CN102235977B - Icp analysis device and analytical procedure thereof - Google Patents

Icp analysis device and analytical procedure thereof Download PDF

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Publication number
CN102235977B
CN102235977B CN201110086370.8A CN201110086370A CN102235977B CN 102235977 B CN102235977 B CN 102235977B CN 201110086370 A CN201110086370 A CN 201110086370A CN 102235977 B CN102235977 B CN 102235977B
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optically focused
plasma
plasma torch
analysis device
icp analysis
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CN102235977A (en
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田边英规
长泽宽治
赤松宪
赤松宪一
松泽修
中野信男
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Hitachi High Tech Science Corp
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Hitachi High Tech Science Corp
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Abstract

The present invention relates to a kind of icp analysis device and analytical procedure thereof, apply flexibly can carry out high sensitivity measuring but the generation direction of principal axis of the fast plasma body of the deterioration of device measures and device deterioration less but the transverse direction of the low plasma body of sensitivity in measuring each feature of measuring and the vergence direction that can carry out highly sensitive and alleviate the deterioration of device measures. It is configured to: in order to described plasma torch is set as arbitrarily angled, taking straight line shape to put ground configuring plasma blowtorch and during optically focused portion as benchmark, at least one is made to rotate into direction relative to getting of the light of the plasma body in the optically focused portion in icp analysis device, thus with arbitrarily angled to putting.

