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TECHNICAL REPORT
Waste Management

Degradation of Biomacromolecules during High-Rate Composting of Wheat Straw–Amended Feces

^a Dep. of Environmental Technology, Wageningen Agricultural Univ., P.O. Box 8129, 6700 EV Wageningen, the Netherlands
^b Lab. of Soil Science and Geology, Wageningen Agricultural Univ., P.O. Box 8129, 6700 EV Wageningen, the Netherlands
^c Lab. of Molecular Physics, Wageningen Agricultural Univ., P.O. Box 8129, 6700 EV Wageningen, the Netherlands
^d Dipartimento di Fisiologia delle Piante Coltivate e Chimica Agraria, Univ. of Milan, Via Celoria 2, 20133 Milano, Italy

* Corresponding author (Adrie.Veeken{at}algemeen.mt.wau.nl)

Received for publication May 26, 2000.

	ABSTRACT

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
Pig (Sus scrofa) feces, separately collected and amended with wheat straw, was composted in a tunnel reactor connected with a cooler. The composting process was monitored for 4 wk and the degradation of organic matter was studied by two chemical extraction methods, ¹³C cross polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) and pyrolysis gas chromatography–mass spectrometry (GC–MS). Wet-chemical extraction methods were not adequate to study the degradation of specific organic compounds as the extraction reagents did not give selective separation of hemicellulose, cellulose, proteins, and lignins. A new method was proposed to calculate the contribution of four biomacromolecules (aliphatics, proteins, polysaccharides, and lignin) from the ¹³C CPMAS NMR spectrum. Pyrolysis GC–MS allowed identification of the composition of the biomacromolecules. The biomacromolecules showed different rates of degradation during composting. High initial degradation rates of aliphatics, hemicellulose, and proteins were observed, where aliphatics were completely degraded and hemicellulose and proteins were partly recalcitrant during the four weeks of composting. The degradation rate of cellulose was much lower and degradation was not completed within the four weeks of composting. Lignin was not degraded during the thermophilic stage of composting but started to degrade slowly during the mesophilic stage. A combination of ¹³C CPMAS NMR and pyrolysis GC–MS gave good qualitative and semiquantitative assessments of the degradation of biomacromolecules during composting.

Abbreviations: CPMAS, cross polarization magic angle spinning • CPR, carbon dioxide production rate • GC–MS, gas chromatography–mass spectrometry • MW, molecular weight • NMR, nuclear magnetic resonance • N_org, organic nitrogen • OUR, oxygen uptake rate • TS, total solids • VFA, volatile fatty acids • VS, volatile solids

	INTRODUCTION

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
IN THE NETHERLANDS, intensive pig production systems produce large amounts of liquid manure with insufficient nearby land for application (Oudendag and Luesink, 1998). However, pig manure can also be seen as a highly valuable resource through the recycling of nutrients and organic matter to soil systems, thus reducing the use of synthetic mineral fertilizers and peat. Valorization and application of pig manure can only be made possible if specific products are produced in an economical way without negative environmental effects. A new approach is the separate collection of feces and urine by a convex conveyer belt in a liquid and solid fraction (Kroodsma et al., 1998). The separation creates options for separate treatment of the liquid fraction into a nitrogen-rich liquid fertilizer (60–70% of total N) and the solid fraction into a stabilized organic fertilizer (95–98% of total P).

The solid fraction can be converted into a stabilized organic fertilizer through composting. Composting will result in breakdown and stabilization of organic matter, mass and volume reduction, and removal of pathogens and plant seeds (Haug, 1993). High-rate composting in a tunnel reactor takes about 4 to 8 wk, after which the compost is put on piles for several months for maturation (Haug, 1993). Application of unstable composts can cause phytotoxicity, N and O₂ deficiency, and unpleasant odor (Hue and Liu, 1995). However, for most applications of compost, the high-rate composting step is sufficient for decomposition of easily degradable organic matter into a stabilized compost. For some functions of compost, such as potential for plant disease suppressiveness (Hoitink and Grebus, 1994) and production of stabilizing agents in land application (Sela et al., 1998), it is even necessary that compost contains biodegradable organic matter. We believe that a high-rate composting step of about 1 mo is sufficient to remove readily degradable organic matter and to obtain high-quality composts that can be applied directly on land without further maturation.

