CN105866156A - Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry - Google Patents

Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry Download PDF

Info

Publication number
CN105866156A
CN105866156A CN201610256731.1A CN201610256731A CN105866156A CN 105866156 A CN105866156 A CN 105866156A CN 201610256731 A CN201610256731 A CN 201610256731A CN 105866156 A CN105866156 A CN 105866156A
Authority
CN
China
Prior art keywords
sample
ray fluorescence
salt
measured
sal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610256731.1A
Other languages
Chinese (zh)
Inventor
杨振
杨剑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou 3v Prevision Instrument Co Ltd
Original Assignee
Suzhou 3v Prevision Instrument Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suzhou 3v Prevision Instrument Co Ltd filed Critical Suzhou 3v Prevision Instrument Co Ltd
Priority to CN201610256731.1A priority Critical patent/CN105866156A/en
Publication of CN105866156A publication Critical patent/CN105866156A/en
Pending legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

Abstract

The invention discloses a method for quickly determining trace elements in salt with X-ray fluorescence spectrometry. The method comprises the following steps: taking a certain amount of a salt sample, and smashing to reach certain granularity; putting the smashed salt sample in a sample cup for ramming to form a salt sample to be measured; measuring the X-ray fluorescence intensity of the salt sample to be measured by using the X-ray fluorescence spectrometry; and calculating the contents of selected elements in the salt based on a formula 1 as shown in the specification, wherein X is the X-ray fluorescence intensity, Y is the percentage contents of the selected elements, and K is a fixed parameter. According to the method, the contents of various metal elements, harmful elements and trace elements such as iodine element in the salt can be detected simultaneously, and the method has the advantages of simple operation, high analysis speed, high accuracy, high sensitivity and the like.

