Microprobe EDS Software-Hardware Specification

for

UCB

Department of Geology

April 1995

 

Table of Contents

A. General Requirements

B. Inclusion of Vendor's Technical Proposal into this Specification

C. Preliminary Testing by Vendor Prior to Shipping

D. Installation and Acceptance Testing

E. On Site Training

F. Documentation

G. Technical Specifications and Requirements

1. Microprobe EDS acquisition and analysis software

2. Energy dispersive x-ray analyzer and image analysis system (EDS)

H. Quantitative acceptance tests to be performed by UCB

I. Miscellaneous

 

A. General Requirements

The vendor shall furnish all facilities, labor, and materials to provide goods and services in accordance with the terms and conditions described in this specification for both the hardware and software. The Vendor shall maintain an inventory of spare and repair parts and such tools and instruments as necessary to properly and efficiently maintain the equipment for the life of the equipment. Spare parts and consumables must be obtainable within a maximum of 20 working days after a purchase order number is received by the Vendor. The specifications listed in this document are the minimum requirements for the Department of Geology and Geophysics microprobe.

Please provide a detailed competitive price quotation for each major component, device or feature. Please quote each price and the system total on a duty free basis (however please include California sales tax @8.25 % and inland transportation costs) as we will be applying for a customs duty exemption. The prices quoted should reflect any educational discounts that can be applied to a non-profit educational organization purchase.

Please include in the quotation any additional equipment or software and pricing that will be required to efficiently operate all equipment features specified in this document if they are not standard equipment or not explicitly stated in the specifications.

A catalog and current price list of all spare parts and assemblies shall be provided by the Vendor with the equipment.

 

B. Inclusion of Vendor's Technical Proposal into this Specification

The Vendor's technical proposal entitled, [ ] dated [ ], is incorporated by reference and made a part of this contract. In the event of any inconsistency between the provisions of this contract and the Vendor's technical proposal, the contract provisions in this document take precedence.

 

C. Preliminary Testing by Vendor Prior to Shipping

Documentation of performance in accordance with following preliminary specifications shall be provided by the Vendor before shipping the equipment. The seller shall provide the necessary personnel, equipment and facilities to conduct these same acceptance tests and the other specifications described in section G. below entitled "Technical Specifications" on the installed equipment, unless this document specifically states that UCB (University of California at Berkeley) shall provide the items required.

Preliminary Performance Specifications to be Received by UCB Prior to Equipment Shipping :

- EDS software specifications 1a

- EDS hardware specifications 2c, 2e, 2f, 2g

 

D. Installation and Acceptance Testing

Acceptance of the equipment shall be based upon completion of installation and after testing of equipment hardware/software performance on site at UCB, McCone hall, Berkeley, CA by personnel selected by UCB.

The equipment shall meet ALL specifications described in this specification and the Vendors included proposal (with appropriate calculated scale factors at UCB's normal operating condition of 15 KeV). The equipment shall meet the specifications before acceptance and again 1 year after acceptance.

Although the instrument will be bought without the Vendor's standard computer system, it will still be necessary for the Vendor to install the standard computer system for the running of acceptance tests, to be conducted on site by UCB and supply all necessary documentation for interfacing to hardware/software. After running the acceptance tests and the hardware/software is accepted, the Vendor will remove the Vendor's standard computer system at no additional cost to UCB.

The acceptance tests shall be performed on samples provided by the Department of Geology at UCB, including thin sections, polished mounts of minerals and oxides and metal elements and alloys. Final payment will be made after all acceptance tests have been completed and the equipment meets all specifications in this document.

The Vendor shall provide all parts, materials, labor, and transportation required to perform preventive and remedial maintenance on the equipment during the installation and acceptance testing period. The maintenance services shall also be performed in accordance with the terms, conditions, and statement of work set forth herein. The Vendor's warranty shall not begin until the equipment has passed all acceptance tests and meets all technical specifications described in this document.

Preventive maintenance shall include, but not be limited to, cleaning, adjusting, inspecting, and testing procedures to keep the equipment in good operating condition, preclude equipment failures to the greatest extent possible, and extend useful equipment life. It includes running of all diagnostics, and repair and replacement of all defective parts.

Remedial Maintenance shall include replacement of parts that do not meet the specifications or requirements described in this document. This includes all transportation, labor and parts required for the parts replacement or upgrade.

All parts, materials, and components, including expendable items, shall be replaced when necessary during the installation and acceptance testing period at no additional cost to the University. Replaced parts shall become the property of the Vendor.

The work to be performed shall be in accordance with the original equipment Vendor's specifications and recommendations. All services are to be performed by competent personnel, experienced and highly qualified to provide required services in accordance with the best commercial practices, without unnecessary delays or interference with University functions.

