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Comparing Methodology for Assessing Mineralizable N and Soil Organic Matter Rigas Karamanos, Western Cooperative Fertilizers Limited,

Calgary, AB and Tee Boon Goh, Department of Soil Science, University of Manitoba, Winnipeg, MB Email: r.karamanos@westcoag.com Introduction It is generally accepted that improvement in the accuracy of N recommendations requires that a reliable estimate of soil N supplying capability is needed. Numerous chemical and biological tests for assessing mineralizable/mineralized soil have been employed over several decades with varying but, generally, little success (Bundy, 2006). The lack of success has been largely attributed to the complexity of the N cycle in soils and the need to integrate numerous, physical, chemical, biological and spatial factors in arriving at the estimate of soil supplying capability. Flaten (2001) argued that nitrate-N combined with an estimate of mineralizable N may lead to better assessment of the N status of soils. This notion was supported by Walley et al. (2003) and an effort was made to calibrate the Illinois amino-sugar N test (ISNT) in Saskatchewan by Torie et al. (2005). However, information is being recently generated arguing the relevancy of the ISNT test for deriving N fertilization guidelines (Laboski et al. 2006). Karamanos and Cannon (2002) suggested a mathematical model to derive mineralizable N that is based on simple soil organic matter (carbon) (SOM) determination; however, Karamanos (2002) demonstrated that variability in SOM levels can be quite significant. A number of methodologies are employed today to determine soil organic matter (SOM), which can be distinguished in two groups, namely, chemical methods and loss on ignition (LOI) methods. The former normally employ chemical oxidation of soil organic carbon (Walkley and Black 1934); the latter placing a soil sample in a oven and heating it to a range of temperatures to destroy organic carbon (any inorganic carbon present in soil samples will also be destroyed). The objectives of this study were to assess bias and precision in determining soil organic matter (SOM) by a variety of methods and ascertain whether there is a relationship between chemical indices for determining mineralizable N and SOM levels. Materials and Methods Three sets of data were utilized to assess bias and precision in determining soil organic matter (SOM) by a variety of methods. The first set of data were from the North American Proficiency Test (NAPT) and included six samples analyzed by 48 to 60 soil testing laboratories by wet oxidation and loss on ignition methodology (Drs. Miller and Kotuby-Amacher, personal communication). The second set of data originated from previous research that compared analytical results of seven soil samples analyzed by six different soil testing laboratories. The final set of data was from 50 samples that were assayed for SOM by six different methodologies; SOM levels calculated from soil organic carbon (SOC) that was determined as the difference between total soil carbon (C) and inorganic C were considered as a basis for comparing the remaining five methodologies that included both wet oxidation and loss on ignition. In addition, the soils in the final set were assayed for hot KCl (Campbell et al. 1977) and amino-sugar (Khan et al. 2001) extractable NH4-N. Results The first set of data demonstrated that although measurements were precise, bias was greater as the SOM increased (Table 1, Figure 1). Thus estimating mineralizable N using the model of Karamanos and

Cannon (2002) would result in 14-18 and 9-15 lb N/acre error by the Walkley Black and loss-on-ignition methods, respectively (Figure 2). Table 1. Statistical analysis of organic matter content assayed by wet oxidation (Walkley Black 1934) and loss on ignition from 1998 NAPT samples % Method Sample No. Minimum Maximum Median MAD1 RMD%2 Values<WL3 SOM-WB 98101 58 2.5 7.3 3.96 0.26 6.4 86 98102 60 0.8 2.5 1.26 0.16 12.3 83.1 98103 58 0.2 1.7 0.6 0.1 16.7 78.9 98104 60 0.7 3.7 1.3 0.18 13.8 91.5 98105 48 0.2 120 24.2 2.2 9.1 72.3 98106 49 4 37 8 1.3 16.3 72.9 98101 57 2.9 17 4.3 0.5 11.6 98102 53 1 2.3 1.4 0.2 14.3 98103 57 0.1 2 0.7 0.11 15.9 98104 56 0.9 4 1.5 0.28 18.7 98105 48 0.2 120 24.2 2.2 9.1 98106 49 4 37 8 1.3 16.3 1 Median Absolute Deviation 2 Relative Median Absolute Deviation 3 Percentage of all reported values within Warning Limits based on 2.5 X (MAD). SOM-LOI 80 84.3 85.5 83.3 72.3 72.9

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10 Upper and lower limits, %

____

Walkley-Black ------- Loss on Ignition

0 0 1 2 3 4 5 6 7 8 9 Organic matter %

Figure 1. Upper and lower limits for the determination of soil organic matter (SOM) of six soils by 48 to 60 different laboratories participating in the NAPTP.

18 ____ 16 Walkley-Black ------- Loss on Ignition

Mineralization, lb N/acre

14

12

10

8 0 1 2 3 4 5 6 7 8 9 Organic matter %

Figure 2. Difference in estimated mineralizable N as a result of methodology bias. The second set of data also demonstrated increased bias at higher SOM levels (Figures 3 and 4).