Description

A kind of X-ray fluorescence spectroscopy quickly measures the method for trace element in Sal
Technical field
The present invention relates to a kind of utilize the method for trace element in X fluorescence spectrum method simultaneously quickly detection Sal, belong to In field of detection of food safety.
Background technology
Sal is flavouring agent the most frequently used in culinary art.The mankind must absorb a certain amount of Sal, guarantee every day The normal operation of body.Therefore, the control to the metallic element in Sal and harmful element content is the most important 's.
Metallic element and harmful element are quite big to the harm of human body, once enter human body, accumulate to a certain extent, Will change the normal physiological function of human body and animal, part can enter nervous system, the normal merit of interference body Can and cause pathological changes.
In Sal, metal element content is to weigh Sal quality and an important indicator of safety.Metal in Sal Element kind is many, and such as copper, zinc, lead, cadmium and barium etc., and its comparision contents is low, and domestic there is no measures simultaneously The coherent detection standard of Determination of multiple metal elements and harmful element content in Sal.
Determination of multiple metal elements, harmful element and iodine in Sal the most accurately, is quickly measured therefore it provides a kind of The method of the trace element such as element is the problem urgently studied in Sal quality and safety detection.
Summary of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to a kind of X-ray fluorescence spectroscopy and quickly measure The method of trace element in Sal, the method can detect various metals and the content of harmful element in Sal simultaneously, The content of Iodine in Table Salt element can also be detected, have simple to operate, analyze that speed is fast, accuracy is high and clever Sensitivity advantages of higher.
To achieve these goals, technical scheme is as follows:
A kind of X-ray fluorescence spectroscopy quickly measures the method for trace element in Sal, comprises the following steps:
1) taking salt sample and make pulverization process, reaching granularity is 30-50 mesh；
2) salt sample after pulverizing makes salt sample to be measured；
3) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of salt sample to be measured；
4) content of chosen elements in salt sample to be measured is calculated by following equation 1,
Formula 1:Wherein, X is x-ray fluorescence intensity, and Y is the quality hundred of chosen elements Proportion by subtraction content, K is preset parameter.
Preferably, the computational methods of K numerical value include:
A) provide a series of normal saline sample with different chosen elements content, size-reduced to particle diameter be 30-50 mesh, then be compacted, form series of standards sample；
B) X fluorescence spectrum method is utilized to measure the x-ray fluorescence intensity of each normal saline sample, and respectively according to each In normal saline sample, the content of chosen elements makes standard curve with corresponding x-ray fluorescence intensity；
C) by following equation of linear regression, preset parameter K and b is calculated,
K = Σ i = 1 n X 2 Y 2 - n X 2 Y 2 ‾ Σ i = 1 n Y i 4 - n ( Y 2 ‾ ) 2 , b = Y 2 ‾ - K X 2 ‾ ,
Wherein,For chosen elements x-ray fluorescence intensity square average,For chosen elements Mass percentage content square average, and X, Y are known.
Preferably, the quality that described salt sample to be measured is taken and the uniform quality of described normal saline sample.
Preferably, the quality of described normal saline sample is more than or equal to 5g.
Preferably, by Cyclone mill, thick Sal granule is polished into the fine grained that granularity is 30-50 mesh.
Preferably, step 3) including: salt sample to be measured is put in test instrunment, and utilizes X-fluorescence light Spectrometry is tested, and described test instrunment is Xray fluorescence spectrometer.
Compared with prior art, the present invention at least has the advantage that
1) salt sample to be measured is without carrying out the pretreatment of complexity, and being not required to distinguish sample is sea salt or mineral salt, Testing time is short, it is only necessary to the percentage composition that just can measure element to be measured in sample in 10 minutes；
2) measuring accuracy is up to 95%.In addition, this detection method will not produce the consumptive material of correspondence with discarded Thing；
3) this method of testing can the most quickly detect Determination of multiple metal elements, harmful element and I in Sal Deng content, and accuracy and highly sensitive.
Accompanying drawing explanation
In order to be illustrated more clearly that present configuration feature and technical essential, below in conjunction with the accompanying drawings and specific embodiment party The present invention is described in detail for formula.
Fig. 1 is that a kind of X-ray fluorescence spectroscopy disclosed in the embodiment of the present invention quickly measures trace unit in Sal The flow chart of the method for element；
Fig. 2 is the As element disclosed in the embodiment of the present invention and Pb element and I element and the test of Ba element Design sketch.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the present embodiment, the technical scheme in embodiment is carried out concrete, clear, complete Describe wholely.
Shown in Figure 1, the embodiment of the invention discloses a kind of X-ray fluorescence spectroscopy and quickly measure in Sal The method of trace element, comprises the following steps:
1) taking a certain amount of salt sample and make pulverization process, reaching granularity is 30-50 mesh；
