CN103364424B - Fluorescent x-ray analyzer - Google Patents
Fluorescent x-ray analyzer Download PDFInfo
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- CN103364424B CN103364424B CN201310005481.0A CN201310005481A CN103364424B CN 103364424 B CN103364424 B CN 103364424B CN 201310005481 A CN201310005481 A CN 201310005481A CN 103364424 B CN103364424 B CN 103364424B
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Abstract
The present invention provides a kind of fluorescent x-ray analyzer, and it can rapidly carry out the good analysis of precision in the analysis of the sample container using liquor sample overflow.This device includes:Sample container (5), by the liquor sample injecting from below (S) from top (51) overflow, the horizontal cross-section in the space within this sample container is adjoint to be extended upward from prescribed depth and broadens this sample container (5);Sample injecting mechanism (7), liquor sample (S) is injected in sample container (5) this sample injecting mechanism;X-ray source (1), this x-ray source irradiates primary X-ray (2) to the top surface of the liquor sample (S) being injected in sample container (5);Testing agency (4), the secondary x rays (3) that the detection of this testing agency produces from liquor sample (S);Controlling organization (8), this controlling organization Control Assay injecting mechanism (7), x-ray source (1) and testing agency (4), so that when the liquor sample (S) being injected in said sample container (5) is from sample container (5) overflow, then stop injection, start to measure.
Description
Technical field
The present invention relates to a kind of fluorescent x-ray analyzer, this fluorescent x-ray analyzer is to being received in sample container
Liquor sample irradiate from x-ray source primary X-ray, detection from liquor sample produce secondary x rays.
Background technology
In the past, there are following fluorescent x-ray analyzers, wherein, setting from the production being directly connected to analytical equipment
Liquor sample is imported in the on-line analyses of METHOD FOR CONTINUOUS DETERMINATION of analytical equipment by standby, processing equipment etc., connects from the lower section of sample container
Continuous injection liquor sample, while making liquor sample overflow (spilling) from the top of sample container, to being received in sample container
In liquor sample top surface irradiate primary X-ray, be measured.But, due to being to enter while making liquor sample overflow
Row measures, therefore by the flowing of liquor sample, the apical side height as the liquor sample of aspect of measure produces change.Thus, measure
Face and the distance change of x-ray source and X-ray detector, the Strength Changes of the secondary x rays being detected are it is impossible to carry out precision
Good analysis.
Then, the coated film apparatus for measuring thickness (patent documentation 1) using following fluorescent x-ray analyzers occurs, should
Fluorescent x-ray analyzer carries out composition analysis to the liquid coating (liquor sample) before application, for setting in automatic coating
To the paint line that application is carried out on metal covering in standby.Wherein as shown in figure 4, the sized roller applicator of application is carried out on roll metallic plate
Connect the secondary coatings tank 115 with overflow launder in the coatings tank 113 of (roll coater), so that the aspect of measure of liquor sample is smoothed
Few with fluctuation, and the distance away from X-ray tube ball 120 and detector 121 with low uncertainty in the case of be measured.
Prior art literature
Patent documentation 1:The real public clear 62-36083 publication of Japan
Content of the invention
The problem to be solved of invention
But, in the application apparatus for measuring thickness described in patent documentation 1, due to making to enter while liquor sample overflow
Row measures, and this aspect of measure (top surface) is not at resting state, therefore does not have the change of the height of aspect of measure it is impossible to carry out precision good
Analysis.
Then, the present invention is directed to above-mentioned existing problem and proposes, and its object is to provide a kind of x-ray fluorescence analysis dress
Put, be analyzed using following sample containers, this sample container by the liquor sample injecting from below from top overflow (spilling),
In this analysis, measure liquor sample in resting state in short time, thus, can rapidly carry out the good analysis of precision.
For solving the technical scheme of problem
To achieve these goals, the fluorescent x-ray analyzer of the present invention includes:Sample container, this sample container will
, from top overflow, the horizontal cross-section in the space within this sample container is with from prescribed depth court for the liquor sample injecting from below
Extend upward and broaden;Sample injecting mechanism, liquor sample is injected in said sample container this sample injecting mechanism;X
Radiographic source, this x-ray source irradiates primary X-ray to the top surface of the liquor sample being injected in said sample container;Testing agency,
The secondary x rays that the detection of this testing agency produces from liquor sample;Controlling organization, this controlling organization controls said sample implanter
Structure, above-mentioned x-ray source and above-mentioned testing agency hold so that working as the liquor sample being injected in said sample container from said sample
During device overflow, then stop injection, start to measure.
