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  • Page 2 Gebrauchsanleitung ....................Seite 3 … 80 Wichtige Hinweise: Die Gebrauchsanleitung ist Bestandteil des Produktes. Vor der ersten Inbetriebnahme bitte sorgfältig lesen, beachten und anschließend aufbewahren. Aus Sicherheitsgründen darf das Produkt ausschließlich für die beschriebenen Zwecke eingesetzt werden. Bitte beachten Sie auch die Gebrauchsanleitungen für eventuell anzuschließende Geräte.
  • Page 3: Table Of Contents

    TABLE OF CONTENT ® Technical Specifications of the Titrator TitroLine 5000 ........83 Notes to the operating manual ....................83 Intended Use ........................... 83 Technical Specifications ......................84 ® 1.3.1 Titrator TitroLine 5000 ......................84 Warning and safety information ....................86 Installation and Commissioning................
  • Page 4 Guarantee ......................158 10 Storage and transportation ................. 158 11 Recycling and Disposal ..................158 Copyright © 2020, Xylem Analytics Germany GmbH Reprinting - even as excerpts - is only allowed with the explicit written authorization. Germany. Printed in Germany.
  • Page 5: Technical Specifications Of The Titrator Titroline 5000

    ® Technical Specifications of the Titrator TitroLine 5000 Notes to the operating manual The provided operating manual will allow you the proper and safe handling of the product. For maximum security, observe the safety and warning instructions in the operating manual! Warning of a general danger: Non-compliance results (can result) in injury or material damage.
  • Page 6: Technical Specifications

    Technical Specifications ® Titrator TitroLine 5000 1.3.1 Translation of the legally binding German version (Release: 18. June 2020) EMC compatibility according to the Council Directive: 2014/30/EU; applied harmonized standards: EN 61326-1: 2013 Low-voltage directive according to the Council Directive 2014/35/EU; Testing basis EN 61 010-1: 2010 for laboratory equipment RoHS Council Directive 2011/65/EU FCC Part 15B and ICES 003...
  • Page 7 RS-232-C Interface: separated galvanically through photocoupler, Daisy Chain function available Data bits: adjustable, 7 or 8 Bit (default: 8 Bit) Stop bit: adjustable, 1 or 2 Bit (default: 1 Bit) Start bit: static 1 Bit Parity: adjustable: even / odd / none Baud rate: adjustable: 1200, 2400, 4800, 9600, 19200 (Default 4800 baud) Address:...
  • Page 8: Warning And Safety Information

    Warning and safety information The device corresponds to protection class III. It was manufactured and tested according to DIN EN 61 010, Part 1, "Protective Measures for electronic measurement devices" and control devices and has left the factory in an impeccable condition as concerns safety technology.
  • Page 9: Installation And Commissioning

    Installation and Commissioning Unpacking and setting up The device has been put together especially for you (basic unit + corresponding modules and accessories), there may be differences with respect to the delivery and the accessories described in this chapter. The scope of delivery, please refer to the attached packing list.
  • Page 10: Back Panel Of The Titrator Titroline 5000

    ® Back panel of the titrator TitroLine 5000 Fig. 1 ® The TitroLine 5000 is equipped with the following connections: Measurement input 1 (DIN or BNC through adapter) for the connection of pH, redox and other measurement or combination electrodes Measurement input for reference electrodes (Ref.) Temperature measurement input for connecting Pt 1000/ NTC 30 electrodes Two RS-232 ports, 4-channel (Mini-DIN):...
  • Page 11: Connection And Installation Of The Piston Burette And The Magnetic Stirrer Tm 50

    Connection and installation of the piston burette and the magnetic stirrer TM 50 The low voltage cable of the power supply TZ 1853 has to be plugged in to the 12 V socket “in”, on the back panel of the titrator. (Fig. 2). Then plug the power supply into the plug socket. Fig.
  • Page 12: Setting The Language

    Setting the language The ex-factory default language setting is English. After the device is switched on and the start-up process is complete, the main menu appears (Fig. 5). Fig. 5 Using <SYS> or <MODE>, you navigate to the system settings («System settings »...
  • Page 13: Dosing Unit And Accessories

