Rocky Mountain Cooperative Program (RMCP)
Rocky Mountain Cooperative Program - Program Protocol
The purpose and scope of this document is to define certain terminology, procedural techniques, criteria and protocol to be utilized by members of the ongoing "Rocky Mountain Cooperative Program" (RMCP) conducted by Rocky Mountain Reference Materials International as it applies to the development, certification and production of certified reference materials.
The International Standards Organization (ISO) definitions, expressed in ISO Guide 30 lists the following:
- Certifying Body - A technically competent body (organization or firm, public or private) that issues a Reference Material Certificate which provides the information detailed in ISO 17034:2016.
- Reference Material (RM) - Material or substance with one or more properties of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials.
- Certified Reference Material (CRM) - Reference material, accompanied by a certificate, one or more of whose property’s values are certified by a procedure which establishes its traceability to an accurate realization of the unit in which the property values are expressed, and for which each certified value is accompanied by an expanded uncertainty.
Rocky Mountain Cooperative Program Design
ASTM Standard E691 applies to Inter-laboratory studies to "Determine the Precision of a Single Test Method". This standard is also a well thought out and logical plan for conducting an Inter-laboratory program involving multiple techniques. Therefore, the planning, conducting, analyzing, protocol and treatment of data resulting from the RMRMs-RMCP is performed utilizing the guidelines established in ASTM E691 where applicable.
Selection of Participating Laboratories
RMCP membership is totally voluntary and consists of approximately 50% actual producers of the materials being analyzed, 40% technically qualified commercial laboratories and 10% representing general industry and academia. All volunteer cooperative labs are invited to participate on each and every candidate material they are deemed competent to analyze. All cooperative labs evaluate only the materials they agree to.
Materials are typically selected from standard industry stocks so as to emulate material types found in the real-life circumstances dealt with by users in their daily Rocky Mountain endeavors. Whenever possible, program materials are secured in a wrought condition. Other methods of manufacture such as continuous cast, sand or static castings are utilized as a last resort and only in the case of those materials being unavailable in wrought condition.
Since most metals are available in bar stock or rod form, a typical "batch" or "series" is defined as a single length of material or a single bar of one continuous length.
The "batch" samples are taken by dividing the bar into a minimum of twelve sub-sections. A 1¼ inch solid test sample is removed from each sub-section. Each 1¼ inch test sample is further subdivided as follows: The "batch" samples are taken by dividing the bar into a minimum of twelve sub-sections. A 1¼ inch solid test sample is removed from each sub-section. Each 1¼ inch test sample is further subdivided as follows:
- Approximately ~10 % (~⅛ in.) of the total sample is converted to chip form (~25 g) for analysis by classical wet chemistry, ICP, AA, and combustion procedures.
- An additional ~10 % (~⅛ in.) is converted to the form of a solid pin disk for determination of C, S, N2 and O2 by combustion or inert gas fusion procedures.
- The remaining 80 % (~1 in.) of each sample remains in a solid disk form for Optical Emission and X-Ray analysis where applicable.
Each member of the "Rocky Mountain Cooperative Program" receives the three sample types and is therefore responsible for a specific sub-section of the batch bar. All sub-sections and corresponding test samples are sequentially marked with matching and unique internal identification numbers so that if abnormalities occur during the RMCP process, each test sample can be traced to the original sub-section. Due to this extensive sampling procedure, homogeneity of the total batch is therefore reflected as a product of the overall statistics and the resulting certified data.
Specific Within Sample Determination of Homogeneity
All materials are assessed for homogeneity. Specific homogeneity testing is determined by the RMCP program management, and incorporates homogeneity test procedures as outlined in ASTM E826, NBS Handbook 91, "Experimental Statistics", as well as other established practices for determination of practical homogeneity.
Methods of Analysis
The RMCP "Rocky Mountain Cooperative Program" encompasses an extremely wide variety of materials. No single method would provide optimum data results. Therefore, the methods utilized are a combination of methods for classical wet chemistry, ICP, AA, Optical Emission and X-Ray spectrometric methods in addition to combustion/inert gas fusion procedures for the determinations of Carbon, Sulfur, Nitrogen and Oxygen.
Extent of Data Reported
It is the policy of RMCP to report data submitted by two or more labs. However, in accordance with the guidelines established by the RMCP membership protocol, final certification occurs only for those elements in which a minimum of six data points remain after final critique. Therefore, data in parentheses ( ) is not certified but provided for information only. Certified Data that was selected by the RMCP membership for additional testing is indicated by brackets [ ].
Traceability to the SI through an NMI is approached in two distinct ways within the RMRMs\RMCP.
- In the case of some matrix groups, specific SRMs are not always available. In this case, the RMCP program members voluntarily make available to the RMCP a variety of SRMs produced by (NBS\NIST), some of which have been collected over almost two decades. In addition to validating test methods and instrument performance, where possible, these resident SRMs are also used in the instrumental calibration curves for that portion of the RMCP which requires instrumental analysis. Affidavits of the RMCP member labs' SRM inventory and their applications are on file and archived in the RMRMs historical database.
