CN112858557A - Method for detecting content of semi-volatile organic compounds in water supply hose - Google Patents
Method for detecting content of semi-volatile organic compounds in water supply hose Download PDFInfo
- Publication number
- CN112858557A CN112858557A CN202110062524.3A CN202110062524A CN112858557A CN 112858557 A CN112858557 A CN 112858557A CN 202110062524 A CN202110062524 A CN 202110062524A CN 112858557 A CN112858557 A CN 112858557A
- Authority
- CN
- China
- Prior art keywords
- semi
- volatile organic
- sample
- organic compounds
- detecting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a method for detecting the content of semi-volatile organic compounds in a water supply hose, which comprises the following steps: s1) sample pretreatment; s2) ultrasonic extraction; s3) purifying; s4) preparing a standard working solution; s5) testing and calculating: detecting by adopting a GCMS gas chromatography-mass spectrometer, obtaining the ratio of the peak area of the standard working solution to the peak area of the semi-volatile organic compound contained in the sample to be detected, drawing a related working curve of the ratio of the peak areas, and calculating by using a calculation formula to obtain the concentration of the semi-volatile organic compound contained in the sample to be detected. The method for detecting the content of the semi-volatile organic compounds in the water supply hose is simple to operate, low in cost, suitable for detecting and researching precipitation of the semi-volatile harmful substances in the water supply hose, and capable of providing technical support for safe use of the products, and being used for health, health and safety prediction of the water supply hose, so that the use risk of the water supply hose is reduced.
Description
Technical Field
The invention relates to the technical field of substance analysis and detection, in particular to a method for detecting the content of semi-volatile organic compounds in a water supply hose.
Background
The water supply hose is mainly divided into a plastic hose and a rubber hose, the types of the water supply hose are PE, PA, PVC, PP, PEX and EPDM according to the main components, and the used filling agents such as plasticizer, organic montmorillonite, flame retardant and the like possibly contain carcinogenic, teratogenic and mutagenic organic matters, which are called three-way high-toxicity organic matters for short.
2,4, 6-trichlorophenol is a chlorophenol compound and is widely applied to plastic additives and fluxing agents. Chlorophenols have hormone-like functions, and genetic diseases and cancers caused by chlorophenols are of great concern among injuries to the human body. The ability to over-penetrate cell membranes and organelle membranes resulting in changes in membrane potential and in the expression of related proteins, leading to mutations, chlorophenols have carcinogenic, teratogenic and mutagenic effects, which have been blacklisted by "priority control of contaminants" in many countries.
2,4, 6-trichlorophenol, 1, 3-dichlorobenzene and hexachlorobutadiene are not included in the national standard GB 23448 semi-volatile toxic substance list, and the related test methods of the prior art for water supply hoses are lack of guidance, and the blank is urgently filled to improve the management level of the sanitary health quality of related products.
Disclosure of Invention
The invention aims to provide a method for detecting the content of semi-volatile organic compounds in a water supply hose, which is simple to operate and low in cost and can be used for the sanitary safety prediction of the water supply hose.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for detecting the content of semi-volatile organic compounds contained in a water supply hose is used for detecting the semi-volatile organic compounds contained in the water supply hose and are 2,4, 6-trichlorophenol, and comprises the following steps:
s1) sample pretreatment: washing a hose to be detected with tap water and ultrapure water for 3 times, then cutting the hose to be detected into small pieces of 5 x 5mm, and sucking water to obtain a sample to be detected;
s2) ultrasonic extraction: weighing the sample to be detected, soaking the sample in a mixed solution of ethyl acetate, acetone and normal hexane to ensure that the sample to be detected is completely soaked, and extracting the sample for 1 hour by using ultrasonic waves under a normal-temperature ventilation environment to obtain an extract liquid;
s3) purifying: standing the extract for 5min, taking 10ml of clear liquid at the upper part of the extract, carrying out primary purification through a C18 small column, collecting a purified liquid at 45 ℃, blowing nitrogen to concentrate the purified liquid to 1ml, if the volume is less than 1ml, using ethyl acetate to fix the volume to 1ml, filtering the purified liquid in a GCMS sample feeding bottle through a filter membrane, and adding 100uL of internal standard solution to obtain a test sample of the extract;
s4) preparing a standard working solution: diluting ethyl acetate into solutions with the concentrations of 0.04, 0.08, 0.1, 0.2, 0.5, 1,2, 5 and 10ppm respectively, and adding 100uL of an internal standard solution respectively to prepare a standard working solution;
s5) testing and calculating: detecting by adopting a GCMS gas chromatography-mass spectrometer to obtain the ratio of the peak area of the standard working solution to the peak area of the semi-volatile organic compound contained in the sample to be detected, drawing a standard working curve by taking the ratio of the peak area of the standard working solution to the peak area of the internal standard substance as an X axis and the ratio of the concentration of the standard working solution to the concentration of the internal standard substance as a Y axis, and calculating by using a calculation formula to obtain the concentration of the semi-volatile organic compound contained in the sample to be detected.
