CN105092501A - Method for determining mercury content in rapeseed oil - Google Patents
Method for determining mercury content in rapeseed oil Download PDFInfo
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- CN105092501A CN105092501A CN201510610500.1A CN201510610500A CN105092501A CN 105092501 A CN105092501 A CN 105092501A CN 201510610500 A CN201510610500 A CN 201510610500A CN 105092501 A CN105092501 A CN 105092501A
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Abstract
The invention discloses a method for determining the mercury content in rapeseed oil. The method for determining the mercury content in the rapeseed oil comprises the following steps that 1, a 10-phenanthroline solution, a hydroxylammonium chloride solution and a sodium acetate buffer solution are prepared; 2, a mercury standard solution is prepared; 3, the double-mercury content is regarded as an x-coordinate and the absorbance is regarded as a y-coordinate to make a mercury standard curve; 4, the rapeseed oil is weighed, concentrated hydrochloric acid, water and glass beads are added, reflux boiling is performed, lower-layer acid extract liquid is filtered by double-layer filter paper after standing and layering, filtrate is fed into a beaker, a conical flask is cleaned, the liquid is poured into a funnel and then is mixed with the filtrate in the beaker after layering, the filter paper is flushed, drying by distillation is performed, and water is added for constant volume so as to obtain a liquid sample; 5, the liquid sample obtained in the step 4 is absorbed in a colorimetric tube, and a mercury marking curve is made as the step 3. The method for determining the mercury content in the rapeseed oil is quick, accurate, simple and convenient to operate, high in sensitivity and smaller in environment pollution, does not use a highly toxic agent, has a minor hazard to human health and can meet the testing demands of ordinary experimenters.
Description
Technical field
The present invention relates to edible oil heavy metal analysis field, specifically referring to a kind of method for measuring mercury content in rapeseed oil.
Background technology
At present, the secondary rapeseed oil that China eats is without refining raw oil, to wherein mercury contaminants content and assay method report less, in international food statutory standard (FAO/CAC) using mercury as pollutant Judging index in edible oil and fat, and define the highest limitation in rapeseed oil.The method surveying mercury content in rapeseed oil in past bibliographical information cannot be applied to the detection of general lab technician, and the need especially had adopt atomic absorption spectrophotometer (AAS), and general laboratory personnel cannot accomplish at all.
Summary of the invention
The object of the present invention is to provide one quick and precisely, easy and simple to handle, highly sensitive, without poisonous reagent, to the less pollution of environment, to the harm of health lighter can meet the method for measuring mercury content in rapeseed oil that general experimenter tests.
The present invention is achieved through the following technical solutions: a kind of method for measuring mercury content in rapeseed oil, comprises the following steps:
(1) 0.1% diethylin bamic acid sodium is prepared, the light amine aqueous solution of 10% hydrochloric acid and sodium acetate buffer solution;
(2) mercury standard solution is prepared;
(3) mercury standard dilution 0.0,0.4,0.8,1.2,1.6,2.0 is drawn in 25mL in color comparison tube, add hydrochloric acid respectively through amine liquid 2mL, with zero pipe zeroing, absorbance is measured with 3cm cell in 510nm wavelength place, two mercury content is abscissa, and absorbance is that ordinate makes mercury typical curve;
(4) rapeseed oil 25 ~ 30g is taken in 250mL triangular flask, add 20mL concentrated hydrochloric acid and 15mL water and beaded glass number, lh is boiled in electric jacket backflow, proceed in 125mL separating funnel after slightly cold, after stratification, lower floor's acid extraction liquid is filtered in 20mL beaker through the double-layer filter paper flushed with watery hydrochloric acid (1:1), divide with hot water and wash triangular flask for several times, pour in funnel, be incorporated in after layering in 200mL beaker, then use a small amount of hot water injection's filter paper, beaker is put on electric furnace and steam to about 5mL, proceeding in volumetric flask adds water is dissolved to 100mL, obtains sample liquid;
(5) the sample liquid 5mL described in absorption step (4) is in 25mL color comparison tube, and same step (3) makes the mark curve of mercury;
(6) content corresponding to curve is searched after measuring absorbance.
