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pellet machine xrf

6 things to consider when making pressed pellets for xrf analysis

6 things to consider when making pressed pellets for xrf analysis

XRF (X-ray Fluorescence Spectrometry) is a chemical analysis tool commonly used for the quality control of raw materials and finished products in many industries including cement, mining and industrial minerals. The capabilities of XRF instrumentation have advanced significantly in the past decade in both sensitivity and stability such that they are no longer the most important source of error in an analysis. Sample preparation is now by far the most significant source of error in the analysis of materials by XRF. Viewed from this perspective, it is clear that high quality sample preparation techniques and practices are the key to achieving consistent and reliable analytical results.

One of the most common methods of preparing samples for XRF analysis is by making pressed pellets. This process is particularly popular as it produces high quality results, is relatively quick and is a low cost approach.

The process of making pressed pellets for XRF analysis includes grinding the sample to a fine particle size, mixing it with a binder/ grinding aid in a grinding or mixing vessel, pouring the mixture into a pressing die and pressing the sample at a pressure of between 15 and 35T. The resulting pellet or tablet is then ready for analysis. While this is a common and relatively straightforward approach to preparing samples for XRF analysis, there are several important aspects that should be considered when designing a sample preparation protocol. These include the particle size of the sample, the choice of binder, the dilution ratio, the amount of pressure applied to the sample and the thickness of the final pellet. An additional consideration is sample contamination.

One of the key aspects of preparing pressed pellets is to make sure that the sample is ground to a particle size of <75m, but <50m is ideal. Depending on the sample type and volume, this can usually be accomplished with a few minutes of grinding with a typical ring and puck pulverizing mill. Small particle size is an important factor in producing pellets that provide the best analytical results because it effects how the sample will compress and bind together when pressed. More importantly, samples with larger or variable particle sizes can lead to heterogeneities in the sample. The sampling depth or critical escape depth for elements contained in a sample is energy dependent and, therefore, different for every element. Longer wavelength elements such as Na will have smaller escape depths than shorter wavelength elements such as Fe. This means that Na analysis is only sampling the first 10m or so of a sample and thus more susceptible to sample heterogeneities on that scale.

Larger particle sizes can result from the presence of hard-to-grind phases in a sample resulting in variable grinding of the sample. The presence of larger particle sizes at the analysis surface of the sample can lead to analysis errors through the "shadow effect" where larger grains shadow the X-ray signal coming from the smaller grains at the surface of the pellet.

The sample binder is literally the glue that holds the sample together. The optimal binder is usually a cellulose/wax mixture that homogenizes with the sample during grinding and will recrystallize under pressure to bind the sample together. These binders are available under various commercial names but are generally similar. Sometimes acrylic binders are used, but these are difficult to homogenize with a sample in a mill and need to be mixed by hand. Some binder grinding agents are available as pre-mixed pellets that can be automatically added to a mill during grinding.

The amount of binder added to a sample is an important consideration because it dilutes the sample and must also be added in the same proportion to every sample in order to avoid dilution errors. Since most modern XRF instruments provide substantial intensity for major elements it is safe to use a significant amount of binder in order to insure a good strong pellet. Weak pellets run the risk of breaking in the spectrometer potentially causing damage to the instrument. A 20-30% binder to sample ratio will almost always produce a very strong pellet that can be dropped onto the ground from a half a meter without breaking. If consumable costs are a concern, a lower binder/sample ratio can be used with some experimentation in order to determine the optimal dilution level.

Once a sample and binder are mixed, the material is pressed in a die using a hydraulic sample press. The pressure applied to a sample should be sufficient to compress the sample completely and recrystallize the binder. One of the most important factors is making sure that the sample is fully compressed so that no void spaces remain in the pellet. A pellet may look good but still contain void spaces which can result in a lowered intensity for lighter elements. You should experiment with your samples using increasing pressure until the intensity for the light elements reaches a maximum and stabilizes. Most samples will reach this maximum at 25-35T of pressure applied for 1-2 minutes. It's also important to release the pressure applied to a sample slowly to prevent cracking of the sample surface.

The thickness of your pellet is important to achieve the best analytical results. The pellet must be infinitely thick to the X-ray beam for all of the elements that are being measured. X-rays produced in the sample must be able to escape the sample without being reabsorbed in order to make it to the detector to be measured. Higher energy elements (usually those with higher atomic numbers) will have deeper escape depths in a sample relative to lower energy elements. The signal coming from higher energy elements sample more of the pellet than those coming from lower energy elements. The sample's ability to reabsorb X-rays is directly proportional to the sample's average atomic mass. The absorption capability of any sample can be calculated from its average elemental composition and the mass absorption coefficient for each element present.