According to the fluorescent x-ray analyzer of the present invention, because the horizontal cross-section in the space in sample container is with from rule
Depthkeeping degree extends upward and broadens, therefore when liquor sample injects, advances with towards the top of sample container, liquid tries
The rate of climb of the top surface of sample is slack-off, if the injection of stop liquid sample, due to forming the water that aspect of measure is not changed in short time
Plane, can measure liquor sample in resting state, therefore can quickly carry out the good analysis of precision.
In the fluorescent x-ray analyzer of the present invention, above-mentioned controlling organization preferably controls above-mentioned x-ray source and above-mentioned inspection
Survey mechanism so that making the stipulated time of the suspended solid sedimentation of the adjacent top surface of liquor sample after the injection of liquor sample stops
Afterwards, start to measure.In this occasion, equally in the mensure of the liquor sample that dregs (slag), particulate material etc. coexist, formed
The horizontal plane that the aspect of measure of liquor sample is not changed in, and be in the dregs swimming the aspect of measure vicinity of liquor sample,
The state of the sedimentations such as particulate material, starts to measure after the stipulated time, thus, can rapidly carry out the good analysis of precision.
In the fluorescent x-ray analyzer of the present invention, said sample container is preferably provided with and for liquor sample to be discharged to bottom
Dump valve, above-mentioned controlling organization is controlled the detection so that secondary x rays in above-mentioned testing agency to above-mentioned dump valve
Afterwards, drain sample.In this occasion, due to discharging the liquor sample of the whole amount having measured, therefore in injection mensure next time
During liquor sample, the liquor sample having measured and the liquor sample measuring next time do not mix, and can correctly measure to sample container
Injection when liquor sample.In addition, in the mensure of the liquor sample that dregs, particulate material etc. coexist, due to liquid examination
Sample, while rinsing the deposit of the dregs of the bottom being deposited in sample container, particulate material etc., is arranged from sample container
Go out, there is no the deposit remaining, therefore impact is not produced on the liquor sample of injection next time, the liquid of next time can be started in short time
The mensure of body sample.
In the fluorescent x-ray analyzer of the present invention, be preferably provided X-ray transparent film, this X-ray transparent film with above-mentioned
Between the top of sample container, there is specified gap.In this occasion, because liquor sample is covered by X-ray transparent film, therefore can prevent
Only the pollution of liquor sample, can prevent the corrosion of the works of the device being caused by corrosive gas that liquor sample produces.
Brief description
Fig. 1 is the schematic diagram of the fluorescent x-ray analyzer representing embodiments of the present invention;
Fig. 2 is the sectional view of sample container in this device and container for capturing;
Fig. 3 is the operational flowchart of the operation representing this device;
Fig. 4 is the schematic diagram measuring device in the past using the coating thickness of fluorescent x-ray analyzer.
Specific embodiment
Below the fluorescent x-ray analyzer of the present invention is illustrated.First, as shown in figure 1, this fluorescent X-ray divides
Analysis apparatus include:Sample container 5, wherein, the liquor sample S injecting from below is from top 51 overflow;Sample injecting mechanism 7, should
Liquor sample S is injected in sample container 5 sample injecting mechanism 7;X-ray source 1, primary X-ray 2 is irradiated by this x-ray source 1
Top surface to the liquor sample S having been injected in sample container 5;Testing agency 4, this testing agency 4 detects and overflows from liquor sample S
The secondary x rays 3 of stream;Controlling organization 8, this controlling organization 8 is controlled to sample injecting mechanism 7, x-ray source 1 and testing agency 4
System, so that when the liquor sample S being injected in sample container 5 is from sample container 5 overflow, then stopping injection, starts to measure;
X-ray transparent film 25, this X-ray transparent film 25 has specified gap between the top 51 of sample container 5;Container for capturing 6,
This container for capturing 6 captures the liquor sample S of top 51 overflow from sample container 51.Particularly, in the device of present embodiment
In, controlling organization 8 is controlled to x-ray source 1 and testing agency 4 so that making liquid try after the injection of liquor sample S stops
After the stipulated time of suspended solid sedimentation of the adjacent top surface of sample S, start to measure.
