SH/T 0034-1990 Determination of active components in additives

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

• Method number: SH/T 0034-90
• Full name: Determination of active components in additives
• English name: not provided in the available source
• Replacement relationship: not provided in the available source (the source states "(determined in 2000)", meaning requires confirmation against the source standard (source-text extraction))
• Approval/implementation: approved by China Petrochemical Corporation 1991-03-27, implemented 1992-04-01

2. Applicable scope and non-applicability

• Applicable: This standard specifies a method for separating dilution oil from additives by rubber membrane sleeve permeation and determining the active components in additives. It is applicable to polymeric additives (molecular weight greater than 2000) such as detergents, dispersants, viscosity index improvers, and pour point depressants.
• Not applicable: not provided in the available source.

3. Method principle

Based on the difference in molecular radius between additives and dilution oil, dilution oil molecules have a small radius and can permeate through the membrane, while additive molecules have a large radius and cannot permeate out, remaining inside the membrane. The material inside the membrane, after treatment and constant weight, is the active component of the additive.

4. Reagents and materials (purity / preparation)

4.1 Materials

• a. Rubber membrane sleeve: meets the requirements of GB 7544 standard, produced by Tianjin Latex Factory, Kangle brand, medium size
• b. Filter paper thimble: diameter 30 mm, height 100 mm
• c. Cotton thread
• d. Medical scissors
• e. Solvent naphtha for rubber industry: meets the requirements of SH 0004

5.2 Reagents

• 5.1 Petroleum ether: analytical grade, 30～60 ℃ and 60～90 ℃
• 5.2 Potassium dichromate: prepare chromic acid cleaning solution with a concentration of 50 g/L (the original text "50[unreadable unit]L" is source-text extraction noise, requires confirmation against the source standard (source-text extraction))

5. Instruments and equipment

• a. Fat extractor: 250 mL
• b. Conical flask: 100 mL
• c. Conical wash bottle: 250 mL
• d. Desiccator
• e. Glass ball open at both ends: diameter 30 mm
• f. Constant-temperature water bath: two-hole or four-hole, constant temperature not exceeding ±1 ℃ (the original text "[unreadable sign]19c" requires confirmation against the source standard (source-text extraction))
• g. Electric thermostatic drying oven: constant temperature not exceeding ±10 ℃ (the original text "[unreadable sign]10C" requires confirmation against the source standard (source-text extraction))
• h. Analytical balance: sensitivity 0.1 mg
• i. Rubber membrane sleeve permeation apparatus: see the figure below (the original figure, source-text extraction not fully presented)

Labels for the rubber membrane sleeve permeation apparatus figure: 1— condenser tube; 2— glass ball; 3— filter paper thimble; 4— rubber membrane sleeve; 5— sample; 6— petroleum ether; 7— water bath; 8— fat extractor

6. Recommended operating conditions

• Extraction reflux temperature: 70 ℃ ± 1 ℃ (the original text "70`C11℃" requires confirmation against the source standard (source-text extraction))
• Extraction reflux time: 6～8 h
• Petroleum ether amount: 250 mL (30～60 ℃)
• Drying temperature: 105～110 ℃
• Water bath: 70 ℃ ± 1 ℃

7. Sampling and sample preparation

• 6.2 Sample handling: shake the sample in a glass bottle (not exceeding three-quarters of the volume) for 5 min to mix it uniformly; viscous additives should be preheated to 70～80 ℃ to make them flow, then carefully stir with a glass rod for 5 min (the original text "5mino" requires confirmation against the source standard (source-text extraction)).
• 7.1 Weigh the test sample 1～2 g (weighed to 0.0002 g) (the original text "[unreadable leading symbols]00028" requires confirmation against the source standard (source-text extraction)) into the prepared rubber membrane sleeve.

8. Analysis procedure

6 Preparation work

• 6.1 Treatment of the rubber membrane sleeve: loosen the rubber membrane sleeve, wash the inside and outside of the rubber membrane sleeve with 60～90 ℃ petroleum ether, then wash with 30～60 ℃ petroleum ether, mainly to remove grease and impurities from the rubber membrane sleeve. Then immediately blow it dry with air, check for air leaks, roll it into its original shape and place it into the filter paper thimble, and clamp the rolled edge of the rubber membrane sleeve onto the upper opening of the filter paper thimble.
• 6.3 Preparation before weighing the sample: place the treated rubber membrane sleeve and filter paper thimble into a desiccator to dry until the difference between two consecutive weighings does not exceed 0.0004 g.
• 6.4 Washing of the conical flask: soak the conical flask in solvent naphtha for rubber industry for 100 mL, then wash the conical flask with laundry detergent, rinse off the alkalinity with water, place it in chromic acid cleaning solution to soak (the original text "chromium 0 4 solution [garbled soaking instruction]" requires confirmation against the source standard (source-text extraction)), finally rinse it clean with water, place it in a constant-temperature drying oven, and dry at 105～110 ℃ to constant weight.

7 Test procedure

• 7.1 Weigh the test sample 1～2 g (weighed to 0.0002 g) into the prepared rubber membrane sleeve, make the length of the rubber membrane sleeve the same as the filter paper thimble, place it into the filter paper thimble, and clamp the rolled edge onto the opening of the filter paper thimble.
• 7.2 Put a glass ball over the opening of the filter paper thimble, loosen the rubber membrane sleeve, let the rubber membrane sleeve cover the entire glass ball, tie the mouth of the rubber membrane sleeve tightly to the mouth of the glass ball with cotton thread, and cut off the excess rubber membrane sleeve.
• 7.3 Place the filter paper thimble together with the rubber membrane sleeve into the fat extractor, add 250 mL 30～60 ℃ petroleum ether into the distillation flask of the fat extractor, place it in a water bath, and reflux at 70 ℃ ± 1 ℃ temperature for 6～8 h. As shown in the figure.
• 7.4 Take out the rubber membrane sleeve, pour the material inside the rubber membrane sleeve into a conical flask that has been brought to constant weight at 105～110 ℃, carefully wash the rubber membrane sleeve with 30～60 ℃ petroleum ether, put the washing liquid into the same conical flask, evaporate off the petroleum ether, then place it in an oven and dry to constant weight.

9. Qualitative and quantitative determination and calculation formula

The active component X [%(m/m)] in the sample is calculated according to the following formula:

X = (m₂ − m₁) / m × 100

Where:

• m₂ — mass of the additive active component and the conical flask, g
• m₁ — mass of the conical flask, g
• m — mass of the test sample, g

(The original formula source-text extraction contains noise; the symbols are based on the above arrangement, requires confirmation against the source standard (source-text extraction))

10. Precision

Judge the reliability of the test results according to the following provisions (95% confidence level):

• 9.1 Repeatability: the difference between two results obtained by the same operator in repeated determinations shall not exceed 1.2% of their arithmetic mean.
• 9.2 Reproducibility: the difference between two results submitted by different laboratories shall not exceed 2.0% of their arithmetic mean.

11. Report

Take the arithmetic mean of two repeated determination results (to three significant figures) as the active component of the sample.

12. Referenced documents

• GB 7544-92 Technical requirements and sampling methods for condoms
• SH 0004 Solvent naphtha for rubber industry

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