This standard specifies the method for determining the mass fraction of sulfated ash in unused additive-containing lubricating oils and additive concentrates used for blending lubricating oils. These additives usually contain one or more metals: barium, calcium, magnesium, zinc, potassium, sodium and tin. Elemental sulfur, phosphorus and chlorine exist in a combined form. The lower limit of the mass fraction of sulfated ash determined in this standard is 0.005%. When the sulfated ash is less than 0.02%, this standard is only applicable to lubricating oils containing only ashless additives. This standard is not applicable to the determination of used engine oils containing lead additives, nor is it applicable to lubricating oils without additives. For these oils, GB/T 508 can be used. Sulfated ash can be used to indicate the concentration of known metal additives in new lubricating oils. When phosphorus is not present, barium, calcium, magnesium, potassium, sodium are converted to sulfates, tin (IV) and zinc are converted to their oxides, and sulfur and chlorine do not interfere. However, when phosphorus is present with metal additives, it is partially or completely retained in the sulfated ash in the form of metal phosphates. This standard involves certain hazardous materials, operations and equipment. However, it is not intended to make recommendations on all safety issues related to this. Therefore, users should establish appropriate safety and protection measures and determine the applicable management system before using this standard. GB/T 2433-2001 Determination of sulfated ash content in additives and lubricating oils containing additives GB/T2433-2001 standard download decompression password: www.bzxz.net

GB/T2433—2001
This standard adopts the international standard IS03987:1994 "Determination of sulfated ash content of additives and lubricating oils containing additives" and amends GB/T2433-1981 "Determination of sulfated ash content of additives and lubricating oils containing additives". Differences between this standard and ISO3987:1994: 1. The standards cited in this standard are all the corresponding national standards currently in force in my country. 2. Added notes on electric furnaces, equipment used for heating evaporating furnaces or crucibles containing samples, and heating with electric furnaces. This standard amends GB/T2433—1981: 1. Added notes in the scope chapter.
2. Deleted the relevant content on the treatment of evaporating furnaces or crucibles. 3. Added the content of the determination of low-ash mineral oil. 4. The blank test is different when the mass fraction of sulfated ash in the sample is less than 0.02%. 5. The use of filter paper is different. bzxZ.net
6. The flame height control is different.
7. The precision has changed.
This standard is proposed by the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the Petrochemical Research Institute of China Petroleum and Chemical Corporation. The drafting unit of this standard: China Petroleum and Chemical Corporation Shanghai Gaoqiao Branch Refinery. The main drafters of this standard: Lu Lihua, Gu Zhenyan, Cheng Guangling. This standard was first issued in 1981.
1 Scope
National Standard of the People's Republic of China
Additives and additives
Determination of sulphated ash in lubricating oils
Petroleum products-Lubricating oils and additives-Determination of sulphated ash GB/T2433-2001
eqvISO3987:1994
Replaces GB/T2433-1981
1.1 This standard specifies the method for determining the mass fraction of sulphated ash in unused lubricating oils containing additives and additive concentrates used for blending lubricating oils. These additives usually contain one or more metals: barium, calcium, magnesium, zinc, potassium, sodium and tin. The elements sulfur, phosphorus and chlorine exist in a combined form.
1.2 The lower limit of the mass fraction of sulphated ash determined by this standard is 0.005%. When the sulfated ash is less than 0.02%, this standard is only applicable to lubricating oils containing only ashless additives. 1.3 This standard is not applicable to the determination of used engine oils containing lead additives, nor is it applicable to lubricating oils without additives. For these oils, GB/T508 can be used.