    Dosing unit and Accessories Fig. 8 TZ 2003 - Drying tube TZ 3282 - Dosing hose without dosing tip and holding bracket TZ 1748 - Stand rod Z 305 - Titration clamp TZ 3620 - Dosing hose with dosing tip and holding bracket: bracket = TZ 3875 TZ 3656 - Titration tip unit (5 pieces);...
  • Page 14: Installing The Burette Tip

    Installing the burette tip The burette tip consists of the elements shaft with threaded clamping joint, hose and slip-on tip (Fig. 9). stop ring marking hose shaft threaded clamping joint Fig. 9 Burette tip - Sequence of assembly: Cut of hose end evenly. Slip parts of the threaded clamping joint on to the hose.
  • Page 15: Initial Filling Or Rinsing Of The Entire Interchangeable Unit

    Initial Filling or Rinsing of the Entire Interchangeable Unit 2.6.1 While the initial filling or rinsing programme is being run, please place a sufficiently dimensioned waste vessel under the titration tip. Initial filling of the interchangeable unit is done using the «rinsing» program. Fig.
  • Page 16 Fig. 13 Fig. 14 Fig. 15 Fig. 16 You can stop the rinsing operation at any time by pressing <STOP> and then resume rinsing with <START>. When the rinsing is finished, you can get back to the start menu by pushing 2 x<ESC>.
  • Page 17: Working With The Titrator Titroline 5000

    ® Working with the Titrator TitroLine 5000 Front Keyboard Fig. 17 Apart from alphanumeric input (a-z, A-Z, 0-9) and a few other functions, almost all functions can be performed using the front keyboard (Fig. 17). <MODE>: Methods selection, rinsing, system settings <EDIT>: Changing the current method, new method, copy and delete method <ESC>:...
  • Page 18: Manual Controller

    Manual controller The manual controller (Fig. 19) is needed for manual titration. It can also be used for starting dosage or other methods. Fig. 19 Mode Black key Grey Key Start of titration, single-step and Filling Manual titration continuous titration Stop of titration including evaluation Dosage through Dosage method Start dosage...
  • Page 19: Menu Structure

    Menu Structure The menu screens shown in this manual serve as an example and may differ from what you see! There are 5 selection menus:  Start or main menu  Method parameters  Method selection  CAL menu  System settings.
  • Page 20 <MODE>/F6 leads you to the select method menu (Fig. 22). Fig. 22 Existing methods (maximum 5) can be selected by pressing <↓> and <↑> and confirming the selection with <ENTER>/<OK>. Once the selection made, you will return to the main menu with the newly selected method. If no method is selected <ESC>...
  • Page 21: Main Menu

    Main Menu After power-up, the main menu is always the first menu to appear. The method displayed will always be the last method that was used (Fig. 25). Fig. 25 Automatic Titration 3.6.1 The method being displayed can now be carried out immediately with <START>. Depending on the method settings, you will be prompted for the sample identification (Fig.
  • Page 22 In the case of an automatic acceptance of the balance data, the weighed-in quantities will be read in from a memory. If the memory does not contain any balance data, a message will appear (Fig. 28). Fig. 28 Pressing the Print key will transfer the balance data, too. Titration will then begin directly after the transfer of the balance data without any further confirmation being necessary.
  • Page 23: Calibration (Cal-Menü)

    The result will be displayed at the end of the titration (Fig. 31). Fig. 31 <MODE> can be used to view the titration curve or further resuts (Fig. 32). The pH und mV titration curves will show the measurement curve (blue) and the 1 derivation (red).
  • Page 24 The titrator will ask you to rinse the electrode and immerse it successively into 2 or 3 buffers (Fig. 34). Fig. 34 The 1 buffer is started with <START>. The 2 and 3 buffers (optional) are to be started with <ENTER>/<OK>. During calibration (Fig.
  • Page 25 Once calibration completed, the display will show the slope and the zero point of the electrode (Fig. 38). Fig. 38 The calibration values will be automatically printed or stored as a PDF file. <ESC> will take you back to the main menu. The current calibration values can be viewed at any time.
  • Page 26: Manual Titration

    Manual Titration 3.6.3 Manual titration is impossible without the manual controller. The mV or pH reading will be displayed (Fig. 41). The value can be selected in the menu item «Titration parameter». Fig. 41 <START> or pressing the black key on the manual controller will start the manual titration method. Following the input of the sample description and/or the weight/volume (optional - please compare also the explanations in ...
  • Page 27 These stages can also be changed during manual titration (Fig. 43). Fig. 43 Stage 5 corresponds to maximum titration speed. Speed is reduced by 50% each time. Example: 20 ml dosing unit Stage 5 100 % 40 ml/min Stage 4 50 % 20 ml/min Stage 3...
  • Page 28: Dosage

