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E-Mail: info@metrohm.com Internet: www.metrohm.com Volume 37 Issue 2-2008/2009 

Contents 

New: 856 Conductivity Module and 867 pH Module ..........3 

New: 888 Titrando and 890 Titrando ...............................5 

New: 860 KF Thermoprep ...............................................9 

New: Water analysis with TitrIC 2.0 ..............................11 

New: 863 Compact VA Autosampler .............................14 

New: Solitrode with rotating seal ...................................14 

Application: ProcessLab ...............................................15 

Customer application: Laboratory automation ...............19 

Customer application: Degradation of bioplastics ..........23 

Conference report: Analytica ........................................25 

Practical tips: Automation & Safety ...............................27 

New Application Notes, Application Bulletins 

and papers ...................................................................29 

Literature corner ...........................................................31 

Literature references ....................................................32 

Metrohm seminars & trade fairs ...................................35 

Titration • Ion Chromatography • VA Trace Analysis • ProcessLab • Automation

Editorial 

Imprint 

Metrohm Information is a customer 

magazine from Metrohm Ltd. and is 

published in English and German. 

Please contact us if you wish to receive 

your own copy regularly. 

Published by: Metrohm Ltd., 

CH-9101 Herisau, 

Switzerland 

Phone +41 71 353 85 85 

Fax +41 71 353 89 01 

info@metrohm.com 

www.metrohm.com 

Editor: Dr. Benedikt Galliker 

bg@metrohm.com 

Printed by: Metrohm Ltd. 

Internet: www.metrohm.info 

ISSN 1424-0904 

Dear Readers, 

Globalization – this catchword also applies to Metrohm. However, for us it is not 

associated with its usual negative attributes. Exactly the opposite is the case: 

Metrohm draws strength from its global complexity. What does «global» mean 

for Metrohm? Today Metrohm is represented in 40 countries by daughter companies. 

Exclusive agencies care for our customers in about 40 further countries. In 

each country – no matter whether it is looked after by a daughter company or by 

an agency – maintaining highest standards is of outmost importance for us. This 

means: 

• Providing comprehensive advice about applications 

• Short delivery times for all instruments 

• Direct availability of accessories and spare parts 

• Well-trained service technicians who can provide rapid and reliable on-site help 

• The same high standards worldwide – a great bonus for all our customers, and 

particularly for those who are global operators themselves 

Switzerland is a hospitable country. Every year we welcome Metrohm employees 

from all over the world to courses and seminars at our Metrohm headquarters. 

Our Product Managers inform them about the latest news, applications and instruments 

in the world of ion analysis. It happens quite often that all the continents are 

represented in Herisau at the same time. Courses aimed at further education and 

training are also regularly held all over the world. In our regional Support Centers, 

which are located in Brazil, South Africa, Singapore and the United Arab Emirates, 

employees from the region gather for training. For the instructors from the Swiss 

Headquarters, this is a great opportunity of not only getting across the correct 

chemistry and analytics, but also of getting to know the different cultures. Obviously, 

this method of passing on know-how is not a one-way street. Our employees 

listen with great attention – not just on their trips – and in this way can bring back 

to Switzerland wishes, suggestions and trends from the various countries. Such 

information helps us to develop the right instruments and applications for the exciting, 

colorful global market – both today and in future. 

A further globalization aspect: today, when most companies have their storerooms 

on trucks on the freeways or on planes in the air (keyword just-in-time production), 

Metrohm’s behavior may appear to be very conservative. Metrohm still has instruments 

and accessories in its storerooms – both in Switzerland and very close to 

you in your local Metrohm agency. This means that we can meet your requirements 

within a very short time and do not have to ship our products round the world by 

express courier. Sending large amounts in a single shipment, as Metrohm does, is 

not just more economical but also more ecological. 

Let‘s return from the global world of ion analysis to this issue of Metrohm Information. 

Here are some of the highlights: we present you a highly modern analytical 

robot system used in fertilizer production in Belgium. You will learn about the 

degradation of bioplastics that is investigated at the University of Stuttgart. We are 

also seizing this opportunity of introducing you to a further new and interesting 

ProcessLab atline application. And last but not least, you can take a first look at the 

latest analytical instruments from Metrohm. 

I wish you much pleasure in reading this issue of Metrohm Information. 

Yours sincerely, 

Dr. Kai Henning Viehweger 

Vice President 

Division Manager Sales and Marketing 

2 Metrohm Information Issue 2-2008/2009

New instruments for pH, ion or conductivity measurements 

856 Conductivity Module and 867 pH Module 

The 856 Conductivity Module is Metrohm’s new conductivity meter. Thanks to the 

five-ring measuring technique, the new conductivity cells have an extremely wide 

linearity range. 

The new 867 pH Module is used for pH and ion measurements. Conventional potentiometric 

sensors can be used as well as «iTrodes», the new intelligent electrodes 

from Metrohm. 

The 856 Conductivity Module and 867 pH Module can be used in many ways: 

– For extending a Titrando by an additional measuring input for pH, ion or conductivity 

measurement (tiamo from version 2.0) 

– As an integrated, software-controlled pH, ion or conductometer in combination 

with PC Control (from version 5.0) 

– As a stand-alone pH, ion or conductometer in combination with the 840 Touch 

Control (software version 5.0) 

– As a completely automated pH, ion or conductometer in combination with the 

814 USB Sample Processor or 815 Robotic USB Sample Processor XL. 

No matter for which applications the two modules are used – you can be sure that 

your measurements comply with the requirements of FDA Standard 21 CFR Part 11. 

The two USB and four MSB connections1 provide the modules with flexibility, offer 

plug-and-play functionality and allow to connect numerous instruments: 

– Printer, sample changer, barcode reader, etc. 

– Up to four stirrers and dosing devices for adding auxiliary solutions or for carrying 

out standard additions fully automatically 

Thanks to the galvanically separated measuring inputs, both instruments can be 

used simultaneously for pH and conductivity measurements in the same beaker. 

__________________________ 

1 MSB = Metrohm Serial Bus 

New: 856 Conductivity Module and 867 pH Module 

The new 856 Conductivity Module and 867 pH Module 

can be operated either with the 840 Touch Control (left) 

or via PC Control (right). 

In combination with a Titrando, the new 856 Conductivity 

Module allows to carry out pH and conductivity measurements 

simultaneously in the same sample vessel. 

Metrohm Information Issue 2-2008/2009 3

New: 856 Conductivity Module and 867 pH Module 

The new five-ring conductivity measuring cell (article 

number 6.0915.100) offers many advantages and is 

easy to handle. 

With the pH Module and a Dosino, available as an option, 

concentrations can also be determined using the standard 

addition method. 

The iUnitrode with Pt 1000 temperature sensor is an intelligent 

pH glass electrode for universal use that has a 

very low alkali error. An 854 iConnect measuring amplifier 

is used to connect the iUnitrode to the 867 pH 

Module. 

856 Conductivity Module and the new five-ring conductivity 

measuring cells 

The new five-ring conductivity measuring cells for the 856 Conductivity Module 

come with a built-in Pt 1000 temperature sensor. They offer a wide linear measuring 

range, i.e. the cell constant remains constant and does not need to be determined 

again even if the measuring range varies widely. Complicated platinization is 

also not required for this type of measuring cells. With their very small immersion 

depth for a five-ring measuring cell (see Table) and a diameter of only 12 mm these 

cells are also very handy! Thanks to the removable cap, the conductivity measuring 

cells are very easy to clean. They are available in two versions. 

Technical specifications of the five-ring conductivity measuring cells 

6.0915.100 6.0915.130 

Shaft length 125 mm 142 mm 

Shaft diameter 12 mm 12 mm 

Minimal immersion depth 34 mm 50 mm 

Cell constant 0.7 cm -1 1 cm -1 

Ideal measuring range 

(with one calibration) 

0.005…20 mS/cm 0.005…100 mS/cm 

Temperature range 0…70 °C 0…70 °C 

The classical conductivity measuring cells with a banana plug, for example 

6.0914.040 for very low conductivities (below 5 μS/cm), can also be connected 

by using an optional adapter box. 

867 pH Module 

As the 867 pH Module is equipped with both a conventional and an intelligent measuring 

input, it can be used for pH, potential, ion and temperature measurements with 

both conventional and intelligent potentiometric sensors. 

If you have any doubts about the condition of your pH electrode, the built-in electrode 

test quickly provides certainty. In addition, tips are also given about how to 

remedy any faults. 

Ion measurements with ion-selective electrodes (ISE) can be made either by direct 

measurement or by standard addition with an optional Dosino or 805 Dosimat. 

iTrodes, the intelligent Metrohm sensors 

The memory chip built into the iTrode stores important data such as the article and 

serial number of the sensor, calibration data and calibration history, time in use and 

calibration interval. All sensor data is read out automatically when the iTrode is connected 

to the 867 pH Module. This means that mix-ups, typing errors or expired 

calibration intervals are eliminated. 


Enter the Titrando world 

The new 888/890 Titrandos: intelligent and easy to use 

The advantages of the new 888/890 Titrandos at a glance: 

• Touch Control with large color display 

• PC Control or tiamoTM titration software for operation via PC 

• Intuitive operation 

• Intelligent Exchange Units 

• iTrodes – intelligent electrodes for the 888 Titrando 

• Potentiometric titration with the 888 Titrando 

• Karl Fischer titration with the 890 Titrando 

• 847 USB Lab Link for Intranet and Internet 

• Complies with FDA 21 CFR Part 11 

Metrohm has extended the well-proven Titrando family by two new titrators. The 

888 Titrando for potentiometric titration and the 890 Titrando for Karl Fischer titration 

have been designed for routine applications in titration laboratories and are intended 

for customers who place the highest demands on operating comfort, data 

management, automation and the traceability of analytical results. The outstanding 

property of the new Titrandos is their user-friendliness, which is based on sophisticated 

technology with the intelligent iTrode sensors and Exchange Units 1 . 

Operation of the Titrandos is either by Touch Control with touch-sensitive screen 

(stand-alone titrator) or via a computer with PC Control or tiamo software. 

Both the 888 Titrando and the 890 Titrando are equipped with a USB port and allow 

connection of a balance, printer, PC, PC keyboard, barcode reader and/or 847 

USB Lab Link as well as a sample changer. The titrators can be optimally adapted to 

meet customer-specific requirements by connecting further dosing elements. 

Comprehensive GLP functions are a matter of course as is compliance with FDA 

21 CFR Part 11. 

__________________________ 

1 Intelligent Exchange Units can be used with the 888 and 890 Titrando; the iTrodes only with the 888 

Titrando. 

New: 888 Titrando and 890 Titrando 

The new members of the Titrando family have everything 

you need. The 888 Titrando (on the left) is perfect 

for potentiometric titrations in routine use. The 890 

Titrando (on the right) performs KF titration at the highest 

level. 



In the Metrohm range of electrodes you will find the 

iTrodes, intelligent electrodes allowing you to utilize the 

full potential of your new 888 Titrando. The combined 

iUnitrode pH glass electrode is one of these electrodes. 

The 888 Titrando: perfect for potentiometric titrations 

The 888 Titrando is the new potentiometric titration system for routine analysis. 

The instrument is equipped with a high-resolution, galvanically separated measuring 

input for conventional and intelligent electrodes (iTrodes) as well as an 

intelligent Exchange Unit. Optionally, numerous additional dosing elements such 

as 805 Dosimats or 800 Dosinos can be connected to the four MSB (Metrohm 

Serial Bus) connections. The 888 Titrando is ideal for dynamic (DET) and monotonic 

(MET) equivalence-point titrations as well as for titrations to a predefined 

endpoint (SET). 

The complete packages we offer allow immediate start up: together with the 888 

Titrando you will receive an intelligent Exchange Unit (20 mL), an «Ecotrode plus» 

combined pH glass electrode, a magnetic stirrer, all the necessary cable connections 

and tubing together with either the 840 Touch Control or the titration software 

tiamo light. 

The 890 Titrando: KF titrations at the highest level 

The 890 Titrando is the new titrator for volumetric Karl Fischer water determinations. 

The sophisticated control algorithm and the improved volume resolution of 

the intelligent Exchange Unit guarantee results of the highest precision. Great value 

has been placed on simple and intuitive user guidance. Icons show whether the titration 

cell contents are still being conditioned or whether you can already start the 

water determination. 

The electrode test and the «Safety stop» parameter prevent the cell from overflowing 

during conditioning, i.e. if the electrode is accidentally connected incorrectly or 

if the titration cell is very moist, conditioning will be terminated after a preset time 

or after the addition of a predefined KF reagent volume. This new feature increases 

working safety in the laboratory. 

