CN106908438A - It is a kind of while detecting that each heavy metal species in tableware polytetrafluorethylecoatings coatings distinguish the micro-wave digestion ICP OES methods of content - Google Patents
It is a kind of while detecting that each heavy metal species in tableware polytetrafluorethylecoatings coatings distinguish the micro-wave digestion ICP OES methods of content Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of while each heavy metal species distinguish the micro-wave digestion ICP OES methods of content in detection tableware polytetrafluorethylecoatings coatings, the method can simultaneously detect various heavy metal leads, cadmium, chromium, arsenic, barium, mercury, selenium, the difference content of antimony in tableware polytetrafluorethylecoatings coatings, for eight heavy metal species distinguish the not exceeded offer test basis of total amount in ensuring tableware coating.The present invention can clear up the impurity in polytetrafluorethylecoatings coatings and principle that not poly tetrafluoro ethylene matrix reacts treatment sample using nitric acid+hydrogen peroxide, quantitative determined with ICP OES methods again, and then obtained eight kinds of difference contents or total amount of harmful heavy metal in tableware polytetrafluorethylecoatings coatings.
Description
Technical field
It is same the present invention relates to a kind of technical field of the assay method for detecting content of beary metal in tableware, more particularly to one kind
When detection tableware polytetrafluorethylecoatings coatings in each heavy metal species distinguish the micro-wave digestion-ICP-OES methods of content.
Background technology
There was only the detection method of the heavy metal transformation amount of tableware polytetrafluorethylecoatings coatings at present, there is no tableware polytetrafluoroethylene (PTFE)
Lead in coating（Pb）, cadmium（Cd）, chromium（Cr）, arsenic（As）, barium（Ba）, mercury（Hg）, selenium（Se）, antimony（Sb）Distinguish content Deng heavy metal
（Total amount）Detection method.
With the continuous innovation of Chemical Engineering Technology, the species of food contact material is also not necessarily limited to original bamboo and wood products, pottery again
The extensive use of the new materials such as ceramic products, macromolecular material has greatly enriched the species of food contact material.Coating is exactly wherein
Important one kind, coating is by intercepting the chance that food contact material base material is contacted with food, it is to avoid base material is straight with food
Contact, it also avoid physics, the chemical reaction between base material and food, therefore can greatly expand the suitable of food contact material
Use scope.But meanwhile, the coating being coated on base material also becomes a kind of food contact material in itself, thus coating security
Also it is directly connected to food security.
With the expansion of the food security range of definition, requirement of the various countries to food contact materials such as coating is improved constantly.
On international market, developed country all establishes strict food contact material rule and standard system, such as administration committee of European Union
（EC）, FDA (Food and Drug Adminstration)（FDA）And the relevant laws and regulations and standard that Japanese work Health and human services department is promulgated.This means that
The food contact material of China's export has to comply with the relevant laws and regulations standard requirement of these importer, just can ensure that the quality of product
Safety simultaneously smoothly enters overseas market.
Except the spy for having the elements such as arsenic, chromium to the minority coating such as teflon coating in the current coating sanitary standard of China
Fixed migration limitation is outer, typically with " heavy metal（In terms of lead）The index of the mg/L of "≤1 is limited.Its principle is some heavy metals
Sulfide precipitation can be generated makes solutions turbid or discoloration, can be compared judgements with certain density vulcanization lead solution, therefore title " with
Lead meter ".In fact the heavy metal for migrating out might not all be lead, may also there is other metals that can produce sulfide precipitation,
Such as iron, zinc, tin.This method cannot to the migration amount Accurate Determining of each metallic element, therefore be a kind of qualitative or sxemiquantitative
Method.
However, from the point of view of real case of the recent European Union to China's issue warning notice, many food contact products be by
It is required to recall in coating shedding, the coating coating that can directly contribute easy to fall off enters human body with food, then ensure coating weight
Total metal content is not exceeded just particularly significant.
