 0000 0022 Fuse 10 A m for 110/115V 0505 0000 0033 Fuse 4 A m for 220/230V

Calibration Set: 12-0782 12-0783 12-0658 12-0662 Temperature calibration Set for PMA-4 comprising of: Calibration Cover Thermometer ASTM 9C -5 to +370 o fficially certified C C Thermometer ASTM 10C +90 to + 370 off icially certified C C

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GENERAL SAFETY RECOMMENDATIONS The instrument should only be used by trained personnel or those who have been instructed accordingly. Alterations on the instrument, especially opening of same or changes to the electrical connections/electronics, should only be done by electro-technicians and then only after receiving permission from PETROTEST INSTRUMENTS GMBH & Co. KG. (Unauthorized changes will also cause cancellation of the guarantee.) Before opening the instrument, disconnect the electrical current. For safety reasons, we recommend using an FI-safety switch, which can be bought from any electrical specialty dealer. It is incorporated in an electrical extension cord with sockets and the entire extension is switched on and off by using the safety switch. When using a flash point or ignition tester as well as heating devices, be certain that no flammable parts are located close to the source of ignition. When using a penetrometer, be careful not to unintentionally release the measuring device as long as the user is manipulating and adjusting for set-up. If pointed or sharp-edged measurement devices, which could injure, are being used, turn off the instrument while the adjustments are being made. We make these recommendations on the assumption that a regular function and safety test is performed at least every six month acc. to DIN VDE 0105, DIN VDE 0701 and VBG 4.

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DANGER OF BURNS ! Because of the use and the dependency upon temperature of the test insert the PMA4 can get very hot, especially near the test insert . Do not touch test insert or close parts of the device without protection. Changes at the device, especially opening it or changing the electronics must only be conducted by trained personnel and only with the explicit permission of PETROTEST INSTRUMENTS GmbH & Co. KG. (Unauthorized changes will result in the loss of warranty). Disconnect from the mains at any time during inspection. For safety reasons insert an FI safety fuse which can be bought in respective stores e.g. in the shape of sockets with integrated FI- safety switch.. We expect a regular safety check every half a year.
FederElastizitt. Eintauchablauf Fett

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