Manual 744 PH Meter EN PDF

METROHM AG = CH-9101 Herisau (Switzerland) pH Meter 744 Series 01 ... 95.10 Ti/kg 8.744.1003,Metrohm — Short Instructions for Use 744 pH Meter Selection of measured quantity Press key. Each keystroke changes the measured ph quantity. Meaning of the symbols in the display "A key must be pressed”, e.g. or input of a value and . "Immerse electrode in butter solution for calibration.” Flashing beaker means "change buffer”. Display of the calibration parameter " slope”, relative slope of the electrode. Display of the calibration parameter "pHas", asymmetry pH. Drift display. Measured value drifts towards higher or lower value. The displayed temperature is measured with a Pt 1000. Hold buffer contains 9 values. Flashing "hold 3" means "the hold buffer is being viewed; the third value is displayed”. Input of numbers Press <»> key several times until the dot at the bottom right of the position you wish to change flashes. Set the desired number with the <> key. Press to store the value. Flashing dot Exit Exit from = calibration (1-point calibration) ~ inquiries and entries ~ viewing the hold buffer = error messages[orn] « Gren Configuration Call-up: <2ND> . Advance inquiries with or . Drift-controlied transfer of a value to the hold butter, 1=yes: Value is transferred when key has been essed and the drift criterion is met. O=no. leads to the next inquiry: Transfer of a value to the hold buffer after elapse of me interval, Time starts when is pressed. gan be stopped and restarted with 6: Immediate transfer when is pressed. reset ti- ransfer Beeper O=n0 tyes Display contrast Time interval for automatic instrument shutdown after the last keystroke. 0=no automatic shutdown. Display of the program version Parameters Call-up: <2ND> . Advance inquiries with or . Temperature. Ifa temperature sensor is connected, the tom- perature is continuously updated. Calibration parameter " slope”, relative slope of the electrode. Calibration parameter "pHas”, asymmetry pH. Preselection of a buffer series Cal-up: With instrument switched off, press and switch on instrument. Selection with , then . 1 Metrohm buffers Pisherbuters > The butter series currently selected Giba/Geigy butters 2 3 c ; Merck/Riedel deHaén buffers { is marked, e.g. "- 1 ~ SP_ Special buttersInstructions for Use for 744 pH Meter Table of contents 1. Getting started 1.1 Connecting electrodes 1.2 Measuring pH values 1.3 pH calibration 1.4 Measuring redox voltages and temperature 1.5 Adjusting the temperature RRONMS 2. pH calibration 2.1 Selecting a buffer series 2.2 pH calibration with special buffers 2.3 General information on pH calibration Now 3. Storing measured values, hold function 3.1 Storing measured values 3.2 Viewing measured values .......... 3.3 Deleting all measured values in the hold butfer 4. Preparations 4.1 Switching on 10 4.2 Mounting in the wall holder 10 43 Setting the operating mode, configuration 4 5. Error messages, problems and troubleshooting 5.1 Error messages... 2... eee eee eee cece eect eee ence enes 12 5.2 Measuring problems 13 5.3 Diagnosis 15 6. Appendix 6.1 Technical specifications 2 6.2 Explanation of technical terms 23 6.3 pH values of buffer solutions 24 6.4 Warranty and certificates 26 6.5 Scope of delivery and ordering designations 29 6.6 Accessories 291. Getting started If you are starting operation with the 744 pH meter for the first time, it is advisable to read through section 4, pages 10 ft. 1.1 Connecting electrodes [| Rear of pH-Meter Power Supply Combined Electrode BH oF redox electrode. Remove the protective- cap from the electrode Pt 1000 Temperature sensor. If an electrode with a built-in Pt 1000 is used, plug the two banana plugs into the connector. sockets provided. = Screw the cable to the electrode. = {Plug the other end of the electrode cable into the pH-Meter. Please turn to page 30 to 300 what electrode is suitable for your masuring problem, Socket for separate reference electrode. Not used if you measure with combined electrodes .1.2 Measuring pH values - Check whether your electrode contains sufficient KCI solution (3 mol/L). It should be filled to a depth just below the fill hole. ‘Add KCI During measurement, the fill hole should remain <—~ solution open. Immerse the electrode in the analysis solution until the diaphragm is covered (app. 2 cm). oon - Switch on the 744 pH Meter: press the key. - Press the key once or more until "pH" appears in the display. ‘The second line always shows the temperature as pH values are temperature dependent. If a Pt 1000 temperature ‘sensor is connected, a thermometer symbol appears in front of the temperature which indicates that the displayed temperature has been measured. Without Pt 1000 , you should enter the current measuring temperatura if itis not already correct, see page 4. ‘The triangle in the display remains lit up until the pH value is "stable". — Wait for the triangle in the display to disappear, 6. your measured value is stable. ~ Take the electrode out of the analysis solution and rinse it thoroughly with dist. water. If need be, carefully dry the electrode with a paper to- wel. — Perform the next measurement. For good pH measurements, a pH calibration should be performed, see following page. After the measurement, the glass electrode must be stored in KCI solution, = 3mol/L (in the reference