CN102768144B - Prepare the method for maximum allocated in water (WAFs) solution and the device of use thereof - Google Patents

Prepare the method for maximum allocated in water (WAFs) solution and the device of use thereof Download PDF

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Publication number
CN102768144B
CN102768144B CN201210234071.9A CN201210234071A CN102768144B CN 102768144 B CN102768144 B CN 102768144B CN 201210234071 A CN201210234071 A CN 201210234071A CN 102768144 B CN102768144 B CN 102768144B
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solution
water
wafs
stirred vessel
tested material
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CN201210234071.9A
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CN102768144A (en
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吴晟旻
刘济宁
王蕾
吉贵祥
石利利
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Nanjing Institute of Environmental Sciences MEP
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Nanjing Institute of Environmental Sciences MEP
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Abstract

The invention discloses method and device that in a kind of water used in the test of chemicals Aquatic Ecotoxicology prepared by maximum allocated solution.Be insoluble in water by a certain amount of or be partially soluble in water (solubleness < 100mg/L, 25 DEG C) tested material directly join in appropriate experimental water, start stirring apparatus, make tested material under the drive of stirring vane, fully contact mixing with test water.After stirring a period of time, sample in a certain time interval, use suitable instrument to detect, until the physicochemical property index characterizing solution system stability tends towards stability.Tested material reaches maximum allocated in water, respectively in solution alternately reaches equilibrium state, i.e. WAFs solution.Open valve, the WAFs solution in stirrer middle layer is flowed directly into holding device.Described method and device go for various be insoluble in water or be partially soluble in water particle, powder, sheet or blocks of solid and liquid, thick liquid and various potpourri WAFs solution preparation.The WAFs solution of preparation, respectively contacts fully, is evenly distributed, stable system, effectively improves accuracy and the accuracy of the test of chemicals Aquatic Ecotoxicology.

