NB/SH/T 0861-2013 Determination of pentane insolubles Membrane filtration method

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Card type: Test method

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

• Standard number: NB/SH/T 0861—2013
• Chinese name: Determination of pentane insolubles Membrane filtration method
• English name: Standard test method for pentane insolubles by membrane filtration
• Replacement relationship: not provided in the available source (the foreword only states "adopted by the redrafting method with modification from ASTM D4055-04 (2009)", and does not mention replacing any national standard)
• Adoption relationship: adopted by the redrafting method with modification from ASTM D4055-04 (2009) "Determination of pentane insolubles by membrane filtration method"
• Publication/implementation: published on 2013-06-08, implemented on 2013-10-01
• Issuing body: National Energy Administration
• Secretariat: Petroleum Fuels and Lubricants Subcommittee of the National Technical Committee for Standardization of Petroleum Products and Lubricants (SAC/TC280/SC1)
• Drafting organization: Dalian Lubricant Research and Development Center of PetroChina Company Limited; participating drafting organization: Lubricant Research and Development (Shanghai) Center of China Petroleum & Chemical Corporation
• Main drafters: Yu Bing, Meng Kuihua, Yang Lijun

2. Scope of application and non-applicability

• 1.1 applies to the determination of pentane insolubles with particle size exceeding 0.8 μm in new and used lubricating oils.
• Note (1.1): Pentane insolubles with particle size smaller than 0.8 μm may be determined using a filter membrane of appropriate pore size; this method can determine pentane insolubles with a studied particle size greater than or smaller than 0.8 μm, but the precision of this standard was established using only a filter membrane with pore size 0.8 μm.
• 1.2 This standard uses International System of Units (SI) units.
• 1.3 Use may involve hazardous materials, operations and equipment, but this standard does not purport to address all of the safety problems associated with its use; it is the responsibility of the user before use to establish appropriate safety and protective measures and to determine the applicability of relevant regulatory limitations. For specific warning statements see Chapter 7, 8.2.1 and Annex A.
• Non-applicability: no explicit "non-applicability" clause is provided in the available source (only the note to 11.1.2 states that the pentane insolubles determined by this method are not suitable for comparison of results between different laboratories).

3. Method principle

• 4.1 In a volumetric flask, mix a sample of new or used lubricating oil with n-pentane. The oil solution is filtered through a 0.8 μm filter membrane filter. The flask, funnel and filter are rinsed with additional n-pentane so that the particulate matter is completely transferred onto the filter. The filter membrane and the particulate matter on it are dried and weighed to obtain the pentane insolubles content.
• Chapter 5 Significance and use: pentane insolubles with particle size above 0.8 μm may cause increased wear and lead to premature failure of equipment used under severe conditions.

4. Reagents and materials (purity / preparation)

• n-Pentane: analytical reagent grade or higher reagent purity (see the reagent entry in 6.x in the source text, source-text extraction number incomplete, requires confirmation against the source standard (source-text extraction)).
• Filter membrane: mixed cellulose ester microporous filter membrane, diameter 47 mm, white (6.1, source-text extraction partially incomplete, requires confirmation against the source standard (source-text extraction)).
• Desiccant: calcium chloride or other desiccant (6.x, source-text extraction number incomplete, requires confirmation against the source standard (source-text extraction)).
• Filtered n-pentane: used for rinsing the filter membrane and washing the volumetric flask and funnel (8.2.1, 8.3.2, 8.3.3).
• Specific preparation method: not provided in the available source (n-pentane is a reagent used directly, with no preparation clause).

5. Apparatus and equipment

(Chapter 6, source-text extraction numbering and text are largely incomplete; the following is the discernible content, requires confirmation against the source standard (source-text extraction))

• 6.1 Mixed cellulose ester microporous filter membrane
• 6.2 Borosilicate glass filter
• 6.3 Borosilicate glass filter (funnel, text incomplete, requires confirmation against the source standard (source-text extraction))
• 6.4 Tweezers: toothless
• 6.x Wash bottle: filled with (n-pentane, text incomplete, requires confirmation against the source standard (source-text extraction))
• 6.6 Analytical balance: sensitivity at least 0.1 mg (the balance sensitivity is unclear in the source transcription; verify this specification against the original before use); Note: use of an antistatic component is recommended
• 6.x Oven
• 6.x Aluminum weighing pan: diameter about 60 mm
• 6.x Desiccator: containing calcium chloride or other desiccant
• 6.x Shaker (mechanical shaker)
• 6.11 to 6.13 entries text incomplete, requires confirmation against the source standard (source-text extraction)
• Note (8.3.4): For weighing of insolubles less than 0.001 g, the use of a semi-microbalance with a sensitivity of 0.01 mg is recommended.

