Features of Jobin Yvon ICP Spectrometers

Features of Jobin Yvon ICP Spectrometers Jobin Yvon S.A.S., Emission Division, Application Laboratory, May 2003 1 Radio Frequency (RF) Generator 1.1 Solid-state generator The solid-state generator offers a short warm-up time, 15 minutes compared to 45 minutes for typical free running generators. 1.2 40.68 MHz generator The JY 40.68 MHz generator has the following advantages over a 27.12 MHz generator: a) Lower background noise leading to an improved signal-to-background ratio and lower detection limits; b) More efficient RF coupling leading to increased power transfer efficiency and a superior more robust plasma; c) Low argon consumption; d) Excellent analytical precision due to stable plasma; protect the users and the instrument. They include: a) Argon gas pressure and flow b) Cooling water pressure and flow c) Plasma compartment door closure d) Excessive reflected power 2 Sample introduction 2.1 Nebulizers Any of the following nebulizers can be supplied with the JY ICP Spectrometers: a) Pneumatic Concentric Nebulizer This is a one-piece concentric glass type nebulizer. It is recommended for the analysis of clean solutions with high acid and salt concentrations, as well as organic solvents. This nebulizer gives excellent long term precision and detection limits. JY uses Type C as the standard, however Types A and K are also available. 1.3 Forward power regulation Stability is better than 0.1%. Power regulation compensates for slow fluctuations in line power supply (±15). 1.4 Computer controlled generator The generator offers computer programmable RF power, start and shutdown of the plasma. It has continuously adjustable, computer-controlled, variable power from 800 to 1550 W. 1.5. Safety interlocks Figure 1: Pneumatic Concentric Nebulizer JY ICPs have a number of safety interlocks to

b) Parallel Flow Nebulizer This is a one-piece Teflon nebulizer. It is ideal for high dissolved solids and for solutions with suspended particles. It is recommended for HF acid based solutions. analyze the hydride and non-hydride forming elements in a single analysis. The sensitivity of the hydride forming elements is enhanced and the sensitivity of the non-hydrides is not adversely affected.this accessory increases productivity and reduces cost of analysis. Argon Sample capillary tube Figure 2: Parallel Flow Nebulizer Figure 3: Concomitant Metals Analyzer c) Steel-Zirconium Nebulizer For the analysis of suspensions in oils, for example wear metals. g) Spark Ablation This accessory provides for the direct analysis of conductive solids, such as metallurgical materials, without the need of sample preparation. d) Ultrasonic Nebulizer For the analysis of sub-ppb concentrations in all types of samples with the exception of HF acid solutions. e) Hydride Generator For increased sensitivity of the hydride forming elements As, Bi, Ge, Hg, Pb, Sb, Se, Sn and Te. f) Concomitant Metals Analyzer (CMA) This patented Hydride Generation System is only available from JY. It provides the opportunity to 2

2.2 Sheath Gas The argon sheath gas, originally patented by Jobin Yvon, enhances performance and stability in all types of matrices, but especially high solids or salts. This device provides an additional argon stream that isolates the sample from the walls of the injector, thereby reducing contact and sample deposition in the injector tube and tip. This feature allows for the aspiration of solutions containing 30% salt directly into the plasma without blockage or drift. It also allows for the improvement of the Alkali detection limits via a computer controlled increase in gas flow to allow for the optimization of viewing height. 2.3 Large Sample Injector Tube JY uses a large 3 mm alumina sample injector tube, this has several advantages, firstly it allows for the analysis of solutions containing high dissolved solids without blockage and drift. The use of the 3 mm injector tube also creates a chain reaction of other advantages: it increases the residence time, this improves the energy transfer efficiency for atomisation, this gives rise to an increased Mg ratio and makes the plasma more robust, and thus reduces matrix interferences. 2.4. Self-Aligning Demountable Torch The Ryton torch body holds the inner and outer quartz tubes as well as the alumina injector tube. All three tubes are easily removed for cleaning and replacement. No alignment is necessary when replacing tubes, as they are pre-aligned. All levels of operators can dismantle, clean, and reassemble the torch. Figure 5: The demountable torch 2.5 Easily Interchangeable Cassettes The torch and sample introduction system is mounted on a pre-aligned cassette. This allows for fast changing without the need for alignment and optimization each time. Cassettes are available for all types of samples including aqueous, organic, HF solutions and hydride generation. The spray chamber is held in place with a springloaded clip, allowing for changing or cleaning without the need to remove the entire cassette. A fully demountable torch is also more cost effective than a one-piece torch, since the tubes can be replaced as needed without replacing an expensive torch assembly. 3