electrolyte). Close the fill hole with the cap. Never store In water: The AgCI of the reference system dissolves better in solutions containing chloride than in pure water (the chloro complex is formed). If an electrode is stored in water, AgC! can preci- pitate in the diaphragm (and clog it) Never store dry: Otherwise, the gel layer of the glass membrane will dry out. You will find details on pH measurements in Metrohm Application Bulletin 188. This is available free of charge from your Metrohm agency.1.3 pH calibration For pH measurements, a calibration is needed from time to time as the measuring properties of the electrodes change. Perform a calibration, e.g. daily before starting your measurements. Two buffer solutions are required for this. If you are using Metrohm buffer solutions, you can immediately start the calibration. Other buffer solutions must first be preselected, see page 5. - Immerse the electrode in the first buffer solution. ~ Press the key. - The display shows the temperature. The finger means that a key must be pressed. To change the temperature, use the <>> and keys. Select the digit you wish to change with the <»> key. You will recognise the selected digit by the flashing dot at the bottom right. Now change the number using the key: Press the key repeatedly until the desired digit is displayed. When the correct value is set, press . 25.0°C, ical If you have a Pt 1000 temperature sensor connected, the = al ~ Your first buffer solution is now measured. After the measurement, the display prompts you to immerse the electrode in the second buffer solution: The buffer beaker flashes. Carry this, out and press . ~ Your second butfer solution is measured. ~ After the calibration, the slope and asymmetry PH (pHas) of the electrode are briefly displayed and the instrument is ready for pH measurements. If the pH meter comes to a stop on display of the slope or the asymmetry pH, the values are outside the limits, see page 7. If you then wish to accept the value, press . Otherwise, press to retain the old value. You have now calibrated the electrode and you are ready to start pH measurements. You can quit the calibration routine at any time by pressing the key. The results of the calibration can be examined and changed with the key sequence <2ND> , see Short Instructions under "Parameters".1.4 Measuring redox voltages and temperature For redox voltage measurements you need a platinum or a gold electrode (see page 31) and for temperature measurements a Pt 1000 temperature sensor. Redox voltages: Temperature: ~ Press the key once or more until ™m\V” appears in the display. Ifyou have a Pt 1000 temperature sensor connected, the ‘temperature together with the thermometer symbol will be displayed in the second lin ‘The trlangle in the display remains lit up until the measured value is “stable”. - Press the key once or more until "°C" appears in the display. The thermometer symbol lights up to show that the temperature has been measured. ‘The trlangle in the display remains lit up until the measured value is "stable". If you measure pH values or redox voltages and have a Pt 1000 temperature sensor connected, the measured temperature always appears in the second line of the display to- ‘gether with the thermometer symbol. 1.5 Adjusting the temperature The measuring temperature can be set with the key sequence <2ND> . - Press <2ND>. ~ The temperature can now be set, see page 3. Measuring and calibration temperatures are identical. If you ‘set a temperature in the calibration procedure, this is also assumed to be the measuring temperature. Conversely, any temperature set here apples to the calibration routine. ~ Confirm the set value with . ~ Quit the inquiry with .2. pH calibration 2.1 Selecting a buffer series The instrument automatically recognises the buffers. As the pH values of different buffer series differ slightly, it is necessary to preselect the butfer series you wish to se in the subsequent calibration. Metrohm buffers are preselected in the factory. If you wish to use a different buffer series, you have to select this. Proceed as follows to select the buffer series: ~ Switch the instrument off. = Press and hold the key while * switching on the instrument ( key). ~ The display for buffer selection appears. ‘The number specifies the buffer series and the dashes "~" indicate which series is currently selected. The following buffer series can be selected: 1 Metrohm buffers 2 DIN/NBS buffers 3 Fisher butfers 4 Merck/Riedel deHaén butters 5 Ciba/Geigy butters If you do not wish to use any of these butters, select SP Special Buffers. For the calibration procedure with special buffers, see page 6. ~ Select the butfer series with the key: Press the key repeatedly until the desired HOLD) buffer series is displayed. Confirm the series ENTER with .2.2 pH calibration with special buffers When you have selected a buffer series, turn to page 3 for the calibration procedure. The calibration procedure with special buffers (buffer preselection SP) differs slightly from the "normal” calibration routine as the pH values of the buffers have to be entered: - Immerse the electrode in the first buffer solution. = Press the key. = The display shows the temperature, which you enter (keys <» >, and ) or which has been measured. = Enter the pH value of your first buffer solution (keys <» > and ) and press . Note that the pH values of your butfer solution are temperature dependent! ~ When you have entered the value, the first solution is measured. You are then prompted in the display to immerse the electrode in the second buffer solution. Carry this out and press the key. ~ Enter the pH value of your second buffer solution and press . 