774 Oven Sample Processor Revolutionary automation of Karl Fischer water determinations right down to the trace level. Karl Fischer instruments Methodological and economic advantages A new concept opens up attractive applications With the 774 Oven Sample Processor Metrohm presents a revolutionary new sample changer. It allows the application of the KF oven method to a series of liquid or solid samples. Combined with a coulometric or volumetric KF titrator, the Oven Sample Processor forms the ideal analysis system for the automatic determination of water in samples that contain interfering components or release their moisture only reluctantly. Typical examples are • crude oil and oil products such as hydraulic oil, multigrade oil or used motor oil as well as • organic amines, toners, plastics, pharmaceuticals, foodstuffs and freeze-dried products (lyophilisates). Convincing advantages Compared with a conventional KF drying oven the 774 Oven Sample Processor offers many advantages: • The automation of the water determination means a considerably increased sample throughput and increased efficiency. The new 774 Oven Sample Processor with the 756 KF Coulometer. • Considerable savings in time. • Manual sample preparation is reduced to a minimum. • No contamination of the oven and titration cell; this means that there are no carryover or memory effects. • Identical and reproducible analysis conditions for all samples; this is shown by the considerably improved precision of the results. • Much lower reagent consumption as the titration solution only requires changing at infrequent intervals. • Improved water release from the sample as the carrier gas does not pass over the sample but is led directly through it. • The use of hermetically sealed sample vessels means that the samples can be transferred into the vials directly from where they are taken. The PTFE-coated septa guarantee a constant and unadulterated water content even after longer storage periods. Instead of a KF Coulometer a volumetric KF titrator can also be used for the water determination; the new 784 KFP Titrino is shown here. The crimping tool in the foreground, a standard accessory, is used for sealing the sample vials. 2 774 Oven Sample Processor Precise and fast results Gaz inlet tube Needle adapter made of PEEK Heated transfer tube (outled heating) Hollow needle with Luer connection (outlet) Hollow needle (inlet) Infrared sensors Guide rod (adjustable) Detail of the double needle system. The carrier gas takes up the water released by the sample and is then led to the titration cell via the heated transfer tube. The 774 Oven Sample Processor’s tower is equipped with beaker sensors based on infrared light for detecting whether a sample vial is present. Sophisticated construction Refined methodology The Oven Sample Processor is characterised by its extremely compact design. The oven heating block, gas pump, solenoid valve, flow meter and flow controller as well as a drying bottle are already built in. The turntable accommodates 35 sample vessels plus one conditioning vessel. If the «20 mm Headspace Vials» are used the maximum sample volume is 7 mL. Airtight sealing of the vials with PTFE-coated septa ensures that the samples do not take up water from the ambient air. The vial containing the sample to be analysed is moved by the turntable to the appropriate position above the oven and then lowered into the heating block. A double hollow needle pierces the septum of the sample vessel. A stream of dry carrier gas (air or inert gas) is led through the heated sample via the inlet needle, which reaches down to the bottom of the vessel. The carrier gas containing the released moisture flows through the outlet needle and then through a heated transfer tube directly into the titration cell, which is mounted on the chassis of the 774 Oven Sample Processor together with a 728 Magnetic Stirrer. Depending on the water content of the sample, the subsequent KF water determination can be carried out either volumetrically or, at the trace level, coulometrically. Simple sample preparation Sample preparation could not be easier and consists of weighing the sample into the sample vial, sealing it with the crimping tool and then placing it in the rack of the sample changer. Contaminating samples present no problem as contamination is restricted to the particular sample vial. Neither the titration cell nor the oven become contaminated; carryover effects therefore do not occur. All samples are analysed under identical and reproducible conditions, which ensures results of the highest precision. Rapid and precise determination of trace amounts of water in critical matrices – no problem with the new 774 Oven Sample Processor. 