CN108548902B - Reference substance for testing rapid biodegradability of chemicals and use method thereof - Google Patents
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- 238000012360 testing method Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000126 substance Substances 0.000 title claims abstract description 33
- 239000013558 reference substance Substances 0.000 title claims abstract description 15
- YQUQWHNMBPIWGK-UHFFFAOYSA-N 4-isopropylphenol Chemical group CC(C)C1=CC=C(O)C=C1 YQUQWHNMBPIWGK-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002054 inoculum Substances 0.000 claims abstract description 58
- 238000006065 biodegradation reaction Methods 0.000 claims abstract description 25
- 231100000209 biodegradability test Toxicity 0.000 claims abstract description 15
- 239000012925 reference material Substances 0.000 claims abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 22
- 239000010802 sludge Substances 0.000 claims description 15
- 230000036284 oxygen consumption Effects 0.000 claims description 14
- 238000011282 treatment Methods 0.000 claims description 13
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 238000010998 test method Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 231100000419 toxicity Toxicity 0.000 claims description 3
- 230000001988 toxicity Effects 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 19
- 238000006731 degradation reaction Methods 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 22
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 12
- 239000004299 sodium benzoate Substances 0.000 description 12
- 235000010234 sodium benzoate Nutrition 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 8
- 239000001632 sodium acetate Substances 0.000 description 8
- 235000017281 sodium acetate Nutrition 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 description 3
- ISAVYTVYFVQUDY-UHFFFAOYSA-N 4-tert-Octylphenol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(O)C=C1 ISAVYTVYFVQUDY-UHFFFAOYSA-N 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- LRTFPLFDLJYEKT-UHFFFAOYSA-N para-isopropylaniline Chemical compound CC(C)C1=CC=C(N)C=C1 LRTFPLFDLJYEKT-UHFFFAOYSA-N 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- -1 ammonium ions Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011081 inoculation Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- YHZQOKUDQQISEW-UHFFFAOYSA-N 4-Cumylphenol Natural products C1=CC(C(C)C)=CC=C1C1=CC=C(O)C=C1 YHZQOKUDQQISEW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical compound [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 231100000290 environmental risk assessment Toxicity 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 231100001267 hazard identification Toxicity 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000008223 sterile water Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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Abstract
本发明公开了一种化学品快速生物降解性测试参比物及其使用方法。所述参比物为4‑异丙基苯酚，在化学品生物降解测试中使用4‑异丙基苯酚作为参比物制备程序对照组，并设置一定添加浓度。4‑异丙基苯酚易于获取，相比于现有参比物不易降解，指示结果稳定，易于保存和结果计算，可有效指示接种物的降解活性，确保快速生物降解测试结果准确可靠。
The invention discloses a chemical rapid biodegradability test reference material and a use method thereof. The reference substance is 4-isopropylphenol, and in the chemical biodegradation test, 4-isopropylphenol is used as the reference substance preparation program control group, and a certain concentration is set. 4-isopropylphenol is easy to obtain, and is not easy to degrade compared with the existing reference materials. The indication results are stable, and it is easy to store and calculate the results. It can effectively indicate the degradation activity of the inoculum, and ensure accurate and reliable rapid biodegradation test results.
Description
技术领域technical field
本发明涉及化学品环境风险评估领域，涉及一种化学品快速生物降解性测试参比物及其使用方法。The invention relates to the field of chemical environmental risk assessment, and relates to a chemical rapid biodegradability test reference material and a use method thereof.
背景技术Background technique
我国是化学品研发、生产、使用大国，化学品的广泛使用带来了潜在环境风险。生物降解性数据是化学品危害鉴定的关键数据，也决定了化学品在环境中的持久性及暴露浓度。my country is a big country in the research and development, production and use of chemicals, and the extensive use of chemicals has brought potential environmental risks. Biodegradability data is the key data for chemical hazard identification, and also determines the persistence and exposure concentration of chemicals in the environment.
