SH/T 0225-1992 Determination of barium content in additives and additive-containing lubricating oils

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Card type: Test method

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

• Standard number: SH/T 0225-92 (confirmed in 2004)
• Chinese title: Determination of barium content in additives and additive-containing lubricating oils
• English title: not provided in the available source
• Supersession relationship: supersedes ZB E60 004-88 (original written as "Z s E60 004-88", requires confirmation against the source standard (source-text extraction))
• First issued: 1961 (original written as "1961)", requires confirmation against the source standard (source-text extraction))
• Reference adoption: partial content of former Soviet Union national standard ГОСТ 13538-68 "Methods for determination of barium, calcium, and zinc content in additives and additive-containing lubricating oils" (original "1'OCI' 13538-6 8", requires confirmation against the source standard (source-text extraction))

2. Scope of application and non-application

• This standard specifies the method for determining the barium content of additives and additive-containing lubricating oils.
• This standard applies to additives and additive-containing lubricating oils.
• Non-applicable scope: not provided in the available source.

3. Method principle

The sample is incinerated to ash, the ash is dissolved in hydrochloric acid, then sulfuric acid is added to precipitate barium from the solution (precipitated as barium sulfate, weighed, and converted to barium content).

4. Reagents and materials (purity / preparation)

• 4.1 Nitric acid: chemically pure.
• 4.2 Hydrochloric acid: chemically pure, diluted with water at volume ratios 1:1 and 1:3 respectively.
• 4.3 Sulfuric acid: chemically pure, diluted with water at volume ratio 1:1.
• 4.4 Barium chloride: chemically pure, prepared as a 100 g/L solution.
• 3.2 Materials: quantitative filter paper, diameter 90～110 mm, slow speed.

5. Apparatus and equipment

• 3.1.1 Apparatus for ash determination.
• 3.1.2 Graduated cylinder: 10 mL.
• 3.1.3 Beakers: 100 mL, 400 mL.
• 3.1.4 Watch glass.
• 3.1.5 Wash bottle: 500 mL.
• 3.1.6 Glass funnel: diameter 50～80 mm.
• 3.1.7 Porcelain crucible: low form, No. 3 or No. 4, or platinum crucible.
• 3.1.8 Test tube: diameter 15～20 mm, length 150～200 mm.
• 3.1.9 Glass rod with both ends fire-polished round: length 150～200 mm, diameter 3～4 mm, with a rubber head.
• Others: high-temperature electric furnace (controllable at 775℃±25℃), desiccator, electric hot plate (covered with asbestos board), oven (105～110℃), analytical balance (weighing accurate to 0.0002 g).

6. Recommended operating conditions

• Ashing temperature: 775℃±25℃.
• Ashing time: 1 h (6.1); barium sulfate ignition 15～20 min (6.5, 6.6).
• Precipitate heating boiling holding time: 5～10 min (6.3).
• Precipitate aging: slightly heat for about 1.5～2 h, or place in a warm place overnight (6.3).
• Washing water temperature: 30～40℃ (6.4).
• Crucible drying temperature: 105～110℃ (5.1).
• Sample preheating temperature (viscous or wax-containing samples): 40～50℃ (5.2).

7. Sampling and sample preparation

• 5.2 Shake the sample in the bottle (its amount should not exceed three-quarters of the bottle volume) for 5 min to mix it uniformly.
• For viscous or wax-containing samples, preheat to 40～50℃ before shaking to mix uniformly.
• 6.1 Weigh additive 5 g, or additive-containing lubricating oil 25 g, into the prepared crucible, both weighed accurately to 0.01 g.
• Note: When determining barium content, the ash obtained after determining the ash content of the sample may also be used for the test.

8. Analytical procedure

• 5.1 Crucible pretreatment: add hydrochloric acid solution (1:3) to the crucible and boil for a few minutes. After pouring out the hydrochloric acid solution, rinse the crucible with distilled water, then place the crucible in an oven at 105～110℃ to dry.
• 6.1 Incinerate the sample to ash according to the ash determination method, and ignite at 775℃±25℃ for 1 h.
• 6.2 Add 10 mL hydrochloric acid solution (1:1) to the crucible with the ash, place on an electric hot plate covered with an asbestos board, and evaporate the solution to nearly dry. Then add 25 mL hydrochloric acid solution (1:1) and heat to dissolve. Then rinse the crucible with distilled water from a wash bottle so that all residual solution in the crucible is washed into a 400 mL beaker.
• 6.3 Add 100 mL distilled water and 10 mL sulfuric acid solution (1:1) to the beaker, immediately cover the beaker with a watch glass, place on an electric hot plate covered with an asbestos board, heat until the liquid boils, and keep boiling for 5～10 min. Then slightly heat the beaker so that the liquid does not reach boiling, for about 1.5～2 h; or move the beaker to a warm place and leave overnight.
• 6.4 When filtering the barium sulfate precipitate with quantitative filter paper, pour the liquid and precipitate onto the filter paper, and collect the filtrate in a clean beaker. After most of the clear filtrate has filtered out, discard the filtrate and place the empty beaker back under the funnel. Then use distilled water from a wash bottle to completely wash the residual precipitate in the beaker onto the filter paper. If the precipitate begins to pass through the filter paper, repeatedly filter the turbid filtrate until the filtrate is completely clear. Wash the precipitate on the filter paper with a small amount of hot distilled water (30～40℃), and check whether washing is complete. Put the last filtered wash water into a test tube, add 100 g/L barium chloride solution 2 drops; if no barium sulfate precipitate appears, washing is considered complete.
• 6.5 After washing is complete, remove the filter paper with precipitate from the funnel, fold it into four, and place it in a pre-constant-weight porcelain crucible (constant weight according to clause 6.6). Then place this crucible at the furnace mouth of a high-temperature electric furnace, with the furnace door open, so that the filter paper carbonizes at low temperature and with ventilation, but the crucible must not be subjected to high heat and the filter paper must not ignite. Only after the filter paper has carbonized, move the crucible into the furnace and ignite at 775℃±25℃ for 15～20 min, so that the carbonaceous matter is burned off, leaving barium sulfate.
• 6.6 Ignite the crucible at 775℃±25℃ for 15～20 min, move into air to cool for 3 min, place in a desiccator to cool for 30 min, and weigh the crucible accurately to 0.0002 g. Repeat the operation until the difference between two consecutive weighings is not greater than 0.0004 g.

9. Qualitative and quantitative determination and calculation formula

The barium content of the sample X [% (m/m)] is calculated according to the following formula:

X = (m₁ × 0.5885 / m) × 100

Where:

• m₁ — mass of the barium sulfate precipitate obtained from the sample during analysis, g;
• 0.5885 — coefficient for converting barium sulfate mass to barium mass;
• m — mass of the sample, g.

10. Precision

• Repeatability: the difference between two results of repeated determinations by the same operator shall not be greater than 4% of the arithmetic mean.

11. Report

Take the arithmetic mean of two results of repeated determinations as the barium content of the sample.

12. Referenced documents

• Ash determination method (the original does not give a specific standard number, not provided in the available source).
• Reference adoption: partial content of former Soviet Union national standard ГОСТ 13538-68 "Methods for determination of barium, calcium, and zinc content in additives and additive-containing lubricating oils" (original "1'OCI' 13538-6 8", requires confirmation against the source standard (source-text extraction)).

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 Q&A reference