CN112710764A - Method for detecting organic mercury in waste textile raw material - Google Patents
Method for detecting organic mercury in waste textile raw material Download PDFInfo
- Publication number
- CN112710764A CN112710764A CN202011524453.6A CN202011524453A CN112710764A CN 112710764 A CN112710764 A CN 112710764A CN 202011524453 A CN202011524453 A CN 202011524453A CN 112710764 A CN112710764 A CN 112710764A
- Authority
- CN
- China
- Prior art keywords
- organic mercury
- textile raw
- waste textile
- mercury
- standard
- 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.)
- Granted
Links
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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
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 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 a production link after being sorted and processed, and the method is beneficial to 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, and also contain 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 hazardous substances, the toxic amount of the organic mercury is 0.5g and the lethal amount is 1-2 g because the organic mercury has very strong toxicity, and the toxic amount mainly affects the nervous system of a 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 cannot be detected. 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 spectrometry detection by using pollutants in the waste textile raw material through ultrasonic-assisted extraction to qualitatively and quantitatively detect the organic mercury in the waste textile raw 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 standard stock solutions with concentration of 100mg/L, and storing at-4 deg.C;
s1-2: preparing a mixed standard working solution: respectively and accurately measuring the standard stock solutions prepared in the step S1-1, diluting the standard stock solutions with methanol again to constant volume, and preparing standard working solutions with series of 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 product;
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.
In a preferred embodiment, in 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, the chromatographic column used for liquid chromatography extraction is a C18 reverse 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 ℃.
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 an 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 content of organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and 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 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 30 min.
In a preferred embodiment, in step S2-2, the eluent for liquid chromatography is a mixed solution of L-cysteine buffered saline and methanol at a flow rate of 1 mL/min.
In a further preferred embodiment, the concentration of the mixed solution of L-cysteine buffered saline and methanol used for 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 standard ion chromatograms are established through organic mercury standards, characteristic ions of different types 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: respectively and accurately measuring the standard stock solutions prepared in the step S1-1, diluting the standard stock solutions with methanol again to constant volume, and preparing standard working solutions with series of 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 product; the chromatographic column adopted by the liquid phase 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 fragments 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/V92: 8); the ultrasonic extraction conditions are as follows: the temperature is 30 deg.C, frequency is 40KHz, and extraction time is 30 min. 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 in the ultrasonic extraction in the step S2-1 into a C18 reverse phase chromatographic column, eluting by using a mixed solution of 0.12% L-cysteine buffered saline and methanol (V/V is 92:8) as an eluent at the flow rate of 1mL/min, carrying out nitrogen blowing concentration, and carrying out constant volume of 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 content of organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and 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.
In this embodiment, the correlation and detection limit verification method includes: and respectively matching with 8 standard working nights of methyl mercury, ethyl mercury chloride, phenyl mercury acetate, ethyl mercury phosphate, diethyl mercury phosphate, triethyl mercury phosphate, sulfanilamide phenyl mercury and the like, and drawing a working curve by taking the mass concentration as a horizontal coordinate and taking a 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, and 7 parallel experiments are carried out under the screened optimal experimental conditions, and the measured recovery rate and relative deviation (RSD) results are shown in table 2.
TABLE 2.8 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 is 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 (10)
1. A method for detecting organic mercury in waste textile raw materials is characterized by comprising the following steps: the method establishes an organic mercury standard chromatogram by using an organic mercury standard substance, and performs liquid chromatogram and inductively coupled plasma mass spectrometry detection by extracting pollutants in the waste textile raw material with the assistance of ultrasonic waves, so as to perform qualitative and quantitative detection on the organic mercury in the waste textile raw material.
2. The method for detecting organic mercury in waste textile raw materials according to claim 1, characterized in that: 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.
3. The method for detecting organic mercury in waste textile raw materials according to claim 2, characterized in that: 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;
s1-2: preparing a mixed standard working solution: respectively and accurately measuring the standard stock solutions prepared in the step S1-1, diluting the standard stock solutions with methanol again to constant volume, and preparing standard working solutions with series of 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 product;
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.
4. The method for detecting organic mercury in waste textile raw materials according to claim 3, characterized in that: in 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.
5. The method for detecting organic mercury in waste textile raw materials according to claim 3, characterized in that: in step S1-2, 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, 1. mu.g/L.
6. The method for detecting organic mercury in waste textile raw materials according to claim 3, characterized in that: in step S1-2, the liquid chromatography extraction adopts a C18 reversed phase chromatographic column, and isocratic elution is carried out by using an eluent; 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 ℃.
7. The method for detecting organic mercury in waste textile raw materials according to claim 2, characterized in that: 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 an 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 content of organic mercury pollutants contained in the waste textile raw material sample to be detected according to the type and characteristic ions determined by the standard working solution total ion current chromatogram measured in the steps S1-3 and S1-4.
8. The method for detecting organic mercury in waste textile raw materials according to claim 7, characterized in that: in 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 30 min.
9. The method for detecting organic mercury in waste textile raw materials according to claim 7, characterized in that: in step S2-2, the liquid chromatography extraction eluent is a mixed solution of L-cysteine buffered saline and methanol at a flow rate of 1 mL/min.