1 There are indications that magnesium reacts differently to other alkali metals in the test. If there is a magnesium additive, caution should be exercised when judging the data. 2 There are indications that the results of samples containing molybdenum are lower because the molybdenum compounds cannot be fully recovered at the ashing temperature. 1.4 Sulfated ash can be used to indicate the concentration of known metal additives in new lubricating oils. When phosphorus is not present, barium, calcium, magnesium, sodium, potassium are converted to sulfates, tin (V) and zinc are converted to their oxides (see note), and sulfur and chlorine do not interfere. However, when phosphorus is present with metal additives, it is partially or completely retained in the sulfated ash in the form of metal phosphates. Note: Because zinc sulfate slowly decomposes into oxides at the combustion temperature specified in this method, when determining samples containing zinc, variable results may be obtained unless the zinc sulfate is completely converted to oxides. 1.5 This standard involves certain hazardous materials, operations and equipment. However, it does not intend to make recommendations on all safety issues related to this. Therefore, users should establish appropriate safety and protection measures and determine applicable management systems before using this standard. 2 Referenced standards
The provisions included in the following standards constitute a part of this standard through reference. Unless otherwise expressly specified in the standard, the following referenced standards should be currently valid standards.
GB/T508 Determination of ash content of petroleum products
GB/T4756 Manual sampling method for petroleum liquids
GB/T6682 Specifications and test methods for water for analytical laboratories 3 Terminology
This standard uses the following terms.
Sulfated ash sulfatedash
The residue after the sample is carbonized is treated with sulfuric acid and heated to a constant mass. Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on September 4, 2001 and implemented on March 1, 2002
4 Summary of the method
GB/T2433-2001
Ignite the sample and burn it until only ash and carbon remain. After cooling, treat the residue with sulfuric acid and heat it at 775℃ until the carbon is completely oxidized. After the ash cools, treat it with sulfuric acid again, heat it at 775℃ and keep the weight constant, and then calculate the mass fraction of sulfate ash. 5 Instruments and materials
5.1 Instruments
5.1.1 Evaporating crucible or glass: Made of silica or porcelain fused together, with a capacity of 50mL~100mL. For samples with a sulfate ash mass fraction of less than 0.2%, use a platinum evaporating crucible or crucible with a capacity of 120mL~150mL. If it is known that the sample contains elements such as phosphorus that are corrosive to platinum, platinum evaporating crucible should not be used. 5.1.2 Gas lamp or electric furnace.
5.1.3 Muffle furnace: can be heated and controlled at 775℃±25℃. It is best to have small holes in the front or back to allow air to slowly pass through the furnace for natural ventilation.
5.1.4 Cooler: does not contain desiccant.
5.1.5 Balance: sensitivity is 0.1mg.
5.2 Materials
5.2.1 Filter paper: ash mass fraction is not more than 0.01%. 5.2.2 Low ash mineral oil: white oil with sulfate ash content below the detection limit of this standard. Its content is determined by the following method: take 100g of white oil, accurate to 0.5g, put it in 120mL150mL of platinum evaporation blood, and determine the sulfate ash content according to the provisions of Chapter 8 of this standard method, and deduct the sulfuric acid blank according to Article 8.11.
6 Reagents
6.1 Distilled water: meet the requirements of GB/T6682 Grade III water. 6.2 Sulfuric acid: analytical grade, mass fraction is 98%. Note: Be careful that sulfuric acid is highly corrosive and has high hydration heat. Protective clothing, gloves and masks should be worn when operating with sulfuric acid. 6.3 Sulfuric acid solution (1:1): slowly add 1 volume of sulfuric acid to 1 volume of water. 6.4 Isopropanol: analytical grade.
6.5 Toluene: analytical grade.
7 Sampling
Unless otherwise specified, samples should be sampled in accordance with GB/T4756. 8 Test steps
8.1 Select an evaporating dish or crucible of appropriate capacity according to the required amount of the sample. 8.2 Heat the evaporating dish or crucible in a muffle furnace at 775℃ and keep it for at least 10 minutes, cool it to room temperature in a cooler, and weigh it to an accuracy of 0.1mg.
8.3 Weigh a sample amount mi (g) calculated according to formula (1) into an evaporator or crucible, accurate to 0.1 mg. m = 10/mg
Where: mo is the mass fraction of sulfated ash expected to be generated, %. (1)
The sample amount should not exceed 80 g. When the mass fraction of sulfated ash of lubricating oil additive is equal to or greater than 2.00%, the sample should be diluted with 10 times the amount of low-ash mineral oil as the sample. If it is found that the difference between the measured sulfated ash value and the expected value exceeds two times, the sample amount is calculated again considering the first measurement result and a second analysis is performed.
