CN103543217A - Determination of phenol in phosphate rock flotation environmental water body by gas chromatography - Google Patents
Determination of phenol in phosphate rock flotation environmental water body by gas chromatography Download PDFInfo
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- CN103543217A CN103543217A CN201210478511.5A CN201210478511A CN103543217A CN 103543217 A CN103543217 A CN 103543217A CN 201210478511 A CN201210478511 A CN 201210478511A CN 103543217 A CN103543217 A CN 103543217A
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Abstract
The invention discloses a method for determining phenol in a phosphate rock flotation environmental water body, relates to a detection method and particularly relates to the method for analyzing the phenol in the phosphate rock flotation environmental water body. The method provided by the invention is realized through the following scheme: a) collecting 1000ml of water sample from the phosphate rock flotation environmental water body, accurately adding 2.00ml of toluene, shaking for 20min and standing for stratification; b) taking 1.0-4.0mu L of organic phase and injecting into a gas chromatograph for determination; c) preparing a standard curve; and d) finding out a corresponding value on the well prepared standard curve, namely a determination result. According to the method provided by the invention, fast qualification of the phenol in the phosphate rock flotation water body can be realized, the quantitative analysis can be developed within a certain concentration range on the qualitative basis, and the method has the characteristics of simplicity, convenience, fast speed, good reproducibility and the like.
Description
Technical field
The present invention relates to a kind of detection method, particularly analyze under rock phosphate in powder flotation environment the method for phenol in water body.
Background technology
Phenol has larger bio-toxicity to human body, human body sucks or absorbs and can cause various diseases through skin, long term toxicity is more severe than formaldehyde, may be along with the life that enters us of " quiet " such as phosphate rock floating agent starting material, hair dye, washing agent, germifuge, paint, antiseptic, tackifier and industrial waste waters, Low Concentration Phenol is carcinogenic to people's Main Function, high concentration phenol is killed livestock, and in numerous flotation of phosphate rock production phenolic comp ' ds pollution, what most probable was introduced is exactly phenol.Industry is interior does not carry out the mensuration for phenol in rock phosphate in powder flotation environment water at present, therefore, sets up phenol qualitativing quantitative measuring method in quick, accurate, economic, applicable rock phosphate in powder flotation environment water, imperative.
Summary of the invention
The object of this invention is to provide that a kind of method is easy, quick, environmental protection, a kind of method of measuring phenol in rock phosphate in powder flotation environment water cheaply.
A kind of method of measuring phenol in rock phosphate in powder flotation environment water of the present invention, realizes by following scheme:
A. get in rock phosphate in powder flotation environment water and gather 1000 ml water samples, accurately add 2.00 ml toluene, jolting 20min, stratification;
B. get in organic phase 1.0 ~ 4.0 μ L inject gas chromatographs and measure;
C. preparation standard curve: take 0.100g phenol, the excellent pure level of phenol GR-, in 100ml volumetric flask or take 1.000g phenol toluene in 1000ml volumetric flask and dissolve constant volume, now concentration is 1 mg/ ml, measure respectively 0,0.5,1,2,3,4ml in a different set of 100ml volumetric flask, after constant volume, draw respectively in 1.0 μ L inject gas chromatographs and measure, wherein take reagent blank as reference, the peak area after integration of take is ordinate, and phenol amount is horizontal ordinate, drawing curve;
D. formerly on ready-made typical curve, find corresponding value.
Toluene extractant described in step a is AR level, and toluene extractant addition is 2.00 ml.
In absorption organic phase 1.0 μ L inject gas chromatographs described in step b, measure, can draw in 1.0 ~ 4.0 μ L inject gas chromatographs and measure according to the amount containing phenol;
Phenol described in step c is GR level, and top grade is pure.
The present invention is that 10.0mg/L ~ 25.0mg/L working curve is best to containing phenol concentration; Sample lower than working curve can be done by separation and concentration, higher than the sample dilution of working curve, does, and the solution of variable concentrations needs different operating curve, and because of the variation of temperature, air pressure, working curve is also wanted corresponding adjustment.
Phenol processes in a kind of mensuration rock phosphate in powder flotation environment water of the present invention, its principle is based on each organism, on gas chromatographic column, to have a peak of a correspondence, phenol belongs to strong polar material in organism, therefore select the BPX-70 quartz capillary column of corresponding strong polarity, select toluene as phenol extraction agent, it is the similar principle that mixes, in rock phosphate in powder flotation environment water, phenol is after toluene separation and concentration, chromatographic column is separated, through flame ionization ditector gas chromatograph FID, detect, according to standard ingredient to go out peak retention time qualitative, retention time of the present invention 2.077 minutes is toluene peak, in the time of 4.877 minutes, it is phenol peak, peak area and the typical curve of each component to be measured are more quantitative
The present invention is by exploring and determined flotation circuit aquametry parameter in rock phosphate in powder column temperature, vaporizer temperature, detector temperature, high pure nitrogen flow rate of carrier gas, post pressure, split ratio, acidity, stabilizer type, concentration, sampling; for practical measurement, testing index can reach the state environment protecting standard << of People's Republic of China (PRC) water quality. and the mensuration HJ505-2009(of volatile phenol replaces GB7491-87) 2009-10-20 day issue >>.
Accompanying drawing explanation
The Tailings Dam water sample phenol figure of Tu1Wei rock phosphate in powder flotation mill.
Fig. 2 is the toluene solution chromatogram that has added phenol
Embodiment
Below by embodiment, the present invention is further illustrated, but be not limited to embodiment.
