CN105606436A - Method for quickly measuring content of five rare earth elements in edible packing material - Google Patents
Method for quickly measuring content of five rare earth elements in edible packing material Download PDFInfo
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Abstract
The invention discloses a method for quickly measuring content of five rare earth elements in an edible packing material. The method comprises the following steps: performing preliminary heating using power of 1200 W through a high-pressure closed microwave digestion method for an HNO3 system, heating to 80 DEG C within 4 min, and stewing for 3 min; performing secondary heating for 1 min to raise the temperature from 80 DEG C to 100 DEG C, and stewing for 2 min; performing third heating to raise the temperature from 100 DEG C to 120 DEG C within 1 min, and stewing for 2 min; performing fourth heating to raise the temperature from 120 DEG C to 180 DEG C within 2 min, and stewing for 15 min. The shortcomings of complicated program, more reagents, long digestion time, pollution to the environment and influence on the health of a human body are overcome; the technical defects of low sensitivity, high detection limit, high spectral interference and incapability of simultaneously measuring the content of various elements are overcome; therefore, the content of the five rare earth elements can be sensitively, efficiently, quickly, synchronously and accurately detected, and the method has great application value.
Description
Invention field
The present invention relates to the technical field of edible packing material composition measurement, specifically, thisInvent La, the Ce, Pr, Sm and five kinds of the Nd that relate in Fast Measurement edible packing material rareThe technical field of earth elements content.
Background technology
Along with the development of packing technique, edible food packaging material is as a kind of bag of greenPackage material, is widely applied. Edible food packaging material refers to and meets outside protection foodSee the functional requirements such as complete, health, safety, and to environment and the free of contamination packaging of food. CanThe feature of feeding habits packaging material be light weight, health, nonpoisonous and tasteless, can directly be adjacent to food Package,Guarantee the quality, fresh-keeping, edible.
Rare earth element belongs to non-human essential chemical element. Modern industry rare earth elements becomesFor the raw material of many new materials, be widely used in the fields such as industry, agricultural, medical science, consumeConstantly increase, thereby the content of various environmental sample and plant rare earth elements is subject to more next in recent yearsMore concerns. Plant can draw rare earth element from soil, and rare earth element can promote plantGrowth, particularly has obvious effect of increasing production to peanut, wheat, corn and paddy rice etc. Due toBioconcentration, feed certain plants property food can cause rare earth element concentration in human body to increaseAdd. Research shows, rare earth element is accumulated to a certain amount of in human body, can deposit the internal organ of human bodyIn certain toxic action, the food that edible content of rare earth exceeds standard for a long time, can be to the liver of human bodyWork the mischief with bone. China standard GB/T 2762-2005 " pollutants in food limitation "The content of middle regulation rare earth oxide must not be greater than 2mg/kg.
The analytical test of rare earth element has a lot of methods, and traditional elemental analysis method comprises light splittingPhotometry, atomic absorption method (flame and graphite furnace), atomic fluorescence spectrometry, ICP transmittingSpectroscopic methodology etc. These methods all respectively have its advantage, but also have its limitation, for example: before sampleProcess complexity, need extraction, enrichment method or suppress to disturb; Can not carry out multicomponent or multielementMeasure time and effort consuming simultaneously; Detectability or the sensitivity of instrument do not reach index request etc. ElectricitySense coupled plasma mass spectrum-ICP-MS (InductivelyCoupledPlasmaMassSpectrometry) technology is the most of shortcomings that almost overcome conventional method, and on this basisOn the more perfect elemental microanalysis method that grows up, thereby be called as the weight of contemporary analytical technologyGreat development. With respect to other analysis and testing technologies, inductivity coupled plasma mass spectrometry (ICP-MS)Have highly sensitively, the range of linearity is wide, multielement simultaneous determination, and spectral line is simple, and background is low etc.Feature is one of optimized analysis method of measuring at present biological sample rare earth elements. Along withICP-MS technology development, its application in food inspection field is more and more extensive, but pinMensuration to edible packing material rare earth elements there is not yet report, using plasma mass spectrumMethod and high-pressure sealed micro-wave digestion sample joint-detection means, realization is measured quickly and accurately canIn feeding habits packaging material, 5 of La, Ce, Pr, Sm and Nd kinds of ree contents have importantFunction and significance.
