Statement of Requirements (Revised 8.18.20).pdf

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 1 for Reference Material Development

Statement of Requirements

TITLE: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron for

Requesting Lab/Division/Group: Materials Measurement Laboratory, Chemical Sciences Division, Inorganic Chemical Metrology Group (646.01)

Background The National Institute of Standards & Technology (NIST) requires high-purity iron and ultrahigh-purity iron in rod form suitable for development into certified reference materials for elemental analysis. The materials will be used to develop renewals of Standard Reference Materials (SRMs) 1766 and 1768, which are going out of stock. These SRMs are used by iron and steel labs to calibrate and to validate test methods for analyses of trace level elements in iron.

The materials are needed in sufficient quantities to make supplies for 20 years or more of SRM sales. The materials must be of high homogeneity with low potential for contamination during processing into the rod form. The manufacturing process will include checks for composition before melting and for composition and homogeneity after forging. Rework may be required in the event heterogeneity is too high, the composition has been contaminated, or there are voids evident in the rod form material.

Objective(s) The objective of this procurement is to obtain the materials required to develop SRM 1766a High-Purity Iron (disk form) and SRM 1768a Ultrahigh-Purity Iron (disk form). Sufficient quantities are required to enable production of 20 years or more supply per SRM, based on recent sales of reference materials demand.

Scope/General Requirements The materials needed by NIST require special manufacturing with high-purity iron for one composition and ultrahigh-purity iron for the second composition. It is necessary to have each material vacuum melted, cast and rolled with special expertise and equipment to ensure no substantial changes in the composition and low heterogeneity of each composition at all points of the manufacturing process. This effort is expected to require a significant amount of quantitative elemental analyses for the 21 elements in the composition specifications and testing for voids in the rods.

Tasks/Specific Requirements* NIST has a need for high-purity iron and ultrahigh-purity iron that would meet the specified criteria below. Therefore, there are two primary tasks: 1) delivery of 1,000 kg of rods of high-purity iron and 2) delivery of 225 kg of rods of ultrahigh-purity iron. Each primary task is comprised of three secondary tasks: a) selection of material for composition; b) melting the required quantity, rolling rods, and testing for composition uniformity; c) package and ship rods to NIST.

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 2 for

Task No. Description Instruction

1a Select or create a high-purity iron composition fitting Table 1 of Special Material Requirements on page 3.

Report by email to NIST TPOC the selected material composition based on test results for the chosen lot or lots .**

1b Melt required quantity of iron in a single batch and roll it into rods of specified dimensions. Number the rods in production order. Choose the first rod and every third rod thereafter for testing. Test chosen rods for voids by magnetic particle testing. Slice off 10 cm (4”) of one end of each chosen rod. Then slice one sample from that end of every chosen rod and perform elemental analyses on every sample slice. Perform four replicate analyses of NIST-supplied SRM 1766 in this batch of elemental analyses.

See Special Material Requirement bullet 1 for form and size of rods. Report test results for all chosen rods and the four analyses of SRM 1766 by email to NIST TPOC. Send test sample slices and 10 cm end slices to NIST for inspection.

See Special Material Requirement bullet 3 on Homogeneity and clause on Other Unique Requirements.

1c Package rods as required, and ship to NIST Gaithersburg.

See Special Requirements 3 and 4.

2a Select or create a ultrahigh-purity iron composition fitting Table 2 of Special Material Requirements on page 4.

Report by email to NIST TPOC the selected material composition based on test results for the chosen lot or lots.**

2b Melt required quantity of iron in a single batch and roll it into rods of specified dimensions. Test every rod for voids by magnetic particle testing. Slice off 10 cm (4”) of one end of each rod. Then slice one sample from that end of every rod and perform elemental analyses on every sample slice. Perform four replicate analyses of NIST-supplied SRM 1766 in this batch of elemental analyses.

See Special Material Requirement bullet 1 for form and size of rods. Report test results for all rods and the four analyses of SRM 1766 by email to NIST TPOC. Send test sample slices and 10 cm end sections to NIST for inspection. See Special Material Requirement bullet 3 on Homogeneity and clause on Other Unique Requirements.

2c Package rods as required, and ship to NIST Gaithersburg.

See Special Material Requirement bullets 3 and 4.

*See Period of Performance on page 6.

**Report existing results for lot or lots chosen in 1a and 2a. If multiple lots will be combined to obtain sufficient weight, report compositions of individual lots.

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 3 for

Special Material Requirements The following material requirements apply to the tasks previously enumerated.

1. Production Size and Unit Dimensions:

The requirement is to produce two different materials – one high-purity iron composition and one ultrahigh-purity iron composition. Each material will consist of a set of rods each having a diameter of 3.5 centimeters and lengths of 2.1 meters to 4.5 meters, with all rods being about the same length.

a. The production run of the high-purity iron material will provide a minimum total produced weight of 1000 kilograms (2200 lbs.), melted and rolled to rod form in a single batch.

b. The production run of the ultrahigh-purity iron material will provide a total produced weight of that material of 225 kilograms (495 lbs.), melted and rolled to rod form in a single batch.

