CN107462626A - A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component - Google Patents

A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component Download PDF

Info

Publication number
CN107462626A
CN107462626A CN201710729590.5A CN201710729590A CN107462626A CN 107462626 A CN107462626 A CN 107462626A CN 201710729590 A CN201710729590 A CN 201710729590A CN 107462626 A CN107462626 A CN 107462626A
Authority
CN
China
Prior art keywords
micro
contacting metal
tobacco juice
carried out
main component
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710729590.5A
Other languages
Chinese (zh)
Inventor
韩书磊
朱风鹏
陈欢
付亚宁
刘彤
庞永强
侯宏卫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Tobacco Quality Supervision and Inspection Center
Original Assignee
National Tobacco Quality Supervision and Inspection Center
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by National Tobacco Quality Supervision and Inspection Center filed Critical National Tobacco Quality Supervision and Inspection Center
Priority to CN201710729590.5A priority Critical patent/CN107462626A/en
Publication of CN107462626A publication Critical patent/CN107462626A/en
Pending legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat

Abstract

A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component.Electronic cigarette ironware is cut first, crushed, add 3 mL70% nitric acid and 1 mL37% hydrochloric acid and micro-wave digestion is carried out to sample, heating is carried out again catches up with acid, after constant volume being diluted using 1% nitric acid, ICP MS full scan qualitative determination is first carried out, then according to sxemiquantitative test result, selects different extension rates to be diluted acid hydrolysis solution, inner mark method ration is carried out to target component using calibration curve method, and then draws the Contents of Main Components of electronic cigarette liquid contacting metal utensil.The present invention is measured using ICP MS methods to electronic cigarette liquid contacting metal utensil main component first, understand or grasped electronic cigarette liquid contacting metal utensil metallic element or metallic particles occur migrate so that be transferred to the possibility of aerosol, the quality and safety control for electronics smoke product provides technical support and scientific basis.

