CN109212062A - A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater - Google Patents
A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater Download PDFInfo
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- CN109212062A CN109212062A CN201811050582.9A CN201811050582A CN109212062A CN 109212062 A CN109212062 A CN 109212062A CN 201811050582 A CN201811050582 A CN 201811050582A CN 109212062 A CN109212062 A CN 109212062A
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- nicotinonitrile
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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
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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
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Abstract
The present invention relates to wastewater recycle technical fields, more particularly to a kind of method with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, the detection method comprises the following steps: 1) solution is prepared: weighing 1-10g sample in 50-250mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1, and it is settled to graduation mark with ultrapure water, sufficiently shake up；2) production of standard curve；3) concentration calculation:
Description
Technical field
The present invention relates to wastewater recycle technical fields, and in particular to a kind of nicotinonitrile in HPLC detection industrial wastewater
With the method for 3- picoline.
Background technique
Industrial wastewater (industrial wastewater) includes production waste water and production waste, refers to industrial production mistake
The waste water and waste liquid generated in journey, wherein containing the industrial production materials outflowed with water, intermediate product, byproduct and producing
The pollutant generated in journey.With the rapid development of industry, the type and quantity of waste water rapidly increase, to the pollution of water body also day
Become extensive and serious, threatens the health and safety of the mankind.Therefore, for protection environment, city is compared in the processing of industrial wastewater
The processing of sewage is even more important.
Nicotinonitrile, also known as nicotinic acid nitrile, molecular formula C6H4N2, molecular weight 104.11 are a kind of white crystals.It can rise
China is dissolved in ethyl alcohol, ether, chloroform, benzene and petroleum ether, is slightly dissolved in water.
The invention discloses a kind of method with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, we
Method is quick compared to the method enhanced convenience that document has, and has very high repeatability and reproducibility.
At present Chinese patent CN104406967A disclose it is a kind of detect ammonia nitrogen in industrial waste water content reagent and its inspection
Survey method, the reagent include the first reagent and the second reagent, and by weight, the first reagent includes methylene blue to the component
10~15 parts, 20~25 parts of pyridine, 60~80 parts of potassium iodide, 50~80 parts of sodium thiosulfate, 70~75 parts of trinitro- salicylic acid,
40~60 parts of inorganic salts, 20~35 parts of phosphoric acid diamines, 60~95 parts of amide；Its preparation is to mix each ingredient；Second reagent
Including 30~40 parts of ammonium chloride, 50~70 parts of sodium metavanadate, 50~65 parts of sulfate, 40~50 parts of sodium tetraborate, nitro phosphorus ammonium
70~80 parts, 50~75 parts of inorganic acid；Its preparation is to mix each ingredient.Detection method: sample to be tested is added in the first reagent
In, after placing 2~3min, the second reagent is added, places 4~5min, observation solution colour variation.The detection reagent energy of the invention
Whether the ammonia-nitrogen content in enough quickly detection industrial wastewaters is exceeded.
Rarely has the report of the method for nicotinonitrile and 3- picoline in HPLC detection industrial wastewater in the prior art.
Summary of the invention
In order to overcome the shortcomings of the prior art, industrial wastewater is detected with HPLC the object of the present invention is to provide a kind of
The method of middle nicotinonitrile and 3- picoline effectively compensates for defect of the existing technology.
The invention discloses a kind of method with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, we
Method is quick compared to the method enhanced convenience that document has, and has very high repeatability and reproducibility.
Laboratory apparatus:
Liquid chromatogram model: Agilent1260
Assay balance model: BSA224S-CW
Volumetric flask: sky wave 100ml
Chromatographic column: C18 reverse chromatograms column
Experiment parameter:
Mobile phase A: water+sodium heptanesulfonate+triethylamine+glacial acetic acid=80mL+0.1g+0.02mL+0.1mL.
Mobile phase=(20-80) % mobile phase A+(10-90) % acetonitrile
Wavelength: 265nm flow velocity: 0.8mL/min solvent: water sample volume: 10-40 μ L
In order to achieve the above purpose, it is achieved by the following technical programs:
A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, the detection method is including such as
Under several steps:
1) solution is prepared: 1-10g sample is weighed in 50-250mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1,
And it is settled to graduation mark with ultrapure water, sufficiently shake up；
2) production of standard curve；
3) concentration calculation:
Preferably, accuracy is 0.1mg when sample weighs in the step 1).