6. Recommended operating conditions

• Filtration vacuum degree: 34 kPa ± 6.67 kPa (8.3.2)
• Filter membrane drying: oven drying for at least 30 min (8.2.2, 8.3.4)
• Cool in desiccator for about 30 min before weighing (8.2.3)
• Weighing accuracy: weigh to 0.1 mg (8.2.3, 8.3.4)
• Shaking: shake on a mechanical shaker for at least 70 min (8.1.2)
• Other conditions (such as oven temperature): not provided in the available source (source-text extraction incomplete, requires confirmation against the source standard (source-text extraction))

7. Sampling and sample preparation

• 8.1.1 Sampling clause text incomplete, requires confirmation against the source standard (source-text extraction).
• 8.1.2 If (the sample, text incomplete) is in the original container (heat to a certain temperature, temperature value source-text extraction incomplete, requires confirmation against the source standard (source-text extraction)) ℃, shake on a mechanical shaker for at least 70 min, so that the insolubles are uniformly (suspended), and weigh the sample as soon as possible.
• Note (8.1.2): If the sample is not prepared as specified, it is difficult to obtain good test precision.
• 8.1.3 Weigh (a certain amount, source-text extraction incomplete, requires confirmation against the source standard (source-text extraction)) g representative (sample). To prevent clogging of the filter membrane, some samples may require a smaller sample amount. If during the test 100 mL sample mixture (liquid) cannot pass through the filter membrane within 2 min, then abandon this (test), and reduce the sample amount in the following order (±10%) and retest: 0.80, 0.64, 0. (51, source-text extraction incomplete), 0.33, 0.26, 0.21, 0.17, 0.13, 0.11, 0.09, 0.07, 0.05, 0.04, 0.03, 0.02 (g). Note: A suitable sample amount is particularly important.
• 8.1.4 Filter through a 0.8 μm filter membrane (fixed amount, text incomplete, requires confirmation against the source standard (source-text extraction)).
• Sampling references: GB/T 4756 "Standard Practice for Manual Sampling of Petroleum Liquids", SY/T 5317 "Standard Practice for Automatic Sampling of Petroleum Liquids in Pipelines" (see Chapter 2).

8. Analytical procedure

• 8.2 Prepare filter membrane
  • 8.2.1 Rinse the filter membrane with filtered n-pentane 100 mL, and place the appropriate side up (see 8.2.1.1) separately into each aluminum weighing pan. Warning: see Chapter 7.
  • 8.2.1.1 Important note: If the (cutting/placement direction, text incomplete, requires confirmation against the source standard (source-text extraction)) of the filter membrane is reversed during the test, the test result is invalid.
  • 8.2.2 Place the aluminum weighing pan into the oven (text incomplete)... take out and place into the desiccator, confirm (determine/cool, text incomplete)... dry for at least 30 min... after drying is completed... (avoid inhaling) hydrocarbon vapors.
  • 8.2.3 When the filter membrane mass (is stable, text incomplete), (cool for about 30 min) weigh the filter membrane mass, weighing to 0.1 mg. Keep in the desiccator for later use.
  • 8.2.4 Place the filter membrane and (aluminum weighing pan, text incomplete)... take the aluminum weighing pan out of the oven (text incomplete).
• 8.3 Filtration
  • 8.3.1 Use tweezers to take the filter membrane out of the aluminum weighing pan and place it in the center of the filtration apparatus, and install the funnel clamp.
  • 8.3.2 Fill the volumetric flask containing the sample with filtered n-pentane to the 100 mL mark. Cap and shake well. Immediately filter the mixture under a vacuum of 34 kPa ± 6.67 kPa. Rinse the volumetric flask twice with a small amount of filtered n-pentane. Pour the rinse liquid along the funnel wall into the filter funnel. Rinse the wall of the filter funnel with a small stream of n-pentane from the wash (bottle).
  • 8.3.3 Remove the clamp and funnel. Rinse the insolubles adhering to the funnel wall onto the filter membrane with n-pentane from the wash bottle. Carefully rinse the filter membrane with n-pentane from the wash bottle, especially the edge portion of the filter membrane. If the insolubles are not completely transferred onto the filter membrane, the test should be redone.
  • 8.3.4 Under the same (vacuum conditions, text incomplete), carefully remove the filter membrane with tweezers, place it in the (weighing) pan originally used, which has been oven-dried and desiccator-cooled in 8.2.2, place it into the oven to dry according to the procedure in 8.2.2, then transfer to a desiccator to cool. Weigh the filter membrane mass, accurate to 0.1 mg.
  • Note (8.3.4): For weighing of insolubles less than 0.001 g, the use of a semi-microbalance with a sensitivity of 0.01 mg is recommended.