2) salt sample after pulverizing is placed in specimen cup compacting, forms salt sample to be measured；
3) salt sample to be measured is put in test instrunment, utilize X fluorescence spectrum method to measure salt sample to be measured X-fluorescence intensity；
4) according to the x-ray fluorescence intensity of salt sample to be measured square with the degree of salt sample to be measured Square proportional, calculate the content of chosen elements in salt sample to be measured by following formula 1,
Formula 1:Wherein, X is x-ray fluorescence intensity, and Y is the percentage ratio of chosen elements Content, K is preset parameter.
Preferably, above-mentioned steps 4) in the numerical computation method of K be:
A) provide a series of normal saline sample with different chosen elements content, size-reduced to particle diameter be 30-50 mesh, then be compacted, form series of standards sample；
B) X fluorescence spectrum method is utilized to measure the x-ray fluorescence intensity of each normal saline sample, and respectively according to each In normal saline sample, the content of chosen elements makes standard curve with corresponding x-ray fluorescence intensity；
C) by following equation of linear regression, preset parameter K and b is calculated,
K = Σ i = 1 n X 2 Y 2 - n X 2 Y 2 ‾ Σ i = 1 n Y i 4 - n ( Y 2 ‾ ) 2 , b = Y 2 ‾ - K X 2 ‾ ,
Wherein,For chosen elements x-ray fluorescence intensity square average,For chosen elements Mass percentage content square average, and X, Y are known.
Preferably, the quality that salt sample to be measured is taken and the uniform quality marking sample.Preferably, standard food The quality of salt sample is more than or equal to 5g.Preferably, by Cyclone mill thick Sal granule is polished into and has The fine grained of certain granules degree.Preferably, test instrunment is Xray fluorescence spectrometer.
Its method of testing is specifically described as a example by heavy metal species by As, Pb two below, the inspection of other element Survey method is identical with embodiment.
This method of testing is:
One) mensuration of standard sample comprises the following steps:
A) take the Sal (quantity is more than or equal to 5g) of a series of difference known As, Pb content, load Specimen cup is compacted, as standard sample；
B) measure the X-ray fluorescence spectra of institute's quasi-salt sample of label taking successively, thus obtain the X of each standard sample Ray fluorescence intensity, according to the degree of As, Pb in each normal saline sample and corresponding X-ray Fluorescence intensity makes standard curve；
C) by following equation of linear regression, preset parameter K and b is calculated,
K = Σ i = 1 n X 2 Y 2 - n X 2 Y 2 ‾ Σ i = 1 n Y i 4 - n ( Y 2 ‾ ) 2 , b = Y 2 ‾ - K X 2 ‾ ,
Wherein,For x-ray fluorescence intensity square average,Mass percent for chosen elements Content square average, and X recorded, and Y is known.
The value of X and Y is updated in above-mentioned equation respectively, K and b can be calculated.
Two) mensuration of salt sample to be measured comprises the following steps:
1) taking the salt sample identical in quality with standard sample, it is 30-50 mesh that pulverization process reaches granularity；
2) salt sample after pulverizing is placed in specimen cup compacting, forms salt sample to be measured；
3) salt sample to be measured is put in test instrunment, utilize X fluorescence spectrum method to measure in salt sample to be measured The X-fluorescence intensity of As, Pb；
4) according to the x-ray fluorescence intensity of salt sample to be measured square with the degree of salt sample to be measured Square proportional, calculate the content of As, Pb in salt sample to be measured by following formula 1, such as Fig. 2 Shown in clearly present the test effect of As, Pb in salt sample to be measured；
Formula 1:Wherein, X is x-ray fluorescence intensity, and Y is chosen elements (As, Pb) Degree, K, b are that preset parameter is relevant with test condition.
Iodine in Sal can prevent the diseases such as thyromegaly, and the too low meeting of Iodine intake causes thyromegaly etc. Iodine deficiency, but the health of body also can be affected by excessive iodine, as animal brain weight saving can be made, Learning memory decline etc..
As in the assay method salt sample to be measured as described above of the content of I, Ba of salt sample to be measured, The assay method of the content of Pb is identical, presents the test effect of I, Ba in salt sample to be measured as shown in Figure 2.
In sum, the X fluorescence spectrum method that the present embodiment provides is to the quick mensuration of various trace elements in Sal Method has the advantage that
1) salt sample to be measured is without carrying out the pretreatment of complexity, and being not required to distinguish sample is sea salt or mineral salt, Testing time is short, it is only necessary to the percentage composition that just can measure element to be measured in sample in 10 minutes；
2) measuring accuracy is up to 95%.In addition, this detection method will not produce the consumptive material of correspondence with discarded Thing；
3) this method of testing can the most quickly detect Determination of multiple metal elements, harmful element and I in Sal Deng the content of trace element, and accuracy and highly sensitive.
Above-mentioned detailed description of the invention, is only technology design and the architectural feature of the explanation present invention, it is therefore intended that allow ripe The stakeholder knowing technique can implement according to this, but above said content is not limiting as the protection model of the present invention Enclose, every any equivalence change made according to the spirit of the present invention or modification, all should fall into the present invention's Within protection domain.

