6. Emission results of amine plant operations from MEA testing at the CO₂ Technology Centre Mongstad (2014)

Anne K. Morken^a,b, Bjarne Nenseter^b, Steinar Pedersen^b, Milan Chhaganlal^a,b, Jane K. Feste^a,b, Rita Bøe Tyborgnes^a,b, Øyvind Ullestad^a,b, Helge Ulvatn^a,b, Liang Zhu^c, Tomas Mikoviny^c, Armin Wisthaler^c, Toine Cents^a,d, Otto M. Bade^e, Jacob Knudsen^e, Gelein de Koeijer^b, Olav Falk-Pedersen^a,f, Espen S. Hamborg^a,b,*

^aCO₂ Technology Centre Mongstad (TCM DA), 5954 Mongstad, Norway ^bStatoil ASA, P.O. Box 8500, 4035 Stavanger, Norway ^cUniversity of Oslo, Department of Chemistry, P.O. Box 1033 Blindern, 0315 Oslo, Norway ^dSasol Technology, PO Box 5486, Johannesburg 2000, South Africa ^eAker Solutions, P. O. Box 222, 1326 Lysaker, Norway ^fGassnova SF, Dokkvegen 10, 3920 Porsgrunn, Norway *Corresponding author

Abstract

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Extensive atmospheric emission monitoring has been conducted at the CO₂ Technology Centre Mongstad (TCM DA) during amine based post-combustion CO₂ capture. The TCM DA amine plant was operated with an aqueous monoethanolamine (MEA) solvent system, treating flue gas from a combined heat and power (CHP) plant. Emission monitoring was conducted by a Fourier Transform Infrared (FTIR) Spectroscopy analyzer, a Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-TOF- MS) analyzer, and manual isokinetic sampling followed by off-line analysis in the laboratory.

Atmospheric emissions of MEA were very low throughout the entire campaign, ranging from a few to a few hundred parts per billion (ppb, 1 ppb = 10^-9 v/v). Atmospheric emissions of MEA amine based degradation products such as nitrosamines and nitramines were below detectable levels. Atmospheric emissions of ammonia (NH₃) were in the low ppm range. Methylamine was emitted at low ppb range.

Absorber wash water sections were found to effectively reduce atmospheric emissions from amine based solvent system.

1. Introduction

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The CO₂ Technology Centre Mongstad (TCM DA) has in collaboration with partners undertaken several months test using the non-proprietary aqueous monoethanolamine (2-aminoethanol, MEA) solvent system at 30 wt% and 40 wt% in an attempt to characterize the performance and atmospheric emissions from such operations [1,2,3]. The operations were carried out at a considerably large scale of about 50.000 Sm³/h of flue gas supply flow rates from a combined heat and power (CHP) plant, as described elsewhere [1,2,3]. In the CHP plant, the natural gas is    combusted in a gas turbine and the flue gas content and characteristics are similar to those of a combined cycle gas turbine (CCGT) power plant. TCM DA has made significant investment in equipment and instrumentation for monitoring of stack emissions. Continuous efforts are being done to improve sampling methods, sampling lines and the instrumental analysis.

Quantitative emission data from a representative CO₂ capture plant is one remaining knowledge gap in the assessment of health and environmental risks posed by the amine-based post combustion capture (PCC) technology  [4]. A health risk analysis for the emissions to air from the amine plant TCM DA was recently published [5]. The emission permit granted to TCM DA by the  Norwegian Environmental  Agency (Miljødirektoratet)  in November 2011 regulates the emission levels for solvent amines, alkylamines, aldehydes and ammonia [6]. It also sets requirements for online monitoring and how to calculate the nitrosamine and nitramine environmental concentrations by a dispersion calculation method. The air and drinking water concentrations of 0.3 ng/m³ and 4 ng/L respectively were associated with negligible excess risk level for cancer (10^-6) after lifelong exposure to nitrosodimethylamine (NDMA). Since all amines that are emitted to air from the absorber stack may undergo photo-oxidation in the atmosphere and be converted to nitramines or nitrosamines they will contribute to the environmental concentrations    as calculated by the dispersion simulation method. In the granted permit the total sum of nitrosamines and nitramines must be below the given limits. Therefore both amine emissions and direct emissions of nitrosamines and nitramines will contribute to the total environmental budget of the harmful compounds.