0.00 pl ~ The second buffer solution is measured. ha) 25.0" = On completion of the calibration, the slope and pHas (asymmetry pH) are briefly displayed.2.3 General information on pH calibration J - The pH calibration remains stored even when the instrument is switched off. ~ Exit from the calibration procedure is possible at any time with the key. If the key is pressed before measurement of the first buffer solution, the old calibration data are retained. On completion of the measurement of the first buffer solution, there is a 1-point calibration. 1 In a 1-point calibration, a new value of pHas is recorded, the old slope is retained. - To continue the calibration procedure, the or key can be used. Any new values entered will be accepted only if the key has been pressed. If the values for the slope and asymmetry pH (pHas) are outside the limits, the calibration procedure stops and the value in the display flashes. This is intended to draw your attention to the unusual values found in your pH calibration. If you nevertheless wish to accept the value, press . If you press , the new value will not be accepted and the old ‘one remains stored. Limits: Slope: 90.0% < slope s 105.0% Asymmetry pH: 6.40 s pHas <_ 8.00 Slope and pHas (asymmetry pH) can be viewed and entered with the key sequence <2ND> , see Short Instructions under ”Parameters”. For good pH measurements, the two buffer solutions should be at the same temperature. You should also perform the calibration at or very close to the temperature at which you will subsequently measure the pH.3. Storing measured values, hold function Up to 9 value pairs ~ measured value and corresponding temperature — can be stored with the key. 3.1 Storing measured values Measured values can be stored with the key. If the hold function is activated, the display shows, e.g. "hold 3”, i.e. 3 pairs of measured values are ‘stored in the hold buffer. Depending on the setting, the measured values can be transferred to the buffer storage in several ways: - Immediately. - When the measured value is stable, i.e. the drift criterion is met (the triangle in the display disappears). - Periodically at preset time intervals. The type of measured value transfer is set with the key sequence <2ND> : - Press <2ND> . The displays can be advanced with . 0 - Transfer stable measured values. d "d” represents drift. 1 = yes, transfer stable measured values. 0 = no. The value can be changed with the key. The entry of 0 leads to the next inquiry: - Measured value transfer periodically at the preset time interval. The time interval is set with the <»> and keys. The key is used to start the process. The display shows "hold 0” until the set time interval has elapsed. After this, the first measured value pair is transferred, the display changes to "hold 1” and the time interval again allowed to elapse etc. The measured value transfer can be interrupted with the key (display "hold”) and then restarted with the same key. If both entries are set to 0, measured value transfer occurs Immediately after the key has been pressed. - — Exit the entry with .3.2 Viewing measured values The measured values can be viewed with the <» > key from the last to the first and with the key from the first to the last. *hold X” flashes in the display. Exit viewing of the measured values with . 3.3 Deleting all measured values in the hold buffer All measured values in the buffer are deleted with the key sequence4. Preparations 4.1 Switching on The display “init” appears after switching on the pH Meter if the power supply was interrupted (power supply plugged out or main power switched off). Display init” confirm with < ENTER > 4.2 Mounting in the wall holder To have the 744 pH Meter ready to hand, it can be mounted in the 6.2051.020 Wall Holder, which can be fixed to the wall.4.3 Setting the operating mode, configuration The operating mode can be configured with the key sequence <2ND> (see also Short instructions under "Configuration". Press <2ND> . Press to move through the displays. Settings for the hold function, see page 8. Ott/on switching of beep Setting 0 or 1 with the key. 4 = beep on beep off O Setting the display contrast Settings 1...4 with the <,> key. 1 = normal setting 4 = setting at high temperatures when the background becomes highly visible. Setting of the automatic shutdown time of the pH meter after the last keystroke. Settings 0...99 min with the keys <» > <,>. 