CN108548902A - A kind of chemicals rapid biodegradability test reference substance and its application method - Google Patents
A kind of chemicals rapid biodegradability test reference substance and its application method Download PDFInfo
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- CN108548902A CN108548902A CN201810671120.2A CN201810671120A CN108548902A CN 108548902 A CN108548902 A CN 108548902A CN 201810671120 A CN201810671120 A CN 201810671120A CN 108548902 A CN108548902 A CN 108548902A
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- reference substance
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of chemicals rapid biodegradability test reference substance and its application methods.The reference substance is 4 isopropyl-phenols, uses 4 isopropyl-phenols as reference substance preparation procedure control group in chemicals biodegradation test, and certain addition concentration is arranged.4 isopropyl-phenols are easily obtained, not degradable compared to existing reference substance, and instruction result is stablized, and are easy to preserve and result calculates, can effectively indicate the degrading activity of inoculum, it is ensured that fast degraded biologically test result is accurate and reliable.
Description
Technical field
The present invention relates to chemical environment risk assessment fields, are related to a kind of chemicals rapid biodegradability test reference
Object and its application method.
Background technology
China is chemicals research and development, production, using big country, and being widely used for chemicals brings Potential environmental risk.It is raw
Object degradability data are the critical datas of chemicals identification, also determine that chemicals persistence in the environment and exposure are dense
Degree.
Generally use the Organization of Economy and Cooperation Development both at home and abroad at present（OECD）The rapid biodegradability test side of formulation
Method（301 series and 310 methods）With intrinsic biodegradability test method（302 series）To measure the quick bio drop of chemicals
Solution property and intrinsic biological degradability.In above-mentioned rapid biodegradability test method, different types of degradation inoculation is used
Object（Such as activated sludge and secondary effluent）, in order to indicate the degrading activity of inoculum, effective test data is obtained, method is recommended
Using sodium benzoate, sodium acetate or aniline as reference substance preparation procedure control group, the biology of reference substance is measured under equal conditions
Degradability, with program control group 14d biological degradation rate results instruction inoculum activity and test result validity.When program pair
Reach by level, i.e., according to a group 14d biological degradation rates：DOC removal rates reach 70%（301A and 301E）, or test two generated
Oxidation carbon amounts reaches theoretical carbon dioxide yield（ThCO2）60%（301 B）Or oxygen demand reaches theoretical oxygen demand
（ThOD) 60%（301C, 301D and 301F), show that inoculum is active, experiment is effective, otherwise it is assumed that experiment is invalid, needs
Again carry out experiment.
The requirement most basic as reference substance be：（1）When being free of inoculum in test(ing) medium, it should not degrade；（2）Contain
When having inoculum, degradation can be stablized.（3）It is easily prepared.
However, OECD is in biological degradability measuring technology guide（OECD, OECD Series on the test
guidelines programme number 2, Detailed review paper on biodegradability
testing. Paris,1995,p38）It points out, due to the too easy degradation of sodium benzoate, sodium acetate or aniline, is used as reference
Object, the degradation rate of program control is hardly possible to be not achieved through level, is had never seen and is passed through level because program control is not achieved
And cause to test invalid situation.It is therefore proposed that sterilizing to test chamber, or find other relatively not degradable reference substances.
This laboratory uses OECD rapid biodegradabilities --- respirometry（301F）, determine addition inoculum and
The biological degradability of 3 kinds of aniline under two kinds of experimental conditions of inoculum, sodium benzoate and sodium acetate reference substances is not added.As a result it sends out
It is existing, it is not added with inoculum（Deionized water）When, sodium benzoate and sodium acetate can also degrade（14 d degradation rates are more than 60%）,
And sodium benzoate is in 4 kinds of test(ing) mediums for not adding inoculum（Deionized water, mineral water, tap water, aqua sterilisa）In 28 days it is complete
Degradable.It confirms that sodium benzoate is too degradable with sodium acetate, is unsuitable for indicating inoculum activity.
It finds at the conditions of the experiments described above, when testing 14 days, aniline is undegraded in the deionized water for being not added with inoculation（Drop
Solution rate is 14%）, degrade when activated sludge is as inoculum（Reach 100%）, show that aniline can refer to a certain extent
Show inoculum activity.But aniline has the disadvantage that as reference substance：（1）Aniline is unstable, easily by the oxygen in air
Oxidation generates benzoquinones, diazo salt, causes frequently replace novel agent and prepares experiment storing solution again every time；（2）Aniline contains
Nitrogen-atoms, there may be ammonia radical ions after degradation（NH3 -）, it is also possible to generate nitrate ion（NO3 -）, or both have can
It can generate, therefore which theoretical oxygen demand degradation rate calculating not can determine that using（ThODNO3Or ThODNH3）, calculated for result
Bring uncertainty.
