B09 Attachment A Specifications_0001.pdf

Performance-Based Work Statement

I - General Information:

A - Introduction: The Reston Electron Microbeam Lab requires a large area energy dispersive silicon drift detector (EDS-SDD) with particle analysis software. The detector will replace the existing EDS detector on the Hitachi SU-5000 field emission SEM.

B - Background: The current system has a medium-sized 30 mm2 detector, which limits the maximum count rate attainable and therefore large area mapping capabilities, especially at low accelerating voltage. More importantly, the software does not allow for useful particle analyses, which prohibits us from meeting the emerging research needs of USGS projects (see Scope below). This software cannot be upgraded. The existing EDS detector has been well used since it’s installation over 5 years ago. However, it is no longer at the state-of-the-art in either detector or software technology.

C - Definitions/Applicable Documents: Large area detector is here defined as an EDS detector with a sensor area greater than or equal to 100mm2.

D – Scope: The general purpose acquiring a large area EDS-SDD for the microbeam laboratory is to increase laboratory capabilities and efficiencies. Specific objectives are to obtain a detector system (hardware + software) capable of: 1.) Full thin section hyperspectral mapping 2.) Creating background and peak overlap maps from raw count data as well as fully quantified maps using ZAF-type correction algorithms.3.) Deconvolving peak overlaps within the particle analysis to distinguish for example particles rich in Pb, Bi and S from each other. 4.) Reducing analysis time through a flexible criteria dialog within the particle analysis software. 5.) Collection of data for 200,000 particles within a single analysis. 6.) Allowing for offline data analysis (currently, there is a bottleneck because of the limited number of computers available with the software for data processing). The estimated approximate cost based on quotations is $140,000.

II - Work Requirements:

A - Technical Requirements:

1 - The EDS system shall be installed on the existing Hitachi SU-5000 scanning electron microscope at the USGS Reston Microbeam Laboratory in Reston, VA. The system shall not interfere with any existing microscope operations and installation shall be coordinated with Hitachi and meet their approval for continued maintenance of the Hitachi instrument under the existing Hitachi-USGS microscope service contract. The EDS must fit in the current EDS port (Port D).

Computers

Minimal employment of multiple computers shall be adhered to whenever possible. Each computer and its input devices (e.g., keyboard, mouse) shall be justified. The minimum specifications for all computers shall be:

i) The processor shall be Intel® Xeon 6 Core processor (or equivalent) or better

ii) Included RAM shall be 16 Gb or better

iii) Windows 10 with 64 bit operating system

iv) All display cards shall be for PCIe bus, minimum 1 Gb on-board RAM and allow for multiple (minimum 2) dual-DVI, dual-display port, or dual- HDMI monitors per computer. The minimum display resolution for all monitors is 1920 x 1200.

v) The computers designated for SEM control and for EDS control shall offer compatibility with one mouse and one keyboard.

vi) The primary hard drive shall be 4 Tb or better.

vii) Monitor(s) shall be a minimum 27 inch wide screen, flat panel.

viii) 10/100/1000 MbpsPCI-E Network Card

ix) USB 3.0, Firewire

-or- The system shall operate on any computer supplied by the user provided the computer and operating system meet minimum system requirements as defined by the vendor.

EDS Silicon Drift Detector Requirements

a) Silicon Drift Detector (SDD) with a 100 mm2 active area 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 Be at approximately 5 wt. % concentration level with 95 % confidence in a beryl (Be3Al2Si6O18) matrix. Test to be performed on a standard mineral sample of beryl at 10 KeV and 1-5 nA sample current, using a thin window detector.

c) EDS detector minimum resolution shall be 127 eV on Mn Ka at 50,000 counts per second. The detector shall maintain this specification after repeated thermal cycling and/or thermal conditioning.

d) The energy calibration, when measured using the same x-ray lines, shall shift less than +/- 0.1% per 24 hours after 8 hours of operation at deadtimes from 0 to 50% and count rates from 0 to 150,000 cps.

e) The detector and electronics shall be capable of sustaining count rates up to 100,000 cps and simultaneously maintain a deadtime of less than 70% in order to perform under fast x-ray mapping conditions.

f) The vendor shall indicate the detector-to-sample distance for uniform collection from a sample area 2 mm2 when spectral mapping if different from the microscope take-off angle. The homogeneous sample can be steel, brass, or copper and elemental maps shall be from soft and hard x-rays (e.g., Fe L & Fe Ka or Cu L & Cu Ka). The vendor shall indicate if and how their collimator affects this distance.

g) The detector will have a manual or automatic retraction mechanism.

h) Includes an extended parts and service warranty (4 years) and multiple software licenses (5 or more).

