CN104807844A - Method for rapidly screening and detecting cadmium content in rice and rice products - Google Patents
Method for rapidly screening and detecting cadmium content in rice and rice products Download PDFInfo
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- CN104807844A CN104807844A CN201510187726.5A CN201510187726A CN104807844A CN 104807844 A CN104807844 A CN 104807844A CN 201510187726 A CN201510187726 A CN 201510187726A CN 104807844 A CN104807844 A CN 104807844A
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Abstract
The invention discloses a method for rapidly screening and detecting cadmium content in rice and rice products. A food heavy metal detector NX-100 F, as an X-ray fluorescence spectrometer, is adopted to determine the cadmium content and the standard-exceeding cadmium content in the rice and the rice products within 180-500s. The method comprises the steps of sample processing, measuring and result determining. A rice sample is unshelled to brown rice, the brown rice grain is directly measured, and a brown rice sample, a rice sample and a rice flour sample are directly measured. The measurement is carried out according to the operating steps of the X-ray fluorescence spectrometer, the result is determined according to the measured time and measured value displayed by the food heavy metal detector NX-100 F, and the judgment accuracy rate is higher than 90%. The method is simple to operate, rapid in determination, does not require chemical reagents, does not cause any pollution to the environment, does not affect the health of operators, is wide in application range, low in environment requirements, and is a rapid, safe and environment-friendly cadmium determining method.
Description
Technical field
The invention belongs to grain and oil goods detection technique field, relate to the rapid screening detection method of cadmium content in a kind of paddy and goods thereof, specifically, relate to the rapid screening detection method of cadmium content in a kind of paddy based on x ray fluorescence spectrometry and goods thereof.
Background technology
Paddy is the main large cereal crops of China, and along with the propelling of industrialization development and urbanization, the situation is tense in the pollution of China's paddy heavy metal pollution particularly cadmium.Bread is the staff of life, eats with An Weixian, and grain quality is safely the cardinal task involved the interests of the state and the people.Coming into the market to effectively control heavy metal pollution grain, ensureing people's health, under existing pollution situation, effective monitoring of heavy metal must be carried out from the whole link of grain circulation.The source of grain circulation and grain purchases link need to grain in heavy metal carry out effective examination and a point storage is deposited, need to detect fast content of beary metal in grain before other links, particularly grain of grain circulation enter grain ration market.
In current paddy and goods thereof, first the detection method of cadmium content needs that treatments of the sample is resolved into solution and measures, consuming time longer, also can produce a large amount of acid mist in digestion process and cause environmental pollution, measure required expensive equipment, higher to personnel's technical requirement, the demand at present a large amount of paddy detected fast can not be satisfied with.For some situation, sample does not need the exact level recording cadmium, if paddy is when storing up, for preventing the cross pollution between paddy, paddy need be carried out a point storage by the content of its cadmium and depositing, and general point 3 kinds, 1. concentration is less than 0.2mg/Kg; 2. concentration (containing two end points) between 0.2mg/Kg to 0.4mg/Kg; 3. concentration is greater than 0.4mg/Kg.1. representing this paddy is specification product, and cadmium content does not exceed standard, and can enter grain ration market; 2. represent this paddy cadmium content slightly to exceed standard, can be used as feed and use, or made by certain process that its cadmium content is up to standard enters grain ration market again; 3. represent this paddy cadmium content severe overweight, forbid using as grain ration or feed, need to carry out processing to do his use again.Therefore, at this moment only need on-the-spotly to carry out rapid screening detection to paddy cadmium content storing up, judge its content range, do not need the exact level knowing paddy cadmium.Cooperation unit before this of our unit has developed the Xray fluorescence spectrometer (patent CN 103822935 A) that directly can use cadmium content in solid Fast Measurement grain, for the quick detection of paddy cadmium achieves possibility.But this patent does not propose concrete scheme for the examination of paddy cadmium content, does not especially provide how examination, how to judge content range and the pollution level of paddy cadmium.