The 890 Titrando also has four MSB connections and a USB connection. 

Together with the 890 Titrando you will also receive all the hardware and software 

that you require for your Karl Fischer titrations: an intelligent Exchange Unit (10 

mL), a double Pt-wire electrode, an 803 Ti Stand, all the necessary cable connections 

and tubing together with either the 840 Touch Control or the titration software 

tiamo light. 

Time-saving KF titrations with the 803 Ti Stand 

Save time with the 803 Ti Stand! It is used for stirring and for replacing 

the used working medium by simply pressing a button. The built-in membrane 

pump aspirates the spent solution and adds fresh working medium 

without the cell having to be opened. This reduces the conditioning time 

enormously. 

The iTrodes – not stupid at all! 

Intelligence creates transparency 

The electrode is the most important component of each titration system. The 

iTrodes represent our new intelligent electrode generation. They guarantee the complete 

traceability of the result to each component involved in the analysis. 

The digital passport – no more errors 

The chip built into the electrode head stores important sensor data such as article 

and serial number, calibration data, calibration history and time in use. All sensor 

data is read in automatically when the sensor is connected to the 888 Titrando. This 

prevents editing errors. The electrode is identified automatically. If the electrode 


does not match that defined in the method, the user will be informed. This means 

that the use of an incorrect electrode is prevented. 

Saving the calibration data – outliers don’t have a chance 

Monitoring functions permit the exclusion of electrodes whose calibration data is 

outside the limits or whose calibration has expired. If the sensor is to be used with 

different instruments or if an inexperienced user is to be prevented from calibrating 

the electrode, the electrode can be calibrated under defined conditions and 

then connected to the particular instrument with the calibration data stored in the 

memory chip. 

Certified dosing elements with brains 

The Metrohm Exchange Units set new standards with respect to operating safety. 

Each Exchange Unit is equipped with a data chip from which the Titrando 

automatically reads off all the data that is required for an error-free titration, i.e. 

type of reagent, titer, last titer determination, expiry date and much more. The 

Titrando compares this data with that of the selected method and carries out a 

plausibility test. If a negative result is obtained an error message appears in clear 

text. 

Additionally, each Exchange Unit is provided with its serial and cylinder numbers 

and supplied with an individual certificate. The Titrando checks the predefined 

intervals for determining the titer of the titrant. This ensures that work is always 

carried out with the correct titer. 

Simple operation 

Profit from our vast experience in the titration sector! We have ensured that your 

work with our potentiometric and Karl Fischer titrators is as easy as possible – even 

if you are new to that field. This is guaranteed by the intuitive and simple operation 

of the instruments, standard user methods for a range of applications and a clever 

help function that is available to you at any time. There is no need to tediously work 

through numerous menus! It is possible to quickly adapt all the parameters and 

standard user methods to meet your particular requirements. User dialogs can also 

be customized to suit the needs of the particular user. This user-friendly concept 

allows you to work efficiently – you only have to select the predefined method and 

can then start immediately. 

All the methods that have been created for Metrohm Titrinos can be automatically 

converted into Titrando methods using a PC. The Titrando itself, the memory card 

or the PC with its numerous additional possibilities is available for storing your 

methods, sample data and results. 

Automation made easy 

An increasing number of samples, time-consuming sample preparation and unattended 

overnight operation quickly justify the use of sample changers. The 888 and 

890 Titrandos have the necessary intelligence to control sample changers. Whether 

small or large sample capacities, one or two processing stations, measuring out the 

sample, sample preparation, liquid handling, rinsing and calibrating the electrodes 

– the 814 USB Sample Processor and 815 Robotic USB Sample Processor XL offer 

a high degree of automation for low investment costs. Sensational: just connect the 

sample changer to the USB interface of the Titrando and the world of automation 

already opens up to you. 

Convince yourself of the many advantages of our new 888/890 Titrandos for 

routine analysis and for users who are new to the Titrando world. Contact your 

local Metrohm agency today for advice and to arrange an instrument demonstration! 


The intelligent Metrohm Exchange Units make a considerable 

contribution to the error-free performance of 

your titrations. These Exchange Units, which are available 

with buret volumes of 1, 5, 10, 20 and 50 mL, can 

conveniently be used with reagent bottles from various 

manufacturers. 

The use of sample changers, for example the 814 USB 

Sample Processor, helps you to manage even large numbers 

of samples. 



888 Titrando and 890 Titrando: an overview 

Intelligent dosing elements for titration 

Additional dosing elements (for dosing only) 

888 Titrando 890 Titrando 

One built-in Dosimat for 

Exchange Unit 

Three 805 Dosimats with 

Exchange Unit 

Three 800 Dosinos with 

Dosing Unit 

Intelligent Exchange Unit with built-in data chip Yes 

Steps per cylinder content (Exchange Unit) 20 000 

One built-in Dosimat for 

Exchange Unit 

Three 805 Dosimats with 

Exchange Unit 

Three 800 Dosinos with 

Dosing Unit 

Measuring interface for pH, U/mV, T/°C 1 – 

Intelligent electrodes iTrodes 1 – 

Measuring input for polarizable electrodes 1 

Operation, dialog Touch Control, PC Control or tiamo 

Stirrer, titration stand 

801 Stirrer (magnetic stirrer) or 802 Stirrer (rod stirrer) 

with 804 Ti Stand or 803 Ti Stand (KF) 

Stirrer and intelligent dosing element connections Four MSB connections (Metrohm Serial Bus, daisy chain) 

Sample changer connections One sample changer via USB 

Connection of balance, printer, PC, PC keyboard, barcode 

reader and/or Lab Link 

Via two USB slave ports, RS-232/USB Box (option) 

Temperature sensor Pt 1000 or NTC – 

Differential amplifier Option – 

Real-time display on Touch Control or PC monitor Yes 

DET Dynamic equivalence point titration Yes – 

MET Monotonic equivalence point titration Yes – 

SET Titration to preset endpoints with 

automatic conditioning 

KFT Volumetric Karl Fischer titration with automatic 

conditioning 

Yes – 

– Yes 

MEAS Measuring mode for pH, U/mV, T/°C, I pol, U pol Yes – 

CAL Calibration with automatic buffer recognition Yes – 

Additional titration curve evaluation for fixed endpoints, 

pK values (HNP) 

Yes – 

Comprehensive GLP functions; complies with FDA 21 CFR Part 11 Yes 


Sample preparation: easy, safe and precise 

The new 860 KF Thermoprep 

The 860 KF Thermoprep is the new Metrohm instrument for thermal sample preparation 

in Karl Fischer titration (KF titration/KFT). It can be combined with a large 

number of KF titrators and KF coulometers for volumetric or coulometric water determinations. 

Stumbling blocks in sample preparation and determination 

Many substances, such as plastics or salts, release their water either very slowly 

or only at high temperatures. This means that they cannot be analyzed by direct 

volumetric or coulometric KF titration. 

Certain samples are either sparingly soluble or not soluble at all in alcohols and 

therefore in Karl Fischer reagents containing alcohols. In order to bring such substances 

into solution, it is necessary to use harmful solubility promoters (such as 

chloroform, xylene …) or, alternatively, to perform complicated sample preparation 

steps. 

If you place the sample directly in the titration vessel you risk contaminating the 

vessel. As a result, the titration vessel has to be cleaned more often and the reagents 

then also need to be replaced. This costs time and, because of the increased 

reagent consumption, also money. In addition, various substances present in the 

sample can undergo side-reactions with the KF reagents used and produce incorrect 

results. 

Be on the safe side with thermal sample preparation 

All the above problems can be avoided with the new 860 KF Thermoprep made by 

Metrohm. The sample is heated in a hermetically sealed vessel. The moisture released 

by the sample is transferred by a stream of dry carrier gas to the titration 

cell and determined there by Karl Fischer titration. Depending on the amount of water 

present, either a volumetric or coulometric titration is carried out. The sample 

itself does not enter the titration cell and therefore does not come into contact with 

the reagents used. This means that interfering side-reactions and matrix effects are 

excluded. 

What benefits does the 860 KF Thermoprep offer you? 

The most important benefits of the 860 KF Thermoprep are: 

• Easy operation 

• Safe procedure 

• Precise results 

New: 860 KF Thermoprep 

The preparation of difficult samples for water analysis 

according to Karl Fischer can be performed easily with 

the new 860 KF Thermoprep. As an example, a setup 

with an 841 Titrando is shown. 

Always be on the safe side by using the 860 KF Thermoprep 

for sample preparation in KF titrimetry (at right). It 

can be optimally combined with Titrandos for KF titration 

or KF coulometers (at left: 756 KF Coulometer). 


New: 860 KF Thermoprep 

Thanks to the operating unit with its well laid-out menu, 

working with the 860 KF Thermoprep is very easy. 

1. Switch on the 860 KF Thermoprep 

and select the temperature. 

2. Place an empty conditioning vial 

in the oven and pierce it with the 

needle. 

3. Switch on the pump, adjust 

the gas flow and start the titrator 

(conditioning). 

4. Weigh out the 

sample into a 

sample vial. 

5. Hermetically seal 

the sample vial 

with a septum using 

the crimping 

tongs. 

Easy operation 

Well laid-out menu guidance makes working with the 860 KF Thermoprep a pleasure. 

All parameters can be set to your requirements by just pressing a few keys. 

The sample preparation is also as easy as can be imagined. All you have to do is 

weigh out your sample into the sample vial and then seal it hermetically. 

Safe procedure 

The extraordinarily stable and well thought-out construction of the 860 KF Thermoprep 

prevents the needle from being lowered beside the septum. You always hit the 

septum – with certainty. 

Often the use of toxic solubility promoters can be avoided by using the oven method 

– harmful solvent vapors are a thing of the past. 

Precise results 

As the analytical conditions are identical for all samples, the results are reproducible 

and precise. The headspace vials are hermetically sealed by a PTFE septum 

and thus guarantee a constant water content, even after the vials have been standing 

around for some time. 

The heated transfer tubing prevents the condensation of water vapor and ensures 

that all the moisture enters the titration cell for determination. 

The sample remains in the sample vessel and does not undergo any side-reactions 

with the KF reagents. 

The analysis – step by step 

You will obtain your results in just a few steps: 

6. Wait until the preset temperature 

has been reached and «Conditioning 

OK» appears. 

7. Start the titration 

at the titrator and 

carry out the following 

steps 8, 9 

and 10 within six 

seconds. 

8. Remove the conditioning vial from 

the oven using the crimping tongs. 

Caution: hot! 

9. Insert the sample 

vial into the oven 

of the 860 KF 

Thermoprep. 

10. Pierce the septum 

with the needle 

and then wait until 

the titration has 

finished. 

11. When the titration 

has finished, remove 

the sample 

vial from the oven 

using the crimping 

tongs. 

Caution: hot! 

Karl Fischer titration with Metrohm and the new 860 KF Thermoprep is easy, safe and 

precise. Convince yourself at your local Metrohm agency! 


Titration, ion chromatography and direct measurements 

Fully automated drinking water analysis with TitrIC 2.0 

Until recently, drinking water analysis was time-consuming, complicated and required 

a lot of manual work. Not anymore! Metrohm‘s TitrIC stands for the fully 

automated analysis of drinking water using titration, ion chromatography and direct 

measurements (pH, conductivity and temperature). All the ionic components are 

determined reliably, rapidly and reproducibly. 

The samples only have to be placed on the sample rack. TitrIC then takes control 

and works irrespective of daytime or nighttime and even at weekends. Intelligent 

control and proven technology guarantee reliable analyses. TitrIC works fully automatically; 

up to 100 samples can be conveniently determined without requiring any 

manual intervention. The results are stored in the internal database and can also be 

shown in the form of a well-laid-out report. The high degree of automation reduces 

costs and increases the precision of the measurements. TitrIC can be conveniently 

controlled by the TitrIC 2.0 software, which is a combination of the well-proven 

tiamo and MagIC Net software packages. 

The low space requirements of TitrIC are well worth mentioning. Synergies between 

titration, direct measurement and ion chromatography from Metrohm come into 

play here. All the methods use the same liquid handling units and a common sample 

changer. This helps to save both costs and space. TitrIC is based on the most 

up-to-date and highly reliable analytical instruments and utilizes the vast know-how 

and experience gathered by Metrohm, the market leader for ion analysis. The investment 

payback time is very short. 

