SPECIFICATION SPECIFICATION Inductively Coupled Plasma Mass Spectrometry System 1. Scope This specification describes the requirements for an Inductively Coupled Plasma Mass Spectrometry System ( System ) for the determination of trace, minor and major elements in environmental swipe samples and related applications. The System includes a Quadrupole Inductively Coupled Plasma Mass Spectrometer and associated equipment, such as sample introduction system (HF-resistant), sample changer, water-to-water cooling equipment for interface parts and RF generator (if applicable), electrical cables, control computer, printer, software. As essential part of the system, a collision or reaction cell is required for controlled interferences removal. The System shall be with full PC control of all instrument settings and compatible accessories. Environmental Sample Laboratory of the IAEA fulfils its service to the IAEA Department of Safeguards by performing bulk and particle analysis of environmental inspection samples. The analysed samples usually contain a few nanograms of uranium (10-9 g) and femtograms to picograms (10-15 g to 10-12 g) of plutonium. Mass spectrometric techniques are implemented as key methods for isotopic analysis of uranium and plutonium, including minor isotopes 234 U and 236 U, as well as for age determination of traces of nuclear materials. With account to the requirements above, the ESL intends to purchase a quadrupole Inductively Coupled Plasma Mass Spectrometry System for screening of elemental composition and isotope ratios of U and Pu in swipe samples as well as in process solutions. For these purposes a mass spectrometer is required that possesses sufficiently high absolute sensitivity, high abundance sensitivity, and capability of simultaneous determination of actinide isotopes and concomitant stable elements that might produce interferences on actinide isotopes in ICP-MS analyses. The performance requirements for the System are based on the ESL procedures for inspection sample analysis. 2. Applicable Documents Following documents shall be used for reference on quantities, units, prefixes and other technical vocabulary in this document: International System of Units (SI). International Bureau of Weights and Measures, 8th edition, 2006; and ISO/IEC Guide 99-12:2007, International Vocabulary of Metrology Basic and General Concepts and Associated Terms, VIM. The following documents from International Union of Pure and Applied Chemistry (IUPAC) shall be used for reference for the requirements in this document:
IUPAC Physical Chemistry Division. Quantities, Units and Symbols in Physical Chemistry. 3rd ed. (the Green Book ). By E. R. Cohen, T. Cvitaš, J. G. Frey, B. Holmström, K. Kuchitsu, R. Marquardt, I. Mills, F. Pavese, M. Quack, J. Stohner, H. L. Strauss, M. Takami, A. J. Thor. RSC Publications, Cambridge, UK (2007); IUPAC. Nomenclature of Inorganic Chemistry. by G. J. Leigh. Blackwell, Oxford (1990); IUPAC. Nomenclature of Inorganic Chemistry. IUPAC Recommendations 2005. by N. G. Connelly, T. Damhus, R. M. Hartshorn, A. T. Hutton. RSC Publishing, Cambridge, UK (2005); and IUPAC. Compendium of Chemical Terminology, 2nd ed. (the Gold Book ). By A. D. McNaught and A.Wilkinson. Blackwell Scientific Publications, Oxford (1997). In the event of conflict between the documents listed above and the content of this Specification, the content of this Specification shall take precedence to the extent of the conflict. 3. Definitions, Acronyms, and Abbreviations The following definitions, acronyms, and abbreviations shall apply throughout this Specification unless defined otherwise hereinafter: ICP-MS shall mean Inductively Coupled Plasma Mass Spectrometer ; Cps shall mean count per second ; m/z shall mean mass to charge ratio ; and Standard prefixes are used accordingly to the International System of Units. 4. Requirements 4.1. Functional and Performance Requirements The System shall meet the following functional and performance requirements: 4.1.1. Detection limits calculated as three times the standard deviation of the blank and peak hopping at 1-point per mass, measured in diluted nitric acid, e.g., in 1% HNO3 shall be as defined in the table below: Element/Isotope Detection limits, ng L -1 56 Fe 3 or smaller 115 In 0.1 or smaller 238 U 0.1 or smaller 4.1.2. Sensitivity measured with a low-flow nebuliser at a sample uptake rate of 0.1 ml min -1 to 0.2 ml min -1 shall be as defined in the table below: Element/Isotope Sensitivity, cps (mg/l) -1
115 In greater than 4 x 10 8 238 U greater than 4 x 10 8 4.1.3. Ratio of oxides and doubly-charged species measured under identical operating conditions that are used to achieve sensitivity and detection-limit specifications shall be as defined the table below: Element Intensity Ratio, % 140 CeO+/ 140 Ce+ smaller than 1.5 137 Ba++/ 137 Ba+ smaller than 3 4.1.4. Background signal measured at m/z = 220 shall be smaller than 0.5 cps 4.1.5. Short-term precision defined as the relative standard deviation (% RSD) and measured in 1 µg L -1 multi-element solution, for instance 24 Mg, 63 Cu, 114 Cd and 208 Pb, without internal standardization shall be smaller than 3% RSD over 20 minutes. 4.1.6. Long-term stability defined as the relative standard deviation (% RSD) and measured in 1 µg L -1 multi-element solution, for instance 24 Mg, 63 Cu, 114 Cd and 208 Pb, without internal standardization shall be smaller than 4% RSD over 2 hours. 4.1.7. Isotope-ratio precision defined, for example, for the isotope ratio of 107 Ag/ 109 Ag using a 25 µg L -1 solution shall be smaller than 0.1% RSD. 4.1.8. Abundance sensitivity defined as the intensity of a given isotope at spectral peak maximum, relative to the intensity of that isotope at 1 amu lower and at 1 amu higher than the mass position corresponding to peak maximum and measured at 238 U or 232 Th shall be better than 5.0 x 10-7 at low mass side of peak and better than 1.0 x 10-7 at high mass side of peak. 4.1.9. Mass range shall be 6-260 amu or wider 4.1.10. Mass calibration stability measured, e.g., using a 1 µg L -1 multi-element solution containing 7 Li, 24 Mg, 115 In, and 238 U shall be better than 0.05 amu over 8 hours of continuous operation. 4.1.11. Dynamic range shall be 9 orders of magnitude or larger 4.1.12. Mass resolution M/ M measured with the 5% peak width definition according to IUPAC Compendium of Chemical Terminology using, e.g., 238 U will be larger than 300.