Specifically, in step S2), the weight ratio of the sample to be detected to the mixed solution is 1: 5.
Specifically, in step S2), the volume mixing ratio of ethyl acetate, acetone, and n-hexane in the mixed solution is 1:3: 3.
Specifically, in step S2), the frequency of the ultrasonic wave is 40kHz, and the power is 500W.
Specifically, in step S3), the filter membrane is an organic filter membrane of 0.45 um.
Specifically, in steps S3) and S4), the internal standard solution is a solution having a content of 50ppm of deuteroflexor of the chemical formula C18D 12.
Specifically, in step S5), the working conditions of the GCMS gc-ms are as follows:
the chromatographic column is a quartz capillary chromatographic column with RXI-5MS of 30 mm multiplied by 0.25 mm;
the thickness of the liquid film is 0.25 um; the temperature of a sample inlet is 300 ℃; the interface temperature is 300 ℃; ion source temperature: 280 ℃;
the temperature rising procedure is as follows: maintaining the initial temperature at 45 deg.C for 4 min; heating to 130 deg.C at 40 deg.C/min, and maintaining for 0 min; heating to 180 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min; heating to 240 deg.C at a speed of 7 deg.C/min, and maintaining for 0 min; heating to 320 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min;
adopting no-split-flow sample injection, wherein the linear velocity of the sample injection is 33 cm/s.
Specifically, in step 5), the calculation formula of the concentration of the semi-volatile organic compound contained in the test sample is as follows:
in the formula, C is the content of semi-volatile organic compounds to be detected in the soak solution, and the unit is ug/ml;
x is the concentration of the extract on the machine, and the unit is ug/ml;
X0the unit of the concentration of the blank extract on the machine is ug/ml;
V1the final volume of the extract is the unit of ml;
V2the volume of the soaking solution is in ml.
Further, the semi-volatile organic compound also comprises all semi-volatile organic compounds indicated in the national standard GB 23448.
Further, the semi-volatile organic compound also comprises 1, 3-dichlorobenzene and/or hexachlorobutadiene.
The invention has the beneficial effects that: the method for detecting the content of the semi-volatile organic compounds in the water supply hose is simple to operate, low in cost and suitable for detecting and researching precipitation of the semi-volatile harmful substances in the water supply hose, and fills the technical blank in the field. And technical support is provided for safe use of the product, and the method can be used for predicting the sanitation, health and safety of the water supply hose, so that the use risk of the water supply hose is reduced.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is not only suitable for detecting 2,4, 6-trichlorophenol, but also suitable for detecting all the semi-volatile organic compounds in the national standard GB 23448 and detecting the semi-volatile organic compounds of 1.3-dichlorobenzene and/or hexachlorobutadiene which are not contained in the national standard GB 23448, and has a wide application range.
Drawings
FIG. 1 is a GCMS chromatogram of a detected EPDM hose of example 1 of the present invention;
FIG. 2 is a GCMS chromatogram of a PEX hose tested according to example 2 of the present invention;
FIG. 3 is a graph showing the operation of the ratio of the peak area of the standard operating solution to the peak area of 2,4, 6-trichlorophenol contained in the EPDM hose tested in example 1 of the present invention;
fig. 4 is a chromatogram of all semi-volatile organic compounds detected by the method for detecting the content of the semi-volatile organic compounds in the water supply hose according to the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The technical solution of the present invention will be further explained with reference to the accompanying drawings 1-3 and the detailed description.
