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Total (Organic) Carbon, Nitrogen and Sulfur Elemental
Analysis of Soils and Eluates
Webinar
Dr. Dominik Margraf
Agenda
Introduction1
CN(S) Analysis of Soils2
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Elemental Analysis of Soil
6/11/2015 Soil and Eluates | Webinar
“Studies predict the world population to increase beyond 8.2 billion within
the next 10 years, demanding ways to optimise the use of agrarian land
to provide a larger food supply.”
• Agricultural science and analytics are the key to
manage the fundamental growing demands for
food, feed and water.
www.gov.uk
Elemental Analysis of Soil
6/11/2015 Soil and Eluates | Webinar
• Carbon and nitrogen are important drivers in the
element cycling of soils.
• Elemental analysis provides essential information
about microbiological activity and organic matter,
enabling a selective fertilization of arable land.
• Understanding the carbon-nitrogen ratio of soil is
therefore of utmost importance.
Agenda
Introduction1
CN(S) Analysis of Soils2
Sample Preparation2.1
Combustion Chemistry2.2
Gas Separation and Detection2.3
runAr Option: Argon vs. Helium as Carrier Gas2.4
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Agenda
Introduction1
CN(S) Analysis of Soils2
Sample Preparation2.1
Combustion Chemistry2.2
Gas Separation and Detection2.3
runAr Option: Argon vs. Helium as Carrier Gas2.4
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Challenges in Sample Preparation
6/11/2015 Soil and Eluates | Webinar
• inhomogeneities within a sample
may cause large deviations
between two measurements
• solution
• milling
• grinding
• large representative sample
– multi gram scale
Total (Organic) Carbon, Nitrogen and Sulfur Elemental Analysis of Soils and Eluates
vario MAX cube CN(S)– Dedicated Soil Analyzer
6/11/2015 Soil and Eluates | Webinar
• Sample is simply filled in upright,
reusable crucible
• Up to 5 g mineral sample
• Up to 5 ml liquid
• Up to 1 g organic sample
vario MAX cube CN(S) – Dedicated Soil Analyzer
6/11/2015 Soil and Eluates | Webinar
• Automatic sample introduction via robotic arm
• soil samples form large amount of ashes
• time saving automatic ash removal
• high lab efficiency
• 90 position carousel as standard
• unattended 24/7 operation
• Robust, maintenance-free mechanical design
Agenda
Introduction1
CN(S) Analysis of Soils2
Sample Preparation2.1
Combustion Chemistry2.2
Gas Separation and Detection2.3
runAr Option: Argon vs. Helium as Carrier Gas2.4
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Combustion According to Dumas Method
6/11/2015 Soil and Eluates | Webinar
Organic compounds consists of C, H, N, O, S, Cl …
Combustion in O2 on oxygen donor at ~ 900°C
O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl...
Typical problem of macro analysis (50 – 5000 mg)
Combustion tube
Unique Post-Combustion
6/11/2015 Soil and Eluates | Webinar
Organic compounds consists of C, H, N, O, S, Cl …
Combustion in O2 on oxygen donor at ~ 900°C
O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl...
post-combustion on catalyst (and H2O removal)
O2, N2, NOX, CO2, SO2, HCl...
