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This standard is developed in accordance with the rules given in GB/T 1.1-2009 Directives for standardization - Part 1: Structure and drafting of standards.
This standard was proposed by China Electricity Council.
This standard is under the jurisdiction of the National Technical Committee on Electrochemistry of Standardization Administration of China.
This standard was drafted by Xi’an Thermal Power Research Institute Co., Ltd.
Chief drafters of this standard: Feng Liping, Liu Yongluo, Xiao Xiuyuan and Lu Xiujuan
This standard is issued for the first time.
In the process of implementing this standard, the relevant comments and recommendations, whenever necessary, may be fed back to the Standardization Center of China Electricity Council (Address: No.1, 2nd Lane, Baiguang Road, Beijing, 100761, China).
Phosphate ester fire-resistant oil - Determination of ageing - Closed cup method
1 Scope
This standard specifies the closed-cup ageing determination method for phosphate ester fire-resistant oil.
This standard is applicable to closed-cup ageing determination for phosphate ester fire-resistant oil. It may also serve as a reference for ageing determination for other ester oils.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB 264 Petroleum products - Determination of acid number
GB/T 601 Chemical reagent - Preparations of standard volumetric solutions
GB/T 5231 Designation and chemical composition of wrought copper and copper alloys
GB/T 7600 Determination of water content in transformer oils and turbine oils in service by coulometric method
GB/T 28552 Determination of acid number in transformer oils and turbine oils by BTB method
DL/T 429.7 Determination of sludge for electric power oils
3 Summary of method
The specimen and copper catalyst are put into a closed container and then aged in a thermostatic drying oven at 115℃±1℃ for 164h. The acid number and sludge precipitation of the specimen are tested before and after the ageing process respectively. The ageing resistance of the specimen is expressed by the increase of acid number and sludge precipitation over the ageing process.
4 Apparatus
The requirements and specifications of the apparatus are as follows:
a) Conical flask with a ground stopper: with a capacity of 250mL.
b) Thermometer: with a measuring range of 0℃~150℃ and a division value of 1℃.
c) Ageing test chamber or electro-thermostatic blast oven: with a temperature control range of room temperature to 300℃, and an accuracy of ±1℃.
d) Mini coulometric titrator: as per the requirements of GB/T 7600.
e) Microsyringe: with a capacity of 250μL or 1mL.
f) Basic microburette: with a capacity of 2mL and a division value of 0.02mL.
g) Measuring cylinder: with a capacity of 50mL or 100mL.
h) Thermostatic waterbath: with a temperature control range of room temperature to 100℃.
i) Spherical reflux condenser tube: about 300mm in length.
j) Balance: with a precision of 0.1g.
5 Reagents and materials
The reagents and materials used in this method are as follows:
a) Isopropanol: analytically pure.
b) 95% ethanol or anhydrous ethanol: analytically pure.
c) Potassium hydroxide: analytically pure. 0.03moL/L ~ 0.05moL/L potassium hydroxide-ethanol standard solution is prepared in accordance with GB/T 601.
d) Basic blue 6B indicator: prepared in accordance with GB/T 264.
e) Bromothymol Blue (BTB) indicator: prepared in accordance with GB/T 28552.
f) Copper wire: T1 copper, with purity of not lower than 99.9%, a diameter of 1.00mm~1.02 mm and a length of 330mm, prepared in accordance with GB/T 5231.
g) Silicon carbide gauze: 100-grit.
h) Filter paper: medium-speed qualitative filter paper with a diameter of 11cm.
i) n-hexane: analytically pure.
6 Preparations
6.1 Clean all glass apparatuses to be used, dry them at 115℃±5℃ and then store in a desiccator for future use.
6.2 Polish the copper wire with silicon carbide gauze, clean the abrasive dusts off the copper wire with filter papers, wind the copper wire into a spiral shape with an outer diameter of 20mm±1mm; clean it with isopropanol, then put it on filter paper, dry it in the air for 5min, and then put it into the desiccator for future use.
Foreword II
1 Scope
2 Normative references
3 Summary of method
4 Apparatus
5 Reagents and materials
6 Preparations
7 Test steps
8 Calculation formula
9 Report
10 Judgment of results
