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iCspec Report Summary

Project ID: 636930
Funded under: H2020-EU.

Periodic Reporting for period 1 - iCspec (in-line Cascade laser spectrometer for process control)

Reporting period: 2015-04-01 to 2016-09-30

Summary of the context and overall objectives of the project

The measurement and control of the composition of material flows in real time is one of the major missions of Process Analytical Technologies (PAT) throughout the chemical industry. In order to pursue and extend this mission the iCspec project develops new cutting-edge analyzers capable of introducing yet unreachable real time measurements of process streams to the (petro-) chemical industry. These analyzers allow production plants to be controlled more closely, to set their product quality more accurately, and to increase their output. At the same time, costs and the environmental impact of waste materials disposed will be reduced.
Analysis of material flows in production processes is a time-consuming activity involving taking samples and measuring them in the laboratory. Online measurements usually use a gas chromatograph, with results taking several minutes. In contrast, the developed analyzers enable measurements to be taken directly in the gas flow or in a bypass line in real time. This method also incurs lower operating expenses than a gas chromatograph, which requires regular calibration and thus strengthens the competitiveness of the European industry, while significantly reducing costs and waste. To make this become reality, the iCspec consortium cooperates to develop a laser spectrometer that analyzes gas mixtures. Siemens coordinates the consortium consisting of eight European partners and the initial objective is to build a demonstrator capable of analyzing hydrocarbon gas mixtures, which will then be tested at Preem, Sweden’s largest refinery.

Laser spectrometry exploits the fact that every light molecule absorbs particularly specific wavelengths. Although laser spectrometers that register individual molecules already exist, no solution is yet available that is capable of recording many industrial gases simultaneously. Achieving this will need a laser source that will ideally cover the required infrared fingerprint range. The new spectrometer uses a few modules with semiconductor laser arrays that can be controlled to enable examination of both absorption lines with single sharp molecular absorption lines and broad absorption bands. Employing laser arrays, the new method is much more robust and thus also suitable for rough operating conditions. Development of the laser source is in the hands of the Commissariat à l’énergie atomique et aux énergies alternatives (CEA) and mirSense a spin-off of III-V Lab and CEA-LETI, based in France; the Politechnika Wrocławska in Poland; and the University of Wurzburg and nanoplus Nanosystems and Technologies GmbH in Germany. Corporate Technology, Siemens’ global research unit, is working with Poland’s Airoptic to develop the spectrometer and establish procedures to evaluate the measurement data.

The planned demonstrator will have to measure the five hydrocarbons methane, ethane, propane, butane and pentane during distillation of gas components at the refinery. But this is not the only application for this new technology: It will also enable emissions from power stations or patient exhaled gases to be measured using only one instead of a range of measurement devices. Likewise, when it comes to analyzing fluids, solid matter or biological tissue laser sources are far superior to the incandescent emitters currently used in spectrometers. Their higher intensity means that lasers penetrate much deeper into the materials being measured and thus generate more information. In the longer term, this new technology will revolutionize measurement technology not just in the process industry but also in medical diagnostics.

Work performed from the beginning of the project to the end of the period covered by the report and main results achieved so far

Interband Cascade Lasers (ICLs) in the 3 – 5 µm spectral range:
For the ICL based sources, two approaches were investigated in the reporting period within the iCspec project: Specialized ICL comb sources for heterodyne spectroscopy and ICL DFB array sources. Before the iCspec project neither of the two device concepts had been demonstrated in the field of ICL technology and the achieved results within the project define the current state of the art for these novel ICL based devices for broad wavelength coverage. For both ICL based device concepts results in the target wavelength range of interest for hydrocarbon sensing have been successfully obtained within the reporting period. A corresponding device design was defined in accordance with deliverable D1.4.