Post-combustion tube
Unique Reduction Using Tungsten
6/11/2015 Soil and Eluates | Webinar
• Reduction tube for binding of excess oxygen
• Effective tungsten for CN mode: W  WO3
• one tungsten atom reacts with three oxygen atoms
• SO2 is bound on tungsten
• for CNS mode tungsten has to be replaced with copper
• Quantitative reduction of NOx to N2
• only N2, CO2 (and SO2 in CNS mode) exit reduction
tube
tungsten
Reduction tube
Agenda
Introduction1
CN(S) Analysis of Soils2
Sample Preparation2.1
Combustion Chemistry2.2
Gas Separation and Detection2.3
runAr Option: Argon vs. Helium as Carrier Gas2.4
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Advanced Purge and Trap Technology
• Prior to detection gases are separated
• unique Advanced Purge and Trap Technology
• absorption column specifically removes CO2 from gas stream and N2 is
being detected
• additional column in CNS mode to specifically absorb SO2
• CO2 absorption column is heated to desorption temperature
• all CO2 is released at one controlled point in time
– focused, sharp peaks without overlap
– separation of C/N ratios up to 7000 : 1
6/11/2015 Soil and Eluates | Webinar
Thermal Conductivity Detector with 10 Year Warranty
• measuring principle
• difference in thermoconductivity
of gases causes detectable
temperature difference
6/11/2015 Soil and Eluates | Webinar
carrier gas +
analyte gas
carrier gas
© http://wikipedia.de
gas thermoconductivity
[W/mK)]
H2 0,186
He 0,1567
Ar 0,0179
N2 0,0260
CO2 0,0168
Why Alternatives to Helium?
6/11/2015 Soil and Eluates | Webinar
• helium is a limited resource
• Nobel Laureate Robert Richardson expects world
supplies to last another 40 years and suggests a
150-fold increase of the helium price
• USA will sell their helium reserves
Robert Richardson
Nobel Laureate in Physics 1996
Argon as Carrier Gas
• difference between argon and e.g.
CO2 large enough?
6/11/2015 Soil and Eluates | Webinar
carrier gas +
analyte gas
carrier gas
© http://wikipedia.de
gas thermoconductivity
[W/mK)]
H2 0,186
He 0,1567
Ar 0,0179
N2 0,0260
CO2 0,0168
Agenda
Introduction1
CN(S) Analysis of Soils2
Sample Preparation2.1
Combustion Chemistry2.2
Gas Separation and Detection2.3
runAr Option: Argon vs. Helium as Carrier Gas2.4
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
runAr Option Experimental Set-up
6/11/2015 Soil and Eluates | Webinar
• instrument: vario MAX cube CN in
helium or argon mode
• samples: certified standard soils
• “sandy”, “loamy”, “silty”, “clay”,
“chalky”
• sample weight: approx. 1000 mg
• triple determination
• three independent measuring days
• identical operator
runAr Option Experimental Results Nitrogen
6/11/2015 Soil and Eluates | Webinar
y = 1,014x + 1,554
R² = 0,99
0
50
100
150
200
250
300
350
400
0 100 200 300 400
ARGONCARRIERGAS;nitrogencontent
[ppm]
HELIUM CARRIER GAS; nitrogen content [ppm]
NITROGEN DAY 1
sandy
silty
loamy
clay
chalky
• excellent
experimental
correlation
• Day 2 and Day 3
summarized as table
• error bars indicate
3 x abs. SD (99%
confidence)
• for further information please
refer to
D. Margraf, Argon as Carrier Gas in CN
elemental analysis of soils, Bulletin of the
Swiss Chemical Soil Society, ISSN 1420-
6773
runAr Option Experimental Results Carbon
6/11/2015 Soil and Eluates | Webinar
• excellent
experimental
correlation
• Day 2 and Day 3
summarized as table
• error bars indicate
3 x abs. SD (99%
