Supplemental files:

A five-stage treatment train for water recovery from urine

and shower water for long-term human Space missions

R.E.F., Lindeboom1,2, J., De Paepe1, M., Vanoppen3, B., Alonso-Fariñas1,4, W., Coessens1,
A., Alloul1,8, M.E.R., Christiaens1, C., Dotremont5, H., Beckers5, B., Lamaze6, D., Demey7,
P., Clauwaert1, A.R.D., Verliefde3 & S.E., Vlaeminck1,8

1
Center for Microbial Ecology and Technology (CMET), Faculty of Bioscience Engineering, Ghent University,
Coupure Links 653, 9000 Gent, Belgium
2
Section Sanitary Engineering, Department of Water Management, Faculty of Civil Engineering and
Geosciences, Delft University of Technology, Stevinweg 1, 2628CN, Delft, The Netherlands
3
Particle and Interfacial Technology Group (PaInT), Faculty of Bioscience Engineering, Ghent University,
Coupure Links 653, 9000 Gent, Belgium
4
Departamento de Ingeniería Química y Ambiental, Universidad de Sevilla, Higher Technical School of
Engineering, Camino de los Descubrimientos s/n, 41092, Seville, Spain
5
VITO, Boeretang 2, 2400 Mol, Belgium
6
ESA/ESTEC, Keplerlaan 1, 2201 AZ, Noordwijk, The Netherlands
7
QinetiQ Space, Hogenakkerhoekstraat 9, 9150 Kruibeke, Belgium
8
Research Group of Sustainable Air, Energy and Water Technology, University of Antwerp, Groenenborgerlaan
171, 2020 Antwerpen, Belgium

S1
Supplemental File A: Details on urine and shower water collection and

reactor setup

Figure A.1: (A) Urine collection setup placed in the men’s room and (B) Shower setup
integrated into the WTUB facility.

S2
Figure A.2: Crystallization reactor, as part of the urine treatment unit (UTU)
A: magnetic stirring and heating plate (MR Hei-Tec, Heidolf®, Schwabach, Germany)
B: level sensor (BC10-QF5,5-AP6X2, Turck, Mülheim an der Ruhr, Germany)
C: pH sensor (pH electrode 5334T w/ Pt1000, Hach, CO, USA)
D: temperature sensor
E: influent inlet
F: NaOH dosage with electromagnetic metering pump (EWN-B11 CER, Iwaki Co, Ltd.,
Tokyo, Japan (not shown))
G: filter basket with glass fiber cloth
H: filter (Kleenpak KA3J100P6 (10 µm), Pall Corporation, NY, USA)
I: filter (Kleenpak KA3NFP6S (0.2 µm), Pall Corporation, NY, USA)
J: dead-end filter basket with electrical conductivity probe (Cond cell 5396, Hach, CO, USA)
K: sample point
L: recycle and feed pump (Model 323E/D, Watson Marlow, MA, USA)

S3
Figure A.3: Nitrification bioreactor of the urine treatment unit (UTU)
A: bioreactor with polyvinyl alcohol beads (Kuraray Aqua Co, Ltd., Tokyo, Japan)
B: pH sensor (Polymetron 8350 series, Hach, CO, USA)
C: influent inlet (effluent of precipitation reactor)
D: NaOH dosage with electromagnetic metering pump (EWN-B11 CER, Iwaki Co, Ltd.,
Tokyo, Japan (not shown))
E: sample point
F: recirculation pump (Peristaltic pump AMP Series, Boyser pumps®, Barcelona, Spain)
G: compressor aerator (KNF N035AN.18, KNF, Freiburg, Germany)
H: EC sensor (Cond cell 5396, Hach, CO, USA) in recirculation loop
I: ultrafiltration (UF) membrane module (type 1/6, ATech-Innovations GmbH, Gladbeck,
Germany)
J: bypass
K: filtration pump (120U/D1, Watson Marlow, MA, USA)
L: pressure relief valve (V185, Frank GmbH, Hessen, Germany)
M: mass flow meter and controller (LIQUI-FLOW, Bronkhorst®, Ruurlo, The Netherlands)
N: sample point UF filtrate