Summary of the invention
High for having no at present relevant detection sensitivity both at home and abroad, specificity is good, easy to operateThe mensuration of La, Ce, Pr, Sm and five kinds of ree contents of Nd in edible packing materialThe report of method, the present invention aim to provide La in a kind of Fast Measurement edible packing material,The method of Ce, Pr, Sm and five kinds of ree contents of Nd, by the technological means of pre-treatment,Overcome the defect that conventional Wet brings, set up in Fast Measurement edible packing materialThe method system of La, Ce, Pr, Sm and five kinds of ree contents of Nd, by adopting HNO3The high-pressure sealed micro-wave digestion pre-treatment of system replaces conventional wet method pre-treating method, adopts inductanceCoupled plasma mass spectrography is tested, and has not only simplified sample pre-treatments and test process,Shorten analysis time, saved testing cost, realized in edible packing materialLa, Ce, Pr, Sm and five kinds of ree contents of Nd sensitive, efficient, quick, synchronousAccurately detect, there is applied value widely.
Patent of the present invention adopts main technical scheme:
By utilizing inductively coupled plasma mass spectrometry principle in edible packing materialThe detection of La, Ce, Pr, Sm and five kinds of ree contents of Nd provides foundation, by adoptingHNO3The method of the high-pressure sealed micro-wave digestion of system substitutes the common Wet in this area, adoptsDirectly measure La, Ce, Pr, Sm and Nd five wherein with icp msPlant ree content, change conventional Wet, not only simplified sample pre-treatments and surveyExamination process, has shortened analysis time, has saved testing cost. By the technological means of pre-treatment—HNO3The high-pressure sealed micro-wave digestion of system, overcomes that program is loaded down with trivial details, reagent dosage is many, clears upTime length, contaminated environment, and affect the drawbacks such as health, also overcome and adopt other to detect skillsSensitivity that art means are brought is low, detect limit for height, can not accurate analysis alkali earth metal content,Testing background is high, spectrum disturbs strong, can not simultaneously to measure multiple element content etc. technological deficiency,La, Ce, Pr, Sm and five kinds of rare earths of Nd in Fast Measurement edible packing material are set upThe method system of constituent content, reaches quick, convenient, detects effect accurately, and it is right to have realizedLa, Ce, Pr, Sm and five kinds of ree contents of Nd in edible packing material sensitive,Synchronous accurately detection efficiently, fast.
The present invention specifically provide La, Ce in a kind of Fast Measurement edible packing material, Pr,The method of Sm and five kinds of ree contents of Nd, concrete grammar step is as follows:
(1) accurately taking the uniform gelatine capsule shell 0.5000g of preparation is placed in acid and boils cleanIn polytetrafluoroethylene (PTFE) counteracting tank, add 8mL nitric acid, carry out micro-wave digestion program heating and decompose.
Described micro-wave digestion program is: adopt power 1200W, heat up for the first time, 4minInside be warming up to 80 DEG C, and be resident 3min under the condition of 80 DEG C in temperature; Rise for the second timeTemperature, is warming up to 100 DEG C by 80 DEG C in 1min, and is resident under the condition of 100 DEG C in temperature2min; Heat up for the third time, in 1min, be warming up to 120 DEG C by 100 DEG C, and in temperature beResident 2min under the condition of 120 DEG C; Carry out the 4th time and heat up, in 2min, be warming up to by 120 DEG C180 DEG C, and be resident 15min under the condition of 180 DEG C in temperature.
(2) after clearing up, be cooled to room temperature, Specimen eliminating liquid is transferred to 50.00mL toolIn plug plastic bottle, use ultra-pure water constant volume.
(3) running parameter of setting ICP-MS instrument, selects ICP-MS instrument directly to measureLa, Ce, Pr, Sm and five kinds of ree contents of Nd, can realize edible packing materialIn the fast detecting of La, Ce, Pr, Sm and five kinds of ree contents of Nd.
The running parameter of described ICP-MS instrument is: atomization gas flow is 0.84L/min,Assisted gas flow is 0.85L/min, and cooling gas flow is 13.5L/min, and lens voltage is-78.0V, scan pattern is PeakJump, and sampling depth is 146, and radio-frequency power is 1400W,The time of staying is 10ms, and acquisition time is 44ms, and reactive/collision throughput is 4.9L/min,CeO/Ce is 0.72%.
In the present invention, by adopting HNO3The method of the high-pressure sealed micro-wave digestion of system substitutes thisThe Wet of the common routine in field, adopts icp ms directly to measure itIn La, Ce, Pr, Sm and five kinds of ree contents of Nd, change conventional Wet,Not only simplify sample pre-treatments and test process, shortened analysis time, saved and tested intoThis. By the technological means-HNO of pre-treatment3The high-pressure sealed micro-wave digestion of system, overcomes journeyOrder is loaded down with trivial details, and reagent dosage is many, and digestion time is long, and contaminated environment affects the drawbacks such as health,Also overcome adopt the sensitivity that brings of other detection technique means low, detect limit for height, can not be accurateAnalyze that alkali earth metal content, testing background are high, spectrum disturb strong, can not measure simultaneously manyThe technological deficiency of kind of constituent content etc., set up La in Fast Measurement edible packing material,The method system of Ce, Pr, Sm and five kinds of ree contents of Nd, reach fast, convenient,Detect accurately effect, realized the La in edible packing material, Ce, Pr, Sm andThe fast detecting of five kinds of ree contents of Nd.
In the present invention, the inductivity coupled plasma mass spectrometry of employing (ICP-MS) has sensitivityHeight, the range of linearity is wide, multielement simultaneous determination, the feature such as spectral line is simple, and background is low, is orderOne of optimized analysis method of front mensuration biological sample rare earth elements, along with ICP-MS technologyDevelopment, its application in food inspection field is more and more extensive. Its general principle:In ICP-MS, ICP is as mass spectrographic high temperature ion source (7000K), and sample enters in passageThe processes such as row evaporates, dissociates, atomization, ionization. Ion passes by sample cone interface and ionCommunication system is into the MS part of high vacuum, and MS part is four extremely fast to scan mass spectrograph, passes throughThe all ions of high-speed sequential scanning separation determination, scan element mass number scope from 6 to 260,And ion after separating by High-Speed Double-Channel detects, concentration linear dynamic range reaches 9The direct mensuration of number level. Therefore, compared with traditional inorganic analysis technology, ICP-MS technologyMinimum detection limit, the widest dynamic linear scope are provided, have disturbed minimum, analytical precisionHigh, analysis speed fast, can carry out multielement simultaneous determination and accurate isotope letter can be providedThe analytical characteristicses such as breath.
The micro-wave digestion program resolves that adopts wet method and the inventive method to provide is entered same sampleRow pretreatment, and measure wherein La, Ce, Pr, Nd, five kinds of rare earth units of Sm with ICP-MSElement. The micro-wave digestion program resolves processing sample providing by the inventive method is provided, there is sampleClear up fast, reagent consumption less, the advantage such as blank value is low, in operating efficiency, the standard of measurement resultThe aspects such as true property are all better than Wet, and processing sample has obtained satisfied result.
The present invention by ICP power, carrier gas flux, sampling depth, ion lens current potential andMeasurement parameters etc. have carried out optimization selection. Under optimization alternative condition, 5 kinds of rare earth elementsThe intensity maximum of single charge ion, and the productive rate of oxide, hydroxide ion is minimum, rare earthElement sensitivity is high, has eliminated matrix effect and other interference, makes measurement result accurately and reliably.Matrix when sample determination not exclusively dissociate or plasma tail flame in the element combination again of dissociatingCan form refractory oxides ion or hydroxide ion, meeting interference measurement, and rare earth elementThe interference of oxide and hydroxide is comparatively serious. By tuning instrument parameter, make CeO/CeRatio be 0.72%, can eliminate oxide interference. In addition, utilize and add online interior markMode eliminate matrix effect and interface effect, selected internal standard element is not subject to isobar overlappingOr the interference of multi-atomic ion, or the isotope of tested element is produced and disturbed, should be institute's test sampleIn product, content is considerably less and even do not have, and selected interior mark and element mass number to be measured should approach. WithThe signal drift that In rectifies an instrument as internal standard element and because non-mass spectrum matrix effect is drawnInhibition or the enhancement effect of the measured object rising. 5 kinds of sensitivity and degrees of accuracy that rare earth element is measuredBest.
By implementing the concrete summary of the invention of the present invention, can reach following beneficial effect:
The present invention is based on using plasma mass spectrography combines with high-pressure sealed micro-wave digestion sampleDetection means, is used HNO3The high-pressure sealed microwave sample of system, than routineDissolution method, has shortened the sample treatment time greatly, and the whole link of clearing up is in air-tight state,Free from environmental pollution, protection health safety; In addition, micro-wave digestion agents useful for same is less,Economize on resources, protection of the environment; Using plasma mass spectrography is tested, can be simultaneously sensitive,The content of 5 kinds of rare earth elements in synchronous Accurate Determining edible packing material efficiently, fast.