confidence)
• for further information please
refer to
D. Margraf, Argon as Carrier Gas in CN
elemental analysis of soils, Bulletin of the
Swiss Chemical Soil Society, ISSN 1420-
6773
y = 1,000x + 63,716
R² = 0,999
0
1000
2000
3000
4000
5000
6000
0 1000 2000 3000 4000 5000 6000
ARGONCARRIERGAS;carboncontent[ppm]
HELIUM CARRIER GAS; carbon content [ppm}
CARBON DAY 1
sandy
clay; silty
loamy
chalky
runAr Option Summary Experimental Results CN
6/11/2015 Soil and Eluates | Webinar
• mean experimental results of three
independent measuring days each
run in triple determination
• exp. results ± 3 x abs. SD at 99%
confidence interval
• Argon and helium based reveal
excellent agreement within the
experimental error
D. Margraf, Argon as Carrier Gas in CN elemental analysis of soils,
Bulletin of the Swiss Chemical Soil Society, ISSN 1420-6773
sample nitrogen
[ppm]
carbon
[ppm]
Helium Argon Helium Argon
Chalky 364 ± 8 370±9 5330±40 5370±50
Clay 188 ± 6 190±20 2080±40 2190±40
Loamy 255 ± 1 260±8 2640±20 2690±50
Sandy 60 ± 10 60±2 820±10 820±30
Silty 169 ± 2 180±10 2120±20 2180±60
runAr option Experimental Results CNS
6/11/2015 Soil and Eluates | Webinar
• Sample amount: 250 – 850 mg
• triple determination
• exp. results ± abs. SD
• runAr also suitable for a variety of
matrices
C [%] N [%] S [%]
Soil
helium
argon
1.78 ± 0.01
1.78 ± 0.02
0.17 ± 0.001
0.18 ± 0.009
0.02 ± 0.001
0.01 ± 0.002
Maize
kernel
helium
argon
43.2 ± 0.02
43.2 ± 0.01
2.66 ± 0.01
2.75 ± 0.01
0.22 ± 0.01
0.24 ± 0.02
Wheat
flour
helium
argon
40.7 ± 0.04
40.5 ± 0.02
1.13 ± 0.002
1.17 ± 0.004
0.08 ± 0.005
0.08 ± 0.009
vario MAX cube – runAr Technology
6/11/2015 Soil and Eluates | Webinar
• Use of Argon has been scientifically proven for
the analysis of soils
• No time-consuming retrofit needed
• Argon instead of helium as a carrier gas further
reduces cost-per-sample
• approx. 10% savings with runAr option
based on German gas prices
• runAr option is free of charge
vario MAX cube – Analysis of Soil
6/11/2015 Soil and Eluates | Webinar
• Soil from banana plantation in Ecuador
• Sample weight: 1000 mg
• CN mode
• exp. results ± abs. SD
Sample C
[%]
N
[%]
C/N
ratio
Fluvisol Ah horizon 1.488 ± 0.003 0.051 ± 0.001 29.2
Fluvisol B horizon 0.670 ± 0.001 0.065 ±0.001 10.3
Fluvisol B/C horizon 1.921 ± 0.004 0.024 ± 0.001 80.0
vario MAX cube – Analysis of Soil
6/11/2015 Soil and Eluates | Webinar
• Soil from a pasture Southwest USA
• Sample weight: 550 - 750 mg
• six-fold determination
• 1 : 1 addition of WO3
Sample C
[%]
N
[%]
S
[%]
Cambisol Ah horizon 1.112 ± 0.001 0.104 ± 0.001 0.0229 ± 0.0005
Cambisol B horizon 1.782 ± 0.010 0.168 ±0.001 0.0231 ± 0.0004
Cambisol Cw horizon 0.335 ± 0.013 0.0532 ± 0.027 0.0094 ± 0.003
Calcisol B horizon 4.187 ± 0.015 0.051 ± 0.001 0.0873 ± 0.0028
vario MAX cube – TC and TOC Analysis
6/11/2015 Soil and Eluates | Webinar
• full agreement with ISO 10694
• triple determination
• exp. results ± abs. SD
• TC sample weight: 1000 mg
• TOC sample weight: 300 mg
• external acidification with 10% HCl
in silver foil cups
• dried at 80°C in silver foil cups
• silver foil cups simply placed in
crucible
• TIC accessible by difference
TC [%] TOC [%]
Soil 1 2.91 ± 0.08 1.33 ± 0.01
Soil 2 2.61 ± 0.06 2.34 ± 0.02
Soil 3 0.525 ± 0.013 0.500 ± 0.015
Soil 4 9.37 ± 0.05 8.89 ± 0.01
Soil 5 1.59 ± 0.04 1.36 ± 0.04
Soil 6 0.685 ± 0.023 0.640 ± 0.008
Fertilizer...
