G20 Operating Manual 4v5t3n

Drives on which the burettes with titrant are installed. Cycles Defines the number of rinse cycles to be executed.

Range of options No | Yes 1…100

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The drives can only be seen if they are connected.

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Drives that are equipped with a PnP burette are opened again at the specific fill rate of the titrant, whereas conventional drives are opened at 100% fill rate.

4.5.3 Dispense Navigation: Home > Manual > Burette > Dispense The "Dispense" operation lets you manually dispense a defined quantity of titrant. a) Select the titrant you would like to dispense. b) Select the drive on which the titrant is installed. (For PnP burettes, the system automatically selects the appropriate drive.) c) Enter the volume to be dispensed in [mL]. d) Enter the filling rate in [%] to define the speed at which you want to refill the burette. (100% is the maximum rate.) e) Press "Start" to start the dispensing procedure. f)

You can select "Stop" to terminate the procedure at any time.

You can determine the following parameters: Parameters

Explanation

Range of options

Titrant Drive

You can select a titrant from the titrants defined in the setup. Defines the drive on which you will use the burette containing the titrant. The volume to be dispensed, in [mL]. The filling rate of the burette in percent. 100% stands for maximum filling rate.

Titrant list 1|2

Volume Fill rate

40

0.001…100 30…100

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Manual Operations

4.5.4 Manual titration Navigation: Home > Manual > Burette > Manual Titration To perform a manually controlled titration, proceed as follows: a) Select the titrant you would like to titrate with. b) Select the drive on which the titrant is installed. (For PnP burettes, the system automatically selects the appropriate drive.) c) Enter the filling rate in [%] to define the speed at which you want to refill the burette. (100% is the maximum rate.) d) Select the sensors you would like to use for the measurement from the list of sensors defined in the setup. e) Select the stirrer output for the stirrer and enter a speed. f)

Specify whether or not you want to run a manual temperature acquisition.

g) If you do not want automatic temperature acquisition, enter the temperature. h) If you want automatic temperature acquisition, select a connected temperature sensor. i)

Select whether the results should be given in the form of consumption (of the titrant) or content (in the sample).

j)

Select the measurement unit and the number of decimal places for the results.

k) For results given as content, select the sample's entry type (volume or weight) and enter the sample quantity m, the density d (for the volume or weight entry types), the molar mass M and the equiva lent number z for the substance to be tested. l)

Specify whether a record should be output to the printer and select which elements should be con tained in that record (results, table of measured values and curve).

m) Press "Start" to start the manual titration and move to the online dialog. n) Press the "Dispense" button once to add a minimum volume of titrant. If you hold down the "Dis pense" button, the system will continuously add titrant. The dispensing rate will increase as you hold down the button. After you release the button, the system will titrate at the minimum speed again the next time the button is pressed. o) Press "Exit" to end the manual titration. During the manual titration, the system will display the measured value, the titrant consumption, and a curve (measured value versus consumption) on the screen. After you finish, a record can automatically be output to the printer. You can also view the results, measured values and curve on the screen. For the results of the manual titration, the system takes as a basis the titrant consumption until the con clusion of the titration. The EQP is not calculated! You can determine the following parameters: Parameters

Explanation

Range of options

Titrant Drive

Titrant list 1|2

Sensor

You can select a titrant from the titrants defined in the setup. Defines the drive on which you will use the burette containing the titrant. The filling rate of the burette in percent. 100% stands for maximum filling rate. The name of the sensor.

Sensor input

The input to which you want to connect the sensor.

Fill rate

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30…100 Sensor list of the sen sor type selected in Setup SENSOR | PT1000

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Manual Operations Unit

Ipol Upol

Titration stand

Speed Temperature manual Temperature

Temperature sensor Sensor input Temperature unit Result

Unit Unit Decimal places Entry type Sample size Density M Report Incl. Results Incl. Measured value table Incl. Curve

The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F Ipol is the polarization current, in [µA], for the voltametric 0.0…24.0 indication. Upol is the polarization voltage, in [mV], for an amperometric 0…2000.0 indication. (Only for polarized sensors with "indication" = "amperometric".) The name of the titration stand. Select the titration stands from the list specified in Setup. Speed in [%]. 0…100 Defines whether to enter the temperature manually ("yes") or No | Yes via a temperature sensor ("no"). If the temperature is entered manually, you can enter it here, -20…200 in [°C]. (Only appears if "Temperature manual" = "Yes" was selected.) Here you can select the required temperature sensor (only Sensor list appears if "Temperature manual" = "No" is selected). The input to which you want to connect the sensor. SENSOR | PT1000 The unit of measure for the temperature measurement (°C | °C | K | °F K | °F). (Only appears if "Temperature manual" = "No" was selected.) Here you can select whether to output the result of the manual Consumption | Content titration as the amount of titrant consumed or as the content in the sample. The unit for stating the result in the form of the titrant con mL | mmol sumption. (Only for "Result" = "Consumption".) The unit for stating the result as the sample content. (Only for mol/L | mol/kg | g/L | "Result" = "Content".) g/kg | % | ppm Specify the required number of decimal places for the results. 1...4 The entry type for the sample size, either "Weight" or "Vol Weight | Volume ume" (only for "Result" = "Content"). The sample size, in [mL] or in [g], depending on the entry 0.0001…100 type selected. (Only for "Result" = "Content".) The density of the sample substance to be determined, in 0.0001…100 [g/mL]. (Only for "Result" = "Content".) The molar mass of the substance [g/mol]. List Defines whether to output a record to the printer after the titra Yes | No tion. Here you can specify whether the record should contain all Yes | No the results. (Only appears for "Record" = "Yes".) Here you can specify whether the record should contain a Yes | No table of measured values. (Only appears for "Record" = "Yes".) Here you can specify whether the record should contain a Yes | No curve. (Only appears for "Record" = "Yes".)

The parameters for temperature acquisition or entering the temperature, "Temperature manual", "Tempera ture", "Temperature sensor", "Sensor input" and "Temperature unit" are omitted for mV sensors and the phototrode.

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Methods

5 Methods To carry out an analysis with the titrator, you require a method. A method is an analysis program and consists of a sequence of method functions (some with method subfunctions), which are processed by the titrator in sequence. In this chapter, you will learn how to access and define methods. The basic building blocks of a titration method consist of sample preparation, stirring and wait times, the actual titration, result calculation and a record. The titrator defines these partial steps as functions that consist of parameters whose values can be changed. Loops Within a method you can define one loop, which can run the series analysis n-times. (see Method Syn tax - Rules for Creating a Method"). The beginning and end of a sample loop are defined by the method functions "Sample" and "End of Sample". The "End of Sample" method function is executed, and the sample loop stopped, only after the last sample in a series. There are the following loop types: ●

A sample loop is for analyzing a sample.

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A calibration loop is for calibrating a sensor.

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A titer loop is for determining the titer of a titrant.

Types of Methods The titrator distinguishes between the following method types with different objectives: ●

GT Method for general titration (contains only sample loops or mixed loops)

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Calibration method for sensor calibration (contains only calibration loops).

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Titer Method for titer determination, contains only titer loops

Preloaded Methods A number of methods have already been stored in the device. These methods were developed by METTLER TOLEDO for specific uses and can be used immediately for the corresponding analysis. You can change these methods in line with your requirements and save them as methods. When creating methods you can revert to method templates, which, according to their objective, specify the structure of the method, and whose parameters already contain the most suitable default values. Method ID You can distinguish between different types of method and individual methods of the same type using their ID:

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Each method has its own unique method identification.

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The method ID of the METTLER TOLEDO methods is composed of the starting letter "M" followed by a sequential number (M001, M002, …)

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The method ID for a method can be chosen at random, however it cannot begin with an "M" fol lowed by a number.

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Methods

5.1 METTLER TOLEDO Methods METTLER TOLEDO methods are preprogrammed methods for executing specific applications (e.g. chlo ride in ketchup). These methods are stored in the device prior to shipping (Methods List) and can be started immediately by the . METTLER TOLEDO methods not only provide the sequence of the method functions, but they also define all of the method function settings. A METTLER TOLEDO method can be saved as a method by saving it under a different method ID. ID M400 M401 M402 M403 M404 M405 M406 M407 M408 M409 M410 M411 M412 M413 M414 M415 M416 M417 M418 M419 M424 M425 M426 M427 M428 M429 M430 M431 M432 M435 M436

Titel Acetic acid in vinegar Ammonium chloride content Free fatty acid content Blank solvent FFA Chloride content in Ketchup Total hardness of tap water Ca + Mg content of tap water Sulfate content Barium content conductometric Copper content Hydrogen peroxide content Vitamin C content voltametric Vitamin C content amperometric SDS content photometric SDS content potentiometric m-Value of tap water (EP) p-Value of tap water Antacid (Stating) HCl content Free SO2 content in wine Bromine number ASTM D1159 Blank ASTM D1159 Acid number ASTM D664 Acid number ASTM D664 Base number ASTM D4739 Blank ASTM D4739 Base number ASTM D2896 Blank ASTM D2896 Chloride content in motor oil Titer 0.1 mol/L NaOH Calibration DG111-SC

Beschreibung EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EP-Titration EP-Titration pH-Statierung EP-Titration EP-Titration EP-Titration EP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration EQP-Titration Messung

M449 M454 M455

Nitrogen Kjeldahl with K-360 Nitrogen Kjeldahl TTL Nitrogen Kjeldahl Manual

EQP-Titration EP-Titration EP-Titration

Titriermittel NaOH NaOH KOH in Ethanol KOH in Ethanol AgNO3 EDTA EDTA BaCl2 Li2SO4 Na2S2O3 KMnO4 DPI DPI Hyamin Hyamin HCl NaOH NaOH NaOH J2 Bromide-Bromate Bromide-Bromate KOH in 2 Propanol KOH in 2 Propanol HCl in 2 Propanol HCl in 2 Propanol HClO4 in acetic acid HClO4 in acetic acid AgNO3 in 2 Propanol 0.1M NaOH pH Puffer: 4.01, 7.00, 9.21 1/2 H2SO4 1/2 H2SO4 1/2 H2SO4

Sensor DG111 DG111 DG113 DG113 DM141 DP5 Ca ISE Ba ISE InLab717 DM140 DM140 DM143 DM143 DP5 DS500 DG111 DG111 DG111 DG111 DM143 DM143 DM143 DG113 DG113 DG113 DG113 DG113 DG113 DM141 DG111 DG111-SC DG111-SC DG111-SC DG111-SC

5.2 Establishing Methods You create a new method by changing the parameters of a delivered METTLER method and saving it under a new method ID or by selecting an appropriate method template from the list of proposals, modi fying it, and saving it under a new ID. Select: Home > Methods a) Choose New to create a new method on the basis of a template.

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Methods b) From the available templates, choose the one that is most similar to the method you wish to create. You can now modify this method in line with your requirements by inserting or removing method functions or modifying its parameters. c) In the "Title" method function, enter a new method ID. Afterwards, a new method will be stored under this method ID. d) Assign a title to your new method. e) Select available method functions to modify their parameters in line with your requirements. f)

Choose Insert to add additional method functions to the template.

g) Now use the arrow-shaped "Insert" button to select the required position for the new method function in the method. (You will only be able to insert the method functions that are allowed in the corre sponding location based on the method syntax.) h) From the list, select the method function that you want to insert. i)

Modify the individual parameters of the method function in line with the resources. The new method function appears in the method.

j)

To delete a method function, select the function in question and then choose Delete. The method function disappears from the method.

k) After inserting all required method functions, you can store the new method in the titrator by choos ing Save. When establishing a new method, follow the rules specified by the titrator. These are described in Chap ter "Method Syntax – Rules for Establishing Methods".

5.2.1 Method Templates When you create a new method, the method templates prescribe the sequence of the method functions. These method templates are not application-specific, but are dependent on the type of titrator. They allow the to establish methods quickly and easily. Most of the settings in the method functions that occur in a standard method already have default values. To convert a method template into a method, it has to be saved under a method ID. Title Description Method type EQP Equivalence point titration General titration EP End point titration General titration Measure Is used for the controlled transfer of a sensor mea General titration suring value. Lern-EQP Is used to determine the best parameters for carry General titration ing out an EQP titration. Titer with EQP Titer determination by EQP titration Titer determination Titer with EP Titer determination by EP titration Titer determination Calibration Sensor calibration (linear regression for all mea Calibration surement points) Segmented calibration Sensor calibration, taking into non-linear Calibration sensor behavior Blank with EQP Blank value determination of a solvent using the General titration equivalence point titration Blank with EP Blank value determination of a solvent using the General titration end point titration pH Sensor test To check the slope, zero point and drift of pH-sen Calibration sors.

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Methods

5.3 Modifying or Deleting Methods You can change methods or METTLER methods and store them under new method IDs. Once a METTLER method has been modified, you will only be able to save it as a copy (or as a method) with a new method ID. Modifying a method To modify a method, select: Home > Methods a) From the displayed list of methods, select the method that you want to modify. b) As soon as the methods functions of the selected method appear on the screen, you can modify the method. c) In the "Title" method function, enter a new method ID. Afterwards, a new method will be stored under this method ID. You can enter up to twenty alphanumeric characters. d) Select available method functions to modify their parameters in line with your requirements. e) Choose Insert to add additional method functions to the template. f)

Now use the arrow-shaped "Insert" button to select the required position for the new method function in the method. (You will only be able to insert the method functions that are allowed in the corre sponding location based on the method syntax.)

g) From the list, select the method function that you want to insert. h) Modify the individual parameters of the method function. The new method function appears in the method. a) To delete a method function, select the function in question and then choose Delete. b) After you have made all of the necessary adjustments, you can store the method in the titrator by choosing Save. Deleting Methods You can easily delete -defined methods from the titrator. Select: Home > Methods a) Select the method that you want to delete. b) Choose Delete method to delete the method from the titrator's memory.

5.4 Starting Methods The titrator offers various ways of starting a method: ●

From the method editor

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By choosing Start from the Home dialog

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By using a shortcut on the Home screen

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Via the Series dialog

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By using the "Setup" dialog (to perform a calibration or titer determination)

You can use the method editor to start any method stored in the titrator. a) From the displayed list in the Methods dialog, select the method that you wish to start (Home > Methods).

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Methods b) As soon as the method functions of the selected method appear on the screen, you can open the Start analysis screen by choosing Start. c) Choose Start again to reach an overview screen on the resources required for the method. (Only if this was defined in the analysis sequence settings.) d) To execute the method, confirm the screen by choosing OK.

