CN101644678B - Method for detecting content of titanium dioxide in emulsion or milk powder - Google Patents
Method for detecting content of titanium dioxide in emulsion or milk powder Download PDFInfo
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- CN101644678B CN101644678B CN2009101771265A CN200910177126A CN101644678B CN 101644678 B CN101644678 B CN 101644678B CN 2009101771265 A CN2009101771265 A CN 2009101771265A CN 200910177126 A CN200910177126 A CN 200910177126A CN 101644678 B CN101644678 B CN 101644678B
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Abstract
The invention relates to a method for detecting content of titanium dioxide in emulsion or milk powder, comprising the following steps: 1) making standard curve of titanium standard solution; 2) sampling; 3) treating a sample; 4) detecting the sample and 5) comparing sample detection results with the standard curve to obtain the content of the titanium dioxide in the sample. The detecting equipment of the invention is an inductively coupled plasma-emitting spectrometer. The detection limit of the spectrometer by using the method is 0.0012mu g/mL, the correlation coefficient r is more than 0.999, and the recovery rate is 93.2%-99%. The method can fast and accurately detect the content of titanium dioxide in emulsion or milk powder, has small probability of element loss and pollution in the preparation process of sample, accurate and reliable results, good repetitiveness and high sensitivity.
Description
Technical field
The present invention relates to a kind of method that detects content of titanium dioxide in emulsion or the milk powder, particularly a kind of method of utilizing the inductively coupled plasma emission spectrometer to measure content of titanium dioxide in emulsion or the milk powder belongs to the technical field that chemical analysis detects.
Background technology
Titanium dioxide formal name used at school titania (TiO
2), molecular weight: 79.88, it is a kind of white inorganic pigment, characteristics have nontoxic, best opacity, best whiteness and luminance brightness, be considered to the present best a kind of Chinese white of performance in the world, be widely used in industries such as coating, plastics, papermaking, printing-ink, chemical fibre, rubber, cosmetics and food.Titania is widely used in each side such as packing and material additive in the dairy products industry as colorant.
Titania itself is nontoxic, but some toxicological experiment shows that titania can be accumulated in facial and the musculature, and health is had certain harm.And also there is not conclusion so far about the research of soluble titanium compound.
GB/T21912-2008 " mensuration of titania in the food " can carry out wet method for us and detect, but because of the diversity of our testing product, wet resolution method can't be finished and detect test, thereby the exploitation that dry method detects necessitates.In order to solve the aforementioned problems in the prior, detection method of the present invention has been accomplished the double effects of energy-conserving and environment-protective, has broken the long problem of ashing time of conventional dry method, has realized interior purpose with the thorough ashing of sample of short time.The NO that has avoided simultaneously wet resolution method to produce again
2Pollution to environment.
Summary of the invention
The purpose of this invention is to provide a kind of method that detects content of titanium dioxide in emulsion or the milk powder, sample utilizes the characteristics of titanium elements through the dissolution of hydrochloric acid, through the atomizing of instrument spray chamber, by high temperature torch pipe, measures, and its step is simple, and the result accurately and reliably.
Purpose of the present invention can realize by the following method:
A kind of method that detects content of titanium dioxide in emulsion or the milk powder may further comprise the steps:
1) makes the typical curve of titanium standard solution:, make canonical plotting between emissive porwer and the concentration automatically by instrument with the standard solution that country mark thing center is bought, the titanium solution of dilution preparation series concentration;
2) sampling: take by weighing 4.0g-5.0g emulsion or milk powder sample;
3) sample preparation: the emulsion or the milk powder sample that take by weighing are put into the 100ml porcelain crucible, the sample that takes by weighing low-temperature heat carbonization on heating plate earlier changes it over to the high temperature furnace ashing again, takes out, add 1: 1 (V/V) nitric acid, be heated to driedly, put into muffle furnace ashing once more, take out cooling, add 5% salpeter solution (V/V) again, be transferred in the 50ml volumetric flask, be settled to 50ml, mixing; Prepare a blank reagent with identical method;
4) test sample: utilize the inductively coupled plasma emission spectrometer to carry out sample detection;
5) resulting testing result of step 4) and the resulting typical curve of step 1) are compared, obtain the content of titanium elements in the sample.
