SH/T 0660-1998 Test method for vapor phase rust preventive oil

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Card type: Test method

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

• Standard number: SH/T 0660-1998
• Chinese name: Test method for vapor phase rust preventive oil
• English name: Test methods for volatile preservative oils
• Replacement relationship: not provided in the available source (no replacement of any standard is mentioned)
• Adoption relationship: equivalently adopts Japanese Industrial Standard JIS K2246-1994 "Rust preventive oil", Article 5.11 "Hydrocarbon solubility test method", Article 5.25 "Volatile matter content test method", Article 5.30 "Acid neutralization test method", Article 5.39 "Vapor phase rust prevention test method", Article 5.40 "Vapor phase rust prevention test method after exposure", and Article 5.41 "Vapor phase rust prevention test method after heating"
• Approval/implementation: approved by China Petrochemical Corporation 1998-06-23, implemented on 1998-12-01; (confirmed in 2004)
• Responsible unit: Research Institute of Petroleum Processing, China Petrochemical Corporation
• Drafting units: Research Institute of Petroleum Processing, China Petrochemical Corporation; Suzhou Special Oil Products Plant
• Main drafters: Long Huali, Fan Hanmei, Bo Yanhong, Hu Peihua, Zhi Rongjuan
• Main differences from JIS K2246-1994 (the source lists 3 items):
  1. Part Two "Determination of volatile matter content": in addition to the container specified in JIS, the sample container may also use an evaporation dish for ash determination conforming to SH/T 0317; the heating device has been supplemented with a cooling reflux system.
  2. Part Three "Acid neutralization test method": JIS 5.30 specifies that the test piece and its preparation follow JIS 5.3.1 and 5.3.2, whereas this standard specifies that they follow SH/T 0218.
  3. Parts Four, Five and Six: when washing the test specimen, JIS specifies methanol, whereas this standard changes it to anhydrous ethanol.

2. Scope of application and non-applicability

• This standard specifies test methods for hydrocarbon solubility, volatile matter content, acid neutralization, vapor phase rust prevention, vapor phase rust prevention after exposure, and vapor phase rust prevention after heating of vapor phase rust preventive oil.
• This standard applies to vapor phase rust preventive oil.
• Not applicable: not provided in the available source.

3. Method principle

This standard is divided into six parts; the method summary of each part is as follows:

• Part One Hydrocarbon solubility test method: place the sample solution whose precipitation value has been determined according to SH/T 0215 at 23℃±3℃ and let it stand for 24h, then observe whether phase change and separation occur. Note: phase change refers to turbidity, gelation, etc.
• Part Two Determination of volatile matter content: place a certain amount of sample on a boiling water bath and heat it; based on the mass change of the sample before and after heating, calculate its volatile matter content.
• Part Three Acid neutralization test method: immerse a test piece coated with hydrobromic acid solution into the sample for 1min, lift it out, and then place it under the conditions of 23℃±3℃ for 4h to evaluate the acid neutralization performance of the sample.
• Part Four Vapor phase rust prevention test method: in a closed container containing the test specimen, place the sample and glycerol solution, maintain under the conditions of 20℃ for 20h, then cool the test specimen so that frost forms on its surface. After 3h, observe whether corrosion occurs on the test specimen.
• Part Five Vapor phase rust prevention test method after exposure: subject the sample maintained under the conditions of 23℃ for 7d to the vapor phase rust prevention test according to Part Four, to examine the vapor phase rust prevention performance of the sample after exposure.
• Part Six Vapor phase rust prevention test method after heating: subject the sample maintained under the conditions of 65℃ for 7d to the vapor phase rust prevention test according to Part Four, to examine the vapor phase rust prevention performance of the sample after heating.

4. Reagents and materials (purity / preparation)

Part One Hydrocarbon solubility test method

• Material: precipitation solvent, specifications are shown in Table 1. Note: it may be prepared by blending petroleum ether with an appropriate amount of benzene.

Table 1 Specifications of precipitation solvent

Part Three Acid neutralization test method

• 15.1 Reagents
  • 15.1.1 Hydrobromic acid: analytical reagent, hydrobromic acid (HBr) content not less than 40.0%(m/m).
  • 15.1.2 Anhydrous ethanol: chemical reagent.
  • 15.1.3 Petroleum ether: 60～90℃, analytical reagent.
  • 15.1.4 Solvent naphtha: meets the requirements of SH 0004.
• 15.2 Materials
  • 15.2.1 Metal test piece: meets the test piece specifications of B in the method of SH/T 0218 A.
  • 15.2.2 Abrasive material: corundum abrasive cloth or abrasive paper of grit 100.
• 16.2 0.1%±0.01%(m/m) Preparation of hydrobromic acid solution: determine the actual concentration of the hydrobromic acid used for the test according to GB/T 621, then weigh an appropriate amount of hydrobromic acid, prepare with distilled water a hydrobromic acid solution of concentration 0.1%±0.01%(m/m), shake thoroughly, store sealed, and set aside. Note: hydrobromic acid is toxic; use it in a fume hood.

