Sample preparation is the most restricting barrier in the analytical process. Furthermore the credibility of an analytical method depends on the quantitative conversion of a solid into a homogeneous solution. The traditional method for wet sample preparation is matrix dissolution. A large volume of reagent (15 - 100ml) is heated for several hours with a hot plate or oven. This process is finished when the analyst decides “at sight” that the digestion is complete.

The disadvantages of this type of digestion are:

- the large quantities of reagents employed,

- potential for contamination

- continuous release of hot acid vapour into the laboratory environment.

An alternative method is microwave decomposition which uses a completely different technology that improves digestion efficiency and increases the safety of laboratory personnel. This is because microwave instruments have been specifically designed to improve the process of the sample preparation.

In view of the advantages of microwave assisted sample preparation, organisations such as the USA Environmental Protection Agency (US-EPA) developed a range of methods that employ this innovative technology. These procedures enable the rapid analysis of metals in water samples (US-EPA 3015) and of metals in soils (US-EPA 3051, US-EPA 3052). The US-EPA3052 method describes the procedure for total sample digestion. In particular, it refers to the treatment of matrices containing silicates (soils, sediments) and organic matrices (soil polluted by oil and hydrocarbons).

The microwave technique can also be applied to determinations of organic pollutants e.g. pesticides, herbicides, phenols, PCB and PCDD/PCDF. For example, the most commonly used method is US-EPA3546: its application enables the sample preparation needed for chromatographic analysis.

US-EPA3546 requires a treatment time of just 30 minutes. The main advantage apart from time-reduction is the efficiency of the process in which solvent and solute are at the same extraction temperature.

Instrumentation: The success of modern microwave systems is due to two major aspects: the high technological level and the maximum ease of use. All parts including software and hardware have been built to reach maximum quality standards allowing the operator to optimize the sample preparation process. These units are equipped with the latest generation sensors for temperature and pressure control in all vessels. Particular attention has been made to the engineering of various types of vessels both in the choice of materials and in the safety systems: they can only release the excess pressure from the vessel.

Future Possibilities And Versatility Of The Technique - Analytical laboratories need different products and matrices are very heterogeneous; therefore, the manufactures have decided to develop and produce carousels with different technical specifications both for different temperature and pressure limits. These solutions increase the versatility of microwave platforms and offer the best solution for all the application fields. The Milestone ETHOS 1 further develops this concept, since it is not dedicated totally to acid digestion, but also to solvent extraction, evaporation and microwave fusion. Four major applications are available with one system.

For further information please call 1800 251 799 or email info@johnmorris.com.au

Coal burning plants are widely recognized as the largest source of man-made mercury pollution. This has lead to stronger regulations on allowable mercury emission creating a greater need for fast, reliable mercury testing in coal and coal combustion products.

Milestone DMA-80 Direct Mercury Analyser enables users to directly analyse coal and coal ash samples in approximately 7 minutes and eliminates the need for expensive chemicals and labour intensive sample preparation. Simply place the sample directly in the instruments and press Start. A built-in 40-position auto sampler allows unattended operation while a wide dynamic range, and low detection limits provides maximum throughput, accuracy, and versatility.

Direct Mercury Analysis is an industry accepted process and has been used to generate US EPA Method 7473 “Mercury In Solids and Solutions by Thermal Decomposition, Amalgamation, and Atomic Absorption Spectrophotometry” and ASTM Method D-6722 “Total Mercury in Coal and Coal Combustion Residues by Direct Combustion Analysis”.

Milestone’s DMA-80 Direct Mercury Analyser enables clinical laboratories to directly analyse blood, hair, nail, and urine samples for trace level mercury (from 0.005 to 1000ng) in minutes, without the need for sample preparation or chemical processing.

With a built-in 40 position auto sampler, unattended operation, and no waste disposal requirements the DMA-80 provides many advantages when compared to conventional methods.

Testing for mercury in fish has become a primary focus point for private and public organisations. Important regulatory and scientific decisions are made depending upon the mercury levels found in fish tissue. Therefore fast and accurate method are required for mercury determination.

Milestone's DMA-80 Direct Mercury Analyser effortlessly analyses liquid and solid samples without sample preparation or waste disposal. The DMA-80 automatically process 40 samples in approximately  4 hours, from start to finish. An intuitive controller uploads sample weights, controls the analysis, and processes data - with built-in report generation.

The Milestone duoPUR is a unique system for sub-boiling the distillation of acids, water, and reagents for ultra-trace applications.