In order to realize method of the present invention better, further, in described step (1), the preparation method of 0.1% diethylin bamic acid sodium is for dissolving 0.1g10-ferrosin in 10mL distilled water.
In order to realize method of the present invention better, further, in described step (1), the preparation method of the light amine aqueous solution of 10% hydrochloric acid is for dissolving the light amine of 10g hydrochloric acid in 100mL distilled water.
In order to realize method of the present invention better, further, in described step (1), the preparation method of sodium acetate buffer solution is water-soluble for taking 8.3g sodium acetate, adds 1mL glacial acetic acid and is diluted to 10mL.
In order to realize method of the present invention better, further, in described step (2), prepare the method for mercury standard solution for accurately to take 8.635g, mercuric sulfate is by [NHFe (SO
4)
312H
2o] be dissolved in 200mL distilled water, add 6mL dilution heat of sulfuric acid (l:3), be diluted to 1000mL, diluted 10 times again before using, 1mL dilution is equivalent to 10 μ g mercury.
The present invention compared with prior art, has the following advantages and beneficial effect:
Invention provides one quick and precisely, easy and simple to handle, highly sensitive, without poisonous reagent, to the less pollution of environment, to the harm of health lighter can meet the method for measuring mercury content in rapeseed oil that general experimenter tests.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto, without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacement and change, all should comprise within the scope of the invention.
Embodiment:
The main implementation step of the present embodiment is as follows:
(1) 0.1% diethylin bamic acid sodium is prepared, the light amine aqueous solution of 10% hydrochloric acid and sodium acetate buffer solution;
(2) mercury standard solution is prepared;
(3) mercury standard dilution 0.0,0.4,0.8,1.2,1.6,2.0 is drawn in 25mL in color comparison tube, add hydrochloric acid respectively through amine liquid 2mL, with zero pipe zeroing, absorbance is measured with 3cm cell in 510nm wavelength place, two mercury content is abscissa, and absorbance is that ordinate makes mercury typical curve;
(4) rapeseed oil 25 ~ 30g is taken in 250mL triangular flask, add 20mL concentrated hydrochloric acid and 15mL water and beaded glass number, lh is boiled in electric jacket backflow, proceed in 125mL separating funnel after slightly cold, after stratification, lower floor's acid extraction liquid is filtered in 20mL beaker through the double-layer filter paper flushed with watery hydrochloric acid (1:1), divide with hot water and wash triangular flask for several times, pour in funnel, be incorporated in after layering in 200mL beaker, then use a small amount of hot water injection's filter paper, beaker is put on electric furnace and steam to about 5mL, proceeding in volumetric flask adds water is dissolved to 100mL, obtains sample liquid;
(5) the sample liquid 5mL described in absorption step (4) is in 25mL color comparison tube, and same step (3) makes the mark curve of mercury;
(6) content corresponding to curve is searched after measuring absorbance.
Wherein, in described step (1), the preparation method of 0.1% diethylin bamic acid sodium is for dissolving 0.1g10-ferrosin in 10mL distilled water; In described step (1), the preparation method of the light amine aqueous solution of 10% hydrochloric acid is for dissolving the light amine of 10g hydrochloric acid in 100mL distilled water; In described step (1), the preparation method of sodium acetate buffer solution is water-soluble for taking 8.3g sodium acetate, adds 1mL glacial acetic acid and is diluted to 10mL; In described step (2), prepare the method for mercury standard solution for accurately to take 8.635g, mercuric sulfate is by [NHFe (SO
4)
312H
2o] be dissolved in 200mL distilled water, add 6mL dilution heat of sulfuric acid (l:3), be diluted to 1000mL, diluted 10 times again before using, 1mL dilution is equivalent to 10 μ g mercury.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: do not departing under principle of the present invention and aim and can carry out multiple change, amendment, replacement and modification to these embodiments, scope of the present invention is by claim and equivalents thereof.
