CN103822895B - A kind of indoor degradation analysis method of synthetic lubricant fluid under non-single degradation factors - Google Patents
A kind of indoor degradation analysis method of synthetic lubricant fluid under non-single degradation factors Download PDFInfo
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Abstract
A kind of indoor degradation analysis method of synthetic lubricant fluid under non-single degradation factors, the method is under illumination and two kinds of degradation factors of microorganism act on jointly, uses a degradation cycle sample and 0 day sample degradation cultural method to complete the degradation process of fully synthetic lubricating oil in esters；Wherein, degradation cycle sample include two kinds of degradation factors jointly act under test sample and the light degradation sample under single factors photodegradation, two classes degraded samples are degraded one cycle of cultivation respectively；Within 0 day, sample includes neutral species and toxic samples, preparation at the end of a degradation cycle sample degradation is cultivated；Ultrasonic disruption cell manipulation, drying, sampling are carried out to above-mentioned four kinds of samples synchronization, determines lubrication residue content by infrared detection, calculate according to the changing value of lubricating oil content before and after degraded and determine its degradation rate.Worst error scope with reference to degradation rate result of calculation and parallel determination investigates repeatability and the stability of data.The method strict logic, science are practical.
Description
Technical field
The invention belongs to lubricating oil degradation technical field, relate to the use of non-single degradation factors, in particular with natural lighting and two kinds of microorganism
The indoor degraded of the fully synthetic lubricating oil in esters of main degradation factors degraded and analysis method.
Background technology
In recent years, lubricating oil be degraded into study hotspot both domestic and external, existing people carries out and grinds microbe application in the biodegradable of lubricating oil
Study carefully.The method evaluated currently with the degradability to lubricating oil for the microorganism is more, comprising: measure European Union's lubrication of basic biological degradation rate
The biodegradable standard method (CEC-L-33-A-93 experimental technique) of oil, measure the OECD method of ultimate biodegradation rate and to detect degradation process
In produced CO2STURM method for Measure Indexes；And with BOD/COD as Measure Indexes, O in test biodegradation process2's
The MITI method etc. of consumption.For the degradability of lubricating oil is analyzed, said method is single degradation factors-biodegradable experimental technique,
The common feature of this kind of experimental technique is that main degradation factors is single, and experienced interference is less, tests and analyze relatively easy, it is easy to draw this experiment
Under the conditions of degraded conclusion.Shortcoming is to have certain error with the actual degraded situation under lubricating oil natural conditions.The degraded of lubricating oil under natural conditions
The not result of single factors effect.But the indoor degradation experiment of the fully synthetic lubricating oil in esters under non-single degradation factors effect not yet shape at present
Become complete method system.
Content of the invention
It is an object of the invention to the problem for above-mentioned existence, offer one is more scientific, logic is tighter, accuracy is higher and has good
Get well indoor degraded and the analysis method of fully synthetic lubricating oil in esters under the repeated non-single degradation factors effect with stability.
