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Sulfur content is one of the most important properties of fuels for quality control. Reliable analysis of sulfur in fuels requires that the analytical instruments are calibrated using accurately prepared sulfur standard solutions. For the purpose, it is important to estimate the accurate sulfur contents in the high purity sulfur compounds used for preparation of the calibration solutions. Because metrological traceability is essential for comparability of measurements, calibrants that are traceable to International System of Units (SI) is required1). Various reference materials for the determination of sulfur have been issued by some organizations, such as the National Institute of Standards and Technology (NIST), the Japan Petroleum Institute (JPI), and others. Recently, certified reference materials (CRMs) for calibration, NMIJ CRM 4215-a2) and NMIJ CRM 4217-a, and reference material (RM), NMIJ RM 4216-a3) have been developed by the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ, AIST). These CRMs and RM are sulfur standard solutions for the measurement of sulfur-free levels (<10 mg kg1). However, no sulfur standard solution for the calibration corresponding to sulfur contents higher than 10 mg kg1 has been issued by NMIJ. Hence, a CRM of high purity dibutyl sulfide, NMIJ CRM 4221-a, has been issued by NMIJ. Dibutyl sulfide was selected, because it is one of the sulfur compounds which are recommended as calibrants for the determination of sulfur in fuels by the Japan Industrial Standards (JIS K 2541 : 2003). The certified value, sulfur content (mass fraction), was determined from the purity of the CRM, molecular weight, sulfur atomic weight, and sulfur content attributable to impurities in the CRM. The purity of the CRM was determined by a freezing point depression method and by a mass balance method in which the total amount of impurities is subtracted from 100 %4). Since the freezing point depression method is a primary method of the measurement and was validated by a mass balance method, the obtained purity is traceable to the SI5). In addition, the calculated molecular weight of the compounds and the atomic weight of sulfur were based on the IUPAC atomic weight table (2009)6). Therefore, the certified value calculated from the above parameters is traceable to the SI.

Development of High Purity Dibutyl Sulfide Certified Reference Material (NMIJ CRM 4221-a) for Determination of Sulfur in Fuels