CN103822895A - Indoor degradation analysis method for synthetic lubricating oil under non-single degradation factors - Google Patents
Indoor degradation analysis method for synthetic lubricating oil under non-single degradation factors Download PDFInfo
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Abstract
The invention relates to an indoor degradation analysis method for synthetic lubricating oil under non-single degradation factors. The method comprises the following steps: under the combined action of two degradation factors including illumination and microorganism, adopting a one-degradation-period sample and zero-day sample degrading cultivation method to complete the degradation process of a total synthetic ester lubricating oil, wherein one-degradation-period samples comprise a test sample under the combined action of two degradation factors and a photodegradation sample under the photodegradation action of a single factor, the two kinds of degradation samples are respectively subjected to degrading cultivation for one period, and zero-day samples comprise a neutral sample and a toxic sample which are respectively prepared after the degrading cultivation of the one-degradation-period samples is finished; performing ultrasonic cell breakage operation, drying and sampling on the four samples synchronously, determining the residual content of lubricating oil through infrared detection, and calculating and determining the degradation rate according to the change value of the content of lubricating oil before and after degradation. The repeatability and the stability of data are inspected by reference to the calculated result of the degradation rate and the maximum error range of parallel determination. The method has a strict logic and is scientific and practical.
Description
Technical field
The invention belongs to lubricating oil degradation technique field, relate to and utilize non-single degradation factors, particularly utilize two kinds of main degradation factors of natural lighting and microorganism degrade indoor degraded and the analytical approach of full ester oil.
Background technology
In recent years, lubricating oil be degraded into study hotspot both domestic and external, existing people carries out microbe application in the biodegradation research of lubricating oil.The method of utilizing at present microorganism to evaluate the degradability of lubricating oil is more, comprising: measure European Union's lubricating oil biodegradation standard method (CEC-L-33-A-93 experimental technique) of basic biological degradation rate, the OECD method of mensuration ultimate biodegradation rate and the CO to be produced in detection degradation process
2for the STURM method of Measure Indexes; And take BOD/COD as Measure Indexes, O in test organisms degradation process
2the MITI method etc. of consumption.For the degradability analysis of lubricating oil, said method is single degradation factors-biodegradation experimental technique, and the common feature of this class experimental technique is that main degradation factors is single, and the interference being subject to is less, experiment is relative simple with analysis, is easy to draw the degraded conclusion under this experiment condition.Shortcoming be with lubricating oil natural conditions under actual degraded situation have certain error.Under natural conditions, the degraded of lubricating oil is not the result of single factors effect.But the indoor degradation experiment of full ester oil under non-single degradation factors effect not yet forms complete method system at present.
Summary of the invention
The object of the invention is the problem for above-mentioned existence, a kind of indoor degraded and analytical approach that has more that science, logic are tighter, accuracy is higher and have full ester oil under the non-single degradation factors effect of good reproducibility and stability is provided.
Technical scheme of the present invention:
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 main degradation factors actings in conjunction of microorganism, adopt a degradation cycle sample and 0 day sample, two class samples degraded cultural methods to complete the degradation process of full ester oil, detect respectively and calculate after pretreatment the content of remaining lubricating oil, according to its degradation rate of changing value calculative determination of lubricating oil content before and after degraded, concrete grammar is as follows:
1st, Preparatory work of experiment;
In two class sample degraded 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 to chromatographically pure for analyzing; Experiment does not all contain hydrocarbon by washing lotion washes clean to guarantee container inner wall with glass container; Microorganism fungus kind derives from from sewage treatment plant's biochemistry pool and obtains and go after filtration deimpurity fresh active sludge filtrate, its dominant bacteria comprise the moving glue bacterium of raw branch (
zoogloearamigera), thread moving glue bacterium (
zoogloea filipendula), Comamonas testosteroni (
comamonas testosteroni), 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) amounting to 10 common bacterial classifications, the viable bacteria concentration of inoculation bacterium liquid is 1.0 × 10
4~ 1.0 × 10
