CN110346502A - The method of 2,4-D and bentazone in water with ion chromatography - Google Patents
The method of 2,4-D and bentazone in water with ion chromatography Download PDFInfo
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- CN110346502A CN110346502A CN201910600841.9A CN201910600841A CN110346502A CN 110346502 A CN110346502 A CN 110346502A CN 201910600841 A CN201910600841 A CN 201910600841A CN 110346502 A CN110346502 A CN 110346502A
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- water
- bentazone
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- leacheate
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
Abstract
The invention discloses in a kind of water with ion chromatography 2, the method of 4-D and bentazone, direct injection analysis after selection Dionex IC-1000 ion chromatograph sample filtering, it is easy to operate, time saving low consumption, eliminate sample pre-treatments and derivative trouble, avoid the use of poisonous and harmful chemical reagent in detection process, substantially reduce analysis time, detection process is faster and accurate, sensitivity significantly improves, and it is at low cost, data reappearance is good, it can be realized fluoride in water, chloride, nitrate nitrogen, it is measured while the anion such as sulfate, there is great application value in the measurement detection field of Drinking Water and its source water, quickly reply water body suddenly accident, ensure common people's safe drinking water.It solves 2,4-D in detection Drinking Water and its source water, bentazone method has the problem of time-consuming, poor accuracy.
Description
Technical field:
The present invention relates to the methods of 2,4-D in water with ion chromatography and bentazone.
Background technique:
2,4-D (see formulas 1), bentazone (see formula 2) are common pesticide, are widely used in the removal and nocuousness of agricultural weed
The prevention and treatment of animals and plants can enter water body through approach such as Groundwater infiltration, rain drop erosion or evaporations in agricultural irrigation.Their toxicity
Though it is not high, there is certain toxic side effect to people, animal, sees the report of its polluted-water in improper use process repeatly.China exists
Joined the test request to 2,4-D, bentazone in " standards for drinking water quality " (GB5749-2006), Limited Doses with
The limit value of World Health Organization's water quality criterion is identical, respectively 0.03mg/L, 0.3mg/L.
The common detection method of 2,4-D, bentazone has gas chromatography, high performance liquid chromatography, liquid chromatography-mass spectrometry
Deng.Gas chromatography, high performance liquid chromatography, sample require extraction pre-treatment or post-column derivation, and there are certain offices for method
It is sex-limited.Sample pre-treatments and derivative trouble are eliminated using liquid chromatography-mass spectrography, sensitivity significantly improves, but instrument cost
Height, method are promoted difficult.National Standard Method samples gas-chromatography-derivatization method, and it is good that detecting instrument gas-chromatography is suitable for measurement thermal stability
And it is easy to gasify and have in gas-chromatography the compound of response.Since 2,4-D and bentazone boiling point height are not easy to gasify, before derivative
2,4-D and bentazone generation need to be easier to the derivative compound of the better methyl of volatilization gasification performance by processing.Ultrasound is needed in derivatization process
It reacts 50min and water management temperature on the rocks is at 10 DEG C -20 DEG C, standard substance need to also be operated according to the pre-treatment of sample to be derived
Change.Because of derivative complex steps and experimental operating conditions require height, and experimental result is not easy to reappear, standard working curve linear correlation system
Number is not achieved 0.995 always, is unable to satisfy test Quality Control requirement.
Summary of the invention:
The object of the present invention is to provide the methods of 2,4-D and bentazone in a kind of water with ion chromatography, select
Dionex IC-1000 ion chromatograph, direct injection analysis after sample filtering, easy to operate, time saving low consumption eliminates sample
Pre-treatment and derivative trouble, avoid the use of poisonous and harmful chemical reagent in detection process, substantially reduce analysis time,
Detection process is faster and accurate, and sensitivity significantly improves, and instrument cost is low, and data reappearance is good, can be realized fluorine in water
It measures while the anion such as compound, chloride, nitrate nitrogen, sulfate, is examined in the measurement of Drinking Water and its source water
Survey field has great application value, quickly copes with water body suddenly accident, it is ensured that common people's safe drinking water solves detection
2,4-D in water, the problem of time-consuming for bentazone method, poor accuracy.
