Preparation of samples in the Steel Industry Pedro Vellosillo September 2015

One of the most important steps when carrying out any type of analysis is the Preparation of the Sample

At the moment of Preparing the Samples the objective is to obtain an homogeneous reduced sample from a bigger lot

1.- The quantity of the sample has to be enough as to be able to carry out all the necessary analysis. The sample must be homogeneous and representative. 2.- The sample has to be collected and kept very carefully to avoid any changes or contamination. 3.- The sample will need to be milled and mixed until becoming a very homogeneus powder, of the appropriate size for analysis. Make sure to avoid any kind of contamination during the process.

61% 27% 6%

30% 19% 11% 9% 8% 7% 6% 4%

7 Sample preparation General aspects Sample taking (Sampling) Representative sampling of the product. Homogenisation Reduction of the size of the particles (crushing) Homogenisation Division of the sample Driying Removal of the moisture in the sample. Milling Finishing of the sample for analysis (200μm / 100μm/ ˃100μm).

8 Sample preparation General aspects Sample taking (Sampling) Get a small quantity of material whose composition may represent exactly the one of the material being sampled.

9 Sample preparation General aspects Homogenisation Initial sample ( 100mm) Final sample (5mm) Homogeniser Rifle divider

10 Sample preparation General aspects Drying Removal of the moisture in the material to work with a sample that is: Dry Environmentally estable

11 Sample preparation General aspects Milling Reduction of the size of the particles up to a granulometry appropriate for analysis The final size of the sample shall depend on the type of analysis to undertake Usual sizes…..˃200µm ˃100µm ˃75μm Up to 100μ Up to 50 μ Sieve unit Samples for analysis ˃100µm

12 Sample preparation General aspects Analysis C/S – O/N – H – TGA – etc.

13 Sample preparation General aspects FRX Analysis Preparation of samples as pellets for FXR

14 Sample preparation General aspects FRX Analysis Preparation of samples as beads for FXR

15 Sample preparation General aspects ICP Analysis / Wet process Preparation of samples by dissolution for ICP or Wet Process analysis

16 Equilab units for the preparation of samples EQR-100 Mill Method: friction, mixing and crushing __________________________________________________________________ Application: Cement Industry, Metalurgical Industry, Thermal Station, Environmental Laboratories, Recycling Plants, Geology and Mineralogy, Ceramics. __________________________________________________________________ Initial granulometry*: < 15mm __________________________________________________________________ Final granulometry*: < 50 μm __________________________________________________________________ Milling speed: Regulable / 1000/1500/2000rpm __________________________________________________________________ Engine power: 750W __________________________________________________________________ Power source: 2 x 220V __________________________________________________________________ Milling jars: Acero 100ml Steel 200ml Tungsten Carbide 100ml Tungsten Carbide 200ml __________________________________________________________________ Dimensions: 104cm (high) x 80cm (width) x 60cm (depth) Approximate weight: 250kg Technical Specifications

17 Equilab units for the preparation of samples EQR-100 Mill The vibratory disc mill EQR-100 is a milling unit especially designed to obtain analitical granulometries in a wide variety of samples, such as glass, earths, slags, metallic oxides, ferroalloys, cements, ceramic materials, amongst many others. It can crush in a very short timespam a vast range of different materials, from semi-hard to the hardest, fragile or fibrous. Easy to handle, and made of sturdy components, this mill is a unit practically maintenance free. Quick Simple Safe Silent 5 working programs For speed and capacity, this is the most widely used type of mill in laboratories

18 Equilab units for the preparation of samples Ball Mixer Mill EQM-400 Method: crushing, milling, friction, mixing and homogenisation __________________________________________________________________ Applications: hard materials, semi-hard and fragile such as coal, coke, glass, slags, minerlas, earths, ceramics, silicate, bones, plastics, wood, electronical waste, cheqmical products, tobacco, cereals, etc. Programs: five independent programs Speed: 100 to 2000 stirs per minute Time: 0 a 99 minutes __________________________________________________________________ Power: 150W _________________________________________________________________ Engine: 220V - 150W _________________________________________________________________ Power source: 220V - 100W _________________________________________________________________ Accessories: 50ml and 25ml jars CW balls: Ø 10mm / Ø 15mm / Ø 20mm / Ø 25mm __________________________________________________________________ Dimensions: 24cm (high) x 31,5cm (width) x 35cm (depth) Approximate weight: 13kg

19 Equilab units for the preparation of samples Ball Mixer Mill EQM-400 Specially designed for: Reducing the size of small quantities of sample to ˃50µm. Homogenisation and mixing of samples with binding agents HOMOGENISATION REDUCTION OF THE SIZE OF THE GRAIN MILLING CRUSHING