S4
Figure A.4. Electrodialysis unit in the urine treatment unit (UTU)
A: ED stack (PCCell ED 64004, PCA GmbH, Heusweiler, Germany)
B: power supply (Type ES300, Delta elektronika BV, Zierikzee, The Netherlands)
C: recirculation pump diluate (Model 323E/D, Watson Marlow, MA, USA)
D: recirculation pump electrolyte (MD-15RM-230GS, Iwaki Co, Ltd., Tokyo, Japan)
E: recirculation pump concentrate (MD-15RM-230GS, Iwaki Co, Ltd., Tokyo, Japan)
F: diluate tank
G: electrolyte tank
H: concentrate tank
I: sample point diluate
J: sample point concentrate
K: pH and EC sensor diluate (pH electrode 5334T w/ Pt1000 and Cond cell 5396, Hach, CO,
USA)
L: EC probe concentrate (Cond cell 5396, Hach, CO, USA)

S5
Figure A.5: Shower water treatment unit (SWTU)
A: storage tank grey water
B: peracetic acid dosing unit
C: mixing tank grey water – ED diluate – RO filtrate
D: nanofiltration unit 1
E: nanofiltration unit 2
F: one recirculation and one pressure booster pump of RO module (only front pump visible)
G: SC1000 controller (Hach, Germany)
H: buffer tank RO concentrate
I: RO unit 1 (Drukhuis 10-730 and 10-731, European Membrane Institute-Twente, The
Netherlands)
J: RO unit 2 (Drukhuis 10-730 and 10-731, European Membrane Institute-Twente, The
Netherlands)
K: one recirculation and one pressure booster pump of RO module (only front pump visible)
L: storage tank hygienic water (RO permeate)

S6
Supplemental File B: Analytical Methods

The concentrations of Cl-, NO2-, NO3-, SO42- and PO43- were determined on a Metrohm 930
Compact Ion Chromatograph (Metrohm, Switzerland) equipped with a conductivity detector
and a metrosep A supp 5 column containing quaternary ammonium groups. Na +, NH4+, K+,
Ca2+ and Mg2+ were determined on a Methrom 761 Compact Ion Chromatograph (Metrohm,
Switzerland) equipped with a conductivity detector and Metrosep A supp 5-150/4.0 column.
Samples were filtered (0.22 µm ChromafilXtra filter) and diluted with milli-Q water to a
range of 0.05 to 100 mgion L-1 before analysis. COD was analysed with Nanocolor® tube test
kits (COD15000; Macherey-Nagel, USA). The COD concentration was determined in
unfiltered samples, since filtering would remove the particulate COD fraction. Samples were
diluted with milli-Q water prior to destruction so that the concentration fell within detection
limit (1000-15000 mg COD L-1). Total Kjeldahl nitrogen (TKN) was analysed according to
Standard methods (4500-Norg B; APHA, 1992). Samples were diluted with milli-Q water
prior to destruction so that the concentration fell within the detection limits (9 - 250 mg NH 4+-
N L-1). Calcium and magnesium concentrations were analysed by means of atomic absorption
spectrometry (Shimadzu, AA6300). The samples were diluted with milli-Q water and
acidified with 1% nitric acid and 2% of Lanthanum solution.

S7
Supplemental File C: Performance data SWTU

Table C.1: Overview of compound specific average retentions in the different membrane
modules as calculated from the concentrations and flows presented in Table 2
(manuscript).
NF Retention RO Retention
(%) (%)

N-total 4 91
N-[NH4+/NH3] 5 66
-
N-NO 3 3 92
-
N-NO 2 51 97
COD 37 95
++
Ca 42 96
+
K 3 94
Na+ 5 96
++
Mg 8 98
P 29 97
-
Cl 5 93
2-
S - SO4 28 96