目前国内外普遍采用经济合作与发展组织（OECD）制定的快速生物降解性测试方法（301系列和310方法）和固有生物降解性测试方法（302系列）来测定化学品的快速生物降解性和固有生物降解性。在上述快速生物降解性测试方法中，采用了不同类型的降解接种物（如活性污泥和二级出水），为了指示接种物的降解活性，获得有效的测试数据，方法推荐使用苯甲酸钠、醋酸钠或苯胺作为参比物制备程序对照组，同等条件下测定参比物的生物降解性，用程序对照组14d 生物降解率结果指示接种物活性及测试结果有效性。当程序对照组14d 生物降解率达到通过水平，即：DOC去除率达到70%（301A和301E），或试验产生的二氧化碳量达到理论二氧化碳产生量（ThCO2） 的60%（301 B），或耗氧量达到理论需氧量（ThOD) 的60%（301C、301D和301F)，表明接种物具有活性，试验有效，否则认为试验无效，需重新开展试验。At present, the rapid biodegradability test methods (301 series and 310 methods) and inherent biodegradability test methods (302 series) developed by the Organization for Economic Cooperation and Development (OECD) are widely used at home and abroad to determine the rapid biodegradability and inherent biodegradability of chemicals. Biodegradability. In the above rapid biodegradability test method, different types of degradable inoculum (such as activated sludge and secondary effluent) are used. In order to indicate the degradation activity of the inoculum and obtain valid test data, the method recommends using sodium benzoate, acetic acid Sodium or aniline was used as the reference material to prepare the program control group, and the biodegradability of the reference material was measured under the same conditions. The 14-day biodegradation rate of the program control group was used to indicate the activity of the inoculum and the validity of the test results. When the biodegradation rate of the program control group reaches the passing level on 14 days, that is: the DOC removal rate reaches 70% (301A and 301E), or the amount of carbon dioxide produced in the test reaches 60% of the theoretical carbon dioxide production (ThCO 2 ) (301 B), or Oxygen consumption reaches 60% of theoretical oxygen demand (ThOD) (301C, 301D and 301F), indicating that the inoculum is active and the test is effective, otherwise the test is considered invalid and the test needs to be re-launched.
作为参比物最基本的要求为：（1）试验介质中不含接种物时，不应发生降解；（2）含有接种物时，可稳定降解。（3）易于制备。The most basic requirements as a reference material are: (1) when the test medium does not contain inoculum, it should not degrade; (2) when it contains inoculum, it can degrade stably. (3) Easy to prepare.
然而，OECD在生物降解性测试技术指南中（OECD，OECD Series on the testguidelines programme number 2, Detailed review paper on biodegradabilitytesting. Paris,1995,p38）指出，由于苯甲酸钠、醋酸钠或苯胺太容易降解，其作为参比物，程序对照的降解率几乎不可能达不到通过水平，从未见过因程序对照达不到通过水平而导致试验无效的情形。因此建议对试验容器灭菌，或者寻找其他相对不易降解的参比物。However, the OECD pointed out in the Technical Guidelines for Biodegradability Testing (OECD, OECD Series on the
本实验室采用OECD快速生物降解性——呼吸计量法（301F），测定了添加接种物和不添加接种物两种试验条件下苯胺、苯甲酸钠与醋酸钠3种参比物的生物降解性。结果发现，未添加接种物（去离子水）时，苯甲酸钠和醋酸钠也能发生降解（14 d降解率大于60%），且苯甲酸钠在不添加接种物的4种试验介质（去离子水、矿泉水、自来水、灭菌水）中28天完全降解。证实苯甲酸钠与醋酸钠太易降解，不适于指示接种物活性。In this laboratory, the OECD rapid biodegradability-respirometry method (301F) was used to determine the biodegradability of aniline, sodium benzoate and sodium acetate under two test conditions with and without inoculum added. The results showed that sodium benzoate and sodium acetate could also be degraded without the addition of inoculum (deionized water) (14 d degradation rate was greater than 60%). , mineral water, tap water, sterilized water) completely degraded in 28 days. It was confirmed that sodium benzoate and sodium acetate were too easily degraded to indicate inoculum activity.
