SH/T 0104-1992 Stability test method for refrigeration oils under the action of refrigerants (Philipp method)

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Card type: Test method

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

• Standard number: SH/T 0104-92
• Chinese full title: Stability test method for refrigeration oils under the action of refrigerants (Philipp method)
• English name: not provided in the available source
• Replacement relationship: not provided in the available source (the source only shows "SH/T 0104-92")
• Reference adoption: Federal German Standard DIN 51593-89 "Test method for stability of refrigeration oils to refrigerants (Philipp method)"
• Approval/implementation: approved by China Petrochemical Corporation 1992-06-06, implemented on 1993-01-01

2. Scope of application and non-application

• Scope of application: This standard specifies the test method for examining the stability of refrigeration oils under the action of refrigerants; it is applicable to refrigeration oils using halogenated hydrocarbons as refrigerants.
• Non-application: not provided in the available source.

3. Method principle

Under specified heating conditions and the vapor action of the refrigerant, after a certain test time, the refrigeration oil is qualitatively tested with silver nitrate-methanol solution for whether a white precipitate is produced.

4. Reagents and materials (purity / preparation)

4.1 Reagents

• 5.1 Silver nitrate: analytical reagent.
• 5.2 Methanol: analytical reagent.
• 5.3 Nitric acid: analytical reagent, prepared as a 20%(m/m) solution.
• 5.4 Ammonia water: analytical reagent.
• 6.2 Preparation of silver nitrate-methanol solution: weigh 0.3 g of silver nitrate, dissolve it in 100 mL of methanol for later use. Before use, add ammonia water to the prepared solution to make it weakly alkaline.
• 7.5 Acidification process: add 2-3 drops of 20%(m/m) nitric acid solution to the silver nitrate-methanol solution.

4.2 Materials

• 4.2.1 Solid carbon dioxide or liquid nitrogen or other coolant.
• 4.2.2 Industrial filter paper.
• 4.2.3 Industrial ethanol.
• 4.2.4 Refrigerant: fluorochloromethane F12 meets the requirements of GB/T 7372, or fluorochloromethane F22 meets the requirements of GB/T 7373.
• 4.2.5 Grinding wheel disc.
• 4.2.6 pH test paper.

5. Instruments and equipment

• 4.1.1 Test apparatus: as shown in Figure 1.
• 4.1.2 Test tube: made of borosilicate glass, outer diameter 9 mm, wall thickness approximately 1.5 mm, on test tube leg A there should be a 70 mm mark, and on test tube leg B there should be a 35 mm mark. The sample inlet of the test tube must have a sealed-off portion, as shown in Figure 2.
• 4.1.3 Aluminum block bath: heating temperature 250℃±5℃ or 175℃±5℃, as shown in Figure 3.
• 4.1.4 Water bath or oil bath: capable of maintaining 40℃±1℃ and 100℃±1℃.
• 4.1.5 Thermometer: 0—300℃; 0—40℃, scale division value 1℃.
• 4.1.6 Glass test tube: volume not less than 5 mL.
• 4.1.7 Syringe: 1 mL, graduation 0.1 mL.
• 4.1.8 Dropping bottle: 50 mL.
• 4.1.9 Cold bath: a vacuum flask that can contain a mixture of industrial ethanol and solid carbon dioxide or liquid nitrogen or other coolant.
• 4.1.10 Vacuum pump.

6. Recommended operating conditions

• Heating temperature: 250℃±5℃ or 175℃±5℃ (aluminum block bath).
• Leg B water bath (or oil bath) temperature: 40℃±1℃.
• Leg A water bath (or oil bath) temperature: 100℃±1℃.
• Vacuum evacuation: under 10—20 Pa, evacuate for 0.5 h.
• Observation interval: every 24 h, observe whether there are condensed droplets shining with silver light in the test tube.
• The liquid levels of the sample and refrigerant in each leg of the test tube are at least 10 mm below the bath liquid surface.
• The test must be conducted in a fume hood equipped with a safety shield.

