PYRO Control terminal

• Monochrome touch-screen industrial grade controller 5” screen• Resolution 240 x 128 dots for sharp process graphic• 1 PS2 port for mouse, 1 RS 484 port for microwave unit,

and 1 RS 232 port for external devices• Methods and process reporting data saved on internal memory• External dimensions 22 x 14 x 5 (h) cm

PYRO SA Control terminal

• Touch-Screen- industrial grade controller 6,5” screen with 65.000 colours

• VGA resolution 640 x 480 for sharp process graphics• 1 USB port to connect printer, 2 PS2 ports for mouse and keyboard,

3 RS 232 ports for external devices• Methods and runs saved on Windows™-compatible

removable flash-card

Standard Methods Compliance

ASTM (American Society of Testing and Materials)D5630-94 (Standard Test Method for Ash Content in Thermoplastics)D1506-99 (Standard Test Methods for Carbon Black-Ash Content)

U.S. Pharmacopeia MethodsUSP 281 (Residue on Ignition) (Sulfated Ash)USP 733 (Loss on Ignition)

SEMI (Semiconductor Equipment and Materials International)SEMI F48-0600 (Test Method for Determining Trace Metals in PolymerMaterials)

Technical Specifications

MILESTONE srlVia Fatebenefratelli, 1/524010 Sorisole (BG) - ItalyTel: +39 035 573857 - Fax: +39 035 575498E-mail: analytical@milestonesrl.comwww.milestonesrl.com

MLS GmbHAuenweg 37 - D-88299 Leutkirch im Allgau - GermanyTel: +49 (0)7561 9818-0 - Fax: +49 (0)7561 9818-12E-mail: mws@mls-mikrowellen.dewww.mls-mikrowellen.de

MILESTONE INC.25 Controls Drive - Shelton, CT 06484 - USATel: (203) 925-4240 - Toll-free: (866) 995-5100Fax: (203) 925-4241E-mail: mwave@milestonesci.comwww.milestonesci.com

MILESTONE GENERAL K.K.KSP, 3-2-1, Sakado - Takatsu-Ku, Kawasaki 213-0012 - JapanTel: +81 (0)44 850 3811 - Fax: +81 (0)44 819 3036E-mail: info@milestone-general.comwww.milestone-general.com

UNI EN ISO 9001: 2000 CERT I F I E D

Microwave hardware

• Single magnetron system with rotating diffuser for homogeneous microwave distribution in the cavity

• Magnetron protected from reflected microwave power• Installed power 1200 watt• Output power up to 1200 watt, controlled via microprocessor• Temperature range 20-1000° C• Microwave cavity entirely made of 18/8 stainless steel housing• Large microwave cavity 37 x 34,5 x 33,5 (h) cm• Muffle volume 3,3 litres• Muffle dimensions 242 x 162 x 84 (h) mm• All hardware protected against acids/organic solvents with polymer coating

both on inside and outside surfaces• Total of safety interlocks 4 micro-switches to prevent microwave emission

with door open• All-metal high-flow exhaust system• Acid scrubber module with high-performance double stage PTFE pump

rated 20 mbar vacuum and 40 l/minute flow rate (PYRO SA only)

• Weight ~ 75 kg• External dimensions 57 x 51 x 61 (h) cm• Power 220V/50-60Hz, 2,4 kW

Specifications are subject to change without notice.

PYROPYRO Sulphate Ashing

MILESTONE

M I C R O W A V E S C I E N C E F O R B E T T E R C H E M I S T R Y

R A P I D M I C R O W A V E A S H I N G S Y S T E M

PYROPYRO Sulphate Ashing

The drawbacks of conventional ashing furnacesThe determination of ash content is an important test procedure, performedin thousands of laboratory each day, for process and quality controlpurposes. Ashing tests are also carried out on polymers, pharmaceuticals,food and feed samples, as a prerequisite in analytical procedures.

Conventional muffle furnaces commonly used for ashing samples areinefficient in a number of respects. While ashing is a relatively simpleprocedure, it is time consuming and a tedious task, requiring hours to beaccomplished. The energy requirements and operating costs associatedwith conventional electrical resistance muffle furnaces are quite high.Another drawback of these furnaces is that working condition in laboratorieswhere they are operated are adversely affected. Laboratory temperaturescan rise to uncomfortable levels, as heat diffuses from furnaces, and odorsgenerated from ashing of the samples become present.

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About MilestoneMilestone has been active since 1988 in the fieldof advanced microwave sample preparation.With over thirty patents and more than 9000instruments installed worldwide, we are theacknowledged industry leader in microwavetechnology. Our commitment is to consistentlyprovide the most effective, safest, and highestquality instrumentation for microwave samplepreparation. By listening to our customers, wehave established a history of developing uniquesolutions to real-world problems in analyticallaboratories around the world.

