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C Elementar Vario MICRO Cube.Pdf The roots of success 100 years ago, in the center of Germany, near Frankfurt, the Elementar has coupled the latest developments in micro high technology industrial company Heraeus developed electronics and mechanics with the vast experience in and manufactured the world‘s first elemental analyzer for elemental analysis. Newly developed separation and organic substances. detection methods have been utilized. From that foundation, a continuous progression of tech- Even the form and color of the new instrument line offer nology in elemental analysis products leads to the estab- improved clarity of the basic concept and special demands lishment of Elementar. Still at the same location today, of elemental analysis. Elementar is the world‘s leading producer of instruments for the analysis of C, H, N, S and O. Given Elementar‘s century long expertise, it is not surpri- sing that our newest development is particularly special. ~ Wide variety of elements measured from nearly all types of samples. ~ Highest precision and accuracy of the analytical results. ~ Unsurpassed reliability and long time stability. ~ High ease of use with a very innovative design. ~ Lowest operation costs and set up requirements. Heraeus Micro Analyzer 1930 The instrument concept - simply sophisticated The measuring principle is impressively simple as shown in the functional diagram. The samples are weighed in tin or silver vessels and loa- The gas mixture is separated in its components on a ded in the integrated carousel for 120 samples. In a fully column by the newly developed temperature programmed automatic process, the transfer of the sample through the desorption (TPD) and is subsequently fed into a thermal ball valve into the combustion tube is performed. conductivity detector (TCD). Each sample is individually flushed with inert gas (Heraeus The TCD is based on thermistor technology, is impervious patent) to remove atmospheric nitrogen, resulting in a zero to damage from oxygen intrusion, and stands out for parti- blank sampling process. cularly high stability and measuring dynamics. The catalytic combustion is carried out at a permanent Right before the detector an electronic gas flow controller temperature of up to 1200 °C. Unique is the furnace war- ensures absolutely stable pressure and flow conditions. ranty of 10 years! This results in a stable instrument calibration over months or even years. For special applications, even 1400 °C can be selected. A connected PC computes the element concentration from Subsequently, the reduction of the combustion gases on the detector signal, and the sample weight on the basis of hot copper is carried out in a second furnace. The formed stored calibration curves. analysis gases, N2, CO2, H2O and SO2 remain in the He car- rier gas stream (alternatively argon carrier gas). He/Ar O2 He/ArRef. Combustion Gas Separation Detection TPD for High Concentration Dynamics Peak graphic - wheat flour (5 mg) N C H S N C H S TCD-Signal (1.94%) (41.18%) (6.74%) (0.12%) (1.94%) (41.18%) (6.74%) (0.12%) TCD-Signal TPD Tem [°C ] 18000 240 1400 16000 220 1200 200 14000 180 1000 12000 160 140 11000 800 120 8000 600 100 6000 80 400 60 4000 40 200 2000 20 0 0 0 0 100 200 300 400 500 600 0 100 200 300 400 500 600 700 t [s] t [s] μg N [y] C-Calibration, entire range μg C [y] N-Calibration, entire range 7765.2 3001.6 0.0 0.0 0.00 peak area (x) 19100814.00 0.00 peak area (x) 10318609.00 The perfect gas separation For the first time, the principle of thermal programmed desorption (TPD) is applied in an elemental analyzer. The CHNS elemental analysis is based on the high tem- Each heating step takes place only after the completion perature combustion and subsequent analysis of the com- of the subsequent peak detection on the TCD. A complete bustion gases. The quantitative separation of the analyte baseline resolution is achieved even for large amounts of gases N2, CO2, H2O and SO2 in the He or Ar carrier gas organic material (up to 7 mg carbon content), as well as for prior to the detection is crucial for the performance of the large relative concentration differences (e.g. low nitrogen complete instrument. with high concentration of carbon). Analysis time is also optimized using this process. Thereby Elementar breaks new ground with the vario MICRO cube. All four analyte gases are separated on one This results in a performance comparable to the great column, by the use of 4 stepped temperatures (patent separation ability of the „purge and trap“ gas separation. pending). With just one column, the TPD system corresponds in sim- plicity to gas chromatographic separations, but without At