The problem arises when the escape depth of a particular element is larger than the thickness of the pellet. Because this is an element dependent issue, a particular pressed pellet may provide good results for some elements but not others. In general, you should make sure your pressed pellet is thicker than the escape depth of the highest energy element you want to measure.

Usually a pellet made with 8-10g of sample for a 32mm diameter pellet or 13-15g of sample for 40mm diameter pellet will be sufficiently thick for the elements that can be measured by even the most powerful WDXRF instruments currently available.

Sample contamination is an additional consideration in the preparation of high quality pressed pellets for XRF analysis. Contamination usually occurs during the sample grinding process and originates from two main sources: the sample preparation device and sample to sample cross contamination.

Sample pulverizers are the sample preparation devices that have the potential to contribute the most contamination to a sample. Pulverizers usually use a ring and puck style grinding bowl to grind samples from coarse chips to a fine powder. This grinding action can add various elements contained in the grinding vessel to your sample which is why care must be used in choosing your grinding medium. Steel, tungsten carbide and ceramics such as alumina and zirconia are the most common choices. Steel can add Fe, Ni and Cr, tungsten carbide will add W and alumina and zirconia will add Al and Zr respectively. It is, therefore, important to consider what elements are being analyzed and choose the grinding vessel accordingly to avoid contamination. Tungsten carbide is often a default choice because of its hardness and because W is usually not a key element for analysis in many applications. The downside is that tungsten carbide is often the most expensive option.

Sample to sample cross contamination in the sample preparation process is potentially the biggest overall contributor to sample contamination. This is particularly true when working in an environment where a wide range of sample types are being analyzed.

XRF is by definition a comparative elementalanalysis technique where the instrument is calibrated with certified reference materials and unknown samples are measured against the resulting calibration curve for each element or oxide. It is therefore critical that all calibration standards and unknown samples be prepared in the same manor to ensure the accuracy of your analysis. Given this requirement you will need to develop a method that will address the issues detailed in this article for the full range of calibration materials and routine samples that you will need to analyze in your laboratory.

The most common contributors to error in the preparation of pressed pellets include the particle size of the sample, the choice of binder, the dilution ratio, the amount of pressure applied to the sample, the thickness of the final pellet and sample to sample cross contamination. The best practices for limiting this error require good method development coupled with attention to detail and consistency.

We can provide a complete range sample preparation equipment and reference materials for XRF analysis. Need some help ? We have a team of specialists who have extensive experience with XRF as well as other analytical techniques. Our team can help you choose the right sample preparation method, reference material or provide some insight into your analytical challenges.

hydraulic presses, xrf sample preparation, spm, hydraulic machines, laboratory testing equipments, kbr die press, thane, india

hydraulic presses, xrf sample preparation, spm, hydraulic machines, laboratory testing equipments, kbr die press, thane, india

Table-top Model Compact & elegant design with safety screens Smooth, simple & effortless operation Powder-coated surface finish Pressure Gauge calibrated in Tons & Kg/sq. cm. Excellent quality seals provide a leak-proof system All contact parts hardened & hard-chrome plated

Table-top Model Compact & sturdy design Side Plate Construction integral with hydraulic cylinder Pump is kept on one side for easy operation Press mounted on a broad base for stability Calibrated pressure gauge & high pressure seals Safety mechanisms to prevent excessive ram stroke & excessive pressure.

Compact Table-top Model Effortless Operation & Excellent Quality Seals Pressure Gauge Calibrated in Tons & Kg/sq. cm. Heating by Cartridge Heaters & Cooling by Chilled Water Thermocouple for temperature sensing PID Temperature Controller for controlling Platen temperature Special Insulation Sheets for heat insulation Made to order Control Panel

Compact design and easy to operate electrical controls with Pressing and Ejection cycle. Pressing Cycle has both Auto and Manual modes whereas Ejection cycle has only Manual (Inching) mode. Steady pressure building and controlled release ensures better pellet quality. Desired Pressure is set on manual pressure switch & actual pressure indicated by made to order Glycerine filled pressure gauge (indicator) Pressure hold time can be set on the timer provided on the front panel. Settable parameters :- pressure & pressure hold time. Safety mechanisms to avoid over pressure and excessive ram stroke.

We, M/s. Kimaya Engineers, are in the business of manufacturing since as early as 1981. We are manufacturers of Hydraulic Lab. Pellet Presses and Pellet Dies for various R & D Applications involving Pellet Preparation from Powder Samples, such as IR / FTIR Solid Sampling, XRF Sample Preparation etc.

We have the expertise to offer various types of Hydraulic Presses and Other Accessories, to meet a wide variety of research applications. Our design skills and stage wise quality control measures enable us to meet the high standards and requirements of Reputed Clients. Use of only reputed bought-out items is strictly followed. Due consideration is given to safety aspects as well as aesthetics.