    Dosage 3.6.4 3.6.4.1 Dosing operation with dosing method Use <START> or the black key of the manual controller to start a dosage method (Fig. 45 and Fig. 46). Fig. 45 Fig. 46 The dosed volume will be briefly displayed (Fig. 47) before the display returns to the main menu (Fig. 45). Fig.
  • Page 29 3.6.4.2 Dosing operation without dosing method A dosing operation can also be performed without any dosing method with <DOS>/<F10> of the external keyboard (Fig. 48). Fig. 48 The volume will be dosed with <ENTER>/<OK> (Fig. 49). Fig. 49 The next volume can be carried out immediately with <ENTER>/<OK>. Filling of the unit following dosage will not occur automatically here, unless the maximum cylinder volume has been reached.
  • Page 30: Method Parameters

    Method parameters From the main menu, <EDIT> will take you to the method parameters (Fig. 50). Fig. 50 Method editing and new method If you select «edit method» or «new method» you will be taken to the modification or new creation of a method. Selecting «new method»...
  • Page 31: Default Method

    Default method The «Default methods» item of the device contains a series of ready-made standard methods which can be conveniently selected (Fig. 52). Fig. 52 Once the selection made, you are directly prompted for the input of the method name (Fig. 53). Fig.
  • Page 32: Delete Method

    Delete Method In this function you will be prompted to know whether the current method is actually to be deleted (Fig. 55). You have to reply «Yes» in explicit terms and also confirm this reply with <ENTER>/<OK>. Fig. 55 Print method The currently selected method can be printed on a connected printer or stored on an USB drive as PDF file (Fig.
  • Page 33: Change Method Parameters

    Change Method Parameters The input or modification of the method name was already described in  4.1 and 4.3 Fig. 57 Method type 4.6.1 On the «Method type» you can select whether you wish to perform a manual or automatic titration, a dosage or whether you wish to prepare a solution.
  • Page 34 4.6.2.1 Linear titration In the case of linear titration, the step size remains identical over the entire titration cycle. Linear titration is often used for complicated or unknown samples. Complicated examples include, for instance, chloride in the trace range (-> very flat curve pattern) or titrations in non-aqueous media. If one would use a dynamic titration control in these cases, this would not yield any benefit.
  • Page 35: Result

    4.6.2.3 End-Point titration The goal of End-Point titration consists in titrating as precisely as possible to an end point given in terms of pH, mV or µA. In the case of pH und mV you can also titrate to two end points. Consumption in the end point will be used as a result.
  • Page 36 One inflection points can be analyzed (Fig. 63). Fig. 63 With «only total consumption» the consumption at the last measured pH/mV value will be used. With «1 EQ» the calculated equivalence points of the titration curve will be used. «Formula» (Fig. 62) offers the following settings (Fig. 64). Fig.
  • Page 37 4.6.3.1 Calculation Formula The appropriate calculation formula is selected on the «Formula selection» submenu (Fig. 66). Fig. 66 The following calculation formulae are available for EQ and EP: Formula for linear and dynamic Formula for titrations to Information titration to EQ1 End-Point (EP 1 and EP2) No formula No result will be determined.
  • Page 38 Calculation of the consumption in the equivalence or end point. EP2*T*M*F1/(W*F2) Formula for the calculation of concentration of a sample. Direct titration to 2 EP. Here EP2 (p and m value) (EP2-EP1)*T*M*F1/(W*F2) Formula for the calculation of the concentration of a sample. Direct titration to 2 EP.
  • Page 39 The values from the global memory were defined in advance by a titration or were manually entered (Fig. 68 and Fig. 69). Fig. 68 Fig. 69 The global memory used is displayed (Fig. 70). Fig. 70 Storing results in global memories is described in  4.6.3.6. The values of the individual parameters of the selected calculation formula, e.g.
  • Page 40 Fig. 71 4.6.3.2 Sample weight and volume (sample quantity) The Sample Quantity (W) item (Fig. 72) is used to select whether one is wishing to use a sample weight or a sample volume for titration or solution preparation (Fig. 73). Fig.
  • Page 41 4.6.3.3 Formula unit The formula unit can be selected in the «Unit» submenu (Fig. 74). Fig. 74 Once the selection made (e.g. «%»), the unit will also be displayed as piece of information (Fig. 75). Fig. 75 By pressing the «INS»...
  • Page 42 4.6.3.5 Statistics The mean value and relative standard deviation can be automatically calculated and documented by using the statistics (Fig. 77). Fig. 77 The calculation of the mean value is already possible from 2 individual values, the calculation of the relative standard deviation is only possible from 3 single values (Fig.
  • Page 43 4.6.3.6 Global Memories If a titration result is to be used again later, such as the factor or titer of a solution or a blind value, this can be saved automatically. The creation of a global memory is only possible if an external keypad is used. The creation of a global memory is possible in the «system settings».
  • Page 44 M01 can be accepted or provided with a designation such as blank value or titer (Fig. 83) Fig. 83 This simplifies later the allocation of the global memory in another method (Fig. 84). Fig. 84 The blind value which was possibly titrated in advance, is always taken into consideration automatically (Fig. 85). Fig.
  • Page 45: Titration Parameters

