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Progress Report
Partitioning Evapotranspiration into Evaporation and Transpiration fluxes
using Stable Isotopes of Oxygen and Hydrogen
March 29, 2023
Presented
by
Pankaj Kumar Thakur
(Project Associate-I) GWHD
National Institute of Hydrology,
Roorkee (Uttarakhand)
Under the supervision
of
Dr. Gopal Krishan
(Principal Investigator)
Scientist ‘D’ GWHD
National Institute of Hydrology,
Roorkee (Uttarakhand)
Content
Soil Water Extraction:
Azeotropic Distillation
Simple, inexpensive, fast and widely usable..
 Can be used for soil of almost
any type and grain size.
 Apparatus (Dean-Stark) has no
memory effect.
 Reagents (toluene/kerosene &
wax) do not affect isotopic
composition of soil water.
 Good Accuracy (±2%) for >3%
water content
• First used by R.M.
Brown and G.B. Allison
in the late 1970s and
was adapted from
Dewar and McDonald
(1961).
We chose Azeotropic Distillation using Standard Dean-
Stark Apparatus for Soil Water Extraction,
Because…
Tested (Revesz and Woods, 1990)
a) Different soil types
b) Variation in soil/toluene ratio
c) Variation in grain size of the soil
d) Memory effect between successive
samples
e) Variability of water content
substitution of kerosene (b.p. 175-
245°C) for toluene
f) Dependence on the isotopic
composition of the soil water
Standard Dean-Stark Apparatus
Source: Sunshine Scientific
Equipments
Conical Flask
(500 ml capacity)
Soil Sampling
Condenser
>90°C
Heating mantle
Sample collection
𝑯𝟐𝑶 +
Principle
Azeotropic mixture
@ 84.1°C
Completely immiscible at
ambient temperature
B.P. = 100°C
Density = 1
gm/cc
B.P. = 110°C
Density = 0.867
gm/cc
Traces of Toluene can
be separated by
adding wax
First, the water content of the soil is determined by weighing, drying
and reweighing a small aliquot of the soil sample.
Appropriate amount of soil sample is taken in the conical flask.
Enough toluene is added so that the soil remains covered throughout
the entire distillation process.
Procedure
Discussion
Test 1: Heating mantle were calibrated for different
temperature
Result: Temperature could not be fixed, so high traces of
toluene came-up with water.
Test 2: Heating mantle was replaced with digital Hot Plate.
Result: Still unable control the required temperature and
therefore high concertation of toluene received with water.
Test 3: Different proportion/ratio of toluene and soil sample
were taken for azeotropic distillation.
Result: Insignificant.
Conclusive Remark
Unable to extract water from soil, effectively using Azeotropic Distillation
and further improvement is needed…
Coating the condenser and the funnel with a solution of
dimethyldichlorosilane compound to change the surface from
hydrophilic to hydrophobic.
 To remove traces of toluene from collected water sample wax would
be used.
 Replacement of toluene by Kerosene/𝐶𝐶𝑙4/Ethanol/Benzine or any
other reagent.
Replacement of heating mantle or Hot plat by Sand Bath or Water
Bath to perform the distillation in controlled temperature.
 Use of Centrifuge method to extract water from soil.
To be carried out…
References
 Jusserand, C., 1980. Extraction de l'eau interstitielle des sediments et des sols. Catena, 7:87 96.
 Stewart, G.L., 1972. Clay-water interaction, the behavior of 3H and 2H in absorbed water, and the isotope effect. J.
Soil Sci. Soc. Am., 36: 421-426.
 Orlowski, N., Pratt, D. L., & McDonnell, J. J. (2016). Intercomparison of soil pore water extraction methods for
stable isotope analysis. Hydrological Processes, 30(19), 3434-3449.
 Allison, G.B. and Barnes, C.J., 1983. Estimation of evaporation from non-vegetated surfaces using natural
deuterium. Nature, 301: 143-145.
 Dewar, W.A. and McDonald, P., 1961. Determination of dry matter in silage by distillation with toluene. J. Sci. Food
Agric., 12: 790-795.
 Revesz, K. and Woods, P.H., 1990. A method to extract soil water for stable isotope analysis. J. Hydrol., 115: 397-
406.
 Millar, C., Pratt, D., Schneider, D.J., and McDonnell, J.J.: A comparison of extraction systems for plant water stable
isotope analysis, Rapid Commun. Mass Spectrom., 32, 1031-1044, https://doi.org/10.1002/rcm.8136, 2018
 Zuecco, G., Amin, A., Frentress, J., Engel, M., Marchina, C., Anfodillo, T., Borga, M., Carraro, V., Scandellari, F.,
Tagliavini, M. and Zanotelli, D., 2022. A comparative study of plant water extraction methods for isotopic analyses:
Scholander-type pressure chamber vs. cryogenic vacuum distillation. Hydrology and Earth System Sciences, 26(13),
pp.3673-3689.
Thank you!