Table C.2: Overview of results (mass balance) of offline measurements during

representative operation.
Day QEDD,in Qshower Qdrain,NF Qdrain,RO* QRO permeate** Recover
water,in y
(L d-1) (L d-1) (L d-1) (L d-1) (L d-1) (%)
1 4.5 3.0 0.87 0.92 6.49 86.5
2 4.5 3.0 0.45 0.65 6.95 92.7
3 4.5 3.0 0.95 1 6.40 85.3
4 4.5 3.0 0.93 1.40 6.36 84.8
5 5.3 3.3 0.81 2.26 7.49 86.7
6 5.3 1.6 0.93 3.12 5.49 79.7
7 5.3 0.1 0 3.6 4.84 90.0
8 5.3 2.4 1.21 0.81 6.41 82.8
9 5.3 7.7 0.30 2.17 12.42 95.2
10 5.3 7.2 1.01 4.56 10.79 86.4
average 5.0 3.4 0.75 2.05 7.36 87.0
* RO concentrate was drained, but 85% was used to dilute urine in the urine treatment plant
** RO permeate was automatically pumped from the collection tank to a preset level in the mixing
tank. With increased flow rates of shower water, the retention time and thus the influence on net RO
permeate production will decrease. Recovery has therefore been calculated based on the actual losses.

S8
A B

C D

E F

S9
G H

I J

K L

S10
M N

O P

Q R

S11
 S T

U V

Figu
re C.1: Overview of WTUB raw anion (A-U) and cation (B-V) measurements taken
during combined operation of stored urine, bioreactor, ED diluate, ED concentrate,
Shower water, Mixing tank, NF concentrate, NF permeate, RO retentate, RO
concentrate and RO permeate.

Background analysis permeability, biofouling and scaling potential

It was hypothesized that with a surface area of 0.052 m 2, 20-40 L d-1 of NF permeate could be

produced assuming an operational pressure between 2-4 bar. The NF flux was however

deliberately reduced during the initial phase because the system was limited by the

permeability of the SWRO membranes in the RO unit. NF permeabilities of >20 L m -2 h-1 bar-1

S12
were achieved. However, after switching to the BWRO, the mixture of shower water and ED

diluate also resulted in a ~50% decrease in permeability from 14 to 7 L m -2 h-1 bar-1. Due to

this reduction in observed permeability, it was not feasible to produce the required flow rate

through the NF without making concessions to the operating conditions.

Figure C.2: Permeability (left axis)and flux (right axis) during the period of operation
for the a) NF and the b) RO. Initially a seawater RO (SWRO) membrane and from the
arrow a brackish water RO (BWRO) membrane was used to treat a 1:1:1 mixture of
shower water, ED diluate and RO permeate. The peaks resulting in increased
permeability were the consequence of cleaning cycles

S13
For the SWRO membrane (DOW-SW30), the hypothesis to produce 20-30 L d -1 of RO

permeate at a pressure of 10-15 bar with 0.04 m 2 membrane surface area was also proven

false. The clean water permeability (2.1 ± 0.3 L m-2 h-1 bar-1) declined within minutes upon

operation with real shower water and ED diluate and stabilised at 0.6 ± 0.1 L m-2 h-1 bar-1

(Figure C.2). Subsequently, it was postulated that a substitution of the SWRO by a BWRO

membrane (DOW-BW30) would result in a higher overall flow rate and reduced pressure

requirement due to the relatively low measured conductivity of the NF permeate (1-3 mS cm -
1
) and RO-concentrate (8-10 mS cm -1). Although the permeability of the BWRO membrane

exceeded the SWRO membrane permeability in the entire operational period a decline from

2.1-2.3 to 0.7-0.9 L m-2 h-1 bar -1 was observed over the course of the experiment (Figure C.2).

In order to understand the observed decline, both the scaling and biofouling potential were

analysed based on the measured water composition and will be described in the next section.

Figure 2A revealed that the addition of ED diluate, which showed limited microbial growth

potential due to the lack of COD, caused a significant increase in the biological growth

potential in the NF permeate, by supplementing the limiting nutrient in shower water (N). The

results of this analysis also correspond with visual observations and the observed decline in

permeability of both the SWRO and BWRO membranes.