(1) rate of recovery is high: in the Fast Measurement edible packing material that the inventive method providesThe method of La, Ce, Pr, Sm, five kinds of ree contents of Nd, by adopting HNO3SystemHigh-pressure sealed Microwave Digestion is effectively dissolved La, Ce, Pr, Sm and five kinds of rare earth elements of Nd,Each element recovery rate is all between 85.50%-102.80%.
(2) detection time is short: adopt conventional method detection time at least need to 6 hours withUpper, adopt La, Ce in Fast Measurement edible packing material provided by the invention, Pr,The method of Sm, five kinds of ree contents of Nd comprises that sample pre-treatments arrives acquisition testing result 1Within hour, compared with greatly shortening the detection time of other method.
(3) detection sensitivity is high: in Fast Measurement edible packing material provided by the inventionThe method of La, Ce, Pr, Sm, five kinds of ree contents of Nd can detect 10-6Rank.
(4) degree of accuracy is good: obtain each element recovery rate and all exist by carrying out recovery testuBetween 85.50%-102.80%, the method degree of accuracy provided by the invention is better.
(5) precision is good: by the parallel laboratory test of many groups, obtain each element relative standard deviation littleIn 5%, La, Ce in the Fast Measurement edible packing material providing provided by the invention,The method precision of Pr, Sm, five kinds of ree contents of Nd is better.
(6) pollute less: in the Fast Measurement edible packing material providing provided by the inventionThe method agents useful for same consumption of La, Ce, Pr, Sm, five kinds of ree contents of Nd is few and notFor poisonous and harmful reagent, few to environment and man body pollution.
(7) flow process is simple: strong operability, be easy to grasp, and as long as possess chemical basic knowledge,Just can finely complete without good special training.
(8) cost is low: La in Fast Measurement edible packing material provided by the invention,The reagent that the method for Ce, Pr, Sm, five kinds of ree contents of Nd is used is the conventional examination of chemistryAgent, low price, is easy to buying, and consumption is few.
(9) La, the Ce in employing Fast Measurement edible packing material provided by the invention,The method of Pr, Sm and five kinds of ree contents of Nd, known according to measurement result, La, Ce,The detection limit of Pr, Sm and five kinds of rare earth elements of Nd is respectively 0.087,0.15,0.40,0.30,0.083 μ g/kg, each element relative standard deviation is less than 5%, 6 determination of recovery rates value and existsBetween 85.50%-102.80%, use the inventive method, measurement result is parallel, and the rate of recovery is high,Precision, the degree of accuracy are good, use that ICP-MS analysis speed is fast, detection limit is low, favorable reproducibility,Sample consumption is few. The method is easy, fast, stable, reliable, is applicable to edible packaging materialThe Fast Measurement of La, Ce, Pr, Sm and five kinds of ree contents of Nd in material.
Brief description of the drawings
Fig. 1 is shown as the canonical plotting of La.
Fig. 2 is shown as the canonical plotting of Ce.
Fig. 3 is shown as the canonical plotting of Pr.
Fig. 4 is shown as the canonical plotting of Sm.
The Nd canonical plotting that Fig. 5 is shown as.
In Fig. 1-5, abscissa is concentration, and ordinate is absorbance.
Detailed description of the invention
, for embodiment, the present invention is described below, still, the present invention is not limited to following enforcement.
The key instrument of selecting in the present invention: icp ms (U.S.'s thermoelectricityCompany), microwave dissolver CEMmars (U.S. CE M company), far infrared acid and alkali-resistance digital displayThermostatic electrothermal plate: MEA – 3 types, (Beijing Jin Bei moral Trade Co., Ltd.), ultra-pure water system:Milli-Q type (Millipore company of the U.S.), (plum Teller-Tuo benefit instrument has electronic balanceLimit company), high speed Universalpulverizer DFY600.
The main agents of selecting in the present invention: nitric acid (top grade is pure), ultra-pure water.
All reagent, instrument, the raw and auxiliary material in the present invention, selected are all well known selecting, but not limiting enforcement of the present invention, other reagent more well known in the art and equipment all canBe applicable to the enforcement of the following embodiment of the present invention. The % that the present invention adopts is according to raw material gross weightPercentage is assessed.