 

E. On Site Training

Training for one designated personnel for the equipment in the operation of all hardware and software shall be provided at destination. Training shall be approximately five days in length, and be conducted during regular business hours Monday through Friday.

 

F. Documentation

Documentation manuals shall be provided for the equipment, that clearly and completely describe hardware and software operation, troubleshooting, and maintenance of all components of the hardware.

All manuals for Vendor supplied third-party items such as the computer, EDS systems, image display, and hard copy devices shall be provided for the equipment. Computer operating system and application documentation in English shall be provided.

General interconnect and wiring schematics in English shall be provided by the Vendor. Detailed equipment schematics shall be available from the vendor in the event that UCB might make future modifications.

 

G. Technical Specifications and Requirements

The Department of Geology at the University of California requires a state-of-the-art microprobe EDS acquisition and analysis software-hardware package to conduct its research programs.

The EDS software-hardware system shall be able to both qualitatively and quantitatively analyze and image all elements from C to U and be able to tolerate repeated themal cycling. In addition, the EDS acquisition and analysis system must meet the following additional requirements specified below :

1. Microprobe EDS acquisition and analysis software :

a) IBM PC or compatible and Microsoft Windows 3.1 based high level (e.g., C, C++, Visual Basic or FORTRAN) programs for complete qualitative and quantitative X-ray microanalysis and image acquisition, processing and analysis, data and image storage, retrieval, and graphical hard copy output

Licenses (and any hardware copy protection devices if necessary) shall be provided for running two copies of the vendor EDS software simultaneously on separate computers. This is to allow UCB to one copy for on-line for acquisition and analysis and another copy for off-line processing of spectra, calculation of quantitative data and image processing of previously acquired spectra, data and x-ray maps

b) the Vendor shall supply documentation of a method to control the Vendor supplied EDS acquisition and beam scan control functions from a user written application using standard Microsoft Windows 3.1 operating system calls such as FindWindow() and SendMessage() routines. The functions required to be accessed by this method include:

- Start and stop x-ray spectrum acquisition

- Save X-ray spectra to file

- Start and Stop image acquisition

- Save image data to file

- Position electron beam a x,y coordinate

This requirement is to allow UCB to develop software to interface to the Vendor's EDS acquisition and beam scan control hardware. The Vendor shall provide some Visual Basic, C or C++ code for demonstarting this type of control.

All vendor provided software upgrades shall be provided at no extra cost to UCB during the warrenty period.

c) the software shall be capable of acquiring the standard calibration data in exactly the same manner (number of elements analyzed, count times, etc.) as the unknowns.

- it shall be possible, to have as a default option, the ability to perform a complete data acquisition on each or all standards for all elements in the run. The complete data for each standard shall be saved and allow for standard re-assignments and comparison of primary and secondary standard analyses.

d) EDS peak identification and peak markers shall display or list :

- ALL (K, L, M, N, a, b, g, etc.) x-ray lines capable of being generated at the operating voltage

e) the quantitative x-ray microanalysis software shall provide complete routines for :

- instrument and standards parameters setup and recall of instrument setups from previous runs

- output of raw spectra to disk file in EMSA spectra standard format

- element and spectral line selection (Ka, La and Ma) standardization and calibration and recall of standard position and intensity calibrations from previous runs

- analysis and reduction of a minimum of 25 elements or oxides (32 preferred), including calculating an element by difference, by stoichiometry, by fixing formulas proportional to oxygen and/or by including fixed concentrations of selected elements (such as carbon)

- oxide cation ratios can be defined by the user during the analytical run for the calculation of oxygen calculated by stoichiometry or measured

- a standard database that can store up to 1000 standards with 25 elements (32 preferred) each and include support for composition input by element weight percent, oxide weight percent (with default or user specified oxide cation ratios), mole or atomic percents or formula atoms, calculate and display elemental k-ratio and matrix correction factors for each element in a specified standard; import a standard composition from a disk file; output selected or all standard compositions to a disk file

- provide correction routines for x-ray intensity data by atomic number, absorption, and fluorescence (ZAF), x-ray emission vs. depth/density [f(pz) or PAP]

- provide complete saving of all instrument settings and user specified analytical options to disk and the ability to recall any sample raw data for further recalculation and to allow restarting the saved run or starting a new run based on a previous run instrument setup

f) the EDS digital mapping and imaging software shall provide for :

- digital x-ray maps at 512 x 512 x 8 bits per pixel (1024 X 1024 by 16 bits per pixel preferred) to be acquired using the EDS detector ROI signals. The maps must be capable of being stored to hard disk or optical storage media in a TIFF or other standard image format

- provide qualitative (with capability for upgrading to fully quantitative) elemental mapping (beam scan with X-Y position using relative or absolute microns or stage position) capability and output of background corrected intensities to image or ASCII file