20 Equilab units for the preparation of samples EQP-100 Press Semi-automatic press for the preparation of beads/pellets of hight quality for analysis in XRF, five automatic programs simple or double cycle, allowing the control of the pressure strentgh and time. Easy to use, this is a robust and durable unit. Technical Specifications: Method: Pressure ___________________________________________________ Applications: Cement Industry, Metallurgical Industry, Thermal Stations, Environmental Laboratories, Reclycling Plants, Geology and Mineralogy, Ceramics. ___________________________________________________ Speed Control: Frequency Converter 0/200Hz ___________________________________________________ Diameter of the sample: 40mm (other diameters under request) ___________________________________________________ Maximum Pressure: 40t ___________________________________________________ Power Engine: 750W ___________________________________________________ Power: 2 x 220V ___________________________________________________ Consumables: Aluminium cups 40mm diam __________________________________________________ Dimensions: 40cm (high) x 51cm (width) x 42cm (depth) Approximate Weight: 75kg

21 Equilab units for the preparation of samples EQP-100 Press Maximum pressure: 650 kg/cm2 Flow: 0,8 l/min Die and punch in Tungsten Carbide

22 Equilab units for the preparation of samples EQH-3.0 Furnace Multi-EQP-100 More than a unit, the EQH-3.0 and the Multi-EQP-100 are tools for the preparation of samples

23 Equilab units for the preparation of samples in the Steel Industry EQH-3.0 Furnace Method: Heating by induction ___________________________________________ Applications: Steel Industry, Foundries ___________________________________________ Programs: five programs ___________________________________________ Time: adjustable / seconds ___________________________________________ Maximum Power: 3KVA ___________________________________________ Power: 220V 50/60 Hz ___________________________________________ Induction Frequency: 120 kHz kHz ___________________________________________ Safety: IP 40 ___________________________________________ Cooling system: by closed internal circuit ___________________________________________ Dimensions: 40 (height) x 51 (width) x 42cm (depth) Approximate weight: 12 kg

24 Equilab units for the preparation of samples in the Steel Industry EQH-3.0 Furnace Able to heat up a sample in seconds, for its subsequent treatment (crushing, cutting or punching). Adjustable heating up times from 0 to 100 seconds. Cooling by internal water circuit (2 l.). Specially designed for the obtention of samples for a quick analysis of Carbon, Sulphur and Nitrogen contents

25 Equilab units for the preparation of samples in the Steel Industry EQH-3.0 Furnace Crushing for arc spectrometry Preparation of pins for C/S N

26 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 One single hydraulic control unit manages up to three working units of interchangeable tools Automatic selection of module and tool from the working unit button

27 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100

28 Equilab units for the preparation of samples in the Steel Industry Multi-EQP-100 Central unit Have hydraulic control unit models ………… ______________________________________________ Maximum flow …………………. 0,8L/min 1,2L/min Maximum pressure…………….650K/cm2 450K/cm2 ______________________________________________ Speed control: frequency converter 25/75Hz ______________________________________________ Engine power: 750W _____________________________________________ Power: 2 x 220V 50/60 Hz ______________________________________________ Touchscreen 7” ______________________________________________ Dimensions Control unit: 40cm (high) x 51cm (width) x 42cm (depth) Control unit weight: 40kg

29 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Tools Specifications of the tools Tool diameter ………….120mm Maximum stroke …………….. 53mm Pellet press tool Pressure control Time control Maximum stroke: 53 mm Diameter of the pellet:30 / 40 mm Flow: 1,17 l/min Maximum pressure: 450 Kg/cm2 Maximum strenght: 50 T Crushing tool Pressure control Time control Contact area: Ø 53 mm Maximum strenght: 50 T Punching tool Pressure control Quantity of pins: 3 Pin diameter: 6 mm (other diameters under request) Maximum strenght: 25 T (limited by software) Cutting tool Pressure control Time control Cutting diameter: bars up to Ø 30 mm Maximum strenght: 50 T

30 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Standard tools Punching Cutting Crushing Pressing

31 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Replacing the tools Practical bayonet mount system allowing a comfortable change of the chosen tool Quick Easy

32 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Software A simple and intuitive software will let us manage all the operations the unit is able to undertake automatically Control screen This will allow us to define the parameters for the different functions: Crushing Pressing Cutting Punching

33 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Software PRENSADOCORTE Presión Tiempo A We will define the tool in each working unit, the working pressure and the time for the pressure. We can also define the stroke of the piston: By pressure By position Each piston has got two detectors allowing us to control the stroke of the same. We can also modify the parameters of each working unit directly on the screen and even select the position detectors

34 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Software Configuration screen. This will let us define the general parameters of the unit, such us: Maximum upwards and downwards pressure Speed in the movement up and down Language (Spanish – English) Pressure calibration

35 Equilab units for the preparation of samples in the Steel Industry MultiEQP-100 Software Diagnosis screens: These will let us manually manage all the working processes the unit can undertake