Embodiment mono-: La, Ce, Pr, Sm and five kinds of rare earths of Nd in edible packing materialThe mensuration of constituent content
La, Ce, Pr, Sm and five kinds of rare earth elements of Nd of measuring in edible packing material containThe method of amount, the method concrete steps of employing are as follows:
(1) accurately taking the uniform gelatine capsule shell 0.5000g of preparation is placed in acid and boils cleanIn polytetrafluoroethylene (PTFE) counteracting tank, add 8mL nitric acid, carry out micro-wave digestion program heating and decompose.
Described micro-wave digestion program is: power 1200W, heats up, in 4min for the first timeBe warming up to 80 DEG C, and be resident 3min under the condition of 80 DEG C in temperature; Heat up for the second time,Be warming up to 100 DEG C by 80 DEG C in 1min, and be resident 2min under the condition of 100 DEG C in temperature;Heat up for the third time, in 1min, be warming up to 120 DEG C by 100 DEG C, and be 120 DEG C in temperatureCondition under resident 2min; Carry out the 4th time and heat up, in 2min, be warming up to 180 by 120 DEG CDEG C, and be resident 15min under the condition of 180 DEG C in temperature.
(2) after clearing up, be cooled to room temperature, Specimen eliminating liquid is transferred to 50.00mL toolIn plug plastic bottle, use ultra-pure water constant volume.
(3) running parameter of setting ICP-MS instrument, selects ICP-MS instrument directly to measureLa, Ce, Pr, Sm and five kinds of ree contents of Nd, can realize edible packing materialIn the fast detecting of La, Ce, Pr, Sm and five kinds of ree contents of Nd.
The running parameter of described ICP-MS instrument is: atomization gas flow is 0.84L/min,Assisted gas flow is 0.85L/min, and cooling gas flow is 13.5L/min, and lens voltage is-78.0V, scan pattern is PeakJump, and sampling depth is 146, and radio-frequency power is 1400W,The time of staying is 10ms, and acquisition time is 44ms, and reactive/collision throughput is 4.9L/min,CeO/Ce is 0.72%.
In the present invention, by adopting HNO3The method of the high-pressure sealed micro-wave digestion of system substitutes normalThe Wet of rule, adopt icp ms directly measure La wherein,Ce, Pr, Sm and five kinds of ree contents of Nd, change conventional Wet, not only letterChange sample pre-treatments and test process, shortened analysis time, saved testing cost. LogicalCross the technological means-HNO of pre-treatment3The high-pressure sealed micro-wave digestion of system, overcomes program loaded down with trivial details,Reagent dosage is many, and digestion time is long, and contaminated environment affects the drawbacks such as health, also overcomesThe sensitivity that adopts other detection technique means to bring is low, detect limit for height, can not accurate analysis alkaliEarth metal constituent content, testing background are high, spectrum disturb strong, can not measure multiple element simultaneouslyThe technological deficiency of content etc., set up La, Ce in Fast Measurement edible packing material,The method system of Pr, Sm and five kinds of ree contents of Nd, reaches quick, convenient, accurateDetection effect, realized the La in edible packing material, Ce, Pr, Sm and Nd fivePlant the fast detecting of ree content.
In the present invention, the inductivity coupled plasma mass spectrometry of employing (ICP-MS) has sensitivityHeight, the range of linearity is wide, multielement simultaneous determination, the feature such as spectral line is simple, and background is low, is orderOne of optimized analysis method of front mensuration biological sample rare earth elements, along with ICP-MS technologyDevelopment, its application in food inspection field is more and more extensive. Its general principle:In ICP-MS, ICP is as mass spectrographic high temperature ion source (7000K), and sample enters in passageThe processes such as row evaporates, dissociates, atomization, ionization. Ion passes by sample cone interface and ionCommunication system is into the MS part of high vacuum, and MS part is four extremely fast to scan mass spectrograph, passes throughThe all ions of high-speed sequential scanning separation determination, scan element mass number scope from 6 to 260,And ion after separating by High-Speed Double-Channel detects, concentration linear dynamic range reaches 9Number level is directly measured from 1ppq to 1000ppm. Therefore, with traditional inorganic analysis technology phaseRatio, ICP-MS technology provides minimum detection limit, the widest dynamic linear scope, interferenceMinimum, analytical precision is high, analysis speed is fast, can carry out multielement simultaneous determination and can carryFor analytical characteristicses such as accurate Isotope Informations.
