BS EN ISO 7526:2020 pdf download – Ferronickels – Determination of sulfur content – Infrared absorption method after induction furnace combustion
6.1.3 Maintain a glass-wool filter (5.4) between the furnace chamber and the analyser and change as necessary. The furnace chamber, pedestal post and filter trap should be cleaned frequently to remove oxide residues.
6.1.4 The manufacturer may recommend setting the programming unit to give a pre-burn period before oxygen enters the furnace chamber. The test portion should be at a red heat during the pre-burn period. When oxygen is introduced for the combustion stage, the temperature increases substantially.
6.1.5 The temperature reached during combustion depends on the furnace, and the type and quantity of metal in the crucible. A high temperature (>1 700 °C) is maintained after the test portion is fused so that the sulfur dioxide can be completely removed from the furnace to the infrared analyser.
6.1.6 The flow rate of oxygen can vary from one instrument to another but is usually about 2,0 l/min during the combustion period.
6.1.7 After the equipment has been idle for a few hours or after cleaning the furnace chamber or filters, the instrument should be stabilized as described in 8.1.
NOTE Features of commercial equipment are given in Annex A.
6.2 Ceramic crucibles and lids. Ceramic crucibles, containing the sample and any additions that can be necessary, are required for the combustion. They shall be of precise dimensions for the system and fit the supporting pedestal post so that the test portion in the crucible is positioned correctly within the induction coil for heating. Typical dimensions of combustion crucibles are: a height of 25 mm, an external diameter of 25 mm, an internal diameter of 20 mm, a wall thickness of 2,5 mm, and a thickness of base of 8 mm. The dimension of the hole of the lid should be larger than 10 mm. Crucibles and lids shall be as specified by the manufacturer of the instrumentation used and shall be capable of withstanding combustion in an induction furnace without evolving sulfur-containing chemicals so that achieving and maintaining blank values within specification is possible. In order to remove any sulfur contamination, pre-ignite the crucibles in air or oxygen in a furnace for not less than 1 h at 1 100 °C and store in a desiccator or a closed container. A resistance furnace with a combustion tube through which a flow of oxygen passes may also be used. Crucible lids, used to help retain the solid oxidation products in the hot zone of the induction coil, shall be pre-ignited in a similar manner.
6.3 Crucible tongs, capable of handling recommended crucibles (6.2).
7 Sampling and sample preparation
7.1 Sampling and sample preparation shall be carried out by normal agreed procedures or, in cases of dispute, by appropriate national standards.
7.2 The laboratory sample is normally in the form of a powder, granules, millings or drillings and no further preparation of the sample is necessary.
7.3 If it is suspected that the laboratory sample is contaminated with oil or grease from the milling or drilling process, it shall be cleaned by washing with high purity acetone and drying in air. 7.4 If the laboratory sample contains particles or pieces of widely varying sizes, the test portion should be obtained by riffling
8.1.1 Assemble the apparatus and prepare it for operation according to the manufacturer’s instructions. Test the furnace and analyser to ensure the absence of leaks.
8.1.2 Condition and stabilize the equipment by combusting several samples, similar to those to be analysed, using appropriate fluxes and accelerators, before attempting to calibrate the system or determine the blank.
NOTE It is not necessary to use pre-ignited crucibles.
8.1.3 Allow the instrument to cycle several times with oxygen flowing and adjust the zero of the instrument.BS EN ISO 7526 pdf download.