0 = no automatic shutdown. Display of the program version (display "P 10”).5. Error messages, problems and troubleshooting 5.1 Error messages The pH-Meter switches off automatically if the hold buffer contains 9 values and if you press the key. Delete the hold buffer with <2ND> . =a) E4 5 E6 12 In calibration, the voltage of solutions of the second butter differs from the measured value of the first buffer solution by less than 6 mV. Exit, Remedy: - Change buffer solution ~ Use fresh butfer solutions = Check electrode After the error E1, the voltage difference is still less than 6 mV. Remedy: - Use fresh buffer solutions. Are both solutions OK? ~ Check electrode, Is the cable connection also OK? Buffer could not be assigned. Exit! Remedy: - Preselect correct buffer series — Use fresh butter solutions — Check electrode The temperature difference between the two buffer solutions is larger than 2°C. Exit: The calibration temperature is lower than 0°C or higher than 99°C. The pH values for buffers are no longer defined outside these limits. Exit: You have a Pt 100 temperature sensor connected instead of a Pt 1000, Metrohm ordering number 6.110.100; or use the combined pH glass electrode with built-in Pt 1000, Metrohm ordering number 6.0238.000. Exit! 5.2 Measuring problems The following table contains a list of the most frequent malfunctions. The corresponding maintenance steps for pH glass electrodes are listed on page 14. The maintenance steps for the diaphragm are also valid for redox electrodes. Possible cause Remedial = Liquid junction potential on [> Use 3 M KCI solution or reference electrode not other suitable reference constant. electrolyte. ~ Loose contact. ; = Electrode not plugged in or | > Rectity fault. defective cable. Display of the pH Meter drifts. |- Reference electrode is not filled. > Top up with 3M KCI or other electrolyte solution, free from air bubbles. » Empty out water and fill with 3M KCI. » Clean diaphragm. » Add conducting salt or use electrode with sleeve diaphragm. » Clean diaphragm. > Service glass membrane. Display of the pH Meter is ”sensitive |- Reference electrode filled to hand capacity’ with water by mistake. ~ Diaphragm clogged. ~ Measurement in poorly conducting solution. =i onc BERP or [Dey deer, a |- Adsorption at glass membrane. = Diaphragm contaminated. - Adsorption at glass membrane. = Deswollen glass membrane after measurments in » Clean diaphragm. » Service glass membrane. Slope too low » Soak electrode in water between the anhydrous solvents. measurements. ~ Old electrode. » Regenerate glass membrane. - Poor buffer solution. [= Buffer solutions ok? = Crack in the glass membrane. - Connector damp or dirty. » Use fresh buffer solutions. » Use fresh buffer solutions. » Use new electrode. » Dry or clean connector.Care of pH glass electrodes Cleaning the diaphragm = After measurements in media with low chloride concentration (precipitated AgCI in the diaphragm ~ dark-coloured diaphragm): place electrode overnight in conc. NH, rinse with water and renew reference electrolyte. = After measurement in sulphide-containing media (Ag2S in the diaphragm —> dark- coloured diaphragm): Place electrode in freshly prepared, slightly acidic 7% thiourea solution. Then rinse with water and renew reference electrolyte. = With organic contaminants: Place electrode for app. 5 minutes in chromosulphuric acid at 80°C, then rinse thoroughly and renew reference electrolyte. = Ifthe above measures do not help: carefully file down diaphragm with a diamond nail file. The outflowing electrolyte should be visible as a dark ring. Care and regeneration of glass membrane - After measurement in non-aqueous media: soak electrode in water between mea- ‘surements. = After measurement in protein-containing media: Immerse electrode for several hours in a solution of pepsin in hydrochloric acid (5% pepsin in c(HCl) = 0.1 moll). Then soak thoroughly. - Regenerating of glass membrane: Immerse glass membrane either for 1 min in a 10% solution of ammonium hydrogenfiuoride (NH4HF2) or for a few seconds in 40% HF. After the etching rinse for app. 10 s in an HCI solution (HgO:conc. HCI = 1:1), Rinse electrode with water and allow to stand for 24 h in the storage solution. - Clean electrode with appropriate solvent after measurements in non-aqueous, contaminating media (e.g. lacquers).5.3 Diagnostic instructions (for program P 10) The 744 pH Meter is a very precise and reliable instrument. Thanks to its rugged construction it is virtually impossible for external mechanical or electrical influences to have an adverse effect on its functions. Although the occasional fault in the instrument cannot be ruled out completely, malfunctions are much more likely to be due to problems with the electrodes (see page 13) or to incorrect operation or use. It is thus advisable to localise any trouble with the aid of this quick and simple diagnostic routine. The user will then need to call METROHM service only if there is really a fault in the instrument. Also, he can give the service engineer much more precise information by referring to the numbered steps of the diagnostic program. When asking for help, always state the series number on the bottom plate (S...., See Pp. 10) and program version (P XX, see p.11). Procedure - The steps must be carried out in sequence and compared with the reactions of the 744 pH Meter (shown indented). In the "yes" case, continue with the next instruction. = If the instrument does not show the expected response ("no" case), the diagnostic step in question must be repeated so as to rule out any operating error. Consistent- ly wrong responses, however, very probably indicate a defect. - Steps marked with a double arrow (3) allow re-entry into the test routine in the event of repetitions, provided the display shows - Pressing the key returns the instrument to the user program. To re- enter the diagnostic program, see preceding paragraph. - Error indication: the display shows ’E’ and a number. Equipment needed — Reference voltage generator, e.g. Metrohm pH Simulator 2.642.0010 (or any voltage source + accurate DVM, class 0.1 mV) - Insulated, high impedance cable link, e.g. Metrohm 6.2108.060 — Pt 1000 simulator, or resistor switchbox, class 0.1 %, or resistor 1 kQ/0.1 % and suitable short cableFig. 