Technical scheme:
A kind of indoor degradation analysis method of synthetic lubricant fluid under non-single degradation factors, the method is common in illumination and two kinds of main degradation factors of microorganism
Under effect, a degradation cycle sample and 0 day sample two class sample degradation cultural method is used to complete the degradation process of fully synthetic lubricating oil in esters,
Detect and calculate the content of remaining lubricating oil after pretreatment respectively, calculate according to the changing value of lubricating oil content before and after degraded and determine its degradation rate,
Concrete grammar is as follows:
The 1st, Preparatory work of experiment；
In two class sample degradation cultivations, the solubility total organic carbon of experimental water should be less than 1 × 10-3g/L；The purity of agents useful for same is pure extremely for analysis
Chromatographically pure；Experiment glass container all with wash liquid totally to guarantee that container inner wall does not contains hydrocarbon；Microorganism fungus kind derives from from dirt
Water treatment plant's biochemistry pool obtains and through filtering off deimpurity fresh activity mud filtrate, and its dominant bacteria includes that raw branch moves glue bacterium
(Zoogloearamigera), thread dynamic glue bacterium (Zoogloea filipendula), Comamonas testosteroni (Comamonas testosteroni), food
Vinegar comamonas (Comamonas acidovorans), aquatic comamonas (Comamonas aquatica), Pseudomonas fluorescens
(Pseudomonas fluorescens), pseudomonas aeruginosa (Pseudomonas aeruginosa), Sphaerotilus natans (Sphaerotilus natans),
Micrococcus luteus (Micrococcus luteus) and Bacillus foecalis alkaligenes (Alcaligenes feacalis) amount to 10 common bacterial classifications, the viable bacteria of inoculation bacterium solution
Concentration is 1.0 × 104～1.0 × 105CFU/mL；Inorganic salts basal medium solution is the aqueous solution being made up of following components, the content of each component
It is respectively KH by g/L aqueous solution2PO4 3.4、Na2HPO4 1.5、(NH4)2SO4 4.0、MgSO4·7H2O the 0.7th, dusty yeast 0.01,
Balance of water, the pH value of culture medium is 7.2～7.6, using fully synthetic lubricating oil in esters as the sole carbon source of growth of microorganism；
The 2nd, two class sample degradation cultivation；
The indoor degradation experiment of fully synthetic lubricating oil in esters is divided into two class samples, i.e. one degradation cycle sample and 0 day sample:
The 2.1st, a degradation cycle sample
A. test sample dual factors degradation process: take the inorganic salts basal medium solution in above-mentioned 1st step of 90mL, adds the fully synthetic ester of 2.0mL
Class lubricating oil, inoculates mentioned microorganism bacterial classification i.e. fresh activity mud filtrate 5.0mL, then is settled to above-mentioned inorganic salts basal medium solution
100mL, with 180r/min～200r/min shaken cultivation 28 days under natural lighting, cultivation temperature is 30 DEG C ± 1 DEG C, and degraded cultivation terminates
After sample method as described in following 3rd step is pre-processed and detects；
B. the single factors degradation process of light degradation sample: take 90mL above-mentioned inorganic salts basal medium solution, adds 2.0mL fully synthetic esters profit
Lubricating oil, then access 0.03M HgCl2Solution 1.0mL, to suppress varied bacteria growing, does not inoculate mentioned microorganism bacterial classification, then with above-mentioned inorganic salts base
Basal culture medium solution is settled to 100mL, and with 170r/min～200r/min shaken cultivation 28 days under natural lighting, cultivation temperature is 30 DEG C
± 1 DEG C, sample method as described in following 3rd step is pre-processed and detects after terminating by degraded cultivation；
The 2.2nd, 0 day sample preparation
C.0 sky neutral species preparation: when preparing test sample and light degradation sample solution, synchronization takes mentioned microorganism bacterial classification i.e. fresh activity sludge filtering
Liquid 5.0mL is placed in 4 DEG C of airtight preservations, at the end of test sample and light degradation sample degradation, takes out these the 4 DEG C bacterium solution preserving immediately by following
Mode prepares neutral species solution:
Take 90mL above-mentioned inorganic salts basal medium solution, inoculate the above-mentioned 4 DEG C microorganism fungus kind 5.0mL preserving, be not added with lubricating oil, then with above-mentioned
Inorganic salts basal medium solution is settled to 100mL, shakes up, and immediately sample method as described in following 3rd step is pre-processed and is detected；
D.0 sky toxic samples preparation: at the end of said one degradation cycle sample degradation process, take 90mL above-mentioned inorganic salts basal medium solution,
Add the fully synthetic lubricating oil in esters of 2.0mL and 0.03M HgCl2Solution 1.0mL, does not access microorganism fungus kind, more basic with above-mentioned inorganic salts
Culture medium solution is settled to 100mL, and sample method as described in following 3rd step is pre-processed and detects after completing by preparation immediately；
3rd, sample pretreatment and detection；
Tetra-groups of sample synchronizations of above-mentioned A, B, C, D are carried out ultrasonic disruption cell, broken time 3min～5min, uses 100mL CCl4Carry out
Extraction, acutely vibrates 5min～8min, stratification, collects extract lower floor organic phase, add 10g anhydrous Na2SO4It is dried 24h, take
Sample, carries out infrared spectrum analysis, in infrared wave number 2930cm of c h bond-1±10cm-1The residue of each C-H compound is quantitatively detected at place respectively
Content；
Must synchronize to carry out to the ultrasonic disruption cell manipulation of above-mentioned tetra-groups of samples of A, B, C, D, corresponding sampling and detection operation also synchronize respectively
Carry out；
The the 4th, under non-single factors effect the degradation rate of fully synthetic lubricating oil in esters calculate and be divided into two parts；
The the 4.1st, the lubricating oil total degradation rate under two kinds of main degradation factors effects calculate:
The the 4.2nd, the lubricating oil photodegradation rate under single factors-light action calculate:
Wherein,
ISample, lightThe infrared light spectrum of the C-H compound residues content of A group test sample,
IPoison, lightThe infrared light spectrum of the C-H compound residues content of B group light degradation sample,
IIn, lightThe infrared light spectrum of the C-H compounds content of C group neutral species,
IPoison, keeps awayThe infrared light spectrum of the C-H compounds content of D group toxic samples.