6/11/2015 Soil and Eluates | Webinar
Agenda
Introduction1
CN(S) Analysis of Soils2
TOC Analysis of Soils and Soil Eluates3
6/11/2015 Soil and Eluates | Webinar
Total (Organic) Carbon, Nitrogen and Sulfur Elemental Analysis of Soils and Eluates
Scope of Parameters
TC = TOC + TIC
TC = NPOC + POC + TIC
TC=Total Carbon
TOC=Total Organic Carbon
TIC=Total Inorganic Carbon
NPOC=Non Purgeable Organic Carbon
POC=Purgeable Organic Carbon
TNb=Total bound Nitrogen
6/11/2015 Soil and Eluates | Webinar
Integrated Autosampler
6/11/2015 Soil and Eluates | Webinar
Automatic sample dosing, automatic sample
changing
• 32 position sampler, 40 ml vials, accepts TOC
certified vials, stirrable, automatic external
acidification for NPOC determination
• 50 position sampler, 12 ml vials, stirrable,
automatic external acidification for NPOC
determination
• 80 position sampler, 7 ml vials, manual external
acidification for NPOC determination
• Suspension method possible
Real High Temperature Combustion
6/11/2015 Soil and Eluates | Webinar
• Temperature programmable up to 1100°C
• High precision sample dosing
• Every part easily acccessible from the front side
• No tools required for maintenance work
• Automatic observation of maintenance intervals
Matrix Separation
6/11/2015 Soil and Eluates | Webinar
Ash finger collects
salt, particles
Catalyst remains
clean
Nitrogen Analysis
• TNb: Total bound Nitrogen, includes all kinds of nitrogen compounds
except N2
• Nitrogen is converted to NO, this reaction requires high temperatures
(< 750°C not sufficient for full recovery)
• 3 detectors available
• IR: maintenance-free, high dynamic range
• Electrochemical cell: high sensitivity, most economic solution
• Chemoluminescence Detector: high sensitivity
6/11/2015 Soil and Eluates | Webinar
Soil Eluates
6/11/2015 Soil and Eluates | Webinar
• Challenge: high salt content from eluent
• Injection volume 0.5ml, combustion
temperature 850°C; automatic external
acidification
• Simultaneous TNb and TOC determination
• No clogging observed
TOC in eluates
TOC
[mg/l]
SDr
[%]
TNb
[mg/l]
SDr
[%]
Soil eluate 1
CaCl2 11 g/l
6.67 4.0 na na
Soil eluate 2
K2SO4 87 g/l
71.1 1.78 12.5 11.2
Soil eluate 3
K2SO4 87 mg/l
136 3.53 27.2 7.70
Suspended Solids
6/11/2015 Soil and Eluates | Webinar
• Challenge: High Amount of Non-
Combustible Particles
• Pretreatment by Ultraturrax, Injection
volume 0.2ml, combustion temperature
850°C, Dilution 1:1000
• No sedimentation observed
• no trend in NPOC
NPOC in solids
(suspension method)
Soil
[w-%]
Theor. Value: 0,37%
Sediment
[w-%]
1st Injection 0,377 2,32
2nd Injection 0,362 2,26
3rd Injection 0,391 2,28
Mean 0,377 2,29
SD 0,014 0,03
SDr 3,86% 1,31%
Fully Automated Analysis of Solid Samples
6/11/2015 Soil and Eluates | Webinar
• Only TOC in water analyzer worldwide
with automatic sample feeder for solids
• Sample feeding by reliable ball valve
technique
• Sample carousel with 80-120 positions
• Solids expansion kit for carbon amounts
up to 20mg C abs.
TOC Determination in Solid Samples
6/11/2015 Soil and Eluates | Webinar
• Sample weight approx. 100 mg
• Solid sample wrapped in silver foil,
externally acidified and dried
• Triple determination
• Combustion temperature 900°C
TOC in solids Surface soil
[w-%]
Clay
[w-%]
Theor. Value:
0.139 w-%
1st det. 4,69 0,139
2nd det. 4,77 0,137
3rd det. 4,80 0,142
Mean 4,75 0,140
SD 0,05 0,003
SDr 1,1% 1,85%
Questions?
