CN110530959A - A kind of quantitative evaluation method for predicting lubricant life - Google Patents
A kind of quantitative evaluation method for predicting lubricant life Download PDFInfo
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- CN110530959A CN110530959A CN201910868409.8A CN201910868409A CN110530959A CN 110530959 A CN110530959 A CN 110530959A CN 201910868409 A CN201910868409 A CN 201910868409A CN 110530959 A CN110530959 A CN 110530959A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The present invention provides a kind of quantitative evaluation methods for predicting lubricant life, the method is using the mixed liquor that is made of aqueous sulfuric acid, ethyl alcohol, silica as test agent, after mixing respectively with sample to be tested and standard sample, the content that linear voltammetry is tested and then determines phenol antioxidant and amine antioxidants in sample to be tested to be measured is carried out.The method of the present invention is simple and convenient for operation, high sensitivity, the oxidation preventive content of phenols and amine in energy while test lubricant, and the test agent used obtains convenience, reagent is environmentally friendly reagent, injury of the test agent to environment and human body effectively is avoided, test result relative standard deviation is less than 5%.
Description
Technical field
The invention belongs to lubricant Quality Detection technical fields, and in particular to a kind of quantitative assessment for predicting lubricant life
Method.
Background technique
In oil liquid monitoring, it is to judge equipment lubrication shape that oxidation preventive content, which is the degree being characterized in oily oxidation deterioration,
The important indicator of state.National and foreign standards generally use spectrophotometry, liquid chromatography, infra-red sepectrometry and carry out in oil product at present
Oxidation preventive content test.Three of the above method is at present only for phenolic antioxidant, but usually used phenols and amine in lubricant
Class two types antioxidant, not can accurately reflect the content of antioxidant in lubricant using three of the above method.
Summary of the invention
A kind of prediction lubricant life is provided it is an object of the invention to overcome in place of the shortcomings of the prior art
Quantitative evaluation method.
To achieve the above object, the technical scheme adopted by the invention is as follows: it is a kind of predict lubricant life quantitative assessment side
Method the described method comprises the following steps:
(1) samples of lubricant to be measured is quantitatively mixed with test agent and is uniformly dispersed, obtain sample to be tested A, the test
Reagent is made of aqueous sulfuric acid, ethyl alcohol, silica；
(2) samples of lubricant of known phenol antioxidant and amine antioxidants content is quantitatively mixed with test agent
It is uniformly dispersed, obtains standard sample B；
(3) using the electrochemical workstation including three-electrode system under the same conditions to sample to be tested A, standard sample B
Linear voltammetry test is carried out with the test agent as blank reagent, obtains sample to be tested A, standard sample B and blank
The volt-ampere curve of reagent, the three-electrode system is by as the glass-carbon electrode of working electrode, platinum wire auxiliary electrode and platinum filament reference
Electrode composition；
(4) the response peak area that the phenol antioxidant in sample is determined on the volt-ampere curve of sample to be tested A is A1, amine
The response peak area of class antioxidant is A2；The phenol antioxidant in sample is determined on the volt-ampere curve of standard sample B
Response peak area is A3, the response peak area of amine antioxidants is A4；It is determined on the volt-ampere curve of blank reagent corresponding
Blank responds peak area；
(5) by external standard method, peak area and the relationship of the content of phenol antioxidant and amine antioxidants are calculated according to response
Out in the samples of lubricant to be measured phenol antioxidant and amine antioxidants content.
The method of the present invention is simple and convenient for operation, high sensitivity, can test lubricant (including lubricating oil and lubricating grease simultaneously
Class) in phenols and amine oxidation preventive content, and the test agent that uses obtains convenience, and reagent is environmentally friendly examination
Agent effectively avoids injury of the test agent to environment and human body, and test result relative standard deviation is less than 5%.
Preferably, in the step (3), voltage amplification is 0.1V/s in linear voltammetry test.
Preferably, the amine antioxidants is aromatic amine antioxidant.
Preferably, the aromatic amine antioxidant is in the range of the response peak on volt-ampere curve is in 0.4V to 0.9V.
Preferably, the phenol antioxidant is in the range of the response peak on volt-ampere curve is in 1.0V to 1.6V.