To evaluate the stability and degradation of organic matter during composting, wet-chemical methods and spectroscopic techniques can be applied to monitor the composition of organic matter. The evolution of the organic matter in soils and forest litter has been studied extensively by the use of wet-chemical analysis (Ryan et al., 1989; Genevini et al., 1997). However, these methods do not allow a true separation between different organic fractions, as chemical extraction suffers from losses during the chemical degradation procedure, secondary reactions, and incomplete release of degradation products (Kögel-Knabner, 1997). Leary et al. (1986) reported that Klason lignin (treatment with concentrated sulfuric acid) may fall far short of the total lignin content in wood. Instead of wet-chemical analysis, solid state ¹³C NMR and analytical pyrolysis techniques have been used to study organic matter transformations for a wide range of natural organic residues (Baldock and Preston, 1995; Baldock et al., 1997; Leinweber and Schulten, 1999). Using solid state ¹³C NMR and pyrolysis GC–MS, the composition of insoluble biomacromolecules such as polysaccharides, lignins, proteins, fatty acids, and cutin can be characterized directly from the bulk material without chemical extraction (Chefetz et al., 2000; Van Bochove et al., 1996)

The objective of the present work was to monitor the degradation of biomacromolecules (aliphatics, polysaccharides, proteins, and lignin) during the high-rate composting of pig feces in a tunnel reactor. For this, the composting of separately collected pig feces was monitored for 4 wk and samples were taken once a week. The changes in organic matter were monitored by two types of wet-chemical extraction methods, solid state ¹³C NMR and pyrolysis GC–MS. A quantitative approach is presented to assess the evolution of the biomacromolecules from the solid state ¹³C NMR spectrum.

	MATERIALS AND METHODS

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
Composting Experiment
The composting reactor was cylindrical and had a height of 0.88 m and a radius of 0.2 m as described by Veeken et al. (1999). At 0.14 m from the bottom a perforated grid was fitted, which supported the composting bed and resulted in an effective reactor volume of 93 L. The reactor was insulated to minimize heat losses to the surroundings (Veeken et al., 1999). Temperature was measured with thermocouples at five locations in the reactor. The temperature of the reactor was controlled by recirculating the air of the reactor over a water cooler, in this way removing both water and heat from the composting reactor. The O₂ level of the reactor was controlled by the flow of incoming fresh, ambient air. Both air flows were controlled by mass flow controllers (Brooks Instrument BV, Veenendaal, the Netherlands). The complete system was controlled and monitored by a computer equipped with an input–output system (RTI-80 board, 5B modules; Analog Devices, Norwood, MA) connected to the various sensors and mass flow controllers. The ammonia in the exit air was absorbed in an acid-washing bottle to measure O₂ and CO₂ concentrations.

The pig feces (Table 1) were obtained from the separate collection of feces and urine on a convex conveyer belt (Kroodsma et al., 1998). The pig feces was manually mixed with 5% of wheat straw (on fresh weight basis) to improve the porosity and structure of the compost bed. The average temperature of the reactor was controlled at 58°C and the O₂ level in the reactor at 100 mL L^-1 by the flow of the gas recirculation and ingoing air, respectively. During composting, flow rates of incoming and recirculation air, concentration of oxygen, carbon dioxide, water, and ammonia in the exit air, weight and composition of condensate, and compost bed temperature were registered. The complete compost bed was turned over once a week and a sample of approximately 1000 g was taken from the bed for chemical analysis. The total compost bed was remoistened after sampling when the moisture content of the compost bed had dropped to less than 400 g kg^-1 total solids (TS).

