CN109239240B - Gas chromatography for determining trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water - Google Patents
Gas chromatography for determining trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water Download PDFInfo
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- CN109239240B CN109239240B CN201811412345.2A CN201811412345A CN109239240B CN 109239240 B CN109239240 B CN 109239240B CN 201811412345 A CN201811412345 A CN 201811412345A CN 109239240 B CN109239240 B CN 109239240B
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- 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
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- G—PHYSICS
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- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Abstract
The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a gas chromatography for determining trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water. The method comprises the steps of enriching a target compound in drinking water by using a novel adsorbent benzoate-magnesium aluminum type hydrotalcite, dissolving the adsorbent by using acid to realize complete elution of the target compound, efficiently extracting the compound by using a small amount of organic solvent, and performing rapid analysis and determination by using a gas chromatography after derivatization. The novel adsorbent adopted by the method realizes the rapid and efficient adsorption of the target object by adopting a dispersed solid-phase extraction mode, and can save a large amount of adsorption time compared with a solid-phase extraction mode; the complete desorption of the target can be realized by using the acid to dissolve the adsorbent; only a small amount of organic solvent is suitable for extraction, and compared with a liquid-liquid extraction method which needs a large amount of organic solvent, the method has the advantages of safety, environmental protection and economic advantage.
Description
Technical Field
The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a gas chromatography for determining trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water.
Background
2,4, 6-trichlorophenol (CAS:88-06-2) and trichloropyridinol (CAS:37439-34-2) are two important insecticides, wherein the trichloropyridinol is an intermediate for synthesizing pesticides such as chlorpyrifos. Because the carboxyl with stronger polarity is contained in the water, trace two substances can be dissolved and stably and durably exist in the water, thereby becoming a source of harmful chemical substances for polluting drinking water.
At present, the two trace substances in drinking water are detected and researched less, the main methods are a liquid chromatography and a chromatography-mass spectrometry combined method, and the pretreatment method mainly focuses on adopting two methods of liquid-liquid extraction and solid-phase extraction. However, the liquid-liquid extraction method has the defect that a large amount of organic solvent is required; the solid phase extraction method has the problems of limited types of usable solid phase extraction fillers, few types of commercial products and troublesome operation.
In recent years, the inventor researches and researches the preparation and modification of Layered Double hydroxide metal oxide (LDHs) Layered materials extensively by research teams, and gradually applies the LDHs Layered materials to the field of trace substance detection on the basis of the LDHs Layered materials. Two notable features of LDHs materials are: space adjustability between the laminate layers and replaceability of the intercalated anions. Based on the method, people can modify the LDHs material according to the difficulty of replaceability of intercalation anions of the LDHs material and the adjustability of the distance between the layers, and then select different types of intercalation anions according to the requirements of practical application to modify the material to obtain a functional material with novel application.
The inventor carries out an adsorption experiment on the two compounds in water by using the benzoate-magnesium-aluminum type hydrotalcite adsorbent in the previous research, and the result shows that the benzoate-magnesium-aluminum type hydrotalcite adsorbent has a good adsorption effect on a target object. On the basis, the inventor further optimizes the performance and application method of the developed adsorbent for enriching the target compound in water, and establishes a gas chromatography for detecting trace 2,4, 6-trichlorophenol and trichloropyridine sodium in drinking water by using benzoate-magnesium-aluminum type hydrotalcite as the adsorbent.
Disclosure of Invention
In order to overcome the defect that a large amount of organic solvent is needed in the liquid-liquid extraction method in the detection pretreatment of trace 2,4, 6-trichlorophenol and trichloropyridine sodium alcoholate in the existing drinking water; the invention also provides a method for detecting 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water by using the gas chromatography, which is based on the novel adsorbent, has the defects of few types of available solid phase extraction products and large time consumption in the adsorption process.
The invention achieves the above object by the following technical means.
A gas chromatography for measuring trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water is characterized by comprising the following steps:
adsorption of the compound of step 1: adding a certain amount of drinking water into a separating funnel, adding 0.20g of benzoate-magnesium-aluminum type hydrotalcite adsorbent, and oscillating for a certain time to enable the adsorbent to adsorb trace 2,4, 6-trichlorophenol and trichloropyridine sodium alcoholate targets in the water;
step 3, extraction and derivatization of compounds: adding a certain amount of anhydrous sodium sulfate and an organic solvent into the centrifugal tube for extraction, performing vortex and centrifugation, separating supernatant into a derivatization bottle, adding a derivatization reagent into the derivatization bottle, sealing, uniformly mixing, and putting the mixture into a constant-temperature water bath to complete an esterification and derivatization process;
analytical testing of the compound of step 4: a saturated sodium bicarbonate solution and a certain amount of solid sodium bicarbonate powder were added to the derivatization vial, vortexed and sonicated, and the upper organic solution was aspirated, filtered and analyzed by gas chromatography.