10 Soil organic matter Other Laboratories, % 9 8 7 6 5 4 3 2 2 3 4 5 6 7 8 9 10 11 12 Soil organic matter Laboratory A, %


Lab B =0.38 + 0.688Lab A, r = 0.976*** Lab C = 0.449 + 0.812Lab A, r = 0.666* Lab D = 1.297 + 0.528Lab A, r = 0.92*** Lab E = 0.981 + 0.624Lab A, r = 0.892*** Lab F = 1.491 + 0.426Lab A, r = 0.903***

Figure 3. Comparison of soil organic matter levels determined by fiver laboratories to a sixth laboratory.

The results from two commonly used chemical assays for estimating N mineralization (hot KCl and amino sugar tests) were correlated with SOM levels in the third set of data. There was a highly statistically significant correlation (r=0.674***) between NH4-N levels extracted by the amino sugar method and SOM levels, thus suggesting that a simple SOM determination would be of equal value in potentially assessing N mineralization. There was no relationship between hot KCl extracted NH4-N levels and SOM (r=373); further, soil extractable NH4-N levels were closely correlated with hot KCl extractable NH4-N (r=0.847***). Overall, all methods used in the final set resulted in similar results, however, bias amongst laboratories was great at all SOM levels (Figures 5a,b).

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Nrate = 58.7 - 12.09OMlowest + 0.77OMlowest2, r2 = 0.97


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recommendation, lb N/acre

25 20 15 10 5 0 2 3 4 5 6 7 8 9 10 Lowest value of organic matter, %

Figure 4. Impact of bias in soil organic matter determination on N recommendation for CWRS wheat. Conclusions 1. Although soil organic matter measurements (SOM) are precise, there is a tendency for greater bias in the data as SOM increase. 2. Higher bias in SOM measurements has an adverse effect on estimates of mineralizable N that are based on SOM. 3. The Illinois amino-sugar N test (ISNT) may not have any relevancy in deriving mineralizable N in western Canada.
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2

(a)
WBtitration = 0.8644x + 0.6622, R = 0.955 WBcolorimetric = 0.8591x + 0.8173, R = 0.942 2 LOI1 = 0.9309x + 0.5937, R = 0.933 LOI2 = 0.9493x + 0.0963, R = 0.907
2 2

11 10 Organic matter, % 9 8 7 6 5 4 3 2 2

Walkley-Black (titration) Walkley-Black (colorimetric) Loss on Ignition 1 Loss on Ignition 2

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12

Organic matter determined from Total C - inorganic C, %

(b)
12 11 10 Organic matter, % 9 8 7 6 5 4 3 2 2 4 6 8 10 12 Organic matter determined from Total C - inorganic C, %

Figure 5. Comparison of soil organic carbon (SOC) levels extracted by five methods to SOC that was determined as the difference between total soil carbon (C) and inorganic C.

References Bundy, L.G. 2006. Nitrogen mineralization estimates for N rate suggestion. p 66-71 in Proc. NorthCentral Industry-Extension Soil Fert. Conf., Des Moines, Iowa, PPI, Brookings, SD. Flaten, D. 2001. The nitrate soil test: Is it reliable? [Online] Available: http://www.umanitoba.ca/afs/agronomists_conf/2001/pdf/flaten.pdf [5 December 2006]. Campbell, C.A., Jame, Y.W., Jalil, A. and Schoenau, J. 1997. Use of hot KCl-NH4-N to estimate fertilizer N requirements. Can. J. Soil Sci. 77: 161-166. Karamanos, R.E. 2002. Soil Testing The Other Side of the Story. Proc. 45th Man. Soil Sci. Soc. Meeting, February 5-6, [Online] Available: http://www.gov.mb.ca/agriculture/msss/2002/mss1587.pdf [5 December 2006]. Karamanos, R.E. and Cannon, K.R. 2002. Virtual soil testing. Is it possible? Comm. Soil Sci. Plant Anal. 33: 1532-2416. Kahn, S.A., Mulvaney, R.L. and Hoeft, R.G. 2001. A simple soil test for detecting sites that are nonresponsive to nitrogen fertilization. Soil Sci. Soc. Am. J. 65: 1751-1760. Laboski, C.A.M., Sawyer, J.E., Walters, D.T., Bundy, L.G., Hoeft, R.G., Randall, G.W. and Andraski, T.W. 2006. Evaluation of the Illinois soil nitrogen test in the north central region. p 86-93 in Proc. North-Central Industry-Extension Soil Fert. Conf., Des Moines, Iowa, PPI, Brookings, SD. Torie, S.J., Pennock, D.J. and Walley, F.L. 2005. Assessing potentially available nitrogen in Saskatchewan using the Illinois amino sugar-N test. In Proc. Soils and Crops 2005 [CD ROM], Extension Div., Univ. of Saskatchewan, Saskatoon, SK. Walley, F., Yates, T., Jokic, A. and Masutti, M. 2003. Assessing soil N availability indices Is inorganic N enough? In Proceedings Soils and Crops 2005 [CD ROM], Extension Div., Univ. of Saskatchewan, Saskatoon, SK. Walkley, A. and Black, I.A. 1934. An examination of the Degtjareff method for determining soil organic matter, and a proposed modification of the chromic acid titration method. Soil Sci. 34: 29-38.