The present invention is achieved by the following technical programs:
The method of 2,4-D and bentazone in a kind of water with ion chromatography, select DionexIC-1000 ion chromatography
Instrument matches the automatic electrolysis generator of leacheate, AS-DV autosampler, ASRS-ULTRA type suppressor, electric conductivity detector, chromatography
Condition are as follows: chromatographic column is IonPacAG19 guard column, IonPacAs19 analytical column, column temperature 29-31, preferably 30 DEG C, Chi Wen 35
DEG C, mobile phase is potassium hydroxide leacheate；Potassium hydroxide eluent concentration is 20-40mmol/L, preferably 30mmol/L；Elution
Flow velocity: 0.8-1.2mL/min, preferably 1mL/min；Suppressor electric current 100mA.
Potassium hydroxide leacheate generates high-purity KOH by the automatic electrolysis generator of leacheate with water electrolysis, cyclic regeneration yin from
Sub- trapping column eliminates the carbonate in water, measures 2,4-D and bentazone.
The acquisition and preservation of water sample, water sampling is placed in vial or polypropylene vial, and is stored in 4 DEG C and is protected from light
In environment, measurement in 2 weeks.Since 2,4-D, bentazone are degradable in chlorinated water, thus be added 5mg/L sodium thiosulfate or
0.01-0.02g ascorbic acid is added to eliminate the influence of chlorine, before measuring water sample after 0.45 μm of miillpore filter head filters directly into
Sample, 250 μ L of quantitative loop volume.
Beneficial effects of the present invention are as follows: present invention selection DionexIC-1000 ion chromatograph, after sample filtering directly
Sample introduction is analyzed, easy to operate, and time saving low consumption eliminates sample pre-treatments and derivative trouble, avoids toxic in detection process
The use of harmful chemical agents substantially reduces analysis time, and detection process is faster and accurate, and sensitivity significantly improves, and
Instrument cost is low, and data reappearance is good, can be realized the same of the anion such as fluoride in water, chloride, nitrate nitrogen, sulfate
When measure, there is great application value in the measurement detection field of Drinking Water and its source water, it is prominent quickly to cope with water body
Send out contamination accident, it is ensured that common people's safe drinking water solves 2,4-D in detection water, and time-consuming for bentazone method, and poor accuracy is asked
Topic.
Detailed description of the invention:
Fig. 1 is 2,4-D and bentazone various concentration leacheate standard solution chromatogram；
Fig. 2 is influence of the interfering ion to 2,4-D, bentazone detection in water.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
National Standard Method samples gas-chromatography-derivatization method, and detecting instrument gas-chromatography is good suitable for measurement thermal stability and is easy to
Gasify and have in gas-chromatography the compound of response.Since 2,4-D and bentazone boiling point height are not easy to gasify, derivative pre-treatment is needed
2,4-D and bentazone generation are easier to the derivative compound of the better methyl of volatilization gasification performance.Ultrasonic reaction is needed in derivatization process
At 10 DEG C -20 DEG C, standard substance need to also be operated according to the pre-treatment of sample and be performed the derivatization for 50min and water management temperature on the rocks.
Inventor's test of many times between -2016 years 2008 finds that because of derivative complex steps and experimental operating conditions require high, experiment knot
Fruit is not easy to reappear, and standard working curve linearly dependent coefficient is not achieved 0.995 always, is unable to satisfy test Quality Control requirement.
Embodiment selects instrument:
Ion chromatograph: (Dionex, model IC-1000), IonPac AG19 guard column (50mm × 4mm),
IonPacAs19 (250mm × 4mm) analytical column, the automatic electrolysis generator of EG40 leacheate, AS-DV autosampler, ASRS-
ULTRA type suppressor, electric conductivity detector assist gas: high pure nitrogen purity 99.99%, syringe 2.5-10mL, 0.45 μm of water
Phase filter.
Reagent: pure water: redistilled water or deionized water；2,4-D standard substances (U.S. Sigma, purity 99%), bentazone
(U.S. Sigma, purity 99.4%)；Hypo solution 5mg/L.
The acquisition and preservation of water sample, water sampling is placed in vial or polypropylene vial, and is stored in 4 DEG C and is protected from light
In environment, measurement in 2 weeks.Since 2,4-D, bentazone are degradable in chlorinated water, thus be added 5mg/L sodium thiosulfate or
0.01-0.02g ascorbic acid is added to eliminate the influence of chlorine, before measuring water sample after 0.45 μm of miillpore filter head filters directly into
Sample, 250 μ L of quantitative loop volume.
Embodiment 1: the method for 2,4-D and bentazone in water with ion chromatography
Dionex IC-1000 ion chromatograph is selected to produce using the automatic electrolysis generator of EG40 leacheate with water electrolysis
Raw high-purity KOH, cyclic regeneration anion trapping column eliminate the carbonate in water, measure 2,4-D and bentazone.It is respectively compared
The molten elution effect of the KOH leacheate of this 3 kinds of various concentrations of 40mol/L, 30mol/L, 20mol/L.With AS-DV automatic sampling
Device, ASRS-ULTRA type suppressor, electric conductivity detector, chromatographic condition are as follows: chromatographic column is IonPac AG19 guard column, IonPac
As19 analytical column, 30 DEG C of column temperature, 35 DEG C of Chi Wen elute flow velocity: 1.0mL/min；Suppressor electric current 100mA.
The result shows that available preferable separating effect (referring to Fig. 1) hydrogen of the KOH solution of 20mol/L, 30mol/L
Potassium oxide eluent concentration is preferably 30mmol/L, and appearance time when 30mol/L is more suitable for quickly detecting (referring to table 1).
Table 1
Embodiment 2: the investigation of interfering ion:
F is investigated-, Cl-, NO3 -, SO4 2-, ClO2 -, ClO3 -, BrO3 -Plasma does 2,4-D, bentazone measurement in water
It disturbs.The result shows that under this chromatographic condition, F-, Cl-, NO3 -, SO4 2-, ClO2 -, ClO3 -, BrO3 -Plasma all in 2,4-D, go out
Appearance before careless pine, it is separated object energy well with other conventional anions, has no interference (Fig. 2).
Embodiment 3: standard curve and detection limit
It is qualitative with the retention time of 2,4-D, bentazone in chromatogram, using external standard method, determine according to peak area size
Amount.2,4-D standard curve concentration ranges are 0.02-~1.50mg/L, and bentazone is 0.05~1.50mg/L, and curve linear is related
Coefficient is respectively as follows: 0.9994,0.9999.
Prepare 2,4-D, the bentazone mixed standard solution of 0.05mg/L, sample introduction measurement.According to being advised in U.S. EPA SW-846
Determine measuring method detection limit, MDL=3.143 δ (δ refers to replication 7 times standard deviations), 4MDL are detection limit (RQL).2,4-
D, the minimum detectability of bentazone is respectively 0.02,0.05mg/L, compared with the measurement of National Standard Method derivative gas chromatography, is directly surveyed
Determining sensitivity can reduce, but meet " standards for drinking water quality " GB5749-2006 limit value 0.03,0.3mg/L detection
Requirement.
Embodiment 4: the actual water sample rate of recovery
Acquisition Guangzhou water factory output water and source water are analyzed as test water.Water sampling is placed on glass
It in glass bottle or polypropylene vial, and is stored in the environment that 4 DEG C are protected from light, measurement in 2 weeks.Since 2,4-D, bentazone are in chlorinated water
It is degradable, therefore the sodium thiosulfate of 5mg/L is added or 0.01-0.02g ascorbic acid is added to eliminate the influence of chlorine, before measurement
Water sample direct injected, 250 μ L of quantitative loop volume after 0.45 μm of miillpore filter head filters.
2,4-D and bentazone are not detected in water sample, 0.50mg/L2,4-D and bentazone are separately added into water sample,
Select DionexIC-1000 ion chromatograph, match the automatic electrolysis generator of leacheate, AS-DV autosampler,
ASRS-ULTRA type suppressor, electric conductivity detector, chromatographic condition are as follows: chromatographic column is IonPac AG19 guard column, IonPac
As19 analytical column, 30 DEG C of column temperature, 35 DEG C of Chi Wen, mobile phase are potassium hydroxide leacheate；Potassium hydroxide eluent concentration is
30mmol/L；Elute flow velocity: 1.0mL/min；Suppressor electric current 100mA.
Potassium hydroxide leacheate generates high-purity KOH by the automatic electrolysis generator of leacheate with water electrolysis, cyclic regeneration yin from
Sub- trapping column eliminates the carbonate in water, measures 2,4-D and bentazone.
Table 2 it is found that 2,4-D and bentazone the rate of recovery 80.38~101.6%, relative standard deviation 0.4~
1.0%, 2,4-D and bentazone have the good rate of recovery and precision in water with ion chromatography of the present invention.
2 mark-on reclaims test result of table
Comparative example 1: reference implementation example 1, the difference is that ion chromatograph is DIONEX ICS1500 type ion chromatography
Analyzer is equipped with electric conductivity detector and anion suppressor；Suppressor: 5 004mm type anion suppressor of DIONEX AERS；
Inhibit electric current:: 99mA；Detector: electric conductivity detector；Detection cell temperature: 30 DEG C；Leacheate: the KOH solution of 30mmol/L.Knot
Fruit is referring to table 3.
Comparative example 2: reference implementation example 1, the difference is that ion chromatograph is the ICS3000 type ion chromatograph (U.S.
DIONEX)；Leacheate: the KOH solution of 30mmol/L.
Comparative example 3: reference implementation example 1, the difference is that ion chromatograph is 2000 leacheate of DIONEX ICS:
The KOH solution of 30mmol/L.As a result referring to table 3.
Table 3
Claims (3)
1. the method for 2,4-D and bentazone in a kind of water with ion chromatography, which is characterized in that select Dionex IC-1000
Ion chromatograph matches the automatic electrolysis generator of leacheate, AS-DV autosampler, ASRS-ULTRA type suppressor, Conductivity detection
Device, chromatographic condition are as follows: chromatographic column is IonPac AG19 guard column, IonPac As19 analytical column, 29-31 DEG C of column temperature, Chi Wen 35
DEG C, mobile phase is potassium hydroxide leacheate；Potassium hydroxide eluent concentration is 20-40mmol/L；Elute flow velocity: 0.9-
1.2mL/min；Suppressor electric current 100mA.
2. potassium hydroxide eluent concentration is 30mmol/ the method according to claim 1, wherein 30 DEG C of column temperature
L elutes flow velocity: 1.0mL/min.
3. the method according to claim 1, wherein water sampling is placed in vial or polypropylene vial,
And it is stored in the environment that 4 DEG C are protected from light, measurement in 2 weeks.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103975068A (en) * | 2011-09-13 | 2014-08-06 | 孟山都技术公司 | Methods and compositions for weed control |
| CN104387157A (en) * | 2005-09-29 | 2015-03-04 | 艾弗里斯国际私人有限公司 | Granular controlled release agrochemical compositions and process for the preparation thereof |
| CN108802243A (en) * | 2018-05-23 | 2018-11-13 | 成都市自来水有限责任公司 | The method for detecting bentazone in water, 2,4-D, 2,4- Dichlorophenols, 2,4,6- trichlorophenols, pentachlorophenol simultaneously |
-
2019
- 2019-07-04 CN CN201910600841.9A patent/CN110346502A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387157A (en) * | 2005-09-29 | 2015-03-04 | 艾弗里斯国际私人有限公司 | Granular controlled release agrochemical compositions and process for the preparation thereof |
| CN103975068A (en) * | 2011-09-13 | 2014-08-06 | 孟山都技术公司 | Methods and compositions for weed control |
| CN108802243A (en) * | 2018-05-23 | 2018-11-13 | 成都市自来水有限责任公司 | The method for detecting bentazone in water, 2,4-D, 2,4- Dichlorophenols, 2,4,6- trichlorophenols, pentachlorophenol simultaneously |
Non-Patent Citations (3)
| Title |
|---|
| 崔勇等: "离子色谱法同时分析水中酸性除草剂灭草松和2,4-滴", 《中国卫生检验杂志》 * |
| 王艳 等: "淋洗液在线发生离子色谱法同时测定水中草甘膦 2,4-D 和灭草松", 《中国卫生检验杂志》 * |
| 赵叙等: "免试剂离子色谱法同时测定饮用水中2，4-D和灭草松残留量", 《微量元素与健康研究》 * |
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