CN102507776B - Method for determining phenol content in water - Google Patents
Method for determining phenol content in water Download PDFInfo
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- CN102507776B CN102507776B CN 201110337766 CN201110337766A CN102507776B CN 102507776 B CN102507776 B CN 102507776B CN 201110337766 CN201110337766 CN 201110337766 CN 201110337766 A CN201110337766 A CN 201110337766A CN 102507776 B CN102507776 B CN 102507776B
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Abstract
The invention relates to a method for determining phenol content in water. The method comprises the following steps of: (1) adding organic solvent into the water containing phenol for preparing sample solution; and (2) injecting the sample solution into a gas chromatograph for determining. The method for determining the phenol content in the water disclosed by the invention is simple, quick and accurate in operation, about ten minutes are used for analyzing one sample, and thus the defect that the existing method is troublesome in operation and long in time is overcome.
Description
Technical field
The invention belongs to the analytical chemistry field.Particularly, the present invention relates to a kind of method of measuring phenol content.
Background technology
The method of phenol content is to adopt GB 7491 " after-distillation with bromine method " in traditional mensuration water, and this method is with the quantity of sample distillation, and wherein volatile phenol collection is obtained collecting liquid; To collect liquid then with excessive potassium bromate bromination, remaining bromine and potassium iodide reaction discharge free iodine; Use sodium thiosulfate solution titrated then, and go out the content of volatile ingredient according to its consumption calculating.
As can be seen, GB 7491 " after-distillation with bromine method " complex operation, time-consuming, a common sample determination needs at least three hours.Therefore,, for example all there is every day the dozens of sample to need to analyze,, guarantees that with being difficult to the accurate of measurement data is with in time as analyzing by GB 7491 " after-distillation with bromine method " for the more situation of analytic sample.
Therefore, still need measure the method for phenol content in the water simple to operate, quickly and accurately.
Summary of the invention
The purpose of this invention is to provide a kind of simple to operate, measure the method for phenol content in the water quickly and accurately.
A kind of method of measuring phenol content in the water of the present invention may further comprise the steps:
(1) in the water that contains phenol, adds organic solvent and prepare need testing solution;
(2) above-mentioned need testing solution inject gas chromatograph is measured.
In described step (1):
Described organic solvent preferably can be an acetone.
In the described need testing solution, described volume of organic solvent percentage composition is preferably at least 40%.
In the described need testing solution, described volume of organic solvent percentage composition more preferably at least 50%.
In the described need testing solution, described volume of organic solvent percentage composition more preferably 50%～80%; For example, can be 50%, 60%, 70% or 80%.
For example, step (1) is added the concrete operations that organic solvent prepares need testing solution in the water that contains phenol: measure the water that 12.5mL contains phenol with pipette and place the 25mL volumetric flask, be settled to scale with organic solvent (for example acetone), mix and promptly get need testing solution.
Not necessarily, if contain the particulate matter that contains influential measurement in the water of phenol, before adding organic solvent, need this water filtration (for example, using miillpore filter) that contain phenol to remove these materials.
In described step (2):
The chromatographic column of described gas chromatograph is the HP-5 capillary column.
Particularly, the condition determination of described gas chromatograph can for:
Instrument: Tianjin, island GC2010 gas chromatograph;
Chromatographic column: HP-5 capillary column (30m * 0.32mm * 0.25 μ m);
Column temperature: 130 ℃;
Sample size: 1 μ L;
Injection port gasification temperature: 325 ℃;
Split ratio: 20: 1;
Carrier gas flux: 23.1mL/min;
Carrier gas: nitrogen;
Detecting device: flame ionization ditector (FID);
Detector temperature: 325 ℃.
Under these conditions, the retention time of phenol is approximately 3.40 minutes.
The present invention adopts phenol content in the gas chromatography determination water, only need in testing sample, to add certain amount of organic solvent (for example acetone), with in the direct inject gas chromatograph of need testing solution, get final product the content of volatile ingredient phenol in the fast measuring water outlet then.Method of the present invention is simple to operate, quick, accurate, analyzes a sample only about consuming time ten minutes.Thereby overcome the shortcoming of existing method complex operation, length consuming time.The method of phenol content is applicable to that mensuration wastewater from chemical industry or other contain the content of the phenol in wastewater of phenol in the mensuration water of the present invention.
Description of drawings
The chromatogram that Fig. 1 obtains with gas chromatograph for determination for standard solution (wherein, ordinate is the response signal of detecting device).
Fig. 2 contains the chromatogram (wherein, ordinate is the response signal of detecting device) that No. 1 need testing solution of acetone obtains with gas chromatograph for determination.
Embodiment
The following examples only are used to explain the present invention, and unrestricted the present invention.
Water is deionized water.The phenol standard items are available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.Acetone is chromatographically pure.
1, instrument and condition determination
Instrument: Tianjin, island GC2010 gas chromatograph (day island proper Tianjin company) has flame ionization ditector (FID).