Wet-Chemical Analysis of Organic Matter
Two wet-chemical techniques developed for wood and forage fiber analysis were used to determine the different organic matter fractions of the compost bed (Ryan et al., 1989). Wood analyses yielded four fractions (Adani et al., 1995): (i) soluble in a benzene–ethanol (16.87 mol L^-1) mixture (50:50 v/v) and ethanol (16.87 mol L^-1), (ii) soluble in 0.94 mol L^-1 sulfuric acid, (iii) soluble in 13.5 mol L^-1 sulfuric acid, and (iv) insoluble in 13.5 mol L^-1 sulfuric acid. Lipids were solubilized by the first extraction step, proteins and hemicellulose by the second step, and cellulose by the third step. The ligno–humic (or lignin) complex was left in the residual fraction (Adani et al., 1995). Forage fiber analyses were performed for neutral detergent fiber (NDF), neutral detergent acid detergent fiber (NDADF), and acid detergent lignin (ADL) according to the Van Soest method (Van Soest et al., 1991). Cell solubles (VS-NDF), hemicellulose (NDF-NDADF), cellulose (NDADF-ADL), and lignin (ADL) were calculated according to Van Soest et al. (1991). Analyses were performed in duplicate.

Solid State Carbon-13 Nuclear Magnetic Resonance Spectroscopy
Solid state ¹³C-NMR spectra were obtained using CPMAS on a wide-bore AMX 300 spectrometer (Brucker, Karlsruhe, Germany) operating at a ¹³C frequency of 75.47 MHz. The following parameters were used: spinning speed of 4.5 kHz; acquisition time of 33 ms; ¹³C 90° pulse length of 4 µs; contact time of 0.8 ms, recycle delay of 1 s, and line broadening of 50 Hz (Conte et al., 1997). For each spectrum, 3600 scans were recorded. It was assumed that for these conditions the spectra could be analyzed quantitatively as stated by Haw et al. (1984).

Pyrolysis Gas Chromatography–Mass Spectrometry and Thermally Assisted Hydrolysis and Methylation
Pyrolysis was carried out on a Curie-Point pyrolyzer (Horizon Instruments, Heathfield, UK) according to Nierop (1998). Samples were pressed onto flattened Curie point wires and heated for 5 s at 610°C. The pyrolysis unit was connected to a gas chromatograph (GC8000; Carlo Erba, Milan, Italy) and the products were separated by a fused silica column coated with CP-Sil 5 (Varian, Palo Alto, CA; film thickness 0.40 µm, length 25 m, i.d. 0.25 mm). Helium was used as carrier gas. The oven was initially kept at 40°C during pyrolysis, next it was heated at a rate of 7°C min^-1 to 320°C and maintained at that temperature for 20 min. The end of the GC column was coupled to a MD 800 mass spectrometer (mass range m/z 45–650, ionization energy 70 eV, cycle time 1 s; Fisons, Manchester, UK). Pyrolysis in the presence of tetramethylammonium hydroxide (TMAH), actually thermally assisted hydrolysis and methylation, was performed by adding a droplet of a 25% solution of TMAH in water to the sample that was pressed onto the Curie point wire, after which the sample was dried using a 100-W halogen lamp, and immediately pyrolyzed.

Quantification of the Organic Matter Evolution from Solid State Carbon-13 Nuclear Magnetic Resonance
If we consider that the ¹³C CPMAS NMR spectra obtained were quantitative, the transformation of various biomacromolecules can be calculated following the procedure of determination of lignin and cellulose in wood (Haw et al., 1984). Four types of carbon can be distinguished in the NMR spectrum: (i) alkyl carbon (0–50 ppm) in lipids, fatty acids, and plant aliphatic biopolymers (e.g., cutin and suberin); (ii) O-alkyl carbon (50–110 ppm) in polysaccharides, proteins, and side chains of lignin; (iii) aromatic carbon (110–160 ppm) in lignin and proteins; and (iv) carbonyl carbon (160–225 ppm) in aliphatic esters, carboxyl groups, and amide carboxyls. As four different types of carbon can be distinguished, four types of biomacromolecules can be calculated from the relative areas. Aliphatics (lipids, biopolymers, fatty acids), polysaccharides (cellulose and hemicellulose), proteins, and lignin were chosen because these are the main biomacromolecules in natural organic matter (Wilson, 1987). Each biomacromolecule was described in terms of average molecular weight (MW, g mol^-1), carbon content per molecule (C), and the fraction of the four different types of carbon. For aliphatic compounds we proposed a MW of 292 with 16 C, derived from a structure of fatty acid long chains and biopolymers (e.g., cutin), assuming one carbonyl group per lipid molecular unit (Kolattukudy, 1980). Polysaccharides had a MW of 162 and six C exclusively constituted of O-alkyl C (Haw et al., 1984). For proteins we assumed an average amino acid composition of pig feces (Skrede et al., 1998). The contribution of the various types of carbon groups was calculated from the amino acid composition. Lignin had a MW of 183 and 9.9 C per molecule, of which 6 were aromatic C, 0.92 methoxyl C, and 3 side chain C (Haw et al., 1984). The characteristics of each biomacromolecule are summarized in Table 2. The relative intensities (I) of the four regions in the ¹³C NMR spectrum depend on the mass distribution of the biomacromolecule according to:

[1a]

[1b]

[1c]

[1d]

where I is the relative intensity of the NMR region (% of total peak area) and f is the mass fraction of each biomacromolecule on a carbon basis. Thus, the biomacromolecular composition of organic matter (on a C basis) can be calculated from the relative intensities of the four regions in the NMR spectrum by the following equations:

[2a]

[2b]

[2c]

[2d]

[3a]

[3b]

[3c]

[3d]

	RESULTS AND DISCUSSION

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
Composting Process
The oxygen uptake rate (OUR; mol O₂ kg^-1 VS h^-1), cumulative oxygen uptake (COU; mol O₂ kg^-1 VS), ratio of carbon dioxide production rate (CPR) and OUR, flow rates of incoming and recirculation air, and temperature of the compost bed are shown in Fig. 1. The compost bed was turned over after 7, 14, and 21 d of composting. The time course of OUR was typical for composting; after a short lag phase a rapid increase in OUR took place until the OUR reached a maximum. During that period biomass and oxygen availability were limiting the degradation of organic matter (Hamelers, 1993). After the maximum, OUR leveled off to an almost constant value. During this period, hydrolysis of organic matter becomes the rate-limiting step of the process. Moreover, OUR increased each time when the total compost bed was turned over. This is due to the redistribution of individual waste particles (Hamelers, 1993) and because more optimal conditions were provided by remoistening the compost bed. The set-point temperature of the compost bed was maintained for about 14 d, after which the temperature gradually fell down. The temperature gradient over the reactor was significantly reduced because air was recirculated (data not shown). The set-point temperature was reached again at the beginning of Week 3, and for a short period after the temperature declined again. The CPR to OUR ratio was greater than 1 during the first 2 d of composting, indicating that more reduced substrates, such as fatty acids, were degraded. A constant ratio of about 0.9 prevailed during the rest of composting, indicating the degradation of polysaccharide-like substrates (Haug, 1993). The flow rates of incoming and recirculation air both increased with increasing OUR because more oxygen was needed for aerobic degradation, and consequently more heat had to be removed from the compost bed.

View larger version (20K): [in this window] [in a new window]   Fig. 1. Characteristics of the composting process. (A) Oxygen uptake rate (OUR) and cumulative oxygen consumption (COU). (B) Ratio of oxygen uptake rate on carbon dioxide production rate (CPR). (C) Flow rates of incoming and recirculation air. (D) Average temperature of the compost bed.

[4]

where M_i and M_f are the initial and final weight of the compost bed (kg), TS_i and TS_f the initial and final total solids content (g kg^-1), and VS_i and VS_f the initial and final volatile solids content (g kg^-1 TS). Based on total mass, degradation of VS amounted to 38% after 4 wk of composting. The pH of the compost bed initially increased due to degradation of VFA but slightly dropped at the end of the composting process due to ammonia volatilization (Table 1). Despite the high loss of ammonia, the total nitrogen content (g N kg^-1 TS) did not decrease significantly because concomitantly a high amount of TS was lost due to the degradation of organic matter.