Parameters that can be determined with TitrIC 

Anion IC with TitrIC 

• Fluoride 

• Chloride 

• Bromide 

• Nitrite 

• Nitrate 

• Phosphate 

• Sulfate 

• … 

Cation IC with TitrIC 

• Lithium 

• Sodium 

• Ammonium 

• Potassium 

• Calcium 

• Magnesium 

• … 

Direct measurements with TitrIC 

• pH 

• Temperature 

• Conductivity 

Titrations with TitrIC 

• p value (titration to pH = 8.2) 

• m value (titration to pH = 4.3) 

• Calcium 

• Magnesium 

Calculations with TitrIC 

• Molar concentration of all cations 

• Molar concentration of all anions 

• Ionic balance 

TitrIC is extremely flexible and can therefore be optimally adapted to suit a wide 

range of analytical tasks. The application determines which parameters are of interest. 

Different methods and procedures can be freely combined with one another. 

New: TitrIC 2.0 

The informative TitrIC report shows all the results at a 

glance. 



This flow chart gives an example of a drinking water 

analysis procedure with TitrIC 5. A sequence of direct 

measurements and titrations runs in parallel to the analysis 

of the drinking water by ion chromatography; this 

saves a lot of time. The sequence proceeds fully automatically. 

The system consists of the 856 Conductivity Module, four 

800 Dosinos, 802 Stirrer (propeller stirrer), 809 Titrando, 

815 Robotic USB Sample Processor XL and 881 Compact 

IC pro with sequential suppression. 

The system consists of the 856 Conductivity Module, 

three 800 Dosinos, 802 Stirrer (propeller stirrer), 855 

Robotic Titrosampler, one 881 Compact IC pro without 

suppression and one 881 Compact IC pro with sequential 

suppression. 

Anions 

F – , Cl – , NO 2 – , Br – , 

NO 3 – , HPO4 2 – , SO4 2 – 

Apart from water analysis, TitrIC is also to be recommended for other applications, for 

example in the fields of food analysis and the electroplating or pharmaceutical industries. 

There are four basic versions of TitrIC 

• TitrIC 4 – the basic system 

855 Robotic Titrosampler 

28...100 Samples / 75...200 mL 

Conductivity 

Te m perature 

pH value 

Titration K A 8.2 (p value) 

Titration K A 4.3 (m value) 

TitrIC 

Database, report 

Fully automated system for the direct measurement of temperature, conductivity 

and pH, the titrimetric determination of p value, m value, calcium and magnesium 

as well as the determination of anions by ion chromatography. 

• TitrIC 5 – for complete anion and cation analysis 

Cations 

Li + , Na + , NH 4 + , K + , 

Mg 2+ , Ca 2+ 


and pH, the titrimetric determination of p value and m value as well as the determination 

by ion chromatography of cations (including calcium and magnesium) and 

anions. 


• TitrIC 6 – the professional solution with sealed sample vessels 




anions. The sample changer is equipped with the DisCover function for automatically 

removing the sample vessel covers. 

• TitrIC 7 – the solution for samples containing particles 




anions. Particle-containing samples have their particles removed by Metrohm Inline 

Ultrafiltration before the ion chromatographic analysis. 

Depending on the ecological system, it may take centuries for rainwater to become 

drinking water. In contrast, with TitrIC you only need a few moments to find out 

about the species contained in drinking water. 



three 800 Dosinos, 802 Stirrer (propeller stirrer), 809 

Titrando, 815 Robotic USB Sample Processor XL, one 

850 Professional IC for anions (sequential suppression) 

and cations. 


two 800 Dosinos, 802 Stirrer (propeller stirrer), 855 Robotic 

Titrosampler, one 850 Professional IC for anions 

with Sample Prep 2, one 872 Extension Module IC Pump 

and an additional iDetector for cation analysis. 


New: 863 Compact VA Autosampler / Rotating seal for Solitrode 

Economic automation for voltammetric trace analysis 

863 Compact VA Autosampler 

The 863 Compact VA Autosampler saves time and money 

– and the reproducibility of the results of your VA 

analyses will improve remarkably! 

The 843 Pump Station empties and rinses the measuring 

vessel and in this way ensures the complete automation 

of voltammetric trace analysis. 

Comfortable pH measurement 

The 863 Compact VA Autosampler is the ideal sample changer for the easy automation 

of VA systems. In combination with the 797 VA Computrace, automation in 

voltammetric trace analysis is now available at a favorable price while occupying 

very little space. In this way, small series of similar samples can be determined with 

high accuracy. 

The sample rack of the 863 Compact VA Autosampler accommodates up to 18 

samples that can be analyzed fully automatically in a single run. The peristaltic 

pump built into the sample changer transfers the sample solution from the sample 

vessel to the measuring vessel of the 797 VA Computrace. All the auxiliary solutions 

that are necessary for the voltammetric determination are added by Dosinos 

during the measuring procedure. The two pumps of the connected 843 Pump Station 

empty and rinse the measuring vessel after each determination. 

The 863 Compact VA Autosampler has two preprogrammed methods that can simply 

be selected via the built-in keyboard. A large LCD display provides up-to-date 

information on the status of the sample changer. 

Existing manually operated 797 VA Computrace systems can easily be extended 

with the 863 Compact VA Autosampler and the 843 Pump Station. 

Advantages of the 863 Compact VA Autosampler 

• Economic automation of voltammetric trace analysis 

• Compact design 

• Can be used to extend existing 797 VA Computrace systems 

• Two different method templates 

• Built-in peristaltic pump 

• 18 sample positions 

New: Solitrode now equipped with rotating seal 

With the Metrohm MVA-3 VA Automation Package you can start work immediately. 

It consists of 797 VA Computrace, 863 Compact VA Autosampler, 843 Pump Station 

and 800 Dosino with Dosing Unit, among other things. The 863 Compact VA 

Autosampler is also available separately. We offer the 843 Pump Station in two versions, 

namely with membrane pumps or with peristaltic pumps. 

Let the sample changer carry out repetitive activities. In this way you can save both 

your resources and valuable time. The automated system analyzes your samples 

with outstanding reproducibility! 

The 6.0220.100 Solitrode is a robust and reliable pH electrode. With its break-proof 

plastic shaft, it is ideal for routine use in the laboratory. 

As a new feature, the Solitrode has now been equipped with a very convenient 

system for sealing and unsealing the electrolyte refill opening. The opening is now 

made accessible by turning the plastic ring counterclockwise and sealed by turning 

it clockwise. 


Bath analysis with ProcessLab 

Monitoring pickling baths in the steel industry 

Scale and rust as steel surface contaminants 

Steel is one of the most important starting materials for innumerable products. The 

world‘s yearly steel production exceeds 1.3 billion tonnes (1). For some time now, 

demand has exceeded production, which has led to massive price increases for 

steel. As a result, new production capacities are being set up and existing plants 

extended at high investment costs. In order to increase the yield while keeping the 

quality constant and costs low, each individual step in the production process must 

be adequately monitored and controlled. An extremely important part of the process 

is pickling the steel, in which impurities resulting from previous production 

steps, for example the scale 1 produced during rolling, or any rust already present, 

are removed and the surface prepared for subsequent process steps. At the same 

time, interfering annealing colors are removed, the surface being passivated by 

the formation of a protective layer and in this way protected against further corrosion. 

Only after the pickling process can steel be formed or its surface treated and, 

for example, used for the production of automobile or metal construction components. 

Removal of impurities by using pickling baths 

The pickling baths used are made up of diluted acids, for example hydrochloric or 

sulfuric acid, or are mixtures of acids such as HNO 3 / HF or H 2SO 4 / H 3PO 4 / HF. 

Accelerants and other auxiliary agents are often added to these mixtures to optimize 

and speed up the process. While pickling removes impurities, the acids used 

also attack the steel surface and partially dissolve it. This is why it is important that 

process-relevant parameters such as dwell time, bath temperature and bath composition 

are controlled and maintained as accurately as possible. This is the only 

way in which a pickling bath can be operated economically and, above all, in a way 

that protects both the environment and resources. Physical parameters such as 

dwell time and bath temperature are easy to monitor, whereas the analysis of bath 

constituents is usually more complicated and must be carried out in an analytical 

laboratory. 

Analyzing pickling baths with ProcessLab 

Steel production is a continuous process that also takes place at night and during 

weekends. Qualified laboratory personnel are often not available twenty-four hours 

a day; this can make uninterrupted analytical process control difficult. This is where 

the Metrohm ProcessLab system for bath analysis opens up completely new possibilities. 

The easy-to-use ProcessLab analysis system is installed directly in the 

process area. The only thing that a process worker has to do is bring a bath sample 

to the ProcessLab and start the system by pressing a single button. ProcessLab 

analyzes the sample completely automatically. Important process information is 

available only a few minutes later. This enables on-site process analysis around the 

clock and results in much more direct and precise process control. 

Controlling the important process parameters 

Each pickling bath consists of numerous constituents and additives, not all of which 

are equally relevant to the process. Four of these analytical parameters have a considerable 

influence on the steel pickling process: the amounts of free and total acid 

and the iron(II) and iron(III) concentrations. The analyses of these parameters is 

described in detail below and in Metrohm Application Bulletin 295 (2). 

__________________________ 

1 Scale is iron(II, III) oxide that forms on the surface of iron or steel when steel is formed or treated at 

high temperatures. 

Surface-treated steel products 

Application: ProcessLab 



ProcessLab analysis system with analysis module and 

TFT operating unit with touch-screen. 

The free acid (FA) is a measure of the acid still available for pickling. It is determined 

by potentiometric titration with an NaOH solution to pH 4.2. It is given as the 

equivalent of an acid present in the bath; in a hydrochloric acid pickling bath, the 

NaOH consumption corresponds to the free acid in g HCl per liter. During the pickling 

process in a hydrochloric acid pickling bath, the free acid reacts with the metals 

to form metal chlorides, which means that the free acid concentration decreases 

and the bath must be topped up by the addition of concentrated hydrochloric acid. 

The total acid (TA) corresponds to the total amount of free acid plus the amount of 

reacted acid. The total acid is determined by titrating with NaOH to pH 8.6. The total 

consumption of NaOH then corresponds to the total acid equivalent. 

The Fe(II) and Fe(III) contents in a pickling bath are important process control 

parameters. They are a measure of the oxidizing power of the pickling bath and 

therefore have a considerable influence on the pickling time and the quality of the 

product. Moreover, if the iron contents are too low or too high, pickling becomes 

ineffective. Fe(II) is frequently determined by titration with potassium permanganate. 

Unfortunately, KMnO4 has the disadvantage that interfering chlorine and chlorine 

dioxide are formed in the presence of hydrochloric acid. Another disadvantage 

is the unstable titer of potassium permanganate solutions. Thus, KMnO4 is not really 

suitable for routine process analysis. In contrast, cerium(IV) is highly suitable; 

it is also a strong oxidizing agent and reacts with Fe(II) according to the following 

equation: 

Fe 2+ + Ce 4+ � Fe 3+ + Ce 3+ 

In this reaction, no interfering intermediate products are formed even in the presence 

of large amounts of chloride and the determination is quantitative. As cerium(IV) 

solutions have a very stable titer they are ideal for the determination of Fe(II) in pickling 

baths. The endpoint of the redox titration is detected by means of an ordinary 

platinum redox electrode. 

In addition to the absolute concentrations of Fe(II) and Fe(III), the ratio of the Fe(II) 

to Fe(III) concentration is also important for an effective pickling process. It should 

always lie within a certain range. Auxiliary agents such as hydrogen peroxide or nitrites 

oxidize Fe(II) to Fe(III) and therefore alter the ratio of these two components. 

Optimal pickling results can only be achieved when the pickling bath has a high oxidizing 

power with an optimal ratio between Fe(II) and Fe(III). 

An overview of the Metrohm analysis system 

The ProcessLab system presented here determines fully automatically those 

parameters that are important for the smooth running of a pickling bath: free acid 

and total acid as well as the Fe(II) and Fe(III) concentrations. The system is installed 


in the vicinity of the process to be monitored and allows the rapid on-site analysis 

of various pickling baths. A ProcessLab analysis system always consists of one 

or several analytical modules adapted to the particular application and a TFT 

operating unit. With the built-in touch-screen (option) operation becomes even simpler 

and more comfortable. 

Both the operating unit and the analysis module are contained in a robust, splashwater-protected 

housing and are ideally suitable for use under rough production 

plant conditions. 

The analysis module of the system described here is also of modular construction. 

A titration vessel with magnetic stirrer, variable and automatic sample metering 

using a sample loop and an 800 Dosino as well as two 800 Dosinos for the exact 

addition of the two titrants Ce(SO4) 2 and NaOH are contained in one housing. 

The peristaltic pumps are used for the automatic addition of reagents and auxiliary 

agents and for rinsing the titration vessel. 