5.5 Stopping Methods Analyses or series of analyses that are in progress can be interrupted or terminated by the in order to intervene in the analysis process or by the titrator itself. The options available in the event of an interruption of the analysis procedure are listed below.

5.5.1 Suspension of an ongoing analysis by the If you wish to make changes when an analysis or series of analyses is in progress, you can interrupt the analysis procedure. Stop the relevant method as follows: Press Stop. The following options appear: Save the series The complete series assigned to the interrupted analysis is saved as a file in the form "SeriesXY". ●

If the maximum permitted number of series (see "Series templates") has been reached, the series is not saved.

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Sample data from a method that is waiting in a queue can be saved by selecting "Suspend" and "Save series data".

Skip current sample The analysis continues with the next sample. The current sample is marked in "Results" as "Skipped". Skipping the current sample loop The analysis omits the current sample loop and continues with the next one. The loop is marked in "Results" as "Skipped" The samples that have been skipped are automatically excluded from the statistics. This applies to all results for the sample; also those that were listed before the sample was skipped. If required, you can still use the "Results" dialog to include the sample in the statistics once the analysis is complete. Further, you can decide whether you wish to cancel or continue the analysis: To do so, choose Continue to continue the analysis or Stop definitely to terminate the interrupted analy sis.

5.5.2 Interruption of an ongoing analysis by the titrator The titrator can interrupt an analysis that is in progress for the following reasons: ●

Exceeding the specified termination parameter "Termination" for the methods "titration (EQP) and titration (EP)".

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Due to end or equivalent points not being found during learn titrations. If no end or equivalent points are found during a learn titration an error message appears and the analysis is interrupted. You have the option of either canceling the titration or continuing after filling a new burette.

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Methods

5.6 Method Syntax – Rules for Establishing a Method A method consists of a sequence of method functions that are executed consecutively when a method is processed. When establishing a method, certain rules (method syntax) must be followed. These funda mental rules are described below:

5.6.1 Types and Possible Number of Loops Nested loops are not permitted. Loops can only be inserted into or deleted from a method as a whole. The number of loops allowed in a method differs depending on the method type and device type: Methodentyp Erlaubte Loop-Typen Maximale Anzahl von Loops pro Methode GT

Titer Kalib.

Sample loop Titer loop Calibration loop Titer loop Calibration loop

1

1 1

5.6.2 Sample Loops The following loop types are available for the various methods for general titration (GT): Sample loop (GT): Sample Titration stand (manual stand) Stir Titration (EQP) Calculation Record Titer loop:

End of sample Sample (Titer) Titration stand (manual stand) Stir Titration (EQP) Calculation Record End of sample

Calibration loop:

Titer Sample (calibration) Titration stand (manual stand) Stir Measure (normal) End of sample Calibration

5.6.3 Inserting and Deleting Loops The following description applies particularly for the GT method type. Only entire loops can be inserted into or deleted from a method. 48

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Methods When you insert a loop using the "Sample", "Sample (Titer)", and "Sample (Calib)" method functions, a regular, correct template that varies according to the loop type is inserted. When deleting one of the stored method functions listed above in gray, the entire loop will be deleted from the method, including all of the method functions it contains.

5.7 Overview of Method functions The number of method functions that can be used within a method is limited. The maximum number of method functions is 11. Functions

Explanation

Possible No. of MFs

Within loop

Out of loop

Title

Title and characteristics of the method. Start of a sample loop. Start of a loop for titer determina tion Start of a loop for sensor calibra tion. Selects titration stand. Pumps a defined volume of a liq uid. Activates a stirrer. Dispenses a defined quantity of titrant. Takes over monitoring a measured value from a sensor. Conducts an equivalence-point titration. Conducts an end-point titration. Conducts an equivalent-pointdetection titration. Converts the analysis results. Concludes a sample loop.

1

No

Yes

total 1

Start of loop

1 2

Yes Yes

No Yes

2 1

Yes Yes

No Yes

total 1

Yes

No

Yes

No

Yes Yes

No No

2 1

Yes End of loop

Yes Yes

total 1

No

Yes

No

Yes

1

Yes

Yes

2

Yes

Yes

1

Yes

Yes

2

Yes

Yes

Sample Sample (titer) Sample (cali bration) Titration stand Pump

Stir Dispense (normal) Measure (nor mal) Titration (EQP) Titration (EP) Titration (LearnEQP) Calculation End of sam ple Titer Assigns the result of a titer sample loop to a titer. Calibration Assigns the result of a calibration loop to a sensor. Blank Assigns a result or an arbitrary val ue to a blank and updates the val ue stored in Setup. Auxiliary Activates external auxiliary instru instrument ments. Drain Drains a volume from the sample vessel.. Record Defines the record data to be out put to the printer.

5.8 Method functions All parameters that can be defined for the following method function are described below.

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Methods

5.8.1 Title Defines the title and type of a method and manages properties such as the creation and change date, the author, and whether or not the method is to be protected. Parameters

Explanation

Range of options

ID

Unique ID of the method.

Title Protect

Title of the method. Protects the method against changes and deletion by any other than the author or the istra tor. Standard operating procedure (SOP: (SOP) Text for a standard operating procedure (if "SOP" = "text" is selected.) ID for the link to a standard operating procedure (if "SOP" = "link" is selected.)

arbitrary (cannot start with "M" followed by a numeric character) Arbitrary Yes | No

SOP SOP-Text SOP ID

None | Text | Link Arbitrary text Arbitrary

5.8.2 Sample The "Sample" and "End of sample" method functions define the beginning and the end of a sample loop. All of the method functions contained in a loop are conducted for each sample in a series. The method functions are conducted in accordance with "End of Sample" only after processing the last sample. Parameters

Explanation

Range of options

Number of IDs ID 1 ID 2-3

Defines the number of sample IDs to be defined. The ID for the first or only sample of an analysis. The name defined here will be used as the default name for the respective sample on the sample loop. (Only appears subject to the settings made for "Number of IDs".) Defines whether the sample should be added with a defined mass, defined volume or defined number of pieces. The sam ple data query will then adjust according to the unit of mea surement. By selecting "fixed volume" or "fixed number of pieces" the sampling weight, sample volume or number of pieces will be entered as the parameter in this method func tion and will not be prompted when conducting the method. Defines the lower limit for the variable entry of data. The unit will depend on the setting for the "entry type" parameter. Does not appear for "fixed" entry types. Defines the upper limit for the variable entry of data. The unit will depend on the setting for the "entry type" parameter. Does not appear for "fixed" entry types. Weight in [g]. Appears only if "entry type" = "fixed weight" was selected. Volume in [mL]. Appears only if "entry type" = "fixed volume" was selected. The number of sample(s). Appears only if "entry type" = "fixed number of pieces" was selected. The weight in [g] per item. Appears only if "entry type" = "number of pieces" or "fixed number of pieces" was selected.

1…3 Arbitrary Arbitrary

Entry type

Lower limit

Upper limit

Weight Volume Pieces Weight per piece

50

Weight | Volume | Number of pieces | Fixed weight | Fixed volume | Fixed num ber of pieces

[g]: 0 … 1000 [mL]: 0 … 1000 [pcs.]: 0 … 106 [g]: 0 … 1000 [mL]: 0 … 1000 [pcs.]: 0 … 106 0…1000 0…1000 0…106 0…1000

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Methods Density

The density of a liquid sample substance, in [g/mL]. Appears only if "entry type" = "weight", "volume", "fixed weight" or "fixed volume" was selected. Correction factor Any correction factor that can be used in calculations. Temperature The temperature in [°C] during the analysis. If temperature monitoring is activated in a titration function, the system will ignore the sample temperature given here. Entry Determines the entryt time for the sample size. If you select "Before", the sample size must be entered before the titration. If "Arbitrary" is selected, the sample size will have to be entered at any time during the titration (no later than when it is used during the calculations). Only appears if "Fixed" val ues are not selected for "Entry Type".

0.0001…100

0.0001…106 -20…200

Before | Arbitrary

5.8.3 Sample (titer) Start of a loop for titer determination Contains all of the necessary data regarding the titrant and the stan dard to be used. Parameters

Explanation

Titrant Standard

You can select a titrant from the titrants defined in the setup. Select the name of the standard from the standards list.

Range of options

Titrant list Select from the stan dards defined in the setup. Entry type Defines whether the quantity (weight or volume) of a liquid or Weight | Fixed weight | solid standard should be entered when the analysis is started Volume | Fixed vol or whether a "fixed weight" or a "fixed volume" should be ume | Number of defined in the method function. pieces | Fixed number of pieces Lower limit Defines the lower limit for the variable entry of sample data in 0...1000 [ml] or [g]. The unit will depend on the setting for the "entry type" parameter. (Applies only for the entry type "Weight" and "Volume".) Upper limit Defines the upper limit for the variable entry of data. The unit 0…1000 will depend on the setting for the "entry type" parameter. Does not appear for "fixed" entry types. Weight Weight in [g]. Appears only if "entry type" = "fixed weight" 0…1000 was selected. Volume Volume in [mL]. Appears only if "entry type" = "fixed volume" 0…1000 was selected. Correction factor Any correction factor that can be used in calculations. 0.0001…106 Temperature The temperature in [°C] during the analysis. If temperature -20…200 monitoring is activated in a titration function, the system will ignore the sample temperature given here. Entry Determines the entryt time for the sample size. If you select Before | Arbitrary "Before", the sample size must be entered before the titration. If "Arbitrary" is selected, the sample size will have to be entered at any time during the titration (no later than when it is used during the calculations). Only appears if "Fixed" val ues are not selected for "Entry Type".

5.8.4 Sample (calibration) Start of a loop for sensor calibration. Contains all of the necessary data regarding the sensor and the cal ibration standard.

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Methods Parameters

Explanation

Range of options

Sensor type Sensor

Specifies the type of sensor that is calibrated The name of the sensor.

Action

Performing a calibration or a pH-sensor test.

pH | ISE | Temperature Sensor list of the sen sor type selected in Setup Calibration | Sensor test

For more information about the method function for the pH-sensor test, refer to "Methods: Method func tions > Method functions for the pH-sensor test" Unit The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F Automatic buffer Defines whether the titrator should automatically identify the Yes | No recognition buffers via the pH buffer list. Only possible for pH sensors. pH buffer list Defines the pH buffer list to be used for the calibration of a pH Select from the pH sensor. buffer lists (Auto pH buffer lists) defined in Setup. List of stan Defines the standards list to be used for the calibration of an Select from the stan dards ISE or conductivity sensor. dards lists defined in Setup. Calibration Here you can define whether the calibration of a pH or ISE Linear | Segmented sensor should be done in a linear or segmented manner. Number of The number of buffers to be used for the calibration of a pH 1…9 buffers sensor. Number of stan The number of standards to be used for the calibration of an 1…9 dards ISE sensor. Buffer 1-9 For the calibration of a pH sensor, up to nine buffers can be Select from the buffer selected from the pH buffer list. list. Standards 1-9 For the calibration of an ISE sensor, up to nine standards can Select from the stan be selected from the standards list. dards list. Standard Select the name of the standard from the standards list. Select from the stan dards defined in the setup. Temperature The temperature during the calibration in [°C] if temperature -20°C…200°C acquisition has not been selected in the "Measurement (nor mal)" method function. Does not appear for temperature sen sors.

5.8.5 Titration stand You can use the following parameters to specify the relevant titration stand. Parameters

Explanation

Range of options

Type

Defines the type of titration stand to be used.

Titration stand

The name of the titration stand.

Rondolino TTL | Manu al stand | Auto stand | External stand Select the titration stands from the list specified in Setup.

5.8.6 Pump You can use this method function to drain a reagent into a sample vessel.

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Methods Parameters

Explanation

Range of options

Auxiliary reagent

The auxiliary reagent to be added.

Volume

The volume to be pumped, in milliliters.

Select from the auxil iary reagents defined in Setup. 0…1000

5.8.7 Stir Activates or deactivates (speed ="0") the stirrer of the current titration stand. Parameters

Explanation

Range of options

Speed Duration

Speed in [%]. 0…100 The stirring time, in [sec]. 0 … 105 After the stirring time has elapsed, the titrator will continue to the next method function without switching off the stirrer. The stirrer is switched off after the analyis is finished or the beaker is changed. The stirrer output is defined by the prior method function "Titration stand".

5.8.8 Dispense (normal) You can use this method function to dispense a precisely defined quantity of titrant. The smallest increment (dV(min)) is 1/20000 of the burette volume, i.e. for the following burettes: 1 mL burette: dV(min) = 0.05 µL 5 mL burette: dV(min) = 0.25 µL 10 mL burette: dV(min) = 0.50 µL 20 mL burette: dV(min) = 1 µL Parameters

Explanation

Range of options

Titrant Volume Dosing rate

You can select a titrant from the titrants defined in the setup. Volume in [mL]. Defines the dosing rate (not including the filling time), in [mL/min]. You can also select a burette type-dependent maximum number.

Titrant list 0.0001…1000 0.01…60

5.8.9 Methods with subfunctions The method functions described below have subfunctions with their own parameters: ●

Measure (normal)

●

Titration (EQP)

●

Titration (EP)

●

Titration (LearnEQP)

5.8.9.1 Measure (normal) For the controlled acquisition of a measured value from a sensor. If a temperature sensor is selected for the measurement, the subfunction "Temperature acquisition" is omitted.

G20

53

Methods Subfunction: Sensor Parameters

Explanation

Type

The type of sensor to be used to perform the measurement.

Sensor

Unit

Indication Ipol Upol

Range of options

mV | pH | ISE | Pho totrode The name of the sensor. Sensor list of the sen sor type selected in Setup The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F Defines how to do the indication. Depending on the unit of Voltametric | Ampero measure: [mV] = voltametric, [µA] = amperometric. metric Ipol is the polarization current, in [µA], for the voltametric 0.0…24.0 indication. Upol is the polarization voltage, in [mV], for an amperometric 0…2000.0 indication. (Only for polarized sensors with "indication" = "amperometric".)

Subfunction: Temperature acquisition Parameters

Explanation

Temperature acquisition

Defines whether to record the temperature, with the aid of a Yes | No temperature sensor, during the execution of the analysis func tion. Defines which temperature sensor to use for the temperature Sensor list acquisition. (Only if "Yes" was selected for temperature acqui sition.) The temperature unit you want to use. °C | K | °F

Temperature sensor Unit

Range of options

Subfunction: Stir Parameters

Explanation

Range of options

Speed

Speed in [%].

