ASTM D6122-23 PDF
Standard Practice for Validation of the Performance of Multivariate Online, At-Line, Field and Laboratory Infrared Spectrophotometer, and Raman Spectrometer Based Analyzer Systems
Standard Practice for Validation of the Performance of Multivariate Online, At-Line, Field and Laboratory Infrared Spectrophotometer, and Raman Spectrometer Based Analyzer Systems
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 52
- Дата публикации:
- 1 июля 2023 г.
- Издание:
- D6122
- ICS:
- 17.180.30
SIGNIFICANCE AND USE 5.1 The primary purpose of this practice is to permit the user to validate numerical values produced by a multivariate, infrared or near-infrared laboratory or process (online or at-line) analyzer calibrated to measure a specific chemical concentration, chemical property, or physical property. If the analyzer results agree with the primary test method to within limits based on the multivariate model for the user-prespecified statistical confidence level, these results can be considered ’validated’ to the user pre-specified confidence limit for a specific application, and hence can be considered useful for that specific application. 5.2 Procedures are described for verifying that the instrument, the model, and the analyzer system are stable and properly operating. 5.3 A multivariate analyzer system inherently utilizes a multivariate calibration model. In practice, the model both implicitly and explicitly spans some subset of the population of all possible samples that could be in the complete multivariate sample space. The model is applicable only to samples that fall within the subset population used in the model construction. A sample measurement cannot be validated unless applicability is established. Applicability cannot be assumed. 5.3.1 Outlier detection methods are used to demonstrate applicability of the calibration model for the analysis of the process sample spectrum. The outlier detection limits are based on historical as well as theoretical criteria. The outlier detection methods are used to establish whether the results obtained by an analyzer are potentially valid. The validation procedures are based on mathematical test criteria that indicate whether the process sample spectrum is within the range spanned by the analyzer system calibration model. If the sample spectrum is an outlier, the analyzer result is invalid. If the sample spectrum is not an outlier, then the analyzer result is valid providing that all other requirements for validity are... SCOPE 1.1 This practice covers requirements for the validation of measurements made by laboratory, field, or process (online or at-line) infrared (near- or mid-infrared analyzers, or both), and Raman analyzers, used in the calculation of physical, chemical, or quality parameters (that is, properties) of liquid petroleum products and fuels. The properties are calculated from spectroscopic data using multivariate modeling methods. The requirements include verification of adequate instrument performance, verification of the applicability of the calibration model to the spectrum of the sample under test, and verification that the uncertainties associated with the degree of agreement between the results calculated from the infrared or Raman measurements and the results produced by the PTM used for the development of the calibration model meets user-specified requirements. Initially, a limited number of validation samples representative of current production are used to do a local validation. When there is an adequate number of validation samples with sufficient variation in both property level and sample composition to span the model calibration space, the statistical methodology of Practice D6708 can be used to provide general validation of this equivalence over the complete operating range of the analyzer. For cases where adequate property and composition variation is not achieved, local validation shall continue to be used. 1.1.1 For some applications, the analyzer and PTM are applied to the same material. The application of the multivariate model to the analyzer output (spectrum) directly produces a PPTMR for the same material for which the spectrum was measured. The PPTMRs are compared to the PTMRs measured on the same materials to determine the degree of agreement. 1.1.2 For other applications, the material measured by the analyzer system is subjected to a consistent additive treatment prior to being analyzed by the PTM...
Abstract
Overview
ASTM D6122-23 provides a comprehensive standard practice for validating the performance of multivariate online, at-line, field, and laboratory infrared spectrophotometer and Raman spectrometer based analyzer systems. Developed by ASTM International, this practice is critical for ensuring the reliability of infrared and Raman analyzers used to measure the physical, chemical, or quality properties of liquid petroleum products and fuels. The validation process ensures that results from these advanced analyzer systems are statistically equivalent to those obtained by traditional primary test methods (PTM), enhancing quality control, process efficiency, and regulatory compliance in the petroleum and fuels industries.
Key Topics
-
Scope of Application
- Covers laboratory, field, at-line, and online infrared (near- and mid-infrared) and Raman analyzers.
- Applies to systems that calculate properties of liquid petroleum products and fuels from spectroscopic data using multivariate modeling.
-
Validation Procedures
- Local Validation: Uses a limited set of real-world samples representative of current production, to show agreement between analyzer and PTM results within user-specified confidence limits.
- General Validation: Employs a broader, more statistically varied sample set, allowing for validation across the full calibration space using established methodologies such as ASTM D6708.
- Ongoing (Continual) Validation: Involves routine quality assurance and control chart monitoring to maintain validated status of analyzer systems after initial validation.
-
Model Applicability
- Emphasizes that validation is only valid for samples that fall within the calibration model’s defined population.
- Outlier detection methods are applied to ensure that the sample spectra are within the calibration range and suitable for reliable measurement.
-
Statistical Confidence and Uncertainty
- Results are only considered validated if they meet user-defined statistical confidence levels.
- The difference between analyzer results and PTM must fall within calculated uncertainty bounds, ensuring high confidence in reported values.
-
Instrument and Model Performance Verification
- Details procedures for verifying both hardware stability and correct model operation.
- Includes performance checks with instrument verification samples to detect any drift or malfunction.
Applications
ASTM D6122-23 is widely applied in:
- Process Analytical Technology: Supporting compliance and optimization in refinery and petrochemical operations by enabling rapid, real-time quality analysis.
- Product Release and Certification: Validating analyzer systems for product property certification in alignment with regulatory and contractual requirements.
- Research and Development: Providing framework for the evaluation of new analyzers, calibration transfers, and multivariate modeling techniques.
- Quality Assurance: Ensuring ongoing analyzer reliability through regular validation, supporting manufacturing consistency and customer confidence.
Industries that benefit include petroleum refining, fuel distribution, quality control laboratories, and chemical processing, where accurate measurement of multiple product qualities is essential.
Related Standards
To effectively implement ASTM D6122-23, familiarity with related ASTM standards is recommended, including:
- ASTM D6708: Statistical assessment of agreement between test methods for the same property.
- ASTM D8321: Development and validation of multivariate analyses for spectroscopic measurements.
- ASTM D3764: Performance validation of process stream analyzer systems.
- ASTM D8340: Performance-based qualification of spectroscopic analyzer systems.
- ASTM D6299: Statistical quality assurance and control charting techniques.
- ASTM E131/E456/E932/E1421: Terminology and performance measurement guidelines for molecular spectroscopy.
These standards provide critical support for sample handling, calibration, measurement, statistical validation, and ongoing quality control.
Adhering to ASTM D6122-23 ensures robust validation of multivariate infrared and Raman analyzer systems, supporting regulatory compliance, process optimization, and industry best practices in liquid fuel and petroleum product analysis.
Технические детали
- Технический комитет
- D02 - Petroleum Products, Liquid Fuels, and Lubricants
- SKU
- ASTM D6122-23
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