A method for detecting the content of semi-volatile organic compounds contained in a water supply hose is used for detecting the semi-volatile organic compounds contained in the water supply hose and are 2,4, 6-trichlorophenol, and comprises the following steps:
s1) sample pretreatment: washing a hose to be detected with tap water and ultrapure water for 3 times, then cutting the hose to be detected into small pieces of 5 x 5mm, and sucking water to obtain a sample to be detected;
s2) ultrasonic extraction: weighing the sample to be detected, soaking the sample in a mixed solution of ethyl acetate, acetone and normal hexane to ensure that the sample to be detected is completely soaked, and extracting the sample for 1 hour by using ultrasonic waves under a normal-temperature ventilation environment to obtain an extract liquid;
s3) purifying: standing the extract for 5min, taking 10ml of clear liquid at the upper part of the extract, carrying out primary purification through a C18 small column, collecting a purified liquid at 45 ℃, blowing nitrogen to concentrate the purified liquid to 1ml, if the volume is less than 1ml, using ethyl acetate to fix the volume to 1ml, filtering the purified liquid in a GCMS sample feeding bottle through a filter membrane, and adding 100uL of internal standard solution to obtain a test sample of the extract;
s4) preparing a standard working solution: diluting ethyl acetate into solutions with the concentrations of 0.04, 0.08, 0.1, 0.2, 0.5, 1,2, 5 and 10ppm respectively, and adding 100uL of an internal standard solution respectively to prepare a standard working solution;
s5) testing and calculating: detecting by adopting a GCMS gas chromatography-mass spectrometer to obtain the ratio of the peak area of the standard working solution to the peak area of the semi-volatile organic compound contained in the sample to be detected, drawing a standard working curve by taking the ratio of the peak area of the standard working solution to the peak area of the internal standard substance as an X axis and the ratio of the concentration of the standard working solution to the concentration of the internal standard substance as a Y axis, and calculating by using a calculation formula to obtain the concentration of the semi-volatile organic compound contained in the sample to be detected.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is simple to operate, low in cost and suitable for detecting and researching precipitation of the semi-volatile harmful substances in the water supply hose, and fills the technical blank in the field. And technical support is provided for safe use of the product, and the method can be used for predicting the sanitation, health and safety of the water supply hose, so that the use risk of the water supply hose is reduced.
Specifically, in step S2), the weight ratio of the sample to be detected to the mixed solution is 1: 5.
It is ensured that the soaked solution completely immerses the sample to be tested.
Specifically, in step S2), the volume mixing ratio of ethyl acetate, acetone, and n-hexane in the mixed solution is 1:3: 3.
The mixed solution of ethyl acetate, acetone and normal hexane with the volume mixing ratio of 1:3:3 is used as the extraction solvent, so that the dissolving efficiency of the semi-volatile organic compounds in the water supply hose can be improved, and the detection efficiency and accuracy of the detection method of the content of the semi-volatile organic compounds in the water supply hose are improved.
Specifically, in step S2), the frequency of the ultrasonic wave is 40kHz, and the power is 500W.
The dissolving efficiency of the semi-volatile organic compounds in the extraction solvent in the water supply hose can be further improved by using ultrasonic waves with the frequency of 40kHz and the power of 500W.
Specifically, in step S3), the filter membrane is an organic filter membrane of 0.45 um.
The organic filter membrane of 0.45um is used for filtering, so that organic matters with larger molecular weight in the test sample can be effectively removed, interference peaks in a GCMS chromatogram are reduced, and the accuracy of the detection method of the content of semi-volatile organic matters in the water supply hose is improved.
Specifically, in steps S3) and S4), the internal standard solution is a solution having a content of 50ppm of deuteroflexor of the chemical formula C18D 12.
Deuterated derivatives of the formula C18D12 are international standards for CAS number 1719-03-5.