B - 12, Digvijay Estate No.2, Pokhran Road No.1,J.K. Gram Post, Upvan Area, Dist :Thane, Thane (W) Pincode : 400606, State : Maharashtra, INDIA (Site is located at 15 to 20 minutes from Mumbai.) / 9869004560 [email protected] [email protected]

xrf pellet press

xrf pellet press

The dies can be identified by removing the cap and observing the die body. The standard die will have a smooth cylinder, where the premium die will have a cutout for the accommodation of a plastic ring. Remove the ring from the die and extend the die shaft until it clicks into place. The shaft can also be removed completely for cleaning. If the shaft is removed, simply insert it back into the die body. When extending, the die will support itself and can be placed unto the table. Insert the funnel into the die. Using the 10-mil sample spoon, measure out a portion of your sample to place into the die. A dry, fine powder will produce the best results.

Introduce the sample into the funnel. If bridging occurs or the sample does not flow completely into the die, tap the funnel and/or die body lightly. When using the standard sample die, the volume is less critical because it is possible to produce pucks of varying thickness.

When using the premium die, at this stage you will insert the plastic ring into the die. The rings are tapered and will only fit into the die in one direction. If the ring does not insert fully, flip the ring over. Using the 10-mil sample spoon, measure out a portion of your sample to place into your die.

Place the lid unto the die and turn to lock the lid. Only turn so that the pin is engaged in the slot. Do not tighten, as the lid can become locked. Do not press down on the die until the lid is in place and latched.

The sample is now ready to be pressed. The press uses hydraulic pressure to press the sample and operates at high pressures. When pressurized, do not touch any hoses or fittings. Unlatch the door to the press and place sample die into the press. Insert the die fully, utilizing the provided guides.

Close and latch the door. Turn the cap to vent. Unlatch the handle locking mechanism and ensure the pressure relief valve is closed and begin to pump. Use full strokes of the pump when pumping to ensure the second stage of the pump is activated.

Observe the pressure gauge and increase pressure until the needle is in the green zone as indicated by the gauge. The pump is regulated to provide up to 5000 PSI. However, ensure that this pressure is not exceeded. Pressure will decrease slightly as the sample is compacted. Once it is stabilized, approximately 5-10 seconds, the pressure can slowly be released by opening the relief valve. Allow the pressure to release fully. Once released and the cylinder is fully retracted, open the door and remove the die.

Remove the cap off the die. If youre using the standard die, the sample is ready to be pressed out. If youre using the premium die, grasp the die body and pull the shaft while twisting to extend the die, then reinsert. This loosens the ring from the shaft and makes removal easier. Close and letch the door. Close relief valve and begin pumping.

The die will rise against the top of the press and the sample will be progressively pressed out of the die. During this process, observe the pressure gauge. The pressure should not exceed a few hundred PSI. If it does, check everything is in order before continuing. Once the sample is completely free of the die, open the pressure relief valve.

The step for the use of the premium sample die are the same as those used with the basic die, except the ring is in place. A variety of cleaning tools are provided in the accessories case. Use these tools to clean excess material form the die parts between runs to minimize contamination.

The denser, flatter, a more uniform puck provides a more reliable surface from which to gain a quality analysis. With no film required between the XRF analyzer and the sample, the risk of a weaker or poor signal is eliminated. The same puck can also be used with other non-destructive testing techniques such as spectral analysis and LIPS.

Optimal pXRF sample analysis relies on a homogenous, densely packed and uncontaminated sample puck. The risks inherent in decisions made on unreliable sample data, are significant and may include the misrepresentation of traces of ore either present or missing.

There are a wide variety of techniques for sample preparation for XRF analysis and the use of XRF cups is common. However, these tend to be expensive, fiddly and time consuming, and very hard to control the sample quality [poor packing, uncompacted].

REFLEX has addressed these risks in the REFLEX PRESS. The innovative sample press is a high-pressure hydraulic press designed to produce a densely-packed, homogenous, sample puck that can be measured by the pXRF [and a range of non-destructive sensors] without the signal attenuation resulting from the use of a film coating and/or poor packing.

The REFLEX PRESS is safe and reliable, engineered and constructed using only high quality, fit for purpose, products. It is also rugged and portable, ideal for use in field camps and onsite laboratories.

The REFLEX PRESS uses high pressure to convert powders to a coherent pressed puck without the need to use binders or costly containers. Removing the need to use sample cups equates to savings of up to $150 per day.

The denser, flatter and more uniform puck provides a more reliable surface from which to gain a quality analysis. With no film required between the pXRF analyser and sample, the risk of a weaker or poor signal is eliminated. The same puck can also be used with other non-destructive testing techniques such as spectral analysis and LIBS.

The REFLEX PRESS comes with a custom designed funnel and sample die to ensure the highest quality, consistent and repeatable, sample puck ensuring data confidence and improved analysis, especially for light elements.