0…100

Subfunction: Acquisition of Measured Values Parameters

Explanation

Range of options

Acquisition

Defines how the measured value is acquired. Equilibrium Con Equilibrium-controlled: The measured value is acquired as trolled | Fixed | Set soon as it stabilizes. Value - Fix: The measured value is acquired after a defined waiting period. - Set value: The measured value is acquired as soon as it has exceeded, or fallen short of, a specific set value. (The Set Value option is not available if the method function is used within a Sample (Calib) loop.)

The following parameters are available for the sensor types: mV, pH, ISE, Phototrode, Polarized Parameters

54

Explanation

Range of options

G20

Methods dE

dt t(min) t(max) Time Mode

Set value

t(max)

Mean value No. of mea sured values dt

Defines the measured value interval. As soon as the change in the measured value over the time period dt is less than dE, the measured value will be acquired. This occurs within the defined time interval of t(min) to t(max). dE is specified in the unchanged unit of the sensor per sec ond: - mV for the mV sensor type, pH, ISE, phototrode and polar ized voltametric - µA for polarized Defines the time component, in [sec] for dE/dt. (For "acquisi tion" = "equilibrium-controlled" only.) Earliest possible time for the measured value acquisition, in [sec]. (For "acquisition" = "equilibrium-controlled" only.) Latest possible time for the measured value acquisition, in [sec]. (For "acquisition" = "equilibrium-controlled" only.) Waiting time, in [sec], before acquisition of a measured val ue when "acquisition" = "Fixed". Mode for the measured value acquisition of the "set value". E > Set value acquires the measured value as soon as the set value has been exceeded. E < Set value acquires the measured value as soon as the measured value falls below the set value. Not available with in a calibration loop (only for "acquisition" = "set value"). Set value in the sensor unit. Measured values will be acquired after they exceed or fall below this value, depending on the mode setting. (For "acquisition" = "set value" only.) Not available within a calibration loop. Latest time for the measured value acquisition, in [sec]. (For "acquisition" = "set value" only.) Not available within a cali bration loop. The system finds a mean value for the saved measured val ue, using a maximum of 10 measured values. When you want to calculate a mean value, you can define the number of measured values used to find that mean value here. Defines the time interval, in [sec], for the measured value acquisition of the measured values to be averaged. (Appears only if "mean value" = "yes" is selected.)

0.1 … 15

1…150 1…150 1…105 1…105 E > Set value | E < Set value

(See "Value Ranges of Sensor Measuring Units and Control Band") 1…105

Yes | No 1…10

1…60

You can define the following parameters for the temperature sensor: Parameters

Explanation

Range of options

dT

Defines the measured value interval. As soon as the change in the measured value during the time period dt is less than dT, the measured value will be acquired. This occurs within the defined time interval of t(min) to t(max). This value is specified in the unchanged unit of the sensor, per second: °C | K | °F (Only for "Acquisition" = "Equilibrium controlled".) Mode for the measured value acquisition of the "set value". T > Set value acquires the measured value as soon as the set value has been exceeded. T < Set value acquires the measured value as soon as the measured value falls below the set value. Not available with in a calibration loop (only for "acquisition" = "set value").

0.1 … 10 Unit: °C | K | °F

Mode

G20

T > set value | T < set value

55

Methods

5.8.9.2 Titration (EQP) Carries out an equivalence-point titration. You can define the relevant parameters for the following sub functions: Subfunction: Titrant Parameters

Explanation

Range of options

Titrant

You can select a titrant from the titrants defined in the setup.

Titrant list

Subfunction: Sensor Type The type of sensor to be used to perform the measurement. Sensor

Unit


Frequency

mV | pH | ISE | Pho totrode The name of the sensor. Sensor list of the sen sor type selected in Setup The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F Defines how to do the indication. Depending on the unit of Voltametric | Ampero measure: [mV] = voltametric, [µA] = amperometric. metric Ipol is the polarization current, in [µA], for the voltametric 0.0…24.0 indication. Upol is the polarization voltage, in [mV], for an amperometric 0…2000.0 indication. (Only for polarized sensors with "indication" = "amperometric".) Polarization frequency in [Hz]; (only for "Type"="Polarized" 4 | 2 | 1 | 0.5 and "Unit"="mV"). The standard frequency is 4 Hz; other val ues should only be used for special applications.


Explanation




Subfunction: Stir Speed Speed in [%].

Range of options

0…100

Subfunction: Predispensing Parameters

Explanation

Range of options

Mode

Specifies the type of addition: Volume: predispenses a specific volume. Potential: system predispenses a substance until a certain potential is reached. Factor: A multiple of the sample size is predispensed. None: does not predispense. Volume in [mL]. The potential at which you want to stop predispensing. (For "mode" = "potential" only.)

Volume | Potential | Factor | None

Volume Potential

56

0.0001…1000 (See "Value Ranges of Sensor Measuring Units and Control Band")

G20

Methods Factor

Wait time

The system calculates the predispensing volume by multiply 0 … 105 ing the factor by the sample size. (For "mode" = "factor" only.) Defines a waiting time, in [sec]. (Either after the predispens 0…32000 ing or, if "predispensing" was set to "none", before the start of titration.)

Subfunction: Control Parameters

Explanation

Range of options

Control

Here you can select from among three predefined control modes ("Normal" | "Fast" | "Cautious"), or you can select "" to define all the parameters as freely editable. If you change from "Normal", "Fast" or "Cautious" to "", the system will copy over the predefined parameter settings and they will then be freely editable. You can select an application depending on the sensor type. The selected application will then provide its own specific parameter set (not for "control" = ""). Here you can select whether to display the preset parameters of the control modes "Normal", "Fast" or "Slow" as noneditable info fields. (Not for "control" = "") Defines whether to always dispense the same volume defined by dV ("incremental") or to adjust the volume to be titrated per step as the titration progresses ("dynamic"). (For control mode "" only) Defines the potential difference targeted per titrant addition. (For control mode "" and dynamic titrant addition only) Defines the temperature difference in the unit of the tempera ture sensor that is targeted for a temperature sensor per titrant addition. (For control mode "" and dynamic titrant addi tion only) Defines the minimum amount for a titrant addition, in [mL]. (For control mode "" and dynamic titrant addition only) Defines the maximum amount for a titrant addition, in [mL]. (For control mode "" and dynamic titrant addition only.) Defines the volume increment, in [mL], for the incremental titrant addition. (For control mode "" and incremental titrant addition only) Type of measuring value acquisition: • equilibrium-controlled: The system acquires the measured value and makes the next titrant addition as soon as a stable measured value is established. • Fixed time: The measured values acquisition and the titrant addition occur according to fixed time intervals. (For control mode "" only) As soon as the change in the measured value during the time period dt is less than dE, the measured value will be acquired. Acquisition takes place no earlier than after t(min) and no later than after t(max). Then the next titrant addition is conducted. (For control mode "" and equilibrium-controlled mea sured value acquisition only) Defines the time interval, in [sec], for calculating dE/dt (or dT/dt for a temperature sensor). (For control mode "" and equilibrium-controlled measured value acquisition only)

Normal | Fast | Cau tious |

Mode

Display para meters Titrant addition

dE(set value) dT(set value)

dV(min) dV(max) dV

Meas. val. acquisition

dE

dt

G20

Application list

Yes | No

Dynamic | Incremental

0.1 … 100 0.1…100

0.0001…1 0.0001…10 0.0001…10

Equilibrium-controlled | Fixed time

0.1 … 15

0.1…15

57

Methods t(min)

t(max)

dt

Earliest possible time for the measured value acquisition, in [sec]. (For control mode "" and equilibrium-controlled measured value acquisition only) Latest possible time for the measured value acquisition, in [sec]. (For control mode "" and equilibrium-controlled measured value acquisition only) Defines the time interval, in [sec], for the "fixed time" mea sured value acquisition. (For control mode "" and mea sured value acquisition = "fixed time" only.)

0.5…150

1…105

0.5…6000

Subfunction: Evaluation and recognition Parameters

Explanation

Procedure

Defines which evaluation procedure to use.

Threshold

Range of options

Standard | Asymmet ric | Minimum | Maxi mum | Segmented Defines the threshold (absolute amount) that must be Standard, asymmet exceeded for the recognition of an EQP. ric and segmented: 0 For the evaluation procedures "Minimum" and "Maximum", … 106 this threshold value refers to the original curve, for "Standard" Minimum and Maxi and "Asymmetric", it refers to the 1st derivative of the original mum: (See "Value curve, and for "Segmented", it refers to the 2nd derivative of Ranges of Sensor the original curve. Measuring Units and The unit depends on the evaluation procedure: Control Band") Standard and asymmetrical: UoM*/mL Minimum and Maximum: UoM Segmented: UoM/mL

* UoM:

Unit of Measurement Tendency Defines the tendency for which the EQP is to be detected (for "Procedures" = "Standard", "Asymmetric" and "Segmented"). Ranges You can define up to three recognition ranges. Outside these ranges, the system will recognize neither EQP's nor EQP can didates. Depending on what is defined here, upper and lower limits are defined for each recognition range and also whether addi tional EQP criteria are to be used for each recognition range. Lower limit 1-3 Defines the lower limit for the recognition range. Does not appear if "0" was selected for "recognition range." The unit of measure will depend on the sensor used. Upper limit 1-3

Add. EQP crite ria

58

Positive | Negative | None 1 | 2 | 3 | 0

(See "Value Ranges of Sensor Measuring Units and Control Band") Defines the upper limit for the recognition range. Does not (See "Value Ranges of appear if "0" was selected for "recognition range." The unit of Sensor Measuring measure will depend on the sensor used. Units and Control Band") Defines whether to take additional EQP criteria into considera Last EQP | Steepest tion. The available selection will depend on the evaluation jump | Lowest value | procedure chosen. They can be defined individually for each Highest value | No recognition range or for the overall recognition range ("recog nition ranges" = "0"). • Last EQP: The system only considers the quantity of EQPs defined under "Last jumps". • Steepest jump: The system only considers the number of steepest jumps defined under "Steepest jumps" • Lowest value: The system only considers the number of lowest values defined under "Lowest values" • Highest value: The system only considers the number of highest values defined under "Highest values". G20

Methods Last jumps Steepest jumps Lowest values Highest values

The quantity of last jumps to be taken into consideration. (For "add. EQP criteria" = "last EQP" only.) The quantity of steepest jumps to be taken into consideration. (For "add. EQP criteria" = "steepest jump" only.) The quantity of lowest values to be taken into consideration. (For "add. EQP criteria" = "lowest value" only.) The quantity of highest values to be taken into consideration. (For "add. EQP criteria" = "highest value" only.)

1…9 1…9 1…9 1…9

Subfunction: Termination Parameters

Explanation

Range of options

At Vmax

Defines the maximum volume, in [mL], at which the titration must be terminated if it has not been terminated already. Defines whether to terminate the titration after reaching a defined potential (with the correct tendency!). The potential at which to terminate the titration. The unit of measure will depend on the sensor used. (For "at potential" = "yes" only.)

0.1…1000

At potential Potential

Yes | No

-100 ... 100 (See "Value Ranges of Sensor Measuring Units and Control Band") Termination ten Defines for which tendency the titration should be terminated. Positive | Negative | dency (For "at potential" = "yes" only.) None At slope Defines whether to terminate the titration after reaching a Yes | No defined slope. This absolute value must be exceeded by one measured value and then be greater than two measured val ues to result in termination. Slope The slope, in [unit of measure/mL], at which to terminate the 0 ... 105 titration. (For "at slope" = "yes" only.) After number of Specifies whether the titration should be terminated after the Yes | No recognized recognition of a specific quantity of EQP candidates. The EQP EQPs candidates must: - Lie within the recognition range - Be above the threshold, and - Show the correct tendency. If no additional EQP criteria should be considered, then EQP candidate = EQP applies. Number of Defines the quantity of EQP candidates after the recognition 1…30 EQP's of which the system should terminate the titration. (For "after number of recognized EQPs" = "yes" only.) Combined ter No: Termination as soon as the first of the selected criteria Yes | No mination criteria from the (Potential | Slope | Number of recognized EQPs) group has been fulfilled. Yes: Termination as soon as all the selected criteria have been fulfilled. Termination of the titration in any case if the maximum volume is reached.

5.8.9.3 Mode An application mode can be selected in the "Control" subfunction for the EQP titration method functions if the "Control" setting is not set to "". Application modes are available for various types of titration (acid/base, redox, argentometry, etc.). If an application mode is selected, the settings for the Control subfunction will be specified based on what is best for the primary uses for the corresponding type of titration. The can choose between three different parameter sets for each application mode (Control "Normal", "Fast" and "Slow").

G20

59

Methods Sensor type

Unit

pH

pH mV mV

mV

ISE

mV ppm pX pM mV %T A mV µA °C °F K

Phototrode

Polarized Temperature

Unit for dE(set value) and dE mV mV

mV

mV

Mode

Acid / Base Acid / Base (non aqu.) Precipitation Precipitation (non aqu.) Redox Precipitation

Precipitation Complexation

mV Redox µA Redox °C, °F, K Acid / Base

5.8.9.4 Titration (EP) Carries out an end-point titration. You can define the relevant parameters for the following subfunctions: Subfunction: Titrant Parameters

Explanation

Range of options

Titrant


Titrant list

Subfunction: Sensor Type The type of sensor to be used to perform the measurement. Sensor

Unit


mV | pH | ISE | Pho totrode The name of the sensor. Sensor list of the sen sor type selected in Setup The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F Defines how to do the indication. Depending on the unit of Voltametric | Ampero measure: [mV] = voltametric, [µA] = amperometric. metric Ipol is the polarization current, in [µA], for the voltametric 0.0…24.0 indication. Upol is the polarization voltage, in [mV], for an amperometric 0…2000.0 indication. (Only for polarized sensors with "indication" = "amperometric".)

Subfunction: Temperature acquisition

60

Parameters

Explanation

Range of options


Defines whether to record the temperature, with the aid of a Yes | No temperature sensor, during the execution of the analysis func tion.

G20

Methods Temperature sensor Unit

Defines which temperature sensor to use for the temperature acquisition. (Only if "Yes" was selected for temperature acquisition.) The temperature unit you want to use.

Subfunction: Stir Speed Speed in [%].

Sensor list

°C | K | °F 0…100

Subfunction: Predispensing Parameters

Explanation

Range of options

Mode

Specifies the type of addition: Volume: predispenses a specific volume. Potential: system predispenses a substance until a certain potential is reached. Factor: A multiple of the sample size is predispensed. None: does not predispense. Volume in [mL]. The potential at which you want to stop predispensing. (For "mode" = "potential" only.)