The user only has to take a sample from the bath and bring it to the system. The 

analysis sequence for the automatic determination of all four parameters is started 

by pressing a single button. The sample is metered automatically, transferred to the 

titration vessel and the concentrations of the analytes determined by titration. All the 

necessary process information is available within only a few minutes, without the 

bath samples having to be taken to the laboratory for analysis. 

Determining the free and total acid 

2 mL sample is metered fully automatically, treated with 20 mL potassium fluoride 

solution (c(KF) = 3 mol/L) to mask the iron, demineralized water is added and the 

solution then titrated with NaOH solution to pH 4.2. The NaOH consumption corresponds 

to the amount of free acid in the bath. A further aliquot of the sample is 

titrated with NaOH solution to pH 8.6; in this case the total amount of NaOH consumed 

corresponds to the total acid concentration in the bath. 

Determining the Fe(II) and Fe(III) concentrations 

Demineralized water is placed in the titration vessel and a sample aliquot of 2 mL is 

added to it automatically. Using a Pt electrode, titration is performed with cerium(IV) 

sulfate solution (c(Ce(SO 4) 2) = 0.1 mol/L) to the first endpoint. The Ce(IV) consumption 

corresponds to the Fe(II) concentration in the pickling bath. 

• EP 

The Fe(III) concentration is then calculated from the free and total acid content taking 

into account the cerimetrically determined Fe(II) concentration. 


Analysis module equipped with Dosinos, peristaltic 

pumps and a titration vessel for automatic pickling bath 

analysis. 

Typical titration curve for the redox-potentiometric Fe(II) 

determination by titration with cerium(IV) sulfate. 



The advantages of the ProcessLab system 

A single analysis system determines all the relevant bath parameters and collects 

important process information. The results are available at any time for the subsequent 

traceability of the process and for making audits easier. The system can 

also transmit status signals, for example if a predefined limit is infringed or if a 

fault occurs in the system. Information about the bath content can also be easily 

transmitted in the form of an analog 4...20 mA signal. The simple process integration 

is clearly one of the many advantages of the ProcessLab system; information 

is immediately available to the personnel in the operations center or the process 

monitoring system. Therefore it is possible to react directly to variations and, if 

necessary, to take countermeasures. If a variation does occur, the correct amount 

of fresh acid or auxiliary agent to be added can be calculated with the aid of the 

included «tiamo for ProcessLab» software; it is even possible to do the addition 

fully automatically. Thanks to the rapid availability of the analytical data, the pickling 

process can be carried out under optimal conditions. On the one hand, this improves 

the quality of the end product, on the other hand, there results a longer operating 

period for the pickling bath with simultaneous reduction of its running costs 

(reduced usage of chemicals). As a result of the cost savings due to more efficient 

bath control and higher-quality end products, a ProcessLab system normally has a 

pay-back time of less than three years. 

Summary 

The quality of the end product is considerably influenced by how well and reproducibly 

the individual process steps are carried out. The Metrohm ProcessLab 

system described here is used for fully automatic on-site analysis of all the relevant 

process parameters of a steel pickling bath. This means that all the analytical 

data is available directly after sampling. The amount of bath additives to be 

added can be calculated automatically and, if required, also added automatically. 

The system offers numerous possibilities for process integration, guaranteeing 

the relevant information is quickly available wherever it is required. 

Thanks to ProcessLab, pickling baths can be used more economically and ecologically 

and operating and disposal costs are considerably reduced. This also makes 

a particular contribution to protecting both resources and the environment. 

References 

(1) International Iron and Steel Institute (IISI), data for 2007, www.worldsteel.org 

(2) Metrohm Application Bulletin AB 295: Determination of Fe2+ , Fe3+ , total and free 

acid in an etching bath (steel industry), Metrohm AG, Switzerland 

Further reading 

Monograph: Practical titration – training manual for titrimetric volumetric analysis, 

2005, 164 pages, Metrohm AG, Switzerland 

Prozessbegleitende Analytik in der Galvanotechnik, T. W. Jelinek, 1999, 440 pages, 

Eugen G. Leuze Verlag, Saulgau 


Background information about Nucomat 

The Belgian company Nucomat1 , enjoys an excellent reputation in the system integration 

sector and as a manufacturer of customer-specific solutions for laboratory automation. 

The core competency of Nucomat lies in the conversion of manual laboratory 

methods into automated systems. Robotics and automation are frequently associated 

with mass production and a large number of constantly repeated steps carried out as 

quickly as possible. As can be seen from the text below, laboratory automation requires 

a different approach often involving other criteria. 

Nucomat builds turnkey units using a building block system made up of autonomous 

work stations linked to a sophisticated control and monitoring system. Nucomat can 

also incorporate instruments from other manufacturers in its systems in order to solve 

specific customer problems. 

Nucomat installed various automated systems all over the world for research applications 

in the fields of life sciences, biotechnology, food technology, body care and 

cosmetics. Other systems are used for environmental analysis, the analysis of ore 

samples, quality assurance/quality control and petrochemical applications. 

Nucomat systems are used for applications such as: 

– Automated determination of copper in ore samples from open-pit mines. The 

system complies with stipulated operating rules and has a built-in quality control 

system. It is in continuous use 24 hours per day, 7 days per week. 

– Automated sample preparation for heavy metal determination in liquid samples 

using ICP-AES. 

– Automated preparation of plutonium reference materials. 

– Recording and observing bacterial growth using measurements for determining 

the oxygen consumption in the development of new food preservatives. 

– Sample preparation of viscous liquids while monitoring pH and viscosity. 

– Cryotube serum aliquotation for clinical studies. 

– Automated screening with a high sample throughput for drug development. 

– Automated filtration for radioligand binding assays. 

An overview of the Nucomat system for the analysis of fertilizers 

The automated Wetchem system for the analysis of fertilizer samples has recently 

been developed by Nucomat in close cooperation with Metrohm (see Fig. 1). The 

system allows multi-species determination (about 10 different species) and also 

carries out the complete sample preparation procedure, which is particularly worth 

mentioning. Sample preparation for wet-chemistry instrumental analysis methods 

still remains tedious and labor-intensive even in modern laboratories if it has to be 

carried out manually. 

Outstanding features of the system are, amongst others: 

– Sampling and sample preparation of liquid and solid samples 

– Several reagent addition possibilities 

– Classical «hotplate» digestion 

– Making up the sample to a given volume by weighing (making to mass) 

Customer application: Automated system for fertilizer analysis 

Automated Wetchem system for fertilizer analysis 

__________________________ 

1 Further information on the Belgian company Nucomat, which was founded in 1988, can be found on 

the internet under www.nucomat.be. 

Fig. 1: One of Nucomat’s product lines is the automated 

«Wetchem system» for the analysis of liquid chemicals. 

System characteristics can be described briefly as «untreated 

sample in, validated result out», as well as the 

possibility of carrying out several analysis methods. 



Fig. 2: The twin systems, each consisting of two 861 

Advanced Compact ICs for the analysis of anions and 

cations, respectively. 

Fig. 3: Computer image of the module with the Metrohm 

ion chromatographs. 

Fig. 4: The Nucomat robotic system for transporting 

samples and containers. The illustration shows details 

of the robot head with the gripper arm mounted eccentrically 

on the spindle axis. 

Fig. 5: As the transport robot is mounted above the working 

area, even Erlenmeyer flasks under the fume hood 

(center of illustration) can easily be accessed. 

– Checking the instrument calibration by control measurements 

– Integrated quality control 

– Automatic system restart after power failure 

– Closed-loop labware utilization (e.g. glass beakers) with built-in washing station 

– Ion chromatography and titration as analysis methods 

– Sample preparation for ICP-AES spectroscopy 

– LIMS compatibility 

Ion chromatography system 

The Nucomat system described below uses 861 Advanced Compact IC ion 

chromatographs from Metrohm. In order to ensure as good a protection against 

breakdown as possible, two twin systems have been installed, each with a 

separate ion chromatograph for the analysis of anions and cations (see Fig. 2 

and 3). 

Robot with gripper arm 

The main robot for sample and flask transport has four degrees of freedom. The 

robot head has a gripper arm (Fig. 4). Movements are based on a Cartesian coordinate 

system, with the belt-driven robot head moving in the X-Y plane and covering 

a maximum area of 2 x 2 meters. Movement along the Z axis (enabling 40 cm 

vertical reach) is performed by a spindle axis. The spindle can be rotated through 

360 degrees for optimal use of the whole available working space. The pneumatic 

gripper is mounted eccentrically on the spindle axis. All the labware inside the fume 

hood can be accessed without any problems (Fig. 5). 

The spatial position of the gripper arm is calculated on the basis of the dimensions 

given in the construction plans and of the index signals from the incremental sensor 

of the robot. No additional teaching is required for directing the robot head to 

any coordinates. 

After installation or maintenance work (for example on the drive motor, incremental 

sensor/encoder or drive belt), the offset of the robot head needs to be determined. 

Therefore a calibration bracket is mounted permanently on the support frame. 

Robot encoder index pulses are then referenced against the calibration bracket 

for proper alignment; no teach-in programming is necessary. 

Analytical procedure 

The Wetchem system analyzes liquids, suspensions, solid fertilizer granules or already 

ground powder samples. After scanning the barcode, the user only has to 

place the samples on the upper conveyor belt. 

The barcode information is linked to a LIMS configuration file containing samplespecific 

parameters: amount of sample, acid to be added, stirring time, digestion 

temperature, final volume, analytical determination method and the corresponding 

measuring parameters. 

Several working solutions can be prepared from one stock solution. In principle, 

each stock solution remains within the reach of the gripper arm until the preparation 

of the working solutions derived from it has been concluded. 

By pressing a button, the user can cause the robot to reject a working solution at 

any time if it does not satisfy the sample preparation quality requirements. The robot 

then automatically prepares a new working solution from the corresponding 

stock solution. 

Wide-neck 250 mL glass Erlenmeyer flasks are suitable for most sample preparation 

steps and determinations (Fig. 6). In contrast, PTFE flasks are used for the determination 

of boron, as digestion in glass vessels would result in contamination of 

the sample and therefore lead to incorrect results for this element. 


After the analysis, the used sample flasks are cleaned with hot water in a washing 

station and are used again. 

Stock solutions that are no longer required, excess working solutions, calibration 

solutions and samples ready for analysis by ICP-AES are transferred to the lower 

conveyer belt by the robot for further processing or disposal. 

The ion chromatographs are controlled by the Metrodata IC Net software, which 

also records the measuring data. The analysis results obtained from this measuring 

data are stored in the internal database and simultaneously exported as ASCII-files 

in order to be read into the LIMS. 

Calibration and verification of the ion chromatographs 

Calibration and control solutions for ion chromatography are simply placed on the 

upper conveyor belt. The robot transfers these calibration solutions directly to the 

ion chromatographs and starts instrument calibration via the IC Net software. The 

operating personnel must ensure that all the necessary calibration solutions are 

available when required. A control solution is then used for the verification of the 

IC. The analysis result for the control solution is compared with the expected value. 

Depending on the result of this comparison, a control character is set to either enable 

the ion chromatographs for the analyses or to block them. 

The operator can insert additional control solutions in order to verify the instrument 

performance and to evaluate the accuracy of the analysis as required by the 

laboratory’s quality control procedures. 

Instrument calibration is carried out at the same time as sample preparation. 

Sampler for liquids and solids 

The dosing station sampler obtains all the relevant information necessary for preparing 

the solutions from the Wetchem control software. The robot provides the 

sampler with the necessary Erlenmeyer flasks for the stock and working solutions. 

The sampler disposes of several hundred magnetic stirrer bars. 

As soon as everything is ready, the preparation of the solutions can begin. The sequence 

consists of determining the tare of the Erlenmeyer flask, providing it with a 

magnetic stirrer bar, adding the sample, dosing in all the necessary reagents and 

transmitting the measured weights for each of these items. 

The program is aborted as soon a serious error is detected during the preparation 

of the solutions. The user can terminate the preparation of a sample solution by 

pressing a button. The affected Erlenmeyer flask is then removed immediately and 

a new solution is prepared. 

Integrated quality control 

The accuracy of the balance is automatically checked at predefined intervals by the 

Wetchem system using a reference weight (Erlenmeyer flask). Each individual step 

in preparing the solutions, e.g. the addition of a certain volume of acid, is checked 

against the measured values from the balance. All measured values are permanently 

stored. 

If the result of a control measurement differs too much from the reference value, 

then the availability of the particular analytical instrument is set to inactive by the 

system control (after confirmation by the operating personnel). In such a case, the 

remaining samples to be analyzed are diverted to a different, active analytical instrument 

or parked until the analytical instrument is activated again. 