2. Elemental Compositions:

a. High-Purity Iron – The high-purity iron material shall be similar in elemental composition to SRM 1766 Low Alloy Steel (disk form). The certificate of analysis for SRM 1766 is included by reference and may be downloaded from https://wwws.nist.gov/srmors/view_cert.cfm?srm=1766. Note, by current industry standards, SRM 1766 is actually high-purity iron rather than low alloy steel. By similar in composition, it is meant the material must contain the elements listed in Table 1 within the ranges given in the table. The contractor shall calculate the mean of the test results for the chosen rods, and the mean value shall be used for comparison to the table ranges.

Where the listed element is an element that is not allowed to be handled in the foundry, the natural tramp amount of the element found in the manufactured material will be acceptable. The respondent shall provide a list of such elements. Any elements other than those in Table 1, known by the producer to be present, shall be of low mass fractions similar to the ranges given in Table 1.

Table 1. Target Composition Ranges by Element for High-Purity Iron

High-Purity Iron

Target Range Target Range Target Range

Low High Low High Low High

Al 0.005 0.010 P 0.001 0.005 Si 0.005 0.020

Sb 0.0005 0.002 Mn 0.035 0.100 S 0.001 0.004

As 0.002 0.006 Mo 0.0015 0.006 Sn 0.0005 0.002

B 0.0001 0.0005 Ni 0.005 0.030 Ti 0.0002 0.002

C 0.008 0.030 Nb 0.002 0.010 W 0.0005 0.002

Cr 0.010 0.040 N 0.001 0.005 V 0.004 0.020

Co 0.001 0.004 O No requirement

Cu 0.008 0.030 Pb 0.001 0.004

b. Ultrahigh-Purity Iron – The ultrahigh-purity iron material shall be similar in elemental composition to SRM 1768 High-Purity Iron (disk form). The certificate of analysis for https://www-s.nist.gov/srmors/view_cert.cfm?srm=1766 https://www-s.nist.gov/srmors/view_cert.cfm?srm=1766 https://www-s.nist.gov/srmors/view_cert.cfm?srm=1766

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 4 for

SRM 1768 is included by reference and may be downloaded from https://wwws.nist.gov/srmors/view_cert.cfm?srm=1768. Note, by current industry standards, SRM 1768 is actually ultrahigh-purity iron rather than high-purity iron. By similar in composition, it is meant that the material must contain the elements listed in Table 2 within the ranges given in the table. The contractor shall calculate the mean of the test results for all rods, and the mean value shall be used for comparison to the table ranges. Where the listed element is an element that is not allowed to be handled in the foundry, the natural tramp amount of the element found in the manufactured material will be acceptable. The respondent shall provide a list of such elements. Any elements other than those in Table 2, known by the producer to be present, shall be of low mass fractions similar to the ranges given in Table 2.

Table 2. Target Composition Ranges by Element for Ultrahigh-Purity Iron

Ultrahigh-Purity Iron

Target Range Target Range Target Range

Low High Low High Low High

Al < 0.003 P < 0.0015 Si < 0.001

Sb < 0.0005 Mn < 0.002 S < 0.0015

As < 0.0005 Mo < 0.0005 Sn < 0.0005

B < 0.0005 Ni < 0.002 Ti < 0.001

C < 0.002 Nb < 0.0005 W < 0.0005

Cr < 0.0005 N < 0.003 V < 0.0005

Co < 0.003 O No requirement

Cu < 0.001 Pb < 0.002

3. Homogeneity of Compositions:

The sought materials are intended for development into NIST SRMs. Therefore, homogeneity throughout the production run is of high priority. The contractor (or subcontractor) must have test capabilities or access to test facilities, as they are required to test the materials after processing to rods to demonstrate the composition meets NIST requirements. As shown in Task Nos. 1c and 2c, the contractor must test samples from designated, individual rods. The mean test results calculated from individual rod results for all listed elements must fall within the ranges of values listed in Table 1 for the high-purity iron and in Table 2 for the ultrahigh-purity iron.

There must be no significant composition change for an individual rod from the population of tested rods (See Special Requirement 4 on rod numbering). This second requirement is intended to identify any significant contamination to the materials or segregation of an element during melting and rolling. By significant, it is meant the highest or lowest test result of a set must not be determined to be an outlier when applying the Dixon criteria for a single outlier at the 1 % significance level as given in ASTM Standard Practice E178-16a, section 7.2.

This significance test was chosen because it does not rely on calculation of the standard deviation of a data set. The 1 % significance level is the most conservative option available in E178.

https://www-s.nist.gov/srmors/view_cert.cfm?srm=1768 https://www-s.nist.gov/srmors/view_cert.cfm?srm=1768 https://www-s.nist.gov/srmors/view_cert.cfm?srm=1768

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 5 for

A third requirement for homogeneity of both compositions is the absence of voids within the rod form material. The absence of voids in the material will be considered to be demonstrated by the absence of voids in the tested rods of each composition used for the above elemental analyses along with the absence of pits greater than 0.5 cm (0.2”) deep in the surfaces of the produced rods. The test sample slices and 10 cm end sections will be shipped to NIST for inspection, and the rods shall be inspected for pits by the contractor (or subcontractor).

Samples for elemental analysis will consist of one slice (thickness minimum 1.2 cm (0.5“)/maximum 3.8 cm (1.5“)) taken from one end of every chosen rod for the high-purity iron and for every rod of the ultrahigh-purity iron, after removal of the first 10 cm (4”) from that end of the rod.

NIST will review the contractor test results and inspect the submitted samples and rod ends for each batch of rods and, within five (5) business days after receipt of test results and samples from the contractor, will declare the batch acceptable or not on the basis of the above composition/homogeneity requirements.

It is recognized that a batch of rods may not entirely meet the requirements. Depending on the extent of the deficiency, NIST may choose to 1) accept a partial batch, 2) loosen composition requirements, or 3) request rework, at the expense of the contractor to create a new batch of rods. Acceptance of a partial batch or loosening of composition requirements would be accompanied by consideration for incomplete delivery.

4. Packaging:

The produced rods shall be numbered at the place and time of their manufacture. The number shall be marked on or into the rod ends in such a manner as to be preserved during shipping and subsequent handling. If possible, the order of numbering shall match the rod production order. Numbering in order of production would aid in identification of composition trends or possible contamination of a batch. The rods shall be packaged for shipment in wood crates or boxes such that each box contains six to eight rods. NIST storage facilities are set up for long term storage of metal rods in boxes having inside dimensions of

15.2 cm (6 in) wide and 8.9 cm ( 3.5 in) deep and overall length up to 4.6 m (15 ft).

5. Shipping:

Test samples shall be shipped by overnight carrier to NIST Gaithersburg, MD, to the attention of the TPOC. Test results shall be sent to TPOC by email.

After acceptance of test results and inspection of samples and end sections by NIST, finished rods shall be shipped to NIST Gaithersburg, MD by ground freight carrier to the attention of the NIST Office of Reference Materials, Building 203, Attention: M. Cronise.

Other Unique Requirements Because the contractor will perform elemental analyses on which basis NIST will decide to reject or to accept materials, it is in the interests of both parties to include a quality assurance material

Statement of Requirements: Manufacture of High-Purity Iron and Ultrahigh-Purity Iron 6 for during each batch of analyses. Every time the contractor performs a batch of elemental analyses of the rods produced under these requirements, they shall measure four replicate samples of SRM 1766. NIST will provide two disks of SRM 1766 to the contractor for this purpose. The test results from SRM 1766 shall be reported by the contractor to the NIST TPOC. In its review of the test results, NIST will consider the results for SRM 1766 as being an indicator of the extent of bias in the contractor test results and of repeatability of its elemental analysis methods, within the limitations of each method at the mass fraction levels encountered. Data on statistical process control helps eliminate issues where the test method drifts over time or suddenly goes out of control rendering new test results incompatible with older test results. NIST will compare the range of the mean of the contractor results per test method per element plus or minus two times the standard deviation of those replicate results to the certified value plus or minus two times the estimated uncertainty published in the Certificate of Analysis. If there is any amount of overlap of the two ranges, the contractor’s mean result will be deemed to be unbiased. If there is no overlap and a bias is detected, it will be taken into account as a correction to the contractor’s mean result for that element for comparison to Table 1 or Table 2, as appropriate. Elements with no certified value for SRM 1766 will not be subject to this evaluation, and the values for standard deviation of the mean in the Certificate shall not apply.

Place of Performance The manufacture of materials shall be done at the contractor’s (or subcontractor's) facilities, using highly specialized equipment. Elemental analysis of representative samples for elemental composition and inspection of rods for surface pits shall be the responsibility of the contractor.

Period of Performance NIST requires delivery of both final products within a period of 200 calendar days from award of contract. However, due to current access restrictions, performance shall not take place until the contractor coordinates with the designated Technical Point of Contact (TPOC) and Contracting Officer (CO). Prior to commencement of performance, the Contractor must ensure NIST’s campus is open and performance can occur. If access restriction to the campus impacts the period of performance, a modification may be executed by the CO to establish a revised PoP.

Government-Furnished Material NIST will provide the contractor with two disks of Standard Reference Material 1766 for the purpose of making quality assurance measurements during elemental analyses of produced materials. The samples of SRM 1766 are for testing only and have no monetary value to the government.