The invention have the advantage that
In degraded conceptual design and implementation process, first non-biodegradation factor-illumination is introduced in the degradable analysis of fully synthetic lubricating oil in esters, real
Non-biodegradation factor and the fully synthetic lubricating oil in esters of biodegradable factors in combination degraded are showed；Establish non-single degradation factors-biological factor and non-
The indoor degradation experiment method of fully synthetic lubricating oil in esters under biological factor synergy, the method strict logic, science is practical；In experimentation,
Toxic samples, neutral species two class sample and test sample, the asynchronous cultivation of illumination sample further reduce experimental error, improve experiment
Precision；The pretreatment of sample uses ultrasonic cell-break method to carry out based on ultimate biodegradation theory, and this processing method can be by high polymer
The mesostate that incomplete Degradation and Transformation becomes is retained in treatment fluid, and the degradation rate of mensuration only relates to be fully converted to CO2And H2The portion of O
Share in the benefit lubricating oil.To sum up, this experimental technique more science, logicality are tighter.
(4) brief description
Fig. 1 is the infrared spectrogram of castor oil-base lubricating oil toxicity lucifuge sample,
Fig. 2 is the infrared spectrogram of the neutral lucifuge sample of castor oil-base lubricating oil,
Fig. 3 is the infrared spectrogram of castor oil-base lubricating oil test sample,
Fig. 4 is the infrared spectrogram of castor oil-base lubricating oil light degradation sample；
Fig. 5 is the infrared spectrogram of reference oil castor oil toxicity lucifuge sample,
Fig. 6 is the infrared spectrogram of the neutral lucifuge sample of reference oil castor oil,
Fig. 7 is the infrared spectrogram of reference oil castor oil test sample,
Fig. 8 is the infrared spectrogram of reference oil castor oil light degradation sample；
Fig. 9 is the infrared spectrogram of cottonseed oil based lubricating oil toxicity lucifuge sample,
Figure 10 is the infrared spectrogram of the neutral lucifuge sample of cottonseed oil based lubricating oil,
Figure 11 is the infrared spectrogram of cottonseed oil based lubricating oil test sample,
Figure 12 is the infrared spectrogram of cottonseed oil based lubricating oil light degradation sample；
Figure 13 is the infrared spectrogram of soya-bean oil based lubricating oil toxicity lucifuge sample,
Figure 14 is the infrared spectrogram of the neutral lucifuge sample of soya-bean oil based lubricating oil,
Figure 15 is the infrared spectrogram of soya-bean oil based lubricating oil test sample,
Figure 16 is the infrared spectrogram of soya-bean oil based lubricating oil light degradation sample.
Illustrating: in the embodiment of the present invention, 4 kinds of samples shown by each chart, 3 panel datas listed by every kind of sample, then each chart comprises
12 ir datas, have 4 data drawing lists, altogether 4 × 12=48 ir datas in embodiment, corresponding one of each data
Infrared spectrogram, amounts to 48 infrared spectrograms.Because collection of illustrative plates is more, as space is limited, no longer list one by one, each sample in each chart
Only list a representative data collection of illustrative plates.
