The Institute for Certified Reference Materials (ICRM) is going to celebrate the 55^th anniversary in March 2018. The results of the ICRM activities in development and production of the certified reference materials (CRM) of raw materials and materials of metallurgical production over the past five years are considered. The nomenclature of the CRM produced by the ICRM includes raw materials (ores and concentrates, ferroalloys and ligatures, fluxes, refractories), metals (cast iron, steel, nickel-base alloys) and waste of metallurgical production (slags and metallurgical fly ashes). To approve the competence, the ICRM has been accredited as a producer of reference materials (RMP) in accordance with the requirements of the International Standard ISO Guide 34:2009 (ISO Guide 34). Testing analytical center of the ICRM (TC) applies both classical methods of chemical analysis (methods of «wet chemistry») and modern physicochemical and physical methods. TC is accredited in accordance with GOST ISO/IEC 17025 – 2009 in the National accreditation system. The competence of Testing Centre has been repeatedly approved by the results of inter-laboratory comparative tests for certification of reference materials produced abroad including those from the European Union (ECRM). The inter-laboratory tests (proficiency tests — PT) are performed by the Provider, ICRM accredited in the National Accreditation System for compliance with the requirements of GOST ISO/IEC 17043:2013. We consider and analyze contradictions in the statutory regulation and resulting difficulties encountered in the activities of producers of reference materials in Russia. The approval of reference materials to be used in the state system for ensuring the uniformity of measurements is possible only on the basis of positive test results. This procedure (RM testing for type approval purposes) has no analogues in the world practice. In accordance with the Russian legislation, the ICRM has got accreditation to perform RM testing for the type approval purposes in 2015. In 2013 – 2017 the Institute developed and certified 7 CRM sets of steel and 3 CRM sets of cast iron for spectral analysis (solids), and 46 CRM for chemical analysis (in dispersed form), including carbon and alloyed steel, cast iron, ferroalloys, ore and concentrates, metallurgical slags.

The experience of JSC «The Institute for Certified Reference Materials» (JSC «ICRM») in organizing and conducting inter-laboratory comparative tests (ICT) is considered. ICT are conducted to determine the values of certified characteristics of standard samples and examine the qualifications of the laboratories. Data on ICT carried out by JSC ISO in 2012 – 2017, as well as information on the ICT program for 2018 are presented. Some issues emerged upon accreditation of the JSC «ICRM» as a provider of inter-laboratory comparative tests are considered.

The results of estimating the accuracy of spectral analysis of steel according to inter-laboratory comparative tests (ICT) conducted by JSC «ISO» to attest standard samples and examine qualification of the laboratories are considered. Data on the consistency of the results of spectral analysis and data of chemical methods and their comparison with analogous data of ICT of foreign standard samples are also presented.

A number of new sets of certified reference materials were produced by the Institute for Certified Reference Materials (ICRM) for spectral analysis of stainless steels and iron-nickel alloys (LG70 – LG75 and LG76 – ISO LG82) and non-alloyed and low-alloyed steels (UG0l – ISO UG9l). These sets of certified reference materials may be used for calibration and accuracy control in x-ray fluorescence and atomic-emission spectrometry. An experiment was carried out to study the consistency of the data obtained with the new sets and those previously released by ICRM and foreign manufacturers of certified reference materials.

A new set of certified reference materials (CRM) of alloyed cast irons CHG50 – ICRM CHG55 has been developed in 2017 at the Institute for Certified Reference Materials. Novel technology thus used provided optimal use of the CRM volume. Special experiment was carried out to evaluate the contribution of heterogeneity to the total uncertainty of CRM. Study of the compatibility of the certified characteristics of the new set with the values of previously released cast irons sets revealed the possibility of using cast iron set CHG50 – CHG55 in x-ray fluorescence and atomic emission spectrometers.

To ensure the traceability of measurements upon determination of carbon, sulfur, nitrogen and oxygen in steels sodium carbonate, sodium sulfate and potassium nitrate, respectively, are used for calibration of automatic analyzers. This approach places the methods of combustion and reductive fusion in the flow of inert gas on a par with the traditional classical chemical methods of determination which include the procedure of calibration by the substance of constant stoichiometric composition. We present the results of participation of the Test Analytical Center of the «Institute for Certified Reference Materials» in the inter-laboratory experiments on analysis of gas-forming elements in standard samples of steels and cast iron EURONORM-CRM.

Reference materials of the branches (RMB) and in house reference materials (IRM) of the materials of metallurgical production are widely used out of the scope of the state control of ensuring the uniformity of measurements. The latter represent the most numerous group of reference materials. We discuss the schemes of certification of RM which ensure the traceability of their certified values.

Potentialities of the method of inductively coupled plasma-atomic emission spectrometry (ICP- AES) in determination of the low content (0.001 – 0.01%) of aluminum in steels are studied. Analytical lines of aluminum and optimum operating parameters of Al determination are specified along with the choice of the sample preparation procedure. A technique for determination of the mass fraction of aluminum in the standard samples of carbon and low alloyed steels is developed. Indicators of the accuracy of the obtained results match the requirements specified for the accuracy of Al determination in the products of ferrous metallurgy.

The procedures of amperometric and potentiometric determination of chromium, manganese, vanadium and cerium in raw and materials of metallurgical production using a weight automatic titrator «TITRION» have been developed and implemented at the Research center of the Institute for Certified Reference Materials (ICRM). The use of the device provides automation of the titration along with collection of information and data processing which reduces the labor costs, shortens the analysis time, and improves the metrological characteristics. The developed methods, included in the branch and Federal Register, cover almost the entire range of the state standard reference samples of the raw and materials of metallurgical production in a wide range of detectable concentrations and match the metrological requirements.