Specifications-final.docx

X-Ray Powder Diffractometer – Specifications I. Background The Materials and Structural Systems Division at the National Institute of Standards and Technology (NIST) is involved in the analysis, and development of standards and codes involving a wide range of construction materials, including cement clinker, cement, fly ash, blast furnace slag, and aggregate and is seeking an instrument to perform X-ray powder diffraction (XRD) study of crystalline and non-crystalline mineral, hydraulic cement, fly ash, slag, clays and other materials as well as polymeric materials in bulk and composite films for coatings.

II. Objective The Division is seeking a new, commercial, multipurpose X-ray powder diffraction instrument for study of these and other materials by qualitative, quantitative, and non-ambient analyses using multiple geometries.

III. Scope/ Minimum Technical Requirements

1) Geometries must include:

a) Bragg-Brentano geometry with vertical Theta-Theta configuration for reflection using flat pressed powder specimen mounts,

b) Reduced radius capability with appropriate slits, user-selectable and user-adjusted to increase Two-Theta coverage as needed for solid state detectors,

c) Transmission using a capillary spinner and focusing mirror optic for Mo radiation,

d) Transmission using X-ray transparent foils,

e) Micro-diffraction of small regions that have been user-identified and selected from a specimen mounted on an automated x,y,z stage using a magnified video imaging system, or video imaging system with laser z-height adjustment capabilities for positioning of the specimen,

f) Instrument must be mounted on wheels to allow moving in the lab.

2) Detectors

a) High efficiency solid-state detector(s) with a combined minimum of 0-, 1-, and 2-dimension data collection modes. Detector or detector combinations supplied with the system must be compatible with Cu, Mo, Ag, Cr, and Co X-ray anode sources and include a scintillation detector with appropriate slits and filters.

3) Instrument optics, sample stages, and X-ray tubes must be configured to permit interchangeability by laboratory users/staff within minutes with no more than 0.02°2 alignment error and must include the following:

a) Single specimen stage,

b) Flat positioning stage with programmable x,y, and z motion for microdiffraction with selection and alignment of the specimen sampling region,

c) Multi-specimen, automatic sample changer with user-controllable rotation and a minimum of 8 specimen positions. Preference given to automatic, individual control of simultaneous spin/wobble data collection,

d) Capillary spinner mount and goniometer head, with adaptors for 0.3, 0.5, 1.0, and 1.5 mm capillaries,

e) Open access to instrument to facilitate storage and exchange of x-ray tubes, sample stages and instrument optics.

4) Specimen holders

a) Cavity mounts with minimum 15 mm diameter, quantity 12

b) Back-load with minimum 15 mm diameter, quantity 12

c) Cavity mounts with minimum 20 mm diameter, quantity 4

d) Side-load mounts, quantity 4

e) Sealed domed specimen holders for environmentally-sensitive materials, quantity 10

f) Capillaries (quartz glass) (0.5, 1.0, 1.5 mm) , quantity 25, each

g) Zero-background inserts (quantity 3) for standard cavity mounts

h) X-ray transmission holders with foil (quantity 3 holders, foil material for at least 100 specimen mounts, e.g., Kapton and/or Etnom, or similar)

i) Sample preparation apparatus for holding back-loading samples

5) System optics to include:

a) Incident optics to include i) a programmable divergent slit and anti-scatter slit assembly operable in both fixed slit or variable mode, or ii) a fixed divergent slit block with manual slit sets for both incident and diffracted beam side and a flat mirror divergent beam optic with K radiation discrimination. Preference will be given to a flat mirror divergent beam optic with K radiation discrimination,

b) Focusing elliptical mirror for high resolution transmission geometry,

c) Discrete point focus optics (e.g., mono- or poly-capillary lenses) for micro-diffraction experiments ranging from 50 m, 100 m, and 300 m spot sizes,

d) Appropriate K filters for both the incident and diffracted beam sides to remove unwanted radiation and fluorescent background for all X-ray/anodes purchased,

e) All appropriate divergence, anti-scatter slits, beam knives/stops, and masks necessary for all radiations used and goniometer radii,

f) One set each of normal- and high-resolution Soller slits for incident and diffracted beam sides.