Invention content
The object of the present invention is to provide a kind of chemicals biological degradability test reference substance and its application methods, are referred to stabilization
Show the degrading activity and test validity of inoculum, improves the quality of biodegradable test data.
To achieve the above object, the technical solution adopted by the present invention is as follows：
The chemicals rapid biodegradability test reference substance is 4- isopropyl-phenols.
The application method of above-mentioned reference substance, in OECD fast degraded biologically test methods（301 series methods）On the basis of, make
It uses 4- isopropyl-phenols as reference substance preparation procedure control group, includes the following steps：
Step 1, according to OECD fast degraded biologically test methods, setting program control group, tested material processing group, inoculum are empty
White control group and toxicity control group, reference substance 4- isopropyl-phenols are added in the test medium of program control group, and are added
Enter inoculum, with preparation procedure control group, without parallel；
Step 2, under periodic measurement program control group zmount of oxygen consumption, dissolved oxygen under tested material processing group same culture conditions
It is one or more in drop amount, carbon dioxide production or DOC abatement amounts, until off-test in 28 days；Program control group is given birth to
Object degradation rate is deducted by program control group zmount of oxygen consumption or dissolved oxygen slippage or carbon dioxide production or DOC abatement amounts
The reasonable percentage by zmount of oxygen consumption or theoretical carbon dioxide yield or organic carbon according to quantity after inoculum blank control group numerical value
Than determination.
A concentration of 1 ~ 100mg/mL of 4- isopropyl-phenols in described program control group.
The inoculum is activated sludge or secondary effluent.
Specifically, a concentration of 12 ~ 50 mg/L of 4- isopropyl-phenols in program control group（301A and 301E methods）, 12 ~ 26
mg/L（301B methods）, 100 mg/L（301C methods）, 1 ~ 4 mg/L（301D methods）, 15 ~ 40 mg/L（301F methods）.
Inoculum concentration is equal with tested material concentration for the treatment of in program control group.Wherein 301A, 301B, 301F method be 3 ~
30 mg activated sludge/L, 301E methods are 0.5 mL secondary effluents/L, and 301D methods are 0.05 ~ 5 mL secondary effluents/L, 301C
Method is 30 mg activated sludge/L；
It is required according to method, zmount of oxygen consumption is compareed handling periodic measurement program under same culture conditions with tested material（301C and
301F）, dissolved oxygen slippage（301D）, carbon dioxide production（301B and 301C）, DOC abatement（301A）, until 28 days try
Test end.
Program control group biological degradation rate presses program control group zmount of oxygen consumption（301C and 301F）Or dissolved oxygen slippage
（301D）Or carbon dioxide production（301B）Or DOC abatement amounts（301A）It is reasonable after deduction inoculum blank control group numerical value
It is determined by the percentage of zmount of oxygen consumption or theoretical carbon dioxide yield or organic carbon according to quantity.
Test validity determination method：10 day observation period of program control group（Reach 10 days after 10% from biological degradation rate
Time）Degradation rate, which reaches, passes through level.
The beneficial effects of the present invention are：
（1）Compared to existing reference substance（Sodium benzoate and sodium acetate）, 4- isopropyl-phenols are less degradable, without inoculum
Test system in it is non-degradable, containing 30 mgL-1Stablize degradation in the test system of activated sludge, can effectively indicate to connect
Kind object activity.
（2）Indicate that result is stablized.Through showing that 4- isopropyl-phenols as reference substance, are adopted with contrasting between laboralories between method
When with same source inoculum, different mechanism for testing rapid biodegradability test results are consistent；Using different vaccination object and not
Same test method, rapid biodegradability test result are consistent；Using the inoculum of separate sources, obtained test result one
It causes.
（3）Compared to existing reference substance（Aniline）, 4- isopropyl-phenols are not easily decomposed, and the stock solution of reagent and preparation is not necessarily to
Often renew, uses simplicity；4- isopropyl-phenols not fix by nitrogen atom, theoretical oxygen demand, and result of calculation determines.