Embodiment bis-: the preparation of standard liquid
1, experimentation
(1) standard operation solution is by La, Ce, Pr, Nd, Sm element GB mother liquor (countryStandard substance research center) 1000mg/L stepwise dilution obtains, per sample in La, Ce, Pr,Nd, Sm content, prepare the standard operation solution of variable concentrations, preparation La, Ce, Pr, Nd,Sm hybrid standard uses liquid concentration: 1.00,10.00,20.00,50.00 μ g/L.
Measure and draw out calibration curve with ICP-MS, the coefficient correlation of measurement result needsMore than 0.999.
(2) drafting of La, Ce, Pr, Nd, Sm element standard working curve
In the concentration (taking μ g/L) of each element standard liquid as abscissa, to inhale accordinglyLuminosity is ordinate, curve plotting.
2, experimental result
The canonical plotting of La, Ce, Pr, Nd, Sm element is referring to accompanying drawing 1, accompanying drawing 2, attachedFig. 3, accompanying drawing 4, accompanying drawing 5, and calibration curve linear relationship and the coefficient correlation of each elementAs shown in table 1.
Table 1: calibration curve linear relationship and the coefficient correlation of each element
| Rare earth element | The range of linearity (μ g/L) | Linear equation | Coefficient correlation |
| La | 0.00～100.00 | Y＝8136.7X-728.26 | 0.999995 |
| Ce | 0.00～100.00 | Y＝11363X-3458.9 | 0.99995 |
| Pr | 0.00～100.00 | Y＝15869X-5977 | 0.99995 |
| Nd | 0.00～100.00 | Y＝3329.5X-793.38 | 0.99998 |
| Sm | 0.00～100.00 | Y＝3166.6X-645.26 | 0.99999 |
Embodiment tri-: the elimination of interference
Matrix when sample determination not exclusively dissociate or plasma tail flame in the element that dissociates againIn conjunction with forming refractory oxides ion or hydroxide ion, meeting interference measurement, and rare earth unitThe oxide of element and the interference of hydroxide are comparatively serious. By tuning instrument parameter, makeThe ratio of CeO/Ce is 0.72%, can substantially eliminate oxide interference. In addition, utilizeLine adds interior target mode to eliminate matrix effect and interface effect, and selected internal standard element is not subject to amountThe interference of the overlapping or multi-atomic ion of heterotope, or the isotope of tested element is produced and disturbed,Should be that in institute's test sample product, content is considerably less and even do not have, and selected interior mark and element mass number to be measuredShould approach. The signal drift rectifying an instrument as internal standard element with In and due to non-mass spectrumThe inhibition of the measured object that matrix effect causes or enhancement effect. It is sensitive that 5 kinds of rare earth elements are measuredDegree and the degree of accuracy are best.
Embodiment tetra-: sample size measurement result
1, experimentation
Utilize method described in embodiment mono-measure La, Ce in gelatine capsule shell, Pr, Nd,The content of these five kinds of rare earth elements of Sm, every kind of rare earth element is measured 6 times, namely carries out 6Inferior parallel laboratory test, and average and relative standard deviation.
2, experimental result
La, Ce in gelatine capsule shell, Pr, Nd, these 5 kinds of ree contents of Sm 6 timesMeasurement result, mean value and relative standard deviation are in table 2.
Table 2: the measurement result of 5 kinds of rare earth elements in gelatine capsule shell (n=6, μ g/kg)
Conclusion: the experimental result that can use the inventive method to obtain by table 2 measurement result is parallelProperty is better, and the relative standard deviation of each element is all less than 5%, and precision is good.
Embodiment five: the mensuration of detection limit
1, experimentation
Utilize the method described in embodiment mono-to reagent blank METHOD FOR CONTINUOUS DETERMINATION 11 times, with standard3 times of computational methods detection limits of deviation.
2, experimental result
Experimental result is in table 5, and the detection limit of five kinds of rare earth elements of the application existsWithin the scope of 0.083-0.40 μ g/kg. The detection limit of 5 kinds of rare earth elements is low, and instrumental sensitivity is high,Can detect La, Ce, Pr, Nd, the Sm of low content.