1 16 a) Prepare Instrument for diagnostic test Switch off pH Meter. Detach all external connections (cables at rear). b) Before switching on, press <2nd>, switch on pH Meter; hold down <2nd> key until 'd - 1’ appears. Keypad test Press <2nd> (as often as needed) until appears, then press Press the keys in the order of their associated key number (see Fig. 1): The corresponding key number will be shown (except with ‘mode’ + quit). PARAM TT puca | 4 fa wrong key number is pressed, this is displayed ‘automatically with ’Ex’ (x = number of wrong key pressed). 6 | pHimviec Keypad with key numbers Display test Press <2nd> (as often as needed) until appears, then press The display test runs automatically through the steps 1-10 shown in Fig. 2. The test can be stopped at any time and started again with . At the end of the test, the display again shows 'd - 4’.- OE eC apH 2 eee”. { Je EY au 222 (8, 333m | YYY || s 555 333 yyy | 555 yu > 666 wT ca # 666 n 22190088 9-18.88... Fig. 2. Display test uy 7 |_, 988 7 x4, ORR > 4, EEPROM test Press <2nd> (as often as needed) until m7) appears, then press The entire display ’d - 6’ flashes several times while the test is running. If the test is successful, 'd - 6’ reappears. > 5. Beep test Press <2nd> (as often as needed) until ised appears, then press A short tune is heard. > 6. Check Instrument calibration The display shows the last method selected before switching off.6.1 Check potential measurement Press (as often as needed) until the display shows the mV range. Use a screened, high-impedance insulated cable to connect a voltage calibrator (mV generator, pH Simulator, etc.) of class 0.1 mV - or a less precise source connected in parallel with an accurate voltmeter (0.1 mV) - to measuring input pH/mV’ of the 744. Set voltage to <2000 mV and compare with displayed reading (tolerance +1 mV). Check high impedance of input: (if the generator allows this). Switch source to ‘high impedance’ (Ri = 1000 MQ) and compare display with the value read off previously. The value must not differ by more than 1 digit. Disconnect calibrator. 6.2 Check temperature measurement Press (as often as needed) until the display shows ’°C’. Attach Pt 1000 simulator or resistor switchbox (or 1k1/0.1 %) to socket "Pt 1000’ and read off the temperature (1 k@ gives 0 °C, tolerance +0.1 °C). Disconnect Pt 1000 simulator (or switchbox). End of dlagnosis The diagnosis carried out so far, together with the tests that run automatically (battery test, RAM and ROM tests), have checked the functions of the 744 pH Meter. For more detailed investigations or more selective repeats one can also work through steps 7- 10. > 7. Power supply check ‘The 744 pH Meter is not fitted with batteries. Consequently, in this test only the voltage of the power supply is displayed. Press <2nd> (as often as needed) until (esa appears, then press come | / The supply voltage should not fall below 3.5 V. If there is an insutficient voltage: Check power supply and replace if necessary. To exit, press (‘d - 2’ reappears)> 8. ROM test , Press <2nd> (as often as needed) until appears, then press The test runs automatically. If there are no defects, three ’-” appear on the display from left to right. RAM-Test Press <2nd> (as often as needed) until appears, then press The test runs automatically. If there are no defects, three '-" appear on the display from left to right. auld GOR ). Initialise RAM It may happen on rare occasions that severe interference upsets the processor functions, causing the system to crash. After such an event the RAM area has to be intialised. Although the instrument's basic data are retained, RAM initialisation should be done only when necessary, as the stored user data (pH calibration data, selected buffers, configurations, etc.) are then erased. Execute step 1. Press If initialisation cannot be avoided, press AL Otherwise quit with . During initialisation three '-’ appear on the display from left to right. The standard parameters are now loaded. The data lost from the user memory then have to be entered again, see Instructions for use, Appendix. Execute step 11. 9> 11, Restore the original situation Reconnect the electrode and temperature probe detached at the start of the diagnostic routine, and carry out a brief function test with these. ‘Summary of key assignments In diagnostic tests (before switching on, press <2nd>) For repeat observations and special applications it may be an advantage to perform a particular check directly. The numbers for each test are therefore given below. Press <2nd> as often as required. d- 1 RAM initialisation - only when necessary! —_d - 5 RAM test d- 2 Battery check (power supply) d - 6 EEPROM test d- 3 Keypad test d-7 ROM test d- 4 Display test d- 8 Beep test 206. Appendix 6.1 Technical specifications Measuring range pH value Voltage Temperature Resolution pH value Voltage Temperature Errors (without measuring probes) PH value ‘over