Wherein the content of the first and second substances,
the drinking water amount in the step 1 is 200mL, and the shaking time is 15 min.
The hydrochloric acid solution in the step 2 is prepared from concentrated hydrochloric acid and water according to the volume ratio of 1:1, and the dosage is 2.00 mL.
In the step 3, 2.0g of anhydrous sodium sulfate, 5.00mL of methyl tert-butyl ether as an organic extraction solvent and 0.10mL of acetic anhydride solution as a derivatization reagent are added, the water bath temperature is 50 ℃, and the derivatization time is 30 min.
The saturated sodium bicarbonate solution in the step 4 is 2.0mL, the solid sodium bicarbonate powder is 0.20g, the vortex time is 30s to 60s, the ultrasonic time is 2min, the filter membrane is an organic phase filter membrane, and the pore diameter is 0.22 μm.
In the above steps, the vortex is 1min to 2min, and the centrifugation is carried out for 3min at the rotating speed of 4500 rpm.
The analytical test conditions for gas chromatography used for the determination were:
a) a chromatographic column: HP-5 capillary column, 30m × 0.32mm, 0.25 μm film thickness; constant flow mode, column flow rate: 2.00 mL/min.
b) Sample inlet temperature: 250 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 2 mu L of the solution; tail gas blowing flow: 60 mL/min.
c) Temperature rising procedure: 60 deg.C (keeping for 2min), heating to 180 deg.C at 10 deg.C/min (keeping for 1min), and heating to 300 deg.C at 30 deg.C/min (keeping for 3.0 min).
d) A detector: electron capture detector, temperature: 325 ℃.
e) Carrier gas: high-purity nitrogen (the purity is more than or equal to 99.999%).
The invention screens the adsorption effects of various modified layered adsorption materials and roasted products thereof on two targets, and finds that the modified material taking benzoate ions as anions has good selective adsorption performance on the two targets, so that the modified material is selected as an alternative adsorbent and is applied and developed. In addition, in the process of research and development of the method, the inventor researches and optimizes the consumption of the adsorbent, the selection and the proportion of the extraction solvent, the selection and the optimization of a target substance derivatization method, the selection and the optimization of chromatographic separation conditions and other factors according to the characteristics of the target substance to be adsorbed, and provides a relatively excellent detection method on the basis.
Meanwhile, in consideration of quantitative accuracy of the target object, the method quantifies the target object by adopting the matrix correction curve on the premise that the isotope of the target object cannot be obtained so as to quantify the target object by an isotope internal standard method, so that systematic errors are eliminated as much as possible, and the quantitative accuracy is improved.
The invention has the advantages that:
(1) the novel adsorbent benzoate-magnesium-aluminum type hydrotalcite adopted by the invention can rapidly adsorb trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in water by adopting a dispersed solid-phase extraction mode, and can save a large amount of adsorption time compared with a solid-phase extraction mode;
(2) according to the invention, by utilizing the characteristic that benzoate-magnesium-aluminum type hydrotalcite adsorbent can be dissolved in acid, the adsorbent after adsorbing the target is dissolved by using a hydrochloric acid solution, so that the target can be completely desorbed from the adsorbent;
(3) the method is only suitable for using a small amount of organic solvent as the extraction solvent of the target object, and has the advantages of safety, environmental protection and economic advantages compared with the liquid-liquid extraction method which needs to use a large amount of organic solvent.
Drawings
FIG. 1 is a chromatogram of a matrix standard solution of 2,4, 6-trichlorophenol and sodium trichloropyridinol in the embodiment, with a concentration of 200.0. mu.g/L, wherein 1 is 2,4, 6-trichlorophenol and 2 is sodium trichloropyridinol.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
(1) The reagent medicines involved in the embodiments of the present invention are as follows:
2,4, 6-trichlorophenol and trichloropyridinol sodium solid standard substance with purity of more than or equal to 98.0 percent, Shanghai Aladdin Biotechnology GmbH;
acetic anhydride, methyl tert-butyl ether, anhydrous sodium sulfate, sodium bicarbonate, analytically pure, national pharmaceutical group;
hydrochloric acid, super pure, group of national medicine; the water is first-grade water meeting the GB/T6682 specification.
(2) The instruments involved in the examples of the present invention are as follows:
KH-75A type electric heating constant temperature air-blast drying oven, Kangheng instruments ltd, Guangzhou;
model 7890B gas chromatograph, electron capture detector, agilent technologies, usa.
