CN112710764B - Method for detecting organic mercury in waste textile raw material - Google Patents
Method for detecting organic mercury in waste textile raw material Download PDFInfo
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Abstract
The invention discloses a method for detecting organic mercury in waste textile raw materials, which comprises the steps of establishing an organic mercury standard chromatogram by using an organic mercury standard substance, and carrying out liquid chromatogram and inductively coupled plasma mass spectrum detection by carrying out ultrasonic-assisted extraction on pollutants in the waste textile raw materials so as to carry out qualitative and quantitative detection on the organic mercury in the waste textile raw materials. The method comprises the steps of establishing pretreatment conditions and detecting a sample; the method comprises the steps of preparing a standard solution of organic mercury pollutants, carrying out liquid chromatography and inductively coupled plasma mass spectrometry detection on the standard solution, determining the types and characteristic ions of the organic mercury pollutants, and further carrying out experimental detection on a waste textile raw material sample. The ultrasonic-assisted extraction enables organic mercury to be fully extracted, further extraction and enrichment are carried out through liquid chromatography extraction, and then the inductively coupled plasma mass spectrometer is used for ion scanning, so that the organic mercury is classified and detected, the method is simple, efficient, accurate and high in sensitivity, and the recycling safety of waste textile raw materials is fully guaranteed.
Description
Technical Field
The invention relates to a method for detecting organic mercury in a waste textile raw material.
Technical Field
The waste textile raw materials can enter the production link after being sorted and processed, and are beneficial supplement of low-end raw material resources in the textile industry. However, the waste textile raw material resources contain various plasticizers, chlorine organic pollutants, o-dichlorobenzene and other pollutants, organic mercury, mercury and compounds thereof, aluminum, cadmium, total chromium, hexavalent chromium, copper and compounds thereof, zinc and compounds thereof, beryllium and compounds thereof, barium and compounds thereof, nickel and compounds thereof, arsenic and compounds thereof, inorganic fluorides, cyanides and other harmful components, so that a series of waste textile raw material detection standards are established in China.
In the above hazardous substances, the toxic amount of the organic mercury is 0.5g and the lethal amount is 1-2 g because of the very strong toxicity of the organic mercury, and the organic mercury mainly affects the nervous system of the human body; therefore, the detection standard is very high, and the waste textile raw material is required not to be detected. However, the current standard method for mercury detection in China mainly aims at the detection of total mercury and mainly aims at water quality, drinking water, water environment and the like. The detection of organic mercury in waste textile raw materials mainly adopts gas chromatography at present, and the detection method has the following defects: on one hand, if the organic mercury content in the waste textile raw material is extremely low, the organic mercury can not be detected easily if the organic mercury is not leached thoroughly during leaching; on the other hand, if the waste textile raw materials contain various hazardous substances, the waste textile raw materials are easily influenced by other substances in the chromatographic separation process, so that the waste textile raw materials cannot be separated, and the result that the waste textile raw materials cannot be detected is obtained. This makes the waste textile material have the risk of national environmental sanitation safety and environmental protection safety, and its reuse goods also has the injury risk that is difficult to predict to the user. Therefore, it is very important to establish a waste textile raw material organic mercury detection mode with high sensitivity and accurate detection.
Disclosure of Invention
Aiming at the existing problems, the invention provides a method for detecting organic mercury in waste textile raw materials, which is characterized in that pollutants in the waste textile raw materials are fully extracted by an ultrasonic-assisted extraction method and then detected by a liquid chromatogram and an inductively coupled plasma mass spectrometry method, so that a simple, efficient and accurate quantitative and qualitative detection method for the organic mercury in the waste textile raw materials is established. The specific technical scheme is as follows:
the method comprises the steps of establishing an organic mercury standard chromatogram by using an organic mercury standard substance, and carrying out liquid chromatogram and inductively coupled plasma mass spectrum detection by carrying out ultrasonic-assisted extraction on pollutants in the waste textile material, so as to carry out qualitative and quantitative detection on the organic mercury in the waste textile material.
The method for detecting the organic mercury in the waste textile raw material comprises the steps of establishing a pretreatment condition and detecting a sample; the method comprises the steps of preparing a standard solution of organic mercury pollutants, carrying out liquid chromatography and inductively coupled plasma mass spectrometry detection on the standard solution, determining the types and characteristic ions of the organic mercury pollutants, and further carrying out experimental detection on a waste textile raw material sample.
