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The Emergence of Oxidative Combustion Microcoulometry: a Historical Overview

Thousands of analysts work on daily basis with combustion analyzers, in laboratories all around the world. One of the elements which can be measured by elemental combustion analyzers are Halogens, due to microcoulometric detection technique. This may

Thousands of analysts work on daily basis with combustion analyzers, in laboratories all around the world. One of the elements which can be measured by elemental combustion analyzers are Halogens, due to microcoulometric detection technique. This may be Total Halogens, Adsorbable Organic Halogens or Extractable Organic Halogens. Analysis of Halogens by this technique has its roots closely related to TE Instruments. How the technique has developed over the years will be explained in this article. A historical overview:

The Cause: 1970-1975

In the Mid-seventies Mr. J. van Woerden owned a small glass manufacturing company called Euroglas. This company produced and repaired glass parts for their customers such as laboratories. Around the same time, Dutch inspection institute KIWA (Keurings Instituut voor Waterleiding Artikelen) operated as a notifying body and certifying company for drinking water products like water pipes, fittings and taps. The KIWA institute was a customers of Euroglas’ glass products.

During that period of time poor quality of surface water became a serious issue in many places throughout the world, including the Netherlands. One of the designated harmful compounds were organic Halogens. As a result of pollution the amount of fish decreased in major rivers. European governments responded and took action. A black list of toxic substances was issued by European commissions, including organic halogens, and a solution to monitor the impact of taken measures was highly necessary. The video below shows a Dutch newsreel from 1974. The KIWA institute performed tests using trout to identify toxins in surface water of major European river the Rhine. Once a harmful substance is present within the water of the inner Rhine river, trouts in the aquarium stop swimming against the current and flee.

The Solution: 1976

In the early 1970s Dr. Kuhn and Dr. Sontheimer of the German research institute EBI (Engler-Bunter-Institute) developed the Adsorbable Organic Halogens method. The above mentioned Dutch KIWA institute was closely involved. Eventually the AOX parameter was officially introduced in 1976 and composed out of the following, now well-known steps:

1. Adsorption on activated carbon

2. Rinsing off the inorganic chlorides

3. Pyrolysis of the organic Halogens

4. Microcoulometric detection technique

The method was standardized in the DIN 38409 Part 14 and incorporated in official German legislation. In the following years other countries also incorporated this new method in official legislation.

The emergence of EOX: 1980

In 1980 an environmental pollution scandal was discovered in Lekkerkerk, the Netherlands. A complete newly build neighborhood called ‘Lekkerkerk West’ with 300 houses, was built on highly contaminated soil. The contamination was revealed after a water pipe broke which had been affected by aggressive chemicals like benzene. It was the first major soil pollution affair in the Netherlands.

This major affair resulted in the Dutch NEN 6402 method to determine Extractable Organic Halogens known as EOX and was incorporated in Dutch legislation in 1980. The main difference between the two methods lies in the sample preparation. For EOX one extracts the organic compound with a solvent, for AOX one adsorbs the organic compounds on activated coal (AOX). Water samples deriving from soil may contain a significant amount of particles. A water sample deriving from soil contains lots of particles. Using a solvent to extract the organic Halogens instead of adsorbing them is therefore much easier.

Commercializing the analyzer: early 1980’s

To monitor the effects of governmental measures against water pollution, an analyzer based upon microcoulometric detection technique was needed. The KIWA and EBI institute were not interested in commercializing this new to be built analyzer. Thereafter Euroglas was approached by the KIWA institute questioning if they were interested in producing such an analyzer. Major parts like the coulometric cell and combustion tube were made out of quartz glass which is able to withstand extreme temperatures. Euroglas agreed and eventually the Euroglas Coulometric System was born: the ECS 1000. The complete system is operated manually. Results need to be calculated by the operator based upon Faraday's laws of electrolysis.

Euroglas expanding: 1980 – 1990

Mr. Günter Arnold experienced the development of AOX analysis by microcoulometric technique at close hand. He worked for a company which delivered laboratory supplies to the EBI institute during development of the AOX method. To sell the newly developed ECS 1000, Euroglas needed to expand on every department. René van der Zalm was one of the first employees to join Euroglas. He became an electronical engineer and is currently Technical Director of TE Instruments. René has been working for more than thirty years with combustion analyzers and can be seen as a true expert. Günter Arnold became the sales representative for the territory of Germany. Nowadays, Günter Arnold still distributes combustion analyzers for TE Instruments. Last year he received an award for this remarkable achievement.

Within a short time Euroglas made a tremendous growth thanks to the sales of ECS 1000 units. Euroglas continued to expand and during the late eighties, Huib Brouwer was appointed as Sales Representative and Rien Sprinkhuizen as Service Engineer. Both men are still actively involved in the same market, now on behalf of TE Instruments. Huib Brouwer as Regional Sales Manager and Rien Sprinkhuizen as General Manager. Looking back on that period:

Rien Sprinkhuizen – General Manager TE Instruments:

“One of the key success factors of the ECS 1000 was removing 'difficult' out of the equation of coulometry. By simplifying the electrolyte recipe and removing the salt bridge from a titration cell, coulometrics became fast, easy and accessible for every operator.”

Huib Brouwer – Regional Sales Manager TE Instruments:

“Throughout my career as a Regional Sales Manager I have sold all three generations elemental combustion analyzers, from the ECS 1000 up to the XPLORER. Before I started working at Euroglas I operated an ECS 1000 myself in a water testing laboratory.”

Voltaweg: 1990’s

The growth continued to pursue and Euroglas was forced to relocate. The company moved to the Voltaweg in Delft, the Netherlands. The product range expanded with the ECS 2000 and the ELS 2000 auto sampler. The ECS 2000 was the successor of the ECS 1000 and showed first signs of digitization with a built-in computer.

Euroglas was eventually acquired by the American multinational Thermo Fisher. Name of the company changed into Thermo Euroglas. Due to the acquisition it became possible to develop combustion analyzers for Total Sulfur by UV-Fluorescence and Total Nitrogen by Chemiluminescence, complementary to the coulometric systems. This marked the beginning of an extensive range of products designed, manufactured and tested at the factory in Delft. All necessary facilities were present at this location: a glass manufacturing area, laboratory, R&D, warehouse, and so on. All the analyzers that have been produced during this period in chronological order:

• ECS 1000

• ECS 2000

• ECS 1600

• ECS 1700

• ECS 1200

• ECS 3000

• TN/TS 3000

• TOC 1200

• HiPerTOC

• DeXtar

• XVI+

• SphiNCX

Birth of the XPLORER: 2010

In 2008, Thermo Fisher decided to close the production site in Delft and move to Cambridge. Former R&D employees, including René van der Zalm and Rien Sprinkhuizen, started a new independent company in 2009: Trace Elemental Instruments. Years of experience, gathered in the previous decades, were put into the development of a complete new combustion analyzer: the XPLORER. This advanced combustion analyzer was introduced in 2010 and developed at the exact same production site to which Euroglas moved 20 years ago.

Designing and manufacturing elemental combustion analyzers is our expertise and became part of life. TE Instruments is more than happy to share this knowledge and support you with everything you need to know about combustion analyzers.

Rene

Details

  • Voltaweg 22, 2627 BC Delft, Netherlands
  • TE Instruments

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