Specifically, in step S5), the working conditions of the GCMS gc-ms are as follows:
the chromatographic column is a quartz capillary chromatographic column with RXI-5MS of 30 mm multiplied by 0.25 mm;
the thickness of the liquid film is 0.25 um; the temperature of a sample inlet is 300 ℃; the interface temperature is 300 ℃; ion source temperature: 280 ℃;
the temperature rising procedure is as follows: maintaining the initial temperature at 45 deg.C for 4 min; heating to 130 deg.C at 40 deg.C/min, and maintaining for 0 min; heating to 180 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min; heating to 240 deg.C at a speed of 7 deg.C/min, and maintaining for 0 min; heating to 320 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min;
adopting no-split-flow sample injection, wherein the linear velocity of the sample injection is 33 cm/s.
The detection stability according to the GCMS working conditions set above is good, and the consistency is good.
Specifically, in step 5), the calculation formula of the concentration of the semi-volatile organic compound contained in the test sample is as follows:
in the formula, C is the content of semi-volatile organic compounds to be detected in the soak solution, and the unit is ug/ml;
x is the concentration of the extract on the machine, and the unit is ug/ml;
X0the unit of the concentration of the blank extract on the machine is ug/ml;
V1the final volume of the extract is the unit of ml;
V2the volume of the soaking solution is in ml.
According to the calculation formula, the content of the semi-volatile organic compounds in the sample to be detected can be quickly calculated.
Further, the semi-volatile organic compound also comprises all semi-volatile organic compounds indicated in the national standard GB 23448.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is suitable for detecting 2,4, 6-trichlorophenol, is also suitable for detecting all the semi-volatile organic compounds in the national standard GB 23448, and has a wide application range.
As shown in fig. 4, which is a chromatogram of the total detectable semi-volatile substances, the labeled peak numbers in the graph correspond to the following substances: 1. bisphenol A; 2. 1, 2-dibromo-3-chloropropane; 3. phenol; 4. a bis-ether; 5. 1, 3-dichlorobenzene; 6. 1, 2-dichlorobenzene; 7. n-nitrosodipropylamine; 8. ethyl chloride; 9. 2, 4-xylenol; 10. 2, 4-dichlorophenol; 11. naphthalene; 12. hexachlorobutadiene; 13. 4-chloro-3-cresol; 14. 2-methylnaphthalene; 15. 2-cresol; 16. acetophenone; 17. 2,4, 6-trichlorophenol; 18. bend-d 12; 19. 3, 3-dichlorobenzidine; 20. dimethyl phthalate; 21. acenaphthene-d 10; 22. acenaphthene; 23. diethyl phthalate; 24. n-nitrosodiphenylamine; 25. pentachlorophenol; 26. phenanthrene-d 10; 27. phenanthrene; 28. anthracene; 29. dibutyl phthalate; 30. fluoranthene; 31. pyrene; 32. butylbenzyl phthalate; 33. a phthalic diester; 34. benzo flower; 35. benzothiazole; 36. 2-hydroxybenzothiazole; 37. n-nitrosodimethylamine; 38. further, the semi-volatile organic compound also comprises 1, 3-dichlorobenzene and/or hexachlorobutadiene.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is not only suitable for detecting 2,4, 6-trichlorophenol, 2,4, 6-trichlorophenol and/or 2,4, 6-trichlorocresol, but also suitable for detecting the semi-volatile organic compounds of 1.3-dichlorobenzene and/or hexachlorobutadiene which are not contained in the national standard GB 23448, and has a wide application range.
Example 1
1. The test instrument: a Quintix224-1CN electronic balance, a KQ-500E ultrasonic instrument, a GCMS-QP2020 gas chromatography mass spectrometer and a JC-WD-12 water bath nitrogen blowing instrument;
2. test reagents: chromatographic grade ethyl acetate, acetone and n-hexane;
3. test procedure:
3.1. sample pretreatment
The EPDM flexible pipe is washed by tap water and ultrapure water for 3 times, the cleaned EPDM flexible pipe is cut into small pieces of 5 x 5mm, water is sucked, and the small pieces are placed in a beaker for standby.