Quantum Cascade Lasers (QCLs) in the 6 – 12 µm spectral range:
For the Quantum Cascade Lasers array in the 6 – 12µm spectral range developed by mirSense, there are two main objectives. The first objective is to realize an array of single mode emitters of Quantum Cascade Laser emitting in continuous wave at room temperature at 6.8 µm with a tunability of 188 nm. In wavenumbers, this corresponds to a central emission of 1460 cm-1 and a tunability of 40 cm-1. The main challenge of this device is to obtain a stimulated emission in the appropriate wavelength range and to manage the thermal load generated during the continuous wave emission improving the thermal dissipation. The gain medium is designed using quantum engineering. The thermal dissipation is improved performing buried configuration with an Iron doped Indium Phosphide regrowth.
The second objective is to realize an array of single mode emitters of Quantum Cascade Laser emitting around 8.7 µm with a broad tunability of 1524 nm. Considering the broad tunability, a pulsed regime is targeted at room temperature for this device. Using Quantum engineering, a multi-stack approach is used to obtain a broad tunability. In the multi-stack, different active regions emitting at different wavelength are grown on a single wafer to keep the monolithic approach mandatory for the realization of compact source.
For both devices, the main constraint is to be compatible with the optical combiners designed by the CEA LETI. The precision required for assembly of the array of QCL and the optical combiner is 0.2% on the emitted wavelength of the single mode QCL. This level of precision required a stable process and a high level of precision on the effective refractive index of the lasers.
Compiling the specifications for the analyzer performance with respect to the requirements from the distillation process:
Based on the target application requirement specifications for the laser-based Hydrocarbon analyzer have been defined. They form the baseline for subsequent development within iCspec and cover all relevant requirements and aspects; in particular for (1) the PAT application itself, (2) the ambient conditions, (3) the measurement characteristics, (4) the mechanical characteristics, (5) the electrical characteristics, (6), the local user Interface (LUI), (7) the communication interfaces, (8) legal regulations, and (9) the maintenance.

Development of a laboratory test environments for MIR laser spectroscopy:
Both laboratory test environments for ICL-Array and QCL-Array sources are operational and allow: (1) precisely defining hydrocarbon test gas mixtures, (2) the thorough characterization of laser array sources, (3) data acquisition with a commercially available EC-QCL source and custom combined ICL-DFB-laser sources, respectively, and (4) data evaluation according to the different evaluation concepts of ICL- and QCL-Array sources.

Develop the data analysis for laser-based spectroscopy on partly overlapping complex spectra:
Algorithms evaluating the complex overlapping HC spectra have been developed and are under constant improvement for QCL- as well as for ICL-sources. Based on these algorithms the optimum spectral range for QCL-Array operation has been chosen. The main strategy covers modelling of direct absorption spectra and WMS spectra, as well as a multi-fit analysis based on an extension of a lookup fit approach, which is in particular advantageous for the overlapping spectral within the 3-5µm spectral range.

Demonstrator C1-C5 gas analyzer based on ICL-spectrometer:
There has been a significant progress regarding development of the ICL-array based C1-C5 spectrometer demonstrator in preparations for the field test. The first unit consisting of a central unit (CU), transmitter and receiver has been realized. It integrates dedicated PCB electronics, opto-mechanics, firmware and software and IP66-classed enclosure. The system in addition incorporates 8-channel multiplexer and well as optical combiner designed for ICL arrays integrated in a special device package.
Apart from that a SO2/SO3 array has been integrated in an industrial GasEye cross duct sensor enclosure and the system is soon ready for a field test.

Demonstrator C1-C5 gas analyzer based on QCL- spectrometer:
Beginning with the requirements specifications, which defined in particular the suited spectral ranges for the QCL-Array sources, the main focus was on the development of specialized electronics for analyzer control, capable of appropriately driving the laser arrays, performing the data acquisition and evaluation. An assessment of first QCL-Array sources with the WMS technique showed the general feasibility.

Progress beyond the state of the art and expected potential impact (including the socio-economic impact and the wider societal implications of the project so far)

Currently the composition of gas mixtures is identified by extractive gas chromatographs with known disadvantages. Extractive analyzers employing fast inline methods would significantly decrease the maintenance costs and reduce waste and pollution. As laser based analyzers provide very short response times, excellent accuracies, afford minimum maintenance, and are resistant to contaminations of the gas stream, they become the most favorable choice for online gas analyzers, whenever they are applicable. However, today only few companies offer laser based solutions due to current technical restrictions. These analyzers are only capable of resolving a very limited amount of different components, restricting them to distinct applications and markets. As the projected analyzers target multi-component analysis for the Hydrocarbon industry they are able to replace gas chromatographs and thus complete and safeguard the future of Siemens’ and Airoptics’ product portfolio.