The Wetchem software 

The Wetchem application program is based on Nucomat’s «Robin» software 

architecture, an event-controlled command-line interpreter with SQL server 

database. 


Fig. 6: View of the rear panels of the ion chromatographs 

and the labware of the Wetchem system (mainly wideneck 

Erlenmeyer flasks) that are necessary for fully 

automatic sample preparation. 



Fig. 7: This illustration shows a chromatogram obtained 

with a fertilizer sample by ion chromatography, 

in which the nitrate, phosphate and sulfate anions are 

determined. 

Ammonium 

Potassium 

Nitrate 

Phosphate 

Magnesium 

Calcium 

Sulfate 

Strontium 

Fig. 8: Cations such as ammonium, potassium, magnesium, 

calcium and strontium can also be determined in the 

fertilizer sample by ion chromatography. 

Fig. 9: This illustration shows the IC Net interface with 

ion chromatograms of cationic standards used for a calibration. 

If problems occur, the IC Net software is ideal 

for troubleshooting. 

If a calibration point is clearly off the calibration curve 

(i.e. the measurement is incorrect), then the corresponding 

calibration solution can simply be analyzed again in 

order to complete the calibration. A control solution must 

first be measured before the ion chromatograph can be 

activated for the analysis. 

The system allows the generation of various user profiles in order, for example, 

to give only the system administrator the right to alter important parameters. All 

alterations to the system configuration are permanently recorded and archived to 

ensure traceability. The same applies for each sample presented to the system after 

scanning, all movements of the robot, all weights and all messages from the 

dosing station. 

If the connection to the LIMS computer should be briefly interrupted, then the 

Wetchem system can still continue to work; data matching takes place when the 

connection is reestablished. 

Metrohm’s compact ion chromatographs 

An 861 Advanced Compact IC Metrohm ion chromatograph consists of: 

– An Eluent Organizer 

– A serial dual-piston pump showing extremely low pulsation with a flow range of 

0.2 to 2.5 mL/min 

– An injection valve allowing manual or automatic sample injection that can 

optionally be equipped with an «internal loop» with a volume of only 0.25 μL 

– A completely metal-free flow path with all components made of PEEK or PTFE 

– A separation column 

– The Metrohm Suppressor Module MSM II for chemical suppression that is responsible 

for the extremely low noise level of only 0.2 nS/cm 

– A conductivity detector with four different measuring ranges: 0...50, 250, 1000 

and 5000 μS/cm 

– The Metrohm data acquisition and control software IC Net that is also used for 

the determination of anions, cations and carboxylic acids 

The sample to be injected is first pumped through an inline filter by a two-channel 

peristaltic pump (this prevents clogging of the separation column) and then enters 

the injection valve of the ion chromatograph. After the injection the valve is switched 

so that the filter can be rinsed with an acidified solution in reverse flow. The unit with 

the peristaltic pump is located directly beneath the ion chromatographs. 

Applications and results 

In addition to the Metrohm ion chromatographs, a titrator is also incorporated in the 

Wetchem system. In this way, the system described above can be used to determine 

the following species and parameters: 

+ K2O, P2O5, total nitrogen content, nitrogen as ammonium (NH4 ), nitrogen as 

– 2 – nitrate (NO3 ), CaO, MgO, strontium, sulfate (SO4 ), chloride (all these substances 

by ion chromatography; Fig. 7 and 8); pH (using a pH electrode), free acid (titration 

with NaOH solution and a pH electrode) as well as B, Al, Fe, Cu, Zn, Cr, Ni, Cd, Mn 

(manual determination using an ICP-AES instrument). 

The Metrohm IC Net software runs as a background process on the Wetchem computer. 

In normal operation, the operating personnel do not have to bother with IC 

Net. However, should a problem occur with the ion chromatographic analysis, the 

IC Net software is an extremely useful diagnostic tool that is available at any time 

(Fig. 9). 

We would like to thank Prof. Chantal Block, Prof. Carlo Vandecasteele and 

Noel Van de Steene (CEO Nucomat) for writing this text and providing us with 

the measurement data and illustrations. 


Enzymatic degradation of bioplastics 

Basic information about bioplastics 

Biogas and biodiesel have been well known to the general public for several years. 

But what are bioplastics and how are they formed? 

For many million years, bacteria have been using carbon compounds as storage 

substances. Among other things, microorganisms require nitrogen and phosphorus 

for growth and cell division. If one of these two elements is missing, cell division 

stops. At the same time, the cells switch their internal program to «storage» 

by taking up carbon, mainly from sugars, fatty acids and other compounds. This 

carbon is then stored inside the cells in the form of granula1 that are made up of 

poly(3-hydroxyalkanoate) (PHA), a group of polyesters of which poly(3-hydroxybutyric 

acid) (PHB) is particularly widespread (Fig. 1). As soon as the bacteria have 

everything they require for cell division again, the stored carbon is consumed. 

PHA compounds (Fig. 2) have material properties that very closely resemble those 

of conventional plastics such as PET. Additionally, they are biodegradable (Fig. 3) 

and can be obtained from self-regenerating raw materials. Other types of bioplastics 

have been developed as well, for example on the basis of corn starch or polylactic 

acid (PLA). Up to now, PHA products have only been used for test purposes: 

PHA isolation and processing is still much more expensive than the manufacturing 

of plastics from crude. 

Depolymerization studies at the University of Stuttgart 

In Prof. Dr. Jendrossek’s workgroup in the Institute for Microbiology at the University 

of Stuttgart, the focus of interest is the degradation of the polymer in the 

cell itself (depolymerization [1]). It is chiefly the enzymes (so-called PHA depolymerases) 

that are responsible for this and they are therefore being studied in detail 

in order to learn more about their exact role within the cell system. Part of this 

enzyme is located on the granula surface and, if needed, splits the long polyester 

molecules into shorter ones that serve as building blocks for cell metabolism. The 

enzyme activity can be measured by the acid that is released by the hydrolysis of 

each ester bond. 

__________________________ 

1 Granula are grain-shaped deposits in biological cells that usually contain storage or secreted substances. 

They can be easily recognized under a microscope. 

Customer application: degradation of bioplastics 

Fig. 1: Electron micrograph of Ralstonia eutropha H16 

cleary showing stored PHB granula (from [2]). 

O CH3 O CH3 O CH3 H O 

O O O H 

n 

Poly-β-hydroxybutyrate (PHB) (n ~ 60) 

Fig. 2: Structural formula of polyhydroxybutyrate (PHB). 

Fig. 3: PHB bottle after incubation in a sewage plant for 

0, approx. 4 and approx. 10 weeks. 


Customer application: degradation of bioplastics 

Fig. 4: Measurement of the hydrolysis rate of native PHB 

granula by PHB depolymerase. 

Incubation in tris buffer for 6 hours. pH set to 8.5 and 

kept constant by automatic addition of c(NaOH) = 10 

mMol/L. pH variation shown as pink curve with y-axis 

at right; volume of added NaOH solution shown as blue 

curve with y-axis at left. 

After 1400 seconds the acid release rate and therefore 

the NaOH consumption increased greatly due to the addition 

of concentrated depolymerase enzyme to the solution. 

Fig. 5: Operation of the 842 Titrando with tiamo control 

and data acquisition software. 

Activity test procedure based on titration 

For the activity test, the granula are isolated from the bacteria and placed in the 

reaction vessel of the 842 Titrando together with several milliliters of a weak buffer 

(Fig. 4). Using this pH-stat titrator allows to detect the weak acid release at the 

small PHB spheres. A very precise and robust pH micro-electrode transmits any 

variation from the set pH value via the tiamo software (Version 1.1) to the Dosing 

Unit of the 800 Dosino. To again obtain the set pH, NaOH (e.g. c(NaOH) = 0.01 

mol/L) is added by the Dosino with an extremely variable dosing rate ranging theoretically 

from 0.01 μL/min up to 60 mL/min. By continuously recording and plotting 

the amount of base consumed versus time, the acid release rate can easily be 

monitored in real time on the computer display (Fig. 4). This procedure is ideally 

suitable for studying the influence of various substances on the hydrolysis rate of 

the PHB granula. A thermostatted reaction vessel equipped with a temperature sensor 

also allows the effects of temperature changes on the release rate of acid to be 

investigated. As two pH-stat titrations can be carried out in parallel with tiamo, 

the acid release can be recorded simultaneously at two different temperatures. Two 

measuring cells and two electrodes (Fig. 5) connected to the 842 Titrando are required 

to do this. 

Evaluation of the results 

At the end of the measurement, the data and the graphs can be entered in a prestructured 

report data sheet and printed out; they can also be exported into other 

programs (Excel, PowerPoint, etc.) for further processing. With tiamo the graphs 

can be compared, reports optimized, comments inserted, etc. There are virtually 

no limits to result presentation. 

We would like to thank Dr. Gebauer from the University of Stuttgart for this summary. 

Further information can be found in the literature or on the Internet [1]. 

Literatur 

[1] Birgit Gebauer and Dieter Jendrossek 

Assay of Poly(3-Hydroxybutyrate) Depolymerase Activity and Product Determination 

Applied and Environmental Microbiology, 72/9 (2006) 6094-6100 

http://aem.asm.org/cgi/content/abstract/72/9/6094 

[2] Jendrossek, D. and Handrick, R. 

Microbiodegradation of polyhydroxyalkanoates 

Annu. Rev. Microbiol. 56 (2002) 403-432 


Trade fair for analytical and laboratory techniques 

The Analytica trade fair is held every two years in Munich. With its accompanying 

conference, it is the most important trade fair for analytical and laboratory techniques 

in the German-speaking countries, if not in the whole of Europe. 

This year, Analytica was held for the 21st time. Metrohm again had one of the largest 

booths and the best place right at the front in Hall A1 (Fig. 1). 

After 27 190 visitors and 847 exhibitors in 2006, this year 32 500 visitors and 1032 

exhibitors came to Munich. Many exhibitors reported larger numbers of visitors and 

more visitors with specific investment plans – this means that the fair was a great 

success. 

We also can confirm this from the Metrohm point of view and are happy about the 

largest number of visitors by far we have ever had at an Analytica. Of course, the 

visitors were mainly interested in the new products: 

– The new 848 and 870 Titrino plus titrator family 

– The branch-specific packages for them for the analysis of food, drinks, oil and 

water 

– The new 865 and 876 Dosimat plus 

– The new 881 and 882 Compact Ion Chromatographs 

– MagIC Net as a comprehensive software solution in ion chromatography 

– The tiamo software, which now also supports the additional possibilities for 

sample preparation with the 815 Robotic Soliprep 

– Favorably-priced automation in voltammetry and IC with the 863 Compact Sample 

Changer 

– Close-to-the-process automation of routine analyses with ProcessLab and the 

new software tiamo for ProcessLab 

Fig.1: The Metrohm booth in Hall A1. 

Analytica trade fair 


Analytica trade fair 

Fig. 2: Many new products and applications arranged 

according to branches were presented at the Analytica 

fair. 

Fig. 3: Birgit Prinz was a very likeable interviewee and 

Dr. Knabe knew an awful lot about soccer – they drew 

a large crowd. 

All these new products were presented in the context of branch-specific applications. 

The main focus was on pharmaceuticals, general chemistry, the environment, food, metals, 

energy and biofuels as well as on the research and education sectors (Fig. 2). 

Soccer, or rather the 2008 European Championship, was our promotional theme 

accompanying the fair. It helped us to arouse the visitors‘ interest. The Metrohm 

championship schedule was much sought after right up to the last day of the fair. 

The absolute highlight was the interview and autograph hour on Wednesday morning. 

About 200 visitors seized the opportunity of seeing Birgit Prinz, Germany’s 

most successful female soccer player, in person and taking home a football with 

her autograph (Fig. 3). 

We don’t want to reveal just what our Development and Marketing Departments are 

preparing for Analytica 2010. Let yourself be surprised and visit us again in Munich, 

23 to 26 March 2010. We look forward to seeing you there. 


Automation and safety go hand in hand 

Laboratory work can be risky. One of the main problems is spilling chemicals of 

any type. In contrast to purely manual laboratory operation, in a fully automated 

analytical system it must be guaranteed that, should an operating error occur, neither 

personnel nor instruments can be harmed by escaping liquids. Metrohm offers 

you many helpful accessories for safeguarding you and your equipment; these are 

presented below. 

