HORIZONTAL Factsheet AOX version: 2/15/2016 SUBJECT Determination of AOX HORIZONTAL number 10 Matrices Soil and sludge Existing standards used as basis Work package DIN 39 414 – S 18 CEN/TC 292, CEN/TC 308, CEN/TC 345, ISO/TC 190 5 Organic parameters Project STREP FP6 HORIZONTAL-ORG Expert Ulla Lund Organisation Eurofins A/S Country Denmark Email Status uol@eurofins.dk Standardisation Committees Desk study First Comments Phase I Final version Phase II Ruggedness August 2003 October 2003 December 2003 Ongoing work www.ecn.nl/horizontal Completion due 31-03-05 Second consultation Completion due 30-05-05 Validation Completion due 31-12-05 Transfer to BT/TF151 Foreseen 31-03-06 Summary of AOX procedure The AOX-procedure describes an empirical method for determination of organically bound chlorine, bromine and iodine adsorbed and occluded in the sample matrix. It is intended for analysis of solid material, such as sludge or soil. The intended concentration range is from 5 mg/kg dry matter to 6 g/kg dry matter. The principle of the method is: Addition of activated carbon to the dried, homogenised solid sample. Elution of inorganic halides and simultaneous adsorption of water soluble organic compounds on the activated carbon by shaking with acidified nitrate solution. Combustion of the sample/loaded activated carbon mixture at > 950ºC in an oxygen stream. Absorption of the hydrogen halides produced followed by determination of the halide ions by argentometric titration, such as microcoulometry. HORIZONTAL Factsheet AOX version: 2/15/2016 Placement of AOX method in overall structure HORIZONTAL SLUDGE, SOIL, TREATED BIOWASTE AND RELATED WASTES SAMPLING IN-SITU ,TRANSPORT, STORAGE SAMPLE PRETREATMENT - INORG INORGANIC CONSTITUENTS PHYSICAL PROPERTIES SAMPLE PRETREATMENT - HYG SAMPLE PRETREATMENT - ORG & BIOL LEACHING ORGANIC PARAMETERS BIOLOGICAL PARAMETERS HYGIENIC PARAMETERS PAH pH Bulk density Characterisation leaching tests Impurities (e.g glass, plastic) E. Coli Stability (bio) Salmonella Germinating weed seeds Clostridium Phytotoxicity Enterococci AOX Electrical conductivity Dry matter Compliance leaching tests PCB Organic matter* Solidity LAS, NP,NPE Nutrients N, P, K* Thixotropic behaviour DEPH, DBP Trace elements solid * Trace elements determination* Piling behaviour Helminth ova BFR Flowability Rapid methods PCCD/PCDF Soluble P Virusses and bacteriophages Pharmaceuticals Plant Pathogens Position of AOX method in the sequence of steps from sampling to reporting Sampling Taking of plan sample Transport & Preparation storage of test portion (x) Extraction/ Leaching Pre-treatment x Detection & Summary Quantification, reports Enumeration x x 1)Sample conservation, storage and transport are issues that generally are covered in as the final step in sampling standards 2) Preparation of the test portion from a laboratory sample is sometimes part of the next step (digestion or analysis preparation) or can be covered in a separate standard 3) Summary of test results is a concise summary of the relevant data for the end-user, which can be merged in an overall test report covering all aspects relevant for the given situation. 4) After defining sampling strategy based on the question to be answered either one of the sampling standards will generally apply. All the following steps will be the same for either route. 5) It is at present not clear where extraction of organic parameters begins and pre-treatment ends. It seems that pre-treatment now includes the extraction step. Major issues of discussion Can soil be covered by the standard? Will a low carbon to sample ratio lead to incomplete combustion? Is inorganic chloride effectively removed during sample pre-treatment?