Description

Icp analysis device and analytical procedure thereof
Technical field
The present invention relates to the inductively coupled plasma body such as inductively coupled plasma body quality analysis apparatus (ICP-MS), luminous light splitting (spectrum) analytical equipment (ICP-OES) of inductively coupled plasma body (following, it is called ICP) analytical equipment, particularly relate to icp analysis device and the analytical procedure thereof of plasma torch (plasmatorch) and the photometric measurer that it is characterized in that icp analysis device.
Background technology
Fig. 5 illustrates the summary construction diagram of a routine existing icp analysis device. Comprising: the plasma torch 51 producing inductively coupled plasma body; This plasma torch 51 is applied the ruhmkorff coil 52 of high-frequency voltage; The optically focused portion 53 that the light of the plasma body axis along plasma torch 51 occurred and the light of plasma body occurred along the direction orthogonal with the axis of plasma torch 51 are introduced respectively; The fixing speculum 54 of spectrum part 56 as target is incided taking the light by the plasma body occurred along the direction orthogonal with the axis of plasma torch 51; And there is the variable mirror 55 of the function of the arbitrary light selecting the light inciding optical splitter to be the light in the generation direction from plasma body and the light of the direction generation orthogonal with to generation direction.
By driving variable mirror 55, according to the light of the plasma body that the light and the direction orthogonal with the axis of plasma torch 51 of analyzing the plasma body that switching occurs along the axis of plasma torch 51 occur, and measured (reference patent documentation 1).
So, from the light of two direction optically focused plasma bodys icp analysis device, its reason is as follows.
First, depend on from the optically focused of axis optical splitter can be made to obtain the light for analyzing near central shaft more. The plasma body of icp analysis device is ring structure, and plasma body occurs near the central shaft in direction to become cold zone behind this high-temperature zone again for cold zone and towards becoming high-temperature zone around it. For the center of the plasma body of ring structure, test portion is introduced into along its central axis direction. Thus, there is more test portion in the cold zone of the heart in the plasma, in other words, measures sensitivity and improves, so having advantage on axial optically focused. But, in axial optically focused, also other things that coexists many are obtained from plasma body together with test portion, therefore analytical results easily affects by it, in addition, high-temperature zone near the central shaft of plasma body has the luminescence from plasma gas, the background (background) when becoming analysis.
On the other hand, from the optically focused of the transverse direction of plasma body, the probability that exists of test portion can't because of more high the closer to central shaft, and the impact of other the thing that coexists in addition is less, therefore has advantage in the precision this point improving analytical results.
Patent documentation 1: Japanese Unexamined Patent Publication 9-318537 publication
Summary of the invention
But, above-mentioned existing icp analysis device produces following problem.
That is, fixing speculum 54 and the variable mirror 55 switching in optically focused direction with switching, it is thus desirable to adjust multiple speculum, and needs the driving mechanism arranging these speculums respectively. In order to meet these requirements, it is necessary to suitable controlling organization, there is the problem of whole device complexity. In addition, in order to possess these mechanisms, cost also can increase. And, from the viewpoint of device lifetime, during owing to axially getting the light into plasma body, optically focused portion is directly by its heat, so the problem that the life-span that there is so-called detection portion is short.
, in the method, in addition the light of the plasma body that the axis along plasma torch 51 occurs and the arbitrary light of the light of plasma body occurred along the axial orthogonal directions with plasma torch 51, all can not be good with sensitivity arbitrarily angled align. Thus, the luminescence from the test portion being incorporated into plasma body can not be got into from the direction of highly sensitive, so being still in inefficient state.
In order to reach above-mentioned purpose, the present invention provides following scheme.
The icp analysis device of the present invention, comprising: the plasma torch introducing the test portion of plasma body gas and droplet; Apply the ruhmkorff coil of plasma torch high-frequency voltage; The luminescence of the test portion excited from the plasma body by occurring by the high-frequency voltage of ruhmkorff coil is carried out the optically focused portion of optically focused; And there is the analyzing and processing portion that the luminescent spectrum to the light after optically focused carries out the spectrum part of light splitting, it is characterized in that, possesses angle-adjusting mechanism, arbitrarily angled in order to plasma torch is adjusted to, it is possible to optically focused portion and plasma torch are relatively moved into direction relative to the getting of light of the plasma body in optically focused portion.
It is movable that angle-adjusting mechanism is made at least one that make plasma torch and/or optically focused portion, and can get into the light of the vergence direction from plasma body. In addition, this movable agency is made by the optically focused portion of plasma torch front end and detector taking straight line shape position arranged opposite as benchmark, by rotating wherein any one or two such that it is able to relatively rotate.
(invention effect)
The icp analysis device of the present invention and measuring method thereof, carrying out getting to optically focused portion into when plasma light with icp analysis device, and not only the axis of plasma light or its positive side surface direction, can implement from any direction that sensitivity is good with high-level efficiency. In addition, make plasma body and from the optically focused portion of light herein axially non-to putting, thus the load that alleviator is suffered because of heating, and the life-span of device can be extended.
Accompanying drawing explanation
Fig. 1 is the concise and to the point figure of the icp analysis device representing whole the present invention.
Fig. 2 is the concise and to the point figure representing the plasma torch involved by icp analysis device of the present invention and the first enforcement mode of detector.
Fig. 3 is the concise and to the point figure representing the plasma torch involved by icp analysis device of the present invention and the 2nd enforcement mode of detector.
Fig. 4 is the concise and to the point figure representing the plasma torch involved by icp analysis device of the present invention and the 3rd enforcement mode of detector.
Fig. 5 is the structure iron of the plasma torch peripheral portion representing a routine existing icp analysis device.
Embodiment
Hereinafter, with reference to Fig. 1, the icp analysis device of brief description the present invention. In addition, accompanying drawing is suitable for changing dimension ratio for the part that dimension ratio is unimportant and is recorded.
Fig. 1 illustrates that the ICP device as the present invention carries out the concise and to the point figure of the device of spectrum analysis.
The gas for the formation of plasma body (argon, nitrogen, helium etc.) is supplied from gas control portion 17 to plasma torch 13. The top of plasma torch 13 becomes opening portion, neighboring, end is configured with ruhmkorff coil 12 thereon, from the gas of gas control portion 17 supply, it is subject to exciting/luminescence from the electric power of high frequency electric source 16, generates plasma body 11 from the opening portion of the top of plasma torch 13.