The establishing of the pretreatment condition specifically comprises the following steps:
s1-1: preparing a standard stock solution: accurately weighing appropriate amount of organic mercury pollutant standard substances, dissolving with methanol, diluting to constant volume, respectively preparing into standard stock solutions with concentration of 100mg/L, and storing at-4 deg.C;
s1-2: preparing a mixed standard working solution: accurately measuring the standard stock solutions prepared in the step S1-1 respectively, diluting the standard stock solutions with methanol again to constant volume, and preparing a series of standard working solutions with gradient concentrations;
s1-3: ion scanning: performing liquid chromatography extraction on each standard working solution prepared in the step S1-2, and then performing inductively coupled plasma mass spectrometry scanning to obtain an ion current chromatogram of each organic mercury standard;
s1-4: determining the species and the characteristic ions: and (4) determining the peak appearing time of each organic mercury standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step (S1-3), and determining the types and characteristic ions of fragment ions in the mass spectrogram, thereby establishing pretreatment conditions.
As a preferable technical solution, in the step S1-1, the organic mercury standard includes: the purities of the methyl mercury, the ethyl mercury chloride, the phenyl mercury acetate, the ethyl mercury phosphate, the diethyl mercury phosphate, the triethyl mercury phosphate and the sulfanilamide phenyl mercury are all more than 99 percent.
In a preferred embodiment, in step S1-2, the gradient concentration of the mixed standard working solution is 300. Mu.g/L, 200. Mu.g/L, 100. Mu.g/L, or 1. Mu.g/L.
In the method for detecting organic mercury in waste textile raw materials, in step S1-2, a chromatographic column used for liquid chromatography extraction is a C18 reverse phase chromatographic column, and an eluent is used for isocratic elution; the inductively coupled plasma mass spectrometry adopts an EXPEC 7000 type inductively coupled plasma mass spectrometer, and the ion source temperature is 250 ℃ and the quadrupole rod temperature is 120 ℃.
In the method for detecting organic mercury in waste textile raw materials, the experimental detection of the waste textile raw material sample specifically comprises the following steps:
s2-1: ultrasonic extraction: cutting a waste textile raw material sample to be detected into fragments, uniformly mixing the fragments with a certain amount of standard mixed standard solution, and standing for 1.5 hours; placing the mixed sample in an ultrasonic cleaner, performing ultrasonic extraction in a water bath, placing the supernatant in a heart-shaped bottle, and repeatedly extracting for 1 time; mixing the extractive solutions, and further enriching and purifying;
s2-2: liquid phase chromatographic extraction: pouring the extract liquid obtained by ultrasonic extraction in the step S2-1 into a C18 reverse phase chromatographic column, eluting by using eluent, carrying out nitrogen blowing concentration, and carrying out constant volume to 1m by using methanol for further detection;
s2-3: mass spectrum detection: performing mass spectrometry detection on the eluent extracted by the liquid chromatography in the step S2-2 by using an EXPEC 7000 type inductively coupled plasma mass spectrometer to obtain an organic mercury ion current chromatogram map contained in the waste textile raw material sample to be detected;
s2-4: determining the target substance: and (4) analyzing the organic mercury ion current chromatogram of the waste textile raw material sample to be detected obtained in the step (S2-3), and determining the type and the content of the organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and the characteristic ions determined by the standard working solution total ion current chromatogram measured in the steps (S1-3) and (S1-4).
In a preferable embodiment, in the step S2-1, the sample cutting specification is 3X 3mm or less; the extracting solution is a mixed solution of L-cysteine buffer saline and methanol; the ultrasonic extraction conditions are as follows: the temperature is 30 deg.C, frequency is 40KHz, and extraction time is 30min.
In a preferred embodiment, in step S2-2, the eluent for liquid chromatography is a mixed solution of L-cysteine buffered saline and methanol, and the flow rate is 1mL/min.