Description

Prepare the method for maximum allocated in water (WAFs) solution and the device of use thereof
Technical field
The present invention relates to chemicals Aquatic Ecotoxicology field tests, the maximum allocated method (WAFs) in a kind of employing water that particularly relates to prepares the method for tested material solution, and the device that the method uses.
Background technology
In Aquatic Ecotoxicology test, the tested material solution preparation of indissoluble thing is difficult point and the focus of research all the time.Some are insoluble in the chemical substance of water due to poorly water-soluble, someone adopts the method for stirring, tested material is fully mixed with test water, but because undissolved tested material is floating, suspend or be deposited in water, tested aquatic organism is eaten by mistake, touch tested material all may produce contingency death, thus makes experimental result produce deviation.Therefore someone adopts the method for mild heat to impel tested material rapid solution, but this method likely changes the physicochemical property of tested material, and reduces the dissolved oxygen concentration in solution, thus affects test result.Also someone adopts the method adding cosolvent to dissolve to impel tested material, but the issuable composite toxicity of the interaction between tested material and cosolvent, and the toxicity that the use of cosolvent may impel tested material impurities dissolves to produce all likely brings impact to the Ecology toxicity assessment of tested material.Somebody uses immobilization technology, and the material utilizing activated charcoal, zeolite etc. to have high-specific surface area fixes tested material, and this technology improves the contact area of tested material and water, facilitates the dissolving of tested material in water.But due to tested material active principle and the impurity different solubility in water, the solution eluted is mostly is components that solubleness is larger, thus test findings is made to produce deviation.In addition, elution process usually needs the longer test period, is unfavorable for the popularization of this technology.
Summary of the invention
The technical problem to be solved in the present invention is that in the test of existing Aquatic Ecotoxicology, the preparation method of tested material solution easily causes test findings to produce deviation, and experiment effect is poor, and some solution preparation method costs are high, the cycle long, be not easy to apply.
For solving the problems of the technologies described above, the present invention establishes a kind of technology of preparing of tested material solution, the technical scheme adopted is: the method preparing maximum allocated in water (WAFs) solution, comprise following steps: step one: tested material directly added in the experimental water be contained in stirred vessel, start stirring apparatus, under room temperature 23 ~ 25 DEG C of conditions, stir at least 24 hours; Step 2: after the aforementioned liquid be stirred is left standstill 1 hour under the condition of room temperature 23 ~ 25 DEG C, at different time points, liquid is sampled respectively, and the relevant physical and chemical index of sampling solution is detected by detecting instrument, the interval time of described sampling is not less than 30 minutes; Step 3: the numerical value of the turbidity of described solution system or total organic carbon (TOC) or other change of the physicochemical property index characterizing solution system stability within the described time interval close to zero time, namely think and be mixed with maximum allocated (WAFs) solution in the water of this tested material in stirrer; When solution left standstill is after 8 hours, solution system still cannot reach balance, and agitating solution 24 hours, then repeats the process of step 2 again, until solution system reaches balance; Step 4: the WAFs solution being positioned at aforementioned stirred vessel middle layer is flowed directly into holding device to required amount, directly can add hydrobiont in described holding device, carry out the test of chemicals ecological toxicology.
For improving the stirring efficiency of the inventive method further, in step one, when in stirred vessel, whirlpool height is not less than liquid surface static height 1/10th.
As a modification of the present invention scheme, the detecting instrument used in step 2 is nephelometer, total organic carbon analyzer.Described nephelometer, total organic carbon analyzer are existing instrument.
The device that the method preparing maximum allocated in water (WAFs) solution uses, comprises support, is fixedly connected on stirring apparatus below support, and be positioned at the holding device below stirring apparatus; Described stirring apparatus comprises power source, gear unit, stirring vane and stirred vessel, the input end of the output terminal connection for transmission unit of described power source, the output terminal of described gear unit stretches in stirred vessel from the top of stirred vessel, and connecting the stirring vane being positioned at stirred vessel, the bottom of described stirred vessel is provided with stopple coupon and downpipe; The water inlet of described stopple coupon is positioned at the middle part of stirred vessel.
As a modification of the present invention scheme, described gear unit comprises the coupling shaft, rotating shaft head and the drive link that connect in turn from top to bottom.
For improving the mixing effect of device further, described stirring vane is sheet semicircular arc.
Advantage of the present invention is: described method cost is low, effective, cycle is short, be easy to widely used solution preparation, indissoluble or the tested material being partially soluble in water can be reached maximum allocated at aqueous phase by the method, form the stabilizing solution system respectively balanced each other, i.e. WAFs solution, thus the accuracy and the accuracy that effectively improve the test of chemicals Aquatic Ecotoxicology.
Accompanying drawing explanation
Fig. 1 is the structural representation of apparatus of the present invention.
1-support 2-power source 3-coupling shaft 4-rotating shaft head 5-set bolt 6-drive link 7-stirring vane 8-stirrer 9-stopple coupon 10-downpipe 11-stopple coupon valve 12-downpipe valve 13-holding device.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described.
As shown in Figure 1, device of the present invention comprises support 1, be fixedly connected on stirring apparatus below support 1, and is positioned at the holding device 13 below stirring apparatus; Described stirring apparatus comprises power source 2, gear unit, stirring vane 7 and stirred vessel 8, and described gear unit comprises the coupling shaft 3, rotating shaft head 4 and the drive link 6 that connect in turn from top to bottom; The output terminal of described power source 2 connects coupling shaft 3, drive link stretches in stirred vessel 8 through the upper cover plate of stirred vessel 8, and connect the stirring vane 7 being positioned at stirred vessel 8, described upper cover plate is fixed by the sidewall of set bolt 5 with stirred vessel 8, and the bottom of described stirred vessel 8 is also provided with stopple coupon 9 and downpipe 10; The water inlet of described stopple coupon 9 is positioned at the middle part of stirred vessel 8, and stopple coupon 9 is provided with stopple coupon valve 11, and described downpipe 10 is provided with downpipe valve 12.Described stirring vane 7 is sheet semicircular arc.
The tested material checked is needed generally to be insoluble in water or to be partially soluble in water, be i.e. solubleness < 100mg/L, 25 DEG C in test.
Stirred vessel volume is fixed, the test water total amount at every turn putting into stirred vessel 8 is consistent, because most tested material swims in the water surface or is deposited in the bottom, therefore the relative equilibrium time of top and bottom can be longer, so the water inlet of stopple coupon 9 to be arranged on the middle part of stirred vessel 8, be convenient to select center section solution test, the schedule speed of testing can be accelerated on the basis ensureing experimental result accuracy
Method of the present invention, comprises following steps:
Step one: unclamp set bolt 5, the upper cover plate of stirred vessel is opened, the tested material taken directly being joined holds in the stirred vessel 8 of experimental water, under room temperature (23 ~ 25 DEG C) condition, start stirring apparatus, under stirring vane 7 rotarily drives, impel tested material fully to contact mixing with test water, stirring intensity be that in stirrer, whirlpool height is not less than liquid surface static height 1/10th, mixing time be stir continuously 24h and more than.
Step 2: after being stirred, sets to zero stirring vane 7 rotating speed, and solution system is left standstill one hour under the condition of room temperature 23 ~ 25 DEG C, and then sample respectively the liquid left standstill at different time points, the interval time of described sampling is not less than 30 minutes; During sampling, open stopple coupon valve 11, sampled by the middle layer of stopple coupon 9 from stirred vessel 8;
Step 3: the numerical value of the turbidity of described solution system or total organic carbon (TOC) or other change of the physicochemical property index characterizing solution system stability within the described time interval close to zero time, namely think and be mixed with maximum allocated (WAFs) solution in the water of this tested material in stirrer; When solution left standstill is after 8 hours, solution system still cannot reach balance, and agitating solution 24 hours, then repeats the process of step 2 again, until detect that solution system reaches balance;
Step 4: open stopple coupon valve 11, the WAFs solution in stirred vessel 8 middle layer flows directly into holding device 13 from stopple coupon 9, regulates described stopple coupon valve 11, controls aquifer yield, until reach required amount of solution in described holding device 13; Directly can add hydrobiont in described holding device 13, carry out the test of chemicals ecological toxicology; Open valve 12, surplus solution is discharged from downpipe 10.