(5) detailed description of the invention
Embodiment 1: the degradation experiment of castor oil-base lubricating oil and reference oil
A kind of new lubricant that castor oil-base lubricating oil is is main material chemical synthesis with castor oil, it is mainly composed of decanedioic acid two-2-monooctyl ester, the last of the ten Heavenly stems two
Acid polyol ester etc.；Reference oil is the castor oil of known degradation rate.
1. the non-single factors degradation experiment of castor oil-base lubricating oil
The 1st, Preparatory work of experiment；
In two class sample degradation cultivations, the solubility total organic carbon of experimental water should be less than 1 × 10-3g/L；The purity of agents useful for same is pure extremely for analysis
Chromatographically pure；Experiment glass container all with wash liquid totally to guarantee that container inner wall does not contains hydrocarbon；Microorganism fungus kind derives from from dirt
Water treatment plant's biochemistry pool obtains and through filtering off deimpurity fresh activity mud filtrate, and its dominant bacteria includes that raw branch moves glue bacterium
(Zoogloearamigera), thread dynamic glue bacterium (Zoogloea filipendula), Comamonas testosteroni (Comamonas testosteroni), food
Vinegar comamonas (Comamonas acidovorans), aquatic comamonas (Comamonas aquatica), Pseudomonas fluorescens
(Pseudomonas fluorescens), pseudomonas aeruginosa (Pseudomonas aeruginosa), Sphaerotilus natans (Sphaerotilus natans),
Micrococcus luteus (Micrococcus luteus) and Bacillus foecalis alkaligenes (Alcaligenes feacalis) amount to 10 common bacterial classifications, the viable bacteria of inoculation bacterium solution
Concentration is 1.0 × 104～1.0 × 105CFU/mL；Inorganic salts basal medium solution is the aqueous solution being made up of following components, the content of each component
It is respectively KH by g/L aqueous solution2PO4 3.4、Na2HPO4 1.5、(NH4)2SO4 4.0、MgSO4·7H2O the 0.7th, dusty yeast 0.01,
Balance of water, the pH value of culture medium is 7.2～7.6, using fully synthetic lubricating oil in esters as the sole carbon source of growth of microorganism；
The 2nd, two class sample degradation cultivation；
The indoor degradation experiment of fully synthetic lubricating oil in esters is divided into two class samples, i.e. one degradation cycle sample and 0 day sample:
The 2.1st, a degradation cycle sample
A. test sample dual factors degradation process: take the inorganic salts basal medium solution in above-mentioned 1st step of 90mL, adds 2.0mL castor oil-base
Lubricating oil, inoculates mentioned microorganism bacterial classification i.e. fresh activity mud filtrate 5.0mL, then is settled to 100 with above-mentioned inorganic salts basal medium solution
ML, with 180r/min～200r/min shaken cultivation 28 days under natural lighting, cultivation temperature is 30 DEG C ± 1 DEG C, and degraded cultivation will after terminating
Sample method as described in following 3rd step pre-processes and detects；
B. the single factors degradation process of light degradation sample: take 90mL above-mentioned inorganic salts basal medium solution, adds 2.0mL castor oil-base lubrication
Oil, then access 0.03M HgCl2Solution 1.0mL, to suppress varied bacteria growing, does not access mentioned microorganism bacterial classification, more basic with above-mentioned inorganic salts
Culture medium solution is settled to 100mL, and with 170r/min～200r/min shaken cultivation 28 days under natural lighting, cultivation temperature is 30 DEG C ±
1 DEG C, sample method as described in following 3rd step is pre-processed and detects after terminating by degraded cultivation；
The 2.2nd, 0 day sample preparation
C.0 sky neutral species preparation: when preparing test sample and light degradation sample solution, synchronization takes mentioned microorganism bacterial classification i.e. fresh activity sludge filtering
Liquid 5.0mL is placed in 4 DEG C of airtight preservations, at the end of test sample and light degradation sample degradation, takes out these the 4 DEG C bacterium solution preserving immediately by following