In a further preferred embodiment, the concentration of the mixed solution of L-cysteine buffer saline and methanol used in the extraction solution and the elution solution is 0.12%; the mixing volume ratio of the L-cysteine buffer saline to the methanol is 92:8.
the invention has the beneficial effects that:
the detection method provided by the invention has the advantages that organic mercury pollutants in the waste textile raw materials are fully extracted by an ultrasonic-assisted extraction method, and then the organic mercury pollutants are detected by a liquid chromatogram and an inductively coupled plasma mass spectrometry method, so that the detection method is simple, efficient and accurate, and the sensitivity is particularly high. And a standard ion chromatogram map is established through the organic mercury standard substance, characteristic ions of different kinds of organic mercury are determined, and then the waste textile raw material sample is detected, so that the result is accurate and reliable. The method comprises the steps of cutting before the detection of a waste textile raw material sample, fully extracting organic mercury in the waste textile raw material through ultrasonic-assisted extraction, further extracting, enriching and purifying through liquid chromatography extraction, and performing ion scanning by using an EXPEC 7000 type inductively coupled plasma mass spectrometer with high sensitivity, so that the organic mercury in the waste textile raw material is fully classified and detected without omission, and the recycling safety of the waste textile raw material is fully ensured.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments.
Example 1
The embodiment is a method for detecting organic mercury in waste textile raw materials, which comprises the steps of establishing an organic mercury standard chromatogram by using an organic mercury standard substance, carrying out liquid chromatogram and inductively coupled plasma mass spectrometry detection by carrying out ultrasonic-assisted extraction on pollutants in the waste textile raw materials, and carrying out qualitative and quantitative detection on the organic mercury in the waste textile raw materials, wherein the method comprises the steps of establishing a pretreatment condition and detecting a sample; the method comprises the steps of preparing a standard solution of organic mercury pollutants, carrying out liquid chromatography and inductively coupled plasma mass spectrometry detection on the standard solution, determining the types and characteristic ions of the organic mercury pollutants, and further carrying out experimental detection on a waste textile raw material sample.
The establishing of the pretreatment condition specifically comprises the following steps:
s1-1: preparing a standard stock solution: accurately weighing appropriate amount of organic mercury pollutant standard substances, dissolving with methanol, diluting to constant volume, respectively preparing standard stock solutions with concentration of 100mg/L, and storing at-4 deg.C; the organic mercury standard comprises: the purities of the methyl mercury, the ethyl mercury chloride, the phenyl mercury acetate, the ethyl mercury phosphate, the diethyl mercury phosphate, the triethyl mercury phosphate and the sulfanilamide phenyl mercury are all more than 99 percent.
S1-2: preparing a mixed standard working solution: accurately measuring the standard stock solutions prepared in the step S1-1 respectively, diluting the standard stock solutions with methanol again to constant volume, and preparing a series of standard working solutions with gradient concentrations; preferably formulated as a concentration gradient: 300. Mu.g/L, 200. Mu.g/L, 100. Mu.g/L, 1. Mu.g/L.
S1-3: ion scanning: performing liquid chromatography extraction on each standard working solution prepared in the step S1-2, and then performing inductively coupled plasma mass spectrometry scanning to obtain an ion current chromatogram of each organic mercury standard; the chromatographic column adopted by the liquid chromatographic extraction is a C18 reversed phase chromatographic column, and the eluent is used for isocratic elution; the inductively coupled plasma mass spectrometry adopts an EXPEC 7000 type inductively coupled plasma mass spectrometer, and the ion source temperature is 250 ℃ and the quadrupole rod temperature is 120 ℃.
S1-4: determining the type and characteristic ions: determining the peak emergence time of each organic mercury standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step S1-3, and determining the types and characteristic ions of fragment ions in the mass spectrogram, thereby establishing pretreatment conditions.