For real-life applications like in the Concordia station, a sanitary design approach would have

prevented micro-organisms to enter this sensitive section of the unit. In previous studies, PAA

solution (1%) was therefore also dosed successfully as a powerful biodegradable oxidizing

agent to stabilize the shower water and control microbial growth. But in the current study a

non-sanitary design was chosen, due to which PAA could contribute to the biofouling

potential. As PAA decomposes into acetic acid and hydrogen peroxide according to the

following equation:

S14
 C 2 H 4 O3 + H 2 O← → H 2 O2 +C H 3 COOH

Once free peroxide (H2O2) is consumed, the equilibrium shifts from peracetic towards acetic

acid, a readily biodegradable carbon source. In the storage tank, the COD concentration was

as high as 1.5 COD g L-1. This was decreased to 0.46 g COD L -1 in the mixing tank (due to

dilution with ED diluate). In line with previous studies, acetic acid/acetate rejection on the NF

was limited [1, 2]. As acetic acid was the main contributor to COD, the rejection of COD by

the ceramic NF was lower than reported elsewhere [3]. The operation of the NF was not

severely affected as active PAA was present in this compartment. However, to prevent

oxidative damage to the RO membranes, the system was steered towards a low PAA

concentration (< 1 mg L-1) in the NF permeate. It is therefore anticipated that due to the

addition of traces of nitrogen through the ED diluate, microbial growth, biofouling and RO-

permeability were limited by carbon instead of nitrogen.

The saturation index (SI) measures the degree of supersaturation of ions in solution with

respect to the chemical equilibrium solubility. Based on the liquid composition urine, ED

diluate, shower water and RO permeate the SI was calculated for the most common

precipitates (Figure C.3). From this the most likely precipitating compounds were selected for

the simulation presented in figure 2B. The stepwise water-removal source code

(https://water.usgs.gov/water-resources/software/PHREEQC/documentation/phreeqc3-html/

phreeqc3-79.htm) was originally developed for evaporative processes, but was adapted to

mimic the effect of an increasing theoretical Volumetric Concentration Factor (VCF) on the

estimated precipitation of calcium phosphate (as indicated by TCP, Ca 3(PO4)2) and

magnesium phosphate (as indicated by NH4 –struvite) [4, 5].

S15
Figure C.3: Saturation index of various minerals in urine, ED diluate, shower water and a mixture of
shower water and ED diluate as calculated in phreeqC.

Due to the negative SI of the ED diluate, the SI for TCP was effectively lowered in the

mixture of shower water and ED diluate (3.6) compared to the SI in shower water only (6.1).

With respect to calcite (CaCO3) a similar decrease in SI was observed from-1.2 to -1.3 for

shower water only compared to shower water mixed with ED diluate (Figure C.3). For both

the shower water and the ED diluate mixed with shower water the maximum precipitates per

liter formed were theoretically around 0.05 mmol L -1 at a concentration factor of 5. It is

noteworthy that without urine pretreatment the mixture would result in 0.21 and 0.27 mmol L -
1
precipitates per liter for NH 4-struvite and TCP (Figure 2B). It was therefore concluded that

the urine pretreatment and addition of ED diluate to shower water successfully decreased the

scaling potential in the NF and RO.

S16
Table C.3. Input data used for phreeqC simulations

SOLUTION 1: fresh 2: ED 3: shower 4: permeate 5: Acid

urine diluate water

pH 7.00 6.3 7.00 8.00 4.00

Density 1.014 1.014 1.014 1.014 1.014
temperature [°C] 35 28 25 25 25
calcium [mg L-1] 135 0.2 13 1
magnesium [mg L-1] 39 1 6 1
sodium [mg L-1] 2209 741 45 66
potassium [mg L-1] 1971 117 26 8
chloride [mg L-1] 3449 283 25 37 3545
ammonium [mg L-1] 771 9 2 2
sulphur [mg L-1] 153 54 7 2
phosphor [mg L-1] 64.9 51 18 2
alkalinity as HCO3 5700 1540 150 134

