CN105954347A - Measuring method for nano titanium dioxide migration quantity in food plastic package product - Google Patents
Measuring method for nano titanium dioxide migration quantity in food plastic package product Download PDFInfo
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- CN105954347A CN105954347A CN201610393920.3A CN201610393920A CN105954347A CN 105954347 A CN105954347 A CN 105954347A CN 201610393920 A CN201610393920 A CN 201610393920A CN 105954347 A CN105954347 A CN 105954347A
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Abstract
The invention relates to a measuring method for nano titanium dioxide migration quantity in a food plastic package product. The measuring method is characterized in that a food plastic package sample is soaked for 10-12 d in acid food simulation liquid at the temperature of 45-50 DEG C; the soaking solution is taken and contains nano titanium dioxide in different particle sizes, ammonium sulfate and concentrated sulfuric acid are added into the soaking solution, heated and dissolved until the solution is clarified to obtain a digestive solution, the solid-to-liquid ratio of ammonium sulfate to the soaking solution is (1.5-2.0):100, and the volume ratio of concentrated sulfuric acid to the soaking solution is (4-6):100; finally, inductive coupling plasma mass-spectrography is used for measuring the concentration C of titanium in the digestive solution, and the titanium dioxide migration quantity is obtained through a formula I. Compared with the prior art, the measuring method is simple, fast, accurate and capable of detecting nano titanium dioxide which is in different particle sizes and is migrated from the food plastic package into food (particularly acid food), the detection limit of the measuring method is 0.15 micrograms/dm<2>, and the recovery rate is 85-95%.
Description
Technical field
The present invention relates to chemical composition detection field, particularly relate to nano titanium oxide in a kind of food plastic packing articles and move
The assay method of shifting amount.
Background technology
Inserts is a kind of plastic processing additives, has reduction cost, improves product properties, improves the effects such as outward appearance.Receive
Rice titanium dioxide is a kind of common filler, and it has the features such as shielding ultraviolet rays, Heat stability is good, hydrophilic, should
The effect such as aging resistance, sterilization can be played in plastic processing, be therefore widely used in food plastic packing articles.But,
When this kind of food plastic packing articles Long Term Contact food, along with time of contact and the change of storage environment, food plastic
Nano titanium oxide in packing articles can migrate in food, especially acid food, affects food quality and there is life
Thing security risk.
About the detection method of titanium dioxide it has been reported that such as GB/T21912-2008 " in food two in prior art
The mensuration of titanium oxide " provide the method for titanium dioxide, the detection side of conventional titanium dioxide in a kind of wet method detection food
Method has spectrophotography, titrimetry and atomic absorption method.But, above-mentioned detection method is the most inapplicable to nanometer two in food
Under the state that in the detection of titanium oxide, and food plastic packing articles, nano titanium oxide migrates to food, there is also
Migration amount is low, have the problems such as multiple different-grain diameter, therefore gives nano titanium oxide migration amount in food plastic packing product
Mensuration bring a difficult problem.
Summary of the invention
The technical problem to be solved is the food plastic bag providing a kind of Detection results good for prior art
The assay method of nano titanium oxide migration amount in dress goods.
The present invention solves the technical scheme that above-mentioned technical problem used: nano-silica in a kind of food plastic packing articles
Change the assay method of titanium migration amount, it is characterised in that food plastic is packed sample and is soaked in acid food simulated solution,
10～12d are soaked at 45～50 DEG C；Take soak, this soak adds ammonium sulfate and concentrated sulphuric acid, and heating for dissolving is extremely
Clarification, obtains digestion solution, and wherein ammonium sulfate is 1.5～2.0:100 with the solid-to-liquid ratio of soak, concentrated sulphuric acid and the volume of soak
Ratio is 4～6:100；Finally, utilize Inductively coupled plasma-mass spectrometry to measure the concentration C of titanium in digestion solution, and pass through
Formula I obtains the migration amount of titanium oxide；
Wherein, W is the migration amount of titanium oxide, and unit is μ g/dm2；C is the concentration of titanium, unit in digestion solution to be measured
For μ g/l；V is acid food simulated solution volume, and unit is ml；S is plastics package surface area of sample to be measured, and unit is
cm2；1.668 is the conversion coefficient of titanium oxide and titanium.