The experimental detection of the waste textile raw material sample specifically comprises the following steps:
s2-1: ultrasonic extraction: cutting a waste textile raw material sample to be detected into fragments with the size of less than 3 multiplied by 3mm, uniformly mixing 1g of the waste textile raw material sample with 10ml of standard mixed standard solution, and standing for 1.5 hours; putting the mixed sample into an ultrasonic cleaner, and carrying out ultrasonic extraction in a water bath; the extract was a mixed solution of 0.12% L-cysteine buffered saline and methanol (V/V = 92: 8); the ultrasonic extraction conditions are as follows: the temperature is 30 deg.C, the frequency is 40KHz, and the extraction time is 30min. Placing the supernatant in a heart-shaped flask, and repeating the above extraction conditions for 1 time; mixing the extractive solutions, and further enriching and purifying;
s2-2: liquid phase chromatographic extraction: pouring the extract obtained by ultrasonic extraction in the step S2-1 into a C18 reverse phase chromatographic column, similarly eluting by using a mixed solution of 0.12% L-cysteine buffer saline and methanol (V/V = 92: 8) as an eluent, wherein the flow rate is 1mL/min, carrying out nitrogen blowing concentration, and carrying out constant volume to 1m by using methanol for further detection;
s2-3: mass spectrum detection: performing mass spectrometry detection on the eluent extracted by the liquid chromatography in the step S2-2 by using an EXPEC 7000 type inductively coupled plasma mass spectrometer to obtain an organic mercury ion current chromatogram map contained in the waste textile raw material sample to be detected;
s2-4: determining the target substance: and (4) analyzing the organic mercury ion current chromatogram of the waste textile raw material sample to be detected obtained in the step (S2-3), and determining the type and the content of the organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and the characteristic ions determined by the standard working solution total ion current chromatogram measured in the steps (S1-3) and (S1-4).
Example 2
In this example, the correlation and detection limit verification, and the sensitivity and accuracy verification were performed on the waste textile raw material organic mercury detection method described in example 1.
The method for verifying the correlation and the detection limit in the embodiment comprises the following steps: and respectively matching 8 standard working nights of methyl mercury, ethyl mercury chloride, phenylmercuric acetate, ethyl mercury phosphate, diethyl mercury phosphate, triethyl mercury phosphate, phenylmercuric sulfadiazine and the like, and drawing a working curve by taking the mass concentration as a horizontal coordinate and the peak area as a vertical coordinate. The detection concentration is verified to be in a linear range of 0.550 mu g/L, correlation coefficients of linear equations of methyl mercury and ethyl mercury are both greater than 0.9999, the detection limit is 2 mu g/kg, and the method is suitable for detecting organic mercury pollutants.
The verification of sensitivity and accuracy in this embodiment is: high, medium and low 3 levels of positive samples are prepared, 7 times of parallel experiments are carried out under the screened optimal experiment conditions, and the measured recovery rate and relative deviation (RSD) results are shown in a table 1.
TABLE 1.8 sample recovery and relative deviation (RSD) of organomercury contaminants
The table shows that the recovery rates of the 3 kinds of additives with different concentrations are all over 80%, wherein the recovery rates of the methyl mercury, the ethyl mercury, the phenylmercuric acetate and the sulfanilamide phenylmercuric are all over 90%, and the recovery rate of the methyl mercury is over 95%; and the relative standard deviation (n = 3) RSD of the whole experiment is 1.8% -45%, which shows that the method has very good sensitivity and accuracy.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. Furthermore, it should be understood that although the present specification describes embodiments, these embodiments are not intended to be included solely, and such description is for clarity only, and those skilled in the art will be able to make the present specification as a whole, and the embodiments of the present invention may be appropriately combined to form other embodiments understood by those skilled in the art.