Among the present invention, described checkout equipment is inductively coupled plasma emission spectrometer (ICP-OES).
Get the titanium elements standard solution of a plurality of variable concentrations in the described step 1), preferred 5 standard models, its standard solution series concentration is as follows:
Element series concentration (unit: μ g/ml)
Titanium (ICP) 0.01 0.05 0.1 0.5 1.0
Preferably, the specimen preparation step 2) comprises heating carbonization treatment, high temperature ashing, acid treatment and high temperature ashing once more, sour solution transfer constant volume.Wherein acidolysis solution is 1: 1 (V/V) nitric acid, and acid is dissolved with 5% (V/V) salpeter solution.
Wherein 1: 1 salpeter solution have with sample in the inorganics effect of reacting.The effect of the difficult composition of being burnt of further destruction is arranged with its sample of handling ashing.
More preferably, emulsion or milk powder sample are prepared by following steps: take by weighing emulsion or milk powder sample, put into the 100ml porcelain crucible, the sample that takes by weighing low temperature (can not boil to get final product) heating on heating plate earlier with sample, anti-defervescence goes out, again it is changed over to 550 ℃ of ashing 30min of high temperature furnace, take out, add 1: 1 (V/V) nitric acid, under 70-80 ℃ temperature, be heated to driedly, put into 550 ℃ of muffle furnaces ashing 1h once more, take out cooling, be transferred in the 50ml volumetric flask with the salpeter solution that adds 5% (V/V) again, be settled to 50ml, mixing.
The spectrum condition of inductively coupled plasma emission spectrometer is as follows: airshed 15L/min; Auxiliary gas (air) flow: 0.22L/min; Atomizer flow 0.82L/min; Sampling volume: 1.4mL/min; Power: 1300W.
Above-mentioned sample makes its atomizing through the instrument spray chamber, by high temperature torch pipe, adopts the multiple-reaction monitoring mode to carry out quantitatively.
The instrument of this method detects and is limited to 0.0012 μ g/mL, and in the element range of linearity, correlation coefficient r is more than 0.999, and the recovery is 93.2%～99% (interpolation level be 0.05,0.5 and 1.0mg/kg).
Detection method of the present invention is simple and easy, quick, accurate and highly sensitive, and its advantage is:
1) method is easy, and particularly the sample preparation process is simple, and element loss and pollution rate are little, compares energy-conservation and environmental protection with existing method.
2) linear dependence is good.
3) detect depth of parallelism height, particularly the testing result to titania is stable, and parallel result is good.
4) high temperature cabonization and ashing for a long time reaches wet clearing up, thereby reaches the purpose of energy savings and environmental protection.Generally speaking, method of the present invention is the method for content of titanium dioxide in a kind of well-adapted fast detecting emulsion or the milk powder for big-and-middle-sized dairy products enterprise.
Description of drawings
Fig. 1 is an ICP canonical plotting according to an embodiment of the invention.
Embodiment
Below in conjunction with embodiment the present invention is done and to illustrate in greater detail.
The drafting of embodiment 1 typical curve
1, the preparation of standard solution
The standard solution of preparation titanium: accurately draw element mark stock solution (concentration: 1000 μ g/ml, single mark that State Standard Matter Research Centre buys), storing solution is made into the intermediate solution of 10 μ g/ml with 5% nitric acid, therefrom gets intermediate solution again and prepare serial solution.Accurately draw intermediate solution by the listed volume of table 1 again and in the 50ml volumetric flask, accurately be settled to scale.
The required stock solution amount of table 1 preparation standard serial solution (unit: ml)
2, reagent
The preparation of (1) 5% nitric acid
Accurately get 50ml red fuming nitric acid (RFNA) (top grade is pure), put into the beaker that fills the 100ml ultrapure water, forward to after the cooling in the 1000ml volumetric flask, accurately the constant volume mixing.
The preparation of (2) 1: 1 nitric acid
Accurately get 50ml red fuming nitric acid (RFNA) (top grade is pure), put into the beaker that fills the 50ml ultrapure water, cooling.
3, detect the OPtima5300DV inductively coupled plasma emission spectrometer (ICP-OES) that uses U.S. Perkin-Elmer company to produce with the inductively coupled plasma emission spectrometer.