First be production standard curve:
Take 0.100g GR-top grade purified petroleum benzin phenol in 100ml volumetric flask, or also can take 1.000g phenol toluene in 1000ml volumetric flask and dissolve constant volume, now concentration is 1 mg/ ml, measure 0,0.5,1,2,3,4ml is in one group of 100ml volumetric flask, after constant volume, draw respectively in 1.0 μ L inject gas chromatographs and measure, wherein take reagent blank as reference, the peak area after integration of take is ordinate, phenol addition is horizontal ordinate, drawing curve.
Note: this experiment is that 10.0mg/L ~ 25.0mg/L working curve is best to containing phenol concentration; Sample lower than working curve can be done by separation and concentration, higher than the sample dilution of working curve, does, and the solution of variable concentrations needs different operating curve, and because of the variation of temperature, air pressure, working curve had better not adopt.
Use instrument: the GCMS-2010plus of Shimadzu company gas chromatograph.
Chromatographic condition: press 100KPa, split ratio before chromatographic column → BPX-70 quartz capillary column, 160 ℃ of column temperatures, 250 ℃ of vaporizer temperature, 260 ℃ of detector temperatures, flow rate of carrier gas 58.8 ml, post: do not shunt, air velocity 400ml/min, hydrogen flow rate 40ml/min.
Next is to test:
Get 2,000,000 tons/year of Tailings Dam water 1000 ml of rock phosphate in powder flotation mill of Haikou phosphorus ore, accurately add 2.00 ml toluene, jolting 20min, stratification; Get in organic phase 1.0 μ L inject gas chromatographs and measure;
Obtain chromatogram 1, from chromatogram 1, learn: in the time of 4.877 minutes, phenol peak retention time is a straight line, without peak, only in retention time, within 2.077 minutes, have a solvent toluene peak, in 2,000,000 tons of Tailings Dam water bodys of known Haikou phosphorus ore, do not contain phenol.Sending Institute of Analysis of Yunnan University to detect in sample does not measure yet.Fig. 2 is the toluene solution chromatogram that has added phenol, and with Fig. 1 and Fig. 2 comparison, result shows, the method can be used for the qualitative of phenol in rock phosphate in powder flotation environment.
On the experimental technique basis of embodiment 1, get water sample 1000 ml in rock phosphate in powder flotation water body, in sample, gradation adds a certain amount of 1mg/ ml phenol/aqueous solution, and inferior mark-on method, accurately adds 2.00 ml toluene, jolting 20min, stratification; Get in organic phase 1.0 μ L inject gas chromatographs and measure;
In sample, gradation adds a certain amount of 1mg/ml phenol/aqueous solution, secondary mark-on method, and between 10-80mg, its recovery is 97.5-106.6%
Average recovery experiment, table 1 method of proof is reliable.
Table 1 recovery testu
| The phenol mg first adding in sample | The phenol mg adding again | The phenol mg recording | Relative error % | Recovery % |
| 13 | 10 | 22.75 | 0.25 | 97.5 |
| 25 | 20 | 44.72 | 0.28 | 98.6 |
| 19 | 40 | 59.48 | 0.48 | 101.2 |
| 8 | 80 | 93.28 | 4.58 | 106.6 |
In 2 embodiment, in certain scope, change reagent dosage, measurement result is comparatively accurate.
Phenol in energy fast qualitative rock phosphate in powder flotation water body of the present invention can be carried out quantitative test within the scope of finite concentration on qualitative basis, has the features such as easy, quick, favorable reproducibility.
Claims (4)
1. a method of measuring phenol in rock phosphate in powder flotation environment water, is characterized in that, by following scheme, realizes:
A. get in rock phosphate in powder flotation environment water and gather 1000 ml water samples, accurately add 2.00 ml toluene, jolting 20min, stratification;
B. get in organic phase 1.0 ~ 4.0 μ L inject gas chromatographs and measure;
C. preparation standard curve: take 0.100g phenol, the excellent pure level of phenol GR-, in 100ml volumetric flask or take 1.000g phenol toluene in 1000ml volumetric flask and dissolve constant volume, now concentration is 1 mg/ ml, measure respectively 0,0.5,1,2,3,4ml in a different set of 100ml volumetric flask, after constant volume, draw respectively in 1.0 μ L inject gas chromatographs and measure, wherein take reagent blank as reference, the peak area after integration of take is ordinate, and phenol amount is horizontal ordinate, drawing curve;
D. formerly on ready-made typical curve, find corresponding value, obtain measurement result.
2. the method for phenol in mensuration rock phosphate in powder flotation environment water according to claim 1, is characterized in that, the toluene extractant described in step a is AR level, and toluene extractant addition is 2.00 ml.
3. the method for phenol in mensuration rock phosphate in powder flotation environment water according to claim 1, it is characterized in that, in absorption organic phase 1.0 μ L inject gas chromatographs described in step b, measure, can draw in 1.0 ~ 4.0 μ L inject gas chromatographs and measure according to the amount containing phenol.
4. the method for phenol in mensuration rock phosphate in powder flotation environment water according to claim 1, is characterized in that, the phenol described in step c is that GR-top grade is pure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872440A (en) * | 2018-08-11 | 2018-11-23 | 中山市永恒化工新材料研究院有限公司 | The measurement method of phenol content in a kind of water |
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| 常青等: "液相微萃取-气相色谱法测定水样中微量酚类污染物", 《理化检验-化学分册》 * |
| 王中柱等: "海水中苯酚及甲酚异构体的气相色谱测定法的研究", 《山东海洋学院学报》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872440A (en) * | 2018-08-11 | 2018-11-23 | 中山市永恒化工新材料研究院有限公司 | The measurement method of phenol content in a kind of water |
| CN108872440B (en) * | 2018-08-11 | 2021-06-29 | 中山市永恒化工新材料研究院有限公司 | Method for measuring content of phenol in water |
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Application publication date: 20140129 |