SOW_FOR_RFQ.pdf

Request for Quotation Number SB1341-16-RQ-0594

Statement of Work

BACKGROUND

At present, the Eagle III µXRF, owned by the National Institute of Standards and Technology, an out-of-date, faulty, and beyond effective service life instrument, has been decommissioned, leaving the Materials

Measurement Science Division (MMSD) with no viable µXRF capability. The decision has been made to purchase a new, state-of-art system with all available modern features for futureproofing the research effort.

Due to the large customer base needing elemental survey, the new system must produce X-ray images much faster and more efficiently than the older models. Most importantly, the new system must be equipped with a silicon drift detector, capable of counting with high linearity into the 100,000 counts per second with high quality data reduction, and 400,000 counts per second survey measurements, allowing for fast point-to-point area maps.

A -focused X-ray fluorescence spectrometer (µXRF) is an instrument capable of analyzing X-rays fluoresced from a sample in an X-ray chamber. Each µXRF has five basic components:

1) An X-ray tube (or multiple tubes)

2) A poly-capillary optic

3) An X-ray detector (or multiple detectors)

4) A sample stage (X, Y, and Z translation)

5) A magnifying optical camera (coupling visible images with composition maps).

X-ray tubes generate what are known as “incident” X-rays. These X-rays are focused into a small spot approximately 15 µm to 50 µm in diameter, typically by a poly-capillary optic. Once focused, the X-ray beam is targeted to coincide with an optical target location on a sample which is moved around on the sample stage.

The sample emits secondary or “fluoresced” X-rays, which are then received by the X-ray detector. Modern µXRF instruments use silicon drift detectors (SDDs) as the primary X-ray detector(s) in the system. These can have large surface areas, such 30 mm2 to 60 mm2 allowing for the collection of a large percentage of emitted X-rays. By automating the motion, X-Y translation, of the sample stage and simultaneous collection, of a magnified optical image, and of the fluoresced X-rays spectra, the µXRF tool can be used to image which elements are fluorescing and image these elemental concentration maps, via spectra peak fitting. X-ray images, also known as hyperspectral images or X-ray spectrum images are a primary method by which composition and structure of complex, large samples can be analyzed.

With the decommissioning of present NIST owned µXRF instrumentation, this type of analysis constitutes a critical need not currently available for the Materials Measurement Science Division. The capability to create these large area compositional maps is a vital to many researchers within MMSD, who routinely analyze complex, heterogeneous materials; a task which could be enhanced significantly through the use of a dedicated µXRF instrument. Also, the Division is actively engaged in creating new measurement methods and analysis techniques based on µXRF technology, requiring an instrument both capable of high volume survey measurements, and state of the art measurement and analysis development. The current state-of-the-art in commercial instrumentation consists of tools with simultaneous excitation energies allowing complex data reduction unavailable with single source excitation, and systems with multiple detectors which allow for distinguishing between fluorescent spectra (which provide elemental analysis) and diffraction spectra (which could provide crystal orientation, if this information can be de-convoluted). This required instrument is intended to provide this dual purpose instrument capability.

BRAND NAME OR EQUAL

This is a brand name or equal requirement. Brand name or equal description is intended to be descriptive, but not restrictive and is to indicate the quality and characteristic of products that will be considered satisfactory to meet the agency’s requirement.

SCOPE OF WORK

The Contractor shall provide one (1) µXRF spectrometer system, Bruker Corporation M4 Tornado, or equivalent, including installation, training and warranty and meeting all salient characteristics and requirements described herein.

REQUIRED SPECIFICATIONS

Section 1: X-ray Optics: Minimum specifications

1. The system must be equipped with one (1) poly-capillary optic coupled to a Rhodium X-ray tube.

a. Must be co-aligned within < 5 m to the cross hair of the coupled optical magnifying camera.

b. The maximum “spot-size*” (long axis of the ellipse) shall not exceed 30 µm.

*The “spot-size” is herein defined as the smallest ellipse in X-Y stage motion, which will contain 86% of total intensity, as measured with the X-ray detector, of the X-ray photons incident upon the sample. [Note that an ellipse containing 86% of total intensity (spot-size) will have dimensions of 1.7 times FWHM (X) by 1.7 times

FWHM (Y) for a Gaussian beam (also known as the 1/e2 widths in the X and Y dimensions).]

The method used for determining the spot size must be provided. The spot-size must be determined by one of three methods:

-Passing the beam over an abrupt (atomic) interface (such as a Cu-Zn interface or some other suitable experiment) and observing the count rate in the Cu and Zn peaks as provided by the X-ray detector (to determine either FWHM or 1/e2 width); or

-Passing the beam over a small diameter hole to measure X-ray signal drop and observing the overall count rate as provided by the X-ray detector (to determine either FWHM or 1/e2 width); or

-Mapping a sample containing semiconducting processed metal (Cr) lines on a quartz substrate of known spacing and deconvolution of the beam profile shape from the resulting image to determine FWHM

(method to be used in qualification).