Claims (6)

1. prepare the method for maximum allocated in water (WAFs) solution, it is characterized in that, comprise following steps:
Step one: tested material directly added in the experimental water be contained in stirred vessel, starts stirring apparatus, under room temperature 23 ~ 25 DEG C of conditions, stirs at least 24 hours;
Step 2: after the aforementioned liquid be stirred is left standstill 1 hour under the condition of room temperature 23 ~ 25 DEG C, at different time points, liquid is sampled respectively, and the relevant physical and chemical index of sampling solution is detected by detecting instrument, the interval time of described sampling is not less than 30 minutes, described in be sampled as the center section of described liquid;
Step 3: the numerical value of the turbidity of described solution system or total organic carbon (TOC) or other change of the physicochemical property index characterizing solution system stability within the described time interval close to zero time, namely think and be mixed with maximum allocated (WAFs) solution in the water of this tested material in stirrer; When solution left standstill is after 8 hours, solution system still cannot reach balance, and agitating solution 24 hours, then repeats the process of step 2 again, until solution system reaches balance;
Step 4: the WAFs solution being positioned at aforementioned stirred vessel middle layer is flowed directly into holding device to required amount, directly can add hydrobiont in described holding device, carry out the test of chemicals ecological toxicology.
2. the method preparing maximum allocated in water (WAFs) solution according to claim 1, is characterized in that: in step one, when in stirred vessel, whirlpool height is not less than liquid surface static height 1/10th.
3. the method preparing maximum allocated in water (WAFs) solution according to claim 1, is characterized in that: the detecting instrument used in step 2 is nephelometer, total organic carbon analyzer.
4. adopt the device of any one method in claim 1-3, it is characterized in that: comprise support, be fixedly connected on stirring apparatus below support, and be positioned at the holding device below stirring apparatus; Described stirring apparatus comprises power source, gear unit, stirring vane and stirred vessel, the input end of the output terminal connection for transmission unit of described power source, the output terminal of described gear unit stretches in stirred vessel from the top of stirred vessel, and connecting the stirring vane being positioned at stirred vessel, the bottom of described stirred vessel is provided with stopple coupon and downpipe; The water inlet of described stopple coupon is positioned at the middle part of stirred vessel.
5. device according to claim 4, is characterized in that: described gear unit comprises the coupling shaft, rotating shaft head and the drive link that connect in turn from top to bottom.
6. device according to claim 4, is characterized in that: described stirring vane is sheet semicircular arc.
CN201210234071.9A 2012-07-09 2012-07-09 Prepare the method for maximum allocated in water (WAFs) solution and the device of use thereof Expired - Fee Related CN102768144B (en)

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