    Titration parameters 4.6.4 The «Titration parameter» submenu is used to determine the actual parameters of the method (Fig. 87 and Fig. 88). Fig. 87 Fig. 88 4.6.4.1 Generally applicable titration parameters Depending on the titration mode (dynamic, linear, End-Point titration), it is possible to enter a variety of parameters.
  • Page 46 The selected measured value is displayed for information (Fig. 90). Fig. 90 «Measuring speed» or drift will determine the span of time after which the measured value will be accepted following a titration step (Fig. 91). Fig. 91 Drift-controlled acceptance of the measured value in terms of mV/min is set by selecting «normal», «fast» or «user-defined»...
  • Page 47 Fig. 92 If normal or fast drift was selected before, the values will be defaulted for user-defined drift. In the present case, for instance, 20 mV for normal drift: (Fig. 93). Fig. 93 Drift-controlled acceptance of the measured value is used in most applications. However, there are applications in which the setting of a fixed holding time for measured value acceptance following the titration step is recommendable.
  • Page 48 After the start of titration, it makes frequently sense to have the sample stirred over a defined period of time, for instance, to allow for the sample to be dissolved. The waiting time to be observed prior to the first addition of titration solution can be set using the <Initial waiting time>...
  • Page 49 4.6.4.3 Linear titration If linear titration control was selected, you have to define the step size (Fig. 97). Fig. 97 Linear step size can be set from 0.0005 to 5.000 ml (Fig. 98) Fig. 98 Linear step width can also be set for End-Point titration (pH, mV and dead stop). In this type of titration, linear step width is used after the first continuous titration stage.
  • Page 50 4.6.4.5 Pretitration If the titration agent consumption is roughly known, you can set a pretitration volume. In this process, a defined volume is dosed (= pretitrated) following the initial waiting time. After the addition of the pretitration volume, another defined span of time is observed as the waiting time before the next titration step is added. The pretitration volume is automatically added to the titration agent consumption.
  • Page 51 Fig. 102 Automatic detection of the equivalence point (EQ) can be switched on and off for linear or dynamic titration (Fig. 103). Fig. 103 If automatic EQ detection is off, titration will continue to the predefined end value in mV or pH or to the maximum ml value, respectively.
  • Page 52: Titration Parameters "End-Point Titration

    Setting of the «maximum titration volume» (Fig. 105) should always make sense. It also serves as a safety criteria to prevent excessive titration, i.e. a possible overflow of the titration vessel. The maximum titration volume can be set between 1.000 and 999.999 ml: Fig.
  • Page 53: Dosing Parameter

    Dosing parameter 4.6.6 The dosing parameters (dosing speed, filling speed and max. dosing/titration volume) are determined for each method (Fig. 108). Fig. 108 This applies to all types of methods such as manual (Fig. 109) and automatic (Fig. 110) titration and dosing Solution Preparation (Fig.
  • Page 54 Fig. 111 The dosing speed can be set in % from 1 to 100 %. 100 % is the maximum dosing speed: Dosing unit Max. dosing speed [ml/min] 20 ml 50 ml The filling speed can be set in terms of seconds from 20 to 240. The standard setting of this value is 30 seconds. For diluted aqueous solutions the filling speed can be six to 20 seconds.
  • Page 55: Sample Identification