With atomizer 15, test portion be atomized together with carrier gas (carriergas) after through by spray room 14, being introduced in the immediate vicinity of plasma body 11 by managing (innertube) in plasma torch 13, be excited and luminous.
From the light of plasma body 11, got behind optically focused portion 2, it is directed to spectrum part 31. Then, the output detected in spectrum part 31, the arithmetic processing section 33 of input data, is displayed on this incidental watch-dog of arithmetic processing section 33. As arithmetic processing section 33, it is possible to use the Personal Computer (PC) sold on market.
The control during mensuration of high frequency electric source 16 or optical splitter 31 is undertaken by electronically controlled platform 32.
Angle-adjusting mechanism 4 be adjustment optically focused portion 2 and plasma torch 13 to the mechanism of the angle put so that the light from plasma body 11 can be got into from any direction by optically focused portion 2. This angle-adjusting mechanism 4 is by controlling from the instruction of arithmetic processing section 33. As its method, optically focused portion 2 and/or plasma torch 13 are carried out on the circle of dotted line as orbit rotation relative to center O.
Hereinafter, illustrate that optically focused portion 2 and plasma torch 13 are to the adjustment of the angle put.
(the first enforcement mode)
First, with reference to Fig. 2, the first enforcement mode of the icp analysis device of the present invention is described.
Fig. 2 illustrates the example plasma torch 13 of icp analysis device of the present invention and a concise and to the point figure for the structure in optically focused portion 2.
As shown in the drawing, its position is fixed in optically focused portion 2, plasma torch 13 become taking with optically focused portion 2 to the position put as benchmark (A-A '), the movable manner of arbitrary angle position can be got.
Movably control by angle-adjusting mechanism 4, plasma torch 13 is moved on inducer 131a. At this moment, plasma torch 13 and inducer 131a drive integratedly. Before and after the driving of inducer 131a, if the position relation of plasma torch 131a and ruhmkorff coil 12 can not change. Plasma torch 13 can also be such mechanism: by establishing the not shown setting unit that can carry to arrange, and this setting unit is set to move at inducer 131a.
Inducer 131a is the shape of 1/4 circular arc, and plasma torch 13 can be made to get arbitrarily angled relative to optically focused portion 2 the scope of 0��90 degree that comprises the positive side surface direction of the axis from plasma body (A-A ') to plasma body (2A-2A '). , it is contemplated that the sensitivity of the situation of test portion or the life-span of device, thus best angle can be set. Specifically, by not shown fixing tool, plasma torch 13 is installed in inducer 131a, such as, be secured in inducer 131a by the pressure etc. of spring. In this case, the main body portion of inducer 131a can use the rail-like parts etc. with concavo-convex portion.In addition, plasma torch 13 can dismount, and is installed to optional position.
Angle-adjusting mechanism 4 is divided into driving part and the fixed part of inducer. Driving part can use any one of following two kinds of modes: the manual operation scheme manually running driving part; Machine unit 33 and electronically controlled platform 32 as supervisory control desk and are utilized and control the drive systems such as motor from signal herein, makes it the automatic operation scheme of operation automatically. Can in the following way in fixed part: when adopting manual operation scheme, such as use bulb plunger etc., by the mode of angle of each arbitrarily angled appointment plasma torch 13 of classification formula, such as, can select which of continuous print angular setting with the use of the pressing of screw; Or, when adopting automatic operation scheme, such as, utilize the umber of pulse of motor to carry out the method for continuous print angular setting, such as, arbitrarily angled sensor be set thus the mode at any angle etc. of prescribed fractionated formula by each.
(the 2nd enforcement mode)
Fig. 3 illustrates the concise and to the point figure of the structure being different from the first enforcement mode as the plasma torch 13 of the icp analysis device of the present invention and the structure in optically focused portion 2.
Relative to first enforcement mode formation for, present embodiment makes optically focused portion 2 move on inducer 311a it is thus possible to set with plasma torch 13 formation arbitrarily angled. Functions and effects in present embodiment are same with the first enforcement mode.
In this case, inducer 311a is used for the driving of spectrum part 31, drives in the way of adjusting the position relation with fixed plasma torch 13.
In addition, angle-adjusting mechanism is except the object driven turns into spectrum part 31 from plasma torch 13, identical with the first embodiment.
(the 3rd enforcement mode)
Fig. 4 illustrates the 3rd enforcement mode of the present invention. Any one that can make optically focused portion 2 or plasma torch 13 in first and second enforcement modes is movable, and in contrast, making in present embodiment both can be movable.
At this moment inducer 131b, 311b, taking plasma torch 13 and optically focused portion 2 to when being configured on straight line with putting as benchmark (C-C '), both are arranged on for this horizontal plane any one side, face up and down. Owing to plasma torch 13 and optically focused portion 2 both sides are movable, respective movable range, corresponding to the shape of 1/8 circular arc, can realize the angle of 0 (plasma body occurs axially)��90 degree (positive side surface direction of plasma body) relatively. So, by making both plasma torch 13 and optically focused portion 2 movable and control by angle-adjusting mechanism 4, obtain reducing the movable range of the device of half and the advantage of setting area can be reduced.
At this moment, inducer 131b, 311b drive plasma torch 13 and spectrum part 31 respectively, and respective angle can independently control.
In addition, angle-adjusting mechanism is same with the first embodiment.
As described above, the icp analysis device of the present invention is characterised in that: can with arbitrarily angled setting plasma torch and the optically focused portion getting into the light from this plasma body.
Moreover, the icp analysis device of present embodiment, as shown in enforcement mode, makes plasma torch 13 and ruhmkorff coil 12 even dynamic, and in addition, optically focused portion 2 is illustrated as integral with spectrum part 31, but is not limited thereto.
In addition, in the present embodiment, the situation of optical splitter is shown, but can also functional quality analyser.
In addition, above-mentioned inducer can also be movable track or inductance groove, as long as being the mechanism to configuration state that can change plasma torch and optically focused portion.
In addition, the present invention is not limited to be recorded in the content of embodiments of the present invention, as long as the formation of the effect (making plasma torch and optically focused portion with arbitrarily angled to putting) of the present invention can be met, just belongs to the scope of the technology of the present invention.
Description of reference numerals
1... luminescence of plasma control portion; 2,2a, 2b, 53... optically focused portion; 3... analyzing and processing portion; 4... angle-adjusting mechanism; 11... plasma body; 12,52... ruhmkorff coil; 13,13a, 13b, 51... plasma torch; 14... room is sprayed; 15... atomizer; 18... test portion; 31,31a, 31b... spectrum part; 131a, 131b, 311a, 311b... inducer; 33... machine unit (computer); 54... speculum is fixed; 55... variable mirror; 56... spectrum part.