849 Level Control 

The thorough cleaning of the sensors used is absolutely essential to obtain exact 

and reproducible results with titrations or other analytical methods. Nowadays this 

cleaning process is carried out between the analyses as standard. Pumps aspirate 

off the titrated solution and rinse the sensors with fresh water. It is of crucial importance 

that the rinsing-solution canister always contains sufficient liquid to ensure 

proper cleaning of sensors; at the same time, the waste canister has to be able to 

accommodate the waste solution. Although this should be checked before the start 

of each series of measurements, checks are occasionally forgotten or canisters 

become empty or full, respectively, during the series of measurements. Depending 

on the system used, it is possible to analyze 100 and more samples within a 

single series. It is therefore mandatory to regularly monitor the filling levels of the 

canisters connected to the appropriate pumps. Continuous visual monitoring of the 

canister filling levels in an automated unit is clearly out of the question. Let our 849 

Level Control take care of this for you. This monitoring instrument, which is directly 

linked to the control software of your sample changer, reliably informs you which 

canister must be filled or emptied. 

The 849 Level Control transmits the sensor signal to a Metrohm automation system. 

In this way, the 849 Level Control can be used in all Metrohm systems in which it 

is possible to scan remote lines (SCAN command). This includes the Titrando instrument 

range with or without an 814 USB Sample Processor or 815 Robotic USB 

Sample Processor XL (a Remote Box is required for each of these) as well as various 

778 Sample Processor and 789 Robotic Sample Processor XL models. 

Beaker sensor 

In order to increase efficiency in routine laboratories, ever more samples are being 

analyzed in ever less space – the analyses are completely automated wherever 

possible. Taking titration as an example, the beakers with the samples to be analyzed 

are simply placed on the rack of an Autosampler. Then, the addition of various 

auxiliary solutions and titrants takes place automatically. As mentioned above, 

after the analysis, the electrodes are rinsed with the appropriate solvents, for example 

water or ethanol. As a result of the ever-increasing number of samples to be 

analyzed, an error can quickly occur and the prepared sample beaker is suddenly 

in the wrong position on the sample rack. In most cases the user only recognizes 

Practical tips: Safety 

The 849 Level Control with the sensor attached to the 

canister. 

The beaker sensor for one-row sample racks in action 

(left). 

Robotic arm with beaker sensor for multi-row sample 

racks (right). 


Practical tips: Safety 

Collection tray with tubing for connection to a waste 

canister. 

778 Sample Processor 

814 USB Sample Processor* 

such errors when it is already too late, i.e. when solvent, titrant and rinsing reagents 

have flooded the instruments used for the analysis and the surrounding laboratory 

bench. If this is not noticed in good time, then not only the automated unit but also 

the PC or other peripherals could be damaged. 

While Metrohm cannot minimize your sample throughput, we can ensure that your 

instruments and personnel are optimally protected against contact with chemicals. 

With our beaker sensor you can start your sample series with a clear conscience 

and be certain that no surprises will occur: the analysis will only be carried out 

when there actually is a beaker in the correct position. 

Collection tray 

Despite the beaker sensor, it is still possible for a beaker to overflow because of 

incorrectly selected stop criteria or too large an amount of sample. In such cases it 

should also be ensured that neither instruments are damaged nor personnel injured. 

Metrohm can also help to eliminate this safety risk with the aid of a collection tray. 

The collection tray is mounted directly beneath the sample rack. Should a sample 

beaker overflow, the tray collects the escaped liquid and discharges it directly into 

the waste canister. In this way, in case of an emergency, only the sample rack and 

a few beakers come into contact with the escaped solutions. 

Automation with Metrohm means much more than simply changing sample beakers. 

We free you from routine work so that you are able to concentrate on more 

important and urgent matters, and at the same time provide maximum safety for 

the user. The collection tray is available in two different sizes and can also easily be 

retrofitted to existing systems. 

Safety for your analysis system at a glance 

789 Robotic Sample Processor XL 

815 Robotic USB Sample Processor XL* 

855 Robotic Titrosampler* 

Level Control yes yes yes 

Beaker sensor in tower yes yes yes 

Beaker sensor on 

robotic arm 

no yes yes 

Collection tray yes yes yes 

The table above shows you which safety measures are compatible with your fully 

automated analysis system. 

* 814, 815 and 855 Sample Changers require an additional Remote Box. 


New Application Notes, Application Bulletins and papers from Metrohm 

New Application Notes, Application Bulletins and papers 

from Metrohm 

Today we offer our customers and all other interested persons more than 1200 free-ofcharge 

application reports; these can be found by an online application search under 

the Web address products.metrohm.com. Their number is continually increasing! 

The following list provides an overview of recent application reports from the various 

ion analysis sectors. 

Application Notes 

Titration 

AN-H-068 Determination of ferric ion by iodometric titration 

AN-H-069 Determination of ferric ion by titration with fluoride 

AN-H-070 Determination of ferric and cupric ions in copper refining solutions 

AN-H-071 Determination of ammonium ions by titration with hypochlorite 

AN-H-072 Determination of low levels of free fatty acids in edible fats and oils 

AN-H-073 Determination of total acid number (TAN) in biodiesel 

AN-H-074 Determination of calcium and magnesium in marine brines 

AN-H-075 Standardization of tetrasodium EDTA solutions 

Ion chromatography – cations 

AN-C-107 Hydroxylamine, ethanolamine, triethanolamine and hydrazine on the 

Metrosep C 3 – 250 cation column 

AN-C-108 Methylamine in the presence of standard cations on the Metrosep C 3 

– 250 cation column 

AN-C-109 Trans-4-methylcyclohexylamine in a pharmaceutical product 

Ion chromatography with suppression 

AN-S-255 Sixteen anions separated on the Metrosep A Supp 7 – 250 using gradient 

elution 

AN-S-256 Thirteen anions separated on the Metrosep A Supp 7 – 250 

AN-S-257 Seven standard anions separated on the Metrosep A Supp 15 columns 

AN-S-258 Eleven anions separated on the Metrosep A Supp 16 – 250 column 

AN-S-259 Phosphate and citrate separated on the Metrosep A Supp 15 – 100 column 

AN-S-260 Organic acid anions in the presence of the standard anions separated 

on the Metrosep A Supp 16 – 250 column 

AN-S-261 Chloride, nitrate and sulfate in produced water 

AN-S-262 Chloride, nitrate and sulfate in cobalt acetate solution using Metrohm 

Inline Dilution 

AN-S-263 Nitrite in the presence of a high concentration of chloride on the Metrosep 

A Supp 16 – 250 

Ion chromatography with UV/VIS detection 

AN-U-38 Sulfide in mining wastewater 

Application Bulletins 

Electrochemical detection 

AB-288 Determination of acidic and alkaline solids by non-aqueous titration 

(English/French/Spanish) 

AB-289 Monitoring parameters in a phosphatizing process (pH, conductivity, 

acidity, alkalinity, fluoride and zinc) (English/French/Spanish) 

AB-290 Comparison of different sampling systems for ProcessLab (English) 

AB-292 Determination of nickel, hypophosphite and alkalinity in electroless 

nickel plating baths (English) 

IC Application Note No. S-258 

Title: Eleven anions separated on the Metrosep 

A Supp 16 – 250 column 

Summary: Determination of fluoride, formate, acetate, chloride, 

methylsulfonate (MSA), nitrite, bromide, nitrate, sulfate, 

oxalate and phosphate using anion chromatography with 

conductivity detection after chemical suppression. 

Sample: Standard solution 

Sample Preparation: None 

Column: 6.1031.430 Metrosep A Supp 16 – 250 

Eluent: 7.5 mmol/L sodium carbonate 

0.75 mol/L sodium hydroxide 

Suppressor: Sequential suppression: MSM (100 mmol/L H2SO4), MCS 

Flow: 1.0 mL/min 

Column temperature: 55°C 

Injection Volume: 20 µL 

Metrohm Information Issue 2-2008/2009 29 

Results: 

Results: 

F - (1) 

mg/L 

Formate (2) 

mg/L 

Acetate (3) 

mg/L 

Cl - (4) 

mg/L 

MSA (5) 

mg/L 

NO2 - (6) 

mg/L 

1.0 1.0 1.0 1.0 1.0 1.0 

Br - (7) 

mg/L 

NO3 - (8) 

mg/L 

SO4 2- (9) 

mg/L 

Oxalate (10) 

mg/L 

PO4 3- (11) 

mg/L 

1.0 1.0 1.0 1.0 1.0 

S-258

New Application Notes, Application Bulletins and papers from Metrohm 

No. 295e 

Application Bulletin 

Of interest 

to: 

General analytical chemistry, metals / electroplating, iron, etching bath, Fe 2+ , Fe 3+ , steel P 1, 10 

Determination of Fe 2+ , Fe 3+ , total and free acid in 

an etching bath (steel industry) 

Summary 

Acid etching baths are used for oxide removal and cleaning of the surface of different 

types of steel. To keep the bath in an optimum condition the Fe 2+ /Fe 3+ and free 

acid/total acid ratios must be maintained within certain limits. Auxiliary substances 

like hydrogen peroxide are added to influence the Fe 2+ /Fe 3+ ratio, which is responsible 

for a constant activity of the bath. 

The quality of the end products depends directly on the correct composition of the 

etching bath. Keeping these parameters in an optimum range results in a permanently 

higher quality and at the same time lowers costs due to lower reagent 

consumptions. 

This bulletin describes the monitoring of an etching bath in the steel industry. 

ProcessLab offers a solution that automatically evaluates the desired bath parameters 

(free acid, total acid, Fe 2+ and Fe 3+ ). Due to the flexibility offered by ProcessLab 

the determination of hydrogen peroxide can be integrated very easily. 

Features/general information 

�� All 4 parameters in one system 

�� OneButton analysis 

�� Easy to operate for semi-skilled staff 

�� Direct feedback of the measured results to the process control system 

�� Can be used for different baths without additional costs 

�� Additional parameters can be measured at minimum costs (e.g. H2O2) �� The method can be used in the lab as well 

Routine process analysis 

Compact analysis systems for process environments 

Frank Portala, Nils Geil and Alfred Steinbach – Metrohm AG, Herisau, Schweiz 

Process analysis has continually increased in importance in recent years. With the aim of recording changing 

process parameters rapidly and independently of a laboratory, analytical measurements have more and 

more been transferred from the laboratory to the plant. This places high demands on the analytical systems. 

They must be robust in order to function under the harsh plant environment and be optimally adapted to 

the particular process; they must also have interfaces for rapid internal and external communication via 

Ethernet, input/output lines, LIMS and databases. 

Introduction 

In view of continually increasing 

competition, production units 

must be operated as economically 

as possible. This means that products 

must be manufactured at high 

throughputs, with a high yield and 

at a favorable price while ensuring 

that the specified product quality is 

maintained. 

This means that monitoring of the 

relevant process parameters is of 

utmost importance. For high analysis 

frequencies in particular, online 

and inline analysis systems directly 

linked to the process are suitable. 

However, if several sampling points 

are to be monitored, a variety of 

parameters to be analyzed or if the 

analysis cycles are longer, then atline 

analysis systems are used, not least 

for cost reasons. In an atline system 

the sample is taken manually and 

analyzed directly at the process line 

(on-site). In this way various samples 

from different process stages or 

units can be quickly processed. 

However, conventional laboratory 

systems are frequently used as atline 

systems, although these are neither 

designed for rough plant conditions 

nor for exchange of information 

with the process environment. 

Moreover, these systems do not 

have a modular construction and as 

a result cannot be optimally adapted 

to the particular process and any 

future requirements. 

Robust atline analysis system 

The ProcessLab system presented 

here is a robust, easy-to-use atline 

analysis system that meets the re- 

Fig. 1: The robust ProcessLab analysis module and operating unit were designed 

for routine analyses. 

quirements for routine analyses 

in plant surroundings (Fig. 1). The 

system is contained in a dust- and 

splash-proof housing and, because 

of its modular design, can easily be 

adapted to meet the specific analytical 

and technical requirements. Each 

instrument consists of an operating 

unit and an analysis module with 

the wet-chemistry and electronics 

parts hermetically separated from 

each other. 

All analysis methods and results are 

centrally recorded, administered in 

a common database and available 

for monitoring as well as for direct 

control. Data can be exported via 

Ethernet to any LIMS, made available 

to a process control system or 

be used in the corporate intranet 

(Fig. 2). The digital and analog in- 

put/output (I/O) components allow 

the system to be easily incorporated 

in the process surroundings. In this 

way it can react to different input 

signals, for example automatically 

measure different parameters depending 

on the sample, trigger 

an alarm if limits are infringed or 

transfer results as analog 4…20 mA 

signals. With the Ethernet connection 

(RJ45) ProcessLab can be integrated 

into a local network or be 

fully operated by remote control. 