2.7 Argon Humidifier (option) The argon humidifier minimizes sample deposition in the torch injector and nebulizer tip by saturing the nebulizer argon flow with water. Improved precision and less interferences are found when analyzing samples with high dissolved solids. 2.8 AS 421 Autosampler (option) Unattended analysis of up to 540 samples with the AS 421 computer controlled, programmable random access automsapler. It features the choice of a variety of sample and standard racks. 2.9 Water Recirculator (option) The water recirculator is necessary for providing a safe, environmentally friendly controlled means of cooling the RF coil. Figure 6: The JY cassette, which includes the demountable torch, the spray chamber, and nebulizer. 2.6 Viewing Zone of the Plasma The large transfer optics of the JY ICPs allows for viewing the entire 6 mm of the Normal Analytical Zone (NAZ) at once. By viewing the entire emission zone at one time, the signal is increased and optimization of conditions on one element gives excellent results on all elements. This eliminates any moving torch mechanisms, thereby increasing the speed and eliminating worries about repositioning accuracy or reproducibility. It also eliminates any wear and tear due to moving parts. 3 Optics 3.1 Minimum of Optical Surfaces Each optical surface causes light loss, the amount depending on the type of optical surface and the coating. Therefore, minimizing the number of optical surfaces improves light throughput. The increased light throughput improves the sensitivity and detection limits of the instrument. Other manufacturers offer auto-alignment hardware and software as a so-called benefit. However, this feature is only necessary due to the limited optical design that does not allow for viewing the entire NAZ. For instance, there is no way to automate such a routine for axial plasma viewing. Figure 7: Czerny-Turner optical configuration, showing the small number of optical surfaces. 4

3.2 Choice of Slit Widths The JY sequential instruments provide automated software that selects the most appropriate slit widths for an analysis based on user input. If precision is of primary importance, the slit widths can be increased. When the best detection limits possible are required, using the smaller slit widths would be appropriate. 3.3 Holographic Grating Holographic gratings offer the advantage of minimum stray light and no ghost images in comparison to ruled gratings. They provide clean spectra and an improved signal-to-background ratio, thus providing improved (lower) detection limits. Holographic gratings are manufactured using precise laser technology, whereas ruled gratings are made using mechanical methods that lead to unavoidable ruling imperfections resulting in increased stray light, higher background and higher detection limits. 3.4 Large Grating The signal gathering power of an instrument is directly proportional to the grating area. A larger grating area provides more signal, allowing for higher signal-to-background ratio and therefore superior detection limits. JY uses the entire surface of the grating for even more light throughput. Using a larger grating allows JY to use lower orders of light and still achieve excellent resolution. Lower order offer more signal, which results in shorter integration time and faster analysis. 3.5 Choice of Grating The following gratings are available for the instruments indicated: 2400 grooves/mm (1st order) JY 2000-2 Spectral Range: Linear Dispersion: Working Resolution: 3600 groove/mm JY ULTIMA 2 and ULTIMA 2C 160-800 nm (120-800nm with Halogen Option) 0.4 nm/mm 0.012 nm Recommended application: rare earths and geological. Spectral Range: 160-500 nm Linear Dispersion: 0.26 nm/mm Working Resolution: 0.007 nm Dual 4320 and 2400 groove/mm (two sided, backto-back gratings) JY ULTIMA 2, ULTIMA 2C and JY 2000-2 Recommended application: Rare Earths, Geological and Precious Metals, where full spectrum is required. Spectral Range: 160-800 nm Linear Dispersion: 0.2 nm/mm (160-420 nm), 0.4 nm/mm (420-800 nm) Working Resolution: 0.005 nm (160-420 nm), 0.010 nm (420-800 nm) 3.6 Direct Drive Grating JY Sequential instruments use a direct drive grating system. The advantages of a direct drive follow: a) Speed: Full wavelength coverage in 7 seconds, with a mechanical reproducibility of 0.0004 nm. b) Precise analysis: A minimum step size of 0.0003 nm permits correct peak location, thus providing more accurate analyses. 2400 grooves/mm (1st and 2nd orders) JY ULTIMA 2, ULTIMA 2C and JY 2000-2* Spectral Range: Linear Dispersion: Working Resolution: 160-800 nm (120-800 nm with the Halogen Option) 0.4 nm/mm in 1st order 0.005 nm in 2nd order, 0.010 nm in 1st order * This grating is used for the JY 2000-2 with the VUV option for the analysis of halogens. 5