As preferably, in described soak, the particle diameter of nano titanium oxide to be detected is 10～100nm.
As preferably, described acid food simulated solution is 4% (volume fraction) acetic acid, typically contains 4% left in vinegar
Right acetic acid, therefore in the present invention using 4% (volume fraction) acetic acid as acid food simulated solution.Food classification is general
Being divided into aqueous food, pick-me-up, oils and fats and surface containing fatty foods, wherein aqueous food is according to the difference of pH again
Being divided into non-acid foods (pH >=5) and acid food (pH ＜ 5), machine inserts typically migrates maximum in acid food,
Therefore the present invention selects acid food to select 4% (volume fraction) acetic acid to be food simulants.
As preferably, the addition of described acid food simulated solution is that every square centimeter of food plastic packaging sample adds
1～1.5ml, acid food simulated solution can be made to contact with food plastic packaging sample fully, preferably simulated foods and food
The plastics packed contact of product.
Further, the addition of described acid food simulated solution is that every square centimeter of food plastic packaging sample adds 1ml.
As preferably, described ammonium sulfate is 1.6:100 with the solid-to-liquid ratio of soak, and concentrated sulphuric acid with the volume ratio of soak is
Nano titanium oxide in soak is cleared up by the Acid system that 4:100, beneficially ammonium sulfate and concentrated sulphuric acid form.
As preferably, the testing conditions of described Inductively coupled plasma-mass spectrometry is: RF power is 1500W, reflects merit
Rate ＜ 5W, fog chamber's temperature is-5 DEG C, and sampling depth is 8mm, and carrier gas flux Ar is 1L/min, and detection ion Ti is
45m/z, peristaltic pump promotes speed 0.3rps.
Compared with prior art, it is an advantage of the current invention that: the present invention is soaked in acidity by food plastic is packed sample
Food simulated solution so that the nano titanium oxide in food plastic packaging sample migrates to, in acid food simulated solution, make
Soak, then clears up the nano titanium oxide of different-grain diameter in soak by ammonium sulfate+concentrated sulphuric acid Acid system, connects
And measure the concentration of titanium in digestion solution by Inductively coupled plasma-mass spectrometry (ICP-MS), and then by formula I
Obtain titanium dioxide concentration, obtain the migration amount of nano titanium oxide.
Assay method in the present invention is easy, quick, accurately, can detect in food (especially acid liquid food) by
The nano titanium oxide of the different-grain diameter that food plastic packaging migrates, and the detection of this assay method is spacing
0.15μg/dm2, the response rate is 86～95%.
Accompanying drawing explanation
Fig. 1 is the tangent plane SEM figure of sample a in the embodiment of the present invention；
Fig. 2 is the tangent plane SEM figure of sample b in the embodiment of the present invention；
Fig. 3 is the tangent plane SEM figure of sample c in the embodiment of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1: the assay method of nano titanium oxide migration amount in food plastic packing articles
Specimen in use, reagent and instrument in 1.1 tests
Selected food plastic packaging sample is that nano titanium oxide PP sheet (is purchased from the Ningbo man connection limited public affairs of plastic
Department), the present embodiment is selected respectively three kinds of different nano titanium oxide PP sheets test, respectively sample a, sample
Product b and sample c；Acid food simulated solution selects 4% (volume fraction) acetic acid, and wherein to be that top grade is pure (purchase glacial acetic acid
In traditional Chinese medicines group)；Concentrated sulphuric acid is top grade pure (being purchased from traditional Chinese medicines group)；Ammonium sulfate is analytical pure (being purchased from traditional Chinese medicines group).
Key instrument used in test is as follows: scanning electron microscope QuantaTM250 (FEI, the U.S.)；Inductive etc. from
Sub-mass spectrograph Agilengt 7500A (Agilent, the U.S.)；Water-bath HH-60 (China of Changzhou state)；Analytical balance XL204
(prunus mume (sieb.) sieb.et zucc. Teller)；Electric hot plate HP10 (IKA).