10. The method for detecting organic mercury in waste textile raw material according to claim 8 or 9, characterized in that: the concentration of the mixed solution of L-cysteine buffer saline and methanol used by the extracting solution and the eluent is 0.12 percent; the mixing volume ratio of the L-cysteine buffer saline to the methanol is 92: 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011524453.6A CN112710764B (en) | 2020-12-22 | 2020-12-22 | Method for detecting organic mercury in waste textile raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011524453.6A CN112710764B (en) | 2020-12-22 | 2020-12-22 | Method for detecting organic mercury in waste textile raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112710764A true CN112710764A (en) | 2021-04-27 |
| CN112710764B CN112710764B (en) | 2023-03-17 |
Family
ID=75544972
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011524453.6A Active CN112710764B (en) | 2020-12-22 | 2020-12-22 | Method for detecting organic mercury in waste textile raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112710764B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969370A (en) * | 2014-05-19 | 2014-08-06 | 莱阳恒润食品有限公司 | Method for simultaneously detecting mathylmercury chloride, ethylmercury chloride, dimethylmercury and diphenylmercury in irrigation water |
| BR112014026310A2 (en) * | 2012-04-26 | 2017-06-27 | Niva | method for detoxifying or measuring at least one compound or at least one fluid in a host body |
| CN107677744A (en) * | 2017-09-28 | 2018-02-09 | 遵义市产品质量检验检测院 | The detection method of form mercury in a kind of animal tissue cell |
-
2020
- 2020-12-22 CN CN202011524453.6A patent/CN112710764B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BR112014026310A2 (en) * | 2012-04-26 | 2017-06-27 | Niva | method for detoxifying or measuring at least one compound or at least one fluid in a host body |
| CN103969370A (en) * | 2014-05-19 | 2014-08-06 | 莱阳恒润食品有限公司 | Method for simultaneously detecting mathylmercury chloride, ethylmercury chloride, dimethylmercury and diphenylmercury in irrigation water |
| CN107677744A (en) * | 2017-09-28 | 2018-02-09 | 遵义市产品质量检验检测院 | The detection method of form mercury in a kind of animal tissue cell |
Non-Patent Citations (4)
| Title |
|---|
| SAMUEL S. DE SOUZA等: "A simple method for methylmercury, inorganic mercury and ethylmercury determination in plasma samples by high performance liquid chromatography–cold-vapor-inductively coupled plasma mass spectrometry", 《ANALYTICA CHIMICA ACTA》 * |
| 中华人民共和国国家质量监督检验检疫总局: "《中华人民共和国出入境检验检疫行业标准》", 21 July 2017 * |
| 刘敏华等: "液相色谱－电感耦合等离子体质谱法测定纺织品中有机汞", 《上海纺织科技》 * |
| 林晓娜等: "微波萃取结合高效液相色谱-电感耦合等离子体串联质谱同步分析水中砷、硒和铬形态", 《食品科学》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112710764B (en) | 2023-03-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Biller et al. | Analysis of Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb in seawater using the Nobias-chelate PA1 resin and magnetic sector inductively coupled plasma mass spectrometry (ICP-MS) | |
| CN105866302B (en) | A kind of method that 7 kinds of biogenic amines in phase chromatogram concatenation QDa while quick detection white wine are closed using ultra high efficiency | |
| Chen et al. | Speciation of mercury in various samples from the micro-ecosystem of East Lake by hollow fiber-liquid–liquid–liquid microextraction-HPLC-ICP-MS | |
| CN102798681A (en) | Method for determining nitrate and nitrite ions in cigarette tipping paper | |
| CN108362786B (en) | Rapid solvent extraction analysis method for N, N-dimethylformamide in soil | |
| CN112326812A (en) | Method for simultaneously detecting five pesticides in underground water by isotope dilution-ONLINESPE-HRMS | |
| CN112684069A (en) | Method for measuring methylnaphthalene compound in water | |
| Bakircioglu et al. | Concentration of cadmium, copper and zinc using water soluble polyacrylic acid polymer | |
| CN112710764B (en) | Method for detecting organic mercury in waste textile raw material | |
| CN112730662B (en) | Method for simultaneously determining two plasticizers, i.e. phthalate and adipate in textile solid waste | |
| Hou et al. | Arsenic species analysis at trace level by high performance liquid chromatography with inductively coupled plasma mass spectrometry | |
| Guéguen et al. | Use of chelating resins and inductively coupled plasma mass spectrometry for simultaneous determination of trace and major elements in small volumes of saline water samples | |
| Akman et al. | Determination of lead and nickel in Apple-Leaves and sea-water by electrothermal atomic absorption spectrometry after solid-phase extraction using Chromosorb-107 filled in a syringe | |
| CN111413432A (en) | Method for detecting trace PFOA (perfluorooctanoic acid) in fluorine-containing polymer emulsion product | |
| CN107632081B (en) | Method for detecting content of octamethylcyclotetrasiloxane in textile by gas chromatography-mass spectrometry | |
| CN114414708B (en) | Method for detecting tetraethylene glycol dimethyl ether | |
| CN105572249A (en) | Method for carrying out risk assessment on influence of activated carbon on wine product | |
| Kumar et al. | Determination of chloride in nuclear-grade boron carbide by ion chromatography | |
| Asadoulahi et al. | Determination of thallium traces by ETAAS after on-line matrix separation and preconcentration in a flow injection system | |
| CN112526030A (en) | Method for analyzing diallyl trisulfide in food industry wastewater | |
| CN111855870A (en) | Method for determining polychlorinated biphenyl compounds in water | |
| CN106324169A (en) | Solid phase extraction-gas chromatography-tandem mass spectrum detection method for amide fungicides in wine | |
| Fan et al. | Simultaneous determination of 20 phthalate esters in oil-free food by UPLC/MS/MS | |
| CN112578071A (en) | Quantitative analysis method for inorganic acid salt in electrolytic stripping powder | |
| CN107490634B (en) | Method for detecting content of hexavalent chromium in printing and dyeing wastewater |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |