Firma:                Perkin Elmer

Modell:              Optima 3000 XL

Kommentar:      Dokumente engl.

Optima 3000 XL ICP

Optical Emission Spectrometer Specifications

System Specifications

Power :                200-240 V, 30A live, single phase, 50 or 60 Hz

Dimensions:        Length: 134.7 cm (53 inches)

                            Height: 144 cm (56.5 inches)

                            Depth: 76 cm (30 inches)

                            Depth with shelf: 103 cm (40.5 inches)

Weight:                454 Kg (998 lb)

Automation: Computer control of all spectrometer funetions, RF generator and plasma gas flows over IEEE-488 Interface.

Environmental: 15 to 35°C with <2.8°C change per hour; relative humidity between 20 and 80% non condensing

ICP System Specifications

Frequeney:                     40 MHz, free-running

Output Power Stability:        <0.1%

Power Output: 800 to 1500 watts, computer controllable in 5-watt increments. RF generator is located in the main Chassis of the instru­ment for efficient use of laboratory space.

RF Shielding: Meets all FCC certification requirements for RF emission (Part 18 of FCC rules and Regulations). Also complies with GTE 0871 Class B.

Coil: 4-turn 1/8-roch copper tubing positioned to allow axial viewing of the plasma

Cooling Water: System requires a flow of –1 Liter/min at 200 to

550 kPa at a temperature between WC and 25°C. Good quality house water or a recireulating cooling system may be used (A Neslab CFT 33 or equivalent is recommended). A filter for removing sediment is supplied with the system.

Shear Gas: The system uses a compressed air shear gas (30 Umin) to push the plasma plume out of the optical path. This minimizes the Impact to the dynamie range caused by the self-absorption that occurs in the cooler plasma plume.

Automatie Ignition: Plasma ignition is computer controlled and totally automated. Using an FAEC macro, the plasma can be turned on at a set time, thus warming up the system prior'to an analysis. Plasma can be turned off automatically after an analysis.

True Power Control: Maintains the plasma power at the set point even when changing sample matrices. During Operation the plasma power is monitored and this Information is used in a feedback loop to control the plasma power at the user-specified level.

Safety Interlocks: System Checks water flow, shear gas pressure, argon pressures, sample compartment door interlocks and plasma stability. These interlocks are constantly monitored and displaved on the computer screen as graphic symbols. If any interlock is'inter- rupted, the plasma is shut down automatically.

Argon Flow Controls

Thermostating: The plasma gas controls are enclosed in an insulated drawer and the temperature is regulated at 40°C.

Plasma Argon Flow: Binary-scaled solenoid valves are computer controlled to regulate the flow automatically within the range of

5 to 20 liter/minute in 1 liter/minute increments. The flow system is interlocked to prevent ignition without plasma gas flowing.

Auxiliar, Argon Flow: Binary-scaled solenoid valves are computer controlled to regulate the flow automatically within the range of 0 to 2.0 liter/minute in 0.1 liter/minute increments.

Nebulizer Argon Flow : The flow is computer controlled, using a mass flow controller, and is variable between 0 and 2.0 liter/minute in 0.001 liter/minute increments.

Sample Introduction System

Torch : The horizontally 7 positioned torch is a demountable design using one-piece quartz tubing for plasma and auxilian gas flow. The standard torch is supplied with a 2.0-mm alumina injector for full corrosion resis­tance to all acids, including hydrofluoric and aqua regia.

Spray Chamber: Scott type pe designed to minimize pulsations from the peristaltic pump and constructed of Ryton® for complete corrosion resis­tance to most acids, including HF, and all organie solvents normally used in ICP analyses.

Nebulizer: Cross-flo• design with chemically resistant GernTips" manufactured from corrosion-resistant (sapphire tips in a PEEK body) material. The system can routinely handle 5090 (vA') solutions of HC1, HNO„,. H-,SO4, H:,PO_ 20% (v/v) HF and 30% (vA-) NaOH. Up to 20'0 NaC1 can be aspirated by the nebulizer for 1 hour without clogging. The system is fully compatible with other nebulizers such as ultra­sonies, concentries (.Nleinhard®) and the Sharp Cone Spray (high solids) nebulizer.

Peristaltic Pump: A three-channel, variable speed, computer-controlled pump. Speed is variable from 0.2 to 2.5 mliminute in 0.1 mL/minute increments using 0.030-inch tubing.

Torch Mount : The QuickChange Torch Module, along with the RF coil. is mounted on the same rigid base as the optical bench. The design of the coil and the mounting system eliminates the need for extensive torch alignment. Both horizontal and vertical viewing of the plasma are opti­mized by computer-controlled movement of the First transfer mirror.

Plasma Miewing: The full plasma is viewed through a n'-blocking, low-transmittance window located in the sample compartment door.

Spectrometer

Polychromator: The Perkin-Elmer high energy (f/6.7) echelle-based polychromator utilizes two detector focal planes and two cross dis­persers. The resolution of the system is 0.007 nm at 200 nm. The 80 by 160 mm echelle grating (manufactured by Perkin-Elmer) has 79 lines per mm and a blaze angle of 63.4 degrees. The cross disperser for the UV region (167-375 nm) is a grating (374 L/mm) with Schmidt correction ineorporated into its surface. The Schmidt correction per­forms aberration correction for the 400-mm radius camera sphere. The cross disperser for the visible region (375-782 nm) is a 60-degree fused-quartz prism.