EDS analysis software and quantitative acquisition requirements:

a) High level graphical user interface program(s) with applications that include spectrum only acquisition, image with point and area analysis, region of interest mapping, hyperspectral mapping, line analysis, chemical phase mapping, automated particle (feature) analysis with phase identification and morphology, spectrum or quantitative analysis matching to a user defined database, phase mapping with feature analysis, mosaic phase mapping with morphological analysis. The application software will run on a Windows 10 64-bit operating system and be native 64-bit compiled not just 64-bit compatible.

b) Off-line licenses (and any hardware copy protection devices if necessary) shall be provided for running two or more copies of the vendor’s system software simultaneously on separate offline computers. This is to allow USGS to have one copy for on-line acquisition and analysis and other copies for off-line processing of spectra, orientations, calculation of quantitative data and image processing of previously acquired spectra, images, data and x-ray maps.

c) All vendor-provided software upgrades shall be provided at no extra cost to USGS for a period of three (3) years after the system final acceptance, as defined in the contract.

d) EDS peak identification and peak markers shall display or list all (K, L, M, N, etc.) x-ray lines capable of being generated at the operating voltage and all sum and escape peaks, and absorption edges for the major peaks.

e) The EDS spectral acquisition software shall include automatic peak identification including artifact peaks (e.g. sum peaks, escape peaks). Sensitivity for auto peak ID should be user adjustable.

f) Unattended automation shall be capable of loading shutdown or standby conditions when the project has finished.

g) The EDS software shall be able to generate synthetic spectra for any compound of known composition and density, given the instrumental conditions and determinable detector characteristics.

h) The EDS acquisition and quantification software shall offer standard-less capability.

Software options for quantifying any element (e.g. H, Li, C, O) by difference, stoichiometry, or specified amount shall be included.

i) If an EDS analysis is claimed to be quantitative (e.g. relative to standard intensities), the analysis shall include a determination of error, and a reference to how it is determined.

j) The quantitative x-ray microanalysis software shall provide complete routines for flexible and robust analysis of all major analytical peaks with a quantitative treatment and correction for spectral interferences, and also (but not limited to):

i) output of raw spectra to disk file in EMSA spectra standard format (or ASCII format),

ii) element and spectral line selection (Kα, Kβ, Lα and Mα) standardization and calibration,

iii) quantitative analysis (non-normalized) of a minimum of 32 elements or oxides, including calculating any element (e.g. hydrogen) by difference, by stoichiometry, by fixing formulas proportional to oxygen. These analyses shall be capable of employing user-provided, multi-element standards.

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

v) a standard database that can store profiles for up to 1000 standards with 32 elements each and include support for composition input by element weight percent or oxide weight percent (with default or user specified oxide cation ratios), or mole or atomic percents or formula atoms. If available, the ability to specify an element by fixed concentration is desirable when using user acquired standard profiles and the sum is NOT normalized to 100%.,

vi) provide correction routines for x-ray intensity data [ϕ(ρz), PAP, XPP, ZAF],

vii) 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, and

viii) background modeling of the x-ray continuum based on the displayed composition, properly scaled and corrected for detector configuration parameters.