Preferably, the concentration of silica is 0.2g/mL test agent in the test agent.
Preferably, the mass fraction of sulfuric acid is 10%~75% in aqueous sulfuric acid in the test agent.
Preferably, the volume ratio of mass fraction is 10%~75% in the test agent aqueous sulfuric acid and ethyl alcohol is
1:25~1:75.
Preferably, the mass fraction of sulfuric acid is 50% in aqueous sulfuric acid in the test agent.
Preferably, the volume ratio of mass fraction is 50% in the test agent aqueous sulfuric acid and ethyl alcohol be 1:25~
1:75。
Preferably, in the step (1), the volume ratio that samples of lubricant to be measured is quantitatively mixed with test agent is 1:
12.5。
Preferably, the partial size of the silica is 80~200 μm.
The beneficial effects of the present invention are: the present invention provides a kind of quantitative evaluation methods for predicting lubricant life, originally
Inventive method has the advantage that
(1) the method for the present invention can pass through the antioxidant of 2 seed types in linear voltammetry test lubricant；
(2) the method for the present invention uses environmentally friendly test agent, can be avoided operator and contacts toxic reagent；
(3) material that the method for the present invention uses is common test agent, can laboratory it is ready-to-use；
(4) reagent that the method for the present invention uses can effectively prevent reagent volatilization failure；
(5) the method for the present invention can understand the behaviour in service of antioxidant in oil liquid in time, aid in determining whether the residue of oil liquid
Service life and prediction optimal oil draining period.
Detailed description of the invention
Fig. 1 is that a kind of quantitative evaluation method of prediction lubricant life of the embodiment of the present invention tests certain 46# steam turbine oil
Volt-ampere result figure.
Fig. 2 is that a kind of quantitative evaluation method of prediction lubricant life of the embodiment of the present invention tests certain 32# steam turbine oil
Volt-ampere result figure.
Fig. 3 is that a kind of quantitative evaluation method of prediction lubricant life of the embodiment of the present invention tests the volt of certain steam turbine oil
Pacify result figure.
Fig. 4 is that a kind of quantitative evaluation method of prediction lubricant life of the embodiment of the present invention tests certain lithium base grease
Volt-ampere result figure.
Fig. 5 is a kind of volt-ampere of the quantitative evaluation method blank testing reagent of prediction lubricant life of the embodiment of the present invention
Result figure.
Fig. 6 is that lubricant life of the invention predicts quantitative evaluation method flow chart.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of quantitative evaluation method of prediction lubricant life as the embodiment of the present invention, the method includes following steps
It is rapid:
(1) by volume it is that 1:12.5 is mixed and is uniformly dispersed with test agent by samples of lubricant to be measured, obtains to be tested
Sample A, the test agent are made of aqueous sulfuric acid, ethyl alcohol, silica, the concentrated sulfuric acid that wherein aqueous sulfuric acid is 50%,
50% concentrated sulfuric acid and ethyl alcohol is 1:75 by volume, and the concentration of silica is 0.2g/mL in test agent；
(2) samples of lubricant of known phenol antioxidant and aromatic amine oxidation preventive content and test agent are pressed into body
Product obtains standard sample B than being that 1:12.5 mixing is uniformly dispersed；
(3) using the electrochemical workstation including three-electrode system under the same conditions to sample to be tested A, standard sample B
Linear voltammetry test is carried out with the test agent as blank reagent, voltage amplification is in the linear voltammetry test
0.1V/s obtains the volt-ampere curve of sample to be tested A, standard sample B and blank reagent, and the three-electrode system is by as work electricity
Glass-carbon electrode, platinum wire auxiliary electrode and the platinum filament reference electrode composition of pole；
(4) the response peak area that the phenol antioxidant in sample is determined on the volt-ampere curve of sample to be tested A is A1, virtue
The response peak area of fragrant amine antioxidants is A2；Determine that the phenols in sample is anti-oxidant on the volt-ampere curve of standard sample B
The response peak area of agent is A3, the response peak area of amine antioxidants is A4；Phase is determined on the volt-ampere curve of blank reagent
The blank response peak area answered is respectively A5, A6, wherein range of the response peak of aromatic amine antioxidant in 0.4V to 0.9V
Interior, the response peak of phenol antioxidant is in the range of 1.0 to 1.6V；
(5) by the relationship of the external standard method content of peak area and phenol antioxidant and aromatic amine antioxidant according to response
Calculate the content of phenol antioxidant and amine antioxidants in the samples of lubricant to be measured.
