GB/T 34100-2017 Determination of total sulfur in light hydrocarbons, engine fuels and other oils by ultraviolet fluorescence method

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Card type: Test method

1. Method number / full title / English title / replacement relationship

• Standard number: GB/T 34100—2017
• Chinese title: Determination of total sulfur in light hydrocarbons, engine fuels and other oils by ultraviolet fluorescence method
• English title: Test method for determination of total sulfur in light hydrocarbons, spark ignition engine fuel, diesel engine fuel, and engine oil—Ultraviolet fluorescence method
• Replacement relationship: not provided in the available source
• Publication date: 2017-07-31; implementation date: 2018-02-01
• Secretariat: National Technical Committee for Standardization of Petroleum Products and Lubricants (SAC/TC 280) (requires confirmation against the source standard (source-text extraction): the source text is garbled “ＳＡＣ／ＴＣ２８０”)
• Drafting organization/drafters: not provided in the available source (source-text extraction is garbled and cannot be confirmed)

2. Scope of application and non-applicability

• Applicable to the determination of total sulfur content in light hydrocarbons, engine fuels and other oils.
• Applicable boiling point range: 25 ℃～400 ℃ (the source text is “２５℃～４００℃”).
• Applicable viscosity range: 0.2 mm²/s～20 mm²/s (the source text is “０．２ｍｍ２／ｓ～２０ｍｍ２／ｓ”).
• Applicable sample types: naphtha, distillate oils, engine fuels, ethanol, fatty acid methyl esters (FAME) and engine oils, etc. (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• Measurement range: 1.0 mg/kg～8000 mg/kg.
• Not applicable to: no explicit “not applicable” clause is provided in the available source; the source text notes that attention is required for “samples with relatively high sulfur content, or relatively low sulfur content, or sulfur content outside the measurement range of this standard” (the source text is garbled, requires confirmation against the source standard (source-text extraction)).

3. Method principle

• The sample is introduced by the injector and burned under high temperature (about 1075 ℃) and oxygen-rich conditions, and sulfides are converted to sulfur dioxide (SO₂).
• The combustion gas is dried and purified, then enters an ultraviolet fluorescence (UV) detector; SO₂ is excited under ultraviolet light, emits fluorescence, and is detected by a photomultiplier tube.
• The fluorescence intensity is proportional to the SO₂ concentration, and the total sulfur content is calculated on this basis.
• The source text has a “———” note explaining matters related to the principle (source-text extraction is garbled, requires confirmation against the source standard (source-text extraction)).

4. Reagents and materials (purity / preparation)

• 4.1 Carrier gas/reaction gas: oxygen (O₂), purity ≥99.998%, sulfur content ≤5 mg/kg (the source text is “≥９９．９９８％，4dK≤５ｍｇ／ｋｇ”).
• 4.2 Carrier gas: argon (Ar), purity ≥99.75%, sulfur content ≤5 mg/kg, requires purification (the source text is “≥９９．７５％，4dK≤５ｍｇ／ｋｇ”).
• 4.3 Desiccant/purification material: specific name not provided in the available source (source-text extraction is garbled, requires confirmation against the source standard (source-text extraction)).
• 4.4 Solvent: must be sulfur-free or low-sulfur, used for dilution and cleaning (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• 4.5 Ultraviolet (UV) detector: used for SO₂ fluorescence detection (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• 4.6 Injector: 10 μL, 25 μL, 50 μL, 100 μL microinjector; injector needle length 50 mm±5 mm.
• 4.7 Reference materials:
  • 4.7.1 Sulfur reference material used for calibration (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
  • 4.7.2 Light hydrocarbon reference material: sulfur content about 1 μg/L～ (the source text is garbled, requires confirmation against the source standard (source-text extraction)), see Table 2.
  • 4.7.3 Gas reference material: see Table 3 (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• 4.8 Diluent: used to dilute high-sulfur samples, must be low-sulfur (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• 4.9 Other materials: not provided in the available source (the source text is “»¼Ÿ（U½|）” ).
• 4.10 Other materials: not provided in the available source (the source text is “¾¿（U½|）” ).
• Note: the source text states 5.2 carrier gas purity ≥99.998%, sulfur ≤5 mg/kg; 5.3 argon purity ≥99.75%, sulfur ≤5 mg/kg; 5.4 solvent must be sulfur-free; 5.5 dimethyl disulfide (DMDS) molecular weight 184.26, sulfur content 17.40%; 5.6 thiophene molecular weight 146.29, sulfur content 21.92%; 5.7 carbon disulfide molecular weight 134.20, sulfur content 23.90%; 5.9 sulfur standard solution 1000 mg/L: weigh 0.5748 g DMDS (or 0.4562 g thiophene or 0.4184 g carbon disulfide) and dissolve in 100 mL solvent.

5. Instruments and equipment

• 5.1 Combustion/injection system: includes injector, combustion tube, heating furnace, etc. (the source text is garbled, requires confirmation against the source standard (source-text extraction)).
• 5.2 Carrier gas: oxygen, purity ≥99.998%, sulfur ≤5 mg/kg.
• 5.3 Argon: purity ≥99.75%, sulfur ≤5 mg/kg, requires purification.
• 5.4 Solvent: sulfur-free solvent.
• 5.5 Dimethyl disulfide (DMDS): molecular weight 184.26, sulfur content 17.40%.
• 5.6 Thiophene: molecular weight 146.29, sulfur content 21.92%.
• 5.7 Carbon disulfide: molecular weight 134.20, sulfur content 23.90%.
• 5.8 Other: not provided in the available source (the source text is “zU¹”).
• 5.9 Sulfur standard solution (stock solution): 1000 mg/L, preparation method see the source text.
• 5.10 Quality control (QC) sample: used for routine quality control, see Chapter 13.