Volume | Potential | Factor | None

Volume Potential

Factor

Wait time

0.0001…1000 (See "Value Ranges of Sensor Measuring Units and Control Band") The system calculates the predispensing volume by multiply 0 … 105 ing the factor by the sample size. (For "mode" = "factor" only.) Defines a waiting time, in [sec]. (Either after the predispens 0…32000 ing or, if "predispensing" was set to "none", before the start of titration.)

Subfunction: Control Parameters

Explanation

End point type

Absolute: Titration is ended when the absolute measured val ue is reached. Relative: The system will take into consideration the differ ence between the desired end point and the measured value at the start of the titration. Tendency Defines the direction of change for the measured value during the titrant addition. If the starting potential, end point and ten dency are inconsistent at the start of the analysis, the system will terminate the analysis immediately. (For "end-point type" = "absolute" only.) End point value The defined titration end point. The unit will depend on the sensor used.

Control band

Dosing rate (max) Dosing rate (min) G20

Range of options Absolute | Relative

Positive | Negative | None

(See "Value Ranges from Sensor Measur ing Units and Control Band") (See "Value Ranges from Sensor Measur ing Units and Control Band")

This number defines the width of the control band. Outside the control band, the system will titrate with the maximum dispensing rate. The smaller the control band, the faster the titrator will react to a deviation from the potential of the defined end point. When the measurement curve reaches the control band, the titrator will slow down the titrant addition to approach the end point in a cautious manner. The unit will depend on the sensor used. The maximum dosing rate in [mL/min]. 0.001…60 The minimum dosing rate in [µL/min].

1 – 104

61

Methods Subfunction: Termination Parameters

Explanation

Range of options

At EP

Defines whether to terminate the titration after reaching the end point. If "no" is selected, after reaching the end point the system will continue acquiring measured values without adding titrant until the maximum time period is reached. The termination delay which defines the time period, in [sec], between reaching the end point and terminating the titration. If during the termination delay the measured value drops below the end point, the system will add further increments and restart the termination delay. (Only if "at EP" = "yes" is selected.) Defines the maximum volume, in [mL], at which the titration must be terminated if it has not been terminated already. Defines the maximum time of the titration, in [sec].

Yes | No

Termination delay

At Vmax Max. time

0…108

0.1…1000 0…108 | ∞

5.8.9.5 Titration(LearnEQP) Learn titration (EQP) is used to determine the best parameters for carrying out an EQP titration. As soon as the settings have been successfully recorded, the titration detection in the method is converted to a normal EQP titration with the recorded settings. You can determine the relevant parameters for the following subfunctions: Subfunction: Titrant Parameters

Explanation

Range of options

Titrant


Titrant list

Subfunction: Sensor Parameters

Explanation

Type

The type of sensor to be used to perform the measurement.

Sensor

Unit

Range of options

mV | pH | ISE | Pho totrode The name of the sensor. Sensor list of the sen sor type selected in Setup The unit of measure to be used for the measurement; the unit mV | pH | ppm | pM | will depend on the sensor type selected. pX | %T | A | µA | °C | K | °F


Explanation




62

Range of options

G20

Methods Subfunction: Stir Parameters

Explanation

Range of options

Speed

Speed in [%].

0…100

5.8.10 Calculation For converting the titration results. Parameters

Explanation

Result type

If you select the parameter "Result type" = "Predefined", the Predefined | Results proposals button is available. With it you can select defined a predefined result from the proposal list. The parameters "Unit", "Formula", and "Constant" are adjusted automatically.

Calculation type

Formula, Result Result unit Constant C

Selected EQP

M Decimal places Result limits

Lower limit Upper limit Interruption out side limits

Record statistics

G20

If you select the parameter "Result type" = " defined", the parameters "Result", "Result unit", and "Constant" is editable. Using this parameter you can perform calculations for the fol lowing categories: direct titration, back titration (automatical, manual), blank compensation and other). For the selection of the result from the proposal list, you have to consider the Parameter "Entry type" used in the method function "Sample". If there is a difference between the "Calcu lation type" and the "Entry type" in "Sample" an error mes sage appears. These parameters are automatically set for results proposals if you have selected the parameter "Result type" = "Prede fined" (these parameters depend on the selected "Calculation type" and the "Entry type" in the method function "Sample". If you have selected "Result type" = " defined" you can edit the parameters "Result", "Result unit" and "Constant C". "Formula" is not editable. You can enter equivalence points (EQP) which you want to consider for the calculation. This parameter is only available if "Titration (EQP)" is selected in a loop. The molar mass of the substance [g/mol]. The number of decimal places for the result. Defines whether limits should be observed for the result. If this function is activated, there will be a message in the record if the result falls outside the defined limits. Defines the lower result limit. Appears only if "result limits" = "yes" was selected. Defines the upper result limit. Appears only if "result limit" = "yes" was selected. Determines whether the method should be interrupted if a value lies outside the defined limits (only appears if the "Lim its" parameter has been activated). A message (which must be acknowledged) appears advising that the process has been interrupted during the time that the message is displayed. Determines whether statistics should also be issued with the results in the protocol along with the result. If the method function "Protocol" "Results" = "No" selected then no statis tics are produced.

Range of options

Direct titration | Back titration autom. | Back titration manual | Blank comp. | Other

Arbitrary | "Constant C=" only a number is allowed

1 ... 10

List 0…6 Yes | No

-108 … 108 -108…108 Yes | No

Yes | No

63

Methods

5.8.11 Record This method function defines the type and scope of the data to be output for a record using the printer (see "Peripherals" > "Printer". If the method function "Record" is placed within a sample loop, the record will include all previous method functions within the current sample loop. If the method function "Record" is placed outside of a sample loop, the record will include all previous method functions listed after the last sample loop in the method procedure. A few settings are not avail able outside of a loop. Parameters

Explanation

Overview

States whether or not a short summary of the results should appear at the top of the protocol.

Range of options

No | Per sample | Per series out of loop: No | Yes Results The results from the "Calculation" method functions. Any sta within loop: Per Sam tistic selected will be recorded after the last sample of a series ple | Per Series | No or multiple determination. Out of Loop: No | Yes Raw results The raw results produced during the determination within loop: Per Sam ple | Per Series | No Out of Loop: No | Yes Measured value The table of measured values of the current sample (not Last titration function | table available out of loop). All titration functions | No Sample data The sample data of a sample loop. (Not available outside of Per sample | Per loop) series | No Resource data All data in the setup regarding the resources used in the Per Sample | Per method. Series | Non Per Sam ple | Per Series | No E–V Titration curve of the current sample. The potential is plotted Last | All | No against the volume (not available out of loop). dE/dV – V The 1st derivation of the titration curve, potential against vol Last | All | No ume (with linear coordinate representation) (not available out of loop). log dE/dV – V The 1st derivative of the titration curve for potential against Last | All | No volume. (With logarithmic ordinate display) (not available outside of loop) d2E/dV2 – V The 2nd derivative of the titration curve for potential against Last | All | No volume. (With linear coordinate display) (not available out of loop) E–t Titration curve of the current sample. The potential is plotted Last | All | No versus the time. (Not available outside of loop) V–t Titration curve of the current sample. The volume is plotted Last | All | No versus the time. (Not available outside of loop) dV/dt – t The 1st Derivative of the titration curve volume against time" Last | All | No (not available out of loop). T–t Titration curve of the current sample. The temperature is plot Last | All | No ted versus the time. (Not available outside of loop) E – V & dE/dV – Two superposed titration curves E – V and dE/dV – V for the Last | All | No V current sample. (Not available outside of loop) V – t & dV/dt – t Two overlaid titration curves "V – t" and "dV/dt – V" of the cur Last | All | No rent sample (not available out of loop). Method Printout of the method used. No | Yes Series data All data from the series run. No | Yes

64

G20

Methods Calibration curve

Calibration curve. The sensor unit of measurement is plotted against the measured values of all samples (not available within loop).

No | Yes

5.8.12 End of sample The "End of Sample" method function closes a sample loop. A sample loop refers to the range of a method through which a sample series will for each sample. The commencement of a sample loop is specified using the "Sample" method function.

5.8.13 Titer The "Titer" method function is only available outside a loop. This method function assigns the result of a sample loop to a titer and updates the value stored in Setup. Parameters

Explanation

TITER=

Specifies for how many results the titer should be determined. (For i=1, i does not have to be defined.) Limits Determines whether limits should be taken into for acquisition of a value. If the value is outside these limits, the value is not transferred to Setup. Interruption out Determines whether the method should be interrupted if a side limits value lies outside the defined limits (only appears if the "Lim its" parameter has been activated). A message (which must be acknowledged) appears advising that the process has been interrupted during the time that the message is displayed. Lower limit Defines the lower limit of a value. Appears only if the "limits" = "yes" setting was selected. Upper limit Defines the upper limit of the concentration limit.

Range of options Mean[Ri], i=1…30 Yes | No

Yes | No

0…100 0.1…100

5.8.14 Calibration This method function assigns the result of a calibration loop to a sensor and updates the sensor setup. Calibration is only performed outside a loop. This method function can be applied both for "Calibration" and "pH-sensor test". The calibration can be performed for "Action" = Calibration" in the "Sample (Cal ib)" method function and the sensor test for "Action" = Sensor test". Parameters

Explanation

Range of options

Limits

Determines whether limits should be taken into for acquisition of a value. If the value is outside these limits, the value is not transferred to Setup.

Yes | No

The "Limits" parameter is only available for "Action" = Calibration". In cases of segmented calibration for pH and ISE sensors, the limits will be defined and observed for each segment. Depending on the sensor type, if the "Limits" checkbox is activated, the following parameters can be determined (100% represents -59.16 mV/pH (sensor type: pH) or to -59.16 mV/[unit]) /Ion charge (sensor type: ISE). The unit corresponds to the unit specified in the previous method function, "Sample (Calib)". (For temperature sensors, only the two info fields for the minimum and maximum zero point are displayed.) For pH and ISE sensors:

G20

65

Methods Parameters

Explanation

Interruption out Determines whether the method should be interrupted if a val side limits ue lies outside the defined limits (only appears if the "Limits" parameter has been activated). A message (which must be acknowledged) appears advising that the process has been interrupted during the time that the message is displayed. Min. slope 1-8 The lower limit for the slope, in [%]. (100% refers to -59.16 mV/pH.) Max. slope 1-8 The upper limit for the slope, in [%]. Min. zero point The lower limit for the zero point. 1-8 Max. zero point The upper limit for the zero point. 1-8

Range of options Yes | No

10…200 10…200 -100…100 -100…100

The determined slope is converted to 25oC and compared with the limits.

5.8.15 pH sensor test The sensor test is used to check the slope, zero point and drift of pH sensors. The test can be started either by using a method or sample series via the "Calibration" method function or directly from the Setup of the sensor concerned (see also "Setup: Hardware > Sensors > Sensor calibra tion / pH sensor test"). ●

The calibration data of the pH sensor is not affected by the test.

●

The results of the sensor test can be printed out.

Starting the sensor test via a method Start the sensor test as follows: a) Select a method of the "Calibration" type or create the appropriate method. b) Select the "Sample (Calibration)" method function. c) In the Sample (Calibration) dialog window, select the following parameters: - "Sensor type" = "pH" - "Action" = "Sensor test" d) Specify the buffer parameters to be used (See "Methods: Method functions > Sample (Calibration)". The sensor test is carried out using two buffer solutions. e) Press OK. f)

Select the "Calibration" method function

g) Define the following parameters in the Calibration dialog: Parameters

Explanation

Interruption out Determines whether the method should be interrupted if a val side limits ue lies outside the defined limits (only appears if the "Limits" parameter has been activated). A message (which must be acknowledged) appears advising that the process has been interrupted during the time that the message is displayed. Min. slope 1-8 The lower limit for the slope, in [%]. (100% refers to -59.16 mV/pH.) Max. slope 1-8 The upper limit for the slope, in [%]. Min. zero point The lower limit for the zero point. 1-8

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Range of options Yes | No

10…200 10…200 -100…100

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Methods Max. zero point The upper limit for the zero point. 1-8 Min. drift The minimum drift value in [mV/30s]. Max. drift The maximum drift value in [mV/30s].

-100…100 -100 to 100 -100 to 100

●

If the values are within the limits, the sensor test is regarded as having been ed.

●

Slope and drift relate to 25°C.

To provide an overview, the relevant method functions have been summarized and listed in the following table: Method functions for the pH sensor test Method function Description Sample (Calibration)

Measure (normal)

Calibration

Record

This method function is used firstly in order to carry out a calibration and secondly for the sensor test. It is selected via the "Action" parame ter. Only two buffers can be defined for the sensor test. The measured values of both calibration solutions (pH buffers) are determined here. In addition, another drift determination is carried out for the second buffer. In the method, the "Calibration" method function for the sensor test is placed after the "End of sample" method function. Essentially, "Calibra tion" corresponds to a calculation function. In the process, it calculates the calibration parameters from the measured values of the calibration loop and the calibration standard values (pH buffer values). These are then compared with the inputted limit values for the zero point, slope and drift. The results of the sensor test are displayed in the "Overview" section of the record. The various selection parameters for titration curves (E – V, dE/dV – V, etc.) which are available during standard titration are invalid for the record.

5.8.16 Blank This method function assigns a result or arbitrary value to a blank value, including the unit. Parameters Name Value B=

Explanation

A name of your choice. Here you can enter a number or you can select a formula from the proposal list (via the Proposal button). Unit The units in which the blank is specified. Limits Determines whether limits should be taken into for acquisition of a value. If the value is outside these limits, the value is not transferred to Setup. Interruption out Determines whether the method should be interrupted if a side limits value lies outside the defined limits (only appears if the "Lim its" parameter has been activated). A message (which must be acknowledged) appears advising that the process has been interrupted during the time that the message is displayed. Lower limit Appears only if "limits" = "yes" was selected. Upper limit Appears only if "limits" = "yes" was selected.

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Range of options Arbitrary 1 ... 120 | Formula Arbitrary Yes | No

Yes | No

-108 … 108 -108 … 108

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Methods

5.8.17 Auxiliary instrument This method function activates external auxiliary instruments and enables the titrator to be controlled by such auxiliary instruments. The parameters described in the following can be defined for all control types. These are followed by parameters that can be defined explicitly for the relevant control type: Parameters

Explanation

Range of options

Control type

The control type of the auxiliary instrument.

Name

A name of your choice.