Although sampling and analysis of flue gases in general are well known, the wet flue gas containing solvent amine, amine degradation products and other trace components give many sampling and analytical challenges. Very limited standard methods are established for such a task. Several studies were undertaken by international experts for the, now terminated, Carbon Capture Plant Mongstad (CCM) project, and much of the work is available for the    public [7]. The CCM project developed a toolbox for qualifying amine based solvent technologies, consisting of the steps liquid sampling, isokinetic gas sampling, sample preservation and sample logistics, sample work-up and analytical procedures, atmospheric chemistry including dry and wet deposition, dispersion modelling including local Mongstad weather conditions, toxicology assessment of major degradation products as nitramines and nitrosamines, solvent degradation rig and test protocol for solvent stress testing as well as process emission reducing technologies. The analytical measurement chain was essential in the toolbox and it is also the basis for the current work.

This work is part of a continuous effort of gaining better understanding of the performance potential of the non- proprietary aqueous MEA solvent system, conducted by TCM DA and its affiliates and owners, in order to test, verify, and demonstrate CO₂ capture technologies [1, 2, 3]. The purpose of the current work is to provide results which quantify the amounts and the compositions of atmospheric emissions sampled and analyzed during amine plant operations treating CHP flue gases. A thorough overview and discussion of available equipment and instrumentation for monitoring of stack emissions will be given. The results are believed to provide realistic emission figures for emission monitoring and control for any future large scale carbon capture and storage (CCS) project due to the considerable size of the TCM DA amine plant.

2. Instrument and analysis

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A description of the TCM DA amine plant is given elsewhere [1,2,3].

2.1 Overall system description and instrument position

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Removing CO₂ from flue gas by using post-combustion amine based CO₂ capture reduces the emission of greenhouse gases to the atmosphere, but inevitably causes some emissions of amines and amine related degradation products to the atmosphere. Thus, qualitative and quantitative analysis of the emitted components is very important, but this task is far from trivial. For practical purposes, analytical instruments are preferably placed at ground level,   but in that case a long sampling line (often >50 m) is required to direct the treated flue gas from the top of the  absorber into the apparatus at ground level. This sample line has to be heated to well above the dew point of the gas   to avoid condensation and possibly unwanted adsorption and/or reaction of emitted components.

TCM DA applies different measurement techniques to monitor and quantify the amounts and concentrations of emitted compounds. Some of the analyzer techniques currently applied on a permanent basis are;

• Fourier Transform Infrared (FTIR) Spectroscopy
• Proton Transfer Reaction Time of Flight Mass Spectrometry (PTR-TOF-MS)
• Manual isokinetic sampling technique  with impingers and subsequent off-line laboratory analysis (carried  out by TCM DA, Statoil CP Laboratory, SINTEF and Ramboll)

Online gas phase concentration measurements are also performed at ground level (via a sample line) using a  Fourier Transform Infra-Red (FTIR) Spectroscopy instrument and a Proton Transfer Reaction – Time of Flight –   Mass Spectrometry (PTR-TOF-MS) device. This online equipment is placed in an analyzer house at ground level. At the absorber top, isokinetic sampling is performed on a regular basis. There is an analyzer house and a shelter on the top of the amine absorber where all the equipment is located, as seen in Figure 1.

Extracted gas is sampled from the stack through an impinger train containing absorption liquids. By onsite measurement of the gas flow and laboratory analysis of the impinger liquids, the gas phase concentration of different components can be determined. The measurement system is shown schematically in Figure 2 and the techniques are further explained in the sections below.