Milestone Innovative PYRO Microwave Ashing System

Microwave ashing a breakthrough for quality control and rapid samplepreparation. Milestone offers two microwave ashing systems to meet theneeds of your laboratory. The PYRO is a highly efficient alternative toconventional muffle furnaces. The PYRO dramatically reduces ashing times,from hours to minutes. The PYRO SA is identical to the PYRO, with an additional module speciallyengineered for sulphate ashing procedures.It allows analysts to add H2SO4 to samples and place crucibles directly intothe microwave muffle furnace without a preliminary charring step. Tedioushandling/monitoring of samples, and operator exposures to acid fumes, areeliminated. The PYRO systems' unique design eliminates equipment corrosion and acidfume pollution, greatly reducing analyst exposure to acid fumes. Theselabstations offer you the fastest, cleanest, most versatile way to ash a widevariety of samples.

PYRO

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PYRO applications

How the PYRO worksA special microwave-transparent ceramic muffle furnace allows microwave energy to pass through and rapidly raise the temperatureof silicon carbide plates located inside the muffle. Porous ceramic honeycomb frits built into the side walls of the muffle furnace allowa constant stream of air to pass over the sample crucibles. The combination of microwave "superheating" and the oxygen from the airflow results in a dramatic reduction of ashing times.

Temperature monitoringA high-precision thermocouple located in close proximity to the bottom of the ashing crucibles (and unaffected by the airflow) monitorstemperatures inside the furnace. The thermocouple's signal is used as a feedback control mechanism to regulate microwave poweroutput and maintain the user selected ramping/ashing temperature.

Choice of cruciblesThe high-efficiency microwave energy coupling characteristics of the silicon carbide heating inserts allows the use of any type of crucible(metal, porcelain, quartz, etc.) within the microwave furnace.

Plastics Food Paper Products

Oil

Pharmaceutical

Coal

High-temperature ceramic muffle

Microwave cavitySiC plate

Air (O2)

Microwave

Exhaust fan

(to fume hood)

Ceramicgrid

Microwave AshingA Breakthrough

for Quality Control and Rapid Sample

Preparation

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Reduced operating costsThe PYRO has an extremely fast heatingrate. A typical ashing temperature of800°C can be reached in 45 minutesfrom room temperature. This eliminatesthe necessity of running the systemovernight, and avoids the lengthy heat uptimes associated with electrical resistancefurnaces, dramatically lowering averagep ower costs.

High sample throughputThe PYRO has an extremely large workingcavity area. You can easily accommodate up to twelvestandard 40 mm wide crucibles at a time.

The PYROsystemreducesashing timesfrom hours tominutes

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To fume hood

More comfortable workingc o n d i t i o n sNo heat added to the laboratory. Thespecial microwave-transparent ceramicmuffle furnace is an outstandinginsulator, minimizing heat loss andtransfer to the surrounding area. Theambient temperature of a laboratory willbe unaffected, even when the unit isrunning at its highest temperatures.

No odors added to the laboratory. Thecombustion of samples containingorganic matter often generates noxiousodors. The built-in exhaust system of thePYRO removes fumes from the interiorof the furnace and directs them throughan exhaust hose to a fume hood or otheroutlet. Unpleasant odors from theashing process are eliminated from thelab environment.

Long operating lifeAll parts of the PYRO system areconstructed of solid stainless steel,unlike domestic microwave units withplastic doors that are both fragile andsusceptible to thermal damage. The unitis specifically designed for laboratoryuse; it is not a modified kitchen-stylem i c r owave. An industrial-grade 12 0 0watt magnetron delivers 1000 watt ofm i c r owave power, microprocessor-controlled, in 10 watt increments.

Faster, cleaner ashing of difficult samplesOur PYRO- F l ow option allows you to processsamples that generate a large amount of volatilesand soot, particularly valuable for the Petroleumand Plastics industries. A perforated quartz tube inthe top of muffle is attached to a compressed airsource and draws out the fumes, volatiles, and sootfrom the chamber. Additional benefits of the PYRO-Flow option include rapid, complete ashing oflarger sample sizes with continuous airflow, efficientexhaust of all pyrolysis gases out of the microwavecavity, and safe and easy to handling and cleaning.

PYROHardwareDesign

Sample Microwave Ashing Microwave Ashing Traditional AshingTemperature (°C) Time (minutes) Time (minutes)

Pet food (ground) 57 5 21 90Cat food 57 5 15 90Po l y p r o p y l e n e 6 50 2 2 80PV C 90 0 15 12 0Po l y e s t e r 60 0 15 4 80Po l y u r e t h a n e 90 0 15 12 0Coal standard AR 278 2 7 50 2 0 12 0Dried egg yolk 9 2 5 2 5 2 40Activated coal 7 50 2 5 180F l o u r 90 0 50 3 60Sa l a m i 60 0 60 3 0 0

TYPICAL ASHING TIMES

The PYRO system dramatically reduces ashing times, from hours to minutes. The following table provides examples of the kind of time reduction you can expect to benefit.