Claims (4)

1. an icp analysis device, comprising:
Plasma torch, introduces the test portion of plasma body gas and droplet;
Ruhmkorff coil, applies high-frequency voltage to described plasma torch;
Optically focused portion, carries out optically focused to the luminescence from test portion, and this test portion utilizes the plasma body produced by the high-frequency voltage of this ruhmkorff coil to excite, thus luminous;
Analyzing and processing portion, has the spectrum part that the luminescent spectrum to the light after optically focused carries out light splitting; And
Angle-adjusting mechanism, it is characterised in that,
Described angle-adjusting mechanism, is configured to: in order to described plasma torch is adjusted to arbitrarily angled, it is possible to plasma torch and optically focused portion are relatively moved into direction relative to the getting of light of the plasma body in described optically focused portion,
This angle-adjusting mechanism, there is inducer, this inducer drives either one or both in described plasma torch and optically focused portion so that described plasma torch relative to described optically focused portion comprise from plasma body axially to the angle of the range set optimum sensitivity of 0��90 degree of positive side surface direction of plasma body.
2. icp analysis device as claimed in claim 1, plasma torch in wherein said angle-adjusting mechanism and the relative movement in optically focused portion, it is possible to any one or two in described plasma torch and described optically focused portion can be moved rotationally.
3. icp analysis device as claimed in claim 1 or 2, wherein said angle-adjusting mechanism utilizes the control of calculation process machine to drive any one in described plasma torch and described optically focused portion, or plasma torch described in independent drive and described optically focused portion both sides.
4. an analytical procedure for icp analysis device, this icp analysis device is the icp analysis device as according to any one of claim 1 ~ 3, and this analytical procedure comprises:
Operation introduced by the test portion that the test portion of plasma body gas and droplet is introduced plasma torch;
The ruhmkorff coil being located at described plasma torch neighboring is applied high-frequency voltage thus makes the luminescence of plasma operation of luminescence of plasma;
Luminescence from the test portion utilizing this plasma exciatiaon is carried out the optically focused operation of optically focused; And
Light after this optically focused is carried out light splitting thus analyzes the analyzing and processing operation of its luminescent spectrum, it is characterised in that,
In described optically focused operation, taking straight line shape to the state configuring described plasma torch with putting and the luminescence from described test portion being carried out the optically focused portion of optically focused as benchmark, make the getting into direction with arbitrarily angled putting of luminescence of plasma body.
CN201110086370.8A 2010-03-29 2011-03-29 Icp analysis device and analytical procedure thereof Active CN102235977B (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2010-076363 2010-03-29
JP2010076363 2010-03-29
JP2011-023122 2011-02-04
JP2011023122A JP5612502B2 (en) 2010-03-29 2011-02-04 ICP analyzer and analysis method thereof

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CN102235977B true CN102235977B (en) 2016-06-08

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JP6335433B2 (en) * 2013-03-28 2018-05-30 株式会社日立ハイテクサイエンス ICP emission spectrometer
JP2015179039A (en) * 2014-03-19 2015-10-08 株式会社日立ハイテクサイエンス Icp emission spectrophotometer
JP2015184167A (en) * 2014-03-25 2015-10-22 株式会社日立ハイテクサイエンス Icp emission spectrophotometer
US10107759B2 (en) * 2014-12-15 2018-10-23 Spectro Analytical Instruments Gmbh Optical emission spectroscope with a pivotably mounted inductively coupled plasma source
CN107860763B (en) * 2017-10-31 2020-01-03 华中科技大学 Online monitoring method and device for concentration of alkali metal and trace element in gas
CN108037076A (en) * 2017-12-30 2018-05-15 杭州谱育科技发展有限公司 Light path system before inductively-coupled plasma spectrometer

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JP2001165857A (en) * 1999-12-10 2001-06-22 Shimadzu Corp Icp emission spectroscopic analyzer
JP3902380B2 (en) * 2000-05-19 2007-04-04 エスアイアイ・ナノテクノロジー株式会社 ICP analyzer
JP4459462B2 (en) * 2001-02-15 2010-04-28 エスアイアイ・ナノテクノロジー株式会社 Inductively coupled plasma spectrometer
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JP2008275372A (en) * 2007-04-26 2008-11-13 Agilent Technol Inc Plasma analyzer and plasma analysis method

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