The system is controlled by the 

tiamo software, which is installed 

on an integrated industrial PC. The 

operating unit with built-in TFT 

monitor, touch-sensitive keyboard 

and touchpad ensures easy and comfortable 

operation. Alternatively, an 

operating unit with touch screen is 

AB-293 Analysis of Bayer aluminate liquors with 859 Titrotherm (English) 

AB-294 How to set up ProcessLab for remote controlling via a local corporate 

Ethernet (TCP/IP based) (English) 

AB-295 Determination of Fe 2+ , Fe 3+ , total and free acid in an etching bath 

(steel industry) (English/French/Spanish) 

AB-296 Liquid handling with the solenoid valve module (English) 

AB-297 Peristaltic pumps for liquid handling (English) 

AB-299 The ProcessLab I/O controller (English) 

AB-300 Determination of cyanide in process water of the steel industry (English) 

Titration 

AB-304 Titration of whole blood and blood plasma for acid-base analysis 

according to Joergensen and Stirum (English) 

AB-305 Check of surfactant electrodes (English/German) 

AB-306 A test method for the determination of the liquid efflux rate (tightness) 

of Metrohm antidiffusion tips via STAT titration (English/German) 

Papers 

Metrohm also publishes articles in a number of printed and online journals. Most 

of the papers listed below from 2008 can be found by using our online application 

search. The publishers concerned will also be pleased to help you. 

English 

1. Biofuel analysis by ion chromatography (The Application Book – March 2008, 

The Application Notebook – February 2008) 

2. Evaluation of extraction methods and bias correction by EPA method 6800 

protocol for mercury species in tuna fish tissue using an ion chromatograph 

coupled to an ICP-MS (The Application Book – Juli 2008 ; The Application Notebook 

– June 2008 and The Column – May 2008) 

3. Driving with biomass (http://www.pro-4-pro.com/de/Lab/Company- 

10592/4739c415803e3.html) 

4. Routine process analysis – Compact atline system for harsh process environments 

(CPP 03/2008) 

5. Determination of carbohydrates in foodstuffs by ion chromatography with 

pulsed amperometric detection (The Application Notebook – September 2008) 

6. Ion chromatography: Carbohydrate analysis in essential and non-essential foodstuffs 

(Food Engineering & Ingredients – October 2008) 

7. Analysis of food samples with ion chromatography after inline dialysis (White 

paper – Decision News – Sept. 2008 

German 

1. Fahren mit Biokraftstoffen (http://www.pro-4-pro.com/de/Lab/Company- 

10592/4739c415803e3.html) 

2. Umfassende Analytik von Biokraftstoffen - Teil 1 (GIT 05/2008) 

3. Umfassende Analytik von Biokraftstoffen - Teil 2 (GIT 06/2008) 

4. Analysensystem für raue Prozessumgebungen (P&A Kompendium 2008/2009) 

5. Ionenchromatographie in der Biokraftstoffanalytik (Laborscope 06/08 und GIT 

Spezial – Separation 1/2008) 

Spanish 

La cromatografía iónica en el análisis de biocombustibles 

(Labciencia – Octubre 2008) 

We wish you a lot of success in your analyses and are pleased that our documents 

are able to support you in your work. 


Book corner 

Ronald L. Rich 

Inorganic Reactions in Water 

Springer, December 2007, 17 illustrations, 521 p., hardcover 

ISBN 978-3-540-73961-6 

About the book 

Organized to facilitate reference to the reagents involved, this book describes the reactions 

of the elements and their mostly simpler compounds, primarily inorganic ones 

and primarily in water. It emphasizes the similarities and differences in actual chemical 

behavior, as opposed to electronic structures and theories, although not exclusively. 

Inorganic Reactions in Water again makes available some of the more comprehensive 

coverage of descriptive aqueous chemistry found in older sources, but now corrected 

and interpreted with the added insights of the last seven decades. It also provides new 

information, including reactions of the recently discovered elements, plus some recent 

data on equilibria, often with mostly qualitative kinetic information, to interpret the redox 

and non-redox phenomena that complicate the chemistry of most elements in water. 

From the preface 

Water as a solvent, and the reactions in it, are supremely important in many fields. The 

excitement of newer fields of chemistry, however, has pushed these reactions down 

the list of priorities for providing convenient reference works. This excitement has often 

made «test-tube chemistry» seem to be passé. 

The Japanese word kagaku for chemistry can be interpreted as change-science. 

Space does not permit a comprehensive, but only a representative, description of the 

reactions, changes, of nearly all the elements and their simpler compounds, primarily 

inorganic ones and primarily in water. Carbonyl complexes, for example, are very far 

from comprehensively mentioned here. 

From the contents 

Introduction 

Hydrogen and the Alkali Metals 

Beryllium and the Alkaline-Earth Metals 

The Rare-Earth and Actinoid Elements 

Titanium through Rutherfordium 

Vanadium through Dubnium 

Chromium through Seaborgium 

Manganese through Bohrium 

Iron through Hassium 

Cobalt through Meitnerium 

Nickel through Darmstadtium 

Copper through Roentgenium 

Zinc through Mercury 

Boron through Thallium, the Triels 

Carbon through Lead, the Tetrels 

Nitrogen through Bismuth, the Pentels 

Oxygen through Polonium, the Chalcogens 

Fluorine through Astatine, the Halogens 

Helium through Radon, the Aerogens 

Appendix A: Periodic Charts 

Appendix B: Atomic and Ionic Energy Levels 

Appendix C: Electrode/Reduction Potentials 

Appendix D: Abbreviations and Definitions 

Index 

Keywords 

Inorganic chemistry 

Physical chemistry 

Reaction chemistry 

Water 

Book corner 

Features 

Fundamental for anyone who works with chemistry 

in water 

Up-to-date reference work directed specifically to 

this need – related books have other emphasis 

Target group 

The book is a must-have for scientists at universities 

and industry working in aqueous reaction 

media. 


Metrohm Information Heft 2/2008 31

Literature references 


Only Metrohm can offer you a range of products that cover the whole spectrum of ion analysis: 

• Ion chromatography 

• Titration (potentiometric, thermometric and Karl Fischer titration) 

• Voltammetric trace analysis 

Additionally, Metrohm offers a variety of other products for the modern analytical laboratory: 

• Columns for ion chromatography 

• Comprehensive automation solutions 

• Dosing devices and liquid handling systems 

• pH and ion meters as well as conductometers 

• Sensors for a wide range of different applications 

• Software for instruments, networks and databases 

• Stability measuring instruments 

• Systems for atline process analysis 

Numerous users in the fields of research, industry and education work with Metrohm products every day and value their reliability, 

accuracy and flexibility. The following scientific papers show examples of the areas in which Metrohm instruments can be used 

and provide application know-how. While we are pleased to be able to offer you this literature service, we are not in a position to 

provide you with photocopies of the original references simply for copyright reasons. Normally, you can have copies made of any 

reference that interests you at your nearest university library and usually at a favorable price. 

Metrohm can offer you free-of-charge and comprehensive application know-how in the form of publications, Application Bulletins 

(AB) and Application Notes (AN). With our new application search under products.metrohm.com you will find the solution to your 

application problem both rapidly and conveniently. Our monographs provide you with valuable information on selected topics and 

analysis techniques. Order your copy free of charge under products.metrohm.com (section: Literature). 

Literature references potentiometric titration 

• Equilibrium studies of binary systems involving lanthanide and 

actinide metal ions and some selected aliphatic and aromatic 

monohydroxamic acids 

Mohamed M. Khalil, Mohamed M. El-Deeb and Rehab K. Mahmoud 

Formation of 1:1, 1:2, and 1:3 binary complexes of Th(IV), UO 2(II), 

Ce(III), and La(III) metal ions with acetohydroxamic acid (Aha), 

benzohydroxamic acid (Bha), and salicylhydroxamic acid (Sham) was 

investigated in aqueous medium using the potentiometric technique 

at 25 °C and I = 0.10 mol·dm –3 NaNO 3. The order of stability of the 

complexes was investigated and is discussed in terms of both the nature 

of hydroxamic acid and the metal ion. The concentration distribution 

of various species formed in solution was evaluated. Evaluation 

of the effect of temperature of the medium on the ionization process 

of ligands and the stability of 1:1 binary complexes has been performed 

at I = 0.10 mol·dm –3 NaNO 3, and the corresponding thermodynamic 

parameters have been calculated and are discussed as well. 

Evaluation of the effect of ionic strength of the medium on both the 

dissociation process and the stability of metal complexes for Sham 

binary systems is reported. In addition, the dissociation constants 

of Aha and stability constants of its 1:1 binary complexes were determined 

in various water+dioxane mixtures under the experimental 

conditions (T = 25 °C, I = 0.10 mol·dm –3 NaNO 3). It was concluded 

that solvent effects have a profound influence on the proton-ligand 

and metal-ligand stability constants. Confirmation of the formation of 

binary complexes in solution has been done using conductivity, cyclic 

voltammetry, and UV-visible spectroscopic measurements. 

J. Chem. Eng. Data 52 (2007) 1571–1579 

• Sensitive potentiometric method for determination of micromolar 

level of polyethoxylated nonionic surfactants in effluents 

M. Sak-Bosnar, D. Madunic-Cacic, R. Matesic-Puac and Z. Grabaric 

The Metrohm NIO surfactant electrode has been used as end-point indicator 

for potentiometric titration of low concentration level of polyethoxylated 

nonionic surfactants. This can be achieved by using of a diluted 

titrant concentration, thus reducing the amount of precipitate formed 

during titration and preventing the electrode deterioration. The solutions 

of low levels (down to 10 –6 mol/L) of selected nonionic surfactants containing 

5 to 23 EO groups were successfully titrated with diluted (as low 

as 10 –4 mol/L) sodium tetraphenylborate as standard anionic titrant, increasing 

up to 20 times the sensitivity of the method. The low surfactant 

concentration has been determined in synthetic formulations of widely 

used detergent products and industrial waste waters. The titration endpoint 

has been determined by applying extended Savitzky-Golay leastsquares 

regression. The accuracy and precision has been evaluated by 

using the standard addition method. Relative standard deviation within 

results was between 3.4 and 12.8% depending on the sample complexity 

and the surfactant concentration level. 

Tenside Surfactants Detergents 44 (2007) 11–18 

• Determination of the stability constants for the binding of sulfonated 

morin with Fe 2+ 

Nursen Binbuga, Julia K. Hasty, Steven R. Gwaltney, William P. Henry 

and Tor P. Schultz 

The complexation of the sodium salt of sulfonated morin (H 5SM – ) with 

Fe 2+ was studied by potentiometric titration as was its deprotonation. 


Only four of the five hydroxy groups were deprotonated under the conditions 

employed. The associated pKa values are 3.80, 7.47, 9.24 and 

11.48. Analysis of the titration data suggests formation of (H3SM)Fe – , 

(H2SM)Fe2– , (HSM)Fe3– and (HSM) 2Fe8– . Log ß values (based on HSM5– as the ligand species) are 24.8, 16.1, 7.1 and 11.6, respectively. Theoretical 

calculations predict that the 7-hydroxy group is deprotonated 

first followed closely by the 3-hydroxy position. Deprotonation of the 

2‘-hydroxy group results in proton migration from the 3-hydroxy oxygen 

atom. These calculations along with previous results suggest that chelation 

of the metal ion likely occurs at the 3-hydroxy-4-keto site. 

Graphical abstract: Analysis of potentiometric titration data leads to 

the conclusion that three 1:1 species are formed between sulfonated 

morin and Fe2+ . Only in the high pH region is a complex formed where 

2 sulfonated morin anions are bound to the metal. Theoretical calculations 

support metal binding at the 3-hydroxy-4-keto site. 

Inorganica Chimica Acta 360 (2007) 2339–2344 

Literature references Karl Fischer titration 

• Automated Karl Fischer titration for liquid samples – 

Water determination in edible oils 

Andrea Felgner, Regina Schlink, Peter Kirschenbühler, Birgit Faas and 

Heinz-Dieter Isengard 

In the field of food analysis, rapid measurements and results are generally 

of high importance. Automation of the Karl Fischer titration 

(KFT), a chemical method for determining water content, enables the 

laboratory staff to deal with more samples in less time; automated 

sequences can include different determination methods and sample 

treatments. Moreover, automation can improve reproducibility and 

precision. 

In this work water determination methods were established with an 

automated KFT system using both the volumetric and coulometric 

KF technique. Aspiration and transfer of the sample are freely defined 

in the methods, which consist of different combinations of so-called 

transfer volumes, air bubbles, special liquids and sample volumes. 