3.2. Ultrasonic extraction and purification
Weighing 10g of the pretreated sample, putting the sample into 50ml of soak solution with the mixing ratio of ethyl acetate, acetone and n-hexane being 1:3:3 to ensure that the sample is completely immersed, sealing the beaker by using a sealing film, and extracting for 1h by adopting ultrasonic waves with the frequency of 40kHz and the power of 500W under the ventilation normal-temperature environment. After extraction, the mixture was left to stand for 5min, and 10ml of the supernatant was subjected to preliminary purification by passing through a C18 column.
And (3) blowing and concentrating the collected purified solution to 1ml at 45 ℃ by using nitrogen, if the volume is less than 1ml, using ethyl acetate to fix the volume to 1ml, filtering the solution by using a 0.45um filter membrane in a GCMS sample injection bottle, and adding 100uL of 50ppm internal standard solution to prepare an extract for later use.
3.3. Preparation of standard working solutions
Purchase of standards with certificates: a50 ppm internal standard solution was prepared of deuterated flexor of formula C18D12, commonly known as flexor D-12.
The ethyl acetate was diluted to a series of standard working solutions of concentrations 0.04, 0.08, 0.1, 0.2, 0.5, 1,2, 5 and 10ppm and 100uL of 50ppm internal standard solution was added for use.
3.4. Measurement of
GCMS is adjusted to the best state, 1.0ul of sample injection measurement is carried out, the ratio of the peak area of the standard working solution to the peak area of the internal standard substance is taken as an X axis, the ratio of the concentration of the standard working solution to the concentration of the internal standard substance is taken as a Y axis, and a standard working curve is drawn as shown in figure 3.
And (3) under the same on-machine condition, performing on-machine analysis on the extraction liquid in the step 3.2 to obtain the ratio of the peak area of the test extraction liquid to the peak area of the internal standard substance.
4. Analysis of test data and results
The linear graph of the working curve is shown in FIG. 3, and the linear regression equation is: y 0.209766x, a correlation coefficient R2 of 0.995, and a corresponding factor RF RSD of 12% < 20%.
And (3) substituting the ratio of the peak area of the extraction liquid measured in the step 3.4 to the peak area of the internal standard substance into the linear regression equation y which is 0.209766x, so as to calculate the content of the 2,4, 6-trichlorophenol in the extraction liquid.
The content of 2,4, 6-trichlorophenol in the soak solution of example 1 was calculated according to the following formula, and the calculation results are shown in table 1 below.
In the formula, C is the content of semi-volatile organic compounds to be detected in the soak solution, and the unit is ug/ml;
x is the concentration of the extract on the machine, and the unit is ug/ml;
X0the unit of the concentration of the blank extract on the machine is ug/ml;
V1the final volume of the extract is the unit of ml;
V2the volume of the soaking solution is in ml.
5. The GCMS chromatogram of example 1 was measured and is shown in FIG. 1.
Example 2
1. The content of 2,4, 6-trichlorophenol contained in the sample was measured using a commercially available PEX hose according to the same method and procedure as described above, and the calculation results of the measurement are shown in table 1 below.
2. The GCMS chromatogram of example 1 was measured and is shown in FIG. 2.
The test results of example 1 and example 2 are shown in table 1.
Table 1 semi-volatile organic compounds and test results contained in example 1 and example 2
In summary, the method for detecting the content of the semi-volatile organic compounds in the water supply hose of the present invention has the advantages of simple and effective operation, low cost and wide detection application range, and the data of the detection results in table 1 show that the method for detecting the content of the semi-volatile organic compounds in the water supply hose of the present invention has a low detection lower limit and high sensitivity.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is simple to operate, low in cost and suitable for detecting and researching precipitation of the semi-volatile harmful substances in the water supply hose, and fills the technical blank in the field. And technical support is provided for safe use of the product, and the method can be used for predicting the sanitation, health and safety of the water supply hose, so that the use risk of the water supply hose is reduced.