2.2 Sampling lines

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The sampling line bundle installed at TCM DA is 101 meters long. It consists of 3 separate lines made from the following materials, respectively:

• PFA Teflon^®
• Electro-polished stainless steel
• Sulfinert^®-treated passivated stainless steel

All lines can be heated to 140 °C. Sample transfer via a heated sampling line has several benefits over placing the equipment at the top of the absorber:

• Easy access to the analyzer for maintenance and calibration and to utilities such as power, gas supplies, etc.
• Increased physical space for the analyzer
• Safer operations

Some negative aspects are however:

• Delayed analyzer response
• Potential degradation reactions and adsorption effects in the sampling line

Potential sample line effects are rarely reported in open literature. It is generally accepted is that the sample path should be kept as short as possible, and that the line temperature should be well above the dew point. However, increasing the temperature too much may lead to unwanted decomposition, to potential formation of nitrosamines, and to other sampling artefacts. Switch between different sample lines should be avoided due to memory effects.

The effects of different sample lines were investigated by Cents et al [8].

• FTIR analyzer

The FTIR model Anafin 2000 is employed at TCM DA to measure standard gas phase components (CO₂, water, NO_x, SO_x) as well as amines, aldehydes and ammonia. The analyzer operates at wave numbers between 500 and 7000 cm^-1, with a resolution of 2 cm^-1. The path length is 7 meters. The detection limit for amines, aldehydes and ammonia is on the order of 1 ppmv. According to the discharge permit from the Norwegian Environmental Agency (Miljødirektoratet), TCM DA is allowed to emit 6 ppmv of total amines as a daily average [6]. For this purpose, the detection limit of the FTIR instrument is satisfactory.

The FTIR is connected via heated sampling lines to sampling probes at the absorber inlet (downstream DCC), absorber outlet and desorber overhead condenser outlet. An automatic stream selector makes it possible to program the plant’s control system to alternate between the different measuring locations as desired. The FTIR is calibrated for a list of standard flue gas pollutants, including CO₂, SO₂, NH₃, etc., as well as solvent amines and some volatile degradation products e.g. aldehydes. The instrument is not set up for measuring alkyl amines, nitrosamines and nitramines.

The FTIR technique has the advantage that the sample is measured without any preconditioning, hence reducing the risk for analytical artefacts. To avoid water condensation, the FTIR gas cell is heated to 85°C and the sampling lines are heated to 120°C. Target compounds contained in mist or droplets are likely to be evaporated at these temperatures. The FTIR monitor thus measures the total content of analytes in the flue gas. A draw-back of the   FTIR technique is the interference from water vapor which results in a relatively high detection limit. The  experience is that NH₃ and amines can be detected down to 1 ppm levels. This is also in accordance with earlier measurements of gaseous emissions in post combustion carbon capture [9, 10].

2.3 PTR-TOF-MS analyzer

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The PTR-TOF-MS (model PTR-TOF 8000) used is manufactured by Ionicon Analytik (Innsbruck, Austria). The PTR technique has been widely used for environmental volatile compound measurements for over a decade. Its measurement principle is based on soft ionization, via proton transfer, followed by high mass resolution mass spectrometric analysis. At TCM DA, the PTR-TOF-MS instrument subsamples from the main sample line through a heated (100-130°C) Siltek inlet line. The sample flow is diluted by a factor of 10 to 20 with bottled synthetic (zero)  air, to avoid ion signal titration caused by high ammonia levels. The PTR-TOF-MS is able to measure amines, ammonia, aldehydes, ketones, carboxylic acids, nitramines and nitrosamines which are all important target   compounds in amine based CO₂ capture. The analytical setup at Mongstad is described in recent publications by Zhu  et al. [11, 12].

2.4 Manual gas emission sampling

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The analytical value chain applied for manual gas emission sampling and analysis is  schematically shown in  Figure 3. This value chain governs the measurement and is described in details below.

