Measurement Techniques. Vol. 42. No. 1l. 1999 Here we present the next series of articles derived from the 6th Ural Meo'ology Conference. which was held in November 1998 in Ekaterinburg. The articles deal with various aspects of the State Reference Materials Service for the compositions and properties of substances and materials. The earlier parts of the selection were published in this journal in Nos. 8 and 10 for 1999. NEW REGULATIONS

CONCERNING THE ISSUE

AND USE OF REFERENCE

MATERIALS I

UDC 389.1:006.354:543

N. G. Semenko

Information is given on newly adopted official documents regulating the development, acceptance, and use of reference materials (RM) together with metrological checks on their issue and ~tse. Various aspects of these official documents are considered, which relate to the licensing of their mant~'acture, the process for generating the technical doctmwnts for reference materials, alld details of their acceptance. This set of official documents covers virtually all the basic" requirements in the issue and use of RMs.

In 1998, regulatory documents (RD) were adopted concerned with new specifications tbr the development, issue, and use o f reference materials (RM), which included one standard [ 1], metrological rules [2], and several metrological recommendations. The basic standard [1] was adopted as a CIS intergovernmental standard in 1997 and was brought into effect from July 1, 1998, by a decree of the Russian State Standard Commission to act as a state standard for the Russian Federation. The originator of the standard was the Ural Metrology Research Institute, which was designated by the head body, the State Service for Reference Materials (SSRM), also in 1998. The new version of the document differs from the previous standard in introducing some new concepts, which are briefly considered below. The terminological section of the standard contains about 30 concepts and definitions of them, including the basic generic concepts of reference material, reference material category, and type of reference material; other terms given and defined are metrological certification of RM, RM certification program, and RM certification methods. The predominant viewpoint taken in drafting and revising the terminology and the other aspects of the standard has been as follows: 1) RM are means of measurement (MM) that are used in the metrological checking of means and methods of pertbrming measurements, usually ones employed as standards (standard MM): 2) RM should be issued and supplied as scientific products with clearly identified features (type, batch, and specimen), and should not be treated as temporary or epistxlically used substances: and 3) the general technical rules and procedures tbr the acceptance, issue, and use of RM should be as close as possible to those used with other MM. That approach means that these regulations more clearly define the aspects that reflect the specific features of RM relative to other MM and thus extend the general concepts of documents in the state measurement system in application to RM. In [ 1], there are lbur categories of RM, of which three are familiar fr~')m previous practice (state RM known as SRM, branch ones (BRM), and local ones (LRM)), together with the additional category of international RM (IRM). The last categoI Partial use has been made of data from other papers given at the conference by I. P. Nosova, D. P. Nalobin, Z. N. Babushkina, and G. G. Troinina in collaboration with the author. Translated from Izmeritel'naya Tcktmika, No. 11, pp. 59---61, November, 1999. 1090