3.7 Simultaneous Internal Standard Capability (option) The internal standard option compensates for changes in signal due to variations in nebulization, gas flows, RF power, electronics, voltage etc, by providing a real time ratio to a reference element. The Internal Standard Monochromator allows any element wavelength to be used as an internal standard. 3.8 Thermal Regulation of Optics The optics are thermally regulated to within ±1 o C to provide excellent long and short term stability in the real lab environment. The temperature can be adjusted to compensate for the highest temperature reached in the laboratory environment, up to 40 o C (104 F). 3.9 Nitrogen Purge for UV Sensitivity The use of a nitrogen purge allows for the analysis of elements below 190 nm with excellent detection limits. The purge includes not only the monochromator itself, but also the optical path from the plasma to the monochromator. The use of the nitrogen purge allows for the analysis of wavelengths down to 160 nm, such as the most sensitive line of Al, at 167 nm. With the Halogen option this wavelength range can be extended down to 120 nm for the analysis of Cl, Br, and I. The use of the nitrogen purge also extends the lifetime of the optics by keeping out dirt, dust, and any sample residue. Vacuum pumps will deposit a film of oil on the surface of the optics and grating, thus requiring regular cleaning of the optics. 3.9.1 Nitrogen Generator (option) A nitrogen generator produces nitrogen from compressed air, reducing operating costs and eliminating the need for a dedicated nitrogen gas supply. JY offers several models of nitrogen generators that provide high purity nitrogen (99.9995%) from 3-6 L/minute. 3.10 Far UV Analysis (option) The VUV analysis option allows for the analysis of the Cl, Br, and I at wavelengths in the VUV. For example, Cl is analyzed at 134 nm with a typical detection limit of 200 ppb. For analysis between 120-160 nm, it is necessary to use MgF 2 optics and increase the nitrogen purge. This feature can be added to the system as an upgrade once the instrument is installed. 3.11 Upgrade to a Combination ICP Any sequential JY ICP can be upgraded in the field to a combination simultaneous/sequential spectrometer with the addition of a polychromator. The viewing of the plasma is done through a direct transfer of the light, with no fiber optic connections. 3.12 High Dynamic Detector system (HDD ) The patented High Dynamic Detector system provides optimum detection across the full range of the spectrum from 160 to 800 nm (down to 120 with the optional halogens kit). They allow measurement of concentration levels ranging from ppb to percentage levels, giving a dynamic range of 10 8 (compared with 10 4 for instruments with solid-state detectors). 4 Analyst Software 4.1 Analyst V5 Software The software runs under Windows 95/98/NT. As a Windows based package the software is intuitive for the novice user. Some of the features include: (a) Step-by-step guide through the creation of a method with the "Wizard" (b) Library of over 125,000 lines (c) Compatibility with automatic, random access autosampler for unattended analysis 6