Sampling. The TCM DA stack is designed to achieve flow conditions suitable for isokinetic flue gas sampling as specified in the standard EN 15259:2007. The stack is insulated to minimize condensation. Sampling nozzles are located at a level 2 meters below the stack exit. A sampling system from Paul Goethe GmbH in Germany is used for allocation of a gas emission sample. The equipment is operated from an associated control unit (iTES). The special sampling equipment configuration is assembled  for amine emissions based on experiences from the  CCM project  [7]. Isokinetic gas sampling principles are used to secure representative sampling from a ducted gas stream where two-phase conditions (particles or droplets with diameter > 1 μm) are present or may occur. From an amine absorber the presence of droplets in the flue gas has to be considered, hence isokinetic gas sampling is an assurance for representative samples.

Capture of analyte. The double tube sampling probe was cooled with pressurized air in order to start   condensation of the extracted gas sample stream. Typical amine emission analytes are captured by two principles, condensation and liquid absorption. It is experienced that the main sampling step is condensation. The condensate flask is kept cool in an ice bath and has a size and design to maximize the condensation capacity. In this way the gas  is dried and further downstream split to subsequent impinger trains or solid adsorbents. It is further experienced that only for the most volatile components like NH₃, small alkyl amines and aldehydes the second trap based on stepwise liquid absorption or solid phase adsorption is significant. In case of mist formation in the absorber, submicron  aerosols will enter the sampling train. It is known that aerosols potentially can have limited retention through liquid sampling systems. In order to improve the capture of aerosols, a high capacity condensation step is followed by jet- impinger flasks to force agglomeration. However mist is normally not associated with the CHP flue gas.

The condensates were preserved with sulfamic acid at site directly after sampling to avoid potential nitrosation of secondary amines [7]. Ammonia and the different amines were absorbed in 0.05 M sulphuric acid, the aldehydes and ketones were adsorbed on DNPH cartridges (Sep-Pak DNPH-Silica  Long Body Cartridges,  Waters).  For nitrosamines and nitramines 10 g/L sulfamic acid solutions were used as second sampling step.

Sample work-up. Samples were brought to TCM laboratory and immediately cooled or frozen for storage until analysis. As a principle the condensate sample was prepared for analysis first and subsequent absorbent solutions  were prepared and analyzed secondly, with various experimental techniques (Table 1). This often includes extensive laboratory work.

Analysis. Expected degradation and emission products from a MEA based solvent system, were assessed from a recent study using the solvent degradation rig for stress testing of MEA [13]. The target analytes for the current    work is given in Table 1. These compounds cover the requirements set forth by the Miljødirektoratet in the emission permit.

Amines, nitrosamines, and aldehydes were analyzed using an LC MS-MS QQQ (Agilent). The condensate from the first impinger was analyzed directly on the LC MS, the acidic impinger solutions were diluted before analysis.

Ammonia was analyzed on an ion chromatograph (IC).

2.6 Additional analyzer techniques: Voice200 and PTR-QMS

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TCM DA also tested a Voice200 analyzer from SYFT Technologies and a PTR-QMS 300 analyzer from Ionicon.

These instruments operate on the same measurement principle as the PTR-TOF-MS but include cheaper and less specific quadrupole mass analyzers. Results from both analyzers compared well with the PTR-TOF-MS data. The results are not presented in this paper.

3. Results and Discussions

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3.1 Analysis of Solvent samples

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Solvent degradation processes were monitored during the course of the entire MEA campaign. The solvent amine, ammonia, and some degradation products were analyzed by TCM DA and Statoil CP laboratories. Alkyl amines, aldehydes, ketone, generic nitrosamines, solvent specific nitrosamines and nitramines were analyzed by Ramboll and SINTEF laboratories.