Output 24 V | Stirrer | Out TTL (Single pin) | Input TTL (Single pin) | RS-232 Arbitrary

5.8.17.1 Control type: 24V output Parameters

Explanation

Mode

Defines the mode for controlling the control output. On | Off | Fixed time - Fixed time: The control output is switched on for the defined time interval. On | Off: The control outlet is switched on or off. After a sam ple series the control outlet is automatically switched off. If "mode" = "fixed time" was selected, a time span in [sec] 0…106 can be defined here for which the control outlet should be switched on.

Time

Range of options

5.8.17.2 Control type: Stirrer Parameters

Explanation

Mode

Defines the mode for controlling the control output. On | Off | Fixed time - Fixed time: The control output is switched on for the defined time interval. On | Off: The control outlet is switched on or off. After a sam ple series the control outlet is automatically switched off. If "mode" = "fixed time" was selected, a time span in [sec] 0…106 can be defined here for which the control outlet should be switched on. Speed in [%]. 0…100

Time

Speed

Range of options

5.8.17.3 Control type: Out TTL (Single pin)

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Parameters

Explanation

Range of options

Mode

Defines the mode for controlling the control output. For TTL On | Off | Fixed Time | signals, the number and type of the output signals is deter Input controlled | mined Sequential . Fixed time: The control output is switched on for the defined time period. On | Off: The control output is switched on or off. TTL input-controlled: A signal received at the control inlet con trols the control outlet. The Auxiliary instrument function is ter minated as soon as the signal changes at the control input or after a defined maximum time has expired. TTL Sequential: The control output runs through a defined sequence.

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Methods Time

If "mode" = "fixed time" was selected, a time span in [sec] can be defined here for which the control outlet should be switched on. Input The name of the auxiliary instrument to serve as the signal input (control input). Appears only for "mode" = "input-controlled". Output signal Normal: The signal is transmitted without conversion. Inverted: The signal is transmitted in inverted form. Appears only for "mode" = "input-controlled". Max. time The maximum waiting time for a signal change, in [sec]. After it expires, the method is continued even if no signal change was detected. Appears only for "mode" = "input-controlled". Number of puls The number of impulses in the planned sequence. es Appears only for "mode" = "sequential." Pulse duration The duration of a pulse in [sec] (time switched on + time switched off). Appears only for "mode" = "sequential". Interval Defines the time span, in [sec], between two impulse starts. Appears only for "mode" = "sequential".

0…106

Auxiliary instrument list in the setup Auxiliary instrument list in the setup 0…106

0…104 0…106 0 … 106 | 0 … 104

5.8.17.4 Control type: TTL input (single pin) Parameters

Explanation

Range of options

Input signal

Indicates whether an increasing or a decreasing input signal should be detected. For communication direction "input" only. The maximum waiting time for a signal change, in [sec]. After it expires, the method is continued even if no signal change was detected. Appears only for "mode" = "input-controlled".

Rising | Falling

Max. time

0…106

5.8.17.5 Control type: RS-232 Parameters

Explanation

Range of options

Send output sequence Output sequence

Defines whether an output sequence should be sent.

Yes | No

The control sequence for the signal receiver - can also con tain a formula enclosed in characters % or control characters in format \xxx where xxx is the decimal number of the control character. G20 s only %R1% or %R2%. (Only if "Send output sequence" is activated). Defines whether the system should wait for a input sequence from the device. "The maximum waiting time for an input sequence in [sec].After it expires, the method will be continued even if no input sequence was detected." (Only if "Wait for input sequence" is activated). The input sequence from the external device. The sequence can contain control characters in format \xxx where xxx is the decimal number of the control character (only if "Wait for input sequence" is activated).

%R%

Wait for input sequence Max. time

Input sequence

G20

Yes | No 0…106 | ∞

Arbitrary

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Methods

5.8.18 Drain You use this method function to drain a specific volume from a sample vessel using a pump (membran , peristalitc- or air pump (Solvent Manager).You can specify the following parameters: Parameters

Explanation

Range of options

Drain pump

Defines which pump is to be used for drainage.

Drain volume Duration

The volume to be drained, in [mL]. The duration to drain the solvent , in [sec]. (Only available if "Drain pump" = "Solvent Manager"

Pump list (pumps defined in setup) 0…1000 0 … 103

5.9 Method functions Within a Loop The method functions that are permitted between the "Sample" and "End of sample" method functions are limited and depend on the loop type. The options within a calibration loop are identical to those in the sample loop with the restriction that they cannot contain any titration method functions, and the method function "Measure (Normal)" must occur (only) once in the loop. The same options that apply for the sample loop also apply for the titer loop, however the (titer) loop must contain at least one titration method function. The following method functions are essentially permissible within a sample loop in arbitrary order. ●

Drain

●

Calculation

●

Blank

●

Dispense (Normal)

●

Auxiliary instrument

●

Measure

●

Record

●

Pump

●

Stir

●

Titration (EP, EQP, LearnEQP)

●

Titration stand

For the method functions "Titration stand", "Calculation", and "Record", certain rules must be followed: ●

The method function "Titration stand" must appear immediately after the loop-initializing functions "Sample", "Sample (Calib)" or "Sample (Titer)".

●

A maximum of four "Titration Stand" method functions within a loop can be applied.

●

It is best to insert the method function "Calculation" after the method function that determines the raw results for the calculation.

●

The method function "Record" can be only inserted after the method function that generates the results the record should contain.

5.10 Method functions Outside of a Loop In addition to the preset "Title" method function, which always appears at the start, additional method functions can be inserted outside a loop depending on the method type:

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Methods - Drain - Calculation - Blank - Dispense (normal) - Auxiliary instrument - Calibration (position is fixed) - Pump - Record - Titer (position is fixed)

G20

●

The method function "Calibration" must appear immediately after the "End of Sample" method func tion of a calibration loop.

●

The method function "Titer" must appear immediately after the "End of Sample" method function of a titer loop.

●

The same options are available for calibration and titer methods. In addition, when entering a loop, enter the method functions "Calibration" or "Titer", as appropriate after the "End of Sample" function.

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Series Templates

6 Series Templates You can use series templates to gather up to 120 individual samples to form a sample series. All sam ples in the series are analyzed one after the other with a defined method (analysis template for sequential processing of samples using the same method). ●

You can create a shortcut on the Homescreen for all series templates.

●

A maximum of 60 sample series can be stored in the titrator.

If you select a series template from this list by clicking on it, you can change its parameters or delete the entire template. You can choose New to create a new series template. The following parameters will be available: Parameters

Explanation

Range of options

Sample series ID Method ID Comments Number of sam ples Number of stan dards Number of buffers

Here you can assign any ID to the sample series.

Arbitrary

Here you can select the Method ID for the relevant method. You can enter a brief comment about the series. Defines the number of samples to be analyzed.

Method list Arbitrary 1…120

The number of standards to be analyzed with a method or series. The number of buffers to be used for the calibration of a pH sensor.

1…120 1…9

During the creation of a sample series, you can choose "Samples" to display the loop list (method type: "GT") or to the standard list (method type "Titer" and "Calibration"). From these lists, you can change predefined sample or standard data or you can create new sample or standards.

6.1 Sample or Standard Parameters The sample list, which can be opened by choosing Samples in the series parameter window, displays all samples of a loop with a number, the first ID, and the sample size (depending on entry type - see "Method functions: Sample"). You can also edit the samples here. ●

Series IDs must be unique, although sample IDs do not have to be.

●

For titer loops, the standard name and the sample size are listed, and for calibration loops the name of the list of standards and the individual standards.

Select an entry from the list. You can define the following parameters for each sample, depending on the type of the loop (Sample, Titer, Calibration): Parameters

Explanation

Range of options

Number ID

The number of the sample. A -defined name for the ID of the sample, in accordance with the "Sample" method function. You can enter the sample size here. For fixed entry types, this field only appears as an info field.

1…120 Arbitrary

Sample size

0 … 1000 [g] | [mL] 0 … 106 [pcs.]

*The

entered value of the sample size has to be valid within the range which is configured in the "Sam ple" method function of the relevant method. Weight per piece Density [g/mL]

The weight in [g] per item. Appears only if "entry type" = "number of pieces" or "fixed number of pieces" was selected. The density of the sample for the entry types "Weight", "Fixed weight", "Volume" and "Fixed volume". Comments You can enter a brief comment about the series. Correction factor Any correction factor that can be used in calculations.

72

0…1000 0.0001…100 Arbitrary 0.0001…106

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Series Templates Temperature

The temperature in [°C] during the analysis. If temperature monitoring is activated in a titration function, the system will ignore the sample temperature given here.

-20…200

For entering the sample parameters, particularly for numerous samples, the titrator provides you with assistance in the entry windows of the "ID 1" and "Sample size" parameters:

These extra icons are a quick, direct way to jump to the entry window of the previous sample or next sample. You can also choose "Sample ID 1" and "Sample size" to switch directly between the entry windows for the sample parameters "ID 1" and "Sample size".

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Analysis Sequences

7 Analysis Sequences 7.1 Starting an Analysis An analysis can be started on the titrator in several different ways: 1. By choosing one of the following buttons: •

Start from the method editor

•

Start from Homescreen

•

Start from the Series dialog

•

Titer to perform a titer determination in Setup (Navigation: Setup > Chemicals > Titrant > Titrant Parameters).

•

Calibration / Sensor test to calibrate or to test pH sensor in Setup (Navigation: Setup > Hardware > Sensors > Sensor Parameters), refer to section "Setup: Hardware > Sensors".

2. Using a -specific shortcut or a direct shortcut from Homescreen. When you create a shortcut by choosing AddToHome (see "Description of Functions > The Interface > Shortcuts and Direct Shortcuts"), the following parameters are available: Parameters

Explanation

Description Immediate start

Any name for the shortcut. Arbitrary The method, series, or manual operation can be started Yes | No immediately. This enables you to start the analysis without using the Start analysis dialog. You can select the free position for the shortcut on the Home 4 screen.

Homescreen position

Range of options

After you create the shortcut, it appears in the selected position in "Home", from where you can select it by tapping the touchscreen. When you start an analysis, whether by using a button or with a shortcut, the system always opens the Start analysis dialog (see "Descripton of Functions > The Interface > The Start Analysis Dialog"). The only exceptions are direct shortcuts ("Immediate start" = "Yes"), whose selected settings permit a direct start. At the start of an analysis, you can still make changes to various settings in the Start analysis dialog. It is therefore possible, for example, to modify the sample size and define the number of samples to be determined. If the analysis you want to start is a single determination, you can enter the sample size or sample ID directly as a parameter in the Start analysis dialog. In general, the sample data can be entered for each individual sample using the Samples button in the Start analysis dialog. In the Sample data dialog that opens when you choose this button, a list of the individual samples is displayed. In addition, the status is displayed for every sample (regardless of the loop type) in the Sample data dia log. The following status levels can be assigned to a sample: ●

Idle: The sample is not yet running and the sample data can still be edited

●

Running: The sample is running but the sample data can still be edited

●

Active: The sample is running and the sample data can no longer be edited

●

Done: Done – the sample has run and concluded and the sample data can no longer be edited

If you select a sample, you can define the following sample data (depending on the method and entry type - see "Method functions: Sample").

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Analysis Sequences To enter sample data, tap on "Sample" in the Start analysis dialog. The Sample data dialog opens. You can tap on an entry in the "Sample list" or you can tap on New to specify the sample data via the follow ing parameters: Parameters

Explanation

Number ID 1 Sample size

The number of the sample. The ID for the first or only sample of an analysis. You can enter the sample size here. For fixed entry types, this field only appears as an info field. Weight per The weight in [g] per item. Appears only if "entry type" = piece "number of pieces" or "fixed number of pieces" was selected. Density You can enter the sample's density, in [g/mL], here. (Does not appear for the entry types "Number of pieces" and "Fixed number of pieces".) Comments You can enter a brief comment about the series. Correction factor Any correction factor that can be used in calculations. Temperature The temperature in [°C] during the analysis. If temperature monitoring is activated in a titration function, the system will ignore the sample temperature given here.

Range of options 1…120 Arbitrary 0 … 1000 [g] | [mL] 0 … 106 [pcs.] 0…1000 0…100

Arbitrary 0.0001…106 -20…200

You can enter the following parameters in the Start analysis dialog, depending on the type of analysis to be started and the resources used: Parameters

Explanation

Range of options

Type Number of sam ples Number of stan dards ID 1 Sample size

The type of analysis to be started. Either Method or Series. Defines the number of samples to be analyzed.

Method | Series 1…120

The number of standards to be analyzed with a method or series. The ID for the first or only sample of an analysis. You can enter the sample size here. For fixed entry types, this field only appears as an info field.

1…120 Arbitrary 0 … 1000 [g] | [mL] 0 … 106 [pcs.]

●

All the parameters that can be edited in the Start analysis dialog or the sample data dialog will over write the settings defined in the method for the same parameters.

●

All non-editable parameters that are displayed as an info field are only shown for orientation purpos es and list the settings from the method.

●

If the sample size must be entered before the analysis but the does not do so, the will be required to enter it immediately before the start of the analysis.

7.2 Analysis Sequence Steps During the processing of an analysis, starting from the start of the analysis and sample addition through to the results display, the titrator displays a range of dialog windows, some of which the has to confirm in order for the analysis to continue. These dialog windows are used to ensure faultless process ing, and also to provide the with information. Depending on the required degree of automation for an analysis, it can, however, be useful and desir able to deactivate particular security questions or information dialogs to ensure that the sequence is processed without interruption. Below are some process flow examples.

7.2.1 Analysis sequence For GT analyses, the sequence with the use of a manual or with the use of an automatic titration stand is shown. In each case, you are told where the individual screens can be switched off in the interface. ●

G20

Analysis sequence for an analysis with a titration stand of the type "Manual stand":

75

Analysis Sequences <Start>

Dialog: Analysis start

Can be switched off for the start via shortcut with the "Imme diate start" parameter during the creation or management of a shortcut.

<Start>

Check: Resources

Can be switched off with the "Show required resources at start" parameter in the analysis sequence settings. (An error message will appear if the resources have already been allo cated or are missing.)

Request: Sample size

Appears when "Entry" = "Before" was selected in the "Sam ple" method function and the sample size = 0. Can be avoid ed by selected a "fixed" entry type.

Add sample

Can be switched off for the start via shortcut with the "Imme diate start" parameter during the creation or management of a shortcut for the first sample.

Dialog: Online

Request: Sample size

For "Entry" = "Arbitary" parameter in the "Sample" method function.