7. Sampling and sample preparation

• 6.1 The sample is first filtered with industrial filter paper.
• 7.1.1 Use a syringe to take 1 mL of sample and inject it into test tube leg A (if oil droplets contaminate the wall of the sealed-off opening, redo the operation).

8. Analysis procedure

8.1 Sealing of the test tube

• 7.1.1 Use a syringe to take 1 mL of sample and inject it into test tube leg A (if oil droplets contaminate the wall of the sealed-off opening, redo the operation).
• 7.1.2 Place test tube leg A containing the sample into a water bath (or oil bath) at 100℃±1℃, and under a vacuum of 10—20 Pa, evacuate for 0.5 h (see Figure 4 for the schematic diagram of refrigerant collection). Then slowly place it into a cold bath to cool. Turn the three-way stopcock so that the refrigerant condenses into test tube leg A. When the refrigerant in test tube leg A is approximately equal in volume to the sample, lift test tube leg A from the cold bath to vaporize the refrigerant while evacuating. Repeat this three times so that the air in the test tube is completely replaced by refrigerant gas.
• 7.1.3 Then place test tube leg A into the cold bath, turn the three-way stopcock so that the refrigerant condenses into test tube leg A, equal in volume to the sample (total height approximately 70 mm), close the three-way stopcock, lift test tube leg A and place test tube leg B into the cold bath to cool. Distill the refrigerant from test tube leg A to test tube leg B (its height approximately 35 mm). Open the three-way stopcock, and while evacuating, quickly seal the sealed-off opening of the test tube.
• Alternative operation method for this step: directly place test tube leg B that has been purged in 7.1.2 into the cold bath, so that the refrigerant condenses into test tube leg B at 1 mL, with a height of approximately 35 mm. Then seal in the same way as above.
• For arbitration testing, the former method shall prevail.
• Note: During the above operations, a safety shield must be worn.

8.2 Heating and observation

• 7.2 Insert test tube leg A into the heating hole of an aluminum block bath heated to the specified temperature (250℃±5℃ or 175℃±5℃). Then immerse test tube leg B into a water bath (or oil bath) at temperature 40℃±1℃; the liquid levels of the sample and refrigerant in each leg of the test tube are at least 10 mm below the bath liquid surface.
• 7.3 During the test, every 24 h, observe whether there are condensed droplets shining with silver light in the test tube; if present, it is considered that hydrogen halide acid has been generated, and the test shall be carried out according to clause 7.5.
• 7.4 If no condensed droplets shining with silver light are found, the test continues until the time specified by the product specification, and then the test is terminated.
• Note: The test must be conducted in a fume hood equipped with a safety shield.

8.3 Inspection

• 7.5 Slowly place test tube leg B into the cold bath; in the cooled state, use a grinding wheel disc to cut the inclined part in the middle of the test tube into two parts. Quickly use a latex tube to connect a drawn-out thin glass tube to one end of test tube leg B. Insert the thin glass tube into a glass test tube containing 5 mL of freshly acidified silver nitrate-methanol solution [acidification process: add 2-3 drops of 20%(m/m) nitric acid solution to the silver nitrate-methanol solution]. Then judge whether white turbidity or white precipitate is produced.

9. Qualitative and quantitative determination and calculation formula

• Qualitative judgment: use silver nitrate-methanol solution to test whether white turbidity or white precipitate is produced.
• 8.1 If no white turbidity or white precipitate is produced, the refrigeration oil is considered to pass the stability test under the action of the refrigerant; otherwise, it fails.
• 8.2 If two tests of the same sample are inconsistent, the passing result shall be taken as the test result of the sample.
• Calculation formula: not provided in the available source.

10. Precision

Not provided in the available source.

11. Report

The test results shall include the following contents:

• a. Sample name;
• b. Refrigerant name;
• c. Test temperature;
• d. Test time;
• e. Stability test pass or fail.

12. Referenced documents

• GB/T 7372 Industrial dichlorodifluoromethane (F12)
• GB/T 7373 Industrial chlorodifluoromethane (F22)
• Reference adoption: Federal German Standard DIN 51593-89 "Test method for stability of refrigeration oils to refrigerants (Philipp 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