4.2. Technical Requirements The System shall meet the following technical requirements: 4.2.1. The System shall be enabled for automated unattended plasma start up and shutdown; 4.2.2. The System shall be enabled for true multitasking, allowing users to reprocess or review data from other worksheets while data is being collected for another application; 4.2.3. The System shall be enabled for full PC control of plasma ignition, XYZ plasma position, nebuliser, plasma and auxiliary gases, gate valve, vacuum system, RF power, collision or reaction cell setup, detector setup, mass calibration, resolution, performance tests and peristaltic pump speed; 4.2.4. The System shall be enabled full post run data editing with automatic redisplay of the results; 4.2.5. All sample introduction equipment shall be HF-resistant; and 4.2.6. The System shall be compatible with other sample introduction systems such as Aridus and APEX Q. 4.3. Essential Accessories The System shall include the following essential accessories: 4.3.1. Collision or reaction cell that shall be installed for controlled interferences removal; 4.3.2. Low-flow nebuliser and temperature-controlled (Peltier cooled) spray chamber that shall be installed; and 4.3.3. Sample changer that shall be enabled for full PC control sample changer and that shall have racks for sample vials ranging from 2 ml up to 50 ml and that shall have a rinsing unit for the probe. The sample changer shall have a capacity for simultaneous handling of at least sixty 15 ml vials and at least twenty 50 ml vials. The sample changer shall have two rinse positions equipped with pumps. The ssample changer shall be acid
resistant and it shall not require any rinsing with water to remove diluted acid residue from the sample changer before the shutdown.
4.4. Spare parts and consumables The System shall include sufficient spare parts and consumables for two years operation such as, but not limited to, the following items and quantities: 5. Marking - Three (3) spare plasma torches; - Three (3) spare injectors ; - Three (3) skimmer cones; - Three (3) sampler cones; - Three (3) spare nebulizers; - One (1) spare temperature-controlled (Peltier cooled) spray chamber; and - appropriate tube sets and all necessary fittings for gas supply and sample introduction systems. The System shall have all safety markings in English language. 6. Packing The Supplier shall suitably pack the System for delivery into clean laboratory of ESL. 7. Quality Requirements The System shall be manufactured, shipped and installed in accordance with the ISO 9000:2000 quality assurance system or an equivalent quality assurance system. 8. Testing and Acceptance The System, prior to shipment, shall be tested for conformance of the System with manufacturer s performance specifications and the minimum requirements specified herein. The System, after installation, shall be tested by Contractor with the IAEA to demonstrate that the performance meets the manufacturer s performance specifications and the minimum requirements specified herein as determined by the IAEA. This on-site acceptance testing of the System shall include the following: (a) The Supplier shall demonstrate to the IAEA the performance for each of the requirements specified in Section 4 above;
(b) The Supplier shall demonstrate: Fully automatic operation overnight; Fully automatic and safe shut down of instrument if argon pressure becomes too low; and Fully automatic closing of analyser valve in case of power loss; (c) The Supplier shall demonstrate to the IAEA that for the software delivered with the System it shall be possible to export all of the information associated with an analysis in a single export operation including the following: a. The time of the measurement as well as the analysis time of the data reduction and export; b. All individual cycle data (selected peak intensities as well as ratios); and c. Overall summary data; The results of the on-site acceptance testing of the System shall be documented by the Supplier in an acceptance protocol, which will be signed by IAEA. 9. Installation and Training 9.1. The Supplier shall install the System in the Environmental Sample Laboratory in Seibersdorf, Austria. 9.2. The Supplier shall provide three-days applications training for up to three IAEA operators on the System s hardware and software and in addition one day of electronics diagnosis and repair training for up to two IAEA engineers. Both trainings shall be provided immediately after the installation of the System. 10. Deliverable Data Items The Supplier shall provide, in both hard copy and electronic format, manuals for operation, maintenance, and software use for the System. All documentation shall be in the English language. 11. Warranty Period The Supplier shall provide two-year warranty for the System.