Container for capturing 6 is arranged along the periphery wall of sample container 5, and the liquor sample S of capture overflow, from delivery pipe
(drain) 62 and discharge.Testing agency 4 includes the secondary x rays 3 occurring from liquor sample S are carried out with the beam splitter of light splitting
The X-ray detector 42 of 41 secondary x rays 3 passing through beam splitter 41 light splitting with detection.The device of present embodiment is polynary
The fluorescent x-ray analyzer of plain mensure type simultaneously, including its quantity testing agency corresponding with analysis object elements quantity
4.
As shown in Fig. 2 sample container 5 according to space in sample container horizontal cross-section from inlet 52 described later to rule
It is certain for determining depth H, expands upward along from prescribed depth H, has inclined plane from prescribed depth H to top
55, there is inlet 52, the outlet 54 liquor sample S being discharged to bottom 53 and the dump valve injecting liquor sample S in bottom
11.The top surface inner face of sample container 5 both can not be the inclined plane 55 of straight line, alternatively bending, step-like.Sample container 5
The spatial form of prescribed depth H and sample container is contemplated that the characteristic of liquor sample S, such as the presence or absence of suspended solid, viscosity, one-tenth
Grade and formed.Spatial form in sample container directly forms inclined plane 55 according to outlet 54.That is, also can be according to the rules
The mode of depth H=0 is formed.Form the characteristic corresponding to the liquor sample S being measured, can be different from internal spatial form
The structure selecting in multiple sample containers 5 and changing.
Inlet 52 is connected with sample injecting mechanism 7.Dump valve 11 is according to the detection of the secondary x rays 3 in testing agency 4
The mode discharging liquor sample S afterwards is controlled by controlling organization 8.
If the X-ray transparent film 25 being arranged at the top 51 of sample container 5 gets too close to the top 51 of sample container 5,
Because X-ray transparent film 25 is subject to polluting of foam, the spittle of liquor sample S etc., there is the danger leading to analysis precision to reduce.
Therefore the specified gap between the top 51 of X-ray transparent film 25 and sample container 5, can be the gap considering above-mentioned item,
Such as, be fixed on according to the mode in the gap with 9mm container for capturing 6 top 61 all-round.Due to by X-ray transparent film
25 Covering Liguid sample S, therefore the pollution of the mensure optical system of fluorescent x-ray analyzer that liquor sample S causes can be prevented,
And the corrosion of the works of device that the corrosive gas being caused by liquor sample S brings can be prevented.In the present embodiment,
It is provided with X-ray transparent film 25, however, it is not necessary to the spy according to the setting environmental condition of fluorescent x-ray analyzer, liquor sample
Property etc. and arrange.
As shown in figure 1, the foul water tank of sample injecting mechanism 7 and the sewage for the treatment of process of storage such as sewage (in figure is not
Illustrate) connect, this sewage is sampled as liquor sample S, is injected into sample from the inlet 52 (Fig. 2) of sample container 5
In container 5.Sample injecting mechanism 7 has for being injected into liquor sample S in sample container 5, or stops the note of this injection
Enter valve (not shown), injection valve is controlled by controlling organization 8.From the beginning of the injection to the liquor sample S of sample container 5
Rise, overflow time when sample container 5 overflow for the liquor sample S being injected is previously stored in controlling organization 8.Pass through
The control of controlling organization 8, opens the injection valve of sample injecting mechanism 7, starts the injection to liquor sample S to sample container 5, such as
Fruit reaches the overflow time being stored in controlling organization 8, then close injection valve, the injection of stop liquid sample S.If as this
Sample, the liquor sample S having been injected into from sample container 5 overflow, then stops injection, starts to measure.Particularly, in present embodiment
Device in, as aftermentioned, so that the suspended solid of the adjacent top surface of liquor sample S is sunk after the injection of liquor sample S stops
After the stipulated time of fall, start to measure.The liquor sample S of overflow discharges from the delivery pipe 62 of container for capturing 6.
Below according to the operating process of Fig. 3, the operating process of the fluorescent x-ray analyzer of present embodiment is said
Bright.
In step S1, in fluorescent x-ray analyzer, set analysis condition, start to analyze.