The method for detecting the content of the semi-volatile organic compounds in the water supply hose is not only suitable for detecting 2,4, 6-trichlorophenol, but also suitable for detecting all the semi-volatile organic compounds in the national standard GB 23448 and detecting the semi-volatile organic compounds of 1.3-dichlorobenzene and/or hexachlorobutadiene which are not contained in the national standard GB 23448, and has a wide application range.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
The technical principle of the present invention is described above in connection with specific embodiments. The description is only intended to explain the principles of the invention; and should not be construed as limiting the scope of the invention in any way. Based on the explanations herein; other embodiments of the invention will occur to those skilled in the art without the exercise of inventive faculty; all of which fall within the scope of the present invention.
Claims (10)
1. A method for detecting the content of semi-volatile organic compounds contained in a water supply hose is characterized by being used for detecting the semi-volatile organic compounds containing 2,4, 6-trichlorophenol in the water supply hose and comprising the following steps:
s1) sample pretreatment: washing a hose to be detected with tap water and ultrapure water for 3 times, then cutting the hose to be detected into small pieces of 5 x 5mm, and sucking water to obtain a sample to be detected;
s2) ultrasonic extraction: weighing the sample to be detected, soaking the sample in a mixed solution of ethyl acetate, acetone and normal hexane to ensure that the sample to be detected is completely soaked, and extracting the sample for 1 hour by using ultrasonic waves under a normal-temperature ventilation environment to obtain an extract liquid;
s3) purifying: standing the extract for 5min, taking 10ml of clear liquid at the upper part of the extract, carrying out primary purification through a C18 small column, collecting a purified liquid at 45 ℃, blowing nitrogen to concentrate the purified liquid to 1ml, if the volume is less than 1ml, using ethyl acetate to fix the volume to 1ml, filtering the purified liquid in a GCMS sample feeding bottle through a filter membrane, and adding 100uL of internal standard solution to obtain a test sample of the extract;
s4) preparing a standard working solution: diluting ethyl acetate into solutions with the concentrations of 0.04, 0.08, 0.1, 0.2, 0.5, 1,2, 5 and 10ppm respectively, and adding 100uL of an internal standard solution respectively to prepare a standard working solution;
s5) testing and calculating: detecting by adopting a GCMS gas chromatography-mass spectrometer to obtain the ratio of the peak area of the standard working solution to the peak area of the semi-volatile organic compound contained in the sample to be detected, drawing a standard working curve by taking the ratio of the peak area of the standard working solution to the peak area of the internal standard substance as an X axis and the ratio of the concentration of the standard working solution to the concentration of the internal standard substance as a Y axis, and calculating by using a calculation formula to obtain the concentration of the semi-volatile organic compound contained in the sample to be detected.
2. The method for detecting the content of the semi-volatile organic compounds in the water supply hose according to claim 1, wherein in the step S2), the weight ratio of the sample to be detected to the mixed solution is 1: 5.
3. The method for detecting the content of the semi-volatile organic compounds in the water supply hose according to claim 1, wherein in the step S2), the volume mixing ratio of the ethyl acetate, the acetone and the n-hexane in the mixed solution is 1:3: 3.
4. The method for detecting the content of the semi-volatile organic compounds in the water supply hose according to claim 1, wherein in step S2), the frequency of the ultrasonic wave is 40kHz, and the power is 500W.
5. The method as claimed in claim 1, wherein in step S3), the filter membrane is a 0.45um organic filter membrane.
6. The method for detecting the content of semi-volatile organic compounds in a water hose according to claim 1, wherein in the steps S3) and S4), the internal standard solution is a solution with a content of 50ppm of deuteroflexor having a chemical formula of C18D 12.