9. Qualitative and quantitative determination and calculation formula

• Calculate the pentane insolubles content in oil by the membrane filtration method, w (mass fraction):
  • Pentane insolubles, % = 100 (M₂ − M₁) / (sample mass, symbol source-text extraction incomplete, requires confirmation against the source standard (source-text extraction))... (Equation 1)
  • Where: M₁ — initial mass of the filter membrane, g; M₂ — final mass of the filter membrane and insolubles, g; (the denominator is the sample mass, symbol source-text extraction incomplete, requires confirmation against the source standard (source-text extraction)).
• Reporting expression (10.1): pentane insolubles (0.8 μm) mass fraction, %.
• 10.2 Some new oils require determination of a baseline value (that is, the blank determination value may not be zero).

10. Precision

• 11.1 Judge the (acceptability, text incomplete) of test results according to the following provisions (confidence level of 95%).
• 11.1.1 Repeatability (r): In the same laboratory, by the same operator, using the same apparatus, according to the same test method, the difference between two consecutive test results obtained on the same test sample shall not exceed the requirement of formula (2): (formula 2 content source-text extraction incomplete, requires confirmation against the source standard (source-text extraction)). Where: X—— the average of the two results.
• 11.1.2 Reproducibility (R): By different operators, in different laboratories, using different apparatus, with the same method, the difference between two single, independent test results obtained on the same test sample shall not exceed the requirement of formula (3): R = 0.759X^0.23 (formula 3, exponent source-text extraction doubtful, requires confirmation against the source standard (source-text extraction)). Where: X—— the average of the two results.
• Note (11.1.2): The interlaboratory precision (reproducibility) of this standard is very poor; therefore, the pentane insolubles determined by this method are not suitable for comparison between results from different laboratories.
• 11.2 Bias: Since pentane insolubles are defined only in this standard, this method has no bias.

11. Report

• 10.1 Report the membrane filtration method pentane insolubles content as follows: pentane insolubles (0.8 μm) mass fraction, %.
• 10.2 Some new oils require determination of a baseline value (that is, the blank determination value may not be zero).
• Other reporting elements (such as test date, apparatus, sample amount, etc.): not provided in the available source.

12. Normative references

• GB/T 514 Specification for glass liquid thermometers for petroleum product testing
• GB/T 4756 Manual sampling of petroleum liquids (GB/T 4756—1998, eqv ISO 3170:1988)
• SY/T 5317 Automatic sampling of petroleum liquids in pipelines (SY/T 5317—2006, ISO 3171:1998, IDT)
• Terms and definitions (Chapter 3): 3.1 pentane insolubles of used oil; 3.2 used oil
• Annex A (normative annex) Warning: A.1 n-pentane (extremely flammable liquid, vapor may cause flash fire; keep away from heat, sparks and open flames; keep container closed; ensure adequate ventilation; avoid vapor accumulation, eliminate all ignition sources, especially non-explosion-proof electrical equipment and heaters; avoid prolonged inhalation of vapor or mist; avoid prolonged or repeated skin contact)

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