SH/T 0065-1991 Sampling of engine coolant or rust inhibitor test samples and preparation of their aqueous solutions

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Card type: Test method

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

• Standard number: SH/T 0065-91 (the original text notes "(confirmed in 200())", requires confirmation against the source standard (source-text extraction))
• Chinese full title: Sampling of engine coolant or rust inhibitor test samples and preparation of their aqueous solutions
• English name: not provided in the available source
• Replacement relationship: not provided in the available source
• Reference adoption: partial content of American Society for Testing and Materials standard ASTM D1176-71(89) "Sampling of engine coolant or rust inhibitor test samples and preparation of their aqueous solutions" and ASTM D4725-87 "Standard Terminology for Engine Coolants" (see "Additional Notes")
• Approval/implementation: approved by China Petrochemical Corporation 1991-06-28, implemented on 1992-07-01

2. Scope of application and non-applicability

• Scope of application: This standard specifies the sampling of engine coolant or rust inhibitor test samples and the preparation method of their aqueous solutions; it is applicable to taking representative engine coolant, engine coolant concentrate, or rust inhibitor from original containers.
• Non-applicability: no explicit non-applicability clause is provided in the available source.
• Note: For the handling method of solid rust inhibitors, see Appendix A (supplementary provision).

3. Method principle

No centralized statement of the principle chapter is provided in the available source. The operational points that can be summarized from the main text are: bring the sample temperature to room temperature and mix uniformly (by stirring, hand shaking, or rolling), and take a representative sample with a pipette or by siphon method; multiphase coolants are sampled after standing separation in a separatory funnel; the preparation of aqueous solutions is expressed as the ratio of the initial volume of the concentrate to the final volume of the aqueous solution at 20 ℃ (volume percentage), and may be prepared by the gravimetric method or the volumetric method.

4. Reagents and materials (purity / preparation)

• Distilled water: used for dilution (5.1.4, 5.2.3).
• Corrosive water: a standard solution containing sulfate ions, chloride ions, and bicarbonate ions each at 100 ppm, added to distilled water in the form of sodium salts (2.4).
• Filter paper: used for suction filtration of suspended solids (4.6).
• Purity grade and other reagent specifications: not provided in the available source.

5. Instruments and equipment

• Stirrer (3.1.3, 3.1.4); an induction motor without brushes or an air motor may be selected to ensure the safe use of flammable liquids (3.1.4 note).
• Pipette (3.1.5, 5.2.2).
• Separatory funnel (4.1, 4.5).
• Volumetric flask (5.1.4, 5.2.2, 6.1 note).
• Beaker (5.1.3, A2).
• Constant-temperature bath: 20 ℃ ± 0.1 ℃ (5.1.5, 5.2.1, 5.3).
• Precision thermometer (5.1.5 note).
• Balance: weighing accurate to ±0.02% of the required mass (5.1.3); in Appendix A, accurate to 0.02% of the weighed sample mass (A2).
• Density measuring apparatus: accurate to 0.0005 g/mL (5.1.1).
• Clean, dry, transparent glass container with a lid (3.2.2, 3.2.6).
• Other specific models and specifications: not provided in the available source.

6. Recommended operating conditions

• Sampling temperature: bring the coolant and its container to room temperature (not lower than 20 ℃) (3.1.1, the original text "not lower than 2090" requires confirmation against the source standard (source-text extraction)).
• Stirring time: start the stirrer for 5 min (3.1.4, the original text "5n in" requires confirmation against the source standard (source-text extraction)).
• Standing of multiphase samples: at least 16 h (4.1, the original text "l6ha" requires confirmation against the source standard (source-text extraction)).
• Aqueous solution preparation temperature: 20 ℃ ± 0.1 ℃ (5.1.5, 5.2.1, 5.3).
• Density measurement temperature: 20 ℃ (5.1.1).
• Other conditions: not provided in the available source.