Nano titanium oxide distributional pattern in 1.2 each sample
Nano titanium oxide PP sheet in scanning electron microscopic observation above-mentioned three is used (sample a, sample b and sample c) to receive
The distributional pattern of rice titanium dioxide, result is distinguished the most as shown in Figure 1, Figure 2 and shown in Fig. 3.By Fig. 1, Fig. 2 and Fig. 3
Understanding, in sample a, sample b and sample c, titanium dioxide nanoparticle often exists with aggregate form, and its particle diameter is big
Little differing, wherein the nano titanium oxide of sample a is based on 10nm, and the nano titanium oxide of sample a with 10nm is
Main, the nano titanium oxide of sample b is based on 30nm, and the nano titanium oxide of sample c is based on 70nm.
The foundation of 1.3 Acid systems
Weigh the nano titanium oxide of four kinds of different-grain diameters (100nm, 60nm, 25nm, 10nm) of 0.01g in platinum earthenware
In crucible, add 4mL concentrated sulphuric acid, be separately added into 0.5g, 1.0g, 1.2g, 1.6g, 2.0g ammonium sulfate, on electric hot plate
Slowly heated and boiled solution is to clarification, and test finds to add 1.6g and 2.0g ammonium sulfate, clears up the most thorough.Other
Under the conditions of clearing up, digestion solution mostly response speed slowly or leaves white precipitate in solution cannot clear up clarification.
Under same experiment condition, add 1.6g ammonium sulfate, sulphuric acid be respectively 2.0mL, 4.0mL, 5.0mL, 6.0mL,
8.0mL, it is incomplete that test shows to add 2.0mL Sulfuric-Acid Digestion, leaves white precipitate, disappearing under the conditions of other in solution
Solve liquid energy faster reaction to clarification.
To sum up can obtain, when clearing up the nano titanium oxide sample containing different-grain diameter in the present invention, the Acid system of selection is:
4mL sulphuric acid+1.6g ammonium sulfate.
1.4 assay method
Taking surface area is 160cm2Above-mentioned food plastic packaging sample, this sample is put into and is equipped with 4% (volume fraction)
In the container of acetic acid, and it is completely soaked in 4% (volume fraction) acetic acid solution, wherein 4% (volume fraction) acetic acid
Addition be that every square centimeter of sample adds 1mL food simulated solution (4% acetic acid).Then, by this immersed with the appearance of sample
Device is immersion treatment 10d in 50 DEG C of water-baths.Finally pipette soak 100mL, be evaporated, add 1.6g ammonium sulfate and
4mL concentrated sulphuric acid, on electric hot plate, heating for dissolving is to clarification.After cooling, transfer water is settled in 100mL volumetric flask,
Measure the concentration (C: μ g/L) of titanium in digestion solution with Inductively coupled plasma mass spectrometry, then calculate two by formula I
Titanium oxide concentration, obtains migration amount W (the μ g/dm of nano titanium oxide2).Above-mentioned Inductively coupled plasma mass spectrometry works
Condition is shown in Table 1.
In formula I:
The migration amount of W titanium oxide, unit is μ g/dm2；
The concentration of titanium in C digestion solution to be measured, unit is μ g/L；
V acid food simulated solution volume, unit is mL；
S sample to be tested surface area, unit is cm2；
1.668 titanium oxides and the conversion coefficient of titanium.
Table 1 Inductively coupled plasma mass spectrometry working condition
Embodiment 2: detection limit and the mensuration of the response rate
2.1 use above-mentioned condition determination, under identical experiment condition, the titanium concentration of 11 blank solutions of METHOD FOR CONTINUOUS DETERMINATION,
The detection limit that 3 times is titanium of its standard deviation, calculates the detection limit of titanium dioxide, the results are shown in Table 2 according to formula I.
The most above-mentioned blank solution is prepared by following steps: 4% (volume fraction) acetic acid solution 100mL, is evaporated, and adds
1.6g ammonium sulfate and 4mL concentrated sulphuric acid, on electric hot plate, heating for dissolving is to clarification.After cooling, transfer water is settled to 100mL
In volumetric flask, gained solution is blank reagent solution.
Table 2 detection limit
As shown in Table 2, the assay method of invention, the detection of its titanium dioxide is used to be limited to 0.15ug/dm2, and repeatability
Good, precision is 4.7%, meets detection demand.
2.2 the response rate
Sample soak to three kinds of different nanometer particle sizes, the mark-on carrying out variable concentrations reclaims, ICP-MS testing result
As shown in table 3.
Table 3 recovery testu
As shown in Table 3, for the sample of different-grain diameter nano titanium oxide, the response rate of the assay method in the present invention is equal
Between 86%～95%.Visible, the method is accurately and reliably, it is adaptable to the detection of different-grain diameter titanium dioxide migration amount.
Claims (7)
1. the assay method of nano titanium oxide migration amount in a food plastic packing articles, it is characterised in that food plastic is packed sample and is soaked in acid food simulated solution, soaks 10～12d at 45～50 DEG C；Take soak, this soak contains the nano titanium oxide of different-grain diameter size, ammonium sulfate and concentrated sulphuric acid is added in this soak, and heating for dissolving is to clarification, obtain digestion solution, wherein ammonium sulfate is 1.5～2.0:100 with the solid-to-liquid ratio of soak, and concentrated sulphuric acid is 4～6:100 with the volume ratio of soak；Finally, utilize Inductively coupled plasma-mass spectrometry to measure the concentration C of titanium in digestion solution, and obtain the migration amount of titanium oxide by formula I；
Wherein, W is the migration amount of titanium oxide, and unit is μ g/dm2；C is the concentration of titanium in digestion solution to be measured, and unit is μ g/l；V is acid food simulated solution volume, and unit is ml；S is plastics package surface area of sample to be measured, and unit is cm2；1.668 is the conversion coefficient of titanium oxide and titanium.
2. assay method as claimed in claim 1, it is characterised in that the particle diameter of the nano titanium oxide to be detected contained in described soak is 10～100nm.
3. assay method as claimed in claim 1, it is characterised in that described acid food simulated solution uses volume fraction to be the acetic acid of 4%.
4. assay method as claimed in claim 3, it is characterised in that the addition of described acid food simulated solution is that every square centimeter of food plastic packaging sample adds 1～1.5ml.
5. assay method as claimed in claim 4, it is characterised in that the addition of described acid food simulated solution is that every square centimeter of food plastic packaging sample adds 1ml.
6. assay method as claimed in claim 1, it is characterised in that described ammonium sulfate is 1.6:100 with the solid-to-liquid ratio of soak, and concentrated sulphuric acid is 4:100 with the volume ratio of soak.
7. the assay method as described in any claim in claim 1～6, it is characterized in that, the testing conditions of described Inductively coupled plasma-mass spectrometry is: RF power is 1500W, reflection power ＜ 5W, fog chamber's temperature is-5 DEG C, and sampling depth is 8mm, and carrier gas flux Ar is 1L/min, detection ion Ti is 45m/z, and peristaltic pump promotes speed 0.3rps.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106996892A (en) * | 2017-03-28 | 2017-08-01 | 四川出入境检验检疫局检验检疫技术中心 | Food contact sheet material specific transfer experiment sampling infuser device |
| CN117129302A (en) * | 2023-08-18 | 2023-11-28 | 承德天大钒业有限责任公司 | Method for dissolving titanium dioxide |
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| CN106996892A (en) * | 2017-03-28 | 2017-08-01 | 四川出入境检验检疫局检验检疫技术中心 | Food contact sheet material specific transfer experiment sampling infuser device |
| CN117129302A (en) * | 2023-08-18 | 2023-11-28 | 承德天大钒业有限责任公司 | Method for dissolving titanium dioxide |
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Application publication date: 20160921 |