1) inductively coupled plasma emission spectrometer (ICP-OES) spectrum condition is:
Plasma flow amount 15L/min; Auxiliary gas (air) flow: 0.22L/min; Atomizer flow 0.82L/min; Sampling volume: 1.4mL/min; Power: 1300W.
2) titanium elements is selected axial observation.
4, detection and result
1) 5 concentration gradient solution of preparation titanium elements, according to the gained data, the drawing standard curve map, related coefficient can reach more than 0.999.Specific series concentration sees Table 2:
Table 2 element series concentration (unit: μ g/ml)
Automatically make canonical plotting between emissive porwer and the concentration by instrument, as shown in Figure 1.
2) with 1: 1 nitric acid, after heating, carry out acidolysis, make the inorganics in the solution react the composition that further destruction is difficult for burning with it, again evaporate to dryness is heated in acid, this process is further destroyed sample composition, allows sample easier finishing this step of ashing under hot conditions.
3) because the linearity of ICP-OES is very wide, so this method is linear fine.In 0.01～300 μ g/L scope, correlation coefficient r=more than 0.999.
4) detection limit is according to 3 times of standard deviation calculation, and method of testing is: with the sample blank duplicate detection, according to the standard deviation that instrument calculates, 3 times of standard deviations are converted into concentration and are detection limit behind the drawing standard curve.The result is as shown in table 3:
The calculating of table 3 detection limit
Detecting in this method solution is limited to 0.0012 μ g/mL.
5, the recovery and precision experiment
(1) recovery experiment
Reclaim experiment to carry out the titanium elements mark-on with a kind of sample, each recovery test is respectively surveyed three times, draws average recovery rate.Test concrete data and see Table 4:
The recovery of table 4 sample and precision
Through the methodology checking, in the experimental concentration scope, more than the r=0.999, the recovery shows that this method meets trace element and detects requirement between 93.2%～99.0%.The RSD of precision experiment is respectively between 1.20%-5.91%.
Embodiment 2
Method: the OPtima5300DV inductively coupled plasma emission spectrometer (ICP-OES) that utilizes U.S. Perkin-Elmer company to produce is measured titania in emulsion or the milk powder.
The detection elements experimental procedure:
1. instrument is prepared:
(1) opens main frame and function software, instrument is transferred to optimum condition, open argon gas, water-cooled circulation, preheating four hours.
2. the preparation of sample: take by weighing 4.0g-5.0g emulsion or milk powder sample, put into the 100ml porcelain crucible, with sample low temperature (do not boil and the get final product) carbonization on heating plate earlier that takes by weighing, reenter 550 ℃ of high temperature furnaces, the 30min ash melts its composition, takes out and destroys other compositions with 1: 1 (V/V) nitric acid, is heated to dried under 70-80 ℃ temperature, put into 550 ℃ of muffle furnaces, ashing 1h once more takes out cooling, uses 5% salpeter solution (V/V) to be transferred in the 50ml volumetric flask again, be settled to 50ml, mixing.
Take by weighing 4.2509g, 4.9560g chocolate milk respectively, 4.3129g and 4.0307g milk powder sample, each sample is done two parallel sample, handles as stated above, measures with ICP.
In order to make the result more accurate, can prepare a blank reagent with identical method, utilize the inductively coupled plasma emission spectrometer to carry out sample detection equally, and from the sample detection result, deduct blank end value.
3. preparing standard solution: according to the described concentration preparing standard solution of table 5, titanium elements is mixed with one group of series standard solution, as shown in table 5:
Table 5 titanium elements series concentration (μ g/ml)
The standard solution mixing for preparing is gone in the polyethylene bottle, treat that the instrument preheating is according to the method drawing standard curve of implementing in 1.
Sample detection:
The ICP method: sample message such as input quality, constant volume before sample introduction, adopt the multiple-reaction monitoring mode to carry out quantitatively, instrument directly calculates the result.The results are shown in Table 6:
Table 6 testing result
Remarks: unit: mg/kg
Find that from last table this method detects breast and dairy products, and to detect parallel result better, it is better to detect parallel result when detection limit, the recovery all can satisfy requirement of experiment, shows that we are applicable to the detection of newborn and dairy products.