Commercially available liquid water standards were used as samples 

for designing basic methods. Furthermore, applications for different 

edible oils were developed. 

Food Chemistry 106 (2008) 1379–1384 

• Moisture profile determination in urea prill. II. Fertiliser caking implications 

García Barneto, Agustin; Ariza Carmona, Jose 

In a previous study, Karl Fischer (KF) titration was used to measure 

the mass of water in concentric layers of urea prill. The obtained data 

demonstrated that the grains of this fertiliser have a linear moisture 

profile. In the present paper, complementary to the previous one, a 

theoretical analysis of the behaviour of a spherical grain sample with 

a linear moisture profile during KF titration is presented. The obtained 

curve of titration fits the experimental data perfectly. The moisture 

content at the grain centre is four times greater than the average moisture 

content, and the layer with the highest water content is located at 

two-thirds of the radius from the centre. Using this theoretical grain 

model and assuming that the intensity of caking is proportional to the 

area and moisture content of the flat contact surface between broken 

or deformed grains, it is possible to explain many observed experimental 

data on fertiliser caking. 

Journal of the Science of Food and Agriculture 87 (2007) 1917–1924 

• Development of insolubility in dehydration of dairy milk powders 

A.J. Baldwin and G.N.T. Truong 

The insolubility of milk powder is affected by the degree of heating in 

the drying process. This phenomenon was studied with milk products 


of different moisture content that were subjected to treatments of defined 

temperature (5–55 °C) and time. Skim milk powder (SMP, protein 

content 36%) was most sensitive over a range of moistures from 15% to 

40%. Milk protein concentrate (MPC) powder (73% protein) was most 

sensitive at higher moisture contents than SMP. At the fastest reaction 

rates, and for both SMP and MPC, the ratio of moisture to protein (calculated 

on a dry basis) was approximately one part moisture to one part 

protein. The rates of development of insolubility in the moist products 

were fitted to the Arrhenius relationship; this allows extrapolation of the 

rate of reaction to conditions in a spray dryer. The factors that affect the 

insolubility reaction are discussed, in particular the effects of the concentrations 

of lactose and minerals. The results explain certain features 

of the current design of milk powder driers and will facilitate overcoming 

problems with the insolubility in high protein powders. 

Food and Bioproducts Processing 85 (2007) 202–208 

Literature references ion chromatography 

• Novel ion chromatography technique for the rapid identification 

and quantification of saturated and unsaturated low molecular 

weight organic acids formed during the Fenton oxidation of organic 

pollutants 

George T. Chi and Katherine D. Huddersman 

The Fenton oxidation process is one of the most widely used technologies 

in the oxidation of organic pollutants. The identification and 

quantification of end products of these oxidation processes is of prime 

importance due to environmental concerns of pollution and toxicity. 

In this work, we have developed a highly sensitive, cheap, easy and 

rapid method of determining low molecular weight mono and dicarboxylic 

acids using ion exclusion chromatography with inverse chemical 

suppression and conductivity detection. Eleven organic acids were 

simultaneously separated in 22 min with detection limits ranging from 

10 to 500 ppb and limits of quantification from 0.05 to 50 ppm. The 

method was tested and proved to be accurate, reproducible, precise 

and highly sensitive. Linearity was in the range of R2 : 0.977…0.999, 

with a percentage error of less than 2% for oxalic and maleic acids, 

and less than 1% for the rest of the organic acids studied. 

Journal of Chromatography A 1139 (2007) 95–103 

• Data quality in water analysis: validation of ion chromatographic 

method for the determination of routine ions in potable water 

Phani Miskaki, Efthimios Lytras, Leonidas Kousouris and Philippos 

Tzoumerkas 

Ion chromatography provides a simple, fast, small sample volume demanding, 

and fit-for-purpose methodology for the concurrent determination 

of 10 ions (F – , Cl – , Br – – 3– 2– + + 2+ , NO3 , PO4 , SO4 , Na , K , Ca and 

Mg2+ ) in surface, ground and potable water samples. 

Current law legislations, as well as the need to constantly provide accurate 

and reliable results, enforce public sector laboratories to practice 

quality management system, according to the EN ISO 17025 standard. 

In this paper, the work that was undertaken for the accreditation 

of the above determinations at the chemical laboratory of EYDAP SA, 

is presented. 

The laboratory has developed two in-house methods, which are carried 

out simultaneously by a dual chromatographic system. The method 

for the analysis of anions is based on the 4110B APHA standard 

method and the one for the cations based on the ISO14911. Deviations 

from the standard procedure made a full method validation imperative, 

therefore, for all 10 ions, method characteristics were determined and 

assessed towards the fitness-for-purpose scope (range of measurement, 

calibration, method detection level, level of quantification, repeatability, 

reproducibility, precision, accuracy, peak resolution). Additionally, 

measurement uncertainty was determined and procedures for 

daily measurement quality control, assessment of individual analyst 

capability, measurement, sample and reagent traceability, and regu- 



lar participation in proficiency testing schemes were implemented. 

Methodology and results for method validation, uncertainty quantification 

and quality control is presented in detail in the full paper. 

Desalination 213 (2007) 182–188 

• Determination of inorganic anions in commercial seed oils and in 

virgin olive oils produced from de-stoned olives and traditional extraction 

methods, using suppressed ion exchange chromatography 

(IEC) 

Giacomo Dugo, Teresa Maria Pellicanò, Lara La Pera, Vincenzo Lo 

Turco, Antonia Tamborrino and Maria Lisa Clodoveo 

Ion exchange chromatography (IEC) with a conductivity detector and 

chemical suppression, was used to evaluate the content of some inorganic 

anions (F – , Cl – – – 3– 2– – , NO2 , NO3 ,PO4 , SO4 , and I ) in commercial 

seed oils and in Sicilian virgin olive oil samples produced both from 

whole and de-stoned olives. Anions separation was achieved with a 

Metrosep Anion Dual 1 column (3.0 × 150 mm; 10.0 μm) packed 

with quaternary ammonium polymethacrylate. The isocratic elution 

was carried out using a solution of carbonate (3.12 mM)/hydrogen 

carbonate (3.25 mM)/2% acetone. Anions were extracted from the oily 

matrix using hot water pH 8 with carbonate/hydrogen carbonate buffer 

in an ultrasound bath. Under these conditions, detection limits ranging 

from 8.4 to 31 μg kg –1 (ppb) were achieved for all the studied anions; 

the precision of the method was within 6.5 rsd%. The analysis of 

vegetable oils provided evidence that the concentrations of bromide, 

nitrite, nitrate and iodide were lower than the detection limits in all the 

studied samples, whereas chlorides were the most abundant inorganic 

anions. Furthermore, the concentration of anions was significantly 

higher in olive oils obtained from the whole fruits than in samples produced 

from de-stoned olives. 

Food Chemistry 102 (2007) 599–605 

Literature references polarography/voltammetry 

• Electrochemical studies and square-wave adsorptive stripping 

voltammetry of Spironolactone drug 

Ahmad H. Al-Ghamdi, Ali F. Al-Ghamdi and Mohammed A. Al-Omar 

A sensitive and reliable stripping voltammetric method was developed to 

determine Spironolactone drug. This method is based on the adsorptive 

accumulation of the drug at a hanging mercury drop electrode and then 

a negative sweep was initiated, which yield a well defined cathodic peak 

at –1000 mV versus Ag/AgCl reference electrode. To achieve high sensitivity, 

various experimental and instrumental variables were investigated 

such as supporting electrolyte, pH, accumulation time and potential, drug 

concentration, scan rate, frequency, pulse amplitude, convection rate and 

working electrode area. The monitored adsorptive current was directly 

proportional to the concentration of Spironolactone and it shows a linear 

response in the range from 1·10 –8 to 2.5·10 –7 mol l –1 (correlation coefficient=0.999) 

and the detection limit (S/N=3) is 1.72·10 –10 mol l –1 at 

an accumulation time of 90 sec. The developed AdSV procedure shows 

a good reproducibility, the relative standard deviation RSD% (n=8) at a 

concentration level of 1.5·10 –7 mol l –1 was 1.4%, whereas the method 

accuracy was indicated via the mean recovery of 97.5%±2.04. Possible 

interferences by several substances usually present in the pharmaceutical 

formulations have been also evaluated. The applicability of this approach 

was illustrated by the determination of Spironolactone in pharmaceutical 

preparation and biological fluids such as serum and urine. 

Analytical Letters 41 (2008) 90–103 

• Palladium biosensor 

Vojtech Adam, Pavel Hanustiak, Sona Krizkova, Miroslava Beklova, Josef 

Zehnalek, Libuse Trnkova, Ales Horna, Bernd Sures and Rene Kizeka 

In this paper we proposed a palladium(II) biosensor. The biosensor 

is based on determining of interactions between palladium(II) and 

metallothionein modified hanging mercury drop electrode by means of 

differential pulse voltammetry. We studied influence of two supporting 

electrolytes (potassium or sodium chloride) on the signals of the 

biosensor. Based on the results obtained we found potassium chloride 

(0.05 M) as the most suitable supporting electrolyte to determine 

palladium(II). The detection limit of the biosensor for palladium ions 

was evaluated as 100 nM with RSD about 10%. Moreover, we utilized 

the biosensor for measurement of the target molecule in the presence 

of human blood serum and human urine. 

Electroanalysis 19 (2007) 1909–1914 

Literature references stability measurements 

• The influence of BHA, BHT and TBHQ on the oxidation stability of 

soybean oil ethyl esters (biodiesel) 

Anderson K. Domingos, Emir B. Saad, Wellington W. D. Vechiatto, 

Helena M. Wilhelm and Luiz P. Ramos 

The effect of synthetic antioxidants such as BHT (butyl-hydroxytoluene), 

BHA (butylhydroxyanisol) and TBHQ (t-butyl-hydroxyquinone) was evaluated 

on the induction time of soybean oil ethyl esters with low oxidation 

stability, employing the Rancimat method (EN14112). Interaction 

effects were also investigated by employing a 23 factorial design, which 

had as minimum and maximum levels the concentrations of zero and 

1500 ppm of each antioxidant. Among the synthetic antioxidants evaluated, 

BHT displayed the highest effectiveness in the concentration range 

from 200 to 7000 ppm. TBHQ displayed a greater stabilizing potential 

when used at higher concentrations (8000 ppm), while BHA was found 

to provide no noticeable increase in the induction time at concentrations 

greater than 2000 ppm. The combined use of these antioxidants, at the 

levels tested in this study, yielded no evidence of any positive synergic 

effect that would justify their use in binary or ternary mixtures. 

Journal of the Brazilian Chemical Society 18 (2007) 416–423 

• Fatty acids, tocopherols, sterols, phenolic profiles and oxidative 

stability of Cucumis melo var. agrestis oil 

Abdalbasit Mariod and Bertrand Matthäus 

Oil extracted from the seeds of Cucumis melo var. agrestis, collected 

from Ghibaish (sandy soil) and Gezira (heavy clay soil) provinces in 

Sudan, was studied in terms of the profile of fatty acids, tocopherols 

and sterols as well as phenolic compounds and oxidative stability by 

Rancimat (Metrohm AG, Herisau, Switzerland). The predominant fatty 

acid was 18:2n-6, representing 61.3 and 61.4% for Ghibaish and Gezira 

samples, respectively. There were no variations among the contents of 

16:0, 18:0, 18:1n-9 and 18:2n-6 between the two samples. �-Tocopherol 

was the predominant tocopherol in both samples, representing 80.7 

and 77.6% of the total tocopherols, respectively, followed by �-tocopherol 

at 18 and 21%, respectively. Total sterol content was 3,879.0 and 

3,785.0 mg/kg for Ghibaish and Gezira samples, respectively. The main 

sterol of the two oils was �-sitosterol. The two samples showed an 

oxidative stability of 5.9 and 5.7 h, respectively. The content of total 

phenolic compounds was determined in each sample according to the 

Folin-Ciocalteau method as 33.0 and 31.9 mg/g of dry product, respectively. 

The phenolic compounds of the oil were separated using a solid 

phase extraction. The fractions were studied by high-performance liquid 

chromatography with diode-array detection, which revealed four peaks 

in the two samples. The major components were catechin, vanillic acid, 

sinapic acid and callistephin. There was little variability according to location 

between the two samples. 

Journal of Food Lipids 15 (2008) 56–67 


Metrohm seminars and trade fairs 

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information on the seminars to be held in your country from your Metrohm agency. 

Ins_Biodiesel_Ranci873_210x143e 

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EN 14112 Fatty acid methyl esters (FAME) – Determination 

of the oxidation stability (accelerated oxidation test) 

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