Table C.4. Input data used for phreeqC simulations

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 10 graph_x 1 / tot("water")
SOLUTION 20 graph_y log10(tot("Na")),
log10(tot("Cl")), log10(tot("Mg")),
[Table D.1] log10(tot("Ca")), log10(tot("P")),
log10(mol("MgHCO3+"))
MIX 1
10 USER_GRAPH 2
20 -headings water Urine_Calcite
3 0.5 Urine_Hydroxyapatite Urine_Dolomite
4 0.5 Urine_Struvite Urine_TCP
5 0.0 -axis_scale x_axis 0 100
-axis_scale y_axis 0 0.001 auto auto
PHASES -axis_titles "Volumetric Concentration
Struvite 390 factor" "Precipitates (moles)"
MgAmmHPO4:6H2O = Mg+2 + AmmH+ -chart_title "Expected Precipitation"
+ PO4-3 + 6H2O -start
log_k -13.26 10 graph_x 1 / tot("water")
20 graph_y equi("Calcite")
TCP equi("Hydroxyapatite") equi("Dolomite")
Ca3(PO4)2 = 3Ca+2 + 2PO4-3 equi("Struvite") equi("Ca3(PO4)2")
log_k -35.2749931
delta_h -76.38 kJ USER_GRAPH 3
-headings water Urine_SI(Calcite)
EQUILIBRIUM_PHASES Urine_SI(Hydroxyapatite)
Urine_SI(Dolomite) Urine_SI(Struvite)
# carbonates... Urine_SI(Ca3(PO4)2)
CO2(g) -3.5 0 -axis_scale x_axis 0 20
Calcite 0 0 -axis_scale y_axis -10 10 auto auto
Dolomite 0 0 -axis_titles "Volumetric Concentration
factor" "Saturation index"
# sulfates... -chart_title "Saturation index"
-start
Gypsum 0 0 10 graph_x 1 / tot("water")
20 graph_y SI("Calcite")
# phosphates SI("Hydroxyapatite") SI("Dolomite")
Hydroxyapatite 0 0 SI("Struvite") SI("Ca3(PO4)2")
Struvite 0 0
Ca3(PO4)2 0 0 USER_GRAPH 4
-headings pH
USER_GRAPH 1 -axis_scale x_axis 0 20
-headings x Urine_Na+ Urine_Cl- -axis_scale y_axis 0 14 auto auto
Urine_Mg+2 Urine_Ca+2 Urine_PO4-3 -axis_titles "Volumetric Concentration
Urine_MgHCO3+ factor" "pH"
-axis_scale x_axis 0 20 auto auto -chart_title "Saturation index"
-axis_scale y_axis -6 1 auto auto -start
-axis_titles "Volumetric Concentration 10 graph_x 1 / tot("water")
factor" "Log(Molality)" 20 graph_y -LA("H+")
-chart_title "Estimated Ion Concentration"
-start REACTION
H2O -1; 0 36 3*4 6*1 2*0.25 0.176 5*0.03

INCREMENTAL_REACTIONS true

END

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Van Dijk, The role of electrostatic interactions on the rejection of organic solutes in aqueous
solutions with nanofiltration, Journal of Membrane Science, 322 (2008) 52-66.

S18
[2] Y.-H. Weng, H.-J. Wei, T.-Y. Tsai, W.-H. Chen, T.-Y. Wei, W.-S. Hwang, C.-P. Wang,
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dynamics in a urine-collecting system, Water Research, 37 (2003) 2571-2582.

S19
Supplemental File D: Details on the theoretical energy balance

Table D.1: Overview of the theoretical energy balance and assumptions.

CCU Energy Demand Assumptions Pilot scale Comments/Industrial scale
pH control negligible 0 kWhe/d
Density Flow Rate Pressure drop
(kg/L) (m3/h) (bar) operated at 100 rpm out of 400. If linear 25 W
PMP CCU pmp3 1.05 0.00375 0.3 0.001 kWhe/d out 100 W