The “spot-size” must be expressed as the major and minor dimensions of the ellipse of 86% intensity (note that either 1/e2 width or FWHM are acceptable expressions, provided the source is known to have Gaussian beam character).

2. Must be capable of mounting a 2nd X-ray source within the instrument housing. The instrument must be designed to accommodate two X-ray sources.

Section 2: Stage, Cabinet and Vacuum System

1. The user must be fully shielded from all radiation produced by the X-ray tubes or the sample.

2. The system must provide a roughing pump for evacuating air from the sample chamber to pressures below 1 kPa.

3. The stage must have a travelling distance of at least 100 mm in the two horizontal directions (X & Y), and at least 60 mm in the vertical direction (Z).

4. The sample chamber must be interlocked such that the X-ray tubes are shuttered whenever the chamber is open.

Section 3: X-ray detector hardware: Required features

1. The system must contain one energy dispersive X-ray detector, aligned to detect fluoresced X-rays from the sample.

a. The X-ray detector must be a silicon drift detector (SDD)

b. The detector must have a minimum active area of 50 mm2.

c. The detector must have an active silicon area of at least 400 m thickness.

d. When counting at an output count rate of 100,000 counts per second, FWHM of the Mn Kα peak must be 150 eV or lower.

e. The system must have ports for the mounting of one additional energy dispersive X-ray detector.

2. The system must be equipped with pulse processor(s) paired to (each of) the X-ray detector (s). The pulse processor(s) must have a software adjustable time constant allowing for tradeoff between energy resolution and count rate.

Section 4: X-ray detector software (single point analysis)

1. The system must include a data analysis and acquisition software package capable of collecting individual X-ray spectra. Additionally, the user must be able to:

a. Set the time of the acquisition in live time or real time seconds, and

b. Save the collected spectra in the MSA (Microscopy Society of America, or .msa extension file) or equivalent open source format.

2. The system must be capable of automating individual point collection. The user must be able to:

a. Manually select stage locations and store them to a table (table of arbitrary size, with no maximum number)

b. Import a series of stage locations from another file for automatic analysis

c. Select automated processing for spectra that includes compositional analysis (elemental identification and ratios between identified species) and net counts (after background subtraction in software defined regions of interest).

i. Automated processing reports must be able to be stored in a tab delimited text file (with file extension of .txt or .dat) or a comma separated variable file (with file extension of

.csv).

Section 5: X-ray detector software (hyperspectral imaging)

1. The system must be capable of collecting a hyperspectral X-ray image.

a. A full spectrum (all energy channels) must be saved at each (X,Y) target point.

b. The user must be able to select the spectral range stored in the database [(min, max) energy region of interest or full energy range].

c. The user must be able to manually select the scan range dimensions and pixel spacing [or supply a table of (X,Y) targets] used to collect the hyperspectral image.

d. The software must save the hyperspectral image to disk periodically (after every collection point) so that partial images can be recovered (and resumed) if the system loses power.

Section 6: Quantitative analysis software

1. The software must be capable of converting net elemental counts in an X-ray spectrum into weight percent compositional values. The user must be able to select the method used to determine the compositional values, and those methods must include:

a. A standardless, “Fundamental Parameters” method

b. A single standard scaling method

c. Multiple standards based quantitative analysis (i.e. calibration curve methods).

2. The software must perform this quantitative analysis on single pixels in an X-ray spectrum image.

3. The software must perform the necessary elemental composition analysis for key elements of interest for heterogeneity testing and for identification of trace substance detection.

a. The instrument must be capable of Instrumental Line Detection limits of less than 5 g/g for the following elements (provided a suitably overlap free matrix sample): Cu, Zn, Sr, Zr, Nb, Mo, Pb, Th, and U.

Section 7: Other requirements

1. In instances where proprietary file types are used to store X-ray data or instrumental parameters, the

Contractor must provide either:

a. adequate documentation (such as a pdf or word document describing the data encoding structure) so as to allow NIST to produce a program capable of reading the file and recovering all of the data and metadata contained therein, or

b. software to convert or use file types that are open source (such as tab-delimited text or comma separated variable) or documented by common trade organizations (such as the NIST Lispix Raw format or the

MSA file format)

2. Documentation provided as part of the previous requirement must not require any NIST employees to sign a non-disclosure agreement of any kind.

3. The system must include an operations and maintenance manual covering proper operation, routine maintenance, and troubleshooting for the instrument and controlling software.

4. All equipment must be new. Used or remanufactured equipment is not allowable.

Installation The Contractor shall install the instrument in Building 217, at NIST Gaithersburg, MD. Installation shall include, at a minimum, uncrating/unpacking of all equipment, set-up and hook-up of all equipment, start-up, demonstration of specifications, and removal of all trash. The instrument must meet all required specifications identified above upon completion of installation.

Installation must take place during normal business hours, between 8:30 am and 5:00 pm Eastern Time, Monday through Friday except Federal Holidays, and must be coordinated with the NIST Technical Point of

Contact (TPOC).

Training

The Contractor shall schedule and facilitate training for two (2) NIST personnel, on-site at NIST Gaithersburg.