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PYRO SAHow the PYRO SA Sulphate AshingworksThe basic principles of operation are thesame as the PYRO, with the addition of theSulphate Ashing Module and the VAC-1000Acid Scrubber. Sulfuric acid fumes releasedfrom crucibles inside the muffle furnace arecontinuously removed, through a quartztube connected to an air-cooled quartzcollection vessel mounted outside of theunit, and to the VAC-1000 acid scrubbermodule.

PYRO SA Sulphate Ashing SystemAshing test procedures performed on pharmaceutical, polymer, and food samplesfrequently involve the use of H2SO4. Hot sulfuric acid vapor released during theseprocedures is both hazardous to analysts and corrosive to equipment. In addition to thesecomplications, sulphate ashing procedures are typically labor-intensive and time-consuming, requiring manual fuming of acid from crucibles and 8-12 hours to complete.Milestone has engineered a unique microwave system for sulphate ashing procedures. The PYRO Sulphate Ashing system enables analysts to add H2SO4 to samples and placecrucibles directly into the microwave muffle furnace without a preliminary charring step.Tedious handling/monitoring of samples, and operator exposure to acid fumes, areeliminated. The labstation is designed for complete operator safety and long life, and performs thecomplete procedure in only 60-90 minutes.Sulfuric acid fumes released from crucibles inside the muffle furnace are continuouslyremoved, through a quartz tube connected to an air-cooled quartz collection vesseloutside the unit, and to the VAC-1000 acid scrubber module.

The PYRO SA is operated via a compact terminal with bright,full-color, touch-screen display.The terminal runs the Milestone’s unique EasyCONTROLsoftware, to provide simple, user-friendly control of themicrowave sample preparation process.

Industrial grade touch-screen controller.

6,5” screen with 65.000 colours

VGA resolution 640x480 for sharp process graphics

1 USB port for printer, 2 PS2 ports for mouse and

keyboard, 3 RS 232 ports for external devices

Methods and runs are saved on a removable flash-card

State-of-the-Art User Interface

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TYPICAL SULPHATE ASHING TIMESSulphate Ashing ModuleSample Microwave Ashing Microwave Ashing Traditional Ashing

Temperature (°C) Time (minutes) Time (minutes)

L a c t o s e 60 0 60 4 80

NFT 80 0 50 4 80

C e l l u l o s e 80 0 80 50 0

H e a vy oil 5 50 2 3 0 960

A n t i b i o t i c s 8 50 6 5 4 80

Ta rtaric acid 80 0 80 50 0

Fast heating ratesthrough specialceramics

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3

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Highest standards of safetyThe door of the PYRO is made ofstainless steel with a lining of ceramicfibers. In the event of a power failure,the door will not be damaged, even ifthe unit is operating at hightemperatures. The unit also has an over-temperature sensor to protect it fromoverheating within the microwave cavity.Four micro-switches will instantaneouslycut off microwave emissions wheneverthe door is opened.

Optimum temperaturehomogeneityA rotating stirrer on top of themicrowave cavity optimizes microwavedistribution in the cavity, and ensurestemperature uniformity. At 900 °C, a ±5°C temperature uniformity across themuffle cavity is attained.

Fast heating ratesA special Al2O3 v a c u u m - f o r m e d ,lightweight ceramic material allow sextremely rapid ramping/heating cycleswithout any damage to the muffle. Thisceramic material has excellent isolatingp r o p e rties, superior to conventionalceramics used in traditional resistance-heated ashing muffles.

Microwave program editing

Simple and reproducible methoddevelopmentThe PYRO labstation is run by an advanced touch-screen controller with a large graphic interf a c e .EasyCONTROL software offers you simple, user-friendly, intuitive operation. Sophisticated PIDalgorithms will follow your preset temperature curveand allows you to modify all parameters, even in themiddle of a run.

EasyCONTROL softwareMilestone’s new EasyCONTROL software is the mostadvanced and powerful operating system in the fieldof microwave sample preparation. Automatic, real-time monitoring and feedback-based control ofmultiple parameters offers unsurpassed processcontrol. Simply recall a factory stored program orcreate a new one. Press ‘Start’, and the system willautomatically follow the defined temperature profile,utilizing a sophisticated PID algorithm.

Actual temperature profile. The microwave power is automatically adjusted basedon continuous feedback, allowing the ashing to followthe desired temperature profile.

Monochrome touch-screen industrial grade controller 5” screen

Resolution 240 x 128 dots for sharp process graphics

1 PS2 port for mouse, 1 RS 485 port for microwave unit, and 1 RS 232 port for external devices

Methods and process reporting data saved on internal memory

State-of-the-ArtUser Interface

PYRO