5cFU/mL; Inorganic salts basal medium solution is the aqueous solution being made up of following component, and the content of each component is respectively KH by g/L aqueous solution
2pO
43.4, Na
2hPO
41.5, (NH
4)
2sO
44.0, MgSO
47H
2o 0.7, dusty yeast 0.01, surplus is water, the pH value of nutrient culture media is 7.2 ~ 7.6, the sole carbon source using full ester oil as growth of microorganism;
2nd, two class sample degraded cultivations;
The complete indoor degradation experiment of ester oil is divided into two class samples, i.e. a degradation cycle sample and 0 day sample:
2.1st, a degradation cycle sample
A. test sample dual factors degradation process: get the inorganic salts basal medium solution in above-mentioned the 1st step of 90 mL, add the full ester oil of 2.0 mL, inoculation mentioned microorganism bacterial classification is fresh active sludge filtrate 5.0 mL, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 180 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
B. the single factors degradation process of light degradation sample: get the above-mentioned inorganic salts basal medium of 90 mL solution, add the full ester oil of 2.0 mL, then access 0.03 M HgCl
2solution 1.0mL, to suppress varied bacteria growing, do not inoculate mentioned microorganism bacterial classification, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 170 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
2.2nd, 0 day sample preparation
C. 0 day neutral sample preparation: in the time of preparation test sample and light degradation sample solution, synchronously getting mentioned microorganism bacterial classification is that fresh active sludge filtrate 5.0 mL are placed in 4 ℃ of airtight preservations, in the time of test sample and light degradation sample degraded end, take out the bacterium liquid of these 4 ℃ of preservations and prepare in the following manner immediately neutral sample solution:
Get the above-mentioned inorganic salts basal medium of 90 mL solution, inoculate microorganism fungus kind 5.0 mL of above-mentioned 4 ℃ of preservations, not apply oil, then be settled to 100 mL with above-mentioned inorganic salts basal medium solution, shake up, immediately sample is carried out to pre-service and detection by method described in following the 3rd step;
D. toxic samples preparation in 0 day: in the time that an above-mentioned degradation cycle sample degradation process finishes, get the above-mentioned inorganic salts basal medium of 90 mL solution, add the full ester oil of 2.0 mL and 0.03 M HgCl
2solution 1.0 mL, do not access microorganism fungus kind, then are settled to 100 mL with above-mentioned inorganic salts basal medium solution, after having prepared, immediately sample are carried out to pre-service and detection by method described in following the 3rd step;
3rd, sample pretreatment and detection;
Above-mentioned A, B, C, tetra-groups of samples of D are synchronously carried out to ultrasonic disruption cell, and broken times 3 min ~ 5 min, with 100 mL CCl
4extract, thermal agitation 5 min ~ 8min, stratification, collects extract lower floor organic phase, adds 10 g anhydrous Na
2sO
4dry 24 h, sampling, carries out Infrared spectroscopy, in infrared wave number 2930 cm of c h bond
-1± 10 cm
-1the residue content of each C-H compound is quantitatively detected respectively at place;
Ultrasonic disruption cell manipulation to above-mentioned A, B, C, tetra-groups of samples of D must synchronously carry out, and samples accordingly and detects operation and also synchronously carry out respectively;
4th, under non-single factors effect, the calculating of the degradation rate of full ester oil is divided into two parts;
4.1st, the lubricating oil total degradation rate under two kinds of main degradation factors effects is calculated:
4.2nd, the lubricating oil photodegradation rate under single factors-light action calculates:
Wherein,
i sample, lightthe infrared spectrum value of the C-H compound residual content of-A group test sample,
i poison, lightthe infrared spectrum value of the C-H compound residual content of-B group light degradation sample,
i in, light-C organizes the infrared spectrum value of the C-H compounds content of neutral sample,
i poison, keeps awaythe infrared spectrum value of the C-H compounds content of-D group toxic samples.
Advantage of the present invention is:
In degraded conceptual design and implementation process, first non-biodegradation factor-illumination is introduced in the degradable analysis of full ester oil, realize non-biodegradation factor and the full ester oil of biodegradation factor combined degradation; Set up the indoor degradation experiment method of full ester oil under non-single degradation factors-biodyne and abiotic factor synergy, the method strict logic, science practicality; In experimentation, toxic samples, neutral sample two class samples have further reduced experimental error with the asynchronous cultivation of test sample, illumination sample, have improved experimental precision; The pre-service of sample adopts ultrasonic cell-break method to carry out based on ultimate biodegradation theory, and the mesostate that this disposal route can become incomplete superpolymer Degradation and Transformation be retained in treating fluid, and the degradation rate of mensuration only relates to and is converted into CO completely
2and H
2the parts of lubricating oil of O.To sum up, more science, logicality are tighter for this experimental technique.
(4) accompanying drawing explanation
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.
Illustrate: in the embodiment of the present invention, each chart is shown 4 kinds of samples, every kind of sample is listed 3 panel datas, each chart comprises 12 ir datas, in embodiment, have 4 data drawing lists, amount to 4 × 12=48 ir data, the corresponding infrared spectrogram of each data, amounts to 48 infrared spectrograms.More because of collection of illustrative plates, as space is limited, to list no longer one by one, the each sample in each chart is only listed a representative data collection of illustrative plates.
(5) embodiment
Embodiment 1: the degradation experiment of castor oil-base lubricating oil and reference oil
Castor oil-base lubricating oil is a kind of new lubricant take castor oil as main material chemosynthesis, and its principal ingredient is decanedioic acid two-2-monooctyl ester, decanedioic 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
1st, Preparatory work of experiment;
In two class sample degraded 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 to chromatographically pure for analyzing; Experiment does not all contain hydrocarbon by washing lotion washes clean to guarantee container inner wall with glass container; Microorganism fungus kind derives from from sewage treatment plant's biochemistry pool and obtains and go after filtration deimpurity fresh active sludge filtrate, its dominant bacteria comprise the moving glue bacterium of raw branch (
zoogloearamigera), thread moving glue bacterium (
zoogloea filipendula), Comamonas testosteroni (
comamonas testosteroni), 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) amounting to 10 common bacterial classifications, the viable bacteria concentration of inoculation bacterium liquid is 1.0 × 10
4~ 1.0 × 10
5cFU/mL; Inorganic salts basal medium solution is the aqueous solution being made up of following component, and the content of each component is respectively KH by g/L aqueous solution
2pO
43.4, Na
2hPO
41.5, (NH
4)
2sO
44.0, MgSO
47H
2o 0.7, dusty yeast 0.01, surplus is water, the pH value of nutrient culture media is 7.2 ~ 7.6, the sole carbon source using full ester oil as growth of microorganism;
2nd, two class sample degraded cultivations;
The complete indoor degradation experiment of ester oil is divided into two class samples, i.e. a degradation cycle sample and 0 day sample:
2.1st, a degradation cycle sample
A. test sample dual factors degradation process: get the inorganic salts basal medium solution in above-mentioned the 1st step of 90 mL, add 2.0 mL castor oil-base lubricating oil, inoculation mentioned microorganism bacterial classification is fresh active sludge filtrate 5.0 mL, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 180 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
B. the single factors degradation process of light degradation sample: get the above-mentioned inorganic salts basal medium of 90 mL solution, add 2.0 mL castor oil-base lubricating oil, then access 0.03 M HgCl
2solution 1.0mL, to suppress varied bacteria growing, do not access mentioned microorganism bacterial classification, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 170 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
2.2nd, 0 day sample preparation
C. 0 day neutral sample preparation: in the time of preparation test sample and light degradation sample solution, synchronously getting mentioned microorganism bacterial classification is that fresh active sludge filtrate 5.0 mL are placed in 4 ℃ of airtight preservations, in the time of test sample and light degradation sample degraded end, take out the bacterium liquid of these 4 ℃ of preservations and prepare in the following manner immediately neutral sample solution:
Get the above-mentioned inorganic salts basal medium of 90 mL solution, microorganism fungus kind 5.0 mL that inoculate above-mentioned 4 ℃ of preservations, do not add lubricating oil, then are settled to 100 mL with above-mentioned inorganic salts basal medium solution, shake up, immediately sample is carried out to pre-service and detection by method described in following the 3rd step;
D. toxic samples preparation in 0 day: in the time that an above-mentioned degradation cycle sample degradation process finishes, get the above-mentioned inorganic salts basal medium of 90 mL solution, add 2.0 mL castor oil-base lubricating oil and 0.03 M HgCl