7. The method for detecting the content of the semi-volatile organic compounds in the water supply hose according to claim 1, wherein in the step S5), the working conditions of the GCMS gas chromatograph-mass spectrometer are as follows:
the chromatographic column is a quartz capillary chromatographic column with RXI-5MS of 30 mm multiplied by 0.25 mm;
the thickness of the liquid film is 0.25 um; the temperature of a sample inlet is 300 ℃; the interface temperature is 300 ℃; ion source temperature: 280 ℃;
the temperature rising procedure is as follows: maintaining the initial temperature at 45 deg.C for 4 min; heating to 130 deg.C at 40 deg.C/min, and maintaining for 0 min; heating to 180 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min; heating to 240 deg.C at a speed of 7 deg.C/min, and maintaining for 0 min; heating to 320 deg.C at a speed of 12 deg.C/min, and maintaining for 0 min;
adopting no-split-flow sample injection, wherein the linear velocity of the sample injection is 33 cm/s.
8. The method for detecting the content of semi-volatile organic compounds in the water hose according to claim 1, wherein in step 5), the calculation formula of the concentration of the semi-volatile organic compounds contained in the test sample is as follows:
in the formula, C is the content of semi-volatile organic compounds to be detected in the soak solution, and the unit is ug/ml;
x is the concentration of the extract on the machine, and the unit is ug/ml;
X0the unit of the concentration of the blank extract on the machine is ug/ml;
V1the final volume of the extract is the unit of ml;
V2the volume of the soaking solution is in ml.
9. The method for detecting the content of semi-volatile organic compounds in the water hose according to claim 1, wherein the semi-volatile organic compounds further comprise all semi-volatile organic compounds indicated in the national standard GB 23448.
10. The method of claim 1, wherein the semi-volatile organic compound further comprises 1.3-dichlorobenzene and/or hexachlorobutadiene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110062524.3A CN112858557A (en) | 2021-01-18 | 2021-01-18 | Method for detecting content of semi-volatile organic compounds in water supply hose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110062524.3A CN112858557A (en) | 2021-01-18 | 2021-01-18 | Method for detecting content of semi-volatile organic compounds in water supply hose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112858557A true CN112858557A (en) | 2021-05-28 |
Family
ID=76006485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110062524.3A Pending CN112858557A (en) | 2021-01-18 | 2021-01-18 | Method for detecting content of semi-volatile organic compounds in water supply hose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112858557A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015014294A1 (en) * | 2013-08-01 | 2015-02-05 | 同方威视技术股份有限公司 | Method used for rapid testing of highly volatile substances of very high concern in textiles |
| CN105572285A (en) * | 2015-12-29 | 2016-05-11 | 江苏中烟工业有限责任公司 | Method for measuring semi-volatile substances in mainstream smoke of cigarettes |
| CN107703236A (en) * | 2017-09-26 | 2018-02-16 | 广东工业大学 | A kind of extraction detection method of Phthalate Esters In Soil |
| CN108152397A (en) * | 2017-12-14 | 2018-06-12 | 浙江工业大学 | The method for detecting hexachlorobutadiene in incineration of refuse flyash, pentachlorobenzene and hexachloro-benzene simultaneously |
| CN109298083A (en) * | 2018-07-05 | 2019-02-01 | 杭州格临检测股份有限公司 | A kind of measuring method of the semi-volatile organic matter based on gas chromatography mass spectrometry |
| CN109633004A (en) * | 2018-12-27 | 2019-04-16 | 嘉兴学院 | A kind of method of trichlorophenol, 2,4,6 ,-T content in detection leather |
-
2021
- 2021-01-18 CN CN202110062524.3A patent/CN112858557A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015014294A1 (en) * | 2013-08-01 | 2015-02-05 | 同方威视技术股份有限公司 | Method used for rapid testing of highly volatile substances of very high concern in textiles |
| CN105572285A (en) * | 2015-12-29 | 2016-05-11 | 江苏中烟工业有限责任公司 | Method for measuring semi-volatile substances in mainstream smoke of cigarettes |
| CN107703236A (en) * | 2017-09-26 | 2018-02-16 | 广东工业大学 | A kind of extraction detection method of Phthalate Esters In Soil |