Results

76

This can be switched on or off via the "Show results after analysis" parameter. (Navigation: Setup > Global settings > Analysis and resources behavior > Analysis sequence setting).

G20

Analysis Sequences

Homescreen / Analysis start ●

Analysis sequence for an analysis with a titration stand of the type "Auto stand" or "Rondolino TTL": <Start>

Dialog: Analysis start

Can be switched off for the start via shortcut with the "Imme diate start" parameter during the creation or management of a shortcut.

<Start>

Check: Resources

Can be switched off with the "Show required resources at start" parameter in the analysis sequence settings (Naviga tion: Setup > Global settings > Analysis and resources behavior > Analysis sequence settings).

Online Dialog

Results

Can be switched off with the "Show results after analysis" parameter in the analysis sequence settings (Navigation: Set up > Global settings > Analysis and resources behavior > Analysis sequence settings). Note: At the end of a series, all results are listed. The display of this list can be switched on or off via the "Show results after analysis" parameter.

Homescreen / Analysis start

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77

Titrator Evaluation Procedure

8 Titrator Evaluation Procedure The identification of equivalence point candidates within a defined recognition range can be done using four different evaluation methods: ●

Standard

●

Minimum / Maximum

●

Segmented

●

Asymmetric

Which method you use for the evaluation will depend on the type of titration or the form of the resulting titration curve. The procedure to be used is defined in the "Evaluation and recognition" method subfunc tion of the "Titration (EQP)".

8.1 Standard Evaluation Procedure The titrator's standard evaluation procedure is based on the chemical model of a classic acid-base titra tion. In this model, the equivalence point of such a titration will be at the point of inflection of the Sshaped titration curve and the curve will be symmetrical with regard to this inflection point. E

For the recognition of an inflection point using the stan dard procedure, the titrator will always look at one group of measured values (a "measured value win dow"). It will examine whether an inflection point is detectable for that group of measured values. This win dow will then be shifted along the curve by one mea sured value and reexamined for points of inflection. The system repeats this procedure until it detects no inflec tion point twice in a row. It then uses the inflection points found to define the most suitable one as the final inflection point of the titration.

(1)

V

(1) Inflection point The standard evaluation procedure initially only identifies points of inflection. Criteria defined by the in the method can influence whether and when an inflection point is to be ed as an EQP candi date. If so defined in the method, the following criteria will have to be fulfilled: ●

The inflection point must lie within a recognition range.

●

It must be above a threshold (refers to the first derivative).

●

The titration curve must demonstrate a specified tendency in the area of the inflection point.

EQPs are only detected in the range of the measured curve which is the specified by the "Tendency" para meter (Positive, Negativ), refer to method function "Titration (EQP): Evaluation and Recognition". If these criteria are fulfilled, the inflection point becomes an EQP candidate. The additional EQP criteria can now be used to influence which EQP candidates are ultimately recognized as equivalence points. For the standard evaluation, the additional EQP criteria "Last EQP" and "Steepest jump" are available. They can be selected individually for each defined recognition range. These criteria can be defined in the "Evaluation and recognition" subfunction of the "Titration EQP" method functions.

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Titrator Evaluation Procedure E [mV]

5

4 (EQP) 3

2 (EQP) 1 V [mL]

Theoretical example for the evaluation of a titration curve with five points of inflection Explanation: This titration curve shows five points of inflection (1 – 5). Inflection points 1, 2 and 4 are recognized as EQP candidates, since only these points lie within the 2 recognition ranges while also fulfilling the "Tendency" and "Threshold" parameters. The specified "Additional EQP criteria" then determine whether the EQP candidates are actually recog nized as EQP. These additional EQP criteria can be defined for every recognition range. In the example shown above, the following were specified as additional EQP criteria: Recognition Range 1: "Last EQP" Recognition Range 2: "No" Of the two EQP candidates found in Recognition Range 1, the system only identifies the second one as an EQP due to the "Final jump" criterion. The first one remains merely an EQP candidate. The termination criterion defined was that the titration should be terminated after the recognition of three EQP candidates ("Termination after EQP" = "3"). In the above example the titration is terminated on identification of the 4th turning point (3rd EQP candidate).

8.2 Minimum / Maximum The result of this evaluation is the calculated minimum (maximum) of the measured titration points. The classic example of a titration curve with a minimum is the photometrically indexed surfactant determina tion. E

The minimum (maximum) is calculated using a poly nomial approximation of the titration curve in the range of the minimum (maximum). The equivalence point recognition is done directly from the titration curve data.

V

8.3 Segmented evaluation Various indication methods (including photometry, conductometry, and amperometry) generate titration curves with linear or approximately linear sections (segmented curves). The titrator uses individual pro cedures to evaluate these curves. For a precise determination of the equivalence point, it is very impor tant that these curves have both linear segments and a clear bend. G20

79

Titrator Evaluation Procedure E

Titration curve The titration curve contains two more less linear seg ments and a bend between these two segments. The evaluation of segmented curves is generally done with the aid of the standard procedure for S-shaped curves, with the system using as its evaluation basis not the titration curve's measured points but the data calculat ed from them in the first derivative. V

1. Derivative

∆E/ ∆V

The first derivative of a segmented curve is the first to demonstrate the typical S shape. Its inflection point is the titration's equivalence point. 2. Derivative The threshold references the second derivative of the titration curve. In other words, the equivalence point for a defined threshold must be above this threshold num ber.

V ∆2E/ ∆V 2

EQPs are only detected in the range of the measured curve which is the specified by the "Tendency" parame ter (Positive, Negativ), refer to method function "Titra tion (EQP): Evaluation and Recognition". Within the segmented procedure the tendency refers to the 1. derivative. V

8.4 Asymmetric For markedly asymmetrical curves, the standard procedure can result in a systematic error. The difference between the true equivalence point and the point of inflection can be greater than the normally achievable precision. For these cases, the titrator uses an evaluation that uses the Tubbs method. This empirical approximation method is a procedure for the evaluation of asymmetrical, analog-regis tered titration curves. It can also be used for digitally recorded titration curves. The Tubbs procedure result will be closer to the true equivalence point for some asymmetrical curves than the inflection point. This evaluation procedure is based on the following considerations: E

Each of the two branches of the titration curve will have a writable osculating circle with a minimal radius. The relationship between the two radii is determined by the curve's asymmetry. The intersection of the connecting lines between the circle center points M1 and M2 and the titration curve produces the desired equivalence point. Theoretical calculations show that the true equiv alence point for asymmetrical titration curves will always lie between the inflection point and the branch of the titration curve with the greater degree of curvature (i.e. the smaller osculating circle).

M2

EQP

M1

V

The titrator uses a hyperbola to approximate those parts of the titration curve located in the area of the greatest curvature. For each approximated hyperbola, the system determines the peak (the point with the greatest curvature). The center points of the assigned smallest osculating circles are the focal points of both hyperbolas. The intersection of the connection lines from the two focal points and the titration curve produces the desired equivalence point, as shown above.

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Titrator Evaluation Procedure The evaluation requires at least six measured values in the area of the greatest curvature before and after the titration curve's inflection point. If the course of the titration curve does not permit the inclusion of the osculating circles, the titrator will use the standard procedure to calculate the equivalence point. You will be notified of this in the record of the "raw results". EQPs are only detected in the range of the measured curve which is the specified by the "Tendency" parameter (Positive, Negativ), refer to method function "Titration (EQP): Evaluation and Recognition".

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81

Analysis Data

9 Analysis Data The "Analysis data" include different types of data that can be used at various times during the planning and execution of an analysis. The system differentiates between the following types of analysis data: Raw data Raw data are defined when you create a method or series. They are automatically generated and stored during the analyses. Raw data are always created for each analysis and cannot be influ enced by the . Method data All data for the method run. Series data All data from the series run, such as e.g. the series ID and the number of samples. Sample data All data from the analyzed samples, such as e.g. the sample size, sample density and sample ID. Resource data Data for all resources used during the execution of an analysis (for example, titrant, auxiliary instrument). The data for a resource are copied from the setup at the time when it is used in an analysis. Table of measured values Tables of measured values are created by some method functions during an analysis and can be output in the record. Raw results Raw results are data determined by the titrator during an analysis, such as used titrant volumes and measured values. The raw results can be converted into the actual analysis results in the "Calculate" method function using the appropriate symbols and formulas.

Results

Some of the raw results are always produced automatically and others are only generated when used within a calculation. Results are the results of the conversions of raw results run within the "Calculate" method function. The results of an analysis can be influenced by the .

Of these, the following can be used in calculations:

82

●

Sample data (such as the sample size or the sample density)

●

Resource data (e.g. mole quantity and equivalence quantity for a substance )

●

Raw results (e.g. blank)

●

Results (the results of a calculation can then be used in a subsequent calculation).

G20

Calculation and Results

10 Calculation and Results The method functions "Titration (EP)" and "Titration (EP)", Measure (normal) and Dispense provide their own raw results within a method. These raw results are saved by the titrator in the order in which the generating method functions are processed within the method. Example: Sequence of the calculations in the method, generating two results Method function Result Title Sample Titration stand Stir Titration (EQP) Calculation Calculation*

R1 R2

End of sample *: Allowed are a maximum of two "Calculation" method functions, which can either be inserted within a loop as well as outside of a loop. The definitions to the parameters you can determine in the "Calculation" method function are available in "Methods: Method functions > Calculation"

10.1 Symbols for calculations Inside the "Calculation" method function, you can access certain analysis data (Raw results, Results, Resource data and Sample data) via the different symbols. The following is a list of the symbols used for the G20. The list also contains additional symbols which are used in the records: Symbol

Meaning

VEQ (=V)

Titrant consumption in [ml] up to the end point or equivalence point. For multiple equivalence points, the consumption is calculated from the previous equivalence point. Titrant volume in [ml] used up to the end of a titration method function, including pretitration. The total titrant volume used during a dispensing method function in [ml]. The excess of titrant (i.e. excess in ml after EQP or EP) added after reaching the end point or equivalence point. Substance quantity in [mmol] used up to the end point or equivalence point. The total substance quantity in [mmol] used up to the end of a titration method function. The total substance quantity in [mmol] used during a dispensing method function. The excess of titrant added after reaching the end point or equivalence point, i.e. mmol excess after EQP or EP. Consumption up to the auxiliary value in [mmol]. The measured potential of a method function "Measure (normal)" in [mV, pH...]. Gives the nominal concentration in [mol/L] of the titrant being used. The ionic concentration in [mol/L], [E=pH, pX, pM]. Duration of the titration in [min]. Dispensing time in [min]. The duration of a measurement in [min].

VEND VENDDi VEX QEQ (=Q) QEND QENDDi QEX QE(H[AuxValue]) E C pw(-E) t tDi tMe

G20

83

Calculation and Results Symbol

Meaning

ESTMe

Initial potential for an analysis with the "Measure (normal)" method function. The potential at the end point or equivalence point of a titration method function. The potential at VEQ/2 of a titration method function (not for titration (EP)). The measured potential after the waiting period for predispensing during a titration method function. The measured temperature in a method function "Measure (normal)" (direct measurement with temperature sensor or concomitant tempera ture acquisition) in [°C], [K], [°F].

EEQ EHNV EPD T

M z B[Blank] m d wp p cst Rx C

Mean[Rx] nEQ

Stands for the molecular weight of a substance (as stored in the setup). Stands for the equivalent number of a substance (as stored in the set up). A blank. Stands for the sample size [g, ml, pcs]. Stands for the density of a sample or a standards [g/ml]. Stands for the weight per piece (can be changed under "Sample") [g]. Stands for the purity of a fixed titer standard [%]. Stands for the concentration of a liquid titer standard [mol/L]. A result x. Stands for a constant that uniquely belongs to the result Rx. This means it can not be used for the calculation of other results. For information on using Constant C, refer to "Results: results proposal lists". The mean value of a result Rx. Stands for the number of equivalent points for the Titration (EQP, Lern EQP) method function.

10.2 Calculation formulas Calculation formulas are used in the "Calculate" method function. One typical example for a formula within the "Calculation" method function would be the expression R=VEQ. In this case, the consumed volume of titrant up to the point at which the end point is reached is assigned to R. All the symbols can be used for analysis data in relations like this. The analysis data to be used must be generated by the method before the "Calculate" method function. Auxiliary values and blanks defined in the setup can generally be used in formulas in the same manner as symbols. The general form for an auxiliary value is: H[Name] (as defined in the setup).

10.3 Results The Results dialog can be accessed directly from Homescreen using the relevant button. ●

The system only saves the results from the last analysis (series or individual sample).

●

When you start a new analysis, you will lose the results from the previous analysis.

●

You can see the results immediately after they are generated.

You can use the various buttons in the "Results" dialog to access different functions. You can, for exam ple,

84

●

view all results of the last analysis

●

view statistics, perform an outlier test and if necessary, exclude samples from the statistics.

G20

Calculation and Results ●

perform recalculations for results in which certain raw data (e.g. sample sizes) have to be adapted retrospectively for a single sample or for all samples in a series.

●

view and print the status and the calculated results of each individual sample.

Results are retained until new results are generated by methods. The results of the "older" of the two sample series are replaced. All the changes performed on the saved results can be reversed with the "Undo changes" button. Changes to results are indicated by an asterisk in the record. Example: VEQ*. All results You can use the All Results button to view the results of the last analysis and print them if a printer is connected to the titrator (see "Printer"). From the Results dialog, you also have the following additional options: ●

Samples View or print the results of an individual sample or exclude the entire sample (see "Results: Samples")

●

Statistics Switch to the "Statistics" dialog (see "Results: Statistics")

Delete all results You can use this button to delete all the data (raw data, raw results, and results) saved by the titrator in the results range. Undo changes If you make changes to the results saved by the titrator after the analysis, you can use Undo changes to discard them. Afterward, the system will reinstate the initial status directly after the conclusion of the analysis, in its original and unchanged state. Statistics For results within a sample loop, you can display and print out statistics. The statistics are only created if more than one sample was analyzed in the corresponding loop. The following calculated values will be displayed as statistical components: ●

Mean value x of a result Rx (Mean [Rx])

●

Standard deviation s

●

Relative standard deviation srel

●

Number of samples per loop nTOT

If a result was excluded from the statistics, all the results from that sample will always be excluded as well. The system will then recalculate the statistics without the excluded sample and label them accord ingly. If the sample's results are then put back into the statistical evaluation, the label will be removed from the statistics. From the Statistics dialog, you also have the following additional options: ●

Samples View, print, or exclude the results of an individual sample (see "Samples")

●

Results View or print all results (see "All Results")

●

Outlier test Perform a test for outliers in the statistical evaluation.

Samples You can use the Samples button to display and print the status and calculated results for each individual sample. The same applies for a series of additional data sets that can be accessed via "Data". This will let you view and print the sample, method and resource data for each sample and view and print the raw results and the measured values.

G20

85

Calculation and Results You can use the Exclude button in the Results: Samples dialog to exclude individual samples from the statistical evaluation. The system will not delete the results of the samples excluded in this way but mere ly label them as excluded. They will no longer be included in the statistics. Samples that have been excluded can be returned to the statistics at any time by choosing "Include". After a sample is excluded, all affected calculations (inside and outside of loops) are performed again. Outlier test If the results of individual samples in a measurement series deviate greatly from the calculated mean val ue, it may make sense to question the significance of these (few) results and treat them as "outliers". Outliers will have the following effects on the overall result of an analysis: ●

The mean value is significantly shifted higher or lower.

●

The standard deviation is increased.

●

The distribution of the individual values around the mean value is distorted and no longer follows a normal distribution.

The titrator has an automatic function for identifying and labeling outliers. You can call this function from the Statistics dialog using the "Outlier test" softkey. You can run an outlier test if you have the results from more than three samples. The procedure used by the titrator is the Grubbs outlier test. For this procedure, the measured value [x*] that has the greatest deviation from the calculated mean value is analyzed.This number is used in the fol lowing equation, together with the mean value [x] and the standard deviation [s]:

PG =

x* - x s

The test variable [PG] is then compared with the corresponding value in the Grubbs table G (N, 90%), which in turn depends on the number of measured values N: N (number of samples) 1

2

3

4

5

6

7

8

9

10

90 %

-

1.15

1.46

1.67

1.82

1.94

2.03

2.11

2.18

N (number of samples) 11

12

13

14

15

16

17

18

19

20

90 %

2.29

2.33

2.37

2.41

2.44

2.48

2.5

2.53

2.56


22

23

24

25

26

27

28

29

30

90 %

2.6

2.61

2.63

2.65

2.67

2.69

2.7

2.72

2.74


32

33

34

35

36

37

38

39

40

90 %

2.77

2.78

2.79

2.81

2.82

2.83

2.84

2.86

2.87


42

43

44

45

46

47

48

49

50

90 %

2.89

2.9

2.91

2.92

2.92

2.93

2.94

2.95

2.96


52

53

54

55

56

57

58

59

60

90 %

2.97

2.98

2.99

3

3

3.01

3.02

3.02

3.03


62

63

64

65

66

67

68

69

70

90 %

3.04

3.04

3.05

3.05

3.06

3.06

3.07

3.07

3.08


72

73

74

75

76

77

78

79

80

90 %

3.08

3.09

3.09

3.1

3.1

3.11

3.11

3.12

3.12

82

83

84

85

86

87

88

89

90

-

2.23

2.58

2.75

2.88

2.97

3.03

3.08


86

G20

Calculation and Results 90 %

3.12

3.13

3.13

3.14

3.14

3.15

3.15

3.16

3.16

3.17


92

93

94

95

96

97

98

99

100

90 %

3.17

3.17

3.18

3.18

3.19

3.19

3.2

3.2

3.21

3.21


102

103

104

105

106

107

108

109

110

90 %

3.21

3.22

3.22

3.22

3.23

3.23

3.23

3.23

3.24

3.24


112

113

114

115

116

117

118

119

120

90 %

3.22

3.25

3.25

3.26

3.26

3.26

3.26

3.27

3.27

3.24

If the calculated test variable PG is greater than the corresponding value taken from the table, the mea sured value x* is identified as an outlier and marked accordingly. After an outlier has been identified, the test is repeated with the remaining measured values (without the already identified outlier) using the newly calculated mean value and new standard deviation. This process is repeated continually until no further outlier can be identified. It is then the 's responsibility to exclude any identified outliers from the statistics. After confirmation, the entire sample is excluded and the statistics are recalculated without the identified and excluded out liers.

10.4 Results proposal lists Proposal list In the "Calculation" dialog window (see "Methods: Method functions > Calculation"), using the Results proposals button, specified results with unit, formula and Constant can be selected. Proposal lists for the "Sample" and "Sample (Titer)" method functions are dependent on the "Entry type" parameter. When the "Entry type" is modified, a validation is immediately carried out to determine whether the selected calculation exists in the corresponding entry type. Result type: Predefined After selecting a result from the proposal list, the "Result unit", "Formula" and "Constant" fields are auto matically populated and can not be modified. Result, Result unit and the entry type selected in the "Sam ple" method function are used to determine the formula. Result type: defined If the parameter "Result type= defined" is selected, you can modify the "Result", "Result unit" and "Constant" fields; though not the formula. The mode " defined" only offers empty proposal lists. A result can only be selected in Predefined mode. If you switch this to " defined", a number can be entered for "Constant C =". The proposal lists inside and outside a loop are different. Inside a loop and for the "Result type=Predefined", the calculation type can also be selected ("Direct titration", "Back titration", "Blankcompensated", "Others"). An auxiliary value exists in the setup. This can not be deleted, nor can addition auxiliary values be creat ed. The name of the auxiliary value is fixed. The different proposal lists are displayed as follows:

10.4.1 Results proposal list inside loop 10.4.1.1 Proposal list for "Calculation type=Direct titration"

G20

Result

Unit

Replace "m" Formula R= according to entry type

Constant C=

Consumption

ml

--

C=1

VEQ

87

Calculation and Results Result

Unit

Consumption

ml/g ml/ml mmol Total consumption mmol Consumption until mmol pot. Content mg/g mol/kg mmol/g mmol/kg ppm % g/100g mg/100g Content g/L mg/L mol/L eq/L meq/L mmol/L


Constant C=

g ml ----

VEQ/m VEQ/m Q QEND QE(H[AuxValue])

C=1

g ml: m*d pc: m*wp

Q*C/m

C = M/z C = 1/z C = 1000/z C = M*1000/z C = M/(10*z)

g: m/d

Q*C/m

ml

C=100*M/z C = M/z C = M*1000/z C = 1/z C=1 C = 1,000 C = 1000/z

10.4.1.2 Proposal list for "Calculation type=Automatic back titration" Result

Unit


Constant C=

Consumption

ml ml/g ml/ml mmol mmol mmol

-g ml ----

VEQ VEQ/m VEQ/m Q QEND QE(H[AuxValue])

C=1

mg/g mol/kg mmol/g mmol/kg ppm % g/100g mg/100g g/L mg/L mol/L eq/L meq/L mmol/L

g

R = (QENDDi-Q)*C/m

C = M/z C = 1/z

Total consumption Consumption until pot. Content

Content

88

ml: m*d pc: m*wp

g: m/d ml

C = 1000/z C = M*1000/z C = M/(10*z)

R = (QENDDi-Q)*C/m


G20

Calculation and Results

10.4.1.3 Proposal list for "Calculation type=Manual back titration" Result

Unit

Consumption

ml ml/g ml/ml mmol Total consumption mmol Consumption until mmol pot. Content mg/g mol/kg mmol/g mmol/kg ppm % g/100g mg/100g Content g/L mg/L mol/L eq/L meq/L mmol/L


Constant C=

-g ml ----


C=1

g

R = (H[AuxValue] –Q) * C = M/z C/m C = 1/z

ml: m*d pc: m*wp

g: m/d ml

C = 1000/z C = M*1000/z C = M/(10*z)

R = (H[AuxValue]–Q) * C/m


10.4.1.4 Proposal list for "Calculation type= Blank-compensated" Result

Unit

Consumption

ml ml/g ml/ml mmol Total consumption mmol Consumption until mmol pot. Content mg/g mol/kg mmol/g mmol/kg ppm % g/100g mg/100g mg KOH/g

G20

Bromine No.

g/100g

Content

g/L mg/L


Constant C=

-g ml ----


C=1

g

R = (Q–B[Blank]) * C/m

C = M/z C = 1/z

ml: m*d pc: m*wp

g: m/d ml

C = 1000/z C = M*1000/z C = M/(10*z)

R = (QE(H[AuxValue])B[Blank]) * C/m R = (QENDB[Blank])*C/m R = (Q–B[Blank]) * C/m

C=100*M/z C = M/z C = M/(10*z) C = M/z C = M*1000/z

89

Calculation and Results Result

Unit


Content

mol/L eq/L meq/L mmol/L

Constant C=

R = (Q–B[Blank]) * C/m

C = 1/z C=1 C = 1,000 C = 1000/z

10.4.1.5 Proposal list for "Calculation type=Others" Result

Unit


Constant C=

Potential pH Ion conc.

mV pH pX pM ppm A %T μA °C K °F mmol/L mol/L

--

E

C=1

--

T

C=1

---

pw(-E)*1000 pw(-E)

C=1

Absorption Transmission Current Temperature

Ion conc.

For Calibration, the results proposals for "Calculation type=Others" also apply.

10.4.1.6 Proposal List for the Method type "Titer" Result

Unit

Replacing "m"

Formula R=

Constant C=

Titer

----

g mL g

m/(VEQ*c*C) C = M/(10*p*z) C = 1/(cst*z) C = d/(cst*z)

10.4.2 Results proposal list outside loop

90

Result

Unit


Constant C=

Mean value Mean value

---

---

C=1 C=1

Mean[R1] Mean[R2]

G20

Appendix

11 Appendix 11.1 Predefined calibration standards for pH sensors METTLER TOLEDO EU (Ref. 25°C)

METTLER TOLEDO USA (Ref. 25°C)

DIN (19266) /NIST (Ref. 25°C)

DIN (19267) (Ref. MERCK (Ref. 25°C) 20°C)

2.00 4.01 4.60 7.00 9.21 10.00 11.00

1.68 4.01 7.00 10.01

1.680 3.557 3.775 4.008 6.865 7.416 9.184 10.014 12.454

1.09 3.06 4.65 6.79 9.23 12.75

1.00 2.00 3.00 4.00 4.66 5.00 6.00 6.88 7.00 8.00 9.00 9.22 10.00 11.00 12.00 13.00

11.1.1 Temperature related values 11.1.1.1 METTLER TOLEDO METTLER TOLEDO EU (Ref. 25°C) Tempera ture [°C] 0 2.03 4.01 5 2.02 4.01 10 2.01 4.00 15 2.00 4.00 20 2.00 4.00 25 2.00 4.01 30 1.99 4.01 35 1.99 4.02 40 1.98 4.03 45 1.98 4.04 50 1.98 4.06 55 1.98 4.08 60 1.98 4.10 70 1.99 4.16 80 2.00 4.22 90 2.00 4.30 95 2.00 4.35

G20

pH

4.66 4.65 4.64 4.63 4.62 4.60 4.61 4.62 4.63 4.64 4.66 4.67 4.69 4.71 4.73 4.75 4.77

7.12 7.09 7.06 7.04 7.02 7.00 6.99 6.98 6.97 6.97 6.97 6.98 6.98 7.00 7.04 7.09 7.12

9.52 9.45 9.38 9.32 9.26 9.21 9.16 9.11 9.06 9.03 8.99 8.96 8.93 8.88 8.83 8.79 8.77

10.65 10.52 10.39 10.26 10.13 10.00 9.87 9.74 9.61 9.48 9.35 9.22 9.09 8.96 8.83 8.70 8.57

11.90 11.72 11.54 11.36 11.18 11.00 10.82 10.64 10.46 10.28 10.10 9.92 9.74 9.56 9.38 9.20 9.02

91

Appendix METTLER TOLEDO USA (Ref. 25°C) Temperature [°C] 5 1.67 10 1.67 15 1.67 20 1.68 25 1.68 30 1.68 35 1.69 40 1.69 45 1.70 50 1.71

pH 4.01 4.00 4.00 4.00 4.01 4.01 4.02 4.03 4.04 4.06

7.09 7.06 7.04 7.02 7.00 6.99 6.98 6.97 6.97 6.97

10.25 10.18 10.12 10.06 10.01 9.97 9.93 9.89 9.86 9.83

11.1.1.2 DIN / NIST DIN (19266) / NIST (Ref. 25°C) Temper ature [°C] 0 1.666 3.577 3.863 5 1.668 3.573 3.837 10 1.670 3.569 3.819 15 1.672 3.565 3.801 20 1.676 3.561 3.787 25 1.680 3.557 3.775 30 1.685 3.553 3.766 35 1.691 3.549 3.759 40 1.697 3.549 3.754 45 1.704 3.544 3.751 50 1.712 3.548 3.748 55 1.715 3.554 3.750 60 1.723 3.560 3.753 70 1.743 3.580 3.763 80 1.766 3.609 3.780 90 1.792 3.650 3.802 95 1.806 3.674 3.815 DIN (19267) (Ref. 25°C) Temperature [°C] 0 1.08 5 1.08 10 1.09 15 1.09 20 1.09 25 1.09 30 1.10 35 1.10 40 1.10 45 1.10 50 1.11

92

pH

4.010 4.004 4.001 4.001 4.003 4.008 4.015 4.026 4.036 4.049 4.064 4.075 4.091 4.126 4.164 4.205 4.227

6.984 6.950 6.922 6.900 6.880 6.865 6.853 6.845 6.837 6.834 6.833 6.834 6.836 6.845 6.859 6.877 6.886

7.534 7.502 7.474 7.451 7.432 7.416 7.405 7.396 7.389 7.386 7.384 7.382 7.380 7.378 7.376 7.374 7.372

9.464 9.392 9.331 9.277 9.228 9.184 9.144 9.110 9.076 9.046 9.018 8.985 8.962 8.921 8.885 8.850 8.833

10.317 10.248 10.180 10.121 10.066 10.014 9.970 9.928 9.892 9.856 9.830 9.804 9.778 9.752 9.726 9.700 9.674