Part Four Vapor phase rust prevention test method

• 21.1 Reagents
  • 21.1.1 Anhydrous ethanol: chemical reagent.
  • 21.1.2 Acetone: analytical reagent.
  • 21.1.3 Glycerol: analytical reagent, prepared with distilled water into a glycerol solution of 35%(m/m).
• 21.2 Materials
  • 21.2.1 Aluminum tube: seamless aluminum tube of aluminum or aluminum alloy, outer diameter 16mm, inner diameter 13mm, length 114mm.
  • 21.2.2 Rubber tube.
  • 21.2.3 Test specimen: SGD3 or GB/T 699 high-quality carbon structural steel as specified in JIS G3108 (chemical composition, carbon: 0.15%～0.20%, manganese: 0.30%～0.60%, sulfur: below 0.045%, phosphorus: below 0.045%), diameter 16mm, length 13mm, with a hole at one end whose diameter and depth are respectively 9.5mm.
  • 21.2.4 Metallographic abrasive paper: grit 320 or W40(40～37μm).
  • 21.2.5 Solvent: solvent naphtha meeting the specifications of SH 0004.

Part Five Vapor phase rust prevention test method after exposure

• 27.1 Reagents: according to the provisions of Article 21.1 of Part Four.
• 27.2 Materials: according to the provisions of Article 21.2 of Part Four.

Part Six Vapor phase rust prevention test method after heating

• 33.1 Reagents: according to the provisions of Article 21.1 of Part Four.
• 33.2 Materials: according to the provisions of Article 21.2 of Part Four.

5. Instruments and equipment

Part One Hydrocarbon solubility test method

• Centrifuge tube: meets the requirements of 3.1 in SH/T 0215.

Part Two Determination of volatile matter content

• 9.1 Heating device: an electric thermostatic water bath with a mouth diameter of 50mm, with a condenser connected at its thermometer insertion port so that vapor is cooled and refluxed.
• 9.2 Container: a glass evaporation dish with an outer diameter of 70mm (see Figure 1 or Figure 2) or an evaporation dish for ash determination conforming to SH/T 0317.
• 9.3 Desiccator: place silica gel desiccant inside.
• Figure 1 Round-bottom evaporation dish, Figure 2 Flat-bottom evaporation dish (dimension labels: 07012, 070±2, unit mm, requires confirmation against the source standard (source-text extraction)).

Part Three Acid neutralization test method

• 14.1 Test piece hook: made of stainless steel wire with diameter 1mm.
• 14.2 Test piece rack: a suitable rack capable of suspending the test piece vertically.
• 14.3 Beaker: 500mL.
• 14.4 Blower: dual-purpose hot and cold.
• 14.5 Desiccator: place silica gel desiccant inside.

Part Four Vapor phase rust prevention test method

• 20.1 Stoppered wide-mouth bottle: 1000mL.
• 20.2 Glass container: glassware with inner diameter 45mm and height not more than 20mm.
• 20.3 Magnifying glass: magnification about 5 times.
• 20.4 Rubber stopper: No. 11 and No. 23, with a hole of diameter about 15mm in the center.
• 20.5 Constant-temperature air bath: capable of accommodating more than four groups of test bodies and capable of maintaining 20℃±2℃.

Part Five Vapor phase rust prevention test method after exposure

• 26.1 Culture dish: diameter 120mm.
• 26.2 Other instruments are according to the provisions of Article 20 of Part Four.

Part Six Vapor phase rust prevention test method after heating

• 32.1 Sample bottle: outer diameter about 40mm, height about 140mm.
• 32.2 Other instruments are according to the provisions of Article 20 of Part Four.

6. Recommended operating conditions

• Part One: standing temperature 23℃±3℃, standing time 24h.
• Part Two: boiling water bath heating 2h; distance from the bath liquid surface to the bottom of the container 20mm～40mm; cooling in desiccator 30min.
• Part Three: sample temperature 23℃±3℃; test piece immersed in acid 1s; immersed in sample and repeatedly dipped and lifted 12 times within 1min; standing 4h.
• Part Four: constant-temperature air bath 20℃±2℃, maintained for 20h; cold water temperature 2.0℃±0.5℃; cooling 3h; relative humidity adjusted to 90% (place 10mL 35%(m/m) glycerol solution in the glass container).
• Part Five: 23℃±3℃ exposure 7d.
• Part Six: 65℃±1℃ maintained for 7d, then cooled to room temperature.