6) X-ray tubes to include:

Cu long-fine focus and Mo long-fine focus. Tubes shall be user-installable and convertible from line to spot focus.

7) All system optics and sample stages must be exchangeable with reconfiguration by the user with no more than a 0.02°2 alignment precision in measurement of the (111) reflection on a fixed silicon plate, or other fixed reference plate (e.g., NIST SRM 1976 sintered alumina for XRD).

8) Instrument Control, data acquisition, processing and analysis Integrated computer for instrument control, data processing and analysis as listed below as minimum requirements:

9) Data Display, Processing and Analysis Full data collection and instrument control software including capabilities for batch control of multiple samples and dedicated, intelligent software application to recognize and facilitate hardware and configuration changes

10) Data analysis software as described below:

a) Comprehensive codes for instrument control, performance monitoring, and data display, manipulation, processing, and analysis.

b) Full qualitative and quantitative analysis of phase compositions using Rietveld and other methods including Reference Intensity Ratio (RIR), internal standard, external standard, and Partial or No Known Crystal Structure (PONCKS).

c) Ability to process powder diffraction data from neutron and synchrotron sources using both full phase/profile analysis and Rietveld.

d) Search-match using multiple powder diffraction databases, including a user-generated database, ability to constrain the search based upon material bulk chemistry,

e) Able to collect, process and analyze data for pair distribution analysis,

f) Data import and export in multiple file formats such as GSAS and X-Y

g) Must be capable of creating and using a user-developed database from user’s CIF files without error in translation.

h) Databases for search-match and Rietveld refinement must include: ICDD PDF 2 and ICSD;

i) Provisions to create a user database based upon CIF files for search-match and Rietveld refinement

11) Safety Enclosure:

a) Shall provide full radiation protection,

b) Doors shall be composed of X-Ray absorbing glass so that the instrument may be observed during operation,

c) Shall provide large-area uninhibited access to the instrument for adjustments and exchange of instrument components. Access doors shall open laterally and provide a minimum of 30 inches wide and 30 inches high opening however, preference will be given to larger opening access.

12) Recirculating water chiller with all connections to the instrument and to house water source for heat dissipation. Water access provided by NIST.

13) UPS to serve as a power conditioner and to carry instrument over short-duration power loss,

14) System delivery, installation, initial setup, confirmation of performance, and on-site initial training by a company field service engineer,

15) 24-hour turn-around time for problem inquiries by telephone or e-mail, and locally-available company field service engineers who specialize in service and repair of that manufacturer’s x-ray powder diffraction instrumentation available within 72 hours.

16) On-site training for a minimum of 2 days to be provided by a qualified manufacturer’s XRD application scientist

17) Training in the manufacturer’s user school for three individuals

18) Optional Items

1) Anton Paar CHC+ chamber, MHG humidity generator, compressed air-cooled, nitrogen cooled, with integration and instrument control software.

2) Cross-slit collimator for sampling spot sizes approximately 500 um to 2 mm, continuously variable in the equitorial and axial direction to collimate the beam from <2 mm up to several mm.

3) Small spot-size collimators for line focus optics to permit rapid microdiffraction analysis of areas ranging from approximately 0.2 mm to 0.5 mm in size without changing tube orientation.

4) Ag long-fine focus X-ray tube

19) Delivery & Acceptance Requirements

Delivery shall be within 150 days after award and installation shall be 15 days after delivery unless special arrangements are agreed upon.

The Contractor shall perform testing after start-up which shall consist of demonstration of the individual instrument components and their appropriate use and performance for data collection, including an analysis of NIST SRM 1976 for evaluation of diffraction peak intensity across the 2-theta scale from 20 degrees to 150 degrees per the SRM 1976 certificate and Lab6 resolution performance test. Evaluation based upon peak position and relative intensity as well as an evaluation for spectral contamination lines. Evaluation will occur after installation on NIST’s instrument in Gaithersburg, MD by the manufacturer’s field service engineer.

20) Government Furnished Property None

21) Security Considerations None

22) Travel None

23) . Place of Performance Gaithersburg, MD