In step S2, after starting analysis, then pass through the control of controlling organization 8, open the injection valve of sample injecting mechanism 7,
As liquor sample S, the inlet 52 (Fig. 2) starting from below holds the sewage being received in inclusion mud in foul water tank to sample
The injection of device 5.
In step S3, the starting to the overflow being stored in controlling organization 8 to the injection of sample container 5 from liquor sample S
Time continues injection, after reaching overflow time, then closes injection valve, the injection of stop liquid sample S.Due in sample container
Space horizontal cross-section with extending upward from prescribed depth H and expand, therefore in the injection of liquor sample S, along
Carry out towards the top of test chamber 5, the rate of climb of the top surface of liquor sample S is slack-off, if overflow time, liquor sample
The injection of S stops, then form, in the short time, the horizontal plane that aspect of measure is not changed in, and liquor sample S remains static.
In step S4, from the injection of liquor sample S stops, swim to the aspect of measure vicinity being in liquor sample S
Dregs, the sedimentation time being stored in controlling organization 8 of the stipulated time of the state of sedimentation such as particulate material, hold in sample
Device 5 is internal to keep liquor sample S.The sedimentation time being stored in controlling organization 8 is contemplated that the characteristic of liquor sample S, such as floating
Trip the presence or absence of material, viscosity, composition etc. and determine.
After step S5, the sedimentation time in being stored in controlling organization 8, start to measure, to the top surface of liquor sample S from
X-ray source 1 irradiates primary X-ray 2, detects the secondary x rays 3 producing from liquor sample S by testing agency 4, liquid is tried
Analysis object elements in sample S carry out quantitation.
If measure terminating, passing through the control of controlling organization 8 in step S6, opening dump valve 11, from sample container 5 row
Go out liquor sample S, then, dump valve 11 cuts out.Now, due to discharging the whole amount of the liquor sample S having measured, therefore in note
When entering the liquor sample S that next time measures, can be in the liquor sample S having measured and the unmixed situation of the liquor sample S having measured
Under, correctly measure liquor sample S when being injected in test chamber 5.In addition, the liquid coexisting in dregs, particulate material etc.
In the mensure of body sample S, liquor sample S is in the precipitation of the dregs to the bottom 53 being deposited in test chamber 5, particulate material etc.
While material is rinsed, discharge from sample container 5, do not residue in the deposit in test chamber 5, thus, do not have
Impact to the liquor sample S of injection next time, can start the mensure of the liquor sample S of next time at short notice.In addition, in device
Timing, is carried out by termly Purified Water being injected in test chamber 5, can remove and accumulates on sample every time microly
Attachment in container 5.
In step S7, in addition to the occasion that mensure person carries out step S8 of the operation of stopping fluorescent x-ray analyzer,
Automatically carry out the mensure (YES) of next time, return to step S2, the liquor sample S of injection mensure next time, step is repeated successively
The operation of rapid S2~S7, continues analysis.Like this, the process of step S2~S7 can be repeated, can be close to METHOD FOR CONTINUOUS DETERMINATION
State is analyzed.In the occasion (no) of the mensure not carrying out next time, carry out step S8.
In step S8, mensure person stops the operation of fluorescent x-ray analyzer, terminates the analysis of the process step of sewage.
Fluorescent x-ray analyzer in the embodiment, because the horizontal cross-section in the space in sample container is adjoint
Extend upward from prescribed depth and broaden, therefore in the injection of liquor sample S, with the top row towards sample container 5
Enter, the rate of climb of the top surface of liquor sample S is slack-off, if the injection of stop liquid sample S, do not have at short notice due to constituting
There is the horizontal plane of the change of aspect of measure, liquor sample S can be measured in resting state, therefore can rapidly carry out good the dividing of precision
Analysis.Particularly, in the device of present embodiment, due to according to the top making liquor sample S after the injection of liquor sample S stops
The mode starting to measure after the stipulated time of suspended solid sedimentation near face makes controlling organization 8 to x-ray source 1 and testing agency
4 are controlled, therefore equally in the mensure of liquor sample S that particulate material etc. coexists, form the aspect of measure of liquor sample S
There is no a horizontal plane changing, and can swim in the aspect of measure vicinity of liquor sample S dregs, the sedimentation such as particulate material
State starts to measure, and rapidly carries out the good analysis of precision.