Moreover, the highest impact will have the short response time of the analysis, which will speed up the process control loop, optimize the product quality and minimize waste. The real-time measurement of the gas components will make it possible to run the process closer to its optimum and reduce the margins for safe operation. The laser analyzer will significantly reduce maintenance costs. Moreover, no carrier gas (H2 or Helium) is required anymore and no expensive calibration gas is needed. The analyzer offers easier and faster maintenance since it might be easily replaced in case of failure, which improves the availability of the process. It will also lead to decreased installation costs since it will be placed close to the sample take off point. This will lead to less hardware requirements, reduced requirements on the sample conditioning system and reduced or no need for sample lines. The measurement will also be more robust against contaminants and process upsets resulting in an improved availability of the measurement. From an environmental standpoint it is a large advantage to reduce or eliminate the need to vent any sample to the atmosphere or the flare. Since a refinery can have a large number of analyzers the reduced power consumption can lead to substantial power savings. More precisely, 2/3 of the analyzers’ CO2-footbprint can be saved when replacing conventional gas chromatographs with the projected ones. Furthermore, the underlying key enabling technology will be transferable with moderate modifications to other important industrial and environmental applications, like combustion control, exhaust gas and environmental monitoring, where e.g. NO, NO2, SO2, SO3, CO, CO2, H2O, H2S and HCs will become simultaneously measurable. Considerable scaling effects in terms of efficiency increase, costs reduction and environmental protection thorough many different industrial applications can be already foreseen.

The outstanding capabilities of these new analyzers are based on three main developments of the iCpsec project: (1) the development of yet unavailable widely tunable laser sources, (2) the integration of these sources into industry grade analyzer systems and (3) the development of novel data evaluation algorithms. Both, Siemens and Airoptic pursue analyzer and software development for the 6 –12 µm and the 3 – 5 µm spectral range, respectively. The setup of a designated test environment for hydrocarbon measurements has been completed, integrated electronics driving the analyzers have been developed and first laser samples have been investigated so far.
The main advantages of the projected laser analyzers stem from the outstanding capabilities of the developed laser sources offering significantly increased spectral coverage of the infrared fingerprint region. The iCspec consortium aligns a powerful team of laser manufacturers, world-renowned high-tech institutes and universities focusing their profound know-how to the development of these novel laser sources: (1) Integrated quantum cascade laser (QCL) arrays are developed by mirSense a spin-off of CEA-Leti and III-V labs. These sources cover the mid-infrared spectral range from 6 – 12 µm by combining in a unique output the emitted light of several actives regions, each covering different parts of the spectrum. (2) Interband cascade laser (ICL) DFB arrays are developed by nanoplus, the University of Würzburg and Politechnika Wroclawska. These sources cover the complementary mid-infrared spectral range from 3 – 5 µm. (3) The output of each array element is combined by a microstructured multiplexer for the QCL and the ICL approach respectively. The multiplexer and designated application specific integrated circuits allowing the fast switching of each laser module are provided by CEA-Leti. (4) An alternative approach performing the spectroscopy of hydrocarbons is the employment of frequency combs. Novel devices for this heterodyne spectroscopy technique are investigated by nanoplus, the University of Würzburg and Politechnika Wroclawska.
In conclusion, the insights in the operability and the experience gained during the test phase of the projected analyzers allow the development of advanced process control strategies. As end-user Preem intends to exploit the benefits of the new technology with respect to cost and energy savings, increased operational safety, increased reliability and environmental protection acting as an industrial pioneer, once the new analyzers will become commercially available. Furthermore, Preem is an important player in the conversion to renewable fuels. The employment of the projected analyzers promotes the vision to lead the transition towards a sustainable society. Preem has a great interest to reduce greenhouse gas emissions and to and contribute to a sustainable society.

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