| CN108152397A (en) * | 2017-12-14 | 2018-06-12 | 浙江工业大学 | The method for detecting hexachlorobutadiene in incineration of refuse flyash, pentachlorobenzene and hexachloro-benzene simultaneously |
| CN109298083A (en) * | 2018-07-05 | 2019-02-01 | 杭州格临检测股份有限公司 | A kind of measuring method of the semi-volatile organic matter based on gas chromatography mass spectrometry |
| CN109633004A (en) * | 2018-12-27 | 2019-04-16 | 嘉兴学院 | A kind of method of trichlorophenol, 2,4,6 ,-T content in detection leather |
Non-Patent Citations (1)
| Title |
|---|
| 李利荣;吴宇峰;杨家凤;时庭锐;: "土壤中64种痕量半挥发性有机污染物的分析方法研究", 分析试验室, vol. 26, no. 01, pages 79 - 84 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Smith et al. | Determination of part-per-trillion levels of polychlorinated dibenzofurans and dioxins in environmental samples | |
| US10627328B2 (en) | Siloxane column based liquid phase microextraction and process | |
| Clement et al. | Environmental analysis | |
| Maceira et al. | Occurrence of plastic additives in outdoor air particulate matters from two industrial parks of Tarragona, Spain: Human inhalation intake risk assessment | |
| Dufková et al. | Determination of C5–C12 perfluoroalkyl carboxylic acids in river water samples in the Czech Republic by GC–MS after SPE preconcentration | |
| García-Córcoles et al. | Chromatographic methods for the determination of emerging contaminants in natural water and wastewater samples: a review | |
| Sloan et al. | Northwest fisheries science center organic analytical procedures | |
| Wu et al. | Evaluating bioavailability of organic pollutants in soils by sequential ultrasonic extraction procedure | |
| Chee et al. | Determination of organochlorine pesticides in water by membranous solid-phase extraction, and in sediment by microwave-assisted solvent extraction with gas chromatography and electron-capture and mass spectrometric detection | |
| CN103592399A (en) | Method capable of simultaneously measuring organochlorine pesticide concentration and synthetic musk concentration in human serum | |
| CN101813677B (en) | Method for analyzing and determining organics persistently containing chlorine in aquatic product | |
| Wang et al. | A novel method based on combining ultrasonic-assisted dispersive solid-phase extraction and low-density solvent dispersive liquid–liquid microextraction (UA-DSPE-LDS-DLLME) for the determination of organophosphorus pesticides in soil | |
| Zhu et al. | Simple and fast determination of perfluorinated compounds in Taihu Lake by SPE-UHPLC–MS/MS | |
| Pan et al. | Solid phase microextraction procedure for the determination of alkylphenols in water by on-fiber derivatization with N-tert-butyl-dimethylsilyl-N-methyltrifluoroacetamide | |
| CN112858557A (en) | Method for detecting content of semi-volatile organic compounds in water supply hose | |
| Parkes et al. | Analysis of volatile fatty acids by ion-exclusion chromatography, with special reference to marine pore water | |
| Wegman et al. | The microcoulometric determination of extractable organic halogen in surface water; application to surface waters of The Netherlands | |
| Frébortová et al. | Trace enrichment of chlorinated phenols from drinking water on chemically bonded sorbents for high-performance liquid chromatography | |
| Nagase et al. | Determination of tributyltin and triphenyltin compounds in hair and fish using a hydrolysis technique and gas chromatography with flame photometric detection | |
| Bergqvist et al. | Lipid removal using semipermeable membranes (SPMs) in PCDD and PCDF analysis of fat-rich environmental samples | |
| Sibali et al. | Levels of selected alkylphenol ethoxylates (APEs) in water and sediment samples from the Jukskei River catchment area in Gauteng, South Africa | |
| HASEGAWA et al. | Liquid Chromatography-mass Spectrometric Analysisof p-cumylphenol and Bisphenol A in Environmental Waters in Nagoya City | |
| Tanaka et al. | Determination of total phthalate esters in wastewaters by differential pulse polarography | |
| Evenset et al. | Screening of new contaminants in samples from the Norwegian Arctic: silver, platinum, sucralose, bisphenol A, tetrabrombisphenol A, siloxanes, phtalates (DEHP), phosphororganic flame retardants | |
| Taheri et al. | The role of agricultural and residential land-uses on organophosphorus and organochlorine pesticides residues in water and sediments of Siahrud River, Qaemshahr |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |