SOW_16RQ1059.pdf

Request for Quotation Number SB1341-16-RQ-1059

Statement of Work

BACKGROUND

The National Institute of Standards and Technology (NIST) has produced several high-purity ( 99.95%) reference materials (SRMs 84L, 136f, 350c, 351, 723e and RM 8040) that the chemical industry uses as primary standards.

NIST requires 1 kg of high purity meta-cresol purple sodium salt (specified as > 99.8 %) for a new Reference Material (RM). The intention is to bottle the meta-cresol purple sodium salt as a NIST Reference Material. Obtaining a free-flowing crystalline material with excellent homogeneity and primary standard grade purity are important considerations.

GENERAL INFORMATION

1. The Contractor shall produce or obtain bulk primary standard grade meta-cresol purple sodium salt, Chemical Abstract Service (CAS) Number 6265-31-4, from a single lot, that meets a purity specification of >99.8%. The total amount required to be delivered is 1kg.

2. Past studies, on smaller scales, have demonstrated the use of flash chromatography to purify indicator grade meta-cresol purple sodium salt from a >90% purity up to a purity of 99.9%. For this acquisition, the Contractor may use a similar secondary purification such as the method developed by Patsavas, Byrne, and Liu (Marine

Chemistry, 2013, 150, 19-24). A substitute method, which achieves similar quality is acceptable. The substitute method must also involve an optimized synthesis of meta-cresol purple sodium salt.

3. Identity and purity of the product shall be tested as follows:

a. CLARITY OF SOLUTION. Dissolve 0.1 g of the salt in 100 mL of water. Not more than a faint trace of turbidity or insoluble matter must remain. Reserve the solution for the tests for visual assessment.

b. VISUAL ASSESSMENT IN ACID AND ALKALINE RANGE. Prepare two separate solutions of 1 g of potassium chloride in 100 mL of water. For the acid range, adjust the pH of one solution to 6.7 (using a pH meter described in ACS Reagent Chemicals

[ninth edition (2000), or later]) with 0.01 N hydrochloric acid or sodium hydroxide. Add 0.1 – 0.3 mL of the 0.1 % solution reserved from the test for clarity solution. The color of the solution shall be yellow. For the alkaline range, adjust the pH of the second potassium chloride solution to 8.1. Add 0.1 –

0.3 mL of the 0.1 % solution reserved from the test for clarity solution. The color of the solution shall be purple.

c.ORGANIC PURITY. Assess organic purity with high performance liquid chromatography (HPLC) on a C18 or C18-Aqueous column to fully resolve and quantify impurity peaks using the following method:

Solvent A: 95% 5mM ammonium formate (adjusted to pH 3.5) with 5% methanol

Solvent B: 5% 5mM ammonium formate (adjusted to pH 3.5) with 95% methanol

Linear Gradient:

Time (min) % Solvent B

0 0

1 0

35 100

40 100

Column temperature: ambient

Detection wavelength: 254 nm, 434 nm, 578 nm

4. The Contractor shall provide a crystalline, free-flowing meta-cresol purple sodium salt material, with a notable absence of lumps or foreign material. The product must be packaged in a single (one) container which provides protection from light such as high-density polyethylene or amber glass with the meta-cresol purple sodium salt material securely contained. Container shall not contain separately packaged sub-containers.

TASKS

1. Not later than 30 days after award, the Contractor shall provide a 10 g candidate batch of material and documentation which summarizes the results of the visual assessment in 2B and HPLC chromatographic data as outlined in paragraph 3(c) of the

General Award Information. This documentation must show that the purity specification of >99.8 % has been met.

The Contractor shall provide the value for the purity of the material, test results of the material including all tests listed in paragraph 3 of the General

Requirements, and a written statement confirming that the test were performed in accordance with paragraph 3 of the General Requirements.

The Contractor shall package the material and report its net mass (not including packaging) that will be shipped to NIST.

NIST will assess the purity by UV spectrophotometry, LC-MS, and NMR. NIST will provide the screening results to the Contractor. If the lot meets all required specifications. NIST will also review the Contractor’s reported results of the assay and tests. Within four business days of receipt of the Contractor’s results, NIST will notify the Contractor whether or not the results are acceptable based on the specifications listed in paragraph 3 of the General Information.

If NIST determines that the batch does not meet all required specifications, written notification will be provided and the Contractor must revise their purification methods accordingly, and re-purify a second 10-gram batch of meta-cresol purple sodium salt.

The Contractor shall have a total of 90 days and three (3) total attempts to provide a candidate batch which meets the purity specification of >99.8%. If none of the candidate batches meet all required specifications, the contract will end and no payment shall be made to the Contractor for any of the work completed.

2. Upon delivery of a successful lot of 10g candidate material, NIST shall provide written authorization for the Contractor to proceed to produce the 1 kg of material. The Contractor shall not proceed to produce the 1kg of material until written approval of the 10g material is provided by NIST. Upon receipt of written approval, the Contractor may also invoice for the 10g candidate material.

The 1kg of material shall be delivered not later than 12 weeks after the Contractor receives the written authorization to produce the 1kg of material.

All reports and documentation that were provided with the 10g of material shall be delivered with the 1kg of material.

NIST will assess the purity of the 1kg batch by UV spectrophotometry, LC-MS, and

NMR. NIST will provide the screening results to the Contractor. If the lot meets all required specifications. NIST will also review the Contractor’s reported results of the assay and tests. Within four business days of receipt of the

Contractor’s results, NIST will notify the Contractor whether or not the results are acceptable based on the specifications listed in paragraph 3 of the General

Information.

If the 1kg batch does not meet required specifications, the Contractor shall take the steps necessary to provide a 1kg batch that meets all required specifications.

The NIST Technical Point of Contact (TPOC) and Contracting Officer (CO) shall work with the Contractor to modify the contract accordingly.

DELIVERABLES

1. 10g candidate batch of material and supporting documentation

Due Date: Not later than 90 days after award

Due Date: Not later than seven months after award

2. 1kg candidate batch of material and supporting documentation

PERIOD OF PERFORMANCE

The period of performance shall be seven months from the date of award.

PLACE OF PERFORMANCE

The place of performance shall be the Contractor’s facility.

ACCEPTANCE CRITERIA

NIST will inspect the container of meta-cresol purple sodium salt material upon its arrival at NIST. The container will be inspected to assess integrity.

Acceptance of the material also will be based on the results of the assay for purity meeting specifications (purity > 99.8 %); and the results of the specification tests listed in the General Requirements, paragraph 3.