GB/T2433—2001
8.4 Carefully heat the evaporator or crucible containing the sample on a gas lamp or electric furnace until the sample is ignited and a flame is generated, and maintain a constant temperature so that the sample can burn evenly and moderately. After the combustion is completed, continue to heat slowly until no smoke is emitted. If the sample contains too much water, so that it foams and the sample components are lost from the evaporating dish, the sample should be discarded and 1mL2mL of isopropanol should be added to the new sample and heated again. If this is still not satisfactory, add 10mL of an equal volume of toluene and isopropanol mixture and mix thoroughly with the sample. Add a few filter papers to the mixture and heat together. Most of the water will be removed when the filter paper begins to burn. Note: If the sample does not ignite when the heating equipment is an electric furnace, the filter paper can be used to ignite until the sample is ignited. 8.5 Allow the evaporating dish or crucible to cool to room temperature, then add sulfuric acid drop by drop to completely wet the residue. Place the evaporating dish or crucible on the electric furnace and heat carefully at a low temperature to prevent splashing. Continue heating until there is no more smoke. 8.6 Place the evaporating blood or glass in a muffle furnace controlled at 775℃ and continue heating at this temperature until the carbon is completely or almost completely oxidized.
8.7 Cool the evaporating blood or crucible to room temperature, add 3 drops of distilled water and 10 drops of sulfuric acid solution, shake the evaporating blood or crucible to completely wet the residue, and then heat as described in 8.5.
8.8 Place the evaporating dish or crucible back into the muffle furnace and keep the temperature at 775°C for 30 min. Cool the evaporating dish or crucible to room temperature in a suitable cooler.
If the sample contains dialkyl or dialkylaryl zinc dithiophosphates and mixtures of these additives, some black residue may be generated at this stage. In this case, repeat the operations in 8.7 and 8.8 until a white residue is obtained. 8.9 Weigh the mass of the evaporating dish or crucible and the residue to the nearest 0.1 mg. 8.10 Repeat the operations in 8.8 and 8.9 until the difference between the two valid weighings does not exceed 1.0 mg. 8.11 If the mass fraction of sulfated ash expected to be generated by the sample is not more than 0.02%, the blank value is determined by adding 1 mL of sulfuric acid to the weighed platinum evaporating dish or crucible, heating until no more smoke is emitted, then heating in a furnace at 775°C for 30 min, cooling to room temperature in a cooler, and weighing to the nearest 0.1 mg. If there is any ash in the sulfuric acid, the mass of the resulting sulfated ash should be corrected by subtracting the mass of ash generated by the sulfuric acid from the total sulfated ash in the sample. The mass of ash generated by the sulfuric acid is determined by multiplying the mass of ash generated by 1 mL of sulfuric acid blank by the total volume of sulfuric acid used. This corrected result, m2 (g), is used when calculating the mass fraction of sulfated ash (see Chapter 9).
9Calculation
Calculate the sulfated ash A (%) in the sample according to formula (2): A = 100m2/ml
Where: m1 - mass of sample, g;
m2 - mass of sulfated ash, g.
10Report
For samples with a sulfated ash mass fraction of less than 0.02%, the result should be accurate to 0.001%, and for samples with a sulfated ash mass fraction greater than or equal to 0.02%, the result should be accurate to 0.01%. 11 Precision
The reliability of the test results shall be determined as follows (95% confidence level). 11.1 Repeatability ()
The difference between two results measured by the same operator using the same instrument under the same operating conditions on the same test material shall not exceed the following value:
When 0.005% ≤ 0.100%, = 0.047 ± 0.86When 0.11% ≤ 25.0%, r = 0.060z0.76 is the average of the two results compared. 2 Reproducibility (R)
GB/T2433—2001
The difference between two separate and independent results obtained by different operators in different laboratories for the same test material shall not exceed the following values:
When 0.005%≤≤0.100%, R=0.189g0.85When 0.11%<<25.0%, R=0.142g:0.76The average value of the two results compared is given in Table 1. Table 1
Examples of precision values ​​
Sulfated ash
Repeatability
Reproducibility
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