Condition determination: chromatographic column: HP-5 capillary column (30m * 0.32mm * 0.25 μ m) (Agilent company); Column temperature: 130 ℃; Sample size: 1 μ L; Injection port gasification temperature: 325 ℃; Split ratio: 20: 1; Carrier gas flux: 23.1mL/ minute; Carrier gas: nitrogen; Detector temperature: 325 ℃.
2, the preparation of standard solution
500mg phenol standard items are dissolved in the 1000mL water as standard solution.
3, the preparation of need testing solution
In the 12.5mL standard solution, add the acetone of 12.5mL, mix, promptly get No. 1 need testing solution (the acetone volume content is 50%).
Perhaps, in the 15.0mL standard solution, add the acetone of 10.0mL, mix, promptly get No. 2 need testing solutions (the acetone volume content is 40%).
Perhaps, in the 10.0mL standard solution, add the acetone of 15.0mL, mix, promptly get No. 3 need testing solutions (the acetone volume content is 60%).
Perhaps, in the 7.5mL standard solution, add the acetone of 17.5mL, mix, promptly get No. 4 need testing solutions (the acetone volume content is 70%).
Perhaps, in the 5.0mL standard solution, add the acetone of 20.0mL, mix, promptly get No. 5 need testing solutions (the acetone volume content is 80%).
4, measure
4.1 the mensuration of phenol content in the standard solution
Described standard solution is injected in the gas chromatograph under the said determination condition measures.The result is referring to Fig. 1.The chromatogram that Fig. 1 obtains with gas chromatograph for determination for standard solution.As can be seen, because that phenol respond in gas chromatograph is little, and because the bonding action of phenol and water, thereby make the peak shape of phenol on chromatogram hangover occur, can't reach quantitative requirement, and then influence the accuracy of phenol detection.
4.2 the mensuration of phenol content in the need testing solution
Described No. 1 need testing solution is injected in the gas chromatograph under the said determination condition measures.The result is referring to Fig. 2.Fig. 2 contains the chromatogram that No. 1 need testing solution of acetone obtains with gas chromatograph for determination.2～No. 5 need testing solution has and No. 1 similar chromatogram (not shown) of need testing solution.As can be seen, interpolation acetone can destroy the bonding force between phenol and hydrone in containing the aqueous solution of phenol, thereby makes that the peak shape of phenol on chromatogram is normal, reaches quantitative requirement fully.
5, methodological study
Further, the inventor has carried out the methodology test to the method for phenol content in the mensuration water of the present invention, comprises the test of recovery test and precision.Preparation and the approaching standard operation liquid of testing sample concentration, sample introduction analysis under above-mentioned GC conditions calculates correction factor (external standard method) according to component concentration and peak area (or peak height).
The preparation of preparation sample solution: accurately take by weighing about 0.50g phenol standard items (being accurate to 0.1mg) in the 250mL volumetric flask, add 125mL acetone, fully shake up, be settled to scale, promptly get the preparation sample solution that contains phenol 2000mg/L with deionized water; Stepwise dilution obtains the preparation sample solution of other concentration then.
Described two parts of water samples are the sample of the variable concentrations of oneself preparing.
Measurement result sees Table 1～2.
Table 1 recovery test result
Table 2 Precision test result
By the test findings of table 1～2 as can be known: the recovery of the method for phenol content is 98.0%～102.4% in the mensuration water of the present invention, and the standard deviation of precision test is 1.03%～1.17%; The method of phenol content is simple to operate in the mensuration water of the present invention, fast, accurately, analyzes a sample only about consuming time ten minutes.
Claims (3)
1. method of measuring phenol content in the water may further comprise the steps:
(1) in the water that contains phenol, adds organic solvent and prepare need testing solution;
(2) above-mentioned need testing solution inject gas chromatograph is measured;
Described organic solvent is an acetone;
In the described need testing solution, described volume of organic solvent percentage composition is at least 40%;
The condition that described need testing solution inject gas chromatograph is measured is: instrument: Tianjin, island GC2010 gas chromatograph; Chromatographic column: HP-5 capillary column, 30m * 0.32mm * 0.25 μ m; Column temperature: 130 ℃; Sample size: 1 μ L; Injection port gasification temperature: 325 ℃; Split ratio: 20:1; Carrier gas flux: 23.1mL/min; Carrier gas: nitrogen; Detecting device: flame ionization ditector; Detector temperature: 325 ℃.
2. the method for phenol content is characterized in that in the mensuration water according to claim 1, and in the described need testing solution, described volume of organic solvent percentage composition is at least 50%.
3. the method for phenol content is characterized in that in the mensuration water according to claim 2, and in the described need testing solution, described volume of organic solvent percentage composition is 50%～80%.
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| CN 201110337766 CN102507776B (en) | 2011-10-31 | 2011-10-31 | Method for determining phenol content in water |
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| CN 201110337766 CN102507776B (en) | 2011-10-31 | 2011-10-31 | Method for determining phenol content in water |
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| CN109358040A (en) * | 2018-05-07 | 2019-02-19 | 萍乡煤科环保科技有限公司 | A kind of measuring method of Phenol for Waste Water content and the measurement device used |
| 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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