（4）OECD rapid biodegradability test method Programs control validity standard is to reach within 14 days to pass through level.
Our law regulation test validity standard is to reach 10 day observation period to pass through level.Availability deciding standard is improved, is added sternly
Reference substance also maintains unanimously the active indicative function of inoculum with the result judgement of tested chemicals.
In general, it is degradable and can not effectively indicate to connect as reference substance to compensate for existing reference substance for 4- isopropyl-phenols
The problem of kind of object degrading activity, the quality of biodegradable test data is improved, it will be for the environmental risk of Scientific evaluation chemicals
Basis is provided.
Description of the drawings
The 4- isopropyl-phenol biological degradation rates that the same inoculums of Fig. 1, different mechanism for testing measure（301D）.
The 4- isopropyl-phenol biological degradation rate results that the different regions Fig. 2 inoculum, different mechanism for testing measure
（301D）.
The 4- isopropyl-phenol biological degradation rate results that the different regions Fig. 3 inoculum, different mechanism for testing measure
（301F）.
Specific implementation mode
The invention will be further described in conjunction with specific embodiments.
Embodiment 1：Three kinds of existing reference substance degradation capabilities
It acquires certain city domestic sewage treatment plant activated sludge and is not adding inoculation using OECD 301F methods as inoculum
Object and addition inoculum（Activated sludge concentration is 30 mgL-1）When, measured concentration is all the aniline of 30 mg/L, benzene first respectively
28 days biological degradation rates of sour sodium, sodium acetate.Sodium benzoate, sodium acetate decline the case where not adding inoculum and addition inoculum
Solution rate, which all reaches, passes through level（28 days degradation rates are more than 60%）, show that sodium benzoate, sodium acetate are not suitable for and indicated for reference substance
Inoculum activity.Only aniline is non-degradable when not adding inoculum（28 days degradation rates are 0）, add inoculum in the case of degrade
（28 days degradation rates are more than 60%）.
Respectively using deionized water, mineral water, tap water and aqua sterilisa as test(ing) medium, when not adding any inoculum,
The rapid biodegradability of sodium benzoate is measured using 301F methods.The results show that in the deionized water, the mine that are not added with inoculum
In spring, tap water and sterile water, sodium benzoate biological degradation rate all reaches 100%, and further formal sodium benzoate completely cannot
Indicate inoculum degrading activity.
Embodiment 2：The screening of 4- isopropyl-phenols
Certain city domestic sewage treatment plant activated sludge is acquired as inoculum, using 301F methods, be not added with inoculum and
Add inoculum（Activated sludge concentration is 30 mgL-1）Under the conditions of, determine the 4- t-octyls that addition concentration is all 30 mg/L
The biological degradability of phenol, 4- isopropyl anilines, 4- nitroanilines, 5 kinds of 4- isopropyl-phenols, ethylene glycol chemicals.As a result table
Bright, in the presence of no inoculum, only ethylene glycol is degraded（28 days degradation rates 90%）, 4- tert-octyl phenols, 4- cumenes
Amine, 4- nitroanilines, 4- isopropyl-phenols are undegraded（28 days degradation rates are 0）.
And in 30 mgL-1In activated sludge test, ethylene glycol and 4- isopropyl-phenols reach fast degraded biologically and pass through
It is horizontal.4- tert-octyl phenols, 4- isopropyl anilines, 4- nitroanilines not up to pass through level.
Should not be biodegradable without reference substance in the presence of inoculum, and reached a certain level in activated sludge presence or activity
When, it can be biodegradable.Accordingly, 4- isopropyl-phenols are suitable as reference substance.
Embodiment 3：Instruction stability of the 4- isopropyl-phenols as reference substance
Different mechanism for testing uniformly use Nanjing city east secondary effluent from sewage treatment plant as inoculum carry out 301D test into
Row contrasting between laboralories, wherein 4- isopropyl-phenols add a concentration of 2 mg/L.Comparison result shows 4- isopropyl-phenol conducts
Reference substance, when using same source inoculum, different mechanism for testing rapid biodegradability test results are consistent（301D is tested
In, 28 d degradation rates are 60% ~ 85%）, see Fig. 1.