6. Recommended operating conditions

• 6.1 Sample according to GB/T 4756 and GB/T 27867. Samples must avoid light and high temperature to prevent sulfur loss.
• 6.2 Samples must be filtered to avoid particulate matter clogging the injector.
• 8.2 Recommended operating conditions are shown in Table 1:
  • Injector (light hydrocarbons): 1 μL/s
  • Injector (gas): 140～160 mm/min
  • Furnace temperature: 1075 ℃±25 ℃
  • Argon flow rate: 450～500 mL/min
  • Oxygen flow rate: 10～30 mL/min
  • Carrier gas flow rate: 130～160 mL/min
• 8.3 Adjust operating conditions according to sample type to ensure complete combustion.

7. Sampling and sample preparation

• 6.1 Sample according to GB/T 4756 and GB/T 27867.
• 6.2 Samples must be filtered to avoid particulate matter.
• 7 Sample preparation: the source text is garbled, requires confirmation against the source standard (source-text extraction).
• 9.2 Test portion preparation: select the injection amount according to sulfur content to avoid exceeding the linear range of the detector.
• 9.3 Calibration:
  • 9.3.1 Prepare the standard series according to Table 2 for calibration.
  • 9.3.2 Calibration curve: at least 5 points, correlation coefficient ≥0.999.
  • 9.3.3 Calibration verification: verify with an independent standard.
• 9.4 Sample determination:
  • 9.4.1 Light hydrocarbon samples: inject according to 4.7.2.
  • 9.4.2 Gas samples: inject according to 4.7.3.
  • 9.4.3 Gas samples: inject according to 4.7.3, and pay attention to the injection amount.
  • 9.4.4 Gas samples: pay attention to the injection amount.
• 9.5 Result calculation:
  • 9.5.1 Calculate according to the formula.
  • 9.5.2 Calculate according to formulas (1) and (2).
  • 9.5.3 Calculate according to formulas (3) and (4).
  • 9.5.4 Calculate according to formulas (5) and (6).

8. Analytical procedure

• 8.1 Operate according to the instrument instructions.
• 8.2 Set operating conditions according to Table 1.
• 8.3 Adjust conditions according to sample type.
• 9.1 Calibration: perform according to 9.3.
• 9.2 Test portion preparation: perform according to 9.2.
• 9.3 Calibration: perform according to 9.3.1～9.3.3.
• 9.4 Sample determination: perform according to 9.4.1～9.4.4.
• 9.5 Result calculation: perform according to 9.5.1～9.5.4.

9. Qualitative and quantitative determination and calculation formulas

• 11.1 Calculate sulfur content X (mg/kg) according to formulas (1) and (2):
  • X = (I - Y) × 1000 / (S × M × Kg) ………………（1）
  • X = (I - Y) × 1000 / (S × V × Kv) ………………（2）
  • Where: I is the sample signal; Y is the blank signal; S is the sensitivity; M is the sample mass; V is the injection volume; Kg is the mass correction factor; Kv is the volume correction factor.
• 11.2 Calculate according to formulas (3) and (4):
  • X = G × 1000 / (M × Kg) ………………（3）
  • X = G × 1000 / (V × D) ………………（4）
  • Where: G is the mass of sulfur in the sample; M is the sample mass; V is the injection volume; D is the dilution factor.
• 12.1 Calculate repeatability (r) and reproducibility (R) at the 95% confidence level.
• 12.2 Repeatability (r):
  • 400 mg/kg and below: r = 0.1788 X^0.75 ………………（5）
  • 400 mg/kg and above: r = 0.02902 X ………………（6）
• 12.3 Reproducibility (R):
  • 400 mg/kg and below: R = 0.5797 X^0.75 ………………（7）
  • 400 mg/kg and above: R = 0.1267 X ………………（8）
• When the sulfur content of 12.4 is below 400 mg/kg, look up r and R in Table 3.
• 12.5 Precision: verify with a standard substance (SRMs).

10. Precision

• 12.1 at the 95% confidence level.
• 12.2 The repeatability (r) formula is given in 12.2.
• 12.3 The reproducibility (R) formula is given in 12.3.
• 12.4 Table 3:
  • 1 mg/kg: r=0.2, R=0.6
  • 5 mg/kg: r=0.6, R=1.9
  • 10 mg/kg: r=1.0, R=3.3
  • 50 mg/kg: r=3.4, R=10.9
  • 100 mg/kg: r=5.7, R=18.3
  • 400 mg/kg: r=16.0, R=51.9
• 12.5 Precision verification: use a standard substance.

11. Report

• The 13.1 report shall include the QC sample results (see 5.10).
• The 13.2 report shall include the information of QC and QA.
• The 13.3 report shall include the QC/QA record, see Appendix C.
• 14 Report: when the sulfur content is below 10 mg/kg, report to 1 mg/kg; when above 10 mg/kg, report to 0.1 mg/kg.

12. Normative references

• GB/T 1884 Standard test method for density of crude petroleum and liquid petroleum products by laboratory determination (hydrometer method)
• GB/T 1885 Petroleum measurement tables
• GB/T 4756 Standard practice for manual sampling of petroleum liquids
• GB/T 27867 Standard practice for automatic sampling of petroleum liquids in pipelines
• GB/T 29617 Standard test method for density, relative density, and API specific gravity of liquids by digital density meter
• SH/T 0604 Standard test method for density of crude petroleum and petroleum products (U-shaped vibrating tube method)
• References:
  • [1] NB/SH/T 0843 Determination of total sulfur content in petroleum products by ultraviolet fluorescence method (requires confirmation against the source standard (source-text extraction))
  • [2] ASTM MNL7 Manual on Presentation of Data and Control Chart Analysis

13. Source and verification

This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.

14. Quick Q&A reference