(3) Analysis and test conditions of a gas chromatograph:
a) a chromatographic column: HP-5 capillary column, 30m × 0.32mm, 0.25 μm film thickness; constant flow mode, column flow rate: 2.00 mL/min.
b) Sample inlet temperature: 250 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 2 mu L of the solution; tail gas blowing flow: 60 mL/min.
c) Temperature rising procedure: 60 deg.C (keeping for 2min), heating to 180 deg.C at 10 deg.C/min (keeping for 1min), and heating to 300 deg.C at 30 deg.C/min (keeping for 3.0 min).
d) A detector: electron capture detector, temperature: 325 ℃.
e) Carrier gas: high-purity nitrogen (the purity is more than or equal to 99.999%).
(4) Preparation of matrix calibration curve and determination of detection limit and quantitative limit
Accurately weighing the two compounds, dissolving with methanol to constant volume, and making into standard stock solution with concentration of 1000mg/L, and storing at-4 deg.C. When in use, the standard stock solution is gradually diluted by deionized water to prepare standard use solution with the concentration gradient of 10.0 mug/L, 20.0 mug/L, 40.0 mug/L, 100.0 mug/L and 200.0 mug/L.
Taking five 500mL separating funnels, adding 200mL deionized water into the separating funnels, respectively taking 5.00mL standard use liquid, then adding 0.20g benzoate-magnesium aluminum type hydrotalcite adsorbent into each funnel, and oscillating for 15min to make the adsorbent adsorb; adding water in a separating funnel into a 50mL centrifuge tube with a plug, centrifuging at the rotating speed of 4500rpm for 3min to separate the solid adsorbent from the aqueous solution and discard the supernatant, combining all the lower-layer solid adsorbents into one centrifuge tube, adding 2.00mL of hydrochloric acid solution diluted by 1 time into the centrifuge tube, and realizing desorption of the adsorbed target after the solid adsorbent is dissolved; adding 2.0g of anhydrous sodium sulfate into the centrifuge tube, adding 5.0mL of methyl tert-butyl ether, whirling for 1min, centrifuging at 4500rpm for 3min, separating 2.00mL of supernatant into a derivatization bottle, adding 0.10mL of acetic anhydride solution, sealing, uniformly mixing, standing in a water bath at 50 ℃ for derivatization for 30min, and finishing the esterification derivatization process; to the above derivatization bottle was added 2.0mL of saturated sodium bicarbonate solution and 0.20g of solid powder of sodium bicarbonate to the above solution, vortexed for 30s and sonicated for 2min, and the upper organic solution was aspirated through an organic phase filter having a pore size of 0.22 μm, and then analyzed and tested by gas chromatography.
And (3) taking the concentration of the 2,4, 6-trichlorophenol and the sodium trichloropyridinol in the sample solution as an X axis, and taking the chromatographic peak area of the 2,4, 6-trichlorophenol and the sodium trichloropyridinol on a gas chromatograph as a Y axis to draw a matrix standard curve and use the matrix standard curve for external standard method quantification.
The triple value of the signal-to-noise ratio S/N is taken as the detection limit of the method (LOD, LOD is 3S/N), the ten times of the signal-to-noise ratio S/N is taken as the quantification limit of the method (LOQ, LOQ is 10S/N), and the detection limit and the quantification limit of each compound in water are calculated by combining the volume of the added matrix.
The relevant parameters of the matrix standard curve, LOD and LOQ are shown in Table 1.
TABLE 1 information on standard curves, detection limits and quantitation limits of 2,4, 6-trichlorophenol and sodium trichloropyridinol substrate
(5) Synthesis of benzoate-magnesium-aluminum type hydrotalcite adsorbent
In order to enable those skilled in the art to repeatedly carry out the relevant experiments of the present invention, a method for synthesizing the benzoate-magnesium-aluminum type hydrotalcite adsorbent, which is a key substance used in the present invention, is now provided as follows:
the reagent and the drug related to the synthesis of the adsorbent are as follows:
sodium benzoate, analytically pure, group of national drugs;
Mg6Al2(OH)16CO3·4H2o, analytical grade, Aldrich, usa.
② the apparatus related to the synthesis of the adsorbent is as follows:
an EXCEL type microwave digestion instrument, Shanghai Yao Instrument science and technology development Co., Ltd., digestion tank volume of 100 mL; microwave muffle furnace (sintering furnace), CEM corporation, usa; model VD53 vacuum drying cabinet, German Bindd technologies; HJ-5 multifunctional constant temperature stirrer, Kantai Ronghua Instrument manufacturing Co., Ltd; FS-12 type separatory funnel oscillator, New optical technology, Japan; 3K-15 type centrifuge, sigma technologies, germany; BF518945C-1 model box resistance furnace (muffle furnace), Saimer Feishell science, USA.