    Sample identification 4.6.7 In the manual titration and in the preparation of solutions it is possible to input a sample identification (Fig. 113). The possible input includes manual, automatic or no sample description at all. Fig. 113 For a sample description of the «manual», a prompt for the sample description will always be displayed at the start of the method (See also ...
  • Page 56: Documentation

    Documentation 4.6.8 Three different format settings are available for documentation (Fig. 115) on a printer or USB device: «short», «standard (with curve) » and «GLP» (Fig. 116). Fig. 115 Fig. 116 Method type Short documentation Standard documentation GLP-documentation Same as ‘Short Same as ‘Standard Automatic Method name, date, time, duration of...
  • Page 57: System Settings

    System settings Fig. 117 From the main menu (Fig. 117) you can access the system settings with <MODE> (Fig. 118). Fig. 118 Setting the national language was already described in  2.4. Calibration settings The Calibration settings item is used to select the buffers for the calibration of the pH electrode as well as to set the temperature of the buffer solution (Fig.
  • Page 58 The temperature can be set from 0.0 to 100.0 °C in increments of 0.1 ° (Fig. 120). Fig. 120 The type of calibration items is used to define whether a 2-, 3-point calibration has to be performed (Fig. 121). Fig. 121 The pH buffers 1 –...
  • Page 59 A list of technical and so-called DIN/NIST buffers will appear (Fig. 123). Fig. 123 After having determined the buffers, the selection is to be confirmed with «Accept values». If the distance between 2 buffer values is too small (for instance, buffer 1 “6.87” and buffer 2 “7.00”), an error message will appear (Fig.
  • Page 60 Replacing the dosing unit 5.2.1 As a rule, the need for replacing the dosing unit occurs only rarely. The dosing unit has to be replaced, if such a replacement becomes necessary as a result of a defect, or of an inspection of the titration unit. The dosing unit is equipped with lateral ribs around its circumference, with one of these ribs being in double design.
  • Page 61 Now unlock the dosing unit (Fig. 129). Fig. 129 Confirm with <ENTER>/<OK> after the attachment has been unlocked. Now, the attachment will be raised all the way up (Fig. 130). Fig. 130 You can now change the attachment (Fig. 131). Fig.
  • Page 62 Pull the attachment off toward the top (Fig. 132). Fig. 132 Attach the new dosing attachment in the same manner (Fig. 133). The two struts of the UV protection must match up with the marking on the housing! Fig. 133 Confirm with <ENTER>/<OK>...
  • Page 63 If you want to change reagents, you can reset the data completely (Fig. 135). Fig. 135 The attachment then moves down again (Fig. 136) and you will be asked to lock the attachment (Fig. 137). Fig. 136 Fig. 137 The following reagents can be entered (Fig. 138 - Fig. 139): ...
  • Page 64: Replacing The Titration Solution

    Fig. 138 Fig. 139 Replacing the titration solution 5.2.2 If titration solutions are to be changed, since differing analysis methods are used, one should first consider whether the time required for frequent changes is not more expensive than the acquisition of another dosing unit. As a principle and in the case of all piston/cylinder- systems, a substitution of the titration solution by another one involves mixing and carry-over processes.
  • Page 65: Globale Memory

    Globale Memory The handling with the global memories is already described in 4.6.3.6 Global Memories. RS-232 Settings ® The «RS232 settings» item can be used to determine the device address of the TitroLine 5000 and set the parameters of the two RS-232 interfaces independent from each other (Fig. 140). Fig.
  • Page 66 It may be set to 1200 - 19200 (Fig. 143). Fig. 143 The parity can be selected amongst «No», «Even» and «Odd». «No» is the default setting (Fig. 144). Fig. 144 You may select between 7 and 8 data bits. 8 bits is the default setting (Fig. 145). Fig.
  • Page 67 You can set data bits at 1, 1.5 and 2. 1 bits is the default setting (Fig. 146). Fig. 146 The RS232-1 can be converted from RS on USB (Fig. 147). Fig. 147 After switching from RS232 to USB and vice versa, a restart is always necessary (Fig. 148). Fig.
  • Page 68: Date And Time