Solid State Carbon-13 Nuclear Magnetic Resonance Spectroscopy
Figure 2 shows ¹³C CPMAS NMR spectra of straw, pig feces, and the compost bed after 1 and 4 wk of composting. First, the peaks in the spectra were assigned to the different carbon types (Baldock and Preston, 1995; Kögel-Knabner, 1997). Alkyl groups can be found around 21 ppm (terminal methyl) and 32 ppm (methylene in aliphatic rings and chains). The signal at 56 ppm can be assigned to methoxyl in lignin (phenolmethoxyl of coniferyl and sinapyl moieties) and in hemicellulose (glucoronic acid in xylan). The region between 60 to 110 ppm shows typical peaks of polysaccharides and proteins, but also that side-chain groups (oxygenated C, C_ß, and C carbon) of the phenylpropane lignin structural unit provided a minor contribution to this region (Haw et al., 1984; Kolodziejski et al., 1982). Signals around 72 to 74 ppm are due to C₂, C₃, and C₅ of cellulose and the peak at 65 ppm can be assigned to crystalline components of C₆ in hexose or C₅ in pentose. Peaks at 83 and 88 ppm are due to noncrystalline and crystalline components of C₄ and the peak at 105 ppm to dioxygenated anomeric C₁ of cellulose. Signals derived from hemicellulose are contained within the cellulose peaks. Signals at 115, 130, 148, and 152 ppm can be assigned to lignin and lignin-derived products: the signal at 115 ppm is due to unsubstituted aromatic carbons ortho or para to substituted carbon, the signal at 130 ppm represents C-substituted aromatic carbon, the signal at 147 ppm to O-substituted aromatic carbon of guaiacol, and the signal at 152 ppm to aromatic carbons connected to methoxy groups in syringol units. The peak at 174 ppm is assigned to carboxylic, amide, and ester groups.

View larger version (14K): [in this window] [in a new window]   Fig. 2. Cross polarization magic angle spinning (CPMAS) 13C nuclear magnetic resonance (NMR) spectra of straw, pig feces, and compost bed after 1 and 4 wk of composting.

[5]

where M_C is the mass of carbon type C (kg), M the total weight of the compost bed (kg), TS the total solids content (g kg^-1), VS the volatile solids content (g kg^-1 TS), and I the relative area of a carbon type in the ¹³C NMR spectrum (% of total peak area). The change in absolute amounts (% of initial amount) of the four carbon types as shown in Fig. 3 gives a completely different picture than the relative amounts (Table 3). The alkyl amount decreased significantly during the first week of composting (40%), indicating the easily degradable nature of alkyl groups. After the first week the rate of decrease declined and after 4 wk 65% of alkyl carbon had disappeared. During the first week, the decrease in alkyl was accompanied by a large decrease in carboxylic carbons (40%), indicating that fatty acids were degraded. The aromatics showed little change during composting, which suggests that that the degradation of lignin under thermophilic conditions was negligible (Tuomela et al., 2000).

View larger version (10K): [in this window] [in a new window]   Fig. 3. Absolute changes in relative areas of the four nuclear magnetic resonance (NMR) regions during high-rate composting of wheat straw–amended pig feces.

View larger version (52K): [in this window] [in a new window]   Fig. 4. Recovery of the four biomacromolecules during sequential forage fiber analysis of the sample after 1 wk of composting (NDF, neutral detergent fiber; NDADF, neutral detergent acid detergent fiber; ADL, acid detergent lignin).

Pyrolysis Gas Chromatography–Mass Spectrometry and Methylation
Pyrolysis GC traces of straw, pig feces, and the compost bed after 1 and 4 wk of composting are shown in Fig. 5. Pyrolysis GC–MS is a qualitative method to determine the composition of a given sample. Comparison of GC traces after pyrolysis of different samples allows a semiquantitative evaluation of possible changes. The pyrolysate of the straw is dominated by lignin-derived guaiacols (2-methoxyphenols) and syringols (2,6-dimethoxyphenols) (Saiz-Jimenez and De Leeuw, 1986). Other important compounds are derived from polysaccharides, and from lipids, especially fatty acids and terpenoids. The pyrolysate of pig feces has abundant signals from fatty acids (C₁₆, C_18:1, and C₁₈), and furthermore from guaiacols, syringols, steroids, and a few from polysaccharides. After 1 wk of composting, the contribution of guaiacols and syringols and especially those of the steroids increased. After 4 wk, the pyrolysate is dominated by the lignin-derived guaiacols and syringols. Fatty acids and steroids decrease significantly, although the latter ones increase relatively with respect to the fatty acids. The distribution pattern of the lignin-derived pyrolysis products again showed no alteration during composting.