The entire optical system is enclosed in a purged and thermostated optical enclosure. The optical enclosure is mounted on the same large optical bench as the sample introduetion system. The optical bench is shock-mounted to the frame of the Instrument so that any floor vibration does not affeet system performance.

Thermostating: The polychromator is thermostated to 38°C. The ther­mostating includes the transfer opties along with the polychromator.

Plasma Viewing: Viewing of the axial plasma is accomplished by com­puter control of a mirror located in the optical path and allows adjust­ment of the plasma viewing in both the vertical and horizontal planes. The viewing position can be optimized by the software.

Shutter and Mereury Recalibration System: The pneumatically operated shutter automatically opens and closes for each sample.

By closing the shutter between each sample, the First transfer mirror is proteeted from long exposures to the intense UV radiation of the plasma, thus extending the useful lifetime of the mirror. The shutter

is computer controlled, and the user can elect to leave the shutter open if desired. A mereury lamp is built into each shutter mechanism and can be viewed when the shutter is closed. The mercury emission line at 253 nm may be automatically monitored by the system and used to update the system wavelength calibration. Frequency of the automatic recalibration is user selectable and can vary between 0.000 and 999 hours. Recalibration will occur even during autosampler analysis.

Detector: Perkin-Elmer Segmented-array Charge-coupled-device Detector" (SCD) consists of 224 addressable subarrays, with over 6000 pixels on a 13- by 18-mm silicon substrate. Typical readout noise — 13 electrons RMS; dark current <100 electrons/pixel/second; readout Speed of 40 µsec/pixel. Two detectors are used with each instrument.

Electronics: Correlated double-sampling data acquisition electronics reduce electronic noise.

System Controller

Computer : DECpc LPv with 66-MHz industry-standard 486DX2 processor, 128-KB eache expandable to 256 KB, 8-MB (70 ns) RAM memorv expand­able to 64 MB, 525-MB, SCSI hard disk drive, 525-MB, 1/4-inch, SCSI tage drive, 3.5-inch (1.44-MB eapaeity) floppy disk drive, one IEEE-488 com‑

munications interface, two RS232C serial Interfaces, one parallel printer interface, SVGA monitor with 512-KB video memory expandable to 1 MB.

Printer: Okidata® Mieroline® 320 or HP® LaserJet® 4 as an Option.

Operating Systems : SCO/UNIX ODT (multitasking and multiuser envi­ronment), MS-DOS®, and Mierosofte Windows".

Optima 3000 Software

The Optima 3000 Software operates in a multitasking, multiuser environment. The multitasking capability of the system allows the ana­lyst to report analytical results, view spectral data on the CRT, perform othef software funetions or other software programs while samples are being analyzed with an autosampler. The software contains standard operating conditions for every element. An analysis can be started using these preselected conditions by entering the element Symbol or selecting them from the periodie table and pressing the analyze key.

Results and/or spectra generated during the analysis can be stored on hard disk. Results can be sent simultaneously to the CRT sereen, printer, hard disk, floppy disk and/or out the communication port to an external computer. Results can also be automatically stored in a comma­delimited ASCII format for use Alth third party programs. Time and date stamps are printed and stored with each result.

Solvent blank allows for sample preparation blanks to be subtracted from samples during the analysis. Also a known sample matrix can be aspirated and its spectrum subtracted from all subse­quent samples.

Calibration curves can be stored and recalled for later use.
Calibration curves can be displayed on the monitor in a log or linear

segle using a linear, linear foree through zero or a weighted-linear fit. Erroneous points can be removed from the curves and all curves can be printed for inelusion in an analytical report.

Element mode is used to establish the parameters used for each element determination. The primary analytical lines are listed for user selection. The subarray number, wavelength range and nm/pixel value are shown for each analytical line listed. Ten standard concentrations are available for each element. Multi-bottle standard calibration is available where all elements need not be in the same standard. Internal standard elements are also selected in the Element mode.

The method entry mode is used for the entry of parameters which apply to the whole analysis and to the individual samples being analyzed and is typically used when emploving the autosampler. The method or sample run list can be created by third party software or LIMS and downloaded to the system.

Two modes of spectral interference correction are present in the software. In addition to the traditional Interfering Element correction (IEC), Multicomponent Spectral Fitting (MSF) is also available. MSF takes advantage of all of the spectral information available from a subar­ray by applying linear least squares mathematies. Raw spectral informa­tion is mathematieally compared to a model and the analyte intensity, is determined.

Sinee the raw spectral information can be stored to disk, it can then be reprocessed with different background correction points, stan­dard concentrations, Internat Standards, IEC tables, etc. This allows the analyst the opportunity to modih, the data processing method and reprocess the spectra without rerunning the samples.

A sequence of commands usually performed by the analyst to accomplish a certain setup or analytieal tack can be entered in the Exec mode. When the Exec narre is entered and the EXECUTE function key is pressed, the software performs the sequence of commands auto­matically as if the analyst was operating the instrument.

Analyst mode permits the creation and selection of "analyst names." All analysts within the laboratorv can create their own directorys or they Gould be named after speeifie applications or accounts. All analytical information, parameter entry data and spectral information created within an analyst directory will be saved only in that directory.

Optimize allows analyses to be performed using Optimum operating parameters which the system itself seleets. System parameters including RF power and nebulizer argon flow can be evaluated for optimization. The parameters can be varied to improve spectral interferenees, detec­tion limits, sensitivity and/or precision.

A Wavelength Table contains over 50,000 analytical wavelengths for use in method development and to aid in the identification of unknown spectral features.