EDS digital mapping and image analysis system

a) Digital x-ray maps to be acquired using the EDS detector ROI signals. At a minimum 1024 x 1024 resolution per map, a minimum of 16 separate x-ray maps (plus 1 BSE or SE channel) must be able to be acquired simultaneously. The maps must be capable of being stored to hard disk in TIFF format with false-color output capability.

b) Acquisition of digital microscope images (secondary, backscattered, x-ray, CL, etc.)

shall utilize full microscope control capability (digital beam control) through digital interface and have the ability to record beam position, accelerating voltage, stage position, magnification, etc. with each acquisition. Image output shall be standard TIFF format.

c) Provide qualitative 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.

d) 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.

e) X-ray maps stored to disk must be registered to stage coordinates for scale calibration for off-line processing. The EDS interface to the instrument must automatically read accelerating voltage, working distance, and stage coordinates for each spectrum and image acquisition.

f) X-ray maps constructed from spectral map datasets must also include net intensity maps which incorporate removal of background and peak overlaps, and the software must also provide a method to export the maps for quantitative post processing.

g) Pulse processing times easily adjustable in software, with at least 6 processing settings from lowest resolution/highest count rate to highest resolution/lowest count rate.

h) Spectrum imaging capability must be provided for at least 1024 x 1024 pixel images and 2048 MCA channels per pixel and the spectrum imaging file formats must be provided. Various tools must be provided for extracting images from the spectrum image data cube including peak identification for composite spectrum or maximal spectrum, data extraction in user defined areas such as polygon, flood-fill, circle, square, point, or linescans.

i) EDS mapping shall include spectral mapping (i.e., saving the entire spectrum). This capability shall also be true of linear determinations (e.g., line scans), and the dwell times for discrete special acquisitions shall be deadtime-corrected.

j) The vendor shall provide an automated stage drift correction for extended mapping sessions. Drift report shall display magnitude of stage drift correction during acquisition and system will automatically stop acquisition and save data if drift is too severe.

k) When the analyzed area is too large for uniform beam exposure or detection, the EDS software shall offer the capability of stitching together multiple x-ray maps or images or by offering a stage scan mode for large area mapping.

l) Subsequent numeric and graphical presentation of line scans and spatial mapping shall include absolute and background corrected counts, weight percent and atomic percent.

m) The EDS software shall accommodate unattended automation of the stage with respect to (1) unattended spectral acquisition from selected points, and (2) automating lines and spatial grids relative to (a) sample center and (b) selected endpoints.

n) The EDS software shall include phase analysis based on either cluster analysis, spectrum matching to a vendor provided database, spectrum matching to a user defined database, principle component analysis, or phase matching based on quantitative analysis of spectrum.

o) The software shall provide automated particle analysis and subgrain analysis with a minimum of twelve thresholds, which includes particle position, chemical composition, and morphology parameters including area, perimeter, aspect ratio, and x and y dimensions. Automated particle analysis can be done from a single field or over large areas. Particle analysis over large areas allows for automated stitching of fields of view.

Training requirements

a) Initial on-site training/familiarization from installation engineer.

b) Two days of on-site applications training from the vendor’s microanalysis applications specialist. Training can be attended by > 4 users. No expiration date on this training.

c) One credit toward on-line training.

2 - Acceptance of the instrument shall be based upon completion of installation and after testing of instrument hardware performance on site at USGS, Reston,VA, to ensure that the instrument meets all vendor factory specifications as determined by vendor field engineers and by personnel selected by USGS. Vendor reserves the right to use samples of its discretion to prove specification compliance. The vendor shall provide the necessary personnel, equipment, and facilities to conduct tests and the other specifications described below on the installed instrument.

Final acceptance is after the instrument meets all specifications in this document and all vendor factory specifications as determined by personnel selected by USGS. The final acceptance tests shall be performed on samples provided by USGS, including metals, alloys, minerals, resolution and magnification standards and insulating materials. Final payment will be made after all acceptance tests have been completed and the instrument meets all specifications in this document.

B - Deliverables:

1 – One EDS-SDD, EDS software and associated computer and monitor for hardware control and requisite training—all meeting the specifications given above.

2 – The above items shall be delivered within 3 months of award.

III - Supporting Information:

A - Place of Performance: USGS Reston, VA

B - Period of Performance: Machine installation and testing shall continue until above specifications and factory specifications are met.

C - Government Technical Contact: TBD

D - Government Furnished Property (GFP):

E - Special Considerations: