Testing Methods for Fertilizers (2013) - FAMIC

1 Testing Methods for Fertilizers ( 2013 ) Incorporated Administrative Agency Food and Agricultural Materials Inspection Center Note:This is unofficial translation. Only the original Japanese texts have effect and the translation is to be used solely as reference material. This center assumes no responsibility whatever for any direct, indirect, special, incidental, consequential damages and any other damages resulting from the use of this contents. No part of this text may be reproduced in any form without permission. 2 Introduction The Official Methods of Analysis of Fertilizers stipulated by the Ministry of Agriculture, Forestry and Fisheries is the only analysis method to assess main components and harmful components in Fertilizers in Japan and contributes to improving quality and securing guaranteed components of Fertilizers .

2 However no new revision has been issued since The Official Methods of Analysis of Fertilizers 1992 was issued. Some quarters such as fertilizer manufacturers and inspection instruction agencies have requested a revised edition of The Official Methods of Analysis of Fertilizers since new kinds of Fertilizers and its new components were added into the public standard, and analysis instruments and technologies have progressed during the period. Incorporated Administrative Agency, Food and Agricultural Materials Inspection Center ( FAMIC ) has revised the Official Methods of Analysis of Fertilizers by introducing the analysis conditions and the analysis Methods , etc. which meet the latest situation. Additionally, FAMIC tried to study how to introduce the analysis Methods or the new analysis instruments to cope with new effective components or harmful components and new Fertilizers which are not documented in the Official Methods of Analysis of Fertilizers , and established new Testing Methods .

3 At the same time, FAMIC conducted a validity test according to the requirements of ISO/IEC 17025 and opened the results and new Testing Methods which were discussed and approved by the Technical Committee for Fertilizers etc. including outside experts on FAMIC s web site in 2008 as The Testing Methods for Fertilizers 2008 . Since then, the contents have been annually added and updated. In this year, four Testing Methods such as melamine (High Performance liquid chromatography ), whose validity were checked at a single laboratory in 2012, were merged as reference Methods , and the Testing Methods for Fertilizes 2013 in which 54 items (components, etc.) and 93 Testing Methods were incorporated was opened on FAMIC s web site. Although the Testing Methods for Fertilizes cannot substitute the Official Methods of Analysis of Fertilizers which is designated as an official method in an official notice of the Ministry of Agriculture, Forestry and Fisheries, reagents and instruments used are stipulated in JIS standards, the validity of the Testing method is checked by referencing IUPAC protocols and it is listed as an analysis method whose validity is checked in The Management Handbook of Heavy Metal in Sludge Fertilizers published by the Ministry of Agriculture, Forestry and Fisheries in August 2010.

4 Therefore FAMIC would like people engaged in the quality control and analysis of fertilizes to use this as a practical document. May, 2013 Incorporated Administrative Agency Food and Agricultural Materials Inspection Center General Director Makoto Kimura 3 External members of The Technical Committee for the Testing Method about Fertilizers (As of March, 2013 ) (Random order, without honorifics) Mayumi AIZAKI Saitama Prefectural Agriculture and Forestry Comprehensive Research Center Masashi UWASAWA Japan Fertilizer and Feed Inspection Association Akira KAWASAKI Incorporated Administrative Agency: National Institute for Agro-Environmental Sciences Narihiro NAITO Incorporated Administrative Agency: National Agriculture and Food Research Organization Munetomo NAKAMURA Japan Food Research Laboratories Akira NOGUCHI Incorporated Educational Institution: Nihon University Kazuyuki YAZIMA Corporate Juridical Person.

5 Niigata Prefectural Institute of Public Health and Environmental Sciences Akemi YASUI Incorporated Administrative Agency: National Agriculture and Food Research Organization 4 Contents Introduction ..2 1. General Rules ..8 Common Items ..8 Validity check of Testing Methods ..12 2. Handling of samples ..13 Storage of samples ..13 Preparation of test samples ..14 Pre-drying ..15 Reduction (Separation) ..17 Grinding ..18 3. General tests ..19 Moisture ..19 Loss on drying method with drying apparatus ..19 Loss on drying method by moisture analyzers ..22 Ash content ..25 Ignition residue method ..25 pH ..26 Glass electrode method ..26 Electrical conductivity ..28 Measurement method with an electrical conductivity meter ..28 Granularity ..30 Dry-type sieving Testing method ..30 Oil content ..32 Diethyl ether extraction method.

6 32 4. Main components, guaranteed components, etc..34 Nitrogen ..34 Total nitrogen ..34 Kjeldahl method ..34 Combustion method ..40 Devarda s alloy Kjeldahl method ..45 Reduced iron Kjeldahl method ..50 Calculation with ammonia nitrogen and nitrate nitrogen ..55 Ammoniac nitrogen ..56 Distillation method ..56 Formaldehyde method ..61 Nitrate nitrogen ..65 Devarda s alloy - distillation method ..65 Reduced iron- distillation method ..70 Phenol sulfuric acid method ..75 Phosphate ..79 Total phosphate ..79 Ammonium vanadomolybdate absorptiometric analysis ..79 Quinoline gravimetric analysis ..85 Soluble phosphoric acid ..88 Ammonium vanadomolybdate absorptiometric analysis ..88 Quinoline gravimetric analysis ..93 5 Citrate soluble phosphoric acid ..96 Ammonium vanadomolybdate absorptiometric analysis ..96 Quinoline gravimetric analysis ..100 Water-soluble phosphoric acid.

7 103 Ammonium vanadomolybdate absorptiometric analysis ..103 Ammonium vanadomolybdate absorptiometric analysis ..108 ( liquid mixed Fertilizers containing phosphonic acid or phosphite) Quinoline gravimetric analysis ..113 Potassium ..116 Total potassium ..116 Flame atomic absorption spectrometry or flame photometry ..116 Sodium tetraphenylborate gravimetric analysis ..120 Citrate soluble potassium ..124 Flame atomic absorption spectrometry or flame photometry ..124 Sodium tetraphenylborate gravimetric analysis ..127 Sodium tetraphenylborate volumetric analysis ..130 Water-soluble potassium ..133 Flame atomic absorption spectrometry or flame photometry ..133 Sodium tetraphenylborate gravimetric analysis ..137 Sodium tetraphenylborate volumetric analysis ..141 Silicic acid ..144 Soluble silicic acid ..144 Potassium fluoride method ..144 Potassium fluoride method (silica gel Fertilizers , etc.)

8 148 Potassium fluoride method ( Fertilizers containing silica gel Fertilizers ) <Reference method> ..152 Perchloric acid method ..157 Lime, calcium and alkalinity ..160 Total lime ..160 Flame atomic absorption spectrometry ..160 Soluble lime ..163 Flame atomic absorption spectrometry ..163 Water-soluble calcium ..166 Flame atomic absorption spectrometry ..166 Alkalinity ..169 Ethylenediamine tetraacetate method ..169 Calculation from soluble lime and soluble magnesia ..175 Magnesia ..176 Soluble magnesia ..176 Flame atomic absorption spectrometry ..176 Citrate soluble magnesia ..179 Flame atomic absorption spectrometry ..179 Water-soluble magnesia ..182 Flame atomic absorption spectrometry ..182 Manganese ..185 Soluble manganese ..185 Flame atomic absorption spectrometry ..185 Citrate soluble manganese ..188 Flame atomic absorption spectrometry .

9 188 Water-soluble manganese ..191 Flame atomic absorption spectrometry ..191 6 Boron ..194 Citrate soluble boron ..194 Azomethine-H method ..194 Water-soluble boron ..197 Azomethine-H method ..197 Zinc ..200 Total zinc ..200 Flame atomic absorption spectrometry ..200 ICP Atomic Emission spectrometry <Reference method> ..203 Water-soluble zinc ..207 Flame atomic absorption spectrometry ..207 Copper ..210 Total copper ..210 Flame atomic absorption spectrometry ..210 ICP Atomic Emission spectrometry <Reference method> ..214 Water-soluble copper ..218 Flame atomic absorption spectrometry ..218 Organic carbon and carbon-nitrogen ratio ..221 Organic carbon ..221 Dichromate oxidation ..221 Combustion method <Reference method> ..224 Carbon-nitrogen ratio ..228 Sulfur ..229 Total sulfur content ..229 Titration analysis <Reference method> ..229 Barium chloride gravimetric analysis <Reference method>.

10 231 Transmitted light analysis <Reference method> ..235 Iron ..239 Water-soluble iron ..239 Flame atomic absorption spectrometry ..239 Molybdenum ..242 Water-soluble molybdenum ..242 Sodium thiocyanate absorptiometric analysis ..242 5. Harmful components ..245 Mercury ..245 Cold vapor atomic absorption spectrometry ..245 Arsenic ..249 Hydride generation atomic absorption spectrometry ..249 Silver diethyl dithiocarbamate absorptiometric analysis ..255 Cadmium ..259 Flame atomic absorption spectrometry ..259 ICP Atomic Emission spectrometry <Reference method> ..263 Nickel ..267 Flame atomic absorption spectrometry ..267 ICP Atomic Emission spectrometry <Reference method> ..271 Chromium ..275 Flame atomic absorption spectrometry ( Fertilizers containing organic matters) ..275 Flame atomic absorption spectrometry ( Fertilizers not containing organic matters).