Thanks for your gift of time…

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Partitioning Evapotranspiration into Evaporation and Transpiration fluxes using Stable Isotopes of Oxygen and Hydrogen

  • 1. Progress Report Partitioning Evapotranspiration into Evaporation and Transpiration fluxes using Stable Isotopes of Oxygen and Hydrogen March 29, 2023 Presented by Pankaj Kumar Thakur (Project Associate-I) GWHD National Institute of Hydrology, Roorkee (Uttarakhand) Under the supervision of Dr. Gopal Krishan (Principal Investigator) Scientist ‘D’ GWHD National Institute of Hydrology, Roorkee (Uttarakhand)
  • 2. Content Soil Water Extraction: Azeotropic Distillation Simple, inexpensive, fast and widely usable..
  • 3.  Can be used for soil of almost any type and grain size.  Apparatus (Dean-Stark) has no memory effect.  Reagents (toluene/kerosene & wax) do not affect isotopic composition of soil water.  Good Accuracy (±2%) for >3% water content • First used by R.M. Brown and G.B. Allison in the late 1970s and was adapted from Dewar and McDonald (1961). We chose Azeotropic Distillation using Standard Dean- Stark Apparatus for Soil Water Extraction, Because… Tested (Revesz and Woods, 1990) a) Different soil types b) Variation in soil/toluene ratio c) Variation in grain size of the soil d) Memory effect between successive samples e) Variability of water content substitution of kerosene (b.p. 175- 245°C) for toluene f) Dependence on the isotopic composition of the soil water
  • 4. Standard Dean-Stark Apparatus Source: Sunshine Scientific Equipments Conical Flask (500 ml capacity) Soil Sampling Condenser >90°C Heating mantle Sample collection
  • 5. 𝑯𝟐𝑶 + Principle Azeotropic mixture @ 84.1°C Completely immiscible at ambient temperature B.P. = 100°C Density = 1 gm/cc B.P. = 110°C Density = 0.867 gm/cc Traces of Toluene can be separated by adding wax
  • 6. First, the water content of the soil is determined by weighing, drying and reweighing a small aliquot of the soil sample. Appropriate amount of soil sample is taken in the conical flask. Enough toluene is added so that the soil remains covered throughout the entire distillation process. Procedure
  • 7. Discussion Test 1: Heating mantle were calibrated for different temperature Result: Temperature could not be fixed, so high traces of toluene came-up with water. Test 2: Heating mantle was replaced with digital Hot Plate. Result: Still unable control the required temperature and therefore high concertation of toluene received with water. Test 3: Different proportion/ratio of toluene and soil sample were taken for azeotropic distillation. Result: Insignificant. Conclusive Remark Unable to extract water from soil, effectively using Azeotropic Distillation and further improvement is needed…
  • 8. Coating the condenser and the funnel with a solution of dimethyldichlorosilane compound to change the surface from hydrophilic to hydrophobic.  To remove traces of toluene from collected water sample wax would be used.  Replacement of toluene by Kerosene/𝐶𝐶𝑙4/Ethanol/Benzine or any other reagent. Replacement of heating mantle or Hot plat by Sand Bath or Water Bath to perform the distillation in controlled temperature.  Use of Centrifuge method to extract water from soil. To be carried out…
  • 9. References  Jusserand, C., 1980. Extraction de l'eau interstitielle des sediments et des sols. Catena, 7:87 96.  Stewart, G.L., 1972. Clay-water interaction, the behavior of 3H and 2H in absorbed water, and the isotope effect. J. Soil Sci. Soc. Am., 36: 421-426.  Orlowski, N., Pratt, D. L., & McDonnell, J. J. (2016). Intercomparison of soil pore water extraction methods for stable isotope analysis. Hydrological Processes, 30(19), 3434-3449.  Allison, G.B. and Barnes, C.J., 1983. Estimation of evaporation from non-vegetated surfaces using natural deuterium. Nature, 301: 143-145.  Dewar, W.A. and McDonald, P., 1961. Determination of dry matter in silage by distillation with toluene. J. Sci. Food Agric., 12: 790-795.  Revesz, K. and Woods, P.H., 1990. A method to extract soil water for stable isotope analysis. J. Hydrol., 115: 397- 406.  Millar, C., Pratt, D., Schneider, D.J., and McDonnell, J.J.: A comparison of extraction systems for plant water stable isotope analysis, Rapid Commun. Mass Spectrom., 32, 1031-1044, https://doi.org/10.1002/rcm.8136, 2018  Zuecco, G., Amin, A., Frentress, J., Engel, M., Marchina, C., Anfodillo, T., Borga, M., Carraro, V., Scandellari, F., Tagliavini, M. and Zanotelli, D., 2022. A comparative study of plant water extraction methods for isotopic analyses: Scholander-type pressure chamber vs. cryogenic vacuum distillation. Hydrology and Earth System Sciences, 26(13), pp.3673-3689.
  • 10. Thank you! Thanks for your gift of time…