Claims (5)
1. A method for detecting organic mercury in waste textile raw materials is characterized by comprising the following steps: the method comprises the steps of establishing an organic mercury standard chromatogram by using an organic mercury standard substance, performing liquid chromatogram and inductively coupled plasma mass spectrometry detection by extracting pollutants in waste textile raw materials with the assistance of ultrasonic waves, and performing qualitative and quantitative detection on the organic mercury in the waste textile raw materials, wherein the method comprises the steps of establishing a pretreatment condition and detecting a sample; the method comprises the following steps of preparing a standard solution of organic mercury pollutants, carrying out liquid chromatography and inductively coupled plasma mass spectrometry detection on the standard solution, determining the types and characteristic ions of the organic mercury pollutants, and further carrying out experimental detection on a waste textile raw material sample, wherein the step of establishing pretreatment conditions specifically comprises the following steps:
s1-1: preparing a standard stock solution: accurately weighing a proper amount of organic mercury pollutant standard substances respectively, dissolving with methanol, diluting to constant volume, preparing standard stock solutions with the concentration of 100mg/L respectively, and storing at-4 ℃ for later use, wherein the organic mercury pollutant standard substances comprise: methyl mercury, ethyl mercury chloride, phenyl mercury acetate, ethyl mercury phosphate, diethyl mercury phosphate, triethyl mercury phosphate and sulfanilamide phenyl mercury, wherein the purity of the methyl mercury, the ethyl mercury chloride, the phenyl mercury acetate, the ethyl mercury phosphate, the diethyl mercury phosphate, the triethyl mercury phosphate and the sulfanilamide phenyl mercury is more than 99 percent;
s1-2: preparing a mixed standard working solution: accurately measuring the standard stock solutions prepared in the step S1-1 respectively, diluting the standard stock solutions with methanol again to constant volume, and preparing a series of standard working solutions with gradient concentrations;
s1-3: ion scanning: performing liquid chromatography on each standard working solution prepared in the step S1-2, and then performing inductively coupled plasma mass spectrometry scanning to obtain an ion current chromatogram of each organic mercury standard;
s1-4: determining the species and the characteristic ions: determining the peak emergence time of each organic mercury standard substance in the mixed standard stock solution according to the chromatogram obtained by ion scanning in the step S1-3, determining the types and characteristic ions of fragment ions in the mass spectrogram, thereby establishing pretreatment conditions,
the experimental detection of the waste textile raw material sample specifically comprises the following steps:
s2-1: ultrasonic extraction: cutting a waste textile raw material sample to be detected into fragments, uniformly mixing the fragments with a certain amount of standard mixed standard solution, and standing for 1.5 hours; placing the mixed sample in an ultrasonic cleaner, performing ultrasonic extraction in a water bath, placing the supernatant in a heart-shaped bottle, and repeatedly extracting for 1 time; mixing the extractive solutions, and further enriching and purifying;
s2-2: liquid chromatography: injecting the extract liquid obtained by ultrasonic extraction in the step S2-1 into a C18 reversed phase chromatographic column, eluting by using eluent, carrying out nitrogen blowing concentration, and carrying out constant volume to 1ml by using methanol for further detection;
s2-3: mass spectrum detection: performing mass spectrometry detection on the eluent of the liquid chromatogram in the step S2-2 by using an EXPEC 7000 type inductively coupled plasma mass spectrometer to obtain an organic mercury ion current chromatogram map contained in the waste textile raw material sample to be detected;
s2-4: determining the target substance: analyzing the organic mercury ion current chromatogram of the waste textile raw material sample to be detected obtained in the step S2-3, determining the type and the content of organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and the characteristic ions determined by the standard working solution total ion current chromatogram measured in the steps S1-3 and S1-4,
wherein the standard mixed standard solution and the eluent are both mixed solution of 0.12% of L-cysteine buffer saline and methanol, and the volume ratio of the 0.12% of the L-cysteine buffer saline to the methanol is 92:8.
2. the method for detecting organic mercury in waste textile raw materials according to claim 1, characterized in that: in the step S1-2, the gradient concentration of the mixed standard working solution is 300. Mu.g/L, 200. Mu.g/L, 100. Mu.g/L and 1. Mu.g/L.
3. The method for detecting organic mercury in waste textile raw materials according to claim 2, characterized in that: in the step S1-2, a chromatographic column adopted by the liquid chromatography is a C18 reverse phase chromatographic column, and an eluent is used for isocratic elution; the inductively coupled plasma mass spectrometry adopts an EXPEC 7000 type inductively coupled plasma mass spectrometer, and the ion source temperature is 250 ℃ and the quadrupole rod temperature is 120 ℃.
4. The method for detecting organic mercury in waste textile raw materials according to claim 3, characterized in that: in the step S2-1, the sample cutting specification is less than 3 x 3 mm; the extracting solution is a mixed solution of L-cysteine buffer saline and methanol; the ultrasonic extraction conditions are as follows: the temperature is 30 deg.C, frequency is 40KHz, and extraction time is 30min.
5. The method for detecting organic mercury in waste textile raw materials according to claim 4, characterized in that: in the step S2-2, the liquid chromatography eluent is a mixed solution of L-cysteine buffer saline and methanol, and the flow rate is 1mL/min.
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