The Rocky Mountain data results for the RMCP developed under this program are therefore "Traceable" to the U.S. Department of Commerce, National Institute of Standards & Technology, (NIST). The specific SRMs applicable to a certification are referenced on the face of the "Certificate of Analyses" for all RMCP certified materials.
Rocky Mountain Proficiency Testing (RMPT)
“Laboratory Performance Evaluations”
Perpetual Monitoring of Instrument Performance
What should one expect from a Proficiency Testing (PT) Program?
A PT program should allow for fast, corrective action in case of problems.
A PT program should be inexpensive, easy to interpret, and comprehensive.
A PT program should provide an assessment of a laboratory's analytical data compared to the true value.
A PT program should provide for a periodic assessment of the performance of a laboratory.
A PT program should satisfy the minimum requirements for laboratory accreditation.
Typical proficiency testing protocol
Typically, PTPs are conducted in a "round-robin" environment and consist of a peer group analyzing unknown materials. More often than not, weeks or months later, data are compiled resulting in a battery of lengthy statistical reports and graphs (often difficult to interpret) detailing how everyone compared to each other. This approach raises a variety of questions. For example, if Total Quality Assurance (TQA) is the objective, how many things can go wrong in your laboratory during the time it takes to get the results back? If the PTP is being used for TQA, what if all participants (the whole peer group) agree, but the result is wrong?
RMPT "Benchmark" Proficiency Testing
The RMPT program is an accredited ISO/IEC 17043 Annex B.2.1 B program. RMPT has access to chemical results on over 250 metal alloys and over 150 aluminum alloys. By using this certified data for comparison, we can offer alloys and compare elements not commonly used in other PT programs and we have eliminated the "round robin” and associated problems. The results still provide a “peer comparison," but the primary benefit is that our clients’ data are compared to the "True Value" because the test samples are actual CRMs. We refer to this as a "Benchmark" comparison, since the test samples are actual CRMs that have been thoroughly examined for homogeneity and statistically characterized during the certification process. Outliers have been identified and eliminated for an unparalleled comparison of our subscribers’ analytical results to the "True Value."
Here’s How the RMPT Program Works
We supply you with a calendar for selecting the date, type of material by matrix group, and sample configuration (i.e., solids, chips, or pins). You can enroll in the program any time you choose. Program pricing is available for monthly, quarterly, or biannual testing. We then send you a “blind” sample from our stock of CRMs based upon your selection. When you have completed the analysis of the blind sample, you send us the results via fax or e-mail. Within 48 hours you will receive your results by fax or e-mail. Your report will include:
- A color-coded "Z-Score Comparison” which compares your results to the actual "Benchmark"
- A color-coded "Z-Score Chart" graphically depicting your data compared to the certified value of the
- A “Certificate of Analysis” confirming which CRM was used as the sample in the
"Color coding" provides you with the instantaneous ability for identifying the problem areas of performance.
Green — indicates data within the acceptable 2 Sigma range above or below the mean.
Yellow — indicates data that have fallen outside the 2 Sigma range but within the 3 Sigma range.
Red — indicates data that have fallen outside the 3 Sigma limit and are possibly out of control.
Note: Your color-coded hard copy will be sent to you by regular mail.
Commitment and Confidentiality
Keep in mind we are a third-party vehicle and a partner in your ongoing quality assurance/quality control (QA/QC) program. The results stay confidential. Our only intention with the RMPT program is to aid our subscribers in determining if "things are the way they should be and if their reported analytical results are good.”
"We Are Part of Your Quality Team”
We DO NOT sit in judgment. We DO NOT certify you to any particular criteria, nor do we certify you to meet any particular industry specifications or regulations. In short, whether you have a single-instrument or a multiple-instrument/multiple- technique environment, the RMPT program affords subscribers a trouble-free QA program that is traceable to NIST and can be easily integrated into the daily laboratory routine.
Please contact us at: RMPT@RMRMs.com for additional information about the program and how to subscribe.
Rocky Mountain Share Program (RMSP)
In that same spirit of cooperation that has become the very foundation of our efforts to develop new CRMs/RMs in the private sector, in September of 2016, the company launched its "Rocky Mountain Share Program." Although many materials are quite common, spectrochemical standards for these materials are essentially non-existent.
The "90/10, 80/20, 70/30" share program is a very simple cost-effective service offered by RMRMs allowing our company to work together with the scientific consumer by sharing the task, as well as the costs of developing new commercial CRMs.
Here's how it works! The customer furnishes RMRMs with the material of the specific alloy, usually in the form of round bar stock. The bar stock should be a minimum of 1¼" in diameter (1½" O.D. is ideal). The overall length should be 10' to 12'. Forms other than bar stock is acceptable as long as the quantity is sufficient for the sampling that is needed for the laboratory examinations. The material is then processed through RMRMs-RMCP for certification as a CRM.
The only cost to the customer is the cost of the material. RMRMs has well-established vendors for most alloy materials and will also assist in location and acquisition. Approximately 30% of the material is expended in the analysis process. After certification, 10% is returned to the customer in any form desired (solids, chips, X-Ray discs, etc.), and RMRMs retains the balance for sale commercially.
That's all there is to it! By working together, we make available one new Traceable CRM or RM for the scientific community.
School - AES, ICP, XRF
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