View larger version (18K): [in this window] [in a new window]   Fig. 5. Pyrolysis gas chromatography traces of straw, pig feces, and the compost bed after 1 and 4 wk of composting (, polysaccharides; , lignin; , fatty acids; , steroids).

Organic Matter Evolution during Composting
As discussed previously, wet-chemical extraction did not result in selective separation of biomacromolecules but can only be used as an indication of the concentrations. Due to the complex composition of our samples and the intrinsic problems of ¹³C NMR to obtain quantitative results, calculations of organic matter composition on the basis of Eq. [1] and [2] should also be interpreted semiquantitatively (Golchin et al., 1997). On the basis of our results of both wet-chemical extraction and ¹³C CPMAS NMR, we could obtain six organic compounds: (i) soluble aliphatics (wood analysis), (ii) insoluble aliphatics (aliphatic-NMR minus soluble lipids), (iii) hemicellulose (forage fiber analysis), (iv) total polysaccharides, (v) proteins (NMR), and (vi) lignin (NMR). As stated earlier, relative contents (g kg^-1) can only give information on the relative degradation rates of compounds, but to obtain information about the degradation, absolute amounts (kg) have to be compared. The development of the absolute amounts of the organic compounds (kg) during 4 wk of composting, as shown in Fig. 6, were obtained following Eq. [5]. Together with the CPR to OUR ratio (Fig. 1), the characteristics of the compost bed (Table 1), and the results of pyrolysis GC–MS, the evolution of organic matter during the composting process could be evaluated qualitatively and semiquantitatively.

View larger version (17K): [in this window] [in a new window]   Fig. 6. Development of total organic matter and specific organic compounds during high-rate composting of wheat straw–amended pig feces.

	CONCLUSIONS

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
High-rate composting of straw-amended pig manure resulted in the degradation of 40% organic matter within 4 wk of composting and drying of the compost bed. High degradation rates of aliphatics, hemicellulose, and proteins were observed during the first week of composting but part of hemicellulose and proteins were recalcitrant during the rest of the composting. The degradation rate of cellulose was much smaller and was only partly degraded within 4 wk. Lignin was not degraded in the thermophilic stage of composting but started to degrade slowly in the mesophilic stage, probably due to an increase in fungal activity. However, no alteration of the lignin structure was observed within 4 wk. After 4 wk of composting, readily degradable organic compounds were degraded and wheat straw-amended pig feces were converted into a stabilized product. We propose that this product can be applied directly on land as organic fertilizer without negative effects on soil and plants. Moreover, the product still contains degradable organic matter, especially cellulose, which could give the compost potential for suppression of plant diseases and stabilization of soil aggregates.

This study again confirmed that wet-chemical extraction methods are not highly selective and only give an estimation of the composition of organic matter. The forage fiber analysis gave an overestimation of the lignin content because proteins and polysaccharides were retained in the lignin structure. Polysaccharides are underestimated because they are not completely extracted. We recommend a combination of ¹³C CPMAS NMR and pyrolysis GC–MS, where ¹³C CPMAS NMR gives a quantitative assessment of the biomacromolecules and pyrolysis GC–MS can be used to identify specific organic compounds of the biomacromolecules.

	ACKNOWLEDGMENTS

 
The research described in this paper is part of the Hercules project, a multidisciplinary collaboration, which is financially supported by the Economy, Environment and Technology Programme of the Dutch government. The authors thank Vinnie de Wilde for performing the composting experiment and Van Soest analysis, and Fulvia Tambone and Barbara Scaglia for wood extraction analysis. The stay of F. Adani in Wageningen was supported by the European Community activity Large-Scale Facility Wageningen NMR Centre.

	NOTES

TOP NOTES ABSTRACT INTRODUCTION MATERIALS AND METHODS RESULTS AND DISCUSSION CONCLUSIONS REFERENCES

 
K.G.J. Nierop, present address: IBED-Physical Geography and Soil Science, Univ. of Amsterdam.

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