CN104297238A - Rapid detection method for mercury in lipstick - Google Patents
Rapid detection method for mercury in lipstick Download PDFInfo
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- CN104297238A CN104297238A CN201410559879.3A CN201410559879A CN104297238A CN 104297238 A CN104297238 A CN 104297238A CN 201410559879 A CN201410559879 A CN 201410559879A CN 104297238 A CN104297238 A CN 104297238A
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Abstract
The invention relates to a rapid detection method for mercury in a lipstick. The detection method comprises the following steps: sample digestion, namely firstly volatilizing the lipstick in a water bath to obtain a volatilized sample; adding the volatilized sample into a test tube, and adding a digestion solution for microwave digestion; then preparing a lipstick aqueous solution, respectively adding the aqueous solution of the to-be-detected sample into two colorimetric tubes to obtain a first test sample and a second test sample; adding an acid solution and a sulfur ion reagent into the first test sample and adding an iodine ion reagent into the second test sample; and if grey and black precipitates appear in the first test sample and orange-red precipitates are generated in the second test sample, judging that mercury is contained in the sample. The detection method is simple to operate, rapid in detection and easy in final judgment, has low requirements on operators and detection equipment, is high in sensitivity and can obtain an accurate detection result. Thus, the detection method can meet requirements of an inspection department on selective examination on lipstick samples in large batches.
Description
Technical field
The invention belongs to cosmetics detection field, be specifically related to the detection method of mercury in lipstick.
Background technology
Heavy metal Hg is a kind of poisonous element, to human body, there is more serious harm, also be the heavy metal uniquely existed in liquid form at normal temperatures, by acting on alimentary canal, respiratory tract and mucocutaneous and cause corresponding disease, also there is significantly damage etc. to organism endocrine and nervous system.Have effect of nti-freckle and whitening in the lipstick short time of compound containing mercury, in recent years, many illegal manufacturers, for seeking exorbitant profit, illegally add compound containing mercury in lipstick of being everlasting, constitute great threat to human health.In recent years, relevant departments' sampling result display, China has major part lipstick to add mercury compound, and comparatively moiety content can reach 0.5%-2.5%.
In Gong Shi China " cosmetics health specification ", the taboo of regulation has material, wherein also specifies that the mercury caused by lipstick impurity or other reasons must not more than 1mg/kg.At present, in China's " cosmetics health specification ", the detection method of regulation mercury is cold-vapour atomic absorption method, Atomic fluorophotometry etc., these detection method sample pre-treatments are complicated, and for up to 2-5h, a large amount of oxynitrides can be produced in sample pretreatment process, all harm is brought to ring mirror and testing staff.For this reason, the invention provides a kind of simple to operate, detect rapidly, the large sample selective examination work of lipstick supervision department to lipstick can be met.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides the method for quick of mercury in a kind of lipstick.
Technical scheme of the present invention is as follows:
A method for quick for mercury in lipstick, comprises the following steps:
(1) Specimen eliminating: by lipstick sample, prior to water-bath is volatilized, obtains the sample after volatilizing; Sample after volatilization is added in test tube, adds digestion solution, close the lid, carry out micro-wave digestion, clear up terminal and emit white smoke for starting.
(2) lipstick aqueous solution is prepared: by the sample obtained aqueous solution soluble in water after clearing up in step (1), hydrophobicity sample first adds surfactant, stirs and evenly mixs, then obtained aqueous solution; The aqueous solution of testing sample is placed in respectively two color comparison tubes, is respectively first part of sample, second part of sample;
The process of (3) first parts of samples: add acid solution, after reaction 5-10min, adds sulphion reagent, observing response phenomenon;
The process of (4) second parts of samples: add iodide ion reagent, observing response phenomenon.
Organic solvent described in step (1) is one or more in ethanol, glycerine, propylene glycol, acetone.
Preferably, step (1) is described bath temperature is 50-80 DEG C, and water bath time is 3-5min.
Preferably, the digestion solution described in step (1) is volume ratio is the nitric acid of 4:1 and the mixed liquor of perchloric acid.
Preferably, the surfactant in step (2) be selected from anionic surfactant, zwitterionic surfactant or non-ionic surfactant one or more.
Preferably, described anionic surfactant be selected from odium stearate, lauryl sodium sulfate one or more; Described zwitterionic surfactant be selected from lecithin or betaine one or more; Described non-ionic surfactant be selected from tween, sapn one or more.
Preferably, the acid solution described in step (3) is selected from one or more in nitric acid or hydrochloric acid.
Preferably, described concentration of nitric acid is 0.3-0.8mol/L, and described concentration of hydrochloric acid is 1.5-2.0mol/L;
Preferably, the sulphion reagent described in step (3) is thioacetic acid amine aqueous solution, and concentration is 0.3-0.6mol/L; Iodide ion reagent described in step (4) is potassium iodide aqueous solution, and volumetric concentration is 10-20%.
Step (3) is if there is grey, black in middle reaction solution, and in step (4), reaction solution occurs that salmon pink precipitates, then judge in sample containing mercury.
The present invention compared with prior art, beneficial effect be embodied in following some:
1. the present invention first carries out pre-service to sample, comprises and first heating in water-bath sample, makes the various organic solvent volatilizations in sample complete, avoids the impact of various organic solvent on subsequent operation, improve the accuracy of testing result; And bath temperature is below 80 DEG C, avoid the loss of material mercury to be checked in sample; After the heating, add digestion solution and carry out micro-wave digestion, can reach between 95%-105% the digestion recovery of lipstick, recovering effect is good, and well can control digestion rate, decreases the loss of mercury in operation, improve the recovery, meanwhile, also can reduce the volatilization of mercury, significantly reduce the volatilization harm of mercury to operator and the pollution to environment.
2. mercury can react with sulphion and iodide ion, generate coloured novel substance, mercury and sulphion react, and grey, black can appear in solution, and mercury and iodide ion react, solution can occur that salmon pink precipitates, the present invention, according to the characteristic chromogenic reaction of above-mentioned mercury, carries out qualitative detection to the mercury in lipstick, easy and simple to handle, terminal easily judges, to operating personnel and checkout equipment less demanding.
3. the present invention is before carrying out chromogenic reaction, first adopts acid solution to infiltrate to sample aqueous solution, mercury ion can be made to move to sample surfaces, accelerate the reaction of mercury and iodide ion and sulphion in subsequent operation, Reaction time shorten, also improve being quick on the draw property.
Embodiment
Embodiment 1
A method for quick for mercury in lipstick, comprises the following steps:
(1) Specimen eliminating: to containing ethanol person, first in 50-80 DEG C of water bath with thermostatic control, water-bath 3min volatilize, obtains the sample after volatilization; Add in test tube by the sample after volatilization, adding volume ratio is the nitric acid of 4:1 and the mixed liquor of perchloric acid, closes the lid, carries out micro-wave digestion, clears up terminal and emits white smoke for starting.
(2) lipstick aqueous solution is prepared: by the sample obtained aqueous solution soluble in water after clearing up in step (1); The aqueous solution of testing sample is placed in respectively two color comparison tubes, is respectively first part of sample, second part of sample;
The process of (3) first parts of samples: add the salpeter solution that concentration is 0.3mol/L, after reaction 5min, adds the thioacetic acid amine aqueous solution that concentration is 0.3mol/L, observing response phenomenon;
The process of (4) second parts of samples: add the potassium iodide aqueous solution that volumetric concentration is 10%, observing response phenomenon.
Step (3) is if there is grey, black in middle reaction solution, and in step (4), reaction solution occurs that salmon pink precipitates, then judge in sample containing mercury.
Embodiment 2
A method for quick for mercury in lipstick, comprises the following steps:
(1) Specimen eliminating: to containing glycerine person, first in 80 DEG C of waters bath with thermostatic control, water-bath 3min volatilize, obtains the sample after volatilization; Add in test tube by the sample after volatilization, adding volume ratio is the nitric acid of 4:1 and the mixed liquor of perchloric acid, closes the lid, carries out micro-wave digestion, clears up terminal and emits white smoke for starting.
(2) lipstick aqueous solution is prepared: by the sample obtained aqueous solution soluble in water after clearing up in step (1); The aqueous solution of testing sample is placed in respectively two color comparison tubes, is respectively first part of sample, second part of sample;
The process of (3) first parts of samples: add the salpeter solution that concentration is 0.8mol/L, after reaction 5min, adds the thioacetic acid amine aqueous solution that concentration is 0.6mol/L, observing response phenomenon;
The process of (4) second parts of samples: add the potassium iodide aqueous solution that volumetric concentration is 20%, observing response phenomenon.
Step (3) is if there is grey, black in middle reaction solution, and in step (4), reaction solution occurs that salmon pink precipitates, then judge in sample containing mercury.
Embodiment 3
A method for quick for mercury in lipstick, comprises the following steps:
(1) Specimen eliminating: to containing propylene glycol person, first in 65 DEG C of waters bath with thermostatic control, water-bath 4min volatilize, obtains the sample after volatilization; Add in test tube by the sample after volatilization, adding volume ratio is the nitric acid of 4:1 and the mixed liquor of perchloric acid, closes the lid, carries out micro-wave digestion, clears up terminal and emits white smoke for starting.
(2) lipstick aqueous solution is prepared: hydrophobicity sample first adds lecithin, stirs and evenly mixs, then obtained aqueous solution; The aqueous solution of testing sample is placed in respectively two color comparison tubes, is respectively first part of sample, second part of sample;
The process of (3) first parts of samples: add the hydrochloric acid solution that concentration is 1.5mol/L, after reaction 8min, adds the thioacetic acid amine aqueous solution that concentration is 0.45mol/L, observing response phenomenon;
The process of (4) second parts of samples: add the potassium iodide aqueous solution that volumetric concentration is 15%, observing response phenomenon.
Step (3) is if there is grey, black in middle reaction solution, and in step (4), reaction solution occurs that salmon pink precipitates, then judge in sample containing mercury.
Above-described embodiment is only the preferred embodiment of the present invention, and should not be construed as limitation of the invention, and those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. the method for quick of mercury in lipstick, is characterized in that, comprise the following steps:
(1) Specimen eliminating: by lipstick sample, prior to water-bath is volatilized, obtains the sample after volatilizing; Sample after volatilization is added in test tube, adds digestion solution, close the lid, carry out micro-wave digestion, clear up terminal and emit white smoke for starting.
2.(2) prepare lipstick aqueous solution: by the sample obtained aqueous solution soluble in water after clearing up in step (1), hydrophobicity sample first adds surfactant, stirs and evenly mixs, then obtained aqueous solution; The aqueous solution of testing sample is placed in respectively two color comparison tubes, is respectively first part of sample, second part of sample;
The process of (3) first parts of samples: add acid solution, after reaction 5-10min, adds sulphion reagent, observing response phenomenon;
The process of (4) second parts of samples: add iodide ion reagent, observing response phenomenon.
3. the method for quick of mercury in lipstick according to claim 1, is characterized in that, the organic solvent described in step (1) is one or more in ethanol, glycerine, propylene glycol, acetone.
4. the method for quick of mercury in lipstick according to claim 1, it is characterized in that, step (1) is described bath temperature is 50-80 DEG C, and water bath time is 3-5min.
5. the method for quick of mercury in lipstick according to claim 1, it is characterized in that, described digestion solution is volume ratio is the nitric acid of 4:1 and the mixed liquor of perchloric acid.
6. the method for quick of mercury in lipstick according to claim 1, is characterized in that, the surfactant in step (2) be selected from anionic surfactant, zwitterionic surfactant or non-ionic surfactant one or more.
7. the method for quick of mercury in lipstick according to claim 4, is characterized in that, described anionic surfactant be selected from odium stearate, lauryl sodium sulfate one or more; Described zwitterionic surfactant be selected from lecithin or betaine one or more; Described non-ionic surfactant be selected from tween, sapn one or more.
8. the method for quick of mercury in lipstick according to claim 1, is characterized in that, the acid solution described in step (3) be selected from nitric acid or hydrochloric acid one or more.
9. the method for quick of mercury in lipstick according to claim 6, it is characterized in that, described concentration of nitric acid is 0.3-0.8mol/L, and described concentration of hydrochloric acid is 1.5-2.0mol/L;
In lipstick according to claim 1, the method for quick of mercury, is characterized in that, the sulphion reagent described in step (3) is thioacetic acid amine aqueous solution, and concentration is 0.3-0.6mol/L; Iodide ion reagent described in step (4) is potassium iodide aqueous solution, and volumetric concentration is 10-20%.
10. the method for quick of mercury in lipstick according to claim 1, is characterized in that, step (3) if in reaction solution there is grey, black, in step (4), reaction solution occurs that salmon pink precipitate, then judge to contain mercury in sample.
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| CN201410559879.3A CN104297238A (en) | 2014-10-18 | 2014-10-18 | Rapid detection method for mercury in lipstick |
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| CN201410559879.3A CN104297238A (en) | 2014-10-18 | 2014-10-18 | Rapid detection method for mercury in lipstick |
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| CN104297238A true CN104297238A (en) | 2015-01-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606555A (en) * | 2016-03-10 | 2016-05-25 | 山东五洲检测有限公司 | Method for detecting content of mercury ions in water |
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| CN1687752A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal mercury rapidly, preparation method and application |
| CN101329277A (en) * | 2007-06-22 | 2008-12-24 | 上海市七宝中学 | Method for testing overproof of mercury contained in spot-removing cream |
| CN101685081A (en) * | 2009-08-24 | 2010-03-31 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring various elements in food additive citric acid through ICP-MS |
| CN101782522A (en) * | 2010-02-09 | 2010-07-21 | 广东省疾病预防控制中心 | Quick detection method of mercury in cosmetics and reagent kit thereof |
| CN103616378A (en) * | 2013-11-28 | 2014-03-05 | 中山鼎晟生物科技有限公司 | Method for detecting mercury in cosmetics |
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- 2014-10-18 CN CN201410559879.3A patent/CN104297238A/en active Pending
Patent Citations (5)
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| CN1687752A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal mercury rapidly, preparation method and application |
| CN101329277A (en) * | 2007-06-22 | 2008-12-24 | 上海市七宝中学 | Method for testing overproof of mercury contained in spot-removing cream |
| CN101685081A (en) * | 2009-08-24 | 2010-03-31 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring various elements in food additive citric acid through ICP-MS |
| CN101782522A (en) * | 2010-02-09 | 2010-07-21 | 广东省疾病预防控制中心 | Quick detection method of mercury in cosmetics and reagent kit thereof |
| CN103616378A (en) * | 2013-11-28 | 2014-03-05 | 中山鼎晟生物科技有限公司 | Method for detecting mercury in cosmetics |
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| 梅旭辉等: "《食品药品化妆品监督管理大全》", 30 June 2004 * |
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| CN105606555A (en) * | 2016-03-10 | 2016-05-25 | 山东五洲检测有限公司 | Method for detecting content of mercury ions in water |
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Application publication date: 20150121 |