7. Sampling and sample preparation

7.1 Direct sampling from original containers (3.1)

• 3.1.1 Bring the temperature of the coolant and its container to room temperature (not lower than 20 ℃).
• 3.1.2 Shake the container to mix the coolant in the container uniformly.
• 3.1.3 Open the lid and insert the stirrer.
  • a. For transparent glass containers with lids or opaque containers, the lid may be opened directly and the stirrer inserted.
  • b. For metal containers without an openable lid, drill two holes in the top of the container and enlarge one of them to allow insertion of the stirrer.
• 3.1.4 Start the stirrer for 5 min to ensure that a uniform mixture can be obtained. Note: An induction motor without brushes or an air motor may be selected to ensure the safe use of flammable liquids.
• 3.1.5 While stirring, take a representative sample with a pipette or by siphon method.
• 3.1.6 When there is no electric stirring, sampling may be carried out by hand shaking. For small packages of coolant, shake vigorously to mix the solution uniformly, then while shaking, take a representative sample by siphon method. However, samples taken under hand shaking cannot be used for arbitration tests.
• 3.1.7 For coolant in large metal drums, the drum may be rolled to mix the coolant uniformly, then immediately stand the metal drum upright and take a sample by siphon method as soon as possible.

7.2 Transfer sampling from original containers (3.2)

• 3.2.1 If the coolant product is contained in a metal container or an opaque glass container, transfer the sample to a transparent glass container with a lid when necessary to facilitate observation during sampling.
• 3.2.2 Stir the coolant as in 3.1.1—3.1.4, then remove the stirrer and immediately transfer the coolant to a clean, dry, transparent glass container with a lid, draining the coolant from the original container as completely as possible. Leave a certain space in the glass container to allow for thermal expansion of the liquid during storage. Note: For metal drums of 20 L or more, it is not necessary to transfer all the coolant, but the representativeness of the transferred sample must be ensured. For single-phase products, after thorough mixing, the coolant is usually drawn by siphon method.
• 3.2.3 Inspect the original container to determine whether the transfer of coolant is complete.
• 3.2.4 If the coolant in the original container has not been completely transferred, pour back a small amount of the transferred coolant, stir thoroughly in the original container to mix, and then pour the coolant together into the glass container.
• 3.2.5 Sample from the glass container as in 3.1.5 and 3.1.6.
• 3.2.6 When not in use, the glass container should be stored in a cool, dry place to prevent sunlight exposure from causing deterioration of the coolant; except during sampling, the lid should be kept tightly closed to prevent evaporation or absorption of moisture.

7.3 Separation of multiphase coolants (Chapter 4)

• 4.1 When the coolant stratifies or precipitates solids, place the representative sample obtained according to clause 3.1 or clause 3.2 into a separatory funnel and let stand for at least 16 h.
• 4.2 Draw off the settled solid or liquid while minimizing the amount of the main liquid phase drawn off.
• 4.3 Drain the main liquid phase into a suitable container, taking care not to include any liquid phase floating on the surface.
• 4.4 Finally, place the liquid phase floating on the surface into a separate container.
• 4.5 If the solid cannot be discharged from the separatory funnel, siphon off the various liquid phases successively from the top of the funnel.
• 4.6 If the solid is suspended and not separated from the liquid phase, filter the liquid phase by suction through appropriate filter paper into a storage container, thereby obtaining a representative sample.

7.4 Handling of solid rust inhibitors (Appendix A, supplementary provision)

• A1 For powdered or granular rust inhibitors, samples should be taken from different parts of the container. If they are blocks, open the entire package, mix uniformly, and sample. If necessary, sample by the quartering method. The sample must not contain portions that have caked due to absorption of moisture and carbon dioxide.
• A2 Immediately weigh the sample, accurate to 0.02% of the weighed sample mass. Place the sample in a beaker, dissolve it with the water specified in the test, and after dissolution, quantitatively transfer it to a volumetric flask, and prepare the sample into aqueous solutions of the specified maximum and minimum concentrations according to Chapter 5 or Chapter 6.

8. Analytical procedure

8.1 Preparation of aqueous solutions (Chapter 5)

The concentration of the coolant aqueous solution is expressed at 20 ℃ as the ratio of the initial volume of the concentrate to the final volume of the aqueous solution, generally expressed as a volume percentage. The aqueous solution may be prepared by the gravimetric method or the volumetric method.