7. Sampling and sample preparation

Part One

• 6.1 At room temperature, add sample 10mL to two clean and dry centrifuge tubes, dilute with precipitation solvent to 100mL, then determine the precipitation value according to SH/T 0215.

Part Two

• 10.1 Wash the container, dry it, and cool it to room temperature in a desiccator.
• 10.2 Take the above two containers, and respectively weigh about 5g of sample, accurate to 0.001g.

Part Three

• 16.1 Preparation of test pieces: proceed according to SH/T 0218 Part One, Chapter 6 “Preparation of test pieces”, but the abrasive material is selected as 100 grade corundum abrasive cloth or abrasive paper, grinding out a new ground surface; there is no specific requirement for roughness.

Part Four

• 22.1 Grinding: use metallographic abrasive paper to grind the non-porous ends of three test specimens; place the metallographic abrasive paper on a glass plate, grind back and forth ten times, then rotate 90° and grind ten times (note: the edge portions of the specimens also need to be polished until free of rust).
• 22.2 Cleaning: immerse the ground test specimens successively in solvent naphtha, anhydrous ethanol, and acetone, each time using gauze to wipe off contaminants on the ground surface, until there is no contaminant on the gauze used for wiping.
• 22.3 Storage: when the test is not to be performed immediately, the test specimens should be stored in a dry container. However, test specimens stored for more than 8h must be reground.

Part Five

• 28 Preparation of test specimens: proceed according to Part Four, Article 22.

Part Six

• 34 Preparation of test specimens: proceed according to Part Four, Article 22.

8. Analytical Procedure

Part One Hydrocarbon Solubility Test Method

• 6.1 At room temperature, add sample 10mL to two clean and dry centrifuge tubes, dilute with precipitation solvent to 100mL, then determine the precipitation value according to SH/T 0215.
• 6.2 Allow the sample solution after the above precipitation value determination to stand at 23℃±3℃ for 24h.
• 6.3 Visually inspect the sample solution in the centrifuge tubes for phase change and separation phenomena.

Part Two Determination Method for Volatile Matter Content

• 10.1 Wash and dry the container, and cool it to room temperature in a desiccator.
• 10.2 Take the above two containers, and respectively weigh about 5g of sample, accurate to 0.001g. Place them on a boiling water bath and heat for 2h; during the test, adjust the distance from the bath liquid surface to the bottom of the container to 20mm～40mm.
• 10.3 Remove the container containing the sample from the water bath, wipe off moisture on the outside of the container with a clean dry cloth, place it in a desiccator to cool for 30min.
• 10.4 Remove the container from the desiccator and weigh it, accurate to 0.001g.

Part Three Acid Neutralization Test Method

• 17.1 Pour 500mL of sample into a beaker, and keep its temperature at 23℃±3℃.
• 17.2 Suspend the three prepared test pieces with hooks, immerse them in 500mL hydrobromic acid solution of concentration 0.1%±0.01%(m/m) for 1s. Observe the acid immersion condition of the test pieces; if a test piece does not wet with acid, then this test piece cannot be used for the test.
• 17.3 Immediately immerse the test pieces treated by 17.2 vertically into the sample prepared according to 17.1, and gently swing back and forth 2～3 times.
• 17.4 Within 1min, repeatedly immerse and lift the test pieces 12 times, then hang the test pieces on the test piece hanger. Place under 23℃±3℃ conditions for 4h.
• 17.5 Use solvent naphtha, petroleum ether, and anhydrous ethanol in sequence to wash off the sample and acid solution adhering to the test pieces, and finally dry them with hot air.
• 17.6 Visually observe whether there is rust, spots, stains, discoloration, etc. within the evaluation area of 50mm×50mm in the middle of the test piece.

Part Four Vapor Phase Rust Prevention Test Method

• 23.1 Insert the perforated end of the test specimen into a 11 grade rubber stopper with a hole of diameter about 15mm at the central part, with an insertion depth of 9.5mm±0.5mm (see Figure 3).
• 23.2 Pass the aluminum tube through the center of the 23 grade rubber stopper, with equal lengths exposed at both ends; insert one end of the aluminum tube below the rubber stopper into the 11 grade rubber stopper until it touches the test specimen mounted on the 11 grade rubber stopper (see Figure 3). When installing the test specimen, do not contaminate it with fingerprints or other contaminants.
• 23.3 On the side of the test specimen, fit a rubber tube over the aluminum tube between the 11 grade and 23 grade rubber stoppers. In addition, fit another 11 grade rubber stopper onto the aluminum tube protruding in the opposite direction.
• 23.4 Place 25mL of sample at the bottom of a wide-mouth bottle with a stopper; in order to adjust the relative humidity to 90%, place 10mL of glycerol solution of concentration 35%(m/m) in a glass container, and use the 23 grade rubber stopper equipped with the test specimen as the stopper to constitute the test assembly (see Figure 4).
• 23.5 Place the test assembly in a constant-temperature air bath maintained at 20℃±2℃; after 20h, fill the aluminum tube with cold water at 2.0℃±0.5℃.
• 23.6 After 3h, remove the test specimen and drain the water from the aluminum tube.
• 23.7 Use a magnifying glass to observe the ground portion of the test specimen, and observe whether rust occurs.
• 23.8 Simultaneously conduct a blank test without adding sample; if no rust occurs in the blank test, the test conditions should be checked, and the test should be redone.