Summary of the invention
In order to overcome the defect existed in prior art, the invention provides the rapid screening detection method of cadmium content in a kind of paddy and goods thereof, have studied the operation steps and result decision method that use x-ray fluorescence method rapid screening paddy cadmium content, judge the cadmium content scope of paddy and goods thereof and the situation that exceeds standard fast.
Described method is x ray fluorescence spectrometry, ultimate principle excites through sigmatron based on sample, obtain the XRF of cadmium in sample (Cd) element, carry out quantitatively according to the funtcional relationship of cadmium (Cd) constituent content in XRF radiant quantity and sample.
Described method is applicable to the quick judgement of paddy and goods (ground rice etc. comprising brown rice, rice and make) cadmium content thereof.
Described method directly provides cadmium content measured value, judges the content range of cadmium in sample and the situation that exceeds standard according to decision rule examination.
Described method does not need sample pre-treatments substantially, and rice sample shelling is for brown rice is directly with brown rice grain mensuration, and brown rice sample, rice sample and ground rice sample directly measure.
Described method does not need any chemical reagent, environmentally safe, does not affect operator ' s health.
Described method is to operating personnel without concrete technical requirement, and slightly doing training can be on duty.
Described method single sample minute is shorter, and most of sample 180s gets final product judged result, and other suspicious specimen can obtain result at 500s, and judging nicety rate reaches more than 90%.
Its technical scheme is as follows:
A rapid screening detection method for cadmium content in paddy and goods thereof, comprises the following steps:
The shelling of step 1, rice sample is for brown rice is directly with brown rice grain mensuration, and brown rice sample, rice sample and ground rice sample directly measure;
Step 2, connect mensuration Xray fluorescence spectrometer power supply, by instrument preheating 10 minutes, instrument preheating only need be started shooting before survey first sample and be carried out, and the mensuration of subsequent sample does not need to continue preheating;
Press instrument instructions after step 3, sample preparation and load sample cup, and be placed in the sample cell of Xray fluorescence spectrometer;
Step 4, to be built by instrument, arrange corresponding sample and measurement parameter is measured by instrument instructions, instrument shows minute and sample cadmium content value in real time;
The content value of step 5, minute according to instrument and sample cadmium judges the content range of cadmium and the situation that exceeds standard.
Preferably, judge in step 5 that the content range of cadmium is as follows with the decision rule of the situation that exceeds standard:
Result is according to 3 of cadmium in rice concentration ranges, and not exceed standard, to exceed standard, severe overweight three kinds of modes represent:
1) concentration is less than 0.2mg/Kg, is designated as and does not exceed standard;
2) concentration is between 0.2mg/Kg to 0.4mg/Kg, containing two end points, is designated as and exceeds standard;
3) concentration is greater than 0.4mg/Kg, is designated as severe overweight.
Preferably, in step 5, the concrete steps of determination methods are:
5.1, when minute reaches 180s, there is 5.1.1, during 5.1.2,5.1.3 situation, directly judge; When there is 5.1.4 situation, continuing to measure to 500s, judging by 5.2.1,5.2.2,5.2.3;
If 5.1.1 the concentration of instrument display cadmium is less than 0.18mg/Kg, then in sample, the concentration of cadmium is less than 0.2mg/Kg, is designated as and does not exceed standard;
If 5.1.2 the concentration of instrument display cadmium is between 0.28mg/Kg to 0.38mg/Kg, then in sample, the concentration of cadmium, between 0.2mg/Kg to 0.4mg/Kg, is designated as and exceeds standard;
If 5.1.3 the concentration of instrument display cadmium is more than or equal to 0.5mg/Kg, then in sample, the concentration of cadmium is greater than 0.4mg/Kg, is designated as severe overweight;
If 5.1.4 the concentration of instrument display cadmium is between 0.18mg/Kg to 0.28mg/Kg, and between 0.38mg/Kg to 0.5mg/Kg, then continue to measure to 500s;
5.2 work as minute reaches 500s, judges by following rule;
If the concentration 5.2.1 now shown is less than 0.2mg/Kg, then in sample, the concentration of cadmium is less than 0.2mg/Kg, is designated as and does not exceed standard;
If the concentration 5.2.2 now shown is between 0.2mg/Kg to 0.4mg/Kg, then in sample, the concentration of cadmium, between 0.2mg/Kg to 0.4mg/Kg, is designated as and exceeds standard;
If the concentration 5.2.3 now shown is greater than 0.4mg/Kg, then in sample, the concentration of cadmium is greater than 0.4mg/Kg, is designated as severe overweight.
Compared with prior art, beneficial effect of the present invention: the rapid screening that present invention achieves cadmium in paddy and goods thereof is checked, improve the detection efficiency of cadmium, reduces testing cost, contributes to any occasion and judges fast Cd concentration of brown rice.
Accompanying drawing explanation
Fig. 1 is the operational flowchart of cadmium content quick screening method in paddy described in invention and goods thereof;
Fig. 2 be invention described in paddy and goods in cadmium content quick screening method result decision flow chart;
Fig. 3 of the present inventionly measures Cadmium detrmination value in gained sample based on heavy metal detector NX-100F in food and schemes over time;
Fig. 4 is the standard value working curve diagram (based on 500s data) measuring Cadmium detrmination value-cadmium in gained sample based on heavy metal detector NX-100F in food of the present invention;
Fig. 5 is the standard value graph of a relation (based on 180s data) measuring Cadmium detrmination value-cadmium in gained sample based on heavy metal detector NX-100F in food of the present invention.
Embodiment
Technical scheme of the present invention is further illustrated below in conjunction with drawings and Examples.
Embodiment 1
Rapid screening checks an x ray fluorescence spectrometry for cadmium content in paddy and goods thereof, comprises sample preparation, mensuration and result and judges three steps.
(1) sample preparation
Rice sample shelling is for brown rice is directly with brown rice grain mensuration, and brown rice sample, rice sample and ground rice sample directly measure, without the need to process.
(2) sample determination
Press instrument instructions after sample preparation and load sample cup, and be placed in the sample cell of Xray fluorescence spectrometer; Built by instrument, arrange corresponding sample and measurement parameter is measured by instrument instructions, instrument shows minute and sample cadmium content value in real time; The content value of the minute according to instrument and sample cadmium judges the content range of cadmium and the situation that exceeds standard.
(3) result judges
Concrete decision method is shown in accompanying drawing 2.
Embodiment 2
Judging nicety rate: according to this decision procedure, select 71 Rice Samples to verify, judicious sample number is 67, rate of accuracy reached 94.37% (see table 1).
Table 1 judging nicety rate
Embodiment 3
This embodiment describes based on Cadmium detrmination value relation over time in heavy metal detector NX-100F working sample in food.
Select any rice sample (cadmium content adopting graphite furnace atomic absorption spectrometry is 0.331mg/Kg), shell as brown rice, the brown rice by specification obtained is loaded sample cup, and is placed in the sample cell of Xray fluorescence spectrometer; Instrument is built, corresponding sample is set by instrument instructions and measurement parameter is measured, instrument shows minute and sample cadmium content value in real time, the sample cadmium content value of record minute and the display of instrument correspondence, take time as horizontal ordinate, with the sample cadmium content value of instrument display for ordinate, mapping, gained figure is shown in accompanying drawing 3.
As seen from the figure, along with the prolongation of minute, measured value is more and more stable, when minute is to 180s, measurement result is basicly stable, and the measurement result of 500s is substantially close to the result that graphite oven atomic absorption obtains, therefore, in order to shorten the judgement time, adopt 180s to carry out preliminary examination, suspicious specimen mensuration finally judges to 500s.