Experimental example 1
For illustrate embodiment 1 prediction lubricant life quantitative evaluation method effect, carry out application verification test.
(1) material and reagent
(1) electrochemical workstation: being equipped with three-electrode system, can output data or analog signal.Three-electrode system includes one
A working electrode (glass-carbon electrode of diameter 3mm), one 0.5 millimeter of diameter of platinum wire auxiliary electrode and one 0.5 millimeter of diameter
Platinum filament reference electrode.The potential of reference electrode between 0~1.8V, the rate of change of auxiliary electrode 0.01 arrive 0.5V/s.
(2) mixer: revolving speed is in 2800~3000/min.
(3) sampler: sample volume is in 0.10mL to 0.50mL.
(4) vial: with bottle cap, volume is in 7mL or so.
(5) reagent: petroleum ether III (is used for cleaning electrode)；Acid reagent；Silica.
(2) experimental method and result
1, using certain 46#, using long-life steam turbine oil, as sample to be tested, original new known phenols is anti-oxidant
Certain 46# long-life steam turbine oil of agent and aromatic amine antioxidant is examined as standard items using the method for embodiment 1
It surveys.
As a result as shown in Figure 1, certain 46# is being new with phenol antioxidant content in long-life steam turbine oil by calculating
Certain 46# long-life steam turbine oil in phenol antioxidant content 57.3%；Certain is with aromatic amine in long-life steam turbine oil
Class oxidation preventive content is 96.8% of aromatic amine oxidation preventive content in certain new long-life steam turbine oil.
2, using certain 32# use antirust steam turbine oil as sample to be tested, original new known phenol antioxidant
Certain 32# with aromatic amine antioxidant is using antirust steam turbine oil to be examined as standard items using the method for embodiment 1
It surveys.
As a result as shown in Fig. 2, by calculating, certain 32# is being new with phenol antioxidant content in antirust steam turbine oil
Certain 32# is with 60.8% of phenol antioxidant content in antirust steam turbine oil；Certain 32# is with aromatic amine in antirust steam turbine oil
Class oxidation preventive content is certain new 32# with 89.9% of aromatic amine oxidation preventive content in antirust steam turbine oil.
3, using certain used steam turbine oil as sample to be tested, original new known phenol antioxidant and virtue
Certain steam turbine oil of fragrant amine antioxidants is detected as standard sample using the method for embodiment 1.
As a result as shown in figure 3, by calculating, phenol antioxidant content is certain new vapour in certain used steam turbine oil
43.9% of phenol antioxidant content in machine oil is taken turns, aromatic amine oxidation preventive content is new in certain used steam turbine oil
Certain steam turbine oil in aromatic amine oxidation preventive content 65.9%.
4, using certain used lithium base grease as sample to be tested, original new known phenol antioxidant and
Certain lithium base grease of aromatic amine antioxidant is detected as standard sample using the method for embodiment 1.
As a result as shown in figure 4, by calculating, certain used lithium base grease phenol antioxidant content is certain new lithium
The 65.7% of phenol antioxidant content in base grease, aromatic amine oxidation preventive content in certain used lithium base grease
It is 31.5% of aromatic amine oxidation preventive content in certain new lithium base grease.
(3) Precision Experiment
Precision test
Using certain steam turbine oil as sample, the method for embodiment 1 carries out repetitive test, with peak area evaluation test knot
The precision of fruit obtains feature volt-ampere curve as shown in figure 3, test result is shown in Table 1.