Mode prepares neutral species solution:
Take 90mL above-mentioned inorganic salts basal medium solution, inoculate the above-mentioned 4 DEG C microorganism fungus kind 5.0mL preserving, be added without lubricating oil, then use
State inorganic salts basal medium solution and be settled to 100mL, shake up, immediately sample method as described in following 3rd step is pre-processed and detects；
D.0 sky toxic samples preparation: at the end of said one degradation cycle sample degradation process, take 90mL above-mentioned inorganic salts basal medium solution,
Add 2.0mL castor oil-base lubricating oil and 0.03M HgCl2Solution 1.0mL, does not access microorganism fungus kind, then is trained by above-mentioned inorganic salts basis
Foster based sols is settled to 100mL, and sample method as described in following 3rd step is pre-processed and detects after completing by preparation immediately；
3rd, sample pretreatment and detection；
Tetra-groups of sample synchronizations of above-mentioned A, B, C, D are carried out ultrasonic disruption cell, and the broken time is 3.0min, uses 100mL CCl4Extract,
Acutely vibration 5min, stratification, collect extract lower floor organic phase, add 10g anhydrous Na2SO4It is dried 24h, sampling, carry out infrared
Spectrum analysis, in infrared wave number 2930cm of c h bond-1±10cm-1The residue content of each C-H compound is quantitatively detected at place respectively；
Must synchronize to carry out to the ultrasonic disruption cell manipulation of above-mentioned tetra-groups of samples of A, B, C, D, corresponding sampling and detection operation also synchronize respectively
Carry out；
The the 4th, under non-single factors effect the degradation rate of castor oil-base lubricating oil calculate and be divided into two parts；
The the 4.1st, the castor oil-base lubricating oil total degradation rate under two kinds of main degradation factors effects calculate:
The the 4.2nd, the castor oil-base lubricating oil photodegradation rate under single factors-light action calculate:
Wherein:
ISample, lightThe infrared light spectrum of the C-H compound residues content of A group test sample,
IPoison, lightThe infrared light spectrum of the C-H compound residues content of B group light degradation sample,
IIn, keep awayThe infrared light spectrum of the C-H compounds content of C group neutral species,
IPoison, keeps awayThe infrared light spectrum of the C-H compounds content of D group toxic samples.
2. the non-single factors degradation experiment of reference oil
The castor oil selecting known degradation rate does reference oil product.
The degraded training method of reference oil sample is identical with above-mentioned castor oil-base lubricating oil.Except that change castor oil-base lubricating oil into reference oil
Product.
Castor oil-base lubricating oil testing result and as shown in the table by calculating the degradation rate that determines:
Table 1 castor oil-base lubricating oil sample infrared detection data
Wherein, Fig. 1 corresponding infrared light spectrum is 0.030, and Fig. 2 corresponding infrared light spectrum is 0.005, and Fig. 3 corresponding infrared light spectrum is 0.007,
Fig. 4 corresponding infrared light spectrum is 0.028.
Then the total degradation rate mean value of castor oil-base lubricating oil is: W=(0.0300-0.0080+0.0050)/0.0300=90.0%
The photodegradation rate mean value of castor oil-base lubricating oil is: R=(0.0300-0.0280)/0.0300=6.7%.
Table 2 reference oil sample infrared detection data
Wherein, Fig. 5 corresponding infrared light spectrum is 0.031, and Fig. 6 corresponding infrared light spectrum is 0.005, and Fig. 7 corresponding infrared light spectrum is 0.006,
Fig. 8 corresponding infrared light spectrum is 0.029.
Then the total degradation rate of reference oil product castor oil is: W=(0.0313-0.0063+0.0053)/0.0313=96.9%
The photodegradation rate of castor oil is: R=(0.0313-0.0287)/0.0313=8.3%.