Claims (6)

1. an X-ray fluorescence spectroscopy quickly measures the method for trace element in Sal, it is characterised in that bag Include following steps:
1) taking salt sample and make pulverization process, reaching granularity is 30-50 mesh；
2) salt sample after pulverizing makes salt sample to be measured；
3) X fluorescence spectrum method is utilized to measure the X-fluorescence intensity of salt sample to be measured；
4) content of chosen elements in salt sample to be measured is calculated by following equation 1,
Formula 1:Wherein, X is x-ray fluorescence intensity, and Y is the quality hundred of chosen elements Proportion by subtraction content, K is preset parameter.
A kind of X-ray fluorescence spectroscopy the most according to claim 1 quickly measures trace element in Sal Method, it is characterised in that the computational methods of K numerical value include:
A) provide a series of normal saline sample with different chosen elements content, size-reduced to particle diameter be 30-50 mesh, then be compacted, form series of standards sample；
B) X fluorescence spectrum method is utilized to measure the x-ray fluorescence intensity of each normal saline sample, and respectively according to each In normal saline sample, the content of chosen elements makes standard curve with corresponding x-ray fluorescence intensity；
C) by following equation of linear regression, preset parameter K and b is calculated,
K = Σ i = 1 n X 2 Y 2 - n X 2 Y 2 ‾ Σ i = 1 n Y i 4 - n ( Y 2 ‾ ) 2 , b = Y 2 ‾ - K X 2 ‾ ,
Wherein,For chosen elements x-ray fluorescence intensity square average,For chosen elements Mass percentage content square average, and X, Y are known.
A kind of X-ray fluorescence spectroscopy the most according to claim 2 quickly measures trace element in Sal Method, it is characterised in that the quality that described salt sample to be measured is taken and the quality one of described normal saline sample Cause.
A kind of X-ray fluorescence spectroscopy the most according to claim 2 quickly measures trace element in Sal Method, it is characterised in that the quality of described normal saline sample is more than or equal to 5g.
A kind of X-ray fluorescence spectroscopy the most according to claim 1 quickly measures trace element in Sal Method, it is characterised in that by Cyclone mill, thick Sal granule being polished into granularity is thin of 30-50 purpose Grain.
A kind of X-ray fluorescence spectroscopy the most according to claim 1 quickly measures trace element in Sal Method, it is characterised in that step 3) including: salt sample to be measured is put in test instrunment, and utilizes X Fluorescent spectrometry is tested, and described test instrunment is Xray fluorescence spectrometer.
CN201610256731.1A 2016-04-22 2016-04-22 Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry Pending CN105866156A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610256731.1A CN105866156A (en) 2016-04-22 2016-04-22 Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610256731.1A CN105866156A (en) 2016-04-22 2016-04-22 Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry

Publications (1)

Publication Number Publication Date
CN105866156A true CN105866156A (en) 2016-08-17

Family

ID=56633063

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610256731.1A Pending CN105866156A (en) 2016-04-22 2016-04-22 Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry

Country Status (1)

Country Link
CN (1) CN105866156A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111458361A (en) * 2020-01-06 2020-07-28 中国地质大学（北京） Portable XRF-based method for measuring content of elements in leech

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0627003A (en) * 1992-07-08 1994-02-04 Fuji Electric Co Ltd Analysis of adhesive
JP2002022845A (en) * 2000-07-03 2002-01-23 Ikuo Jinno Radiation detector
CN101706461A (en) * 2009-11-10 2010-05-12 天津出入境检验检疫局化矿金属材料检测中心 Method for detecting metallic silicon impurity content by using X-ray fluorescent spectrometry
CN102359972A (en) * 2011-07-18 2012-02-22 山西太钢不锈钢股份有限公司 Full-elemental analysis method for stainless steel sample
CN104181183A (en) * 2014-09-12 2014-12-03 江苏天瑞仪器股份有限公司 Method for rapidly measuring lead element in grain by X fluorescent spectrometry
CN104198513A (en) * 2014-09-12 2014-12-10 江苏天瑞仪器股份有限公司 Quick determination method for cadmium element in grains with X-ray fluorescent spectrometry
CN104297276A (en) * 2014-08-29 2015-01-21 无锡英普林纳米科技有限公司 Method for analysis of trace elements in geological sample by X-fluorescence spectrum
CN104730098A (en) * 2015-04-03 2015-06-24 甘肃酒钢集团宏兴钢铁股份有限公司 Rapid analysis method of high-content harmful element in blast furnace iron material