    Date and Time The factory time setting is Central European Time. This setting may be changed, where necessary (Fig. 149). Fig. 149 RESET RESET will reset all settings to the factory setting. All methods will also be deleted! So please print the methods or export/copy them to a connected USB storage medium (this will be possible with a higher update!).
  • Page 69: Stirrer

    Stirrer Stirrer «On» means, that the magnetic stirrer TM 50 can also be used for stirring if now method has been executed. This is the standard setting (Fig. 152). Fig. 152 If the stirrer is set to «Off», it is only started if a method is executed. Device Information This point contains information about the device (Fig.
  • Page 70: Data Exchange

    5.11 Data exchange All methods with all parameter settings and global memories can be stored and restored on a connected USB- memory. It is also possible to transfer the settings from one titrator to another one. The backup will be started with «Settings backup»...
  • Page 71 The backup folder on the USB-memory Stick starts with the backup date (Fig. 158). Fig. 158 Confirm the selection with <ENTER>/<OK>. “Settings are being restored” is displayed during the restoring process of the backup in blue (Fig. 159). Fig. 159...
  • Page 72: Software Update

    5.12 Software Update Fig. 160 An update of the device software (Fig. 160) requires a USB stick containing a new version. For this operation, the two files that are needed have to be located in the root directory of the USB device (Fig. 161). Fig.
  • Page 73 After starting the update using <ENTER>/<OK>, next thing to appear is the following graphic (Fig. 163), Fig. 163 which will change after a few seconds to the following display (Fig. 164). Fig. 164 Upon completion of the update (approx. 4 - 5 minutes), the device will shut down the software completely and proceed to a new start.
  • Page 74 Communication via RS-232 and USB-B interface General Information ® The TitroLine 5000 has two serial RS-232-C interfaces to communicate data with other devices. By means of these two interfaces it is possible to operate several devices on one computer (PC) interface. In addition to that, ®...
  • Page 75 Command Description Reply aaAA automatic allocation of device address aaMC1...XX choosing a method “filling burette“. Aufsatz wird gefüllt. aaBF aaBV output of dosed volume in ml aa0.200 aaDA dose volume without filling, with adding the volume aaDB dose volume without filling, reset of the volume aaDO dose volume with filling, without adding the volume aaGF...
  • Page 76 7 Connection of Analytical Balances and Printers Connection of Analytical Balances As it often happens that the sample is weighed in on an analytical balance, it makes sense to connect this ® balance to the TitroLine 5000. The balance must have a RS-232-C-interface and the connection cable must be configured accordingly.
  • Page 77 Balance data editor Pressing «F5/balance symbol» will invoke the so-called balance data editor. A list with the existing balance data will appear (Fig. 166). Fig. 166 The balance data can be edited one by one. Following a change, a star will appear opposite the weighed-in quantity (Fig. 167). Fig.
  • Page 78 If no balance data is available, the «No balance data found» message will appear (Fig. 169). Fig. 169 Printers The results, calibration data and methods can be printed on the following media  HP PCL compatible printer (A4)  Seiko DPU S445 (Thermo paper 112 mm width) ...
  • Page 79 Maintenance and Care of the Titrator The preservation of the proper functioning of the device requires testing and maintenance work to be performed on a regular basis. Regular inspections are essential prerequisites for the correctness of the volume and the proper functioning. The accuracy of the volume is determined by all chemicals-carrying components (piston, cylinder, valve, titration tip and hoses).
  • Page 80 Detailed description of the inspection and maintenance work Wipe off using a soft cloth (and some water with a normal household detergent). Leaking connections can be identified by moisture or crystals at the threaded connections of the hoses, at the sealing lips of the piston inside the dosing cylinder or at the valve. If any liquid becomes visible below the first sealing lip, it has to be checked at short timely intervals whether any liquid will build up under the second sealing lip, too.
  • Page 84 SI Analytics Gebäude G12, Tor Rheinallee 145 55122 Mainz Deutschland, Germany Tel. +49(0)6131.66.5042 Fax. +49(0)6131.66.5105 E-Mail: Service-Instruments.si-analytics@xyleminc.com SI Analytics is a trademark of Xylem Inc. or one of its subsidiaries. © 2020 Xylem, Inc. Version 200826 US 825 288 2...

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