• Please use chat window
• Dr. Dominik Margraf
• margraf@elementar.de
6/11/2015 Soil and Eluates | Webinar

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  • 1. Total (Organic) Carbon, Nitrogen and Sulfur Elemental Analysis of Soils and Eluates Webinar Dr. Dominik Margraf
  • 2. Agenda Introduction1 CN(S) Analysis of Soils2 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 3. Elemental Analysis of Soil 6/11/2015 Soil and Eluates | Webinar “Studies predict the world population to increase beyond 8.2 billion within the next 10 years, demanding ways to optimise the use of agrarian land to provide a larger food supply.” • Agricultural science and analytics are the key to manage the fundamental growing demands for food, feed and water. www.gov.uk
  • 4. Elemental Analysis of Soil 6/11/2015 Soil and Eluates | Webinar • Carbon and nitrogen are important drivers in the element cycling of soils. • Elemental analysis provides essential information about microbiological activity and organic matter, enabling a selective fertilization of arable land. • Understanding the carbon-nitrogen ratio of soil is therefore of utmost importance.
  • 5. Agenda Introduction1 CN(S) Analysis of Soils2 Sample Preparation2.1 Combustion Chemistry2.2 Gas Separation and Detection2.3 runAr Option: Argon vs. Helium as Carrier Gas2.4 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 6. Agenda Introduction1 CN(S) Analysis of Soils2 Sample Preparation2.1 Combustion Chemistry2.2 Gas Separation and Detection2.3 runAr Option: Argon vs. Helium as Carrier Gas2.4 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 7. Challenges in Sample Preparation 6/11/2015 Soil and Eluates | Webinar • inhomogeneities within a sample may cause large deviations between two measurements • solution • milling • grinding • large representative sample – multi gram scale
  • 9. vario MAX cube CN(S)– Dedicated Soil Analyzer 6/11/2015 Soil and Eluates | Webinar • Sample is simply filled in upright, reusable crucible • Up to 5 g mineral sample • Up to 5 ml liquid • Up to 1 g organic sample
  • 10. vario MAX cube CN(S) – Dedicated Soil Analyzer 6/11/2015 Soil and Eluates | Webinar • Automatic sample introduction via robotic arm • soil samples form large amount of ashes • time saving automatic ash removal • high lab efficiency • 90 position carousel as standard • unattended 24/7 operation • Robust, maintenance-free mechanical design
  • 11. Agenda Introduction1 CN(S) Analysis of Soils2 Sample Preparation2.1 Combustion Chemistry2.2 Gas Separation and Detection2.3 runAr Option: Argon vs. Helium as Carrier Gas2.4 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 12. Combustion According to Dumas Method 6/11/2015 Soil and Eluates | Webinar Organic compounds consists of C, H, N, O, S, Cl … Combustion in O2 on oxygen donor at ~ 900°C O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl... Typical problem of macro analysis (50 – 5000 mg) Combustion tube
  • 13. Unique Post-Combustion 6/11/2015 Soil and Eluates | Webinar Organic compounds consists of C, H, N, O, S, Cl … Combustion in O2 on oxygen donor at ~ 900°C O2, N2, NOx, CO2 CO, CH4, SO2, H2O, HCl... post-combustion on catalyst (and H2O removal) O2, N2, NOX, CO2, SO2, HCl... Post-combustion tube