Test sample titanium elements content of the present invention is simplified to three hours with a series of processes of resolution method pre-treatment and finishes, and has solved wet resolution method when increasing work efficiency greatly and has taken a sample and clear up incomplete problem when too much.The present invention does not have other interference, has finished the easy purpose that also reaches energy conservation and environmental protection of method when optimizing link.
Claims (6)
1. method that detects content of titanium dioxide in emulsion or the milk powder may further comprise the steps:
1) make the typical curve of titanium standard solution: with the standard solution of buying, the titanium solution of dilution preparation series concentration is made canonical plotting between emissive porwer and the concentration automatically by instrument;
2) sampling: take by weighing 4.0g-5.0g emulsion or milk powder sample;
3) sample preparation: the emulsion or the milk powder sample that take by weighing are put into the 100ml porcelain crucible, the sample that takes by weighing low-temperature heat carbonization on heating plate earlier changes it over to the high temperature furnace ashing again, takes out, add 1: 1 (V/V) nitric acid, be heated to driedly, put into muffle furnace ashing once more, take out cooling, add 5% salpeter solution (V/V) again, be transferred in the 50ml volumetric flask, be settled to 50ml, mixing;
4) test sample: utilize the inductively coupled plasma emission spectrometer to carry out sample detection;
5) resulting testing result of step 4) and the resulting typical curve of step 1) are compared, obtain the content of titanium elements in the sample.
2. detection method as claimed in claim 1 is characterized in that getting in the described step 1) 5 standard models.
3. detection method as claimed in claim 2 is characterized in that: the series concentration of described standard solution is 0.01,0.05,0.1,0.5 and 1.0 μ g/ml.
4. detection method as claimed in claim 1, it is characterized in that: the described sample preparation condition of step 3) is the low-temperature heat carbonization with the sample degree of being that do not boil, again it is changed over to 550 ℃ of ashing 30min of high temperature furnace, take out to add 1: 1 (V/V) nitric acid, under 70 ℃-80 ℃ temperature, be heated to driedly, put into 550 ℃ of muffle furnaces ashing 1h once more, take out cooling, add 5% salpeter solution (V/V) again and be transferred in the 50ml volumetric flask, be settled to 50ml, mixing.
5. detection method as claimed in claim 1 is characterized in that: the spectrum condition of described inductively coupled plasma emission spectrometer is as follows: plasma flow amount 15L/min; Secondary air amount: 0.22L/min; Atomizer flow 0.82L/min; Sampling volume: 1.4mL/min; Power: 1300W.
6. as claim 1 or 5 described detection methods, it is characterized in that: adopt axial observation for described titanium elements.
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| CN102095708A (en) * | 2010-12-02 | 2011-06-15 | 北京师范大学 | Method for determining concentration of nano titanium dioxide in water by fulvic acid fluorescent quenching |
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| CN102866042B (en) * | 2011-07-05 | 2014-09-10 | 内蒙古蒙牛乳业（集团）股份有限公司 | Pretreatment method of Acesulfame-K and detection method for potassium in Acesulfame-K |
| CN102419277B (en) * | 2011-08-16 | 2015-01-28 | 中国检验检疫科学研究院 | Identification detection method of nano titanium dioxide in sun-screening cosmetic |
| CN103424306A (en) * | 2012-05-25 | 2013-12-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | Ashing method and detection method using the same |
| CN102866154B (en) * | 2012-10-13 | 2015-04-22 | 云南新立有色金属有限公司 | Method for measuring content of titanium dioxide in titanium concentrate |
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| CN105628484A (en) * | 2014-11-05 | 2016-06-01 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for pre-treating sample used for detection of mineral matter element in feed and detection method thereof |
| CN106033072A (en) * | 2015-03-20 | 2016-10-19 | 北京三元食品股份有限公司 | Method for detecting mineral elements in raw milk and dairy products in high throughput mode |
| CN106290180A (en) * | 2015-05-18 | 2017-01-04 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of Pb in food, chromium, cadmium and the detection method of copper content |
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| CN102095708A (en) * | 2010-12-02 | 2011-06-15 | 北京师范大学 | Method for determining concentration of nano titanium dioxide in water by fulvic acid fluorescent quenching |
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