在上述试验条件下发现，试验14天时，苯胺在未添加接种的去离子水中未降解（降解率为14%），在活性污泥作为接种物时发生降解（达到100%），表明苯胺一定程度上可以指示接种物活性。但是苯胺作为参比物存在如下缺点：（1）苯胺不稳定，极易被空气中的氧气氧化生成苯醌、偶氮盐，导致需频繁更换新试剂并每次重新制备试验储备液；（2）苯胺含有氮原子，降解后可能产生氨根离子（NH3 -），也可能生成硝酸根离子（NO3 -），或者两者都有可能生成，因此降解率计算不能确定使用哪个理论需氧量（ThODNO3还是ThODNH3），为结果计算带来不确定性。Under the above test conditions, it was found that aniline was not degraded in deionized water without inoculation (degradation rate was 14%) at the 14th day of the test, and degraded (reached 100%) when activated sludge was used as inoculum, indicating that aniline was to a certain extent. Inoculum activity can be indicated on the . However, aniline as a reference material has the following disadvantages: (1) aniline is unstable, and is easily oxidized by oxygen in the air to generate benzoquinone and azo salts, resulting in frequent replacement of new reagents and preparation of test stock solutions every time; (2) ) Aniline contains nitrogen atoms, which may generate ammonium ions (NH 3 - ), nitrate ions (NO 3 - ), or both after degradation, so the calculation of the degradation rate cannot determine which theoretical aerobic to use amount (ThOD NO3 or ThOD NH3 ), which brings uncertainty to the calculation of the result.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种化学品生物降解性测试参比物及其使用方法，以稳定指示接种物的降解活性及试验有效性，提高生物降解测试数据的质量。The purpose of the present invention is to provide a chemical biodegradability test reference material and its use method, so as to stably indicate the degradation activity and test validity of the inoculum, and improve the quality of the biodegradation test data.
为实现上述目的，本发明采用的技术方案如下：For achieving the above object, the technical scheme adopted in the present invention is as follows:
所述化学品快速生物降解性测试参比物为4-异丙基苯酚。The chemical rapid biodegradability test reference is 4-isopropylphenol.
上述参比物的使用方法，在OECD快速生物降解测试方法（301系列方法）基础上，使用4-异丙基苯酚作为参比物制备程序对照组，包括以下步骤：The use method of the above reference substance, based on the OECD rapid biodegradation test method (301 series method), uses 4-isopropylphenol as the reference substance preparation procedure control group, including the following steps:
步骤一，按照OECD快速生物降解测试方法，设置程序对照组、受试物处理组、接种物空白对照组和毒性对照组，将参比物4-异丙基苯酚添加到程序对照组的试验培养基中，并加入接种物，以制备程序对照组，无平行；
步骤二，在与受试物处理组相同培养条件下定期测量程序对照组氧消耗量、溶解氧下降量、二氧化碳生成量或者DOC消减量中的一种或多种，直至28天试验结束；程序对照组生物降解率按程序对照组氧消耗量、或溶解氧下降量、或二氧化碳生成量、或DOC消减量扣除接种物空白对照组数值后占理论氧消耗量、或理论二氧化碳产生量、或有机碳按量的百分比确定。
所述程序对照组中4-异丙基苯酚浓度为1~100mg/mL。The concentration of 4-isopropylphenol in the program control group was 1-100 mg/mL.
所述的接种物为活性污泥或者二级出水。The inoculum is activated sludge or secondary effluent.
具体地，程序对照组中4-异丙基苯酚浓度为12~50 mg/L（301A和301E方法），12~26mg/L（301B方法），100 mg/L（301C方法），1~4 mg/L（301D方法），15~40 mg/L（301F方法）。Specifically, the concentration of 4-isopropylphenol in the program control group was 12~50 mg/L (301A and 301E methods), 12~26 mg/L (301B method), 100 mg/L (301C method), 1~4 mg/L (method 301D), 15~40 mg/L (method 301F).
程序对照组中接种物浓度与受试物处理浓度相等。其中301A、301B、301F方法为3~30 mg活性污泥/L，301E方法为0.5 mL二级出水/L，301D方法为0.05~5 mL二级出水/L，301C方法为30 mg活性污泥/L；The concentration of the inoculum in the program control group was equal to that of the test substance treatment. Among them, 301A, 301B, 301F method is 3~30 mg activated sludge/L, 301E method is 0.5 mL secondary effluent/L, 301D method is 0.05~5 mL secondary effluent/L, 301C method is 30 mg activated sludge /L;
根据方法要求，在与受试物处理相同培养条件下定期测量程序对照氧消耗量（301C和301F）、溶解氧下降量（301D）、二氧化碳生成量（301B和301C）、DOC消减（301A），直至28天试验结束。According to the method requirements, periodically measure the program control oxygen consumption (301C and 301F), dissolved oxygen decline (301D), carbon dioxide production (301B and 301C), DOC reduction (301A) under the same culture conditions as the test substance treatment, until the end of the 28-day trial.