  • 14. Unique Reduction Using Tungsten 6/11/2015 Soil and Eluates | Webinar • Reduction tube for binding of excess oxygen • Effective tungsten for CN mode: W  WO3 • one tungsten atom reacts with three oxygen atoms • SO2 is bound on tungsten • for CNS mode tungsten has to be replaced with copper • Quantitative reduction of NOx to N2 • only N2, CO2 (and SO2 in CNS mode) exit reduction tube tungsten Reduction tube
  • 15. Agenda Introduction1 CN(S) Analysis of Soils2 Sample Preparation2.1 Combustion Chemistry2.2 Gas Separation and Detection2.3 runAr Option: Argon vs. Helium as Carrier Gas2.4 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 16. Advanced Purge and Trap Technology • Prior to detection gases are separated • unique Advanced Purge and Trap Technology • absorption column specifically removes CO2 from gas stream and N2 is being detected • additional column in CNS mode to specifically absorb SO2 • CO2 absorption column is heated to desorption temperature • all CO2 is released at one controlled point in time – focused, sharp peaks without overlap – separation of C/N ratios up to 7000 : 1 6/11/2015 Soil and Eluates | Webinar
  • 17. Thermal Conductivity Detector with 10 Year Warranty • measuring principle • difference in thermoconductivity of gases causes detectable temperature difference 6/11/2015 Soil and Eluates | Webinar carrier gas + analyte gas carrier gas © http://wikipedia.de gas thermoconductivity [W/mK)] H2 0,186 He 0,1567 Ar 0,0179 N2 0,0260 CO2 0,0168
  • 18. Why Alternatives to Helium? 6/11/2015 Soil and Eluates | Webinar • helium is a limited resource • Nobel Laureate Robert Richardson expects world supplies to last another 40 years and suggests a 150-fold increase of the helium price • USA will sell their helium reserves Robert Richardson Nobel Laureate in Physics 1996
  • 19. Argon as Carrier Gas • difference between argon and e.g. CO2 large enough? 6/11/2015 Soil and Eluates | Webinar carrier gas + analyte gas carrier gas © http://wikipedia.de gas thermoconductivity [W/mK)] H2 0,186 He 0,1567 Ar 0,0179 N2 0,0260 CO2 0,0168
  • 20. Agenda Introduction1 CN(S) Analysis of Soils2 Sample Preparation2.1 Combustion Chemistry2.2 Gas Separation and Detection2.3 runAr Option: Argon vs. Helium as Carrier Gas2.4 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 21. runAr Option Experimental Set-up 6/11/2015 Soil and Eluates | Webinar • instrument: vario MAX cube CN in helium or argon mode • samples: certified standard soils • “sandy”, “loamy”, “silty”, “clay”, “chalky” • sample weight: approx. 1000 mg • triple determination • three independent measuring days • identical operator
  • 22. runAr Option Experimental Results Nitrogen 6/11/2015 Soil and Eluates | Webinar y = 1,014x + 1,554 R² = 0,99 0 50 100 150 200 250 300 350 400 0 100 200 300 400 ARGONCARRIERGAS;nitrogencontent [ppm] HELIUM CARRIER GAS; nitrogen content [ppm] NITROGEN DAY 1 sandy silty loamy clay chalky • excellent experimental correlation • Day 2 and Day 3 summarized as table • error bars indicate 3 x abs. SD (99% confidence) • for further information please refer to D. Margraf, Argon as Carrier Gas in CN elemental analysis of soils, Bulletin of the Swiss Chemical Soil Society, ISSN 1420- 6773
  • 23. runAr Option Experimental Results Carbon 6/11/2015 Soil and Eluates | Webinar • excellent experimental correlation • Day 2 and Day 3 summarized as table • error bars indicate 3 x abs. SD (99% confidence) • for further information please refer to D. Margraf, Argon as Carrier Gas in CN elemental analysis of soils, Bulletin of the Swiss Chemical Soil Society, ISSN 1420- 6773 y = 1,000x + 63,716 R² = 0,999 0 1000 2000 3000 4000 5000 6000 0 1000 2000 3000 4000 5000 6000 ARGONCARRIERGAS;carboncontent[ppm] HELIUM CARRIER GAS; carbon content [ppm} CARBON DAY 1 sandy clay; silty loamy chalky