Heating CCU condensate 1.5 4.2 0.021 kWhe/d COP = 3 4 to 40 ºC

Heating CCU flush 0.3 4.2 0.002 kWhe/d COP = 3 20 to 40 ºC
Heating CCU concentrate 5.8 4.2 0.023 kWhe/d COP = 3 30 to 40 ºC
Heating CCU urine 1.5 4.2 0.002 kWhe/d COP = 3 37 to 40 ºC
Total 0.049 kWhe/d
0.008 kWh/L
UTU Energy Demand Assumptions Pilot scale Comments/Industrial scale
Pump 1 1.05 0.3 0.3 0.082 kWhe/d
Pump 2 1.05 0.000375 0.3 0.000 kWhe/d
Compressor 0.0225 0.5 0.276 kWhe/d compressor (pressure drop = height of the bed;
Cooling (from 40 to 28) 0.006 kWhe/d mass flow from aeration ratio)
Total 0.364 kWhe/d
0.056 kWh/L
Compressor calculations Efficiency 0.75
Pressure in the botton 1.25 aeration ratio (m3/s·m3) 0.02
W (kJ/kmol) 569 air molar flow (kmol/d) 1.31

EDU Energy Demand Assumptions Pilot scale Comments/Industrial scale

Pump 1,2 and 3 1.05 0.045 0.5 0.02 kWhe/d stable flow rate at 250mL/min
Flow rate
(L/d) (Wh/L) Ref
Power Supply 7.5 4.3 [13] 0.03 kWhe/d
0.05 kWhe/d Industrial ratio ==> 2 kWh/m3 (or lower) =20
Urine 4.300 kWh/m3 0.15 kWh/d
0.008 kWh/L 0.023 kWh/L
NF Energy Demand Assumptions Pilot scale Comments/Industrial scale
Pump 1 (Feeding) 1.05 0.000563 6.28 0.003 kWh/d Assuming no recirculation to the tank
Operation at cross-flow velocity 1,5 m/s (flow
Pump 2 (Recirc.) 1.05 0.208 0.780.149 kWh/d rate and pressure drop from preliminary study)
Total 0.152 kWh/d Industrial ratio ==> 1 kWh/m3 (or lower) =10
Permeate 13.2 kWh/m3 0.135 kWh/d
0.024 kWh/L 0.021 kWh/L
RO Energy demand Assumptions Pilot scale Comments/Industrial scale
Pump 1 (Feeding) 1.05 0.000417 14.3 0.005 kWh/d Assuming no recirculation to the tank
Operation at cross-flowrate 140 L/h (flow rate
Pump 2 (Recirc.) 1.05 0.14 0.6 0.077 kWh/d and pressure drop from preliminary study)
Total 0.082 kWh/d Industrial ratio ==> 3 kWh/m3 (or lower) =30
Permeate 9.7 kWh/m3 0.3 kWh/d
0.013 kWh/L 0.047 kWh/L

TOTAL Cumulative Energy Demand Pilot scale Industrial scale

0.70 kWh/p·d 1.00 kWh/p·d
Total hardware 255 kWh/p·y 364 kWh/p·y
Total hardware 0.11 kWh/L 0.15 kWh/L
Total chemicals 167 kWh/p·y
Total chemicals 0.07 kWh/L
0.18 kWh/L 0.23 kWh/L
Estimated total 0.2 kWh/L

S20
Table D.2: Overview of the theoretical energy balance and assumptions. CED: cumulative energy demand

Chemicals Transport
Consumption kg/p.y kWh/kg Ref kWh/p.y kg/L CED (MJ/kg) kWh/kg kWh/p.y. kWh/L (kWh)
NaOH Urine 13 2 [1] 26 0.005597 19 5.28 68.61 0.029537
NaOH GW 7 2 [1] 14 0.003014 19 5.28 36.94 0.015905
HCl 3 4.81 [2] 14 0.001292 14.50 4.03 12.08 0.005202
Oxonia (0,1
%vv) 10 4 [3] 0.04 0.004305 0.02 0.01 0.06 2.52E-05
O2 9 15.88 [5] 147 0.004
Total 33 202 0.014207 Total 118 0.05 3.575
Production
NO3 9.6 3.61 [4] 35 0.004133 15.89 4.41 42.37 0.018242 1.040
2- +
Ca3(PO4)2, NH3, SO4 , and K were produced in neglectable quantities, but may be useful as fertilizer
Total (saved) 36 Total (saved) 44 0.02
Total chemicals 167 kWh/p·y
Total chemicals 0.07 kWh/L

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