SOW_final.pdf

Statement of Work (SOW)

H3WM03

Wavelength Dispersive X-ray Fluorescence (WDXRF) Spectrometer

1. SCOPE - This Statement of Work (SOW) provides the requirements/specifications for the furnishing, shipping, assembling, installing, verification, calibration, testing, and training of a wavelength dispersive x-ray fluorescence (WDXRF) spectrometer suitable for elemental quantitative analysis of plasma spray powders, quantitative elemental analysis of metals used on jet engines and aircraft, elemental quantification of aerospace coatings, and elemental quantification of corrosion products, chemicals, reaction products, and foreign materials that are encountered in depot activities. The WDXRF instrument shall detect all elements from Boron (B) to Americium (Am) with sufficient resolution, sensitivity, accuracy, precision, and reproducibility to satisfy all items in this

SOW. The contractor shall provide all labor, tools, equipment, materials, parts, personal protective equipment (PPE), transportation, shipping and any other incidentals necessary to complete the requirements of this SOW. The contractor shall provide basic operational training for all supplied equipment/software to Tinker AFB personnel following installation by the contact acceptance by government personnel.

2. REQUIREMENTS/SPECIFICATIONS

2.1 DESIGN - The instrument shall be of the manufacturer’s current design. It shall be a new unit and include any additional features necessary to comply with the requirements specified herein. Additional features which are not specified herein, but are part of the manufacturer’s current design, shall be included in the furnished equipment.

2.2 SAFETY - The instrument shall be equipped with all necessary safety devices per

American National Standard for WDXRF instrumentation for protection against exposure to x-rays. It shall have any other protective devices as necessary to prevent x-ray exposure to the operator, damage to the equipment, or erroneous data input or output. X-ray safety requirements are Less than 1 μSv/hour at 10 cm from the outside surface.

2.3 WARRANTY – The vendor shall provide a complete standard commercial warranty on the instrument and X-ray tube.

2.4 GENERAL SPECIFICATIONS

2.4.1 - Instrument shall be a sequential (scanning) WDXRF spectrometer with a minimum 4.0 KW generator and Rhodium tube. The instrument shall incorporate an end window X-ray tube capable of an output of no less than 4 kW and operate between a maximum lower limit of 20 kV and minimum upper limit of 60 kV. The x-ray tube current shall operate between a maximum lower limit of 10 mA and minimum upper limit of 160 mA. The x-ray tube and optics must be below the sample as many types and varying amounts of liquids, loose powders, widely ranging quantities of reaction products, and samples with entrained air that all must be quickly analyzed with minimal sample preparation. The WD optical path shall be arranged in such a manner that the following protections for the x-ray tube are as follows: 1) dust protection at the sample port, 2) filter in place over x-ray tube when sample is in motion, 3) optical path designed so debris falling from a sample is retained in the well around the tube, and 5) protective coating on tube window. X-ray tubes that allow the degradation of light element signal over time due to the deposition of W inside the tube are not acceptable.

2.4.2 - Stability of the generator shall be as good as or better than 0.0006% for 10% mains variation.

2.4.3 - The goniometer shall incorporate a readout to measure actual angular position for maximum accuracy and reproducibility. The goniometer shall incorporate a decoupled theta/2 theta drive system. The goniometer shall employ accurate absolute angular encoders on the output theta and

2-theta shafts. Angular accuracy shall be as good as or better than 0.0025˚ θ and 2θ. Angular reproducibility shall be as good as or better than 0.0001˚ θ and 2θ.

2.4.4 - A minimum of eight crystals shall be used to cover the full measurable range. The

8 crystals will exhibit d-spacings either identical to or very similar to those listed below to best meet all requirements of this SOW.

1. 2d=0.2848 nm for the K-lines covering V-Ce and L-lines covering Pr-Am.

2. 2d = 0.4027 nm with high reflection intensity for K-lines covering K-V and Nb-I and L-lines covering In-Ce.

3. Curved Ge-111 (2d=0.6532 nm) for K-lines covering P-Cl and L-lines covering

Zr- Ru.

4. 2d = 0.8746 nm for k-lines of Si and Al and L-Lines of Rb and Br.

5. d-spacing (2d = 5.0 nm) for O-Mg.

6. d-spacing (2d = 19.0 nm) for Boron.

7. d-spacing (2d = 12.0) nm for Carbon.

8. d-spacing (2d = 11.0 nm) for Nitrogen analysis

9. d-spacing (2d = 3 nm for Mg analysis

10. d-spacing (2d=4.9908 nm)

11. d-spacing (2d=11.0000 nm)

12. d-spacing (2d=16.0000 nm)

13. d-spacing (2d = 12 nm)

14. d-spacing (2d=30 nm)

2.4.5 - A minimum of three (3) distinct collimators of different spacings (acceptance angles) shall be provided.

2.4.6 - The tube filters included with instrument shall include the following: Ni, Al, and brass (no less than four distinct filters) such that resolution and sensitivity is sufficient to achieve every item of this SOW including the concentration ranges and detection limits of Appendix I.

2.4.7 - The instrument shall have a minimum of three collimator-mask-sample-holder-aperture-diameters to accommodate a range of sample sizes. The collimator-mask-sample-holder-aperture-diameters shall range from a minimum that is no greater than 10-mm-diameter to a maximum of no less than 35-mm-diameter. The instrument shall be able to analyze the flat face of a cylindrical sample with maximum height of no less than

45mm and maximum diameter no less than 50 mm. instrument shall be capable of analyzing the entire flat face of a cylindrical sample with minimum diameter no greater than 10 mm and maximum height of no less than 45 mm without any x-ray fluorescence from the sample cup being detected.

2.4.8 - The detectors shall include a flow proportional counter detector for light element

(long wavelength) detection, scintillation counter for heavy element (short wavelength) analysis, and a sealed Xe detector for the medium wavelength x-rays. The sealed Xe detector shall be mounted behind the flow detector so that both detectors can be used simultaneously for improved analysis of k-lines of Sc-Ni (4.0-7.5 KeV) and L-lines of

Pr-W. All three detectors shall be capable of having linear response for high count rates.

The scintillation detector shall have a very high dynamic range exhibiting linear range up to no less than 3.5 Mcps. The simultaneous use of the sealed Xe detector and flow detector will also exhibit a very high dynamic range exhibiting linear range up to no less than 3.5 Mcps.

2.4.9 - Spectrometer shall incorporate modern counting electronics including Dual multichannel (MCA) analyzers with digital signal processors for optimal performance. The counting electronics shall incorporate automatic dead time correction and automatic selectable pulse shift correction. The counting electronics will be capable of supporting accurate data collection scanning speeds of 10-degrees-two-theta-per-second.

2.4.10 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify

Mg at a detection limit of no greater than 0.10 percent-magnesium-by-weight in any aluminum base alloy in both Helium environment and vacuum.

2.4.11 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify silicon at detection limits no greater than 0.01 weight percent in nickel alloys containing

8.0-weight-percent- tungsten in both Helium environment and vacuum.

2.4.12 - Spectrometer resolution and sensitivity shall be sufficient to resolve L-lines of Hf, Ta, Re, and W for nickel alloys with detection limits given in Appendix 1.

2.4.13 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify Re at detection limits no greater than 0.01 weight percent for nickel alloys that contain major W, Ta, and Hf.

2.4.14 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify Hf at detection limits no greater than 0.01 weight percent for nickel alloys that contain major W, Ta and Re.

2.4.15 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify

Ta at detection limits no greater than 0.01 weight percent for nickel alloys that contain major W, Hf, and Re.

2.4.16 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify

W at detection limits no greater than 0.02 weight percent for nickel-based superalloys that contain major amounts of Ta, Hf, and Re.

2.4.17 - Spectrometer resolution and sensitivity shall be sufficient to accurately quantify sulfur at detection limits no greater than 0.01% in nickel-based superalloys that contain

4.5% molybdenum in either Helium environment or vacuum.

2.4.18 - The spectrometer shall be equipped with an integrated X-Y-Z sample changer.

The sample changer shall have the capability of loading solid samples into sample holders and handle all required sample holder movements. The sample changer shall incorporate a design with removable changer trays that can be preloaded externally during sample changer operation.

2.4.19 - Software package shall include factory installed standard-less fundamental parameter (FP) analysis of various sample types based on factory analysis of a set of glass beads and/or briquettes containing all elements O (Oxygen) - U (Uranium). FP-measurement- program shall take no greater than 30 minutes to cover the elements from

O - U. This FP- measurement-program shall be fully capable upon installation. The set of glass beads and briquettes that were analyzed at the factory to create the FP- program shall be provided with the instrument. This FP-measurement-program shall be capable of semi-quantitative analysis of solids, pressed or loose powders, fused beads, and liquids where the program includes provisions for detailed sample and sample preparation information. Automated results from the FP-measurement-program shall be an output data file listing each element of the analyzed sample and its relative concentration.

Automated results shall also include the spectrum from each 2-theta scan along with each

XRF peak identified. Background subtraction, peak identification, overlap and matrix corrections, calculation of semi- quantitative concentrations and normalization are all done automatically for a fast and easy semi-quantitative analysis of unknown samples.

This means that immediately after installation at the site, the instrument is ready to perform meaningful analysis on unknown samples by a technician. The set of glass beads and briquettes used to generate the FP-program will be provided with the instrument. This FP program shall contain nominally 11 different 2-theta scans of differing combinations of crystals, collimators, detectors, tube filters, tube voltage/current, PHD settings. Software shall allow addition of scans to this analytical program as needed. The application shall be expanded to generating 2-theta scans of the lighter elements of Boron, Carbon, and Nitrogen after delivery and during installation.

2.4.20 - Software package shall include ability to type standardize using only one certified reference material (CRM). The software shall allow two-theta scans of the

CRM and analyte to be graphically compared.

2.4.21 - FP matrix correction algorithms are available for a single analytical program for

Nickel, Cobalt, and Iron high temperature alloy analysis. No less than 100 certified reference materials comprising steel, high- temperature alloys, and super-alloys will be measured at the OEM factory prior to installation in order to generate the appropriate FP algorithm that calculates matrix corrections appropriate to Nickel, Cobalt, and Iron high temperature alloys from the theoretical laws governing the physics of x-rays. This special program will be prepared by measuring a wide range of nickel, iron, and cobalt alloys over a wide range of concentrations. The elements to be included are as follows: Al, Si, P, S, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Y, Zr, Nb, Hf, Mo, Ta, and W. This application uses the FP model as a matrix correction model. The FP model calculates matrix corrections that are specific to each sample. This model will enable accurate analyses over very wide ranges in concentration and in very different types of Ni-Fe-Co samples. Over 250 certified reference materials covering these superalloys are available at Tinker AFB, OK.

This specialized analytical program shall be formed at the factory and completed at

Tinker AFB using CRMs covering a wide range of superalloys with different calibrations for chill cast versus slow cast (different calibrations for different metallurgical micro-structures).

2.4.22 - FP matrix correction algorithms are available for a single analytical program to analyze copper alloys including brass, leaded brass, manganese brass, aluminum bronze, phosphor bronze, leaded bronze, bronze, and cupro nickel. This specialized analytical program shall be formed at the OEM factory prior to installation. Certified reference materials will be measured at the OEM factory prior to installation to generate the appropriate FP algorithm that calculates matrix corrections appropriate to copper alloys from the theoretical laws governing the physics of x-rays. This special program will be prepared by measuring a wide range of copper alloys over a wide range of concentrations at the factory. The elements to be included are the following: Mg, Al, Si, P, S, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb, Bi. This application uses the FP model as a matrix correction model. The FP model calculates matrix corrections that are specific to each sample. This model will enable accurate analyses over very wide ranges in concentration and in very different types of copper alloys.

2.4.23 - FP matrix correction algorithms for aluminum base, titanium base, magnesium base, lead base, zinc base, and low alloy steels shall be provided with instrument.

2.4.24 - Spectrometer with software package shall allow for oxygen quantification (film thickness) to be used as complementary technique to GDOES-depth profiling and XPS for discernment/compliance of different anodizing processes: Sulfuric acid bath, alumilite, oxydal, chromic acid, oxalic acid, and Ematal where the oxide film thickness ranges from 5-60 microns on aluminum surface.

2.4.25 - Instrument shall be capable of analyzing all elements within the maximum and minimum limits given in Appendix 1 in both vacuum and Helium environments.

2.4.26 - Instrument shall be capable of analyzing Boron in nickel-base braze materials that contain 3% boron. Instrument shall be capable of analyzing carbon and nitrogen in nitrocarburized case hardened materials.

2.4.27 - A trace analytical program shall be included to obtain the most accurate possible net intensities for analyte peaks which are subject to large corrections for background and spectral overlap. This TRACE analytical program shall use primary and secondary mass absorption coefficients (MACs) to make matrix corrections to net intensities prior to calculation of calibration equations for analyte elements and prior to calculation of the analyte concentrations for unknown specimens.

2.4.28 - Spectrometer shall be capable to conduct liquid analyses I.A.W. ASTM D2622

Standard Test Methods for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry for ultralow sulfur concentrations in petroleum samples.

2.4.29 - Spectrometer and software shall be capable to conduct the following ASTM analyses:

1) ASTM E1085-16 Standard Test for Analysis of Low Alloy Steels by Wavelength

Dispersive X-ray Fluorescence Spectrometry.

2) ASTM E539 Standard Test Method for X-Ray Emission Spectrometric Analysis of

Titanium alloys by Wavelength Dispersive XRF Spectrometry.

3) ASTM E572-94 Standard Test Method for X-ray Emission Spectrometric Analysis of

Stainless Steel.

4) ASTM D4927-10 Standard Test Methods for Elemental Analysis of Lubricant and

Additive Components-Barium, Calcium, Phosphorous, Sulfur, and Zinc by Wavelength

Dispersive X-Ray Fluorescence X-Ray Fluorescence Spectroscopy.

2.4.30 - The spectrometer shall be housed in a cabinet that is sealed and thermally controlled.

2.4.31 - The spectrometer shall be mounted on heavy duty wheels for easy mobility and an umbilical cord for power, gasses, and water supplies interfacing with a wall unit for easy installation and maintenance.

2.4.32 - The spectrometer shall have a sample introduction system that incorporates an airlock, sample turret and gravity positioning of the sample cups over the X-ray source for ultimate sample to sample precision. X-ray tube shall remain energized at full operating power during sample loading to prevent instability and unnecessary thermal shock to the X-ray tube. The spectrometer shall be able to be loaded both manually and via an X-Y-Z sample changer. The sample loading port shall be equipped with an optical sensor capable of differentiating between liquid and solid samples to prevent accidental loading of liquid samples in vacuum.

2.4.33 - A helium purge system for the analysis of liquids and loose powders shall be included with spectrometer. The helium system shall flush the entire optical path with a constant flow of helium where the sample, detector, crystal, and x-ray tube are all in contact with Helium and are all at the same Helium pressure throughout the Helium-purge analysis. Light element sensitivity and detection limits under Helium purge will meet the requirements in Appendix 1.

2.4.34 - The spectrometer shall be provided with a Refrigerated Water Re-circulating

System (RWRS) to cool the rhodium anode using a water-cooled condenser.

2.4.35 - The RWRS shall be equipped with a flow meter to visibly display flow rate of water through WDXRF spectrometer. The pump and equipment shall be automatically de-energized if water flow stops.

2.4.36 - The RWRS shall be equipped with a high temperature thermostat to measure the supply water temperature. If the temperature of the water in the reservoir rises above thermostat setting of 80 degrees F, the switch contacts shall open which is in turn interlocked to the WDXRF electrical control-circuit such that the tube will de-energize when water temperature rises above 80 F.

3 ON-SITE INSTRUMENT INSTALLATION VERIFICATION AND TRAINING

3.1 The vendor shall provide on-site installation and verification by demonstration that the instrument is in working order and meets all the requirements of the SOW. Installation and verification shall be accomplished during normal operating hours of Monday –

Friday 7:00 am – 3:00 pm.

3.2 The vendor should include 4 days of on-site application support by an applications specialist. The on-site application support shall be provided during normal operating hours of Monday – Friday 7:00 am – 3:00 pm.

4 QUALITY ASSURANCE

4.1 QUALITY CONFORMANCE INSPECTION

4.1.1 - A quality conformance inspection shall be conducted after installation of the instrument is completed, ensuring calibrations have been tested and verified to be accurate under supervision of government representatives and/or SME’s. Failure of any item to pass any examination or test shall be cause for rejection. The WDXRF spectrometer, and its associated equipment, within this purchase will remain the property of the contractor until all items of this quality conformance inspection have been passed and accepted by the government representative(s).

4.1.2 - The installed instrument shall meet all the requirements stated in the SOW, conform to the vendor’s own drawings, specifications, standards, and quality assurance practices.

Appendix 1. Each element listed under each base metal below will be accurately quantified in the given range in relative weight present.

Iron-base (Low alloy, Tool, cast, and stainless steels)

Si 0.01 - 19 (PHD windows are adjustable and set to exclude FeK-beta (4th order)) Mn 0.01 - 19 P 0.01 - 2 S 0.01 - 0.4 Cr 0.01 - 32 Mo 0.01 - 9.5 Al 0.02 - 3.0 Co 0.02 - 21 Cu 0.01 - 8 Nb 0.01 - 3.0 Ti 0.01 - 3.0 V 0.01 - 10 W 0.02 - 20 Pb 0.005 - 0.4 Sn 0.01 - 0.3 Mg 0.02 - 0.2 As 0.01 - 0.2 Zr 0.02 - 0.2 Bi 0.01 - 0.04 Ca 0.01 - 0.02 Ce 0.01 - 0.5 Sb 0.02 - 0.2 Te 0.01 - 0.05 Se 0.02 - 0.3 Ta 0.02 - 0.7 Zn 0.01 - 0.04 La 0.01 - 0.2