Tables 1 and 2 data show: under non-single degradation factors effect, and the castor oil-base lubricating oil most degradation rate of 28 days reaches 90.3%,
Average degradation rate is 90.0%, and the worst error of parallel determination is 0.6%；And the most degradation rate of reference oil product castor oil is 96.9%, averagely drop
Solution rate is 96.9%, and the worst error of parallel determination is 0.1%；The detection data of two kinds of oil products are respectively provided with preferably repeatability and stability；Document
The biological degradation rate published value of the castor oil-base lubricating oil reported is 88.37%, and the biological degradation rate published value of reference oil product castor oil is
96.0%, use the degradation rate under the single factors effect that the oil product degradation rate data that obtain of this programme report than document high, illustrate in microorganism
With under the comprehensive function of illumination, the degradation effect of lubricating oil and reference oil is superior to single factors-biodegradable effect；On the other hand, lubricating oil
The photodegradation rate maximum of 28 days is 6.8%, and the worst error of parallel determination is 0.3%, and the reference oil photodegradation rate maximum of 28 days is 9.7%,
The worst error of parallel determination is 3.2%, and the light degradation detection data of two kinds of oil products are respectively provided with preferably repeatability and stability.Conclusions proves
The feasibility of this experimental program.
Embodiment 2: the degradation experiment of cottonseed oil based lubricating oil
Except in sample culturing basigamy system add carbon source change cottonseed oil based lubricating oil in addition to, other as sample degradation experimentation, sample pretreatment and
Infrared detection, identical with embodiment 1 by calculating the method and steps determining degradation rate, sample detection result and by the fall that determines of calculating
Solution rate is as shown in the table:
Table 3 cottonseed oil base based lubricating oil sample infrared detection data
Wherein, Fig. 9 corresponding infrared light spectrum is 0.042, and Figure 10 corresponding infrared light spectrum is 0.007, and Figure 11 corresponding infrared light spectrum is 0.010,
Figure 12 corresponding infrared light spectrum is 0.039.
Then the total degradation rate mean value of cottonseed oil based lubricating oil is:
W=(0.0420-0.0103+0.006)/0.0420=89.8%
The photodegradation rate mean value of cottonseed oil based lubricating oil is:
R=(0.0420-0.0397)/0.0420=5.5%.
Table 3 data show: under non-single degradation factors effect, and the cottonseed oil based lubricating oil most degradation rate of 28 days reaches 90.7%, averagely
Degradation rate is 89.8%, and the worst error of parallel determination is 2.9%, in addition, the lubricating oil photodegradation rate maximum of 28 days is 6.9%, and parallel survey
Fixed worst error is 2.1%, and the detection data of lubricating oil are respectively provided with preferably repeatability and stability；The cottonseed oil based lubricating oil that document has been reported
Biological degradation rate published value be 88.7%.The degradation rate data using this programme to obtain are higher than the degradation rate under the single factors effect reported,
Illustrate under the comprehensive function of microorganism and illumination, all than single factors, biodegradable effect is good for the degradation effect of lubricating oil, it was demonstrated that this reality
The feasibility of proved recipe case.
Embodiment 3: the degradation experiment of soya-bean oil based lubricating oil
In addition to the carbon source adding in sample culturing basigamy system changes soya-bean oil based lubricating oil into, other are such as sample degradation experimentation, sample pretreatment and red
Outer detection, identical with embodiment 1 by calculating the method and steps determining degradation rate, sample detection result and by the degraded that determines of calculating
Rate is as shown in the table:
Table 4 soya-bean oil based lubricating oil sample infrared detection data
Wherein, Figure 13 corresponding infrared light spectrum is 0.037, and Figure 14 corresponding infrared light spectrum is 0.008, and Figure 15 corresponding infrared light spectrum is
0.013, Figure 16 corresponding infrared light spectrum is 0.035.
Then the total degradation rate mean value of soya-bean oil based lubricating oil is: W=(0.0367-0.0130+0.0073)/0.0367=84.4%
The photodegradation rate mean value of soya-bean oil based lubricating oil is: R=(0.0367-0.0340)/0.0367=7.3%.
Table 4 data show: under non-single degradation factors effect, and the soya-bean oil based lubricating oil most degradation rate of 28 days reaches 85.7%, averagely drops
Solution rate is 84.4%, and the worst error of parallel determination is 1.5%；On the other hand, the lubricating oil photodegradation rate maximum of 28 days is 8.2%, parallel
The worst error measuring is 2.5%, and the detection data of lubricating oil are respectively provided with preferably repeatability and stability；The soya-bean oil based lubricating oil that document has been reported
Biological degradation rate published value be 77.9%, use the degradation rate data that obtain of this programme higher than the degradation rate under the single factors effect reported,
Illustrate under the comprehensive function of microorganism and illumination, all than single factors, biodegradable effect is good for the degradation effect of lubricating oil, it was demonstrated that this reality
The feasibility of proved recipe case.