Different mechanism for testing use location secondary effluent from sewage treatment plant（2 laboratories use 301D methods, 4- different
Propylphenol adds a concentration of 2 mg/L）Or activated sludge（7 laboratories use 301F methods, the addition of 4- isopropyl-phenols dense
Degree is 18.6 ~ 35.2 mg/L）It is compared as between inoculum the method for developing, comparison result shows using different regions inoculum
（Activated sludge or secondary effluent）From different test methods, rapid biodegradability test result is consistent（28 d degradation rates, 301D
It is 93.5% ~ 100% for 88% ~ 89%, 301F）, see Fig. 2 and Fig. 3.
Embodiment 4：The measurement of tested material
Using 301F methods, 6 processing are set, 4- isopropyl-phenols measure the biological degradability of certain tested material as reference substance,
Experiment setting is as follows：
Bottle 1 and bottle 2（Tested material processing）：Tested material（Respectively 32.8 mg/L and 32.8 mg/L）+ inoculum（30 mg
SS/L）；
Bottle 3 and bottle 4（Inoculum blank control）：Inoculum（30 mg SS/L）；
Bottle 5（Program compares）：Reference substance（40 mg/L）+ inoculum（30 mg SS/L）；
Bottle 6（Toxicity control）：Tested material（32.0 mg /L）+ reference substance（40 mg/L）+ inoculum（30 mg SS/L）.
Open BOD analyzers（OxiTop®Control 6, WTW, Germany）, start blender（It is coated containing polytetrafluoroethylene (PTFE)
Magnetic stirrer）, under dark condition, it is 22 °C ± 1 °C to keep temperature, measures zmount of oxygen consumption daily.After 28 days respectively
Zmount of oxygen consumption in 6 assay flasks is read, and calculates biological degradation rate.
Measurement result shows：10 day observation period biological degradation rate of program control group is 90.5%（> 60%）；Toxicity control 14
Its biological degradation rate is 54.3%（> 25%）, tested material processing zmount of oxygen consumption is more than inoculum blank control oxygen consumption during experiment
The 60% of amount, tested material is to inoculum unrestraint effect.In conclusion this experiment is effective.Under the conditions of efficiency test, tested material
The biological degradation rate of 24d is 0 %.
Claims (5)
1. a kind of chemicals rapid biodegradability tests reference substance, which is characterized in that the chemicals rapid biodegradability
Test reference substance is 4- isopropyl-phenols.
2. the application method of chemicals rapid biodegradability test reference substance described in claim 1, which is characterized in that in OECD
On the basis of fast degraded biologically test method, using 4- isopropyl-phenols as reference substance preparation procedure control group.
3. the application method of chemicals rapid biodegradability test reference substance according to claim 2, which is characterized in that packet
Include following steps：
Step 1, according to OECD fast degraded biologically test methods, setting program control group, tested material processing group, inoculum are empty
White control group and toxicity control group, reference substance 4- isopropyl-phenols are added in the test medium of program control group, and are added
Enter inoculum；
Step 2, under periodic measurement program control group zmount of oxygen consumption, dissolved oxygen under tested material processing group same culture conditions
It is one or more in drop amount, carbon dioxide production or DOC abatement amounts, until off-test in 28 days；Program control group is given birth to
Object degradation rate is deducted by program control group zmount of oxygen consumption or dissolved oxygen slippage or carbon dioxide production or DOC abatement amounts
The reasonable percentage by zmount of oxygen consumption or theoretical carbon dioxide yield or organic carbon according to quantity after inoculum blank control group numerical value
Than determination.
4. the application method of chemicals rapid biodegradability test reference substance according to claim 3, which is characterized in that institute
State a concentration of 1 ~ 100mg/mL of 4- isopropyl-phenols in program control group.
5. the application method of chemicals rapid biodegradability test reference substance according to claim 3, which is characterized in that institute
The inoculum stated is activated sludge or secondary effluent.
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| US20030220436A1 (en) * | 2002-01-22 | 2003-11-27 | Gencer Mehmet A. | Biodegradable polymers containing one or more inhibitors and methods for producing same |
| WO2005007587A1 (en) * | 2003-07-11 | 2005-01-27 | Universität Stuttgart | Method for the biological breakdown of effluent containing nitroaromatics |
| CN101626829A (en) * | 2007-03-21 | 2010-01-13 | Omya发展股份公司 | Process for the removal of endocrine disrupting compounds |
| US20180070825A1 (en) * | 2014-10-21 | 2018-03-15 | uBiome, Inc | Method and system for microbiome-derived characterization, diagnostics and therapeutics for conditions associated with functional features |
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