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ACTIVE CARBON: EVALUATING
METHODOLOGY OF A
LABORATORY METHOD
SKYE WILLS
MICHEAL ROBOTHAM
CANDISS WILLIAMS
RICH FERGUSON
STEVE MONTEITH
ACTIVE CARBON
• Carbon that is oxidized in a dilute permanganate (KMnO4) solution
• Thought to be related to labile or ‘active’ forms of carbon
• Shown to be more sensitive to management than other measures of soil organic carbon
• Referred to more specifically as POX-C (Culman et al., 2012)
ACTIVE C IN SOIL SURVEY
• A study was conducted to determine the comparability between laboratory
and field methods (Stiles et al.,2011)
• NRCS-Soil Science Division has a program to measure dynamic soil properties
• Measure soil properties under multiple land use and/or management systems
• Kellogg Soil Survey Laboratory has been working to find consistent
repeatable methods that work for ALL soils
• Irregularities and inconsistencies have been noted by technicians
BASIC PROCEDURE
• Kellogg Soil Survey Laboratory
• Air Dry and Grind Soil to <2mm
• Weigh out sample
• Originally 5 g
• Now 2.5 g is recommended (Culman et al., 2012)
• Sample weight is adjusted when invalid results are obtained
• Standard Amount of KMnO4 is added
• A bright magenta color
• Solution and Soil react for 10 min
• An aliquot of solution is removed
• Centrifuge to separate solution from soil solids
• Solution color is assessed with a spectrophotometer (550nm)
• Bleaching is proportional to the amount of active carbon in the sample
• Less color = more active carbon
• A calculation is used to determine the amount of POX-C
QUESTIONS
• Is changing the weight of soil used an appropriate way to modify the
procedure?
• Can/should we fine-grind samples (<80um) to get a more representative
sample (especially with high particulate organic matter)
<2mm grind Fine grind (<80um)
SOIL WEIGHT
Not Distinguishable
from Blank
Below Detection
Limits
KMnO4 C (mg kg−1) = (0.02 mol L−1 − A) x (9000 mg C mol−1) x (0.02 L
solution /sample wt.) x AD/OD
GRIND SIZE
Active Carbon Standard Deviation
STATISTICAL ANALYSIS
• Analysis of Variance Table
•
• Response: ac
• Df Sum Sq Mean Sq F value Pr(>F)
Grind 1 15815809 15815809 15.066 0.0001198 ***
wt_class 4 99874453 24968613 23.784 < 2.2e-16 ***
Grind:wt_class 4 3636652 909163 0.866 0.4842380
Residuals 438 459814361 1049804
Statistically Significant
Grind Size YES
Weight Class YES
Interaction
(Grind x Weight Class) NO
OVERVIEW
Weight
Grind 0.25 0.5 1.0 2.5 5.0
Fine Grind 2171 1703 1329 933 617
2mm Grind 1629 1137 899 684 521
PRACTICAL IMPLICATIONS
• This technique does not appear to be a reliable laboratory method.
• Some still find it informative for less formal uses (demonstrations, assessments)
• Only one weight and grind should be used in each project
• Currently, 2.5g is recommended
• If an alternate prep is required – use it for the entire project
How can you make this
determination before you start the
analysis?
Sample
Weight
Percent Valid
Results
0.25 38%
0.50 58%
1.00 79%
2.50 84%
5.00 59%
Estimate Organic
Carbon Content
(generally)
PRACTICAL GUIDANCE
• color saturation and darkness (low value) are
indicative of high active carbon
• Background color of red, yellow or grey is not
important
• many small aggregate in the 2mm ground
sample
• many fine plant and root segments
Things that indicate high Active Carbon
WHAT WEIGHT SHOULD YOU USE?
Valid results for sample sizes < 2.5g
WHAT WEIGHT SHOULD YOU USE?
Valid results for sample sizes > 0.5g
All had valid results for sample sizes at 2.5g
PROJECTS THAT COMPARE VERY DIFFERENT
SYSTEMS
Pasture - Relatively low levels Native Longleaf Pine – High levels
Tifton Soil Series (Georgia) Surface Samples
Both of these samples have valid results at 1g
SUMMARY
• As soil health indicators become more quantitative there is a desire to develop rigorous
laboratory and field based tests.
• Active Carbon (POX-C) analysis is dependent upon sample amount and preparation
• Measured values increase as the sample amount and grind size decrease
• Further work is needed to understand what this method is measuring
• Values are only appropriate for comparing similar soils
• When used for field assessments – one standard weight should be used
• This method will not be relevant for some soils and situations
• NSSC is investigating the interpretation of active carbon comparisons across soil orders and
land-use systems
QUESTIONS?
Active carbon evaluating methodology   willis
Active carbon evaluating methodology   willis

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Active carbon evaluating methodology willis

  • 1. ACTIVE CARBON: EVALUATING METHODOLOGY OF A LABORATORY METHOD SKYE WILLS MICHEAL ROBOTHAM CANDISS WILLIAMS RICH FERGUSON STEVE MONTEITH
  • 2. ACTIVE CARBON • Carbon that is oxidized in a dilute permanganate (KMnO4) solution • Thought to be related to labile or ‘active’ forms of carbon • Shown to be more sensitive to management than other measures of soil organic carbon • Referred to more specifically as POX-C (Culman et al., 2012)
  • 3. ACTIVE C IN SOIL SURVEY • A study was conducted to determine the comparability between laboratory and field methods (Stiles et al.,2011) • NRCS-Soil Science Division has a program to measure dynamic soil properties • Measure soil properties under multiple land use and/or management systems • Kellogg Soil Survey Laboratory has been working to find consistent repeatable methods that work for ALL soils • Irregularities and inconsistencies have been noted by technicians
  • 4. BASIC PROCEDURE • Kellogg Soil Survey Laboratory • Air Dry and Grind Soil to <2mm • Weigh out sample • Originally 5 g • Now 2.5 g is recommended (Culman et al., 2012) • Sample weight is adjusted when invalid results are obtained • Standard Amount of KMnO4 is added • A bright magenta color • Solution and Soil react for 10 min • An aliquot of solution is removed • Centrifuge to separate solution from soil solids • Solution color is assessed with a spectrophotometer (550nm) • Bleaching is proportional to the amount of active carbon in the sample • Less color = more active carbon • A calculation is used to determine the amount of POX-C
  • 5.
  • 6. QUESTIONS • Is changing the weight of soil used an appropriate way to modify the procedure? • Can/should we fine-grind samples (<80um) to get a more representative sample (especially with high particulate organic matter) <2mm grind Fine grind (<80um)
  • 7. SOIL WEIGHT Not Distinguishable from Blank Below Detection Limits
  • 8. KMnO4 C (mg kg−1) = (0.02 mol L−1 − A) x (9000 mg C mol−1) x (0.02 L solution /sample wt.) x AD/OD
  • 9. GRIND SIZE Active Carbon Standard Deviation
  • 10. STATISTICAL ANALYSIS • Analysis of Variance Table • • Response: ac • Df Sum Sq Mean Sq F value Pr(>F) Grind 1 15815809 15815809 15.066 0.0001198 *** wt_class 4 99874453 24968613 23.784 < 2.2e-16 *** Grind:wt_class 4 3636652 909163 0.866 0.4842380 Residuals 438 459814361 1049804 Statistically Significant Grind Size YES Weight Class YES Interaction (Grind x Weight Class) NO
  • 11. OVERVIEW Weight Grind 0.25 0.5 1.0 2.5 5.0 Fine Grind 2171 1703 1329 933 617 2mm Grind 1629 1137 899 684 521
  • 12. PRACTICAL IMPLICATIONS • This technique does not appear to be a reliable laboratory method. • Some still find it informative for less formal uses (demonstrations, assessments) • Only one weight and grind should be used in each project • Currently, 2.5g is recommended • If an alternate prep is required – use it for the entire project How can you make this determination before you start the analysis? Sample Weight Percent Valid Results 0.25 38% 0.50 58% 1.00 79% 2.50 84% 5.00 59% Estimate Organic Carbon Content (generally)
  • 13. PRACTICAL GUIDANCE • color saturation and darkness (low value) are indicative of high active carbon • Background color of red, yellow or grey is not important • many small aggregate in the 2mm ground sample • many fine plant and root segments Things that indicate high Active Carbon
  • 14. WHAT WEIGHT SHOULD YOU USE? Valid results for sample sizes < 2.5g
  • 15. WHAT WEIGHT SHOULD YOU USE? Valid results for sample sizes > 0.5g
  • 16. All had valid results for sample sizes at 2.5g
  • 17. PROJECTS THAT COMPARE VERY DIFFERENT SYSTEMS Pasture - Relatively low levels Native Longleaf Pine – High levels Tifton Soil Series (Georgia) Surface Samples Both of these samples have valid results at 1g
  • 18. SUMMARY • As soil health indicators become more quantitative there is a desire to develop rigorous laboratory and field based tests. • Active Carbon (POX-C) analysis is dependent upon sample amount and preparation • Measured values increase as the sample amount and grind size decrease • Further work is needed to understand what this method is measuring • Values are only appropriate for comparing similar soils • When used for field assessments – one standard weight should be used • This method will not be relevant for some soils and situations • NSSC is investigating the interpretation of active carbon comparisons across soil orders and land-use systems