程序对照组生物降解率按程序对照组氧消耗量（301C和301F）、或溶解氧下降量（301D）、或二氧化碳生成量（301B）、或DOC消减量（301A）扣除接种物空白对照组数值后占理论氧消耗量、或理论二氧化碳产生量、或有机碳按量的百分比确定。The biodegradation rate of the program control group is based on the oxygen consumption (301C and 301F) of the program control group, or the amount of dissolved oxygen decline (301D), or the amount of carbon dioxide generation (301B), or the amount of DOC reduction (301A) minus the value of the blank control group of the inoculum Afterwards, it is determined as a percentage of the theoretical oxygen consumption, or the theoretical carbon dioxide production, or the organic carbon.
试验有效性判定方法：程序对照组10天观察期（自生物降解率达到10%之后的10天时间）降解率达到通过水平。Method for determining the validity of the test: the program control group has a 10-day observation period (10 days after the biodegradation rate reaches 10%), and the degradation rate reaches the passing level.
本发明的有益效果在于：The beneficial effects of the present invention are:
（1）相比于现有参比物（苯甲酸钠与醋酸钠），4-异丙基苯酚较不易降解，在不含接种物的试验体系中不降解，在含有30 mg·L-1活性污泥的试验体系中稳定降解，可以有效指示接种物活性。( 1 ) Compared with the existing reference substances (sodium benzoate and sodium acetate), 4-isopropylphenol is not easily degraded, and does not degrade in the test system without inoculum. The sludge is stably degraded in the test system, which can effectively indicate the activity of the inoculum.
（2）指示结果稳定。经方法间和实验室间比对表明，4-异丙基苯酚作为参比物，采用同一来源接种物时，不同测试机构快速生物降解性测试结果一致；采用不同接种物与不同测试方法，快速生物降解性测试结果一致；采用不同来源的接种物，得到的测试结果一致。(2) Indicates that the result is stable. The inter-method and inter-laboratory comparisons show that when 4-isopropylphenol is used as a reference material, when the same source inoculum is used, the rapid biodegradability test results of different test institutions are consistent; The biodegradability test results were consistent; using inoculum from different sources, the test results were consistent.
（3）相比于现有参比物（苯胺），4-异丙基苯酚不易分解，试剂和制备的贮备液无需经常换新，使用简便；4-异丙基苯酚不含氮原子，理论需氧量固定，计算结果确定。(3) Compared with the existing reference substance (aniline), 4-isopropylphenol is not easy to decompose, the reagent and the prepared stock solution do not need to be replaced frequently, and it is easy to use; 4-isopropylphenol does not contain nitrogen atoms, theoretically The oxygen demand is fixed, and the calculation result is determined.
（4）OECD快速生物降解性测试方法中程序对照有效性标准为14天达到通过水平。本方法规定试验有效性标准为10天观察期达到通过水平。提高了有效性判定标准，加严了参比物对接种物活性的指示作用，也与受试化学品的结果判定保持了一致。(4) In the OECD rapid biodegradability test method, the program control effectiveness standard is 14 days to reach the pass level. This method stipulates that the test validity standard is the 10-day observation period to reach the pass level. The effectiveness judgment standard has been improved, and the indication function of the reference substance on the inoculum activity has been tightened, which is also consistent with the result judgment of the tested chemical.
总体而言，4-异丙基苯酚作为参比物弥补了现有参比物易降解而无法有效指示接种物降解活性的问题，提升了生物降解测试数据的质量，将为科学评估化学品的环境风险提供基础。In general, 4-isopropylphenol as a reference material makes up for the problem that the existing reference material is easy to degrade and cannot effectively indicate the degradation activity of the inoculum, and improves the quality of the biodegradation test data, which will serve as a basis for scientific evaluation of chemicals. Environmental risks provide the basis.
附图说明Description of drawings
图1 同一接种物、不同测试机构测定的4-异丙基苯酚生物降解率（301D）。Figure 1 4-Isopropylphenol biodegradation rate (301D) measured by the same inoculum and different testing institutions.
图2 不同地区接种物、不同测试机构测定的4-异丙基苯酚生物降解率结果（301D）。Fig. 2 Results of 4-isopropylphenol biodegradation rate (301D) measured by inoculum in different regions and by different testing institutions.
图3 不同地区接种物、不同测试机构测定的4-异丙基苯酚生物降解率结果（301F）。Figure 3 Results of 4-isopropylphenol biodegradation rate (301F) measured by inoculum in different regions and by different testing institutions.
具体实施方式Detailed ways
结合具体实施例对本发明作进一步说明。The present invention will be further described with reference to specific embodiments.
