ASTM WK57245

    New Test Method for Sulfur, Chlorine, Calcium, Vanadium, Iron and Nickel in Crude and Residual Oil by Wavelength or Energy Dispersive X-ray Fluorescence Spectrometry

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    Developed by Subcommittee: D02.03 | Committee D02 | Contact Staff Manager



    WK57245

    1. Scope

    1.1 This test method covers the quantitative determination of total sulfur, chlorine, calcium, vanadium, iron and nickel in crude and residual oil in the concentration ranges shown in in table 1 using X-ray Fluorescence (XRF) techniques. Sec. 1and Table 1 will be modified after ILS to reflect statistical breakouts in section 8 performance criteria, PLOQs, r and R values. TABLE 1 Elements and Ranges of Applicability ElementConcentration Range Sulfur0.1 to 5.0 mass % Chlorine5 to 200 mg/kg Calcium25 to 800 mg/kg Vanadium5 to 500 mg/kg Iron5 to 500 mg/kg Nickel5 to 150 mg/kg 1.2 Sulfur is measured for informational purposes and is not measured for the performance based qualification criteria (sec. 8). For measurement of sulfur by standard test method use ASTM D4294, D2622 or other suitable standard test method for sulfur in crude and residual oils. 1.3 The values of the pooled limit of quantification (PLOQ) and method repeatability (r) and reproducibility (R) for a specic instrument depends on instrument source power, X-ray source type, detection type, and the practices established by the laboratory to perform the method. More specific description to be written after ILS statistical breakout. NOTE 1Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at low mass fraction of chlorine, calcium, vanadium, iron and nickel must be determined by the Performance Based test described in Section 8 in this method. 1.4 The material may contain entrained water at ambient conditions, liqueable with moderate heat, or soluble in hydrocarbon solvents. 1.5 Samples containing higher concentrations than shown in Table 1 must be diluted to bring the elemental concentration of the diluted material within the scope of this test method (see sec. 9.2). 1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6.1 The preferred concentrations units are mass % for sulfur, and mg/kg for chlorine, calcium, vanadium, iron and nickel. 1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.


    Keywords


    Rationale

    Users and commercial labs in the petroleum industry request a standard test method for screening, monitoring and precisely measuring sulfur, chlorine, calcium, and the metals vanadium, iron and nickel in crude and residual oil for various needs in all sectors, upstream, midstream and downstream. Rather than several instrument-specific methods, this work item addresses a single performance-based approach to include WDXRF and EDXRF systems using polychromatic or monochromatic excitation.

    The title and scope are in draft form and are under development within this ASTM Committee.

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    Work Item Status

    Date Initiated:
    01-09-2017

    Technical Contact:
    Scott Fess

    Item:
    057

    Ballot:
    D02 (19-02)

    Status:
    Negative Votes Need Resolution