Preferably, the making step of standard curve is as follows:
A) mother liquor A: nicotinonitrile 0.02-0.1g, 3- picoline 0.01-0.03g standard specimen merging certain volume is weighed
Volumetric flask in, it is spare with solvent dissolved dilution to scale；
B) it standard specimen solution 1: is added in 100mL volumetric flask from 25mL is pipetted in mother liquor A, is settled to scale with solvent, for use；
C) standard specimen solution 2: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 1, be settled to scale with solvent,
For use；
D) standard specimen solution 3: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 2, be settled to scale with solvent,
For use；
E) standard specimen solution 4: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 3, be settled to scale with solvent,
For use；
F) it hand sampling: first uses ultrapure water rinse sample introduction needle 20-25 times, then with the certain number of sample to be tested rinse sample introduction needle
Sample introduction afterwards, Loading sequence are from low concentration to high concentration, and control sample volume is certain.
Preferably, volumetric flask volume is 100mL in the step a).
Preferably, sample volume is (20-40) μ L in the step f).
It preferably, is 20-25 times with sample to be tested rinse number in the step f).
Wherein:
Concentration of the C-to each component in sample introduction solution, μ g/mL.
M1-sample quality, g；
The total dilution volume of N-sample, mL
Using above-mentioned technical solution, beneficial effects of the present invention are as follows:
The invention discloses a kind of method with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, we
Method is quick compared to the method enhanced convenience that existing literature has, and has very high repeatability and reproducibility.The method of the prior art
Detection needs the longer time, and therefore, the present invention has higher detection efficiency.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiment of the present invention, the common skill in this field
Art personnel every other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, the detection method is including such as
Under several steps:
1) solution prepare: weigh 1g sample in 50mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1, and with surpass
Pure water is settled to graduation mark, sufficiently shakes up；
2) production of standard curve；
Wherein, the making step of standard curve is as follows:
A) mother liquor A: the volumetric flask of nicotinonitrile 0.02g, 3- picoline 0.03g standard specimen merging certain volume is weighed
In, it is spare with solvent dissolved dilution to scale；
B) it standard specimen solution 1: is added in 100mL volumetric flask from 25mL is pipetted in mother liquor A, is settled to scale with solvent, for use；
C) standard specimen solution 2: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 1, be settled to scale with solvent,
For use；
D) standard specimen solution 3: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 2, be settled to scale with solvent,
For use；
E) standard specimen solution 4: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 3, be settled to scale with solvent,
For use；
F) hand sampling: first using ultrapure water rinse sample introduction needle 20 times, then with sample introduction after sample to be tested rinse sample introduction needle 25 times,
Loading sequence is from low concentration to high concentration, and control sample volume is 40 μ L；
3) concentration calculation:
Embodiment 2:
A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, the detection method is including such as
Under several steps:
1) solution is prepared: being weighed 10g sample in 250mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1, is used in combination
Ultrapure water is settled to graduation mark, sufficiently shakes up；
2) production of standard curve；
Wherein, the making step of standard curve is as follows:
A) mother liquor A: in the volumetric flask for weighing nicotinonitrile 0.1g, 3- picoline 0.01g standard specimen merging certain volume,
It is spare with solvent dissolved dilution to scale；
B) it standard specimen solution 1: is added in 100mL volumetric flask from 25mL is pipetted in mother liquor A, is settled to scale with solvent, for use；
C) standard specimen solution 2: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 1, be settled to scale with solvent,
For use；
D) standard specimen solution 3: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 2, be settled to scale with solvent,
For use；
E) standard specimen solution 4: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 3, be settled to scale with solvent,
For use；
F) hand sampling: first using ultrapure water rinse sample introduction needle 25 times, then with sample introduction after sample to be tested rinse sample introduction needle 20 times,
Loading sequence is from low concentration to high concentration, and control sample volume is 20 μ L；
3) concentration calculation:
Embodiment 3:
A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, the detection method is including such as
Under several steps:
1) solution prepare: weigh 2g sample in 100mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1, and with surpass
Pure water is settled to graduation mark, sufficiently shakes up；
2) production of standard curve；
Wherein, the making step of standard curve is as follows:
A) mother liquor A: the volumetric flask of nicotinonitrile 0.05g, 3- picoline 0.02g standard specimen merging certain volume is weighed
In, it is spare with solvent dissolved dilution to scale；
B) it standard specimen solution 1: is added in 100mL volumetric flask from 25mL is pipetted in mother liquor A, is settled to scale with solvent, for use；
C) standard specimen solution 2: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 1, be settled to scale with solvent,
For use；
D) standard specimen solution 3: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 2, be settled to scale with solvent,
For use；
E) standard specimen solution 4: being added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 3, be settled to scale with solvent,
For use；
F) hand sampling: first using ultrapure water rinse sample introduction needle 20 times, then with sample introduction after sample to be tested rinse sample introduction needle 20 times,
Loading sequence is from low concentration to high concentration, and control sample volume is 30 μ L；
3) concentration calculation:
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of method with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater, which is characterized in that the detection
Method comprises the following steps:
1) solution is prepared: being weighed 1-10g sample in 50-250mL volumetric flask 1,2, and accurate recording sample weighting amount numerical value m1, is used in combination
Ultrapure water is settled to graduation mark, sufficiently shakes up；
2) production of standard curve；
3) concentration calculation:
2. the method according to claim 1 with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater,
It is characterized in that, accuracy is 0.1mg when sample weighs in the step 1).