The concentration of the solvent amine was observed to remain stable over the extended period of the campaign

indicating reasonable degradation rates of the solvent amine. The main degradation products of MEA were found to be amides, amino acids and other amines. Heat stable salts were also measured through the entire campaign, anions (OA, GA, FA, NO₃^–) by IC and total heat stable salts (HSS) by ion exchange and titration. Figure 4 displays the evolution of various degradation products and heat stable salts in the solvent. The components and amounts found were expected from an aqueous based MEA solvent system [9].

Two solvent specific nitrosamines, N-nitrosodiethanolamine (NDELA) and N-nitroso-2-hydroxyethyl-glycine (Nitroso-HeGly), were detected in the solvent as the degradation process progressed (Figure 5). The total concentrations of nitrosamines (TONO) were measured to be 797 μmol/L.

Since MEA is a primary amine it is not expected to form a stable nitrosamine. The identified compounds are thus formed from secondary amines occurring as impurities in the solvent or being formed during the degradation reactions. As is shown in Figure 5, there are still some unidentified nitrosamines in the used solvent sample. These nitrosamines are formed from high molecular weight amines and have low volatility. Only in the first water wash stage low quantities of nitrosamines were found (see below).

The solvent specific nitramine (MEA-NO₂) was detected at a concentration of approximately 2 mg/L (Table 3).

3.2 Analysis of wash water samples

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MEA was periodically measured in the wash water from both water wash sections. The wash water sections are specifically designed to physically absorb gaseous and entrained aqueous MEA before the depleted flue gas is   emitted to atmosphere. Figure 6 shows that the liquid phase concentration in the first wash water section (Lower    wash water – right y-axis) was about 100 times higher than the upper section (Upper Water Wash – left y-axis). The results from 16/12-2013 show higher results, the temperature in the  flue gas was 47°C and this will give higher    MEA concentrations. Going from 30 to 40 wt% MEA in the solvent, will  also give higher MEA concentrations in    the water wash sections and this is measured at 19/2-2014, where the solvent MEA concentration was 40 wt%.

Methylamine and minor amounts of ethylamine were also found in water wash samples, as presented in Table 3.

Figure 6 clearly demonstrates the effectiveness of two water wash sections.

The concentration of alkylamines, nitrosamines and nitramines in wash water samples are given in Tables 2 and 3. TONO were above detection limit only in the first water wash section, in one of two samples. This clearly   indicates that nitrosamine volatility is low and that nitrosamines escaping from the solvent are efficiently captured in the first water wash section.  No generic or solvent specific nitramines were found in either of the wash water  sections.

Methylamine and minor amounts of ethylamine were found in low concentrations (μg/L) and it is seen that the water wash also has effect of these volatile compounds. No generic or solvent specific nitramines were found in either of the wash water sections.

3.4 Analysis of gas emission samples

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Thirteen manual isokinetic sampling emission campaigns  were conducted during the MEA-campaign. All  emission samples were collected by TCM DA, except one which was performed by FORCE Technology. The amine plant operating conditions and detailed emission results are given in Tables 4 to 6. All nitrosamine and nitramine emissions  were below detection limits. Emissions of alkyl amines  were limited and only methylamine is quantified  in the low ppb range. Possible emission of unknown compounds has been investigated via PTR-TOF-MS. A list of identified or tentatively identified compounds is  given in Table 7.   No alkylamines, nitrosamines and nitramines  were detected by PTR-TOF-MS.

Figure 6 and Figure 7 display atmospheric emission results of MEA and NH₃ from absorber outlet over the entire campaign. Figure 6 display emission results from the FTIR and PTR-TOF-MS analyzer in comparison with results from manual isokinetic sampling and analysis. The MEA FTIR results are not considered to be reliable in the low  ppm range, since they are below/around the detection limit. The first measurement (performed on the 26th of November) showed emissions above 300 ppb. The reason for the higher amine emission in the first measurement is related to amine plant operating conditions. The NH₃ emissions were reasonably low and as expected for MEA.

