GB/T 17040-2008 Petroleum and petroleum products — Determination of sulfur content — Energy-dispersive X-ray fluorescence spectrometry

Summary page. This page is a compiled excerpt/summary of the standard — it is not the full standard text and does not replace it. Verify every value against the official standard and the product certificate before use.

GB/T 17040-2008 specifies the determination of sulfur content in petroleum and petroleum products by energy-dispersive X-ray fluorescence spectrometry; this page is a historical study note on the withdrawn 2008 edition, covering its scope, principle, calibration, counting and precision.

Evidence note: original historical study material based on the original of the 2008 edition; it was withdrawn on 2019-10-01 and wholly replaced by the 2019 edition. It is not the full text of the standard or a controlled operating procedure, and technical review is pending. Method precision is not the uncertainty of a product batch.

Official version status: Designated original PDF physical pages 1 and 2. Compiled from the 8 physical pages of the original of GB/T 17040-2008, issued 2008-08-25, implemented 2009-02-01, replacing the 1997 edition. The official record lists withdrawal on 2019-10-01 and wholesale replacement by the 2019 edition; this page is for historical method study, does not call the old edition current, and does not replace the 2019 entry. The two official services both belong to the national standards information system and are not independent technical acceptance.

Scope: Designated original PDF physical pages 3 and 4. The original method covers a sulfur mass fraction of 0.0150 %–5.00 % for the petroleum and petroleum products listed. Lower concentrations in the counting table or the calibration table do not automatically extend the scope of the method. M85/M100 require matrix-matched standard samples; original 5.4 states explicitly that the repeatability, reproducibility and bias of this edition do not cover such fuels.

Principle and interferences: Designated original PDF physical pages 3 and 4. Energy-dispersive X-ray fluorescence compares the response of the sulfur Kα characteristic radiation with calibration samples. Spectral interferences and matrix effects are handled separately; built-in correction functions of the instrument must still be verified or the calibration rebuilt — the manufacturer's preset curve cannot be regarded as directly applicable. The absorption effect of high-oxygen fuels and the matrix-matching limitation are retained.

Apparatus conditions: Designated original PDF physical page 4. Original 6.1.1: effective excitation energy above 2.5 keV; 6.1.2: minimum sample depth 4 mm; 6.1.3: sulfur Kα energy 2.3 keV with a resolution not exceeding 800 eV. These are equipment conditions of the method, not guaranteed product specifications. Radioactive-source shielding and instrument safety must be implemented by trained personnel under controlled documents; the complete construction and safety procedures have not been reconstructed.

Reagents and reference materials: Designated original PDF physical pages 4 and 5. Di-n-butyl sulfide (DBS) must have a verified, accurate sulfur content and cannot be accepted on purity alone; the original note that the sulfur content is generally 21.91 % is not a value for any product or batch certificate. White oil and other diluents have a sulfur content below 2 mg/kg. Window material must resist attack by the sample and suit the instrument; the effect of high aromatics on the film material is handled under the original limits.

Sampling and sample preparation: Designated original PDF physical page 5. Follow the originally cited sampling procedure; analyse promptly after filling the cell and deal with bubbles produced by agitation. Reusable cells must be clean and dry, disposable cells must not be reused, and a new window film is used for each sample. A change of film type or thickness requires recalibration; a cleanliness check is not equivalent to a passed calibration.

Initial standard samples: Designated original PDF physical page 5. The two initial standards, 0.1 % and 5.0 %, are each prepared by weighing and cannot be replaced by serial dilution from a single high-concentration standard. Original 9.1.3 and 9.1.6 specify weighing to 0.1 mg, and the actual sulfur content must include the sulfur in the diluent. The compositions in the original table are historical calibration study and do not promise that reagents are available or that products are suitable. Sulfur mass fraction % | Diluent g | DBS g 5 | 48.6 | 14.4 0.1 | 43.6 | 0.200

Weighted standard preparation formula: Designated original PDF physical page 5. Original equation (1): S = (m_DBS × S_DBS + m_MO × S_MO)/(m_DBS + m_MO). Both masses are in g; S, S_DBS and S_MO are sulfur mass fractions expressed in %, and percentage inputs must not be mixed freely with g/g decimals. Each symbol corresponds to the original mass fraction and mass units; this page provides no standard-preparation calculator.