near room temperature, N2 fl ows unimpeded through the signifi cant compromises of separation ability and drift the column while CO2, H2O and SO2 are adsorbed. After the problems. detection of the N2 peak, the column temperature is quickly increased to approximately 60°C, which releases the CO2. While TPD separation allows for the simultaneous determi- After detection of the CO2, the column is stepped to over nation of the elements C, H, N and S, it is also possible to 100°C for release and detection of the H2O. Finally, the SO2 confi gure for the determination of only one, two or three is desorbed at a column temperature of over 200 °C. elements (i.e. CHN, CNS, CN, N or S). In these cases, the dynamic range of the analyzer can be extended (e.g. > 10 mg carbon in CN mode), and time per analysis is reduced (~3 min for N). User Interface Instrument Software Audit T rail in accor dance to 21 CFR Part 11 System Check Digitalization in the user‘s interest In our time an analytical instrument can only be as good as its micro electronics and software. The vario MICRO cube sets new standards as the first ele- The design and operation of the Windows based software mental analyzer in which all instrument functions are digi- is a key component of our whole system. Our software is tally controlled and monitored. This results in completely written and developed at our own premises by our own new possibilities of automatic operation, optimization as personnel according to strict ISO 9001 requirements. well as remote control and diagnosis over the internet. The software allows for a continuous monitoring of real The basis for this is the use of the new micro processor time conditions of the analyzer in both numerical and generation with 24 bit signal processing and electronic graphical forms, easy and efficient input of run information sensors for all gas flows and pressures. with automated functions, cut and paste data to or from Excel, as well as statistical analysis options. The vario MICRO cube‘s firmware (internal software of the analyzer) is stored on flash EPROMS, which can be eas- The system is designed for intuitive operation, but content ily updated via PC or the internet. The critically important sensitive help is just a click away. Automatic optimization fast signal communication between components in the of parameters, monitoring of maintenance intervals and analyzer (such as the detector signal) is handled by the service messages, LIMS data transfer are all integrated fail-safe CAN bus technology. into the system. Graphical leak checking with pictorial guides for each step are a new favorite feature of users. A commercial PC or laptop serves as the user interface for control and evaluation. Our software runs under the We also feature our unique browser based pictorial parts Windows operating system and offers features and capa- list, with drill down operation and exploded component bilities too numerous for a complete listing here. diagrams. Data safety and validity can be assured with the available 21 CFR Part 11 compliant option. Carbon * Hydrogen * Nitrogen * Sulfur * Sulfanilic Acid 41.54 ± 0.03 4.01 ± 0.01 8.14 ± 0.019 18.51 ± 0.006 Measurements: 6 Weight: 1 mg N-F-dibenzolsulfonimide 45.65 ± 0.07 3.20 ± 0.01 4.46 ± 0.01 20.20 ± 0.2 Measurements: 6 Weight: 1 mg Benzylcysteine * HCI 52.97 ± 0.063 6.85 ± 0.010 6.82 ± 0.023 15.52 ± 0.022 Measurements: 6 Weight: 1 mg Spruce Needles 49.13 ± 0.05 6.41 ± 0.04 1.84 ± 0.01 0.10 ± 0.01 Measurements: 6 Weight: 1 mg Soil 0.216 ± 0.004 0.457 ± 0.003 0.007 ± 0.001 0.0052 ± 0.0005 Measurements: 5 Weight: 50 mg Coal 75.49 ± 0.09 4.90 ± 0.01 1.93 ± 0.02 0.51 ± 0.03 Measurements: 6 Weight: 7 mg Mineral Oil 87.62 ± 0.06 9.46 ± 0.02 0.21 ± 0.01 1.27 ± 0.04 Measurements: 6 Weight: 6 mg Teflon 24.51 ± 0.12 – – – – – – Measurements: 5 Weight: 1 mg Glass Fiber Filter 0.166 ± 0.008 0.026 ± 0.002 0.114 ± 0.007 Measurements: 6 Weight: 400 ml Chlorine * PVC 40.40 ± 0.05 5.13 ± 0.04 – – 44.36 ± 0.89 Measurements: 6 Weight: 2 mg * Element concentration in [%], Standard deviation in [%] One instrument – a world of applications The vario MICRO cube is the ideal instrument for the universal elemental analysis of CHNS, as well as optional O and Cl. The applications cover all organic and the majority of Element concentrations of well below 100 ppm to 100 % inorganic samples of solid or liquid material. Its special are detectable with the standard detector (TCD). strength lies in the sample weight in the lower milligram range regarding detection limit, concentration dynamics For even lower detection limits, special detectors can and the possibility to also analyze difficult samples e.g.
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