Claims (5)
1., for measuring a method for mercury content in rapeseed oil, it is characterized in that: comprise the following steps:
(1) 0.1% diethylin bamic acid sodium is prepared, the light amine aqueous solution of 10% hydrochloric acid and the blue indicator of 0.1% Moschus phenol;
(2) mercury standard solution is prepared;
(3) mercury standard dilution 0.0,0.4,0.8,1.2,1.6,2.0 is drawn in 25mL in color comparison tube, add hydrochloric acid respectively through amine liquid 2mL, with zero pipe zeroing, absorbance is measured with 3cm cell in 510nm wavelength place, two mercury content is abscissa, and absorbance is that ordinate makes mercury typical curve;
(4) rapeseed oil 25 ~ 30g is taken in 250mL triangular flask, add 20mL concentrated hydrochloric acid and 15mL water and 3 ~ 8 beaded glasses, lh is boiled in electric jacket backflow, proceed in 125mL separating funnel after slightly cold, after stratification, lower floor's acid extraction liquid is filtered in 20mL beaker through the double-layer filter paper flushed with watery hydrochloric acid, divide with hot water and wash triangular flask for several times, pour in funnel, be incorporated in after layering in 200mL beaker, then use a small amount of hot water injection's filter paper, beaker is put on electric furnace and steam to about 5mL, proceeding in volumetric flask adds water is dissolved to 100mL, obtains sample liquid;
(5) the sample liquid 5mL described in absorption step (4) is in 25mL color comparison tube, and same step (3) makes the mark curve of mercury;
(6) content corresponding to curve is searched after measuring absorbance.
2. a kind of method for measuring mercury content in rapeseed oil according to claim 1, is characterized in that: in described step (1), and the preparation method of diethylin bamic acid sodium is for dissolving 0.1g diethylin bamic acid sodium in 100mL distilled water.
3. a kind of method for measuring mercury content in rapeseed oil according to claim 1 and 2, is characterized in that: in described step (1), and the preparation method of the light amine aqueous solution of 10% hydrochloric acid is for dissolving the light amine of 10g hydrochloric acid in 100mL distilled water.
4. a kind of method for measuring mercury content in rapeseed oil according to claim 1 and 2, it is characterized in that: in described step (1), the preparation method of the blue indicator of 0.1% Moschus phenol is that dissolving 0.19 bromothymol blue is in 4.3mL, in the NaOH solution of 0.05mol/L, be diluted with water to 100mL.
5. a kind of method for measuring mercury content in rapeseed oil according to claim 1 and 2, it is characterized in that: in described step (2), prepare the method for mercury standard solution for accurately to take 3.126g, mercuric sulfate is by being dissolved in 200mL distilled water, be settled to 2000mL, absorb above-mentioned titer 10mL during use and be diluted to 100mL, the mercurous 1 μ g/mL of this solution.
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| CN201510610500.1A CN105092501A (en) | 2015-09-23 | 2015-09-23 | Method for determining mercury content in rapeseed oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770221A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Method for determining mercury content in acid-making wastewater enriched by wet method |
| CN108871917A (en) * | 2018-08-29 | 2018-11-23 | 重庆科技学院 | The analysis method of heavy metal element chromium and lead in a kind of quick detection vegetable oil |
| RU2696958C1 (en) * | 2018-12-10 | 2019-08-07 | Федеральное государственное бюджетное учреждение науки "Институт токсикологии Федерального медико-биологического агентства" (ФГБУН ИТ ФМБА России) | Method of determining mercury in biological materials |
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770221A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Method for determining mercury content in acid-making wastewater enriched by wet method |
| CN108871917A (en) * | 2018-08-29 | 2018-11-23 | 重庆科技学院 | The analysis method of heavy metal element chromium and lead in a kind of quick detection vegetable oil |
| RU2696958C1 (en) * | 2018-12-10 | 2019-08-07 | Федеральное государственное бюджетное учреждение науки "Институт токсикологии Федерального медико-биологического агентства" (ФГБУН ИТ ФМБА России) | Method of determining mercury in biological materials |
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN111442960B (en) * | 2020-04-20 | 2023-12-29 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
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Application publication date: 20151125 |