The training shall provide a thorough demonstration of all equipment functions, equipment operation and basic troubleshooting. The training may be completed on-site at NIST immediately after successful completion of installation and demonstration of specifications.

Warranty

The Contractor shall provide, at a minimum, a one-year warranty for the equipment. The warranty shall cover all parts, labor and travel. The warranty shall commence upon successful completion of delivery, installation, training and demonstration of all required specifications.

Option Line Items

The following are option line items. Quoters must provide a firm-fixed price for all option line items. The price for these option line items shall remain valid for a period of 12 months from the date of award.

The Government may exercise one or more of the option line items, at its discretion, at the time of award and/or at any time within 12 months from the date of award. Option line items will be exercised by the issuance of a modification (Standard Form 30).

OPTION LINE ITEM - X-ray Optics – Reference Section 1.

The system must be equipped with one (1) collimated Mo X-ray tube.

a. Must be co-aligned within <10 µm to the cross hair of the coupled optical magnifying camera.

b. Must use a collimator permanently aligned to the X-ray tube.

c. The “spot-size” must not exceed 2 mm in any dimension.

OPTION LINE ITEM - X-ray detector hardware – Reference Section 3.

The system must be equipped with a second energy dispersive X-ray detectors, aligned to detect fluoresced X-rays from the sample.

a. The X-ray detector must be a silicon drift detector (SDD)

b. The detector must have a minimum active area of 50 mm2

c. The detector must have an active silicon area of at least 400 m thickness

d. When counting at an output count rate of 100,000 counts per second, FWHM of the Mn Kα peak must be 150 eV or lower.

Acceptance testing

The “spot size” (the ellipse of primary intensity, as defined in Section 1) of the beam will be measured at NIST using the Cu-Zn interface method or imaging reference artifact, provided by NIST.

1. The instrument must be tested at NIST once the installation is complete.

2. The “spot size” (the ellipse of primary intensity, as defined in Section 1) of the beam shall be measured at NIST using the Cu-Zn interface method or imaging reference artifact, provided by NIST.

3. The instrument will have a radiation survey conducted by the NIST Radiation Safety Division (RSD).

The RSD will ensure that there is no X-ray radiation escaping the instrument and that the X-ray interlocks are working properly.

4. The energy resolution and output count rate of the detector will be tested to ensure compliance with

Section 3 using a specimen of pure copper and calculated using DTSA II.

5. A full spectra for each the four NIST samples (from section 6) must be made available for analysis.

These spectra must be at least 512 points over full energy range. In addition, qualitative compositional analysis for each point should be provided.

6. A full, hyperspectral X-ray image over an area no smaller than 10 cm2 will be acquired and the subsequent data will be saved in an open source format.

7. Four samples will be provided by NIST with the elements Cu, Zn, Sr, Zr, Nb, Mo, Pb, Th, and U, and the relative mass fractions (weight percentage) must be determined.

PERIOD OF PERFORMANCE

Delivery, installation and training shall be completed not later than five months from the date of award.

PLACE OF PERFORMANCE

All work shall be completed at the Contractor’s facility. Installation of the instrument and training shall be accomplished at NIST, Gaithersburg, Maryland.

DELIVERABLES

Description Quantity Due Date

Analytical instrument One (1) 90 days after award of this requirement.

Installation of the analytical instrument Once 120 days after award of this requirement.

Operations and maintenance manual for the analytical instrument

One (1) 120 days after award of this requirement

Training of NIST personnel at NIST, Gaithersburg, MD

Once 150 days after installation.

GENERAL INFORMATION

Safety: The Contractor employee shall be responsible for knowing and complying with all installation safety prevention regulations. Such regulations include, but are not limited to, general safety, fire prevention, and waste disposal.

Security: NIST is a restricted campus. An identification badge is required for access for entry into buildings and also is shown to the armed Security Police when entering the campus.

Identification Badges: Contractor employees shall comply with NIST identification and access requirements.

The Contractor employee is responsible for absences due to expired identification and access documents. Each

Contractor employee shall wear a visible identification badge provided by the NIST Security Office. The badge must show the full name, title, and if required by NIST, the words “Contractor” in front. The Contractor employee shall turn in the NIST identification badge and vehicle pass to the TPOC, COR, or Contracting

Officer (CO) upon termination of their services under this contract.

Vehicle Registration: All Contractor employees must register their vehicles with the NIST Security Office to gain access to the campus. A valid driver’s license, Government-furnished civilian ID, proof of insurance and current registration must be presented to the NIST Security Office, at which time a NIST vehicle pass must be issued. The pass shall be displayed on the vehicle’s rear view mirror in accordance with instructions. The

Contractor employee shall follow NIST procedures for removal and turn-in of the vehicle pass upon termination of services under this contract.

Media Inquiries: The Contractor employee shall not respond to any media inquiries. Any inquiries from the media shall be immediately relayed to the TPOC, COR, and/or CO. There shall be no interviews, comments, or any other response without the knowledge and approval of the NIST Director.