Validation and Development of Gravimetric Method for Humic Acid Determination
Keywords:
Validation, Gravimetric, Development, Fertilizers, MethodAbstract
Samples of fertilizer undergo testing to ascertain the levels of nutrients they contain, but the results differ depending on the method used. Thus, the primary aim of this research was to create and verify a method for determining humic acid using gravimetric analysis. The gravimetric method for quantifying humic acid contents was validated at the Soil & Water Testing Laboratories (SWTL), Accredited for ISO: 17025 in D.G.Khan. The validation process encompassed repeatability, reproducibility, limit of detection, limit of quantification, recovery, and bias. Descriptive stat were used in the study (i.e Average, Standard Deviation, relative standard deviation, etc.), and for Reproducibility T-test was employed. The detection as well as quantification limits were 0.145% and 0.484% Humic acid, respectively. With a repeatability RSD of 0.4725%, the reproducibility showed T-calculated values of 0.05, which were below the T-tabulated threshold of 2.262. The alpha value for T used in this study was 0.05 (5% level of significance or 95% confidence interval, i.e K2. The recovery of Humic acid was 102.34%. The Z-scores for the results (QUATEST3 www.quatest3.com.vn) in Vietnam fell within the satisfactory range. The coefficient of correlation (0.999%) indicates a strong connection between the true value of Humic acid and the calculated values. This result indicates that the performance of the method was best. As all the parameters performed well and gave accurate results as per standard criteria. Therefore, the approach could be effectively applied for determining humic acid in fertilizers.
References
Albiach R, Canet R, Pomares F, and Ingelmo F. Organic matter components and aggregate stability after the application of different amendments to a horticultural soil. Bioresour. Technol. 2001. 76, 125–129. doi: 10.1016/S0960-8524(00)00090-0
AOAC. Official Method of Analysis of AOAC International, 20th Edition, 2016 AOAC Official Method 2.7.05 Method No. 973.04 chapter 2; 53.
BybOrdin A, and Ebrahimian, E. Growth, yield and quality components of canola fertilized with urea and zeolite. Commun. Soil Sci. Plant Anal. 2013; 44, 2896–2915. doi: 10.1080/00103624.2013.823986
Billingham, KL. Humic products-potential or presumption for agriculture? Can humic products improve my soil? . .. .2012 in 27th Annual Conference (Orange, NSW: Grassland Society of NSW Inc.).
Canellas LP, Canellas NOA, Luiz Eduardo LES, Olivares FL, Piccolo A. Plant chemical priming by humic acids. Chem. Biol. Technol. Agric. 2020 (7): 12. doi: 10.1186/s40538-020-00178-4
Codex Alimentarius Commission. Requirements for the use of single-laboratory verification for Codex purposes. Codex Alimentarius Committee. Codex Committee on Methods of Analysis and Sampling. 24th Session, November 2002; 1-12.
De Melo BAG, Motta FL, Santana MHA.. Humic acids: Structural properties and multiple functionalities for novel technological developments. Mater. Sci. Eng. C. 2016: 62, 967–974. doi: 10.1016/j.msec.2015.12.001
Estefan G, Sommer R, Ryan J. Methods of Soil, Plant and Water Analysis: A Manual For the West Asia and North Africa region. ICARDA. 2013.
El-Bassiouny H SM, Bakry, BA, El-Monem Attia AA, Abd Allah MM.. Physiological role of humic acid and nicotinamide on improving plant growth, yield, and mineral nutrients of wheat (Triticum durum L.) grown under newly reclaimed sandy soil. Agric. Sci. 2014. 05, 687–700. Doi: 10.4236/as.2014.58072
Fuentes M, Baigorri R, González-Gaitano G, García-Mina JM. New methodology to assess the quantity and quality of humic substances in organic materials and commercial products for agriculture. J. Soils Sediments. 2018; (18): 1389–1399. doi: 10.1007/s11368-016-1514-2
Gollenbeek L, Van Der Weide R. Prospects for Humic Acid Products From Digestate in the Netherlands. Report WPR-867. 2020; 40 (5). doi: 10.18174/541280
Hayes MHB, Swift RS. Vindication of humic substances as a key component of organic matter in soil and water. Adv. Agron. 2020;. (163): 1–37. doi: 10.1016/bs.agron.2020.05.001
ISO. Guide 34 General Requirements for the Competence of Reference Material Producers. 2nd, International Organization for Standardization, Geneva, Switzerland. 2009. 1-34
ISO. Fertilizers and soil conditioners- Determination of humic acid and hydrophobic Fulvic acid concentrations in fertilizer materials. Geneva, Switzerland. ISO 19822:2018(E).2018(8); 1-16
Kelapa T, Banyuasin K.. Effects of humic substances on plant growth and mineral nutrients uptake of wheat under conditions of salinity. Asian J. Crop Sci. 2016; (1): 87–95. doi: 10.3923/ajcs.2009.87.95.
Magnusson, B. Eurachem Guide: The Fitness for Purpose of analytical methods, Laboratory guide to method Verification and related topics, (2nd edition). 2014. ISBN 978-91-87461-59-0.
Mukherjee A, Lal R, Zimmerman AR. Impacts of 1.5-year field aging on biochar, humic acid, and water treatment residual amended soil. Soil Sci. 2014; (179): 333–339. doi: 10.1097/SS.0000000000000076.
NATA. Guidelines for the Verification and verification of chemical test methods, NATA technical note 17, 2009.
PSQCA. Pakistan Standard Specification for Potassium Sulphate. ICS: 65.080 PSQCA Karachi PS:5610: 2023 (Rev). 1-12.
Rose MT, Patti AF, Little KR, Brown AL, Jackson WR, Cavagnaro TR.. A meta-analysis and review of plant-growth response to humic substances: Practical implications for agriculture. Adv. Agron. 2014; (124): 37–89. doi: 10.1016/B978-0-12-800138-7.00002-4
Sible CN, Seebauer JR, Below FE. Plant biostimulants: a categorical review, their implications for row crop production, and relation to soil health indicators. Agronomy 11, 1297. doi: 10.3390/agronomy. 2021. 110 71297.
Validation of Analytical Methods for Food Control, Report of a Joint FAO/IAEA Expert Consultation, December 1997, FAO Food and Nutrition Paper No. 68, FAO, Rome 1998; 17-19. ISBN: 9251041318.
Wiesler F, Hund-Rinke K, Gäth S, George E, Greef JM, Hölzle LE.. Anwendng von organischen Düngern und organischen Reststoffen in der Landwirtschaft. Berichte uber Landwirtschaft 94, 1. doi: 10.12767/buel. 2016 v94i1.124
Wu S, Li R, Peng S, Liu Q, Zhu X.. Effect of humic acid on the transformation of soil heavy metals. IOP Conf. Ser.. Mater. Sci. Eng. 2017: 207, 012089. doi: 10.1088/1757-899X/207/1/012089
Yang F, Antonietti M.. The sleeping giant: A polymer view on humic matter in synthesis and applications. Prog. Polym. Sci. 2020. 100, 101182. doi: 10.1016/j.progpolymsci.2019.101182.
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