实施例1：三种现有参比物降解能力Example 1: Degradability of Three Existing References
采集某城市生活污水处理厂活性污泥作为接种物，使用OECD 301F方法，在不添加接种物与添加接种物（活性污泥浓度为30 mg·L-1）时，分别测定浓度皆为30 mg/L的苯胺、苯甲酸钠、醋酸钠的28天生物降解率。苯甲酸钠、醋酸钠在未加接种物和添加接种物的情况下降解率都达到通过水平（28天降解率超过60%），表明苯甲酸钠、醋酸钠不适用用于参比物指示接种物活性。只有苯胺在未加接种物时不降解（28天降解率为0），添加接种物情况下降解（28天降解率超过60%）。Activated sludge was collected from an urban domestic sewage treatment plant as inoculum, and the OECD 301F method was used. When no inoculum was added or when inoculum was added (the concentration of activated sludge was 30 mg·L -1 ), the concentrations were determined to be 30 mg respectively. 28-day biodegradation rate of aniline, sodium benzoate and sodium acetate per L. The degradation rates of sodium benzoate and sodium acetate both reached the passing level without adding inoculum or adding inoculum (the degradation rate exceeded 60% in 28 days), indicating that sodium benzoate and sodium acetate are not suitable for use as reference materials to indicate inoculum activity . Only aniline did not degrade without inoculum (0 degradation rate at 28 days), and degraded with inoculum addition (degradation rate over 60% at 28 days).
分别以去离子水、矿泉水、自来水和灭菌水作为试验介质，不添加任何接种物时，使用301F方法测定苯甲酸钠的快速生物降解性。结果显示，在未添加接种物的去离子水、矿泉水、自来水和无菌水中，苯甲酸钠生物降解率都达到100%，进一步正式苯甲酸钠完全不能指示接种物降解活性。Deionized water, mineral water, tap water and sterilized water were used as test media, respectively, and the 301F method was used to determine the rapid biodegradability of sodium benzoate without adding any inoculum. The results showed that in deionized water, mineral water, tap water and sterile water without inoculum, the biodegradation rate of sodium benzoate reached 100%, and further formal sodium benzoate could not indicate the degradation activity of inoculum at all.
实施例2：4-异丙基苯酚的筛选Example 2: Screening of 4-isopropylphenol
采集某城市生活污水处理厂活性污泥作为接种物，使用301F方法，在未添加接种物及添加接种物（活性污泥浓度为30 mg·L-1）条件下，测定了添加浓度皆为30 mg/L的4-叔辛基苯酚、4-异丙基苯胺、4-硝基苯胺、4-异丙基苯酚、乙二醇5种化学品的生物降解性。结果表明，当无接种物存在时，只有乙二醇发生降解（28天降解率90%），4-叔辛基苯酚、4-异丙基苯胺、4-硝基苯胺、4-异丙基苯酚均未降解（28天降解率为0）。Collecting activated sludge from an urban domestic sewage treatment plant as inoculum, using the 301F method, under the conditions of no inoculum addition and addition of inoculum (activated sludge concentration of 30 mg·L -1 ), the added concentration was determined to be 30 mg·L -1 . Biodegradability of five chemicals, 4-tert-octylphenol, 4-isopropylaniline, 4-nitroaniline, 4-isopropylphenol, and ethylene glycol in mg/L. The results showed that when there was no inoculum, only ethylene glycol was degraded (90% degradation rate in 28 days), 4-tert-octylphenol, 4-isopropylaniline, 4-nitroaniline, 4-isopropyl Phenol was not degraded (0 degradation rate at 28 days).
而在30 mg·L-1活性污泥试验中，乙二醇和4-异丙基苯酚达到快速生物降解通过水平。4-叔辛基苯酚、4-异丙基苯胺、4-硝基苯胺均未达到通过水平。In the 30 mg·L -1 activated sludge test, ethylene glycol and 4-isopropylphenol reached the fast biodegradation passing level. 4-tert-octylphenol, 4-isopropylaniline, 4-nitroaniline did not reach the passing level.
无接种物存在时参比物应不生物降解，而在活性污泥存在或活性达到一定程度时，可以被生物降解。据此，4-异丙基苯酚适合作为参比物。The reference substance should not biodegrade in the absence of inoculum, but can be biodegraded in the presence or activity of activated sludge to a certain extent. Accordingly, 4-isopropylphenol is suitable as a reference.
实施例3：4-异丙基苯酚作为参比物的指示稳定性Example 3: Indicative stability of 4-isopropylphenol as a reference
不同测试机构统一使用南京市城东污水处理厂二级出水作为接种物开展301D试验进行实验室间比对，其中4-异丙基苯酚添加浓度为2 mg/L。比对结果表明，4-异丙基苯酚作为参比物，采用同一来源接种物时，不同测试机构快速生物降解性测试结果一致（301D试验中，28 d降解率为60%~85%），见图1。Different testing institutions uniformly used the secondary effluent of Nanjing Chengdong Sewage Treatment Plant as the inoculum to carry out the 301D test for inter-laboratory comparison, in which the concentration of 4-isopropylphenol was 2 mg/L. The comparison results show that when 4-isopropylphenol is used as the reference material, when the same source inoculum is used, the rapid biodegradability test results of different test institutions are consistent (in the 301D test, the 28-day degradation rate is 60%~85%), see
不同测试机构使用所在地区污水处理厂二级出水（2家实验室使用301D方法，4-异丙基苯酚添加浓度为2 mg/L）或活性污泥（7家实验室使用301F方法， 4-异丙基苯酚添加浓度为18.6 ~ 35.2 mg/L）作为接种物开展方法间比对，比对结果表明，采用不同地区接种物（活性污泥或二级出水）与不同测试方法，快速生物降解性测试结果一致（28 d降解率，301D为88%~89%，301F为93.5%~100%），见图2和图3。Different testing institutions use the secondary effluent of the sewage treatment plant in their area (2 laboratories use the 301D method, the concentration of 4-isopropylphenol is 2 mg/L) or activated sludge (7 laboratories use the 301F method, 4- Cumylphenol was added at a concentration of 18.6-35.2 mg/L) as the inoculum to carry out the comparison between methods. The comparison results showed that the inoculum (activated sludge or secondary effluent) in different regions and different test methods were used for rapid biodegradation. The performance test results are consistent (28 d degradation rate, 301D is 88%~89%, 301F is 93.5%~100%), see Figure 2 and Figure 3.
实施例4：受试物的测定Example 4: Determination of Test Substances
采用301F方法，设置6个处理，4-异丙基苯酚作为参比物，测定某受试物的生物降解性，试验设置如下：The 301F method was used, 6 treatments were set, and 4-isopropylphenol was used as the reference substance to determine the biodegradability of a test substance. The test settings were as follows:
-瓶1和瓶2（受试物处理）：受试物（分别为32.8 mg /L和32.8 mg /L）+ 接种物（30mg SS/L）；-
-瓶3和瓶4（接种物空白对照）：接种物（30 mg SS/L）；-
-瓶5（程序对照）：参比物（40 mg/L）+ 接种物（30 mg SS/L）；- bottle 5 (program control): reference (40 mg/L) + inoculum (30 mg SS/L);
-瓶6（毒性对照）：受试物（32.0 mg /L）+ 参比物（40 mg/L）+ 接种物（30 mg SS/L）。- Bottle 6 (toxicity control): test substance (32.0 mg/L) + reference substance (40 mg/L) + inoculum (30 mg SS/L).
打开BOD测定仪（OxiTop® Control 6，WTW，德国），启动搅拌器（含聚四氟乙烯包覆的磁性搅拌子），在黑暗条件下，保持温度为22°C ± 1°C，每天测定氧消耗量。28天后分别读取6个试验瓶中氧消耗量，并计算生物降解率。Turn on the BOD analyzer (OxiTop ® Control 6, WTW, Germany), start the stirrer (with a teflon-coated magnetic stir bar), maintain the temperature at 22°C ± 1°C in the dark, and measure every day oxygen consumption. After 28 days, the oxygen consumption in the 6 test bottles was read, and the biodegradation rate was calculated.
测定结果表明：程序对照组10天观察期生物降解率为90.5%（> 60%）；毒性对照14天生物降解率为54.3%（> 25%），试验期间受试物处理氧消耗量大于接种物空白对照氧消耗量的60%，受试物对接种物无抑制效应。综上所述，本试验有效。在有效试验条件下，受试物24d的生物降解率为0 %。The measurement results showed that the biodegradation rate of the program control group during the 10-day observation period was 90.5% (> 60%); the 14-day biodegradation rate of the toxic control group was 54.3% (> 25%), and the oxygen consumption of the test substance treatment during the test was greater than that of the inoculation. 60% of the oxygen consumption of the blank control, the test substance had no inhibitory effect on the inoculum. In conclusion, this test is effective. Under the effective test conditions, the biodegradation rate of the test substance 24d was 0 %.
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