operational voltage range over temperature of use range Voltage over operational voltage range ‘over temperature of use range Temperature ‘over operational voltage range over temperature of use range Measuring rate PH value with alternating temperature measurement Voltage with alternating temperature measurement Temperature pH measurement Temperature compensation of the slope in the temperature range pH callbration Type Buffer solutions which can be used for the automatic buffer recognition, temperature dependence of the pH values considered automatically Special buffers without automatic recognition Signal amplifier Input resistance Offset current pH = 0.00 14,00 U_ = =1990 ... +1990 mv t= 180.0... +199.9 °C ApH = 0.01 AU = 1mV At = 01°C + 0.01 + 0.14% of (meas.value-pH7) + 0.20% of (meas.value-pH7) mV 1 0.05% of meas.value 0.18% of meas.value ee +0. $0.1°C + 0.4% of final value 1°C 1.9 measurements/s each 1.9 measurements/s each 3.8 measurements/s 0.0...100.0 °C 1- or 2-point-calibration Metrohm, DIN/NBS, Fisher, Merck/Riedel deHaén, Ciba/Geigy > 10199 <3°10-713A 24Display Type Digit height Dialog Housing Materials Housing Keypad membrane Protection against static discharges Ambient temperature, humidity Operational temperature Storage, transport Humidity Reference conditions ‘Adjusting interval Temperature Operational voltage Error influence quantities Operational voltage range Temperature of use range Safety specifications Power supply Power supply Current consumption Dimensions Width Length Height Weight incl. stand rod ep 10 mm for measured value 6.9 mm for temperature with pictograms Polybutylenterephthalate (PBTP) Polyester (PET) inner walls of housing coated with aluminum -10...55 °C -40...60 °C 5...85 % rel. humidity annually 23 42°C 6.0 £0.1V 6V + 5% 0...65 °C Designed and tested in accorance to IEC publication 1010, safety class Ill. This ‘manual contains some information and warnings which have to be followed by the User to ensure safe operation and to retain the apparatus in safe condition. 6.2117.050 or 6.2119.050 6V DC + 5%, O1A max. 15mA with Pt1000 172 mm 188 mm 40mm 900 g6.2 Explanation of technical terms Asymmetry pH Buffer solutions Calibration Diaphragm Drift pHas PH calibration See pH calibration. Butfer solutions have an exactly known pH value at a specified temperature. They are used for the pH calibration. See pH calibration Part of the electrode which forms a conductive connection between the analysis solution and the reference electrolyte solution. PH electrodes have either a round ceramic diaphragm directly above the glass bulb or a sleeve diaphragm. Measured values are usually not immediately stable when an electrode is immersed in the analysis solution. The measured value changes somewhat over a period of time. This change is called drift. In the 744 pH Meter, such drifting values are marked in the display with a triangle. The triangle fades as soon as the measured value is more stable than a preset drift threshold. Drift threshold: pH: 0.028 pH/min U/mv: 1.875 mVimin v°C: 0.974 °C/min See pH calibration In the pH calibration, the measured voltage is plotted against the specified pH value of the buffer solution. This results in a straight line (at least in the middle pH range). The intersection point of this straight line with the pH axis gives the asymmetry pH, pHas. The slope of the line at 25°C is theoretically 59.16 mV per pH unit. This slope is specified as a relative slope 1 = 100%. Real pH calibrations usually result in a somewhat lower slope. 23pH value The pH value specifies the acidity or alkalinity of a solution, At pH = 7, the solution is neutral. Solutions with PH values less than 7 are acidic, those with pH values greater than 7 alkaline. Redox measurements Voltage measurement with a platinum or a gold electrode. The ratio of a reduced to an oxidised substance is measured. Reference electrolyte The reference electrolyte solution is an essential part of the reference electrode. In most cases, KCI solution, 3 mol/L is used. Slope See pH calibration You will find additional information in the Metrohm monograph "Electrodes in potentiometry” and in Metrohm Application Bulletin 188. Both these publications can be obtained free of charge from your Metrohm agency. 6.3 pH values of buffer solutions SR] is | zen Tove +£0.02 £0.02 £0.02 390 923 DIN/NBS butters 918 0 0 5 5 10 913 10 15 9.08 15 20 8.04 20 25 25 30 30 685 35 35 eas 38 38 eae 40 0 684 45 5 683 50 50 683 55 55 683 60 60 684 85 65 6.84 70 70 6.85 a 75 68s 80 80 6.86 85 85 esr 80 90 688 95 85 423 6.89 pH 4: potassium hydrogen phthalate Cr potassium hydrogen phthalate pH 7: potassium/sodium hydrogen phosphate phosphate pH 8: borax F: borax according to DIN 19266 (1979) 24BSRSASRSASHSEBRERBASOO 20 25 30 35 38 40 45 50, 55 60, 65 70 75 20, 85 90 95 pHa pH 7: potassium dihydrogen phosphate/NaOH BH: potassiumisodium dityerogen (SB 107) phosphate pH 10: potassium borate/carbonate/KOH (SB pH 9: boric acid/KCVNaOH 1); The values indicated by Riedel deHaén may vary until up to ApH 0.02. wo interpolated or extrapolated values ‘The values without * correspond to the ‘manufacturer's specifications. SRSISRSRSHESRERS pH 7: potassium/sodium hydrogen phosphate pH 9: borax/potassium dinydrogen phosphate 256.4 Warranty and certificates Warranty ‘The warranty regarding our products