Using the pressed puck and the REFLEX XRF, light elements such as Al have a consistently higher response (8-15%). This will flow through to decreased detection limits and better precision for light elements. The consistent workflow of the REFLEX PRESS will also reduce inter-sample variation resulting from poor packing of material and other inconsistencies, making data analysis more reliable.

The REFLEX PRESS together with the REFLEX XRF Solution (which includes REFLEX XRF, REFLEXHUB-IQ and REFLEX ioGAS) provides the first on-site geoanalysis solution available in the market. This enables decisions to be made on-site, saving both time and money.

The REFLEX PRESS is provided with two separate dies for the making the puck. The STANDARD puck is produced without a protective sleeve and is most useful for minimising costs when the sample will be discarded after analysis, or analysis is performed immediately after pressing. The PREMIUM puck is produced within a custom plastic sleeve that makes the sample very robust for longer term storage, potential re-assaying or archive, and reduces cleaning time after each sample. The plastic sleeves are sold in boxes of 500 and can be easily labelled for reference.

sample preparation of pressed pellet xrf/xrd cement analysis

sample preparation of pressed pellet xrf/xrd cement analysis

Weknow that dependable analysis relies onconsistent sample preparation. Whatever your requirements, our range of pulverising, pressing and fusing equipment control sample quality at every stageto give yourepresentative and repeatable samplesas well as precisex-ray analysis.

Allofourunitsareeasyand safe to use,and especially designed to improveefficiency in your laboratory. Whetheryou select amanual ora fullyautomaticQCXdevice,youll find the digital control and touch screen make it simple to run.The high-output automatic machine feature a range of automated functions that cut back on time-consuming manual tasks, leaving your laboratory analysts free to perform more meaningful work.

The safety of your workers is a priority for you, and for us, too.Our machinesare fitted with safetyfeatures like auto-stop mechanisms,andprotective shieldsto prevent injury from debris. Good,ergonomicdesignis at the heart of what we do.Soyou can focus on results, safe in the knowledge that thecomfort andwell-being of your staffis in hand.

And, the innovative soft pressing technology of theQCXASP100 Automated Soft Press is specifically designed to handlea varietyofmaterialswhile successfully limitingthe biascaused bythepreferred orientation of mineral phases.

When faced with fast turnaround demandsin your cement laboratory, you cant go past the QCX P40M Manual XRF Press-a compact and powerfulmachinethat can achieve both high press forces and high sample throughput.You canenterup to16 processing programs,with fully adjustablepressing parameters. Thispracticalunitgives youprecise control and reliable performance.

We know that, inindustries where accuracy and precision are essential in sample preparation,you need the highest quality equipment so that contamination is minimised. That is why we offer arange of sample preparation equipmentwhichare hard to beat when it comes toquality performance and reliability of results.

Automated and manual pulverising mill configurations are available and operate as a standalone machine or as part of a robotic cell.You can rest easy knowing that our state-of-the-art technology meanssamplescanbe prepared rapidly in an environment where cleanliness and efficiency are top priorities.

FLSmidth provides sustainable productivity to the global mining and cement industries. We deliver market-leading engineering, equipment and service solutions that enable our customers to improve performance, drive down costs and reduce environmental impact. Our operations span the globe and we are close to 10,200 employees, present in more than 60 countries. In 2020, FLSmidth generated revenue of DKK 16.4 billion. MissionZero is our sustainability ambition towards zero emissions in mining and cement by 2030.

xrf pellet press | laval lab

xrf pellet press | laval lab

This manually-operated hydraulic Pellet Press is ideal for fast and easy preparation of both solid and highly permeable pellets of solid samples for X-ray fluorescence analysis or infrared spectroscopy.

Different pressing tools are available for pellets with 40, 32, 15 or 12 mm. Its as easy as this: fill in the sample, close the magnetically-held door and build-up the desired pressure using the hand lever thats it.

The Atlas 15T and 25T manual presses work by hand pumping a hydraulic fluid (oil) to raise a piston and compress a sample held in the pressing area. The press consists of a pump block assembly, where the oil is pressurized by the simple pumping action from a handle, and nthe sample pressing side, where the pressurized oil is forced under the piston assembly. When resistance is offered by a sample, the pressure builds up in the system is shown on the 15 or 25 Tons load gauge, located on the pump block assembly.

The Atlas 15T and 25T manual presses work by hand pumping a hydraulic fluid (oil) to raise a piston and compress a sample held in the pressing area. The press consists of a pump block assembly, where the oil is pressurized by the simple pumping action from a handle, and nthe sample pressing side, where the pressurized oil is forced under the piston assembly. When resistance is offered by a sample, the pressure builds up in the system is shown on the 15 or 25 Tons load gauge, located on the pump block assembly.

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