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0627003A (en) * 1992-07-08 1994-02-04 Fuji Electric Co Ltd Analysis of adhesive
JP2002022845A (en) * 2000-07-03 2002-01-23 Ikuo Jinno Radiation detector
CN101706461A (en) * 2009-11-10 2010-05-12 天津出入境检验检疫局化矿金属材料检测中心 Method for detecting metallic silicon impurity content by using X-ray fluorescent spectrometry
CN102359972A (en) * 2011-07-18 2012-02-22 山西太钢不锈钢股份有限公司 Full-elemental analysis method for stainless steel sample
CN104297276A (en) * 2014-08-29 2015-01-21 无锡英普林纳米科技有限公司 Method for analysis of trace elements in geological sample by X-fluorescence spectrum
CN104181183A (en) * 2014-09-12 2014-12-03 江苏天瑞仪器股份有限公司 Method for rapidly measuring lead element in grain by X fluorescent spectrometry
CN104198513A (en) * 2014-09-12 2014-12-10 江苏天瑞仪器股份有限公司 Quick determination method for cadmium element in grains with X-ray fluorescent spectrometry
CN104730098A (en) * 2015-04-03 2015-06-24 甘肃酒钢集团宏兴钢铁股份有限公司 Rapid analysis method of high-content harmful element in blast furnace iron material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111458361A (en) * 2020-01-06 2020-07-28 中国地质大学（北京） Portable XRF-based method for measuring content of elements in leech

Similar Documents

Publication Publication Date Title
Marques Jr et al. Magnetic susceptibility and diffuse reflectance spectroscopy to characterize the spatial variability of soil properties in a Brazilian Haplustalf
CN101975788B (en) Method for identifying quality of edible oil with low-field NMR (Nuclear Magnetic Resonance)
Liu et al. Feasibility of estimating heavy metal concentrations in Phragmites australis using laboratory-based hyperspectral data—A case study along Le'an River, China
CN103822935B (en) The quick analytic instrument of heavy metal cadmium and analytical approach in a kind of non-destructive determination food
Gutiérrez-Ginés et al. Assessment of field portable X-ray fluorescence spectrometry for the in situ determination of heavy metals in soils and plants
CN106706691A (en) Method for judging heavy metal detection type of portable X-ray fluorescence spectrometry
CN106442514B (en) A kind of simple overdelicate bivalent cupric ion colorimetric detection method
Hoke et al. Reconsideration of bone postmortem interval estimation by UV-induced autofluorescence
CN106153656A (en) A kind of X fluorescence spectrum method rapid assay methods to heavy metal in soil cadmium element
CN105021640A (en) Rapid X-ray fluorescence spectrometric determination method for elemental selenium in cereals
Clark et al. Examination of lead concentrations in new decorative enamel paints in four countries with different histories of activity in lead paint regulation
CN105866156A (en) Method for quickly determining trace elements in salt with X-ray fluorescence spectrometry
CN103134770B (en) Eliminate moisture detects total nitrogen content of soil impact method near infrared spectrum
He et al. An integrated system for quantitative EDXRF analysis based on fundamental parameters
CN101349662B (en) Portable metallic element analyzer
Czédli et al. Investigation of the bioaccumulation of copper in fish
CN104833653A (en) Method for rapidly analyzing content of hexogen in mixed explosive
Griesche et al. The advantage of using in-situ methods for studying hydrogen mass transport: Neutron radiography vs. carrier gas hot extraction
CN101984351A (en) Measuring method of grade of magnetic iron made of fine iron powder and measuring device thereof
CN104807844A (en) Method for rapidly screening and detecting cadmium content in rice and rice products
Sandeep et al. Diffuse reflectance spectroscopy of a tropical southern Indian lake sediment core: A window to environmental change
Tsroya et al. Fast determination of 90Sr/90Y activity in milk by Cherenkov counting
Yankovich et al. Methods of Statistical Control for Groundwater Quality Indicators
CN105137229A (en) Rapid determination method for biologic particle wave-band-cross comprehensive electromagnetic attenuation capability
Zhang et al. Quantitative analysis of overlapping x-ray fluorescence spectra for Ni, Cu, Zn in Soil by orthogonal signal correction and partial least squares algorithm

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160817