The method detection limit of table 3:La, Ce, Pr, Nd, Sm5 kind rare earth element
| Rare earth element | Detection limit (μ μ g/kg) |
| La | 0.087 |
| Ce | 0.15 |
| Pr | 0.40 |
| Nd | 0.083 |
| Sm | 0.30 |
Embodiment six: the mensuration of recovery of standard addition
1, experimentation
Same experimental conditions add respectively 100 μ g/kg, 200 μ g/kg, 400 μ g/kg this 3Plant five kinds of rare earth element mixed standard solutions of variable concentrations in gelatine capsule shell, and utilize realThe method described in example one executed is measured these 5 kinds of La, Ce in gelatine capsule shell, Pr, Nd, SmThe content of rare earth element, continuously replication 6 times.
2, experimental result
Experimental result is in table 4, and result shows that each sample mark-on recovery all existsBetween 85.50%-102.80%, comply with the national standard requirements, the application's Fast Measurement edibility bagThe method degree of accuracy of La, Ce in package material, Pr, Sm, five kinds of ree contents of Nd is high.
Table 4: 5 kinds of rare earth element recovery testu results in gelatine capsule shell
Embodiment seven: check experiment
The micro-wave digestion program resolves that adopts wet method and the inventive method to provide is entered same sampleRow pretreatment, and measure wherein La, Ce, Pr, Nd, Sm5 kind rare earth unit with ICP-MSElement, the results are shown in Table 5.
Table 5: the comparison result of two kinds of pre-treating methods
Note: adding scalar is 100 μ g/kg
Table 5 shows, disappears with the degree of accuracy microwave more provided by the invention of Wet Determination resultThe method of separating is slightly poor, and the large usage quantity of reagent, and digestion time is longer, and uses the inventive methodThe micro-wave digestion program resolves processing sample providing, have that Specimen eliminating is fast, reagent consumption less,The advantages such as blank value is low, in operating efficiency, the aspects such as the accuracy of measurement result are all better than wet methodClear up, processing sample has obtained satisfied result.
As mentioned above, can realize preferably the present invention, the above embodiments are only to thisBright preferred embodiment is described, and not scope of the present invention is limited, not de-Design from the present invention under the prerequisite of spirit, those of ordinary skill in the art are to technical side of the present inventionVarious distortion and improvement that case is made, all should fall in the definite protection domain of the present invention.
Claims (2)
1. a method for La, the Ce in Fast Measurement edible packing material, Pr, Sm, five kinds of ree contents of Nd, is characterized in that, concrete assay method is:
(1) accurately take the uniform gelatine capsule shell 0.5000g of preparation and be placed in acid and boil clean polytetrafluoroethylene (PTFE) counteracting tank, add 8mL nitric acid, carry out micro-wave digestion program heating and decompose;
Described micro-wave digestion program is: adopt power 1200W, heat up for the first time, be warming up to 80 DEG C in 4min, and be resident 3min under the condition of 80 DEG C in temperature; Heat up for the second time, be warming up to 100 DEG C by 80 DEG C in 1min, and be resident 2min under the condition of 100 DEG C in temperature; Heat up for the third time, be warming up to 120 DEG C by 100 DEG C in 1min, and be resident 2min under the condition of 120 DEG C in temperature; Carry out the 4th time and heat up, be warming up to 180 DEG C by 120 DEG C in 2min, and be resident 15min under the condition of 180 DEG C in temperature;
(2) after clearing up, be cooled to room temperature, Specimen eliminating liquid is transferred in 50.00mL tool plug plastic bottle, use ultra-pure water constant volume;
(3) running parameter of setting ICP-MS instrument, selects ICP-MS instrument directly to measure La, Ce, Pr, Sm and five kinds of ree contents of Nd, can realize the fast detecting of La, Ce, Pr, Sm and five kinds of ree contents of Nd in edible packing material.
2. the method for La, the Ce in Fast Measurement edible packing material as claimed in claim 1, Pr, Sm, five kinds of ree contents of Nd, it is characterized in that, the running parameter of described ICP-MS instrument is: atomization gas flow is 0.84L/min, assisted gas flow is 0.85L/min, cooling gas flow is 13.5L/min, lens voltage is-78.0V, scan pattern is PeakJump, sampling depth is 146, radio-frequency power is 1400W, and the time of staying is 10ms, and acquisition time is 44ms, reactive/collision throughput is 4.9L/min, and CeO/Ce is 0.72%.
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