By using a duoPUR system, ultra-trace water and acids can be prepared from standard reagent grade, saving up to 90% of the cost of purchasing ultra-pure reagents.

The duoPUR is microprocessor controlled and programmable for efficiently distilling different acids and mixtures. All parts in contact with purified reagents are constructed of high quality quartz and PTFE materials.

John Morris Scientific are pleased to offer Milestones large industrial grade muffle microwave ashing furnace – the PYRO.

The PYRO can reach temperatures of 1000°C from room temperature in less than an 1 hour (for a remarkable savings in energy costs). The outside of the PYRO stays cool so the ambient temperature of the lab is unaffected. The ceramic muffle furnace accommodates standard ceramic, quartz, platinum and nickel crucibles.

For methods that require H₂SO₄, the optional PYRO SA module enables analysts to add sulfuric acid directly to a sample without a preliminary charring step, while safely ramping the temperature and evacuating and neutralizing acid vapours.

In Pharmaceutical, Cosmetics, and Personal Care industries there are many guidelines to follow. Those working in Quality Control and Quality Assurance often have the toughest guidelines.

There is often a need to quickly and accurately determine the total inorganic content in samples to satisfy USP method 281-ROI & 733-LOI, as well as meet ASTM D5630-94, ASTM D1506-99 requirements. Milestone's PYRO Microwave Ashing System meets the requirements for "electronically heated" furnaces in these USP methods, and the requirements for applications using a "microwave-heated" furnace.

Unlike conventional muffle furnaces, the PYRO can reach 1000°C in less than an hour, making it up to 20× faster than traditional methods. Therefore it is energy efficient and cost effective. The PYRO features a special insulation which reduces heat loss and transfer to the surrounding area, while the built-in exhaust system prevents exposure of chemical fumes to laboratory personnel.

Frequently, ashing test procedures performed on pharmaceutical samples involve the use of H₂SO₄. Hot sulfuric acid vapour released during these labour intensive and time consuming procedures is both hazardous to analysts and corrosive to surrounding equipment. An optional module allows analysts to add H₂SO₄ to samples, then place crucibles directly into the system without a preliminary charring step. Samples are complete in approximately an hour, eliminating tedious handling/monitoring of samples and operator exposure to acid fumes.

Microwave Accelerated Synthesis has become an accepted technology across a range of industries including pharmaceutical, fine chemical, biotech, polymers and agrichemical. As a result, there is a growing demand for the ability to scale-up these reactions from grams to kilograms.

Milestone is pleased to offer the MicroSYNTH Microwave Scale-Up System for performing parallel, batch, and continuous flow reactions with the same platform. This unique system can be configured to meet your specific needs and easily adapted as your needs change in the future.

Method Optimisation and Parallel Processing – Process single or multiple reactions simultaneously under identical conditions using your existing chemistry.

Batch Reactions – The MicroSYNTH has a volume of 300 mL and can operate at sustained temperatures of 230°C and 30 bar, without any loss of reagents or volatile fractions.

Continuous Flow Reactions – The MicroSYNTH allows you to scale-up from millilitres to litres with an adjustable flow rate of 12 to 100 mL/minute, all while retaining complete control of all reaction parameters.

The Milestone ETHOS 1 is specifically designed for sample preparation and provides analysts with the possibility to perform fusion by microwave for the first time.

Fusion is enabled by the MultiFAST-4 rotor which complements the ETHOS 1 system and extends the range of application possibilities, representing a significant innovation and enhancement for its consolidated capabilities.

A variety of difficult samples including cements, ores, slag, sediments, soils, feldspatic rocks, ceramics, pigments, glasses and quartz can be successfully prepared for XRF, AA and ICP analysis.

With silicon carbide crucibles the Milestone MultiFAST-4 is the only microwave fusion system available which and reach up to 1,000°C in few minutes.

Milestone’s MicroSYNTH, MultiSYNTH and FlowSYNTH microwave laboratory stations allow synthetic and organic chemists to run reactions faster than ever before, with higher yields and better purities.

The MultiSYNTH also allows researchers to scale up experiments from milligrams to kilograms without needing to alter reaction parameters.

Milestone’s microwave enhanced synthesis offers precise control over conditions of temperature and pressure while maintaining unsurpassed ease of use. Milestone has a complete line of microwave instrumentation which provide synthetic laboratories with the ability to:

• MicroSYNTH - manufacture compounds from small quantities
• MultiSYNTH - the flexibility of scale up from small quantities to large quantities
• FlowSYNTH - batch flow