8.1.1 Gravimetric method (5.1)

• 5.1.1 Measure the density of the concentrate at 20 ℃, accurate to 0.0005 g/mL.
• 5.1.2 Given the volume of the coolant aqueous solution to be prepared at 20 ℃, calculate the mass of concentrate required.
  • Example: Use a concentrate with a density of 1.0120 g/mL at 20 ℃ to prepare 30%(V/V) aqueous solution 100 mL.
  • The mass of concentrate required is: 0.30 × 100 × 1.0120 = 30.360 (g)
  • This mass must be corrected for buoyancy; the correction value usually used for engine coolant is 0.103 g/100 mL. Therefore, in this example, the corrected mass of concentrate required is: 30.360 − 0.103/100 × 0.30 × 100 = 30.329 (g) (the original text "30.329(8)" requires confirmation against the source standard (source-text extraction)))
• 5.1.3 Accurately weigh the concentrate in a beaker at room temperature, accurate to ±0.02% of the required mass.
• 5.1.4 Pour the weighed concentrate into a volumetric flask, rinse the concentrate in the beaker several times with distilled water or the corrosive water used in the test, collect the rinsings in the volumetric flask, and dilute to near the mark with the specified water above.
• 5.1.5 Invert the volumetric flask several times to mix the aqueous solution uniformly, taking care to avoid loss of solution from the stopper of the volumetric flask. Place the volumetric flask in a 20 ℃ ± 0.1 ℃ constant-temperature bath and keep it for a sufficient time so that the temperature of the solution reaches the bath temperature. Note: The time required for constant temperature varies with the solution and its concentration; this time can be conveniently judged from the temperature of a container holding the same or a similar solution placed in the constant-temperature bath for the same time. The temperature is measured by a precision thermometer inserted in that solution.
• 5.1.6 After the solution reaches the bath temperature, dilute to the mark with the specified water that has been equilibrated at 20 ℃ ± 0.1 ℃. Invert the volumetric flask several times to mix the solution uniformly, then transfer the solution to a container.

8.1.2 Volumetric method (5.2)

• 5.2.1 Place the sample obtained from clause 3.1 or clause 3.2 in a constant-temperature bath at 20 ℃ ± 0.1 ℃.
• 5.2.2 After the sample reaches the bath temperature, use a pipette to draw the required volume of sample and transfer it to a volumetric flask. Note: The volumetric method is only applicable to engine coolants.
• 5.2.3 Dilute with distilled water or the corrosive water used for the test to near the mark. Handle according to 5.1.5 and 5.1.6.

8.1.3 Preparation of aqueous solutions of coolants that exhibit layering or precipitation of solids (5.3)

• Because measuring the density of such samples is relatively difficult, the volumetric method is generally used for preparation. Before drawing the sample, the sample should be brought to 20 ℃ ± 0.1 ℃ in a constant-temperature bath, then handled according to clause 3.1 or clause 3.2 and 5.2.2 and 5.2.3.

8.2 Treatment of a second-phase mixture separated due to dilution with water (Chapter 6)

• 6.1 Sampling is carried out according to 3.1.2—3.1.5. Note: If a second phase separates during preparation of the aqueous solution in a volumetric flask, the entire mixture should be transferred to a stirrable container before sampling.
• 6.2 If the two phases need to be separated, proceed according to Chapter 4.

9. Qualitative and quantitative determination and calculation formulas

• Concentration expression: At 20 ℃, it is expressed as the ratio of the initial volume of the concentrate to the final volume of the aqueous solution, generally expressed as a volume percentage (Chapter 5).
• Gravimetric calculation formula (5.1.2 example):
  • Required mass of concentrate = volume fraction × volume of aqueous solution × 20 ℃ density
  • Mass after buoyancy correction = calculated mass − correction value/100 × volume fraction × volume of aqueous solution
  • Example: 0.30 × 100 × 1.0120 = 30.360 g; 30.360 − 0.103/100 × 0.30 × 100 = 30.329 g
• Other qualitative and quantitative determinations, detection limits: not provided in the available source.

10. Precision

Not provided in the available source.

11. Report

Not provided in the available source.

12. Referenced documents

• ASTM D1176-71(89) "Sampling of test samples of engine coolants or rust inhibitors and preparation of their aqueous solutions" (referenced adoption)
• ASTM D4725-87 "Standard terminology for engine coolants" (referenced adoption, partial content)
• Other referenced standards: not 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-reference Q&A