  • 24. runAr Option Summary Experimental Results CN 6/11/2015 Soil and Eluates | Webinar • mean experimental results of three independent measuring days each run in triple determination • exp. results ± 3 x abs. SD at 99% confidence interval • Argon and helium based reveal excellent agreement within the experimental error D. Margraf, Argon as Carrier Gas in CN elemental analysis of soils, Bulletin of the Swiss Chemical Soil Society, ISSN 1420-6773 sample nitrogen [ppm] carbon [ppm] Helium Argon Helium Argon Chalky 364 ± 8 370±9 5330±40 5370±50 Clay 188 ± 6 190±20 2080±40 2190±40 Loamy 255 ± 1 260±8 2640±20 2690±50 Sandy 60 ± 10 60±2 820±10 820±30 Silty 169 ± 2 180±10 2120±20 2180±60
  • 25. runAr option Experimental Results CNS 6/11/2015 Soil and Eluates | Webinar • Sample amount: 250 – 850 mg • triple determination • exp. results ± abs. SD • runAr also suitable for a variety of matrices C [%] N [%] S [%] Soil helium argon 1.78 ± 0.01 1.78 ± 0.02 0.17 ± 0.001 0.18 ± 0.009 0.02 ± 0.001 0.01 ± 0.002 Maize kernel helium argon 43.2 ± 0.02 43.2 ± 0.01 2.66 ± 0.01 2.75 ± 0.01 0.22 ± 0.01 0.24 ± 0.02 Wheat flour helium argon 40.7 ± 0.04 40.5 ± 0.02 1.13 ± 0.002 1.17 ± 0.004 0.08 ± 0.005 0.08 ± 0.009
  • 26. vario MAX cube – runAr Technology 6/11/2015 Soil and Eluates | Webinar • Use of Argon has been scientifically proven for the analysis of soils • No time-consuming retrofit needed • Argon instead of helium as a carrier gas further reduces cost-per-sample • approx. 10% savings with runAr option based on German gas prices • runAr option is free of charge
  • 27. vario MAX cube – Analysis of Soil 6/11/2015 Soil and Eluates | Webinar • Soil from banana plantation in Ecuador • Sample weight: 1000 mg • CN mode • exp. results ± abs. SD Sample C [%] N [%] C/N ratio Fluvisol Ah horizon 1.488 ± 0.003 0.051 ± 0.001 29.2 Fluvisol B horizon 0.670 ± 0.001 0.065 ±0.001 10.3 Fluvisol B/C horizon 1.921 ± 0.004 0.024 ± 0.001 80.0
  • 28. vario MAX cube – Analysis of Soil 6/11/2015 Soil and Eluates | Webinar • Soil from a pasture Southwest USA • Sample weight: 550 - 750 mg • six-fold determination • 1 : 1 addition of WO3 Sample C [%] N [%] S [%] Cambisol Ah horizon 1.112 ± 0.001 0.104 ± 0.001 0.0229 ± 0.0005 Cambisol B horizon 1.782 ± 0.010 0.168 ±0.001 0.0231 ± 0.0004 Cambisol Cw horizon 0.335 ± 0.013 0.0532 ± 0.027 0.0094 ± 0.003 Calcisol B horizon 4.187 ± 0.015 0.051 ± 0.001 0.0873 ± 0.0028
  • 29. vario MAX cube – TC and TOC Analysis 6/11/2015 Soil and Eluates | Webinar • full agreement with ISO 10694 • triple determination • exp. results ± abs. SD • TC sample weight: 1000 mg • TOC sample weight: 300 mg • external acidification with 10% HCl in silver foil cups • dried at 80°C in silver foil cups • silver foil cups simply placed in crucible • TIC accessible by difference TC [%] TOC [%] Soil 1 2.91 ± 0.08 1.33 ± 0.01 Soil 2 2.61 ± 0.06 2.34 ± 0.02 Soil 3 0.525 ± 0.013 0.500 ± 0.015 Soil 4 9.37 ± 0.05 8.89 ± 0.01 Soil 5 1.59 ± 0.04 1.36 ± 0.04 Soil 6 0.685 ± 0.023 0.640 ± 0.008
  • 30. Fertilizer... 6/11/2015 Soil and Eluates | Webinar