Part Five Vapor Phase Rust Prevention Test Method After Exposure

• 29.1 Place about 120mL of sample in a culture dish, without covering the lid, and expose at 23℃±3℃ for 7d.
• 29.2 Subject the exposed sample to the vapor phase rust prevention test according to Part Four, Article 23.

Part Six Vapor Phase Rust Prevention Test Method After Heating

• 35.1 Place about 120mL of sample in a sample bottle, stopper it tightly, keep at 65℃±1℃ for 7d, then cool to room temperature.
• 35.2 Subject this sample to the vapor phase rust prevention test according to Part Four, Article 23.

9. Qualitative and Quantitative Determination and Calculation Formulas

Part One Result Judgment (Article 7)

• When neither of the sample solutions in the two centrifuge tubes shows phase change or separation, it can be judged as “no phase change, no separation”; if one of the two centrifuge tubes shows phase change or separation, redo the test. If in the redone test one or more (including one) of the two centrifuge tubes still shows phase change or separation, it can be judged as “phase change, separation”.

Part Two Calculation (Article 11)

The volatile matter content of the sample X[% (m/m)] is calculated according to formula (1):

X = (m₁ − m₂) / m₁ × 100

Where:

• m₁ —— mass of sample before heating, g;
• m₂ —— mass of sample after heating, g.

(Note: the original source-text extraction formula is typeset as “x[unreadable sign]m = m2 x 100 / m ,”, which has been arranged according to context and requires confirmation against the source standard (source-text extraction).)

Part Two Report (Article 12)

• Take the average of the two determination results as the determination result of the volatile matter content of the sample, and round to 0.1%(m/m).

Part Three Result Judgment and Report (Article 18)

• 18.1 When none of the evaluation areas of the three test pieces shows rust, spots, or stains, report as “qualified”.
• 18.2 When one of the three test pieces shows rust, spots, or stains in its evaluation area, the test should be redone. If the retest result still shows rust, spots, or stains in the evaluation areas of one or more (including one) test pieces, report as “unqualified”.

Part Four Result Judgment (Article 24)

• This test is conducted simultaneously with three test specimens. If two or more (including two) of the three test specimens rust, it is judged as rusting; if one of the three test specimens rusts, the test should be redone. When after the redone test one or more (including one) test specimens show rust, it is judged as rusting.

Part Five Result Judgment (Article 30)

• According to Part Four, Article 24.

Part Six Result Judgment (Article 36)

• According to Part Four, Article 24.

10. Precision

• Not provided in the available source (only Part Two, Article 12 specifies taking the average of two determination results and rounding to 0.1%(m/m); no precision limit is given).

11. Report

• Part Two: take the average of the two determination results as the determination result of the volatile matter content of the sample, and round to 0.1%(m/m).
• Part Three: report “qualified” or “unqualified” according to Article 18.
• Part One, Part Four, Part Five, Part Six: the original text does not separately list a “Report” clause; the results are expressed as judgment conclusions (see Section 9).

12. Normative References

The provisions of the following standards, through reference, constitute a part of this standard. Unless otherwise explicitly specified in the standard, the following referenced standards shall all be currently effective standards.

• GB/T 262 Petroleum products — Determination of aniline point
• GB/T 621 Hydrobromic acid (the original source-text extraction is written as “[garbled hydrobromic-acid name]”, requires confirmation against the source standard (source-text extraction))
• GB/T 699 Technical conditions for high-quality carbon structural steel
• GB/T 1884 Crude petroleum and liquid petroleum products — Laboratory determination of density (hydrometer method)
• GB/T 1885 Petroleum measurement tables
• GB/T 6536 Petroleum products — Determination of distillation
• SH 0004 Solvent naphtha for the rubber industry
• SH/T 0215 Determination of precipitation value and wear properties of rust-preventive oils and greases
• SH/T 0218 Preparation method of test pieces for rust-preventive oils and greases
• SH/T 0317 Technical conditions for acceptance of porcelain utensils for petroleum product testing
• JIS G3108 General steel for grinding rod steel

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 for Questions and Answers