Certain the steam turbine oil oxidation preventive content test result of table 1
Using oxidation preventive content in the method for the present invention test lubricant, simple testing process, test agent obtains convenience,
Test result relative standard deviation is less than 5%, and use environment friendly test agent, effectively avoids to environment and human body
Injury.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of quantitative evaluation method for predicting lubricant life, which is characterized in that the described method comprises the following steps:
(1) samples of lubricant to be measured is quantitatively mixed with test agent and is uniformly dispersed, obtain sample to be tested A, the test agent
It is made of aqueous sulfuric acid, ethyl alcohol, silica；
(2) samples of lubricant of known phenol antioxidant and amine antioxidants content is quantitatively mixed into dispersion with test agent
Uniformly, standard sample B is obtained；
(3) using the electrochemical workstation including three-electrode system under the same conditions to sample to be tested A, standard sample B and work
Linear voltammetry test is carried out for the test agent of blank reagent, obtains sample to be tested A, standard sample B and blank reagent
Volt-ampere curve, the three-electrode system is by as the glass-carbon electrode of working electrode, platinum wire auxiliary electrode and platinum filament reference electrode
Composition；
(4) the response peak area that the phenol antioxidant in sample is determined on the volt-ampere curve of sample to be tested A is A1, amine is anti-
The response peak area of oxidant is A2；The response of the phenol antioxidant in sample is determined on the volt-ampere curve of standard sample B
Peak area is A3, the response peak area of amine antioxidants is A4；Corresponding blank is determined on the volt-ampere curve of blank reagent
Respond peak area；
(5) by external standard method, peak area and the relationship of the content of phenol antioxidant and amine antioxidants calculate institute according to response
State the content of phenol antioxidant and amine antioxidants in samples of lubricant to be measured.
2. the method according to claim 1, wherein voltage increases in linear voltammetry test in the step (3)
Width is 0.1V/s.
3. according to the method described in claim 2, it is characterized in that, the amine antioxidants is aromatic amine antioxidant.
4. according to the method described in claim 3, it is characterized in that, sound of the aromatic amine antioxidant on volt-ampere curve
Ying Feng is in the range of 0.4V to 0.9V.
5. according to the method described in claim 4, it is characterized in that, response peak of the phenol antioxidant on volt-ampere curve
In the range of 1.0V to 1.6V.
6. the method according to claim 1, wherein the concentration of silica is 0.2g/ in the test agent
ML test agent.
7. the method according to claim 1, wherein in the test agent in aqueous sulfuric acid sulfuric acid quality
Score is 10%~75%.
8. the method according to the description of claim 7 is characterized in that mass fraction is 10%~75% in the test agent
The volume ratio of aqueous sulfuric acid and ethyl alcohol is 1:25~1:75.
9. the method according to claim 1, wherein samples of lubricant to be measured and test try in the step (1)
The volume ratio that agent quantitatively mixes is 1:12.5.
10. the method according to claim 1, wherein the partial size of the silica is 80~200 μm.
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Citations (5)
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|---|---|---|---|---|
| US4744870A (en) * | 1986-12-23 | 1988-05-17 | University Of Dayton | Method for evaluating the remaining useful life of a lubricant |
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| CN104345085A (en) * | 2013-08-01 | 2015-02-11 | 中国石油化工股份有限公司 | An electrolytic solution and uses thereof |
| CN104597101A (en) * | 2015-01-05 | 2015-05-06 | 武汉材料保护研究所 | Method for measuring antioxidant content in lubricating oil by use of linear sweep voltammetry |
-
2019
- 2019-09-12 CN CN201910868409.8A patent/CN110530959A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| US4744870A (en) * | 1986-12-23 | 1988-05-17 | University Of Dayton | Method for evaluating the remaining useful life of a lubricant |
| CN102507715A (en) * | 2011-11-14 | 2012-06-20 | 湖南省湘电试验研究院有限公司 | Method for detecting antioxidant of electric oil |
| CN103323515A (en) * | 2013-03-29 | 2013-09-25 | 宁波出入境检验检疫局检验检疫技术中心 | Method for detecting residual anti-oxidant content in industrial lubricating oil while in operation |
| CN104345085A (en) * | 2013-08-01 | 2015-02-11 | 中国石油化工股份有限公司 | An electrolytic solution and uses thereof |
| CN104597101A (en) * | 2015-01-05 | 2015-05-06 | 武汉材料保护研究所 | Method for measuring antioxidant content in lubricating oil by use of linear sweep voltammetry |
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Application publication date: 20191203 |