Embodiment 4
This embodiment describes the drafting based on the typical curve of heavy metal detector NX-100F rapid screening rice and product cadmium content in food of the present invention.
Select seven rice samples with different cadmium concentration, the standard value of its cadmium content uses GFAAS (graphite furnace atomic absorption spectrometry) to measure.Rice sample is shelled for brown rice, the brown rice by specification obtained is loaded sample cup, and is placed in the sample cell of Xray fluorescence spectrometer; Instrument is built, corresponding sample is set by instrument instructions and measurement parameter is measured.Record this seven rice sample 500s place cadmium measured values.
With the standard value of paddy cadmium for horizontal ordinate, with the cadmium measured value of instrument during 500s for ordinate, mapping (see accompanying drawing 4).
This typical curve is y=1.25x-0.048, r2=0.96.This figure can be used as the canonical plotting of this invention based on heavy metal detector NX-100F rapid screening rice and product cadmium content in food, generally, typical curve provides for instrument producer, if relatively large deviation appears in measuring process, according to said method can repaint typical curve.
Embodiment 5
This embodiment describes the drafting measuring the standard value working curve diagram (based on 180s data) of Cadmium detrmination value-cadmium in gained sample based on heavy metal detector NX-100F in food of the present invention.
Select 71 rice samples with different cadmium concentration, the standard value of its cadmium content uses GFAAS (graphite furnace atomic absorption spectrometry) to measure.Rice sample is shelled for brown rice, the brown rice by specification obtained is loaded sample cup, and is placed in the sample cell of Xray fluorescence spectrometer; Instrument is built, corresponding sample is set by instrument instructions and measurement parameter is measured.Record this 71 rice sample 180s place cadmium measured values.
With the standard value of paddy cadmium for horizontal ordinate, with the cadmium measured value of instrument during 180s for ordinate, mapping (see accompanying drawing 5).Scheme known thus, when 180s, when cadmium measured value is less than 0.18mg/Kg, then in sample, the actual concentrations overwhelming majority of cadmium is less than 0.2mg/Kg; When the concentration of instrument display cadmium is between 0.28mg/Kg to 0.38mg/Kg, in sample, the actual concentrations of cadmium is substantially between 0.2mg/Kg to 0.4mg/Kg; When the concentration of instrument display cadmium is more than or equal to 0.5mg/Kg, then in sample, the actual concentrations of cadmium is greater than 0.4mg/Kg substantially, determines primitive decision rule and flow process (see accompanying drawing 2) that the method judges cadmium concentration scope and the degree that exceeds standard based on this.
The rapid screening that described method achieves cadmium in paddy and goods thereof is checked, is improve the detection efficiency of cadmium, reduces testing cost, contributes to any occasion and judges fast Cd concentration of brown rice and the situation that exceeds standard.
The above, be only best mode for carrying out the invention, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses, and the simple change of the technical scheme that can obtain apparently or equivalence are replaced and all fallen within the scope of protection of the present invention.
Claims (3)
1. the rapid screening detection method of cadmium content in paddy and goods thereof, is characterized in that, comprise the following steps:
The shelling of step 1, rice sample is for brown rice is directly with brown rice grain mensuration, and brown rice sample, rice sample and ground rice sample directly measure;
Step 2, connect mensuration Xray fluorescence spectrometer power supply, by instrument preheating 10 minutes, instrument preheating only need be started shooting before survey first sample and be carried out, and the mensuration of subsequent sample does not need to continue preheating;
Press instrument instructions after step 3, sample preparation and load sample cup, and be placed in the sample cell of Xray fluorescence spectrometer;
Step 4, to be built by instrument, arrange corresponding sample and measurement parameter is measured by instrument instructions, instrument shows minute and sample cadmium content value in real time;
The content value of step 5, minute according to instrument and sample cadmium judges the content range of cadmium and the situation that exceeds standard.