is limited to rectification free of charge in our workshops of defects that can be proved to be due to material, design or manufacturing faults which appear within 12 months from the day of delivery. Transport costs are chargeable to the orderer. For day and night operation, the warranty is valid for 6 months. Glass breakage in the case of electrodes or other glass parts is not covered by the warranty. Checks which are not a result of material or manufacturing faults are also charged during the warranty period. For parts of outside manufacture insofar as these constitute an appreciable part of our instrument, the warranty stipulations of the manufacturer in question apply. With regard to the guarantee of accuracy, the technical specifications in the Instruc- tions for Use are authoritative. Concerning defects in material, construction or design as well as the absence of guaranteed features, the orderar has no rights or claims except those mentioned above. If damage of the packaging is evident on receipt of a consignment or if the goods show signs of transport damage after unpacking, the carrier must be informed immediately and a written damage report demanded. Lack of an official damage report releases METROHM from any liability to pay compensation. It any instruments and parts have to be returned, the original packaging should be used if at all possible. This applies above all to instruments, electrodes, burette cy- linders and PTFE pistons. Before embedment in wood shavings or similar material, the parts must be packed in a dustproof package (for instruments, use of a plastic bag is imperative). If open assemblies are enclosed in the scope of delivery that are sensitive to electromagnetic voltages (2.9. data interfaces etc.) these must be returned in the associated original protective packaging (9.9. conductive protective bag). (Exception: assemblies with built-in voltage source belong in a non-conductive protective packaging). For damage which arises as a result of non-compliance with these instructions, no warranty responsibility whatsoever will be accepted by ME- TROHM. 26lonenanalytik ¢ Analyse des ions ¢ Ion analysis @ Analisis iénico A Metrohm 744 pH Meter Metrohm Ltd. (CH-9101 Herisau Switzerland Phone +41 71 53 85 85 Fax+41 7153 89 01 Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for seourity and to system validation issued by the manufacturing company. Name of commodity: 744 pH Meter System software: Stored in ROMs Name of manufacturer: Metrohm Ltd., Herisau, Switzerland This Metrohm instrument has been built and has undergone final type testing according to the standards: Electromagnetic compatibility: Emission EN55022 / class B, EN50081-1/92 Generic emission Electromagnetic compatibility: Immunity EN50082-1/92 Immunity 1EC801-2/91 class 3, EN50082-2, NAMUR Static discharge 1EC801-3 Radiated rf electromagnetic field immunity 16C801-4 El. fast transient requirements 1EC801-5 “Surges” immunity EN50093 Voltage dips, short interruptions Security specifications 1EC1010, EN61010 class 2, UL3101-1 The technical specifications are documented in the instruction manual. The system software, stored in Read Only Memories (ROMs) has been validated in connection with standard operating procedures in respect to functionality, analytical perfor- mance, and accuracy of results. The features of the system software are documented in the instruction manual. Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for quality as- ‘surance in design/development, production, installation and servicing. Herisau, Sept. 14. 1995 ~. Fant Khan Dr. J. Frank Ch. Buchmann Development Manager Production and Quality Assurance Manager 27lonenanalytik ¢ Analyse des ions ¢ Ion analysis Analisis iénico ©.Metrohm 744 pH Meter Metrohm Ltd. CH-9101 Herisau ‘Switzerland Phone +41 71 53 8585 Fax+41 71 53 89 01 EU Declaration of Conformity The METROHM LTD. company, Herisau, Switzerland herby certifies, that the instrument: 744 pH Meter meets the requirements of EC Directives 89/336/EWG and 73/23/EWG. Source of the specifications: EN 5081-1 Electromagnetic compatibil , basic specification Emitted Interference EN 50082-1 Electromagnetic compatibility, basic specification Interference immunity EN 61010 Safety requirements for electrical laboratory measurement and control equipment Description of the instrument: pH Meter for measurements of pH, voltages and temperature Herisau, September 14, 1995 ~. Yang Dr. J. Frank Head of engineering dept. 28 A fem ao Ch. Buchmann Head of production dept. Management representative6.5 Scope of delivery and ordering designations 744 pH Meter ... 2.744.0014 including the following accessories: 4 Clamping ring 10 mm = 6.2013.010 1 Stand rod 30 ...... + 6.2016.050 1 Electrode Holder 6.2021.020 1 Power Supply, Euro 220 6.2117.050 1 Hexagon Screw » V.017.8016 1 Instructions for Use for 744 pH Meter .. + 8.744.1003 744 pH Meter 2.744.015 like 2.744,0014 but with another Power Supply: 1 Power Supply, USA 100V...120V/6V DC 6.2119.050 744 pH Meter like 2.744.014, additional with 1 LL-Solitrode with built-in P00... 2... 6.6 eee eee renee eee 6.0228.000 744 pH Meter .. like 2.744.0015, additional with 1 LL-Solitrode with built-in P1000... 6... cece eee ee ee tees 6.0228.000 6.6 Accessories, Electrodes 6.6.1 General Pt 1000 temperature sensor Cable for Pt 1000 temperature sensor, length 1 im 6.1110.100 6.2104.080 length 2 m 6.2104.110 Wall holder ... 