Calibration range and roles of standards: Designated original PDF physical page 6. Original Table 2 lists low and high calibration concentration sets as examples, with blank cells left blank. The roles of calibration standards, check standards not used in building the curve, and QC materials representing routine samples are kept separate. The original storage requirements for standards and QC are method arrangements such as a dark place and relatively low temperature; no general storage temperature is given, and no product transport, storage or shelf life is inferred. No. | Low set 0.0020–0.1 % | High set 0.1–5.0 % 1 | 0.000 | 0.000 2 | 0.0020 | 0.100 3 | 0.0050 | 0.500 4 | 0.0100 | 1.00 5 | 0.0300 | 2.50 6 | 0.0600 | 5.00 7 | 0.100 | –

Sample loading and counting: Designated original PDF physical pages 6 and 7. Loading is usually about three quarters of the cell volume and must satisfy the minimum depth; volatile samples must be prevented from deforming the window or leaking liquid. Each calibration standard is counted twice, repeating with a new cell and a fresh portion of sample. The two counting ranges of Table 3 overlap at 0.100 %, and the original does not state which side the boundary belongs to, so no automatic branch is added. Sulfur mass fraction % | Counting time s 0.000–0.100 | 200–300 0.100–5.00 | 100

Calibration check and sample re-measurement: Designated original PDF physical pages 6 and 7. After the curve has been established, check standards are used to verify it; the relative error between the measured and the recommended value must not exceed 3 %, otherwise the instrument is adjusted and recalibrated. This is not r/R or batch uncertainty. Samples are measured twice consecutively and the mean is taken; if the mean lies outside the range of the curve, the sample is measured twice more using a curve that covers that mean.

Results and quality control: Designated original PDF physical page 7. Results are reported as sulfur mass fraction in %, rounded to three significant figures, without importing the reporting branch of the 2019 edition. QC frequency is determined by the quality status and stability demonstrated by the measurements; the original example for normal use is once a day or twice a week, and the new edition's provision of at most 10 samples must not be transferred. Results are recorded and the state of statistical control is assessed; results outside control limits require investigation of the cause.

Precision and bias: Designated original PDF physical pages 7 and 8. Original 15.1 gives, at the 95 % confidence level, r = 0.02894(X + 0.1691) and R = 0.1215(X + 0.05555), where X is the mean sulfur mass fraction of two results in %; these cannot be exchanged for the power form of the 2019 edition or for batch certificate uncertainty. Original 15.2 is phrased for a single laboratory yet speaks of reproducibility, and its linkage with the cross-laboratory definition in 15.1.2 awaits review. In Table 4 the significance for SRM 1623c is "yes", which cannot be generalised to mean that no material shows significant bias. NIST material | S/% | Bias | Significant SRM 1616a | 0.0146 | 0.0009 | No SRM 2724a | 0.0430 | 0.0008 | No SRM 1617a | 0.173 | 0.0003 | No SRM 1623c | 0.381 | −0.0119 | Yes SRM 1621e | 0.948 | −0.0198 | No SRM 2717 | 3.02 | 0.0072 | No

Source range and unverified items: Designated original PDF physical pages 1, 2, 3, 4, 5, 6, 7 and 8. The 8 physical pages of the original of the same edition were reviewed; the formulas, tables and key figures listed were cross-checked locally against the original images, and OCR was used only for locating text. The complete instrument, software corrections and controlled safety procedures have not been fully technically reviewed, and independent technical acceptance is still to be verified. Scans are not published, and the historical material implies nothing about current standard equivalence, product applicability, values or supply.

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