0543-1972/99/4211-1090522.00 9 1999 Kluwer Academic/Plenum Publishers

ry has been adopted in accordance with a convention [3] and includes RM permitted lbr free use in the CIS countries alter their acceptance in the appropriate sequence by the authorities there. The issue of RM in accordance with the standard can be based in the form of a single production batch, repeating batches, or short-series production. Reference materials in all categories are permitted tbr use in accordance with their purpose only after their acceptance by competent authorities, which are dealt with later on. This applies equally to RM made abroad, whose unchecked use is not allowed by the standard. For RM in any category, it is necessary to establish the metrological characteristics (certified values lbr the RM and the error levels of them), which are given in the RM documentation. The standard deals with the methods of standardizing the metrological characteristics and the forms of representation used for them. The general procedure tbr developing an RM covers the usual stages for developing a new product and envisages that not only will the RM be manufactured but also that technical documentation will be formulated, which should include the following obligatory features: the technical specification for developing the RM and the programs and methods of primary RM certification forming part of it, together with the description of the type of RM, the RM certificate (with instructions for using the RM), and labels for the RM samples. The general specifications for the content and form of these documents are also given in the standard. Documents such as the description of the RM type and the RM certificate are introduced instead of the previously formulated certificates for the RM and differ from them in content and ibrm. These documents readily incorporate closely similar specifications for the documentation tbr MM and RM, and this has been supported by many comments received from organizations concerned with the draft for the standard. The program and methods tbr the primary certification of the RM specify content, volume, and thcilities used for the experimental examination of the RM and in accordance with the standard are subject to obligatory metrological evaluation, while on the whole, the technical documentation tbr the type of RM should be subject to checks at the stage preceding the confirmation of the RM. A positive conclusion from that evaluation and check on the documentation for the RM is a basis Ibr confirming it by a competent body that has been assigned the necessary powers. In accordance with the standard, the corresponding RM categories are confirmed by the following: by the Intergovemmental Council on Standardization, Metrology, and Certification for the CIS for IRM, the Russian State Standard Commission for SRM, competent bodies at branch level for BRM, and directors of organizations for LRM. That list does not mention explicitly industrial branch level bodies having the right to accept BRM because the definition of those bodies requires additional organizational decisions t. Confirmation of the type of SRM is indicated by the issue by the developing o~anization of a certificate conl~rning the type of SRM, whose period of validity it is recommended should be usually established as five years. After the lapse of that time, the certificate can be extended if it is still possible and necessary to continue the issue of the SRM of the corresponding type. Also, types of SRM tbr which certificates are issued are entered into the state register of confirmed types of SRM, which is maintained by the Ural Metrology Research Institute in accordance with the metrological rules [4]. The state register is accompanied by an archive of technical documentation for the confirmed types of SRM. It is not permitted to use this documentation or to distribute the information contained in it without the agreement of the designers of the RM. As regards the formulation of documentation lbr BRM and LRM, the standard does not directly regulate the procedures lbr confirming and recording them. Decisions on these topics are delegated to industry-branch bodies, with recommendation that they should set up a procedure not conflicting with the general concepts in the standard relating to that SRM category. RM are used in accordance with the requirements of the RD tor methods of checking or calibrating MM and on the basis of the sections in the technical documentation and RD dealing with methods of monitoring, testing, and using them in accordance with the instructions on the use of the RM, which as a rule are part of the RM certificate. The areas of application tbr the various categories of RM differ in accordance with the spheres covered by the powers of the bodies that confirm the corresponding RM categories. I In accordance with the general structure of the country's metrological service, the role of such bodies should be assigned to subdivisions of the central bodies in federal management agencies responsible tbr metrological support to the corresponding branches. 1091

For example, IRM can be used in all branches of the Russian economy (including spheres covered by state metrological monitoring and supervision) if no limitations have been imposed during their adoption. SRM can also be used freely in all branches of the economy and in all lbrms of metrological operation. The sphere of application for a BRM is restricted to that branch of industry and to the forms of metrological operation covered by the powers of the body that confirmed the BRM. Correspondingly, the sphere of use for an LRM is restricted to the organization in which it was confirmed. It can be permitted to distribute BRM and LRM outside the areas of activity of the organizations that have confirmed such RM on decision by the corresponding interested organization as suitably formulated. It is not permitted to use BRM and LRM in spheres to which the state metrological supervision service applies. Metrological monitoring and supervision apply to the issue and use of RM as a variety of MM, and this is provided either by parts of the state metrological service SMS or by the metrological services of legal persons and state management offices. The standard envisages in particular the following detailed forms of operation during metrological monitoring: 1) licensing the issue and sale of SRM of continued types (including inspection monitoring accompanying licencing); 2) accrediting metrological services with the right to evaluate documentation for BRM and LRM presented for conllrmation: and 3) metrological supervision of the issue, state, and use of RM in metrological operations. The metrological rules [2] regulate the procedure for licensing operations in making and selling RM. According to this, the licensing of legal persons with the right to make and sell RM is provided by SMS bodies in the area where the licensee is established. The general procedure for licensing activities concerned with RM does not have any essential differences from that in licensing for MM [3], so [2] reflects mainly features due to the specific aspects of issuing RM, which, according to the document, is done in the form of short-series or individually repeated batches of production, where there is differentiation over the issue of the RM: by the developer in accordance with his own technical documentation, by the nmnufacture in accordance with the documentation of the developer (another legal person), or by the manufacturer in accordance with his own technical documentation for the type of SRM, which has previously been entered into the state register. The licensing procedure differs somewhat for the various forms of RM production, which is reflected in [2]. As regards licensing the fight to sell RM, it has no substantial differences from licensing the right to sell MM, with the exception that the list of requirements imposed on the licensee excludes demonstrating the practical use of the RM, since that has no practical significance. The specific feature of licensing RM issue from repeating batch production occurs because the issue of the RM is usually cyclic, as batches of the RM are issued periodically with intervals lbr example of 0.5--2 years or sometimes more. Correspondingly, the production or technological cycle in producing a batch of RM occupies only a small part of the time interval between the issues of RM batches, so there are long gaps in the operation, during which it is not necessary to keep the equipment and MM in a state of constant readiness (this is one of the obligatory conditions in licensing the issue of MM). For that reason, the periodicity in inspecting licensees should match the rhythm of issuing RM batches in order that the inspection should apply to the production cycle in the issue of each successive batch of RM or each second or third one in accordance with the operating cycle. For the same reason, [2] contains the statement that recommendations are made to SMS bodies on the periodicity of the inspection of licensees when the type of SRM is confirmed. Also, the papers from certifying repeated batches of RM are subject to additional metrological evaluation on the basis of the inspection at the head body of the State Service for Reference Materials, primarily when statistical results are presented from interlaboratory certification. There is a further circumstance on the issue of SRM by the manufacturer in accordance with his own documentation, provided that the technical and metrotogical characteristics coincide with those of the previously confirmed types of SRM. Such situations are particularly c o m m o n for numerous ranges of RM for the compositions of various solutions containing ions or salts of harmful or toxic substances. If the metrological evaluation of the documentation lbr such RM (in the head body of the State Service) shows that the confirmed types of SRM contain an analog, then the issue of such RM is based on a license without recording the new type of SRM. A license for the fight to make such SRM is formulated by the SMS body on recommendation from the head body of the State Service tbr Reference Materials. 1092