The content of the invention
Shortcoming the invention aims to overcome above-mentioned prior art, there is provided a kind of to detect tableware polytetrafluoroethyl-ne simultaneously
Each heavy metal species distinguish the micro-wave digestion-ICP-OES methods of content in ene coatings, and this is detected in tableware polytetrafluorethylecoatings coatings simultaneously
Micro-wave digestion-ICP-OES the methods that each heavy metal species distinguish content can be while detect a various huge sum of moneys in tableware polytetrafluorethylecoatings coatings
Category lead, cadmium, chromium, arsenic, barium, mercury, selenium, the difference content of antimony, do not surpass to ensure in tableware coating that eight heavy metal species distinguish total amount
Mark provides test basis.In itself and do not exist heavy metal element due to polytetrafluoroethylene (PTFE) material, but it is in process of production not
, exactly generally there is heavy metal etc. in impurity in this section harmful in the impurity of evitable generation about 3-5% mass fractions
Material.Present invention utilization nitric acid+hydrogen peroxide can clear up the impurity in polytetrafluorethylecoatings coatings and not PTFE base
The principle treatment sample that body reacts, then quantitative determined with ICP-OES methods, and then obtain tableware polytetrafluorethylecoatings coatings
In eight kinds of difference contents or total amount of harmful heavy metal.
The present invention can eight kinds of toxic heavy metal elements difference total amounts in Simultaneous Quantitative Analysis tableware polytetrafluorethylecoatings coatings
Detection, and the existing detection technique that can only analyze tableware coating heavy metal transformation amount is entirely different, is its very necessary benefit
Fill, the method for heavy metal of the present invention detection can more reflect and cover with being combined to the method for detection heavy metal transformation amount in the prior art
The security of polytetrafluorethylecoatings coatings tableware.
The technical solution adopted for the present invention to solve the technical problems is：It is a kind of to detect tableware polytetrafluorethylecoatings coatings simultaneously
In each heavy metal species distinguish the micro-wave digestion-ICP-OES methods of content, comprise the following steps：
（1）Sample is obtained：Tableware polytetrafluorethylecoatings coatings surface is gently scraped using ceramic tip, it is impossible to scrape tableware matrix, obtained
No less than 0.5g samples；
（2）Sample treatment：Sample is placed in 105 DEG C of baking ovens and is dried to constant weight, accurately weigh sample 0.15g in micro-wave diminishing pot
In, while doing Duplicate Samples and blank test, 10mL nitric acid and 2mL hydrogen peroxide are added in each counteracting tank, the lid of counteracting tank is covered,
It is put into microwave dissolver and is processed to normal temperature, normal pressure, open counteracting tank, is filtered to 25mL capacity digestion solution with filter paper
Bottle is simultaneously settled to predetermined scale with deionized water, stand-by；
（3）The making of standard working curve：Series standard reference solution is prepared with the standard liquid of various elements；Lead, mercury, antimony,
Selenium, chromium, the standard reference solution of arsenic are fabricated to following various concentrations：0、1.0、2.0、5.0、10.0 mg/L；The standard ginseng of cadmium
Following various concentrations are fabricated to than solution：0、0.5、1.0、2.5、5.0 mg/L；The standard reference solution of barium be fabricated to as
Lower various concentrations：0th, 1.0,5.0,10.0,15.0 mg/L, while doing blank test；To the series standard reference solution for preparing
Determined using ICP-OES methods, obtain normal response value of the eight kinds of elements of the above under various concentrations, reduce blank, obtain each unit
The fit equation and coefficient correlation of the standard curve of element, it is specific as follows：
Pb:Y=453.6X+15.0, R2=0.9999
Ba:Y=19540X-585.5, R2=0.9999
Sb:Y=569.1X-8.4, R2=0.9999
Se:Y=402.1X-14.5, R2=0.9999
Cr:Y=23480X-489.7, R2=0.9999
Cd:Y=22420X-36.6, R2=0.9999
Hg:Y=965.8X-50.7, R2=0.9999
As:Y=8186X-67.9, R2=0.9999；
（4）The measure of sample：Determined using ICP-OES methods, obtain eight kinds of concentration of element more than in digestion solution, substituted into and calculate public
Formula：Xi=C*V/m, you can obtain eight kinds of difference contents of element in sample；Wherein the Xi of computing formula is represented：It is various in sample
The content of element, unit mg/kg；C is represented：The concentration of various elements in digestion solution, unit mg/L；V is represented：Digestion solution constant volume body
Product, Unit/mL；M is represented：Sample quality, unit g.
Further, the step（2）In the treatment conditions of microwave dissolver be：Under 1000W power, will clear up
Tank rises to 165 DEG C in 8min from room temperature, then 220 DEG C are risen in 10min and 25min is kept.
Further, the step（3）Or/and（4）In ICP-OES methods determine condition of work be：High frequency power
1150W, nebulizer gas pressure 25Psi, secondary air amount 1.0L/min, two-way plasma observation mode.
In sum, it is of the invention while detecting that each heavy metal species in tableware polytetrafluorethylecoatings coatings distinguish the microwave of content
Clearing up-ICP-OES methods can be while detects various heavy metal leads, cadmium, chromium, arsenic, barium, mercury, selenium, antimony in tableware polytetrafluorethylecoatings coatings
Difference content, to ensure the eight heavy metal species difference not exceeded offer test basis of total amount in tableware coating.Due to polytetrafluoro
Ethene material is in itself and in the absence of heavy metal element, but it inevitably produces about 3-5% mass fractions in process of production
Impurity, exactly generally there is the harmful material such as heavy metal in impurity in this section.The present invention utilizes nitric acid+dioxygen
Water energy enough clears up the impurity in polytetrafluorethylecoatings coatings and principle that not poly tetrafluoro ethylene matrix reacts treatment sample,
Quantitative determined with ICP-OES methods again, and then obtained in tableware polytetrafluorethylecoatings coatings containing respectively for eight kinds of harmful heavy metals
Amount or total amount.
Specific embodiment
Embodiment 1
It is a kind of while each heavy metal species distinguish the microwave of content in detection tableware polytetrafluorethylecoatings coatings described by the present embodiment 1
- ICP-OES methods are cleared up, is comprised the following steps：
（1）Sample is obtained：Tableware polytetrafluorethylecoatings coatings surface is gently scraped using ceramic tip, it is impossible to scrape tableware matrix, obtained
No less than 0.5g samples；
（2）Sample treatment：Sample is placed in 105 DEG C of baking ovens and is dried to constant weight, accurately weigh sample 0.15g in micro-wave diminishing pot
In, while doing Duplicate Samples and blank test, 10mL nitric acid and 2mL hydrogen peroxide are added in each counteracting tank, the lid of counteracting tank is covered,
It is put into microwave dissolver and is processed to normal temperature, normal pressure, open counteracting tank, is filtered to 25mL capacity digestion solution with filter paper
Bottle is simultaneously settled to predetermined scale with deionized water, stand-by；
（3）The making of standard working curve：Series standard reference solution is prepared with the standard liquid of various elements；Lead, mercury, antimony,
Selenium, chromium, the standard reference solution of arsenic are fabricated to following various concentrations：0、1.0、2.0、5.0、10.0 mg/L；The standard ginseng of cadmium
Following various concentrations are fabricated to than solution：0、0.5、1.0、2.5、5.0 mg/L；The standard reference solution of barium be fabricated to as
Lower various concentrations：0th, 1.0,5.0,10.0,15.0 mg/L, while doing blank test；To the series standard reference solution for preparing
Determined using ICP-OES methods, obtain normal response value of the eight kinds of elements of the above under various concentrations, reduce blank, obtain each unit
The fit equation and coefficient correlation of the standard curve of element, it is specific as follows：
Pb:Y=453.6X+15.0, R2=0.9999
Ba:Y=19540X-585.5, R2=0.9999
Sb:Y=569.1X-8.4, R2=0.9999
Se:Y=402.1X-14.5, R2=0.9999
Cr:Y=23480X-489.7, R2=0.9999
Cd:Y=22420X-36.6, R2=0.9999
Hg:Y=965.8X-50.7, R2=0.9999
As:Y=8186X-67.9, R2=0.9999；
（4）The measure of sample：Determined using ICP-OES methods, obtain eight kinds of concentration of element more than in digestion solution, substituted into and calculate public
Formula：Xi=C*V/m, you can obtain eight kinds of difference contents of element in sample；Wherein the Xi of computing formula is represented：It is various in sample
The content of element, unit mg/kg；C is represented：The concentration of various elements in digestion solution, unit mg/L；V is represented：Digestion solution constant volume body
Product, Unit/mL；M is represented：Sample quality, unit g.
