SH/T 0194-1992 Determination of active sulfur in additives and additive-containing oils

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Card type: Test method

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

• Standard number: SH/T 0194-92
• Full title: Determination of active sulfur in additives and additive-containing oils
• English name: not provided in the available source
• Replacement relationship: replaces ZE E34 012-88
• Other: confirmed in 2000; reference adoption of ASTM D1662-69(1979) "Standard Test Method for Active Sulfur in Cutting Fluids"

2. Scope of application and non-applicability

• Scope of application: This standard specifies the method for determining active sulfur in additives and additive-containing oils; it is applicable to additives and additive-containing oils.
• Not applicable: not provided in the available source.

3. Method principle

Take a 50g test sample (additive products must be diluted to a certain concentration before sampling), react with copper powder (added in two portions, each time 5g, with an interval of 10min) at 149℃ for 1h. The difference between the total sulfur content of the test sample before and after reaction with copper powder is the active sulfur content, expressed as a mass percentage [%(m/m)].

4. Reagents and materials (purity / preparation)

• 4.2.1 Copper powder: chemically pure, 200 mesh (equivalent to a particle linear diameter of 0.053mm).
• 4.2.2 Liquid paraffin: chemically pure, distillation temperature greater than 320℃.
• 4.2.3 White oil: sulfur content should be less than 0.01%(m/m) [determined according to SH/T 0253].
• 4.2.4 Absorbent cotton.
• Dilution solvent: liquid paraffin or white oil (see 5.1.1).

5. Instruments and equipment

In addition to the instruments used in SH/T 0253 and SH/T 0303, the following instruments are also required:

• 4.1.1 Beaker: tall form, with spout, made of heat-resistant glass, 200mL.
• 4.1.2 Stirrer: made of glass in an inverted T shape, with blades of length, height, and thickness respectively 25mm × 6mm × 1mm symmetrically mounted on a rod with a diameter of 6mm.
• 4.1.3 Stirring motor: should be able to maintain a rotation speed of 500r/min±25r/min.
• 4.1.4 Electric furnace: closed type, 200V, 1kW.
• 4.1.5 Mercury contact thermometer: 0～200℃, with a scale division of 1 or 2℃.
• 4.1.6 Thermometer: 0～200℃, with a scale division of 1℃.
• 4.1.7 Electronic relay.
• 4.1.8 Variable transformer.
• 4.1.9 Tray balance: sensitivity of 0.1g.

6. Recommended operating conditions

• Reaction temperature: 149℃±3℃ (5.3).
• Stirring speed: 500r/min±25r/min (4.1.3).
• Copper powder addition: in two portions, each time 5g±0.2g, with an interval of 10min (5.4).
• Reaction time: continue reaction for 1h±2min (5.4).
• Heating control: when the test sample temperature reaches about 100℃, adjust the transformer so that the temperature rises slowly; when it reaches 146℃, adjust the mercury contact thermometer so that it stabilizes at 149℃±3℃ (5.3).

7. Sampling and test sample preparation

• 5.1.1 Additive test sample: use liquid paraffin or white oil as the dilution solvent, dilute by mass to 10%(m/m) or another concentration required by the submitter, then weigh 50g±2g into a tall-form beaker.
• 5.1.2 Additive-containing test sample: directly weigh 50g±2g into a tall-form beaker.

8. Analysis procedure

• 5.2 Place the beaker in a closed electric furnace, install the stirrer so that its blades are within 5mm from the bottom of the beaker. Insert the thermometer and mercury contact thermometer, adjust their respective positions, and start the stirrer.
• 5.3 Turn on the power to the closed electric furnace. When the test sample temperature reaches about 100℃, adjust the transformer so that the test sample temperature rises slowly. When the test sample temperature reaches 146℃, adjust the mercury contact thermometer so that it stabilizes at 149℃±3℃.
• 5.4 Weigh two portions of 5g±0.2g copper powder. Add the first portion of copper powder to the test sample and control the stirring speed so as to ensure that the added copper powder is uniformly dispersed in the test sample without layered settling. After 10min, add the second portion of copper powder and continue the reaction for 1h±2min.
• 5.5 After the reaction is completed, filter out the copper powder with filter paper while hot, ensuring that the filtrate contains no copper powder particles.
• 5.6 Determine the total sulfur content of the test sample before and after reaction with copper powder; for sulfur content greater than 1%(m/m), use the method of SH/T 0303; for sulfur content equal to or less than 1%(m/m), use the method of SH/T 0253.

9. Qualitative and quantitative determination and calculation formulas

• 6.1.1 When the dilution concentration is 10%(m/m), the active sulfur of the additive X₁[%(m/m)] is calculated according to formula (1): X₁ = (S₁ − S₂) × 10 Where: S₁—total sulfur content of the test sample before reaction, %(m/m); S₂—total sulfur content of the test sample after reaction, %(m/m).
• 6.1.2 For other dilution concentrations, the active sulfur of the additive is represented by the active sulfur of the test sample. The active sulfur of the test sample X₂[%(m/m)] is calculated according to formula (2): X₂ = S₃ − S₄ Where: S₃—total sulfur content of the test sample before reaction, %(m/m); S₄—total sulfur content of the test sample after reaction, %(m/m).
• 6.2 The active sulfur of the additive-containing oil test sample X₃[%(m/m)] is calculated according to formula (3): X₃ = S₅ − S₆ Where: S₅—total sulfur content of the test sample before reaction, %(m/m); S₆—total sulfur content of the test sample after reaction, %(m/m).
• Note: The variable subscripts in the formulas (S₁～S₆, X₁～X₃) are identified according to the original text of source-text extraction; some symbols are unclear in the source text and require confirmation against the source standard (source-text extraction).

10. Precision

Use the following provisions to judge the reliability of test results (95% confidence level).

• 7.1 Repeatability: The difference between two results obtained by the same operator on the same test sample in repeated determinations shall not exceed 0.11 times the arithmetic mean of their active sulfur mass percentages.
• 7.2 Reproducibility: The difference between test results obtained by two laboratories on the same test sample shall not exceed 0.243 times the arithmetic mean of their active sulfur mass percentages.

11. Report

Report the arithmetic mean of two results from repeated determinations. For results of 6.1.2, the dilution concentration shall be stated.

12. Referenced documents

• SH/T 0253 Determination of total sulfur content in light petroleum products (coulometric method)
• SH/T 0303 Determination of sulfur content in additives (coulometric method)

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 reference Q&A