The concrete steps of synthesizing the adsorbent are as follows:
(a) roasting: mg of purchased Mg-Al type hydrotalcite6Al2(OH)16CO3·4H2Placing O in a muffle furnace, heating at a heating rate of 5 ℃/min to 500 ℃, and roasting for 6h to obtain a roasted product Mg6Al2O8(OH)2；
(b) Weighing: 5.761g of sodium benzoate intercalation agent and 7.236g of roasted product Mg are weighed in a microwave digestion tank6Al2O8(OH)2。
(c) Microwave crystallization hydrothermal synthesis: boiling deionized water and keeping for 30min, adding 100mL into the microwave digestion tank filled with the intercalation agent and the roasting product, sealing, placing the microwave digestion tank into a microwave digestion instrument, and performing microwave heating at 150 ℃ for 30min to complete synthesis;
(d) washing and drying: pouring out all solids and liquid in the microwave tank, heating and stirring with deionized water boiled for more than 30min to remove carbon dioxide, shaking, washing, centrifuging, vacuum drying at 90 deg.C for 12h, grinding, and storing.
Example 1
In this example 1, tap water was used as a sample matrix to perform a standard recovery experiment to verify the feasibility of the method of the present invention, and the treatment was performed according to the following steps:
1. adsorption of the compound:
adding 200mL of tap water into a 500mL separating funnel, adding 5.00mL of two compound standard solutions with the concentrations of 10.0 mu g/L, 20.0 mu g/L and 200.0 mu g/L respectively into the tap water, preparing and obtaining a three-level six-parallel standard sample, adding 0.20g of benzoate-magnesium-aluminum type hydrotalcite adsorbent, and oscillating for 15min to enable the adsorbent to adsorb;
2. desorption of the compound:
adding water in a separating funnel into a 50mL centrifuge tube with a plug, centrifuging at the rotating speed of 4500rpm for 3min to separate the solid adsorbent from the aqueous solution and discard the supernatant, combining all the lower-layer solid adsorbents into one centrifuge tube, adding 2.00mL of hydrochloric acid solution diluted by 1 time into the centrifuge tube, and realizing desorption of the adsorbed compound after the solid adsorbent is dissolved;
3. extraction and derivatization of compounds:
adding 2.0g of anhydrous sodium sulfate into the centrifuge tube, adding 5.00mL of methyl tert-butyl ether, whirling for 1min, centrifuging at 4500rpm for 3min, taking the supernatant into a derivatization bottle, adding 0.10mL of acetic anhydride solution, sealing, uniformly mixing, standing in a water bath at 50 ℃ for derivatization for 30min, and finishing the esterification derivatization process;
4. and (3) analysis, test and verification:
to the above derivatization bottle was added 2.0mL of saturated sodium bicarbonate solution and 0.20g of solid powder of sodium bicarbonate to the above solution, vortexed for 30s and sonicated for 2min, and the upper organic solution was aspirated through an organic phase filter having a pore size of 0.22 μm, and then analyzed and tested by gas chromatography.
The parameters relevant to the spiking recovery experiment of example 1 are shown in Table 2.
Table 2 experimental data on the addition concentration and recovery rate of the tap water sample (n ═ 6)
Example 2
In this example 2, a standard recovery experiment was performed using well water as a sample matrix to verify the feasibility of the method of the present invention, and the treatment was performed according to the following steps:
1. adsorption of the compound:
adding 200mL of well water into a 500mL separating funnel, adding 5.00mL of two compound standard solutions with the concentrations of 10.0 mu g/L, 20.0 mu g/L and 200.0 mu g/L respectively to prepare a three-level six-parallel standard sample, adding 0.20g of benzoate-magnesium-aluminum type hydrotalcite adsorbent, and oscillating for 15min to adsorb the adsorbent;
2. desorption of the compound:
adding water in a separating funnel into a 50mL centrifuge tube with a plug, centrifuging at the rotating speed of 4500rpm for 3min to separate the solid adsorbent from the aqueous solution and discard the supernatant, combining all the lower-layer solid adsorbents into one centrifuge tube, adding 2.00mL of hydrochloric acid solution diluted by 1 time into the centrifuge tube, and realizing desorption of the adsorbed compound after the solid adsorbent is dissolved;
3. extraction and derivatization of compounds:
adding 2.0g of anhydrous sodium sulfate into the centrifuge tube, adding 5.00mL of methyl tert-butyl ether, whirling for 1min, centrifuging at 4500rpm for 3min, taking the supernatant into a derivatization bottle, adding 0.10mL of acetic anhydride solution, sealing, uniformly mixing, standing in a water bath at 50 ℃ for derivatization for 30min, and finishing the esterification derivatization process;
4. and (3) analysis, test and verification:
to the above derivatization bottle was added 2.0mL of saturated sodium bicarbonate solution and 0.20g of solid powder of sodium bicarbonate to the above solution, vortexed for 30s and sonicated for 2min, and the upper organic solution was aspirated through an organic phase filter having a pore size of 0.22 μm, and then analyzed and tested by gas chromatography.
