SH/T 0136-1992 Test method for sulfides in petroleum wax

AI-translated method card — human verification pending. This is not an official translation of the standard. Unclear source values remain unverified; check the original standard and product certificate before use.

Card type: Test method

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

• Standard number: SH/T 0136-92
• Chinese name: Test method for sulfides in petroleum wax
• English name: not provided in the available source
• Replacement relationship: From the date of implementation of this standard, the former national standard GB 11084-89 "Test method for sulfides in petroleum wax" is void.
• Adoption relationship: This standard equivalently adopts the test method for "sulfides" in Item 3.3 of the 1982 edition of the Japanese Standard for Cosmetic Raw Materials "Paraffin".
• Technical administration and drafting: Technically administered by Fushun Research Institute of Petroleum and Petrochemicals; drafted under the responsibility of Fushun Research Institute of Petroleum and Petrochemicals; main drafter Tian Tingling.
• Approval and implementation: Approved by China Petrochemical Corporation 1992-05-20, implemented on 1992-05-20.

2. Scope of application and non-applicability

• This standard specifies the test method for sulfides in petroleum wax.
• This standard applies to paraffin, petrolatum, and white oil for cosmetics.
• Not applicable: not provided in the available source.

3. Method principle

First add anhydrous ethanol 2mL to the test sample, then add 2 drops of clear sodium plumbite solution, shake to mix and simultaneously heat at 70℃ for 10min; if no obvious dark color appears compared with the ethanol liquid layer of the comparison test, the sulfide test of the test sample is judged to pass.

4. Reagents and materials (purity / preparation)

• Anhydrous ethanol: analytical reagent.
• Lead oxide (PbO): analytical reagent. The source writes "lead oxide (P60)", suspected to be a misrecognition of source-text extraction in PbO, requires confirmation against the source standard (source-text extraction).
• Sodium hydroxide: analytical reagent. Prepare 200g/L sodium hydroxide solution. The concentration unit is garbled in the source transcription. Verify the stated concentration against the original standard before preparing the solution.
• Preparation of saturated sodium plumbite solution (5.1): take 200g/L sodium hydroxide solution 100mL, add it into a 150mL narrow-mouth bottle with a stopper, weigh lead oxide 12g and add it into the narrow-mouth bottle containing the sodium hydroxide solution, tightly close the stopper, shake vigorously for 30min, then let stand to settle for 24h, and remove the clear liquid by decantation. If the solution is turbid, filter it through a funnel packed with a glass fiber filter layer. Store the clear saturated sodium plumbite solution in a 150mL stoppered narrow-mouth bottle for later use.
• Reagent for comparison test: 200g/L sodium hydroxide solution (in the comparison test tube, no sodium plumbite solution is added; instead, 2 drops of 200g/L sodium hydroxide solution are added).

5. Instruments and equipment

• 4.1 test tubes: made of hard glass, with ground stoppers, length 140mm±3mm, outer diameter 14mm±1mm, volume 16mL±1mL. The upper opening of the test tube has a rim to facilitate seating in the water bath cover; the test tubes and stoppers are both marked with the same number.
• 4.2 burette: 25mL.
• 4.3 graduated cylinder: 100mL.
• 4.4 beaker: 150mL.
• 4.5 narrow-mouth bottle: 150mL, with a ground stopper.
• 4.6 stopwatch: precision 0.1s.
• 4.7 pipette: 5mL.
• 4.8 constant-temperature water bath: operating temperature range <100℃. Temperature control precision ±0.5℃. The source "<1000C" "t 0.590 0" is source-text extraction noise, requires confirmation against the source standard (source-text extraction).

6. Recommended operating conditions

• Constant-temperature water bath temperature: 70℃±0.5℃.
• Heating time: after the sample has completely melted, continue heating for 10min; after adding anhydrous ethanol, continue heating for 5min; after the shaking operation is completed, continue heating in the water bath for 5min.
• Shaking: quickly remove the test tube from the water bath, press the stopper with the index finger, and shake the test tube vertically and vigorously three times, with an amplitude of 12～15cm; after shaking, release the stopper to vent, reinsert the stopper, and at the same time quickly return the test tube to the constant-temperature water bath. The above operation is performed once per minute and repeated five times (during each shaking cycle, the time the test tube is outside the water bath must not exceed 3s).
• If layering is poor: the three test tubes may continue to be heated for an extended time of 5～10min, and comparison is made after layering.

7. Sampling and test sample preparation

• Use three test tubes (one of which is used for the comparison test) to separately weigh 4g of the sample to be tested, weighed accurately to 0.2g.
• For white oil samples, measure 4mL with a pipette.
• Insert the test tube stoppers, place the test tubes in a constant-temperature water bath and heat; after the sample has completely melted, continue heating for 10min.

8. Analytical procedure

• 5.1 Prepare saturated sodium plumbite solution: see Section 4.
• 5.2 Heat the constant-temperature water bath to 70℃±0.5℃ and set aside for use.
• 5.3 Use three test tubes (one of which is used for the comparison test) to separately weigh 4g of the sample to be tested, weighed accurately to 0.2g (for white oil samples, measure 4mL with a pipette), and insert the test tube stoppers. Place the test tubes in a constant-temperature water bath and heat; after the sample has completely melted, continue heating for 10min, open the stopper and add anhydrous ethanol 2mL with a pipette, insert the test tube stopper and continue heating for 5min, open the stopper and add 2 drops of sodium plumbite solution with a dropper (in the comparison test tube, no sodium plumbite solution is added; instead, 2 drops of 200g/L sodium hydroxide solution are added), then insert the stopper again, then quickly remove the test tube from the water bath, press the stopper with the index finger, and shake the test tube vertically and vigorously three times, with an amplitude of 12～15cm; after shaking, release the stopper to vent, reinsert the stopper, and at the same time quickly return the test tube to the constant-temperature water bath. The above operation is performed once per minute and repeated five times (during each shaking cycle, the time the test tube is outside the water bath must not exceed 3s). Then continue heating the test tubes in the water bath for 5min; after the sample and ethanol solution in the test tubes have separated into layers, remove the test tubes from the constant-temperature water bath, place them in front of white filter paper or observe the upper ethanol solution toward the light; if the ethanol layer of the test test tube does not show an obvious dark color compared with the ethanol layer of the comparison test tube, the sulfide test of the sample is deemed to pass. If the sample and ethanol solution layer poorly, the three test tubes may continue to be heated for an extended time of 5～10min, and comparison is made after layering.

9. Qualitative and quantitative determination and calculation formula

• This method is a qualitative judgment (pass / fail); no calculation formula is provided in the available source.
• Judgment rule: if the ethanol layer of the test test tube does not show an obvious dark color compared with the ethanol layer of the comparison test tube, the sulfide test of the sample is deemed to pass.

10. Precision

• When the parallel test results of the same operator differ, repeat determination must be carried out; when the two results of the repeat determination are the same, the test result may be reported. If the repeat test still gives two different results, the test is determined to fail.
• No other precision indicators are provided in the available source.

11. Report

• When the parallel test results of the same operator differ, repeat determination must be carried out; when the two results of the repeat determination are the same, the test result may be reported. If the repeat test still gives two different results, the test is determined to fail.
• No detailed provisions on report format are provided in the available source.

12. Referenced documents

• GB 11084-89 "Test method for sulfides in petroleum wax" (void from the date of implementation of this standard).
• Japanese Standard for Cosmetic Raw Materials 1982 edition "Paraffin" Item 3.3 "sulfides" (source of equivalent adoption).
• No other normative referenced documents are provided in the available source.

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