2solution 1.0 mL, do not access microorganism fungus kind, then are settled to 100 mL with above-mentioned inorganic salts basal medium solution, after having prepared, immediately sample are carried out to pre-service and detection by method described in following the 3rd step;
3rd, sample pretreatment and detection;
Above-mentioned A, B, C, tetra-groups of samples of D are synchronously carried out to ultrasonic disruption cell, and the broken time is 3.0 min, with 100 mL CCl
4extract, thermal agitation 5 min, stratification, collects extract lower floor organic phase, adds 10 g anhydrous Na
2sO
4dry 24 h, sampling, carries out Infrared spectroscopy, in infrared wave number 2930 cm of c h bond
-1± 10 cm
-1the residue content of each C-H compound is quantitatively detected respectively at place;
Ultrasonic disruption cell manipulation to above-mentioned A, B, C, tetra-groups of samples of D must synchronously carry out, and samples accordingly and detects operation and also synchronously carry out respectively;
4th, under non-single factors effect, the calculating of the degradation rate of castor oil-base lubricating oil is divided into two parts;
4.1st, the castor oil-base lubricating oil total degradation rate under two kinds of main degradation factors effects is calculated:
4.2nd, the castor oil-base lubricating oil photodegradation rate under single factors-light action calculates:
Wherein:
i sample, lightthe infrared spectrum value of the C-H compound residual content of-A group test sample,
i poison, lightthe infrared spectrum value of the C-H compound residual content of-B group light degradation sample,
i in, keep away-C organizes the infrared spectrum value of the C-H compounds content of neutral sample,
i poison, keeps awaythe infrared spectrum value of the C-H compounds content of-D group toxic samples.
2. the non-single factors degradation experiment of reference oil
Select the castor oil of known degradation rate to do reference oil product.
The degraded training method of reference oil sample is identical with above-mentioned castor oil-base lubricating oil.Difference is to change castor oil-base lubricating oil into reference oil product.
Castor oil-base lubricating oil testing result and as shown in the table by the degradation rate of calculative determination:
Wherein, the infrared spectrum value that Fig. 1 is corresponding is that the infrared spectrum value that 0.030, Fig. 2 is corresponding is that the infrared spectrum value that 0.005, Fig. 3 is corresponding is that the infrared spectrum value that 0.007, Fig. 4 is corresponding is 0.028.
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%.
Wherein, the infrared spectrum value that Fig. 5 is corresponding is that the infrared spectrum value that 0.031, Fig. 6 is corresponding is that the infrared spectrum value that 0.005, Fig. 7 is corresponding is that the infrared spectrum value that 0.006, Fig. 8 is corresponding is 0.029.
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%.
Table 1 and table 2 data show: under non-single degradation factors effect, the castor oil-base lubricating oil most degradation rate of 28 days reaches 90.3%, and average degradation rate is 90.0%, and the maximum error of replicate determination is 0.6%; And the most degradation rate of reference oil product castor oil is 96.9%, average degradation rate is 96.9%, and the maximum error of replicate determination is 0.1%; The detection data of two kinds of oil products all have good repeatability and stability; The biological degradation rate published value of the castor oil-base lubricating oil that document has been reported is 88.37%, the biological degradation rate published value of reference oil product castor oil is 96.0%, the oil product degradation rate data of using this programme to obtain are higher than the degradation rate under the single factors effect of bibliographical information, illustrate under the combined action of microorganism and illumination, the degradation effect of lubricating oil and reference oil is all better than single factors-biodegradable effect; On the other hand, the lubricating oil photodegradation rate maximal value of 28 days is 6.8%, and the maximum error of replicate determination is 0.3%, and the reference oil photodegradation rate maximal value of 28 days is 9.7%, the maximum error of replicate determination is that the light degradation detection data of 3.2%, two kind of oil product all have good repeatability and stability.Conclusions proves the feasibility of this experimental program.