- image acquisition and processing software shall be provided for X and Y manual and automated beam control and digitization of sample coordinates, pixel and frame averaging, software selectable X-Y internal/external beam scan control, background subtraction, contrast/brightness, image enhancement, RGB combination maps, false color processing, text annotation, X-Y scatter plotting of intensities

- x-ray maps stored to disk must be registered for scale calibration for off-line processing

 

2. Energy dispersive x-ray analyzer and image analysis system (EDS) :

a) EDS detector (Si(Li) 10mm2) shall have built-in safeguards against vacuum system degradation or failure, through durable detector window composition, design and construction and provide vacuum protection interlocks. The window must be rated to withstand at least 2 atmospheres (or 15 PSIG) and shall be able to withstand repeated venting of the column chamber to atmosphere or dry N2.

b) the window composition shall be of the thin window type and shall be able to detect C at approximately the 1 % level with 99 % confidence (test to be performed on a standard steel sample of composition in weight percent : 1.04 carbon, 9.9 Ni and 89.06 Fe) at 15 KeV and 30 nA sample current, using a thin window detector.

c) EDS detector resolution shall be 138 eV (or less) at Mn ka (measured on Mn metal) at 15 KeV and at a count rate of 1000 cps (or more). Under the same conditions, the detector resolution shall also be 85 eV at F ka (or less) at a count rate of 1000 cps. Under the same conditions used to measure these resolutions, confirm that the full width and 1/10th the maximum for Mn ka is less than or equal to 1.9 FWHM. The detector shall maintain this specification after repeated thermal cycling and/or thermal conditioning.

In addition the detector resolution shall be 152 eV (or less) at Mn ka (measured on Mn metal) at 15 KeV and at a count rate of 10,000 cps (or more).

d) the background intensity at 1/2 the energy of the Mn ka peak (as simulated using an Fe55 radioactive source supplied by the EDS Vendor) shall be less than 1/10,000 of the peak intensity of the Mn ka peak

e) the Si double energy peak intensity shall be less than 1/200 (or less than 0.5%) of the parent Si ka peak intensity as measured on Si metal at 15 KeV with a deadtime of 50 %, when measured under the same conditions as (c).

f) the count rate linearity shall be less than 1 % as determined by measuring the throughput integrated count rate on pure Si metal vs. beam current, when beam current is varied by an amount sufficient to change the deadtime from approximately 10 % to 50 % in increments of 10 %.

g) the apparent Si peak due to the Si dead-layer and internal fluorescence of the EDS detector shall produce an apparent k-ratio of less than 0.002 relative to pure Si metal as observed in a sample of pure Co metal at 15 KeV at 30 nA beam current when no special software correction is applied

h) the energy calibration as measured on Cu ka, Si ka and F ka using pure Cu, Si and CaF3, shall drift less than 0.1% over a period of 8 hours and less than 1.0% over a period of 1 month. The energy calibration, when measured using the same x-ray lines, shall shift less than 10 ev or 1 channel at deadtimes from 0 to 90% and count rates from 0 to 30,000 cps.

i) the detector and electronics shall be capable of sustaining count rates up to 30,000 cps and simultaneously maintain a deadtime of less than 70% in order to perform under typical microprobe analytical conditions.

 

H. Quantitative acceptance tests to be performed by UCB :

The following analytical tests shall be performed for evaluation of the EDS quantitative analysis system at UCB :

- several mineral standards of known accuracy (supplied by UCB) shall be used to demonstrate that the EDS quantitative analysis can routinely and repeatedly produce quantitative analysis with an accuracy of 5 % relative (+/- 2.5 %) for major elements (Z > 11) and accuracy equivalent to counting statistics for minor elements at 15 KeV using pure oxides and simple silicate standards

- the tests will be performed at various operating conditions from 15 to 20 KeV and 5 to 50 nA

- the raw intensities and backgrounds will be printed out along with the integrated beam current. Quantitative analyses for all elements in oxide weight percent of both the standards and unknowns will be printed out along with the averages, standard deviations, standard errors, P/B, k-ratios, ZAF correction factors and for the standards the variance from the value entered in the standard database for each element

- the mole percents, formula based on oxygen (if applicable to the sample), results in elemental (and oxide, if applicable) weight percent (including O measured or by stoichiometry), detection limits at several different confidence levels and level of homogeneity will be calculated and displayed

 

I. Miscellaneous :

If this Purchase Order, including those documents forming a part hereof by reference or incorporation, provides for or requires the submission of any work to UCB for approval, any such approval given by UCB prior to final acceptance shall not relieve the seller of its responsibility for complying with the specifications and other provisions of this Purchase Order. Any such approval shall not be construed as an assumption by UCB of the responsibility that such work complies with or will comply with the specifications or other provisions of this Purchase Order.

 

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