3. the method according to claim 1 with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater,
It is characterized in that, the making step of standard curve is as follows:
A) mother liquor A: the appearance of nicotinonitrile 0.02-0.1g, 3- picoline 0.01-0.03g standard specimen merging certain volume is weighed
It is spare with solvent dissolved dilution to scale in measuring bottle；
B) it standard specimen solution 1: is added in 100mL volumetric flask from 25mL is pipetted in mother liquor A, is settled to scale with solvent, for use；
C) it standard specimen solution 2: is added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 1, is settled to scale with solvent, for use；
D) it standard specimen solution 3: is added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 2, is settled to scale with solvent, for use；
E) it standard specimen solution 4: is added in 100mL volumetric flask from 25mL is pipetted in standard specimen solution 3, is settled to scale with solvent, for use；
F) it hand sampling: first uses ultrapure water rinse sample introduction needle 20-25 times, then laggard with the certain number of sample to be tested rinse sample introduction needle
Sample, Loading sequence are from low concentration to high concentration, and control sample volume is certain.
4. the method according to claim 3 with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater,
It is characterized in that, volumetric flask volume is 100mL in the step a).
5. the method according to claim 3 with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater,
It is characterized in that, sample volume is 20-40 μ L in the step f).
6. the method according to claim 3 with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater,
It is characterized in that, with sample to be tested rinse number is 20-25 times in the step f).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811050582.9A CN109212062A (en) | 2018-09-07 | 2018-09-07 | A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater |
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| CN201811050582.9A CN109212062A (en) | 2018-09-07 | 2018-09-07 | A method of with nicotinonitrile and 3- picoline in HPLC detection industrial wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112834643A (en) * | 2020-12-31 | 2021-05-25 | 郑州原理生物科技有限公司 | Method for measuring 2, 6-dihydroxy-4-methylpyridine and 2, 6-dihydroxy-3-cyano-4-methylpyridine |
| CN114594178A (en) * | 2022-01-25 | 2022-06-07 | 贵州健安德科技有限公司 | Method for detecting 3-methylpyridine in 30% chlorantraniliprole suspending agent by using HPLC (high performance liquid chromatography) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112834643A (en) * | 2020-12-31 | 2021-05-25 | 郑州原理生物科技有限公司 | Method for measuring 2, 6-dihydroxy-4-methylpyridine and 2, 6-dihydroxy-3-cyano-4-methylpyridine |
| CN112834643B (en) * | 2020-12-31 | 2022-03-18 | 郑州原理生物科技有限公司 | Method for measuring 2, 6-dihydroxy-4-methylpyridine and 2, 6-dihydroxy-3-cyano-4-methylpyridine |
| CN114594178A (en) * | 2022-01-25 | 2022-06-07 | 贵州健安德科技有限公司 | Method for detecting 3-methylpyridine in 30% chlorantraniliprole suspending agent by using HPLC (high performance liquid chromatography) |
| CN114594178B (en) * | 2022-01-25 | 2024-04-02 | 贵州健安德科技有限公司 | Method for detecting 3-methylpyridine in 30% chlorantraniliprole suspending agent by utilizing HPLC |
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