Aluminum-base

Si 0.01 - 20 Fe 0.01 - 12 Cu 0.01 - 10 Mn 0.01 - 0.9 Mg 0.10 - 12 Cr 0.01 - 0.5 Ni 0.01 - 2.8 Zn 0.01-12 Ti 0.01 - 0.3 Ag 0.01 - 1

Bi 0.005 - 0.1 Ca 0.01 - 0.04 Cd 0.005 - 0.5

Ga 0.01 - 0.1 La 0.01 - 0.05

P 0.01 - 1 Pb 0.01 - 1.5 Sb 0.01 -0.6

Sn 0.01 - 0.1

V 0.01 - 0.1 Zr 0.01 - 0.3

COPPER-BASE

Zn 0.01 - 45 Pb 0.01 - 17 Sn 0.01 - 14.8 P 0.01-1 Mn 0.01 - 5.5 Ni 0.01 - 34 Si 0.01 - 6.1 Mg 0.01 - 0.18 Cr 0.01 - 2.4 Te 0.01 - 0.15 As 0.01 - 0.4 Sb 0.01 - 1.7 Bi 0.01 - 5.0 Ag 0.01 - 1.6 Co 0.01 - 2.4 Al 0.01 - 12.0 S 0.01 - 0.20

Ni-Fe-Co high temperature alloys

Si 0.01 - 4.0 (relevant to nickel alloys with high W) Mn 0.01 - 10 P 0.01 - 0.9 S 0.01 - 0.3 (relevant to nickel alloys with high Mo) Cr 0.01 - 36 Fe 0.01 - 100 Mo 0.01 - 34

V 0.01 - 3 Cu 0.01 - 41

W 0.01 - 13 Co 0.01-100 Nb 0.01 - 6 Al 0.01 - 6 Ti 0.01 - 6 Zr 0.01 - 0.3

Ta 0.01 - 12.0 (holds for alloys with high Hf, Re, and W) Hf 0.01 - 2.0 (holds for alloys with high Ta, W, and Re) Re 0.01 - 5 (holds for alloys with high Ta, W, and Hf) Y 0.01 - 5 (resolution is sufficient to resolve Y-K lines from Ni-Alloy sum peaks)

Pt 0.01 - 0.5

Titanium-base

Al 0.02 - 8 Sn 0.01 - 11 Zr 0.01 - 6 Mo 0.01 - 16 V 0.01 - 5.6 Si 0.01 - 1 Mn 0.02 - 7 Cr 0.01 - 4 Ni 0.01 - 0.6 Fe 0.01 - 3 Cu 0.02 - 2.5 Nb 0.01 - 7 Pd 0.01 - 0.2 Y 0.01 - 0.05 Ta 0.01 - 0.2 Ru 0.01 - 0.2

Pb-base Sn 0.01 - 64.4 Ag 0.01 - 3.4 Sb 0.01 - 17 Bi 0.01 - 54 Cd 0.005 - 0.5 Al 0.01 - 0.1 As 0.03 - 1.5 Au 0.01 - 0.3 Ca 0.01 - 0.16 Cu 0.01 - 0.6 Fe 0.01 - 0.03 In 0.01 - 0.3

Ni 0.01 - 0.02 P 0.01 - 0.02 S 0.01 - 0.03 Se 0.01 - 0.03

Te 0.01 - 0.09 Zn 0.01 - 0.06 Pd 0.01 - 0.008

Sn-base

Pb 0.01 – 61 Bi 0.01 – 60 Sb 0.01 – 9.7 Cu 0.01 - 9 Zn 0.01 - 9.9 Ag 0.01 - 9 Al 0.01 - 0.1 As 0.01 - 0.6 Au 0.01 - 0.25 Cd 0.005 - 0.14 Co 0.01 - 0.022 Fe 0.01 - 0.1 Ge 0.01 - 0.8 In 0.01 - 0.1 Ni 0.01 - 4 P 0.01 - 0.02 S 0.01 - 0.01 Se 0.01 - 0.07

Zn-base Al 0.02 - 60 Cu 0.01 - 3.5 Pb 0.02 - 3 Sn 0.01 - 2.4 Cd 0.005 - 0.6 Fe 0.01 - 2 Mg 0.02 - 0.1