The step（2）In the treatment conditions of microwave dissolver be：Under 1000W power, by counteracting tank in 8min from
Room temperature rises to 165 DEG C, then 220 DEG C are risen in 10min and 25min is kept.
The step（3）Or/and（4）In ICP-OES methods determine condition of work be：High frequency power 1150W, nebulizer gas pressure
25Psi, secondary air amount 1.0L/min, two-way plasma observation mode.
The above, is only presently preferred embodiments of the present invention, and any form is not made to technical scheme
On limitation.Every any simple modification made to above example according to technical spirit of the invention, equivalent variations and repair
Decorations, still fall within the range of technical scheme.
Claims (3)
1. a kind of while detect that each heavy metal species in tableware polytetrafluorethylecoatings coatings distinguish the micro-wave digestion-ICP-OES methods of content,
It is characterised in that it includes following steps：
（1）Sample is obtained：Tableware polytetrafluorethylecoatings coatings surface is gently scraped using ceramic tip, it is impossible to scrape tableware matrix, obtained
No less than 0.5g samples；
（2）Sample treatment：Sample is placed in 105 DEG C of baking ovens and is dried to constant weight, accurately weigh sample 0.15g in micro-wave diminishing pot
In, while doing Duplicate Samples and blank test, 10mL nitric acid and 2mL hydrogen peroxide are added in each counteracting tank, the lid of counteracting tank is covered,
It is put into microwave dissolver and is processed to normal temperature, normal pressure, open counteracting tank, is filtered to 25mL capacity digestion solution with filter paper
Bottle is simultaneously settled to predetermined scale with deionized water, stand-by；
（3）The making of standard working curve：Series standard reference solution is prepared with the standard liquid of various elements；Lead, mercury, antimony,
Selenium, chromium, the standard reference solution of arsenic are fabricated to following various concentrations：0、1.0、2.0、5.0、10.0 mg/L；The standard ginseng of cadmium
Following various concentrations are fabricated to than solution：0、0.5、1.0、2.5、5.0 mg/L；The standard reference solution of barium be fabricated to as
Lower various concentrations：0th, 1.0,5.0,10.0,15.0 mg/L, while doing blank test；To the series standard reference solution for preparing
Determined using ICP-OES methods, obtain normal response value of the eight kinds of elements of the above under various concentrations, reduce blank, obtain each unit
The fit equation and coefficient correlation of the standard curve of element, it is specific as follows：
Pb:Y=453.6X+15.0, R2=0.9999
Ba:Y=19540X-585.5, R2=0.9999
Sb:Y=569.1X-8.4, R2=0.9999
Se:Y=402.1X-14.5, R2=0.9999
Cr:Y=23480X-489.7, R2=0.9999
Cd:Y=22420X-36.6, R2=0.9999
Hg:Y=965.8X-50.7, R2=0.9999
As:Y=8186X-67.9, R2=0.9999；
（4）The measure of sample：Determined using ICP-OES methods, obtain eight kinds of concentration of element more than in digestion solution, substituted into and calculate public
Formula：Xi=C*V/m, you can obtain eight kinds of difference contents of element in sample；Wherein the Xi of computing formula is represented：It is various in sample
The content of element, unit mg/kg；C is represented：The concentration of various elements in digestion solution, unit mg/L；V is represented：Digestion solution constant volume body
Product, Unit/mL；M is represented：Sample quality, unit g.
2. according to claim 1 a kind of while detecting each heavy metal species difference content in tableware polytetrafluorethylecoatings coatings
Micro-wave digestion-ICP-OES methods, it is characterised in that the step（2）In the treatment conditions of microwave dissolver be：In 1000W
Under power, counteracting tank is risen to 165 DEG C in 8min from room temperature, then 220 DEG C are risen in 10min and 25min is kept.
3. each heavy metal species contain respectively in a kind of tableware polytetrafluorethylecoatings coatings of detection simultaneously according to claim 1 and 2
Micro-wave digestion-ICP-OES the methods of amount, it is characterised in that the step（3）Or/and（4）In ICP-OES methods determine work
Condition is：High frequency power 1150W, nebulizer gas pressure 25Psi, secondary air amount 1.0L/min, two-way plasma observation mode.
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