Claims (1)
1. the indoor degradation analysis method of synthetic lubricant fluid under non-single degradation factors, the method is in illumination and two kinds of microorganism
Main degradation factors acts on down jointly, uses a degradation cycle sample and 0 day sample two class sample degradation cultural method to complete entirely to close
Become the degradation process of lubricating oil in esters, detect and calculate the content of remaining lubricating oil after pretreatment respectively, according to profit before and after degraded
The changing value of grease content calculates and determines its degradation rate, and concrete grammar is as follows:
The 1st, Preparatory work of experiment；
In two class sample degradation cultivations, the solubility total organic carbon of experimental water should be less than 1 × 10-3g/L；Agents useful for same
Purity is pure to chromatographically pure for analyzing；Experiment glass container all with wash liquid totally to guarantee that container inner wall does not contains nytron
Thing；Microorganism fungus kind derives from and obtains from sewage treatment plant's biochemistry pool and through filtering off deimpurity fresh activity mud filtrate, its
Dominant bacteria includes that raw branch moves glue bacterium (Zoogloea ramigera), thread dynamic glue bacterium (Zoogloea filipendula), C testosteroni
Monad (Comamonas testosteroni), vinegar comamonas (Comamonas acidovorans), aquatic Comamonas
Bacterium (Comamonas aquatica), Pseudomonas fluorescens (Pseudomonas fluorescens), pseudomonas aeruginosa
(Pseudomonas aeruginosa), Sphaerotilus natans (Sphaerotilus natans), micrococcus luteus (Micrococcus luteus)
Amounting to 10 common bacterial classifications with Bacillus foecalis alkaligenes (Alcaligenes feacalis), the viable bacteria concentration of inoculation bacterium solution is 1.0 × 104~
1.0×105CFU/mL；Inorganic salts basal medium solution is the aqueous solution being made up of following components, and the content of each component presses g/L
Aqueous solution is respectively KH2PO4 3.4、Na2HPO4 1.5、(NH4)2SO4 4.0、MgSO4·7H2O the 0.7th, dusty yeast 0.01,
Balance of water, the pH value of culture medium is 7.2～7.6, using fully synthetic lubricating oil in esters as the sole carbon source of growth of microorganism；
The 2nd, two class sample degradation cultivation；
The indoor degradation experiment of fully synthetic lubricating oil in esters is divided into two class samples, i.e. one degradation cycle sample and 0 day sample:
The 2.1st, a degradation cycle sample
A. test sample dual factors degradation process: take the inorganic salts basal medium solution in above-mentioned 1st step of 90mL, adds
The fully synthetic lubricating oil in esters of 2.0mL, inoculates mentioned microorganism bacterial classification i.e. fresh activity mud filtrate 5.0mL, then uses above-mentioned nothing
Machine salt basal medium solution is settled to 100mL, with 180r/min～200r/min shaken cultivation 28 days under natural lighting,
Cultivation temperature is 30 DEG C ± 1 DEG C, and sample method as described in following 3rd step is pre-processed and detects after terminating by degraded cultivation；
B. the single factors degradation process of light degradation sample: take 90mL above-mentioned inorganic salts basal medium solution, adds 2.0mL
Fully synthetic lubricating oil in esters, adds the HgCl that concentration is 0.03M2Solution 1.0mL, to suppress varied bacteria growing, does not inoculates
Mentioned microorganism bacterial classification, then it is settled to 100mL with above-mentioned inorganic salts basal medium solution, with 170r/min under natural lighting
～200r/min shaken cultivation 28 days, cultivation temperature is 30 DEG C ± 1 DEG C, degraded cultivation terminate after by sample by following 3rd step institute
The method of stating pre-processes and detects；
The 2.2nd, 0 day sample preparation
C.0 sky neutral species preparation: when preparing test sample and light degradation sample solution, synchronization takes mentioned microorganism bacterial classification and is