  • 31. Agenda Introduction1 CN(S) Analysis of Soils2 TOC Analysis of Soils and Soil Eluates3 6/11/2015 Soil and Eluates | Webinar
  • 33. Scope of Parameters TC = TOC + TIC TC = NPOC + POC + TIC TC=Total Carbon TOC=Total Organic Carbon TIC=Total Inorganic Carbon NPOC=Non Purgeable Organic Carbon POC=Purgeable Organic Carbon TNb=Total bound Nitrogen 6/11/2015 Soil and Eluates | Webinar
  • 34. Integrated Autosampler 6/11/2015 Soil and Eluates | Webinar Automatic sample dosing, automatic sample changing • 32 position sampler, 40 ml vials, accepts TOC certified vials, stirrable, automatic external acidification for NPOC determination • 50 position sampler, 12 ml vials, stirrable, automatic external acidification for NPOC determination • 80 position sampler, 7 ml vials, manual external acidification for NPOC determination • Suspension method possible
  • 35. Real High Temperature Combustion 6/11/2015 Soil and Eluates | Webinar • Temperature programmable up to 1100°C • High precision sample dosing • Every part easily acccessible from the front side • No tools required for maintenance work • Automatic observation of maintenance intervals
  • 36. Matrix Separation 6/11/2015 Soil and Eluates | Webinar Ash finger collects salt, particles Catalyst remains clean
  • 37. Nitrogen Analysis • TNb: Total bound Nitrogen, includes all kinds of nitrogen compounds except N2 • Nitrogen is converted to NO, this reaction requires high temperatures (< 750°C not sufficient for full recovery) • 3 detectors available • IR: maintenance-free, high dynamic range • Electrochemical cell: high sensitivity, most economic solution • Chemoluminescence Detector: high sensitivity 6/11/2015 Soil and Eluates | Webinar
  • 38. Soil Eluates 6/11/2015 Soil and Eluates | Webinar • Challenge: high salt content from eluent • Injection volume 0.5ml, combustion temperature 850°C; automatic external acidification • Simultaneous TNb and TOC determination • No clogging observed TOC in eluates TOC [mg/l] SDr [%] TNb [mg/l] SDr [%] Soil eluate 1 CaCl2 11 g/l 6.67 4.0 na na Soil eluate 2 K2SO4 87 g/l 71.1 1.78 12.5 11.2 Soil eluate 3 K2SO4 87 mg/l 136 3.53 27.2 7.70
  • 39. Suspended Solids 6/11/2015 Soil and Eluates | Webinar • Challenge: High Amount of Non- Combustible Particles • Pretreatment by Ultraturrax, Injection volume 0.2ml, combustion temperature 850°C, Dilution 1:1000 • No sedimentation observed • no trend in NPOC NPOC in solids (suspension method) Soil [w-%] Theor. Value: 0,37% Sediment [w-%] 1st Injection 0,377 2,32 2nd Injection 0,362 2,26 3rd Injection 0,391 2,28 Mean 0,377 2,29 SD 0,014 0,03 SDr 3,86% 1,31%
  • 40. Fully Automated Analysis of Solid Samples 6/11/2015 Soil and Eluates | Webinar • Only TOC in water analyzer worldwide with automatic sample feeder for solids • Sample feeding by reliable ball valve technique • Sample carousel with 80-120 positions • Solids expansion kit for carbon amounts up to 20mg C abs.
  • 41. TOC Determination in Solid Samples 6/11/2015 Soil and Eluates | Webinar • Sample weight approx. 100 mg • Solid sample wrapped in silver foil, externally acidified and dried • Triple determination • Combustion temperature 900°C TOC in solids Surface soil [w-%] Clay [w-%] Theor. Value: 0.139 w-% 1st det. 4,69 0,139 2nd det. 4,77 0,137 3rd det. 4,80 0,142 Mean 4,75 0,140 SD 0,05 0,003 SDr 1,1% 1,85%
  • 42. Questions? • Please use chat window • Dr. Dominik Margraf • margraf@elementar.de 6/11/2015 Soil and Eluates | Webinar