(d) Multi-user security (e) A choice of analytical mode of analysis, including single point and Gaussian fit Time: 115 seconds Number of measurements: 228,900 Dynamic range: 5 X 10 10 Figure 9: A spectrum acquired using Win-IMAGE (f) Data export capability (g) Correction for weight/volume dilution factors (h) On-line help at any point in the software showing a wavelength range of 160 to 320 nm. C. Software The NAVIGATOR software brings the full power of Win-IMAGE to the analyst in a user-friendly Windows environment. Figure 8: The Analyst "Tasks and Sequences" window. 4.2 Win-IMAGE and IMAGE Navigator (option) Win-IMAGE and IMAGE Navigator allow the full acquisition of the spectrum in less than 2 minutes with no compromise in optical resolution. a) High dynamic range electronics A patented electronic system extends the dynamic range of the detector to 5 X 10 10. It allows the acquisition on the same detector of both trace and major concentrations, eliminating possible saturation or necessary set up. b) Fast acquisition electronics A fast data acquisition board allows fast scanning and acquisition of the full spectrum Data on acquisition of entire spectrum: Four main functions are available: a) Search of a specific element in a spectrum After selection of an element in the periodic table, NAVIGATOR displays the five most intense emission lines for that element, overlaid with the corresponding parts of the spectrum to determine if the element is in the solution. The heights of the theoretical lines are calibrated for 10 ppm, allowing for an estimation of the element concentrations. b) Peak identification Mouse driven zooming capabilities allow the user to select any peak in the spectrum. NAVIGATOR identifies the selected peak using a 125,000-line library, and then displays the five most intense lines for that element to confirm identification and to estimate the concentration. c) Full automatic semi-quantitative analysis The most powerful feature of the NAVIGATOR, the semi-quantitative analysis, returns the concentra- 7

01 tion ranges of all elements selected by the user. It features: - Point and click selection of desired elements from a periodic table or selection of all ICP elements - Selection of concentration ranges - Display of the concentration results in a colorcoded periodic table - Detailed reporting of the concentration results - ASCII storage of the results in any data processing software d) Quantitative analysis 4.3 Remote Diagnostics (option) Remote diagnostics allows remote access to the computer and instrument from a JY Service/Application Center for service troubleshooting and applications support. Using a modem, the software allows all functions within the instrument to be tested. This lowers maintenance cost by eliminating unnecessary service calls and reduces downtime. Note: Remote Diagnostics is not available in all areas of the world. Please contact Jobin Yvon Service for more information. 4.4 ALLIANCE Service ALLIANCE is an extension of JY to more than 3500 users of JY ICP, Glow Discharge, and Spark spectrometers around the world. The global program is accessed through the JY website at www.jyhoriba.com/emission/alliance. It offers an online spare parts and accessories catalog, which provides online quote requests and World Link - a user forum. This worldwide JY user discussion group features communication with our applications and service centers around the world. Calibration of the NAVIGATOR with standards allows for quantitative analysis. Figure 10: The five most sensitive lines of Fe, displayed within Win-IMAGE, for two different samples. In the USA: Jobin Yvon Inc. 3880 Park Avenue Edison, NJ 08820 Tel: 1-732-494-8660 Fax: 1-732-494-8796 E-mail: emission@jobinyvon.com 1-866-JobinYvon www.jobinyvon.com In France: Jobin Yvon S.A.S. 16-18, rue du Canal 91165 Longjumeau Cedex Tel: (33) 1/64 54 13 00 Fax: (33) 1/69 09 90 88 Germany: (49) 89/46 23 17-0 Italy: (39) 2/57 60 56 90 U.K.: (44) 20/82 04 81 42 In Japan: Horiba Ltd. 2 Miyanohigashi, Kisshoin Minami-ku, Kyoto 601-8510 TEL: (81) 75 313 8121 FAX: (81) 75 321 5725 www.horiba.com China: (86) 10/6836 6542 Spain: (34) 91/724 16 57 Other Countries: Contact JY S.A.S. 8