According to TCM DA experience the aldehyde concentrations were varying from low ppbv to several hundred ppbv during operations. Results found in this campaign and earlier campaigns are in agreement, and they are confirmed by third party. The FTIR is not measuring aldehydes below 1 ppm, but PTR TOF gives a good agreement to results found by isokinetic sampling and analysis, see tables 7 and 8. The PTR TOF is a good candidate for a reliable online analyzer of aldehydes in the ppb range.

Comparison of emission results from three sampling and analysis methods is somewhat tricky as there are some fundamental differences like; sampling point, sample extraction principles and sample transfer to the collecting or detection units. In this case  manual  samples are collected on the top of  absorber using isokinetic extraction  principles while the online methods are extracted non-isokinetic and switched in through a 101 meter long sampling line. Hence a comparison of MEA emission data can reflect differences  in the  sampling  configuration.  The analytical differences are first of all related to instrumental detection limits. Taking sampling and analytical  differences into account the comparison of results is summarized and illustrated in figure 6. It is clear that the FTIR data is affected by high detection limit and by then increased uncertainty for this low ppm to ppb-level. Results from manual sampling and online PTR-TOF-MS are first of all according to both methods reported in a low concentration level (0,001 – 0,3 ppmv). The variation between the two data sets is significant and in general manual sampling reflects lower values than online PTR-TOF-MS results. Based on TCM-experience it is likely that the different sampling set-up explain this. TCM has experienced during this MEA campaign, that switch between different sampling points and long heated sampling lines are challenging and need to be tested more and further optimized to secure stable and representative gas composition.

The manual isokinetic sampling and analysis is considered to be a reference method for TCM DA. Isokinetic

sampling and analysis is verified by two independent third party companies (during earlier campaigns by Kema/SGS and FORCE, and in this MEA campaign by FORCE).

PTR-TOF-MS was also used for screening of potential other emissions. A list of identified or tentatively    identified compounds is given in Table 7. It is noted that PTR-TOF-MS did not detect any emissions of alkylamines, nitrosamines or nitramines.

3.4 Third party gas emission measurement

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One third-party emission measurement was done on January 6. FORCE Technology carried out isokinetic sampling onto a solid sorbent (Thermosorb/N) in combination with condensate collection in an impinger. The condensate was analyzed separately. Analysis of collected samples was done by Isconlab GmbH. The results show that all nitrosamine and nitramine emissions were below detection limits.

4. Conclusion

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Extensive atmospheric emission monitoring has been conducted at the CO₂ Technology Centre Mongstad (TCM DA) during amine based post-combustion CO₂ capture. The TCM DA amine plant was operated with the aqueous MEA solvent system treating flue gas from a combined heat and power plant (CHP). Emission monitoring was conducted by a Fourier Transform Infrared (FTIR) Spectrometry analyzer, a Proton Transfer Reaction Time-of-   Flight Mass Spectrometry (PTR-TOF-MS) analyzer, and manual isokinetic sampling followed by off-line analysis in the laboratory.

Atmospheric emissions of monoethanolamine (MEA) were very low throughout the complete campaign, and determined to be in the parts per billion (ppb) range. Atmospheric emissions of MEA amine based degradation products such as nitrosamines and nitramines were below detectable levels. Atmospheric emissions of ammonia (NH₃) were in the low ppm range, and alkyl amines in the low ppb range.

Absorber wash water sections were found to effectively reduce possible atmospheric emissions from amine based solvent system.

Acknowledgements

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The authors gratefully acknowledge the staff of TCM DA, Gassnova, Statoil, Shell, Sasol, and Aker Solutions for their contribution and work at the TCM DA facility, and the staff of the Statoil CP laboratory for their contribution  and work with the LC-MS measurements.

The authors also gratefully acknowledge Gassnova, Statoil, Shell, and Sasol as the owners of TCM DA and Aker Solutions for their financial support and contributions.

Appendix  A. Abbreviations

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References

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