Fresh activity mud filtrate 5.0mL is placed in 4 DEG C of airtight preservations, at the end of test sample and light degradation sample degradation, takes out
These 4 DEG C preserve bacterium solution immediately in the following manner prepare neutral species solution:
Take 90mL above-mentioned inorganic salts basal medium solution, inoculate the above-mentioned 4 DEG C microorganism fungus kind 5.0mL preserving, be not added with profit
Lubricating oil, then it is settled to 100mL with above-mentioned inorganic salts basal medium solution, shake up, immediately sample is pressed following 3rd step institute
The method of stating pre-processes and detects；
D.0 sky toxic samples preparation: at the end of said one degradation cycle sample degradation process, take 90mL above-mentioned inorganic
Salt basal medium solution, adds the fully synthetic lubricating oil in esters of 2.0mL and the HgCl that concentration is 0.03M2Solution 1.0mL,
Do not access microorganism fungus kind, then be settled to 100mL with above-mentioned inorganic salts basal medium solution, prepare after completing immediately by sample
Product method as described in following 3rd step pre-processes and detects；
3rd, sample pretreatment and detection；
Tetra-groups of sample synchronizations of above-mentioned A, B, C, D are carried out ultrasonic disruption cell, broken time 3min～5min, uses
100mL CCl4Extract, acutely vibrate 5min～8min, stratification, collect extract lower floor organic phase, add
10g anhydrous Na2SO4It is dried 24h, sampling, carry out infrared spectrum analysis, in infrared wave number 2930cm of c h bond-1±10
cm-1The residue content of each C-H compound is quantitatively detected at place respectively；
Must synchronize to carry out to the ultrasonic disruption cell manipulation of above-mentioned tetra-groups of samples of A, B, C, D, corresponding sampling and inspection
Survey operation also to synchronize respectively to carry out；
The the 4th, under non-single factors effect the degradation rate of fully synthetic lubricating oil in esters calculate and be divided into two parts；
The the 4.1st, the lubricating oil total degradation rate under two kinds of main degradation factors effects calculate:
The the 4.2nd, the lubricating oil photodegradation rate under single factors-light action calculate:
Wherein,
ISample, lightThe infrared light spectrum of the C-H compound residues content of A group test sample,
IPoison, lightThe infrared light spectrum of the C-H compound residues content of B group light degradation sample,
IIn, lightThe infrared light spectrum of the C-H compounds content of C group neutral species,
IPoison, keeps awayThe infrared light spectrum of the C-H compounds content of D group toxic samples.
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| CN101586148A (en) * | 2009-06-26 | 2009-11-25 | 河北大学 | Method for degrading crude oil with protozoan infusorian |
| CN101690939A (en) * | 2009-07-13 | 2010-04-07 | 延安市微生物研究所 | Method for degrading crude oil by separating compound bacteria solution from contaminated fossil oil sample |
| CN101748184A (en) * | 2009-12-31 | 2010-06-23 | 天津南开大学蓖麻工程科技有限公司 | Biodegradation test method of synthetic oil and vegetable oil-based lubricating oil product |
| CN102559194A (en) * | 2010-12-09 | 2012-07-11 | 大庆油田有限责任公司 | Method for controlling process of degrading crude oil by microbes for oil extraction and application of method |
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| CN101586148A (en) * | 2009-06-26 | 2009-11-25 | 河北大学 | Method for degrading crude oil with protozoan infusorian |
| CN101690939A (en) * | 2009-07-13 | 2010-04-07 | 延安市微生物研究所 | Method for degrading crude oil by separating compound bacteria solution from contaminated fossil oil sample |
| CN101748184A (en) * | 2009-12-31 | 2010-06-23 | 天津南开大学蓖麻工程科技有限公司 | Biodegradation test method of synthetic oil and vegetable oil-based lubricating oil product |
| CN102559194A (en) * | 2010-12-09 | 2012-07-11 | 大庆油田有限责任公司 | Method for controlling process of degrading crude oil by microbes for oil extraction and application of method |
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