13.423 13.207 13.003 12.810 12.627 12.454 12.289 12.133 11.984 11.841 11.705 11.574 11.449 11.324 11.199 11.074 10.949

pH 3.12 3.11 3.10 3.09 3.07 3.06 3.05 3.05 3.04 3.04 3.04

4.67 4.67 4.66 4.66 4.65 4.65 4.65 4.65 4.66 4.67 4.68

6.89 6.87 6.84 6.82 6.80 6.79 6.78 6.77 6.76 6.76 6.76

9.48 9.43 9.37 9.32 9.27 9.23 9.18 9.13 9.09 9.04 9.00

13.89 13.63 13.37 13.16 12.96 12.75 12.61 12.45 12.29 12.09 11.98

G20

Appendix 60 70 80 90

1.11 1.11 1.12 1.13

3.04 3.04 3.05 3.07

4.70 4.72 4.75 4.79

6.76 6.76 6.78 6.80

8.92 8.88 8.85 8.82

11.69 11.43 11.19 10.99

11.1.1.3 MERCK MERCK (Ref. 20°C) Temper ature [°C] 0 0.96 5 0.99 10 0.99 15 0.99 20 1.00 25 1.01 30 1.01 35 1.01 40 1.01 45 1.01 50 1.01 60 1.02 70 1.02 80 1.02 90 1.02

pH

2.01 2.01 2.01 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.01 2.01 2.01

3.05 3.05 3.03 3.01 3.00 3.00 3.00 3.00 2.98 2.98 2.97 2.97 2.97 2.97 2.96

MERCK (Ref. 20°C) (continued) Tempera ture [°C] 0 7.13 8.15 5 7.07 8.10 10 7.05 8.07 15 7.02 8.04 20 7.00 8.00 25 6.98 7.96 30 6.98 7.94 35 6.96 7.92 40 6.95 7.90 45 6.95 7.88 50 6.95 7.85 60 6.96 7.83 70 6.96 7.80 80 6.97 7.78 90 7.00 7.75

G20

4.05 4.04 4.02 4.01 4.00 4.01 4.01 4.01 4.01 4.01 4.00 4.00 4.00 4.00 4.00

4.68 4.68 4.67 4.67 4.66 4.66 4.66 4.66 4.67 4.67 4.68 4.69 4.70 4.71 4.72

5.06 5.05 5.02 5.01 5.00 5.00 5.00 5.00 5.00 5.01 5.01 5.04 5.05 5.10 5.14

6.04 6.02 6.01 6.00 6.00 6.02 6.03 6.03 6.04 6.05 6.06 6.10 6.12 6.17 6.24

6.98 6.95 6.92 6.90 6.88 6.86 6.86 6.85 6.84 6.84 6.84 6.84 6.84 6.86 6.88

pH

9.24 9.16 9.11 9.05 9.00 8.95 8.91 8.88 8.85 8.82 8.79 8.73 8.70 8.66 8.64

9.46 9.40 9.33 9.28 9.22 9.18 9.14 9.10 9.07 9.04 9.01 8.96 8.93 8.89 8.85

10.26 10.17 10.11 10.05 10.00 9.94 9.89 9.84 9.83 9.79 9.74 9.67 9.62 9.55 9.49

11.45 11.32 11.20 11.10 11.00 10.90 10.81 10.72 10.64 10.56 10.48 10.33 10.19 10.06 9.93

12.58 12.41 12.26 12.10 12.00 11.88 11.72 11.67 11.54 11.44 11.33 11.04 10.90 10.70 10.48

13.80 13.59 13.37 13.18 13.00 12.83 12.67 12.59 12.41 12.28 12.15 11.75 11.61 11.39 11.15

93

Appendix

11.1.1.4 FLUKA FLUKA (Ref. 20°C) Temperature [°C] 0 10 20 30 40 50 60 70 80 90

0.94 0.99 1.00 1.00 1.01 1.01 1.01 1.01 1.02 1.02

pH

1.99 1.99 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00

FLUKA (Ref. 20°C) (continued) Tempera ture [°C] 0 7.13 8.18 10 7.05 8.09 20 7.00 8.00 30 6.98 7.94 40 6.97 7.90 50 6.96 7.86 60 6.96 7.82 70 6.97 7.80 80 6.98 7.77 90 7.00 7.75 NOVARTIS (FLUKA) (Ref. 20°C) Temperature [°C] 0 4.01 5 4.00 10 4.00 15 4.00 20 4.00 25 4.01 30 4.01 35 4.02 40 4.03 45 4.04 50 4.06 55 4.07 60 4.09 65 4.11 70 4.13 75 4.14 80 4.16 85 4.18

94

3.03 3.02 3.00 3.00 2.99 2.98 2.98 2.98 2.98 2.97

4.03 4.02 4.00 4.00 4.00 4.00 4.00 4.00 4.00 4.00

5.05 5.02 5.00 5.00 5.00 5.02 5.04 5.07 5.10 5.13

6.03 6.01 6.00 6.02 6.04 6.06 6.09 6.13 6.18 6.24

pH

9.24 9.11 9.00 8.93 8.86 8.80 8.75 8.71 8.67 8.64

10.24 10.10 10.00 9.90 9.82 9.75 9.68 9.62 9.55 9.49

11.45 11.20 11.00 10.81 10.64 10.48 10.33 10.19 10.06 9.93

12.58 12.26 12.00 11.75 11.53 11.31 11.09 10.88 10.68 10.48

13.71 13.35 13.00 12.66 12.37 12.10 11.84 11.61 11.40 11.20

pH 7.11 7.08 7.05 7.02 7.00 6.98 6.97 6.96 6.95 6.94 6.94 6.93 6.93 6.93 6.94 6.94 6.95 6.96

9.20 9.15 9.10 9.05 9.00 8.96 8.91 8.88 8.84 8.80 8.77 8.74 8.71 8.69 8.67 8.65 8.63 8.61

G20

Appendix 90 95

4.21 4.23

6.97 6.98

8.60 8.59

11.1.1.5 FISCHER FISHER (Ref. 25°C) Temper ature [°C] 0 5 0.95 10 0.98 15 1.01 20 1.01 25 1.00 30 1.02 35 1.03 40 1.02 45 1.03 50 1.03 55 60 65 70 75 80 85 90 95

pH

1.98 1.98 2.02 2.00 2.00 2.00 2.02 2.01 2.01 2.01

2.98 2.97 3.00 3.00 3.00 3.02 3.03 3.03 3.04 3.04

4.01 3.99 4.00 3.99 4.00 4.00 4.01 4.02 4.03 4.04 4.06 4.07 4.09 4.11 4.13 4.14 4.16 4.18 4.21 4.23

5.05 5.04 5.03 4.99 5.00 5.00 5.01 5.01 5.04 5.06 5.08

6.07 6.05 6.06 6.05 6.00 6.00 5.99 5.98 5.97 5.97 5.96

7.13 7.10 7.07 7.05 7.02 7.00 6.99 6.98 6.97 6.97 6.97 6.97 6.98 6.99 7.00 7.02 7.03 7.06 7.08 7.11

8.15 8.13 8.08 8.01 8.00 8.00 8.00 7.95 7.94 7.94 7.93

9.166 9.126 9.089 9.055 9.022 8.991 8.961 8.930 8.902 8.874 8.845 8.815 8.784

10.34 10.26 10.19 10.12 10.06 10.00 9.94 9.90 9.85 9.81 9.78 9.74 9.70 9.68 9.65 9.63 9.62 9.61 9.60 9.60

11.80 11.69 11.46 11.31 11.17 11.00 10.88 10.76 10.62 10.52 10.41

11.1.1.6 JIS / JJG JIS Z 8802 (Ref. 25°C) Temperature [°C] 0 1.666 5 1.668 10 1.670 15 1.672 20 1.675 25 1.679 30 1.683 35 1.688 40 1.694 45 1.700 50 1.707 55 1.715 60 1.723 70 1.743 80 1.766 90 1.792 95 1.806

G20

pH 4.003 3.999 3.998 3.999 4.002 4.008 4.015 4.024 4.035 4.047 4.060 4.075 4.091 4.126 4.164 4.205 4.227

6.984 6.951 6.923 6.900 6.881 6.865 6.853 6.844 6.838 6.834 6.833 6.834 6.836 6.845 6.859 6.877 6.886

7.534 7.500 7.472 7.448 7.429 7.413 7.400 7.389 7.380 7.373 7.367 7.361 7.355 7.349 7.343 7.337 7.331

9.464 9.395 9.332 9.276 9.225 9.180 9.139 9.102 9.068 9.038 9.011 8.985 8.962 8.921 8.885 8.850 8.833

10.32 10.24 10.18 10.12 10.06 10.01 9.97 9.92 9.89 9.86 9.83 9.80 9.77 9.74 9.71 9.68 9.65

95

Appendix JJG119 (Ref. 25°C) Tempera ture [°C] 0 1.668 5 1.669 10 1.671 15 1.673 20 1.676 25 1.680 30 1.684 35 1.688 40 1.694 45 1.700 50 1.706 55 1.713 60 1.721 70 1.739 80 1.759 90 1.782 95 1.795

96

pH

3.599 3.591 3.583 3.575 3.567 3.559 3.551 3.547 3.547 3.550 3.555 3.563 3.573 3.596 3.622 3.648 3.660

4.006 3.999 3.996 3.996 3.998 4.003 4.010 4.019 4.029 4.042 4.055 4.070 4.087 4.122 4.161 4.203 4.224

6.981 6.949 6.921 6.898 6.879 6.864 6.852 6.844 6.838 6.834 6.833 6.834 6.837 6.847 6.862 6.881 6.891

7.515 7.490 7.467 7.445 7.426 7.409 7.395 7.386 7.380 7.379 7.383 7.387 7.391 7.399 7.407 7.415 7.419

9.458 9.391 9.330 9.276 9.226 9.182 9.142 9.105 9.072 9.042 9.015 8.990 8.968 8.926 8.890 8.856 8.839

13.416 13.210 13.011 12.820 12.637 12.460 12.292 12.130 11.975 11.828 11.697 11.553 11.426 11.172 10.918 10.664 10.537

G20

Subject index

12 Subject index 2 24V Output

24

A All Results Analysis and Resources Behavior Analysis Sequence Settings Resource Behavior Analysis data Analysis Sequence Analysis, starting Application Modes Asymmetric evaluation procedure Auxiliary instruments Auxiliary instruments, manual operations Auxiliary reagents Auxiliary values

85 28 29 82 75 74 59 80 24 37 13 30

B Beep Blank value Board data Board firmware Burettes

26 30 32 31 32

C Calculations Results Calibration starting Calibration standards Chemicals Calibration standards Substances Titer standards Titrant Configuring a balance More Control band Control Type 24V Output Input TTL (Single Pin) Out TTL (Single Pin) RS-232 Stirrer Curve progression Minimum / Maximum

G20

83 74 13 13 15 15 12-13 22 18 68 69 68 69 68 79

97

Subject index D Data storage Date and time Deleting results Dispensing Drives

27 27 85 40 32

E Emergency stop (reset) End-Point Titration Equivalence-Point Titration Evaluation and Calculation Evaluation procedure asymetric Introduction

8 60 56 82 80 78

F Firmware History

31

G Global settings Analysis and Resources Behavior System Management

28 27 28

H Hardware Peripherals Sensors Home

21 16 8

I Identification, titrator Import/Export, data Info button Input TTL (Single Pin) Interrupt Analysis Titrator Ion Selective Sensors ISE Sensors

27 30 8 25 47 47 18 18

K Keyboard layout Define

27

L Language, setting Layout of terminal Learn Titration (EQP) Linear Calibration Loop

98

25-26 8 62 19

G20

Subject index Insertion and Deletion Types and numbers

48 48

M Manual operations Auxiliary instruments Burette Pump Sensor Stirrer Manual Titration Measure (Normal) Method Delete Start Method editor Method functions Maximum number Parameters Within Loop Method functions, parameters Auxiliary Instrument Blank Value Calculation Calibration Dispense (Normal) Drain End of Sample Measure (Normal) Pump Record Sample Sample (Calibration) Sample (Titer) Stir Titer Titration (EP) Titration (EQP) Titration (LearnEQP) Titration Stand Method ID Method syntax Method Templates Method Types Methods Creating Modify Subfunctions Suspend METTLER TOLEDO Methods Minimum / Maximum

G20

37 39 34 34 33 41 53 46 46 43 49 49 70 68 67 63 65 53 70 65 53 52 64 50 51 51 53 65 60 56 62 52 43 48 45 43 44 46 53 47 44

99

Subject index Curve progression mV Sensors

79 17

O Online Dialog Out TTL (Single Pin) Outlier test Overview Method functions

10 25 86 49

P PC Settings Peripherals Balances USB Stick pH Sensor pH sensor test Phototrode Plug and Play Sensors Setup Polarized Sensor Measure With Preloaded Methods Printer Peripherals USB Printer Pump and Stirrer Detection Pump, manual operations Pumps

23 22 22 17 66, 74 17 16 36 43 22 22 29 34 21

R Reset button Reset to factory settings Resource Behavior Result type Predefined defined Results proposals Results, deleting Rinse Burette Rinse Multiple Burettes RS-232

8 31 29 87 87 87 85 39 40 25

S Sample Sample Loops Sample parameters Sample Results Sample, Titer, Calibration Loops Sartorius balances Screen, setting 100

50 48 72 85 43 22 26 G20

Subject index Segmented Evaluation procedure Segmented evaluation procedure Sensor pH Sensor test Potentiometric Sensor calibration Setup Sensor Calibration Linear Calibration Segmented Calibration Sensor test Method function: Calibration Method functions Method funktion MF Calibration Setup starting Sensors Configure Sensors, manual operations Series templates Service & Maintenance Board data Board firmware Burettes Data Import/Export Drives Reset to factory settings Terminal Titrator Firmware History Update Setup menu Shortcuts Sorting lists Standard evaluation procedure Start analysis Starting analysis Statistics Stirrer Stirrer (0-18V Output) Subfunctions Methods Substances Suspending options Symbols for calculations System settings

79 79 20 35 18 19 20 66 66 20 66 18, 20 74 16 34 72 32 31 32 30 32 31 32 31 32 12, 12 9, 26 9 78 10 75 85 33 25 53 15 11 83 27

T Temperature Sensor Measure With

G20

35

101

Subject index Template Methods Time and date Title, parameters Titrant Titration (EP) Titration (LearnEQP) Titration stands Titrator identification Touchscreen operations

49 27 50 12-13 60 62 24 27 8

U Undo Changes Updating USB Compact Printer USB Stick, configuring Interface settings Keyboards Language Screen Shortcuts

85 32 22 22 8, 9 27 25-26 26 26

V Value ranges Control band Sensors Values Auxiliary values Blank

102

18 18 30 30

G20

Subject to technical changes.

© Mettler-Toledo AG 2009

51710727 0909/2.12 Printed in Switzerland

Mettler-Toledo AG, Analytical, Sonnenbergstrasse 74, CH-8603 Schwerzenbach, Switzerland Tel. ++41 (0)44 806 77 11, Fax ++41 (0)44 806 73 50, Internet: www.mt.com

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