In the device of present embodiment, liquor sample is the sewage of the treatment process of sewage, but however it is not limited to dirty
Water, both can be to surface treatment liquid that liquid coating, metal surface are surface-treated etc., alternatively continuously sampled
Liquor sample.
The device of present embodiment enters as the wavelength-dispersion type fluorescent x-ray analyzer of multielement simultaneous determination type
Go explanation, but, assembly of the invention both can be the wavelength-dispersion type fluorescent x-ray analyzer of sweep type, can be also energy
The fluorescent x-ray analyzer of amount decentralized.
The explanation of label:
Label 1 represents x-ray source;
Label 2 represents primary X-ray;
Label 3 represents secondary x rays;
Label 4 represents testing agency;
Label 5 represents sample container;
Label 7 represents sample injecting mechanism;
Label 8 represents controlling organization;
Label 11 represents dump valve;
Label 25 represents X-ray transparent film;
Label H represents prescribed depth;
Label S represents sample.
Claims (4)
1. a kind of fluorescent x-ray analyzer, it includes:
Sample container, this sample container is by the liquor sample injecting from below from top overflow, the space within this sample container
Horizontal cross-section with extending upward from prescribed depth and broaden;
Sample injecting mechanism, liquor sample is injected in said sample container this sample injecting mechanism;
X-ray source, this x-ray source irradiates primary X-ray to the top surface of the liquor sample being injected in said sample container;
Testing agency, the secondary x rays that the detection of this testing agency produces from liquor sample;
Controlling organization, this controlling organization controls said sample injecting mechanism, above-mentioned x-ray source and above-mentioned testing agency so that working as
It is injected into liquor sample in said sample container when said sample receptacle overflow, then stops injection, start to measure.
2. fluorescent x-ray analyzer according to claim 1, wherein, above-mentioned controlling organization control above-mentioned x-ray source and
Above-mentioned testing agency is so that make the rule of the suspended solid sedimentation of the adjacent top surface of liquor sample after the injection of liquor sample stops
After fixing time, start to measure.
3. fluorescent x-ray analyzer according to claim 1 and 2, wherein, said sample container has liquor sample
It is discharged to the dump valve of bottom, above-mentioned controlling organization is controlled to above-mentioned dump valve so that penetrating in the secondary X of above-mentioned testing agency
After the detection of line, drain sample.
4. fluorescent x-ray analyzer according to claim 1 and 2, wherein, arranges X-ray transparent film, this X-ray is saturating
Cross, between film and the top of said sample container, there is specified gap.
Applications Claiming Priority (2)
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JP2012-071536 | 2012-03-27 | ||
JP2012071536A JP5488632B2 (en) | 2012-03-27 | 2012-03-27 | X-ray fluorescence analyzer |
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CN103364424B true CN103364424B (en) | 2017-03-01 |
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CN (1) | CN103364424B (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
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EP3249394B1 (en) | 2016-05-26 | 2018-09-12 | Malvern Panalytical B.V. | X-ray analysis of drilling fluid |
JP6423048B1 (en) * | 2017-06-16 | 2018-11-14 | マルバーン パナリティカル ビー ヴィ | X-ray analysis of drilling fluid |
CN109406557A (en) * | 2018-12-07 | 2019-03-01 | 长沙开元仪器有限公司 | A kind of fluid sample on-line analysis device |
JP6982031B2 (en) | 2019-07-18 | 2021-12-17 | 日本電子株式会社 | X-ray fluorescence measuring device |
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JPS49131993U (en) * | 1973-03-12 | 1974-11-13 | ||
US7722821B2 (en) * | 2004-11-17 | 2010-05-25 | Chemplax Industries, Inc. | Sample cup for use in X-ray spectroscopy with internal overflow reservoir |
CN2886571Y (en) * | 2006-04-16 | 2007-04-04 | 卢德国 | Full-automatic biochemical analyzer kit |
CN102432454A (en) * | 2010-09-07 | 2012-05-02 | 日本化学工业株式会社 | Barium titanyl oxalate particle, method for preparing the same and method for preparing barium titanate |
CN102128849B (en) * | 2010-12-03 | 2013-03-13 | 浙江大学 | Online sampling device and online sampling method for X-ray fluorescent spectrograph |
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JP2013205081A (en) | 2013-10-07 |
JP5488632B2 (en) | 2014-05-14 |
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