Embodiment 2: the degradation experiment of cottonseed oil based lubricating oil
Except the carbon source adding in sample culturing basigamy system changes cottonseed oil based lubricating oil into, other are as identical with embodiment 1 with step in sample degradation experiment process, sample pretreatment and infrared detection, method by calculative determination degradation rate, sample detection result and to pass through the degradation rate of calculative determination as shown in the table:
Wherein, the infrared spectrum value that Fig. 9 is corresponding is that the infrared spectrum value that 0.042, Figure 10 is corresponding is that the infrared spectrum value that 0.007, Figure 11 is corresponding is that the infrared spectrum value that 0.010, Figure 12 is corresponding is 0.039.
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, the cottonseed oil based lubricating oil most degradation rate of 28 days reaches 90.7%, average degradation rate is 89.8%, the maximum error of replicate determination is 2.9%, in addition, the lubricating oil photodegradation rate maximal value of 28 days is 6.9%, and the maximum error of replicate determination is 2.1%, and the detection data of lubricating oil all have good repeatability and stability; The biological degradation rate published value of the cottonseed oil based lubricating oil that document has been reported is 88.7%.The degradation rate data of using this programme to obtain are higher than the degradation rate under the single factors effect of having reported, illustrate under the combined action of microorganism and illumination, the degradation effect of lubricating oil is all good than the biodegradable effect of single factors, has proved the feasibility of this experimental program.
Embodiment 3: the degradation experiment of soya-bean oil based lubricating oil
Except the carbon source adding in sample culturing basigamy system changes soya-bean oil based lubricating oil into, other are as identical with embodiment 1 with step in sample degradation experiment process, sample pretreatment and infrared detection, method by calculative determination degradation rate, sample detection result and to pass through the degradation rate of calculative determination as shown in the table:
Wherein, the infrared spectrum value that Figure 13 is corresponding is that the infrared spectrum value that 0.037, Figure 14 is corresponding is that the infrared spectrum value that 0.008, Figure 15 is corresponding is that the infrared spectrum value that 0.013, Figure 16 is corresponding is 0.035.
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, the soya-bean oil based lubricating oil most degradation rate of 28 days reaches 85.7%, and average degradation rate is 84.4%, and the maximum error of replicate determination is 1.5%; On the other hand, the lubricating oil photodegradation rate maximal value of 28 days is 8.2%, and the maximum error of replicate determination is 2.5%, and the detection data of lubricating oil all have good repeatability and stability; The biological degradation rate published value of the soya-bean oil based lubricating oil that document has been reported is 77.9%, the degradation rate data of using this programme to obtain are higher than the degradation rate under the single factors effect of having reported, illustrate under the combined action of microorganism and illumination, the degradation effect of lubricating oil is all good than the biodegradable effect of single factors, has proved the feasibility of this experimental program.
Claims (1)
1. the indoor degradation analysis method of synthetic lubricant fluid under a non-single degradation factors, the method is under illumination and two kinds of main degradation factors actings in conjunction of microorganism, adopt a degradation cycle sample and 0 day sample, two class samples degraded cultural methods to complete the degradation process of full ester oil, detect respectively and calculate after pretreatment the content of remaining lubricating oil, according to its degradation rate of changing value calculative determination of lubricating oil content before and after degraded, concrete grammar is as follows:
1st, Preparatory work of experiment;
In two class sample degraded 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 to chromatographically pure for analyzing; Experiment does not all contain hydrocarbon by washing lotion washes clean to guarantee container inner wall with glass container; Microorganism fungus kind derives from from sewage treatment plant's biochemistry pool and obtains and go after filtration deimpurity fresh active sludge filtrate, its dominant bacteria comprise the moving glue bacterium of raw branch (
zoogloearamigera), thread moving glue bacterium (
zoogloea filipendula), Comamonas testosteroni (
comamonas testosteroni), 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) amounting to 10 common bacterial classifications, the viable bacteria concentration of inoculation bacterium liquid is 1.0 × 10
4~ 1.0 × 10