6.2051.020 6.6.2 For pH measurements Solutions: Ready-to-use solutions, 500 ml Buffer pH 4 : 6.2307.100 Buffer pH 7 6.2307.110 Buffer pH 9 + 6.2307.120 Sets buffer concentrate 50 mi each, “total 250 mi buffer solution Buffer pH 4 and pH 7 and 3M KCI solution .. 6.2302.010 Buffer pH 4, pH 7 and pH 9 + 6.2304,000Which electrode do you use for your measuring problem? Normally, the 6.0228.000 Solitrode or 6.0238.000 electrode, both with built-in Pt1000, can be used. If you have any problems with your pH measurements, the following list may help you finding the right electrode. Fill LL electrodes with aqueous KCI solution only. Together with the electrodes you need a separate 6.2104.020 electrode cable (1 m) 1): 6.0726.100 separate reference electrode: 6.2106.020 cable (1 m); inner and ‘outer electrolyte LiC! sat. in Ethanol. Water Boiler feed water (outer electr. 0.1 M KCI) Drinking water Ground water . Rain water (outer electr. 0. 1 M KCl - Swimming pool water... . Waste water (change electro! lyte req! 6.0219.100 6.0219.100, 6.0239.100 6.0219.100, 6.0239.100 6.0219.100 6.0219.100, 6.0239.100 6.0219.100, 6.0239.100 Foodstutts Beer 6.0239.100 Cheese (cleaning with pepsine, s.page 14) .. 6.0234.100, 6.0238.100 Cheese (< 15 °C; cleaning with pepsine, s.page 14) 6.0214.100 Cream (clesning with pepsine, spage 1 aan 6.0219.100, 6.0239.100 Fruit juices. 6.0239.100 Fruits Fruits (< 15 °C) 6.0234.100, 6.0236.100 6.0214.100 Jam (> 50 °C) 6.0219.100 Ketchup .... 6.0239.100 Mayonnaise (cleaning with pepsine, s.page 14). 6.0289.100 Meat (cleaning with pepsin, s.page 14) ....... 6.0234.100, 6.0236.100 Meat (< 15 °C; cleaning with pepsine, spage 14) 6.0214.100 Mik (cleaning with pepsine, page 14) Molasses .. 6.0219.100, 6.0239.100 6.0239.100, 6.0219.100 Mustard 6.0239.100 New wines .... 6.022.100 Salad dressing . 6.0239.100 Vegetable j ivices | 6.0239.100 Vine 6.022.100 Vinegar 6.022.100 Yogurt (cleaning with pepsine, s.page 14) Cosmetics, Detergents Creams (non-aqueous, sep. meas iat electrodes) 6.0219.100, 6.0239.100 6.0133.100 + 6.0726.100 Decalcifying agent 6.0222.100 Detergents 6.0219.100, 6.0235.100, 6.0239.100 Lotions (partly aqueous) 0.2.2... 0s ce cece ee eee 6.0219.100, 6.0239.100, 6.0235.100 Mouth wash .. 6.029.100, 6.025.100 Pastes . 6.0239.100' Shampoo . 6.0235.100, 6.0239.100 ‘Skin (surface 6.0217.000 30Soap . 6.0239.100, 6.0235.100 Tooth paste 7 ‘ + 6,0239.100 Tooth wash ....... . . « 6.0239.100, 6.0235.100 Washing agent, liquid 6.0235.100, 6.0239.100 Pharmaceutics, agrochemistry Fertilizers (change electrolyte frequently) ....... 2.64. 6.0219.100 Ointments (non-aqueous, sep. meas./ret.« ee - 6.0133.100 + 6.0726.100 Soil samples (slurry) . +++» 6,0219.100 Urine 6.0220.100, 6.0222.100 Leather, paper, textiles Bleaching bath - 6.0220.100, 6.0222.100 Dye bath - 6,0239.100, 6.0219.100 Paper (surface) + 6.0217.000 Tanning bath .... . 6.0222.100, 6.0220.100 Textiles (surface) + 6.0217.000 Lacquers, paints 6.0222.100 . 6.0239.100 Adhesives, alkaline (nso with solvent) Lacquers (rinse with solvent) . Paints, alkaline ......... + 6.022.100 Suspensions (aqueous) * 6.0239.100 Suspensions (non-aqueous, sep. meas./ref.electrodes) . 6.0133.100 + 6.0726.100 Metals, galvanics Caustic bath (change electrolyte frequently). . 6,0219.100 Galvanic baths (change electrolyte frequently) + 6,0219.100 Photo, printing Photo baths (outer electrolyte KNO3 sat) ..... 6.60.05 6.0219.100 General Emulsions + 6.0239.100 Low-ionie media (outer electrolyte 0.1 M KC) . + 6.0219,100 Small sample volumes Small sample volumes(<15 °C) Surface, e.g. skin, paper . . - 6.0234.100, 6.0236.100 + 6.0204.100, 6.0214.100 + 6.0217.000 6.6.3 For redox measurement Solutions: Redox standard solution + 250 mV, 250 ml .. 6.2306.020 3M KCl solution, 250 ml 6.2308.020 Electrodes: A separate electrode cable forms part of the electrode: Length 1m 6.2104.020 Length 2 m 6.2104.030 Length 3 m 6.2104.040 6.0415.100 6.0413.100 Comb. platinum electrode. Comb. gold electrode .. . 31Index Texts which appear in the display are printed in italics. Keys are marked with < >. Calibration. . Cortificates . . Ciba/Geigy butters = pH values - selection D qd... Diagnosis Diaphragm DIN/NBS butfers - pH values - selection Display contrast 2 E Electrodes = connecting ... = care and maintenance . 14 + selection 30 Entering values . 3 Error messages... 2 F Finger... a Fisher buffers pH values 25 - selection 6 G Glass electrode = problems H Hand . hold ! init Input of values... Installation. so M Merck buffers ~pH values ............0- + selection Measuring. = problems = temperature. Measured values = storing ..... - viewing + transferring Metrohm buffers = pH values - selection ° Ordering numbers . . 30 13 tities 18 = measurement + value . .. Program version . Ptt000 ...R Redox ~ electrodes... 31 measurements. 4,24 Reference electrolyte 4,24 Riedel deHaén buffers = pH values eee ee - selection coe . 6 s Shutdown time... ou ‘Scope of delivery poocoo f.) Setting the operating mode... . " Slope .....+ + 24 5,6 23 T tee : Technical specifications . Temperature ...... Temperature sensor ‘Thermometer : Troubleshooting ...... v Values renter... seers 3 - viewing 8 - storing 8 Version. " Ww ‘Wall holder 10 Warranty 26

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