Description

A kind of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke connects The method for touching ironware main component
Technical field
The invention belongs to physico-chemical analysis technical field, and in particular to a kind of micro-wave digestion-inductivity coupled plasma mass spectrometry The method that method determines tobacco juice for electronic smoke contacting metal utensil main component.
Background technology
In recent years, electronic cigarette is in the gesture of rapid growth in world market.Electronic cigarette enterprise is typically entered with less harmful, smoking cessation etc. Row product marketing, although many studies have shown that, electronic cigarette may be lower than traditional cigarette harmfulness, but also has some evidences Show, electronic cigarette is also not harmless, and its long-time is also unknown using the influence to health.In the potential hazard of electronic cigarette In, poisonous metal exposure is one of harm source of people's common concern, because electronic cigarette utensil is largely metal material, bag Include liquid storage cylinder, heater strip etc., and tobacco juice for electronic smoke is with these ironwares during contacting, metal ingredient or metallic particles It may move in tobacco juice.Secondly, in electronic cigarette aspiration procedure, electronic cigarette heater strip can produce hundreds of in atomization process The high temperature of degree, this cause metallic element in the metal material that is contacted with tobacco juice for electronic smoke or metallic particles occur migration and then The probability for being transferred to aerosol greatly increases.People can endanger health to the prolonged suction of metallics, and this causes people to get over More to pay close attention to potential hazard caused by electronics smoke product tobacco juice contacting metal material.
But the research that is exposed to electronic cigarette poisonous metal of people is concentrated mainly on the research of tobacco juice for electronic smoke and aerosol On, and the research to tobacco juice exposing metal material is relatively fewer.For example, Goniewicz etc. utilizes inductively coupled plasma matter Spectrum（ICP-MS）Instrument is analyzed similar to 16 kinds of metallic elements in the electronic cigarette product aerosol of cigarette 12 kinds of brands, concurrently Nickel content in existing 150 mouthfuls of electronics smoke sols is in 0.11 ~ 0.29 μ g, and cadmium content is in 0.01 ~ 0.22 μ g, and lead content is 0.03 ~0.57 μg（Tobacco Control, 23, 133-139.2014）.Catherine etc. is using ICP-MS to 10 kinds of electronic cigarettes The metallic element of tobacco juice is analyzed contained by cigarette bullet, it is found that lead, chromium, nickel, cadmium, the content of manganese are respectively 4.89 ~ 1970 μ g/L, 53.9~2110 μg/L, 58.7~22600 μg/L, 0.204~12.4 μg/L, 28.7~6910.2 μg/L （Environmental Research, 152, 221-225.2017）.Williams etc. is sent out using inductively coupled plasma Penetrate spectrometer（ICP-OES）Metal element content in Integral electronic cigarette tobacco juice and aerosol is analyzed, and found Nickel, chromium, the content of lead are respectively 0.005 μ g, 0.007 μ g, 0.017 μ g in 10 implication colloidal sols（PLoS ONE, 8, e57987.2013.）.Then, Williams etc. also using ICP-OES to the tin in Integral electronic smoke sol, copper, zinc, Silver, chromium content are analyzed, and utilize SEM（SEM）With X-ray energy spectrum analyzer（EDX）To heater strip and its Welding material etc. has carried out microexamination and principal component analysis, but target component is only limitted to five kinds of compositions of the above, and does not carry out Quantitative analysis, also to liquid storage cylinder etc., other tobacco juice contacting metal materials are not analyzed（PLoS ONE, 10, e0138933.2015）.
The content of the invention
The purpose of the present invention is based on above-mentioned technical deficiency, and this research establishes micro-wave digestion-inductively coupled plasma The method of body mass spectrometric determination tobacco juice for electronic smoke contacting metal utensil main component, and according to semi-quantitative analysis result, to content Of a relatively high element carries out accurate quantitative analysis, has drawn the Contents of Main Components of tobacco juice contacting metal utensil.
The purpose of the present invention is achieved through the following technical solutions：
A kind of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component Method, the ironware for contacting tobacco juice for electronic smoke is crushed, take the sample powder 10 ~ 30 mg, added in counteracting tank, then 3 mL70% nitric acid and 1 mL37% hydrochloric acid are added, closing is screwed, is placed on microwave dissolver, according to the micro-wave digestion program of setting Cleared up, micro-wave digestion program is specific as follows：Room temperature100 ℃（5 min）200（20 min）；Disappear After solution, room temperature is cooled to, and carries out heating and catches up with acid；Sample solution in counteracting tank is transferred to 50 mL plastics volumetric flasks In, rinse counteracting tank 3-4 times with 1% nitric acid, cleaning fluid is transferred in volumetric flask in the lump, with 1% nitric acid constant volume, is carried out after shaking up ICP-MS is tested, and then draws the Contents of Main Components of tobacco juice for electronic smoke contacting metal utensil；Instrumental Analysis process：First carry out complete Scan qualitative determination, then according to sxemiquantitative test result, select different extension rates to be diluted acid hydrolysis solution, so to containing The element measured in 0.1 more than ppb carries out accurate quantitative analysis；Instrument concrete analysis condition setting：Power：1550 w；Carrier gas stream Speed：1.0 L/min；Wriggling revolution speed：0.1 rpm；Analytical model：Crash mode（He）；Collision gas flow velocity：5 ml/min.It is fixed Amount method：Internal standard method, internal standard element are72Ge、115In and209Bi。
In the present invention, the ironware is electronic cigarette solution storage cavity or filter tip etc..Composition in quantitative analysis include but It is not limited to Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pb, Sb, Cd etc..
Compared with prior art, mechanism of the invention and advantage are：
（1）Tobacco juice for electronic smoke contacting metal utensil main component is measured using ICP-MS methods first, understands or grasps Tobacco juice for electronic smoke contacting metal utensil metallic element or metallic particles occur to migrate and then be transferred to the possibility of aerosol, So as to provide technical support and scientific basis for the quality and safety control of electronics smoke product.
（2）Inductivity coupled plasma mass spectrometry (ICP-MS) detection limit is low, the concentration range of linearity up to 7 ~ 8 orders of magnitude, And the larger various elements of content difference can be determined simultaneously, thus as an important tool of elementary analysis.Therefore, this research Using ICP-MS as analytical instrument, Qualitative and quantitative analysis while realizing Determination of multiple metal elements.
（3）The selection of pre-treating method：Because tobacco juice for electronic smoke contacting metal utensil weight is relatively large, directly carry out micro- Ripple resolution can consume substantial amounts of acid, and pollute environment, and therefore, this research is cut using instruments such as cutting clamp, casing knifes to it Cut, crush, and weigh 10-30 mg metal materials and analyzed, while measurement result accuracy is ensured, subtract to greatest extent Lack the use of acid hydrolysis solution, and then reduce environmental pollution.In terms of the selection of acid hydrolysis solution, 4 mL70% nitric acid, 1 are compared ML37% hydrochloric acid, the mL37% hydrochloric acid of 3 mL70% nitric acid+1 and the mL37% hydrochloric acid of 1 mL70% nitric acid+3 to the solute effect of object, It was found that the mL37% hydrochloric acid effects of 3 mL70% nitric acid+1 are best, the mL37% hydrochloric acid of 3 mL70% nitric acid+1 finally is used as acidolysis Liquid.Involved % is percent by volume in the present invention.
（4）Object quantitative approach：Because the composition of target analytes is unknown, the acid hydrolysis solution of high concentration is selected first Full scan qualitative determination is carried out, then according to sxemiquantitative test result, selects different extension rates, is carried out using ultra-pure water dilute Release, and according to the concentration preparing standard solution of target compound, accurate quantitative analysis point is carried out to element of the content in 0.1 more than ppb Analysis, quantitative approach use internal standard method.
（5）The selection of internal standard element：ICP-MS analysis during, be usually added into be marked with correction matrix caused by element ring It should change and compensate the influence of long term signal drift.Pass through the full scan to essential element in tobacco juice for electronic smoke contacting metal utensil Analysis, find conventional internal standard element72Ge、115In and209Bi Element detection results are below the detection limit of instrument, therefore use72Ge、115In and209The internal standard element that Bi elements detect as ICP-MS.
Embodiment
The present invention is further described by specific examples below, but does not limit the present invention.
Embodiment 1：
1st, instrument and reagent
Icp mses（ICP-MS7900；Agilent）, microwave dissolver（MarsX_press, the U.S. CEM）；Electronic balance（German Sartorius CP225D, sensibility reciprocal：0.01 mg）；Metal ion standard liquid（Environmental standard is molten Liquid, Agilent）；37% hydrochloric acid（German Merk）；70% nitric acid（German Merk）；Ultra-pure water used is by Milli-Q systems （Milford, MA, USA）It is made；Metallic element standard liquid（Environmental standard solution, Agilent. Ca, Fe, K, Mg, Na:Concentration is 1000 μ g/mL；Ag, Al, As, Ba, Be, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sb, Se, Th, TI, U, V, Zn:Concentration is 10 μ g/mL）.
2nd, sample pre-treatments
The ironware for contacting tobacco juice for electronic smoke is crushed, takes the sample powder 10 ~ 30 mg, is added in counteracting tank, then is added Enter 3 mL70% nitric acid and 1 mL37% hydrochloric acid, screw closing, be placed on microwave dissolver, enter according to the micro-wave digestion program of setting Row resolution, micro-wave digestion program are specific as follows：Room temperature100 ℃（5 min）200（20 min）；Disappear After solution, room temperature is cooled to, and carries out heating and catches up with acid；Sample solution in counteracting tank is transferred to 50 mL plastics volumetric flasks In, rinse counteracting tank 3-4 times with 1% nitric acid, cleaning fluid is transferred in volumetric flask in the lump, with 1% nitric acid constant volume, is carried out after shaking up ICP-MS is tested, and then draws the Contents of Main Components of tobacco juice for electronic smoke contacting metal utensil.
3rd, instrumental conditions
Instrumental Analysis process：Full scan qualitative determination is first carried out, then according to sxemiquantitative test result, selects different extension rates Acid hydrolysis solution is diluted, and then accurate quantitative analysis is carried out to element of the content in 0.1 more than ppb；Instrument makes a concrete analysis of bar Part is set：Power：1550 w；Flow rate of carrier gas：1.0 L/min；Wriggling revolution speed：0.1 rpm；Analytical model：Crash mode （He）；Collision gas flow velocity：5 ml/min.Quantitative approach：Internal standard method, internal standard element are72Ge、115In and209Bi。
According to said determination method, liquid storage cylinder, filter tip of several electronic cigarettes etc. are selected, is measured shown in its main component following table （Unit：%）, it follows that electronic cigarette solution storage cavity material is mainly ormolu etc.：
。

Claims (4)

  1. A kind of 1. micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component Method, it is characterised in that：The ironware for contacting tobacco juice for electronic smoke is crushed, the sample powder 10 ~ 30 mg is taken, adds Enter in counteracting tank, add 3 mL70% nitric acid and 1 mL37% hydrochloric acid, screw closing, be placed on microwave dissolver, according to setting Micro-wave digestion program cleared up；After resolution, room temperature is cooled to, and carries out heating and catches up with acid；By the sample in counteracting tank Solution is transferred in 50 mL plastics volumetric flasks, and counteracting tank is rinsed 3-4 times with 1% nitric acid, and cleaning fluid is transferred in volumetric flask in the lump, With 1% nitric acid constant volume, ICP-MS tests are carried out after shaking up, and then show that the main component of tobacco juice for electronic smoke contacting metal utensil contains Amount；Instrumental Analysis process：Full scan qualitative determination is first carried out, then according to sxemiquantitative test result, selects different extension rates Acid hydrolysis solution is diluted, and then accurate quantitative analysis is carried out to element of the content in 0.1 more than ppb；Instrument makes a concrete analysis of bar Part is set：Power：1550 w；Flow rate of carrier gas：1.0 L/min；Wriggling revolution speed：0.1 rpm；Analytical model：Crash mode （He）；Collision gas flow velocity：5 ml/min；Quantitative approach：Internal standard method, internal standard element are72Ge、115In and209Bi。
  2. 2. according to the method for claim 1, it is characterised in that the ironware is electronic cigarette solution storage cavity or filter tip.
  3. 3. according to the method for claim 1, it is characterised in that the composition in quantitative analysis include but is not limited to Al, V, Cr、Mn、Fe、Co、Ni、Cu、Zn、Ag、Pb、Sb、Cd。
  4. 4. according to the method for claim 1, it is characterised in that micro-wave digestion program is specific as follows：Room temperature100 ℃（5 min）200（20 min）.
CN201710729590.5A 2017-08-23 2017-08-23 A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component Pending CN107462626A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710729590.5A CN107462626A (en) 2017-08-23 2017-08-23 A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710729590.5A CN107462626A (en) 2017-08-23 2017-08-23 A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component

Publications (1)

Publication Number Publication Date
CN107462626A true CN107462626A (en) 2017-12-12

Family

ID=60550197

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710729590.5A Pending CN107462626A (en) 2017-08-23 2017-08-23 A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component

Country Status (1)

Country Link
CN (1) CN107462626A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108680560A (en) * 2018-04-16 2018-10-19 湖南云天检测技术有限公司 The assay method of total silver content in a kind of silver-containing antibacterial material
CN114749042A (en) * 2022-04-12 2022-07-15 宁波江丰电子材料股份有限公司 Dissolving method of AgCuTi alloy

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103529117A (en) * 2013-05-02 2014-01-22 福建中烟工业有限责任公司 Measuring method for cobalt content in lining paper of cigarette
CN103954678A (en) * 2014-05-26 2014-07-30 国家烟草质量监督检验中心 Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes
CN104215627A (en) * 2014-05-09 2014-12-17 武汉红金龙印务股份有限公司 Method for microwave digestion-inductively coupled plasma mass spectrometer (ICP-MS) determination of metal ions such as lead, arsenic, cadmium and chromium in cigarette case
CN104316590A (en) * 2014-09-16 2015-01-28 河北中烟工业有限责任公司 Inductively coupled plasma mass spectrometry method for simultaneous determination of chromium, nickel, arsenic and lead in hot melt adhesive for cigarette

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103529117A (en) * 2013-05-02 2014-01-22 福建中烟工业有限责任公司 Measuring method for cobalt content in lining paper of cigarette
CN104215627A (en) * 2014-05-09 2014-12-17 武汉红金龙印务股份有限公司 Method for microwave digestion-inductively coupled plasma mass spectrometer (ICP-MS) determination of metal ions such as lead, arsenic, cadmium and chromium in cigarette case
CN103954678A (en) * 2014-05-26 2014-07-30 国家烟草质量监督检验中心 Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes
CN104316590A (en) * 2014-09-16 2015-01-28 河北中烟工业有限责任公司 Inductively coupled plasma mass spectrometry method for simultaneous determination of chromium, nickel, arsenic and lead in hot melt adhesive for cigarette

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108680560A (en) * 2018-04-16 2018-10-19 湖南云天检测技术有限公司 The assay method of total silver content in a kind of silver-containing antibacterial material
CN114749042A (en) * 2022-04-12 2022-07-15 宁波江丰电子材料股份有限公司 Dissolving method of AgCuTi alloy

Similar Documents

Publication Publication Date Title
Karthikeyan et al. Microwave assisted sample preparation for determining water-soluble fraction of trace elements in urban airborne particulate matter: evaluation of bioavailability
Ferreira et al. Nickel determination in saline matrices by ICP-AES after sorption on Amberlite XAD-2 loaded with PAN
Bezerra et al. On-line system for preconcentration and determination of metals in vegetables by inductively coupled plasma optical emission spectrometry
Zhang et al. Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap
CN103954678B (en) The detection method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of cigarette ash
CN103471879A (en) Smoke gas collecting device and method for quickly and accurately determining seven heavy metals in smoke gas
Melucci et al. Trace level voltammetric determination of heavy metals and total mercury in tea matrices (Camellia sinensis)
Butler et al. Atomic spectrometry update–a review of advances in environmental analysis
Swami et al. Trace metals analysis of legal and counterfeit cigarette tobacco samples using inductively coupled plasma mass spectrometry and cold vapor atomic absorption spectrometry
CN107462626A (en) A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component
Mendil Determination of Cd (II), Cu (II), and Pb (II) in some foods by FAAS after preconcentration on modified silica gels with thiourea
de Almeida et al. Use of fiberglass support in the application of dried-spot technique with dispersion liquid-liquid microextraction for the determination of Co, Cr, Cu, Ni and Pb by Energy Dispersive X-Ray Fluorescence Spectrometry
CN107957412A (en) A kind of heating board digestion of arsenic and mercury-atom fluorimetry method in soil
Lu et al. Study on tea harvested in different seasons based on laser-induced breakdown spectroscopy
Arslan et al. Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS)
Butler et al. Atomic spectrometry update. Environmental analysis
CN107271534A (en) The method that a kind of micro-wave digestion-inductively coupled plasma mass spectrometry determines electronic cigarette heater strip Contents of Main Components
Xiang et al. Determination of trace copper (II) in food samples by flame atomic absorption spectrometry after cloud point extraction
CN103630601A (en) Determination method for specific migration quantities of multiple elements in cigarette filter
Evans et al. Atomic spectrometry update. Advances in atomic spectrometry and related techniques
Mao et al. Simultaneous trapping of Zn and Cd by a tungsten coil and its application to grain analysis using electrothermal inductively coupled plasma mass spectrometry
CN103995044A (en) Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette butt
Garcia et al. An environmentally friendly analytical procedure for nickel determination by atomic and molecular spectrometry after cloud point extraction in different samples
Ghaedi et al. A solid phase extraction procedure for Fe3+, Cu2+ and Zn2+ ions on 2-phenyl-1H-benzo [d] imidazole loaded on Triton X-100-coated polyvinyl chloride
JP5319485B2 (en) Method and apparatus for measuring cadmium in food

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
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20171212