The parameters relevant to the spiking recovery experiment of example 2 are shown in Table 3.
Table 3 experimental data on the addition concentration and recovery rate of the well water sample (n ═ 6)
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the spirit of the invention, which falls within the scope of the invention, and therefore the scope of the patent of the invention shall be governed by the appended claims.
Claims (6)
1. A gas chromatography for measuring trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water is characterized by comprising the following steps:
(1) adsorption of the compound: adding a certain amount of drinking water into a separating funnel, adding 0.20g of benzoate-magnesium-aluminum type hydrotalcite adsorbent into the drinking water, and oscillating for a certain time to enable the adsorbent to adsorb trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in the water;
(2) desorption of the compound: transferring the mixture of the adsorbent and water in the separating funnel into a centrifuge tube with a plug, centrifuging to separate the solid adsorbent from the aqueous solution and discard the supernatant, combining all the lower-layer solid adsorbents into one centrifuge tube, and adding a certain amount of hydrochloric acid solution to dissolve the solid adsorbent to complete desorption of the adsorbed compound;
(3) extraction and derivatization of compounds: adding a certain amount of anhydrous sodium sulfate and an organic solvent into the centrifugal tube for extraction, performing vortex and centrifugation, taking supernatant liquid to a derivatization bottle, adding a derivatization reagent into the supernatant liquid, sealing, uniformly mixing, and putting the mixture in a constant-temperature water bath to finish the derivatization process;
(4) analytical testing of compounds: a saturated sodium bicarbonate solution and a certain amount of solid sodium bicarbonate powder are added to the derivatization flask, vortexed and sonicated, the upper organic solution is aspirated, filtered and subjected to analytical testing using gas chromatography under the following conditions:
a) a chromatographic column: HP-5 capillary column, 30m × 0.32mm, 0.25 μm film thickness; constant flow mode, column flow rate: 2.00 mL/min;
b) sample inlet temperature: 250 ℃; and (3) sample introduction mode: no shunt sampling; sample introduction amount: 2 mu L of the solution; tail gas blowing flow: 60 mL/min;
c) temperature rising procedure: keeping at 60 deg.C for 2min, heating to 180 deg.C at a rate of 10 deg.C/min, keeping for 1min, heating to 300 deg.C at a rate of 30 deg.C/min, and keeping for 3.0 min;
d) a detector: electron capture detector, temperature: 325 ℃;
e) carrier gas: high-purity nitrogen with the purity more than or equal to 99.999 percent.
2. The gas chromatography for measuring the trace 2,4, 6-trichlorophenol and the trichloropyridinol sodium in the drinking water as claimed in claim 1, wherein the drinking water amount in the step (1) is 200mL, and the shaking time is 15 min.
3. The gas chromatography method for determining the trace amount of 2,4, 6-trichlorophenol and sodium trichloropyridinol in drinking water as claimed in claim 1, wherein the hydrochloric acid solution in step (2) is prepared from concentrated hydrochloric acid and water according to a volume ratio of 1:1, and the dosage is 2.00 mL.
4. The gas chromatography method for measuring trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water according to claim 1, wherein the anhydrous sodium sulfate added in step (3) is 2.0g, the organic extraction solvent is 5.00mL of methyl tert-butyl ether, the derivatization reagent is 0.10mL of acetic anhydride solution, the water bath temperature is 50 ℃, and the derivatization time is 30 min.
5. The gas chromatography method for measuring trace 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water as claimed in claim 1, wherein the saturated sodium bicarbonate solution in step (4) is 2.0mL and the solid powder of sodium bicarbonate is 0.20g, the vortex time is 30s to 60s, the ultrasonic time is 2min, the filter membrane for filtration is an organic phase filter membrane, and the pore size is 0.22 μm.
6. The gas chromatography method for measuring the trace amount of 2,4, 6-trichlorophenol and trichloropyridinol sodium in drinking water according to claim 1, wherein the vortexing is performed at a speed of 4500rpm for 3min and 1min to 2 min.
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