As regards the accreditation of metrological services with the right to perform metrological evaluation of RM documentation, the general procedure here is reflected in the [6] metrological rules, and in particular in sections 1.2, 1.3, 4.2.2, and SO Oil.

Here it must be emphasized that we are dealing with metrologicat services or other parts of organizations officially charged with the metrological evaluation and monitoring of documentation for BRM and LRM, as well as with the preparation of expert evaluations on the confirmation of the corresponding RM categories. Unfortunately, this circumstance is not set out clearly in [6], which has already led to misunderstandings, in particular because people have not always met the requirements of the document concerning the participation in the accreditation by a representative of the head body in the State Reference Materials Services (sections 1.2 and 4.2.2). This is all the more necessary because that head body has formulated certain obligatory specifications for completing the form for the accreditation area, but these are not reflected in the rules. Metrological supervision of the issue and use of RM is at present provided within the framework of the general supervisory functions realized by the SMS and also by the metrological services of legal pe~ons, and consequently the supervision is not always effective. One reason for this has been the long delay in revising the basic document [7], for which a new version containing recommendations on the supervision of RM was prepared more than a year ago. There are reasons t'or supposing that the performance of the state metrological supervision will be improved considerably when the new version of these rules is introduced.

REFERENCES 1.

2.

GOST 8.315-97: The State System of Measurements: R~ference Materials for the Composition and Properties of Substances and Materials: Basic Concepts [in Russian]. PR 50.2.021-98: The State System of Measurements: Procedurefor Licensing the Manufacture and Sale of State Reference Materials [in Russian].

3.

"Convention and collaboration on the creation and use of reference materials for the composition and properties of substances and materials (adopted in Tashkent, 1992)," Standarty i Kachestvo, No. 1 (1993).

4.

PR 50.2.020-96: The State System of Measurements: Procedurefor Operating the State Register of Confirmed Types of Reference Materials [in Russian]. PR 50.2.005-97: The State System of Measurements: Procedurefor Licensing Activities in the Manufacture, Repair. Sale. and Disposal of Means of Measurement [in Russian]. PR 50.2.013-97: The State System of Measurements: Procedurefor Accrediting the Metrotogical Services of Legal Persons with the Right to Certify Means of Making Measurements and Conducting the Metrological Evaluation of Documents [in Russian]. PR 50.2.009-94: The State System of Measurements: ProcedureJbr Performing State Metrological Supervision on the Issue. State. and Use of Means of Measurement. Certified Methods of Making Measurements. Standards, and Obedience to Metrological Rules and Regulations.

5. 6.

7.

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