ISO 15597 Petroleum and Related Products - Determination of Chlorine and Bromine Content - Wavelength-Dispersive X-Ray Fluorescence Spectrometry

ISO 15597 Petroleum and Related Products - Determination of Chlorine and Bromine Content - Wavelength-Dispersive X-Ray Fluorescence Spectrometry

“I” published by the International Organization for Standardization (ISO)SO 15597 Petroleum and related products - Determination of chlorine and bromine content - Wavelength-dispersive X-ray fluorescence spectrometryThe standard describes a method for determining the chlorine and bromine contents of liquid petroleum products, synthetic oils and fluids, and petroleum product additives (including used oils) soluble in organic solvents and having negligible or accurately known chlorine/bromine contents. This method is applicable to products or additives having chlorine contents in the range of 0,000-5 to 0,100 mass percent and bromine contents in the range of 0,001-0 to 0,100 mass percent. Other elements are generally immiscible, but lead is miscible at contents above 0,1500 percent (m/m).

ISO 15597 Petroleum and Related Products - Determination of Chlorine and Bromine Content - Wavelength-Dispersive X-Ray Fluorescence Spectrometry

Used lubricants can present special problems due to the variety of potentially interfering elements in relatively high concentrations. For used lubricants, the lower limit of sensitivity can generally be 0,0050 percent (m/m).

In principle, the test sample and a bismuth solution serving as an internal standard are mixed in a specified mass ratio and exposed to the primary radiation of an X-ray tube in a sample cell. The chlorine or bromine content of the sample is determined from calibration curves prepared using chlorine or bromine calibration standards.

Unless otherwise specified, samples should be collected in accordance with the procedures specified in ISO 3170 or ISO 3171. Samples should be collected after thorough mixing and subdivision of the sample. Viscous samples are heated to a temperature that fluidizes the sample and, if necessary, homogenized using a homogenizer or mixer. For the purposes of this procedure, the term sample includes solutions prepared from semi-solid or solid petroleum products, as appropriate, pretreated or diluted with additives.

In the complex world of petroleum refining and quality control, ensuring the purity and safety of fuels and lubricants is paramount. Contaminants such as chlorine and bromine can lead to engine corrosion, environmental hazards, and regulatory non-compliance. This is where ISO 15597, an international standard that enables the precise determination of chlorine and bromine content in petroleum and related products using wavelength-dispersive X-ray fluorescence spectrometry (WD-XRF), comes into play.

This standard has become a cornerstone for laboratories worldwide by providing a non-destructive, rapid analysis technique that minimizes sample preparation and maximizes accuracy.

The ISO 15597 standard specifies a standard procedure for determining the amount of chlorine and bromine in petroleum products such as crude oil, refined fuels, lubricants, and additives. These halogens typically enter the supply chain through impurities in crude oil or processing aids, and their levels must be monitored to comply with stringent environmental regulations, such as those of the U.S. Environmental Protection Agency (EPA) or the European Union's REACH framework.

This standard outlines the calibration, measurement, and verification steps to ensure that results are reliable within specified limits and will typically detect concentrations down to levels higher than parts per million (ppm).

At the heart of the ISO 15597 standard is wavelength-dispersive X-ray fluorescence spectrometry, a powerful and evolving analytical technique. This instrument uses a diffraction grating to separate X-ray fluorescence wavelengths and provides superior resolution for elements such as chlorine and bromine.

The operating steps of the system are as follows:

  • Sample preparation: A small portion of the liquid petroleum product is placed in a sample container, usually undiluted, to preserve the matrix.
  • Excitation: The sample is bombarded with a high-energy X-ray beam from a tube source (e.g., rhodium or tungsten anode).
  • Emission: Atoms in the sample absorb energy and emit characteristic fluorescent X-rays.
  • Detection and analysis: A crystal analyzer (e.g., LiF for the halogens) diffracts X-rays into a detector. The intensity of these lines is proportional to the concentration of the element, calibrated against certified reference materials.

This method excels at multi-element analysis, making it ideal for routine quality control in refineries.

The ISO 15597 standard applies to petroleum products with chlorine and bromine contents ranging from 1 mg/kg to several percent by mass. It is particularly useful for:

  • Refinery control: Monitoring of desulfurization processes where halogens are present together with sulfur.
  • Environmental compatibility: Ensuring low halogen levels in fuels to avoid acid rain precursors or groundwater pollution.
  • Product certification: Approval of lubricants and additives for automotive and industrial use.

This standard has been adopted worldwide, with national versions such as DIN ISO 15597 in Germany and BS ISO 15597 in the United Kingdom, ensuring harmonised testing protocols.

Adopting the ISO 15597 standard has numerous advantages over traditional wet chemistry methods such as titration or combustion ion chromatography. For example,

  • Speed: Results are available within minutes according to the ISO 15597 standard. Results are available in hours to days with traditional methods.
  • Sample destruction: Non-destructive according to ISO 15597. Destructive by traditional methods.
  • Precision: Repeatability plus/minus 0,5–2 percent relative to ISO 15597. Variable, often higher error with traditional methods.
  • Cost: Low per sample after initial setup in ISO 15597. High in traditional methods due to reagents and labor.
  • Versatility: Processes solids, liquids and slurries to ISO 15597. Traditional methods are limited to liquids.

Because of these advantages, major manufacturers have made their wavelength-dispersive X-ray fluorescence spectrometry (WD-XRF) devices compatible with this standard and have become indispensable for petrochemical laboratories.

Ultimately, the ISO 15597 standard is a testament to ISO's role in promoting global standardization in developing safer and cleaner petroleum products that power the world. By providing a robust and efficient method for halogen analysis, it not only safeguards industrial processes but also contributes to environmental management. As this standard continues to evolve, it will continue to support the petroleum sector's transition to more environmentally friendly practices.

Our organization, which has been operating for many years and meticulously follows global developments in science and technology, employs a team of experienced professionals and a broad infrastructure to conduct testing, measurement, and analysis in a wide range of areas for businesses across all sectors. In this context, we also provide testing services in accordance with the ISO 15597 Petroleum and related products - Determination of chlorine and bromine content - Wavelength-dispersive X-ray fluorescence spectrometry standard.

WhatsApp