2. the rapid screening detection method of cadmium content in paddy according to claim 1 and goods thereof, is characterized in that, judges that the decision rule of the content range of cadmium and the situation that exceeds standard is as follows in step 5:
Result is according to 3 of cadmium in rice concentration ranges, and not exceed standard, to exceed standard, severe overweight three kinds of modes represent:
1) concentration is less than 0.2mg/Kg, is designated as and does not exceed standard;
2) concentration is between 0.2mg/Kg to 0.4mg/Kg, containing two end points, is designated as and exceeds standard;
3) concentration is greater than 0.4mg/Kg, is designated as severe overweight.
3. the rapid screening detection method of cadmium content in paddy according to claim 1 and goods thereof, it is characterized in that, in step 5, the concrete steps of determination methods are:
5.1, when minute reaches 180s, there is 5.1.1, during 5.1.2,5.1.3 situation, directly judge; When there is 5.1.4 situation, continuing to measure to 500s, judging by 5.2.1,5.2.2,5.2.3;
If 5.1.1 the concentration of instrument display cadmium is less than 0.18mg/Kg, then in sample, the concentration of cadmium is less than 0.2mg/Kg, is designated as and does not exceed standard;
If 5.1.2 the concentration of instrument display cadmium is between 0.28mg/Kg to 0.38mg/Kg, then in sample, the concentration of cadmium, between 0.2mg/Kg to 0.4mg/Kg, is designated as and exceeds standard;
If 5.1.3 the concentration of instrument display cadmium is more than or equal to 0.5mg/Kg, then in sample, the concentration of cadmium is greater than 0.4mg/Kg, is designated as severe overweight;
If 5.1.4 the concentration of instrument display cadmium is between 0.18mg/Kg to 0.28mg/Kg, and between 0.38mg/Kg to 0.5mg/Kg, then continue to measure to 500s;
5.2 work as minute reaches 500s, judges by following rule;
If the concentration 5.2.1 now shown is less than 0.2mg/Kg, then in sample, the concentration of cadmium is less than 0.2mg/Kg, is designated as and does not exceed standard;
If the concentration 5.2.2 now shown is between 0.2mg/Kg to 0.4mg/Kg, then in sample, the concentration of cadmium, between 0.2mg/Kg to 0.4mg/Kg, is designated as and exceeds standard;
If the concentration 5.2.3 now shown is greater than 0.4mg/Kg, then in sample, the concentration of cadmium is greater than 0.4mg/Kg, is designated as severe overweight.
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Cited By (3)
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| CN105410593A (en) * | 2015-11-19 | 2016-03-23 | 湖南省粮油产品质量监测中心 | Cadmium content reduction treatment method aiming at rice with cadmium pollution of different standard exceeding degrees |
| CN106950238A (en) * | 2017-05-26 | 2017-07-14 | 广东省粮食科学研究所 | A kind of Fast nondestructive evaluation and the method for filtering out low cadmium rice or brown rice simultaneously |
| CN112415035A (en) * | 2020-11-17 | 2021-02-26 | 湖南生物机电职业技术学院 | Method for measuring cadmium content in ratoon rice |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006284378A (en) * | 2005-03-31 | 2006-10-19 | National Institute Of Advanced Industrial & Technology | Simplified analysis method of heavy metal in agricultural product |
| CN103645201A (en) * | 2013-12-13 | 2014-03-19 | 彭新凯 | Method for rapidly detecting heavy metal cadmium in rice based on X-ray fluorescence |
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| CN105410593A (en) * | 2015-11-19 | 2016-03-23 | 湖南省粮油产品质量监测中心 | Cadmium content reduction treatment method aiming at rice with cadmium pollution of different standard exceeding degrees |
| CN106950238A (en) * | 2017-05-26 | 2017-07-14 | 广东省粮食科学研究所 | A kind of Fast nondestructive evaluation and the method for filtering out low cadmium rice or brown rice simultaneously |
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