5cFU/mL; Inorganic salts basal medium solution is the aqueous solution being made up of following component, and the content of each component is respectively KH by g/L aqueous solution
2pO
43.4, Na
2hPO
41.5, (NH
4)
2sO
44.0, MgSO
47H
2o 0.7, dusty yeast 0.01, surplus is water, the pH value of nutrient culture media is 7.2 ~ 7.6, the sole carbon source using full ester oil as growth of microorganism;
2nd, two class sample degraded cultivations;
The complete indoor degradation experiment of ester oil is divided into two class samples, i.e. a degradation cycle sample and 0 day sample:
2.1st, a degradation cycle sample
A. test sample dual factors degradation process: get the inorganic salts basal medium solution in above-mentioned the 1st step of 90 mL, add the full ester oil of 2.0 mL, inoculation mentioned microorganism bacterial classification is fresh active sludge filtrate 5.0 mL, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 180 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
B. the single factors degradation process of light degradation sample: get the above-mentioned inorganic salts basal medium of 90 mL solution, add the full ester oil of 2.0 mL, then access 0.03 M HgCl
2solution 1.0mL, to suppress varied bacteria growing, do not inoculate mentioned microorganism bacterial classification, be settled to 100 mL with above-mentioned inorganic salts basal medium solution again, under natural lighting with 170 r/min ~ 200 r/min shaken cultivation 28 days, cultivation temperature is 30 ℃ ± 1 ℃, and degraded is carried out pre-service and detection by sample by method described in following the 3rd step after cultivating and finishing;
2.2nd, 0 day sample preparation
C. 0 day neutral sample preparation: in the time of preparation test sample and light degradation sample solution, synchronously getting mentioned microorganism bacterial classification is that fresh active sludge filtrate 5.0 mL are placed in 4 ℃ of airtight preservations, in the time of test sample and light degradation sample degraded end, take out the bacterium liquid of these 4 ℃ of preservations and prepare in the following manner immediately neutral sample solution:
Get the above-mentioned inorganic salts basal medium of 90 mL solution, inoculate microorganism fungus kind 5.0 mL of above-mentioned 4 ℃ of preservations, not apply oil, then be settled to 100 mL with above-mentioned inorganic salts basal medium solution, shake up, immediately sample is carried out to pre-service and detection by method described in following the 3rd step;
D. toxic samples preparation in 0 day: in the time that an above-mentioned degradation cycle sample degradation process finishes, get the above-mentioned inorganic salts basal medium of 90 mL solution, add the full ester oil of 2.0 mL and 0.03 M HgCl
2solution 1.0 mL, do not access microorganism fungus kind, then are settled to 100 mL with above-mentioned inorganic salts basal medium solution, after having prepared, immediately sample are carried out to pre-service and detection by method described in following the 3rd step;
3rd, sample pretreatment and detection;
Above-mentioned A, B, C, tetra-groups of samples of D are synchronously carried out to ultrasonic disruption cell, and broken times 3 min ~ 5 min, with 100 mL CCl
4extract, thermal agitation 5 min ~ 8min, stratification, collects extract lower floor organic phase, adds 10 g anhydrous Na
2sO
4dry 24 h, sampling, carries out Infrared spectroscopy, in infrared wave number 2930 cm of c h bond
-1± 10 cm
-1the residue content of each C-H compound is quantitatively detected respectively at place;
Ultrasonic disruption cell manipulation to above-mentioned A, B, C, tetra-groups of samples of D must synchronously carry out, and samples accordingly and detects operation and also synchronously carry out respectively;
4th, under non-single factors effect, the calculating of the degradation rate of full ester oil is divided into two parts;
4.1st, the lubricating oil total degradation rate under two kinds of main degradation factors effects is calculated:
4.2nd, the lubricating oil photodegradation rate under single factors-light action calculates:
Wherein,
i sample, lightthe infrared spectrum value of the C-H compound residual content of-A group test sample,
i poison, lightthe infrared spectrum value of the C-H compound residual content of-B group light degradation sample,
i in, light-C organizes the infrared spectrum value of the C-H compounds content of neutral sample,
i poison, keeps awaythe infrared spectrum value of the C-H compounds content of-D group toxic samples.
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Citations (5)
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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 |
| JP2011122968A (en) * | 2009-12-11 | 2011-06-23 | Jx Nippon Oil & Energy Corp | Lubricating oil deterioration monitoring device |
| 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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2011122968A (en) * | 2009-12-11 | 2011-06-23 | Jx Nippon Oil & Energy Corp | Lubricating oil deterioration monitoring device |
| 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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