774 Oven Sample Processor 3 774 Oven Sample Processor – overview A nice specimen! Lift Gaz inlet tube Air iinlet filter Protective cover Heatable transfer tube Coulometric cell with generator and indicator electrode Doppelhohlnadel 728 Magnetic stirrer Sample rack for 35 Sample vessels and 1 conditioning vessel Durchflussregler Inertgaseinlass Anschlüsse für die Trockenflasche Trockenflasche mit Molekularsieb Plug cover Oven with protective housing 4 774 Oven Sample Processor 774 Oven Sample Processor 5 Neue Massstäbe in Bedienung und Applikation View of the heating block of the 774 Oven Sample Processor and the KF cell in which the coulometric water determination is carried out. Behind the splash guard the double needle system for the carrier gas inlet and outlet can be seen. Flexible and user-friendly Interesting application possibilities The 774 Oven Sample Processor offers freely programmable processing sequences, a removable sample rack and the flexible connection to various Metrohm instruments via the serial RS 232C interface or the «Remote» interface. Standard methods for common applications are preprogrammed in the instrument; this makes routine work much easier. For more demanding applications these methods can be simply modified with user-specific sequences and thus be adapted to the requirements of your analysis. Programming and entering of commands are carried out conveniently in English, German, French or Spanish via the separate keypad. The 774 Oven Sample Processor thus provides the optimal solution for both routine tasks and demanding special applications. The oven temperature can be programmed as required in the range 50 ... 250 °C, the heating rate being up to 15 °C/min. An optimised determination procedure or even a special temperature profile can be developed for each sample and stored as a method. In this way it is possible to heat up sensitive samples gently whereas thermally stable, unproblematic substances can be heated to the required temperature in a very short time. Freely programmable, special temperature profiles offer, for example, the possibility of recording the kinetics of water release as a function of the temperature. Combined with a Metrohm KF Coulometer or KF Titrator, the Oven Sample Processor forms a powerful standalone analysis system for the automatic determination of water according to the KF oven method. Connection of a PC equipped with TiNet 2.4 or VESUV 3.0 Metrodata software opens up even more possibilities with regard to the flexibility of the processes as well as for documentation and data management. 6 774 Oven Sample Processor Technical specifications of the 774 Oven Sample Processor Oven Temperatures Temperature range 50…250 °C Heating power 82 W Heating rate (50…150 °C) 15 °C/min Gas pump Flow range (air) 0…300 mL/min or 0…18 L/h Nominal operating range 5...40 °C at 20…80% relative humidity Transport and storage –20...+60 °C 60 °C <50% relative humidity 50 °C <85% relative humidity 40 °C <95% relative humidity Power connection Display LCD, 2 lines of 24 characters each, height 5 mm Sample changer Voltage 100...120 V, 220...240 V Frequency 50...60 Hz Power consumption 120 VA Capacity 35 sample vessels plus 1 conditioning vessel Sample vessels als» «20 mm Headspace Vi- Design and testing in accordance with IEC 1010 / EN 61010 / UL 3101-1, safety class I Dimensions (approx.) Height 38,3 mm Diameter 21,8 mm Protection code IP 22 Seal Septum cover consisting of a PTFE-coated siliconrubber septum and an aluminium crimp-cap Sample volume Maximum 7 mL Materials Sample changer housing tiple Metal housing with mulstove enamel Keypad housing Crastin (PBTB), inside aluminium-coated Keypad cover Polyester, chemically resistant Safety specifications Dimensions Height 51 cm Width 38 cm Depth 55 cm Weight (without accessories) 15,9 kg Oven Oven block Aluminium Cover PTFE Inner sleeve Chromium steel RS 232C data interface For computer or printer connection Programmable for communication with external devices Remote-I/O-lines Programmable parallel port for controlling external devices 774 Oven Sample Processor 7 Ordering information, options 774 Oven Sample Processor 2.774.0010 774 Oven Sample Processor Highly flexible instrument combining sample changer, oven and gas pump. Accommodates 35 sample vessels («20 mm Headspace Vials») and one conditioning vessel. Programming and manual operation via keypad equipped with a two-line LCD display. Extensive accessories including, e.g., crimping tool, 1000 sample vials and 1000 septum covers. Options Connecting cables 6.2141.020 Cable Remote 774 – Titrino or 756 KF Coulometer 6.2125.110 Cable RS 232C 774 – Titrino or 756 KF Coulometer 6.2125.060 Cable RS 232C 774 – PC (25 pins – 25 pins) 6.2125.110 Cable RS 232C 774 – PC (25 pins – 9 pins) Consumables and additional items 6.2419.000 Sample vials («20 mm Headspace Vials»), 1000 pieces, total volume 9 mL, maximum sample volume 7 mL 6.1448.050 Septum covers, 1000 pieces, consisting of a PTFE-coated silicon-rubber septum and an aluminium crimp-cap 2.728.0040 728 Magnetic Stirrer 6.2816.050 Inlet needle Accessories for mounting the inlet needle at a higher position: 6.1808.040 Adapter, M6 exterior thread, M8 interior thread 6.1808.090 Adapter, M8 exterior thread, M6 interior thread Subject to modifications Printed byMetrohm Ltd., Herisau, Switzerland 11-1999-11 – 8.774.6003 8 774 Oven Sample Processor
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