CN102279219A - Inductively coupled plasma mass spectrometry method - Google Patents
Inductively coupled plasma mass spectrometry method Download PDFInfo
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- CN102279219A CN102279219A CN201110176492A CN201110176492A CN102279219A CN 102279219 A CN102279219 A CN 102279219A CN 201110176492 A CN201110176492 A CN 201110176492A CN 201110176492 A CN201110176492 A CN 201110176492A CN 102279219 A CN102279219 A CN 102279219A
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Abstract
The invention provides an inductively coupled plasma mass spectrometry and data analysis method. The inductively coupled plasma mass spectrometry and data analysis method is used for testing the concentration of ions to be tested, and comprises the following steps of: selecting polyatomic ions which are formed by combining the ions to be tested with other elements, instead of the ions to be tested, as test objects; manufacturing a standard curve by a standard addition method instead of an external standard method so as to eliminate other interference; and for the test of a standard product, also selecting the polyatomic ions as the test objects so as to process final data.
Description
Technical field
The present invention relates to the trace element field tests, more particularly, the present invention relates to a kind of inductivity coupled plasma mass spectrometry test and data analysing method.
Background technology
Icp ms (ICP-MS) is the delicate of current test elements.Its groundwork principle is to utilize ICP (inductively coupled plasma) with aerosolized fluid sample gasification, atomization ionization more earlier, and then utilize the mass separation system that ion is separated successively, ion separately is impingement of electrons multiplier output electronic signal respectively, just can know the concentration of this element in the sample according to the signal intensity comparison of signal intensity and standard substance.
Wherein, the mass separation system separates according to the mass-charge ratio of ion, like this just can exist a kind of multi-atomic ion to disturb.Such as, test phosphorus P, P
+The mass-charge ratio of ion is 31, and have a lot of N atoms and O atom to combine to be excited then an electronics in ICP, has also formed mass-charge ratio and be a kind of ion of 31.Like this, conventional piece-rate system just can not be separated them, can also think this ion by mistake to be P
+Ion, final detection result will be bigger than normal, and Here it is, and so-called multi-atomic ion disturbs.
Wherein, ICP is formed by Ar gas, adds air residual in the vacuum, own contained H in the fluid sample
2O etc., so as a rule, the concentration of the Ar among the ICP, H, N, O is very high, is far longer than the element that will test.And mutually combine formed multi-atomic ion or above-mentioned atom of above-mentioned atom is bigger with remaining certain atom in conjunction with the interference that formed multi-atomic ion (polyatomic ion) is produced relatively, needs to eliminate.
Prior art generally adopts dual mode to eliminate or reduce multi-atomic ion and disturb.
Method one is the high-resolution mass separation of an employing system, it is separated with a little difference of mass of ion to be measured according to the quality of multi-atomic ion.But this system price costliness, seldom mechanism for testing can bear.
Method two is the mass separation system that adopts conventional resolution, but before the mass separation system, increase a reaction tank, in reaction tank, feed H2 or He, part scientific research institution also once attempted NH3 gas, utilize these gas molecules that the multi-atomic ion bump is made its dispersion and forms independent ion or atom, make it obtain an electronics deionization thereby perhaps react, perhaps utilize these gas molecules and ion collision and form method that kinetic energy discriminates against and reduce this multi-atomic ion and disturb (as shown in Figure 1) with multi-atomic ion.Yet this mechanism is very complicated and can not eliminate the multi-atomic ion interference effectively, and complex operation.
Therefore, hope can propose a kind of technical scheme that can eliminate or avoid multi-atomic ion to treat the interference that test ion produces effectively.
Summary of the invention
One object of the present invention just provides a kind ofly can eliminate or reduce inductivity coupled plasma mass spectrometry test and the data analysing method that multi-atomic ion is treated the interference that test ion produces effectively.
The invention provides a kind of inductivity coupled plasma mass spectrometry test and data analysing method, be used for testing the ion concentration to be measured of solution to be measured, it comprises: select to treat that measured ion combines the multi-atomic ion that forms as tested object with other element, but not employing treats that measured ion itself is as tested object; For example utilize standard addition method but not external standard method is manufactured typical curve to eliminate remaining various interference; Select this multi-atomic ion to handle so that do final data equally for the test of standard items as tested object.
Preferably, in a concrete example, in described inductivity coupled plasma mass spectrometry method of testing, described solution to be measured is hydrofluorite, treats that measured ion is a phosphonium ion.
Inductivity coupled plasma mass spectrometry method of testing of the present invention characterizes object ion concentration by utilizing multi-atomic ion concentration, thereby the strong multi-atomic ion of avoiding existing in the real work disturbs, and measures object ion concentration more accurately than conventional method; And this method is very simple, operation easily, and very strong practical application meaning is arranged.
Description of drawings
In conjunction with the accompanying drawings, and, will more easily more complete understanding be arranged and more easily understand its attendant advantages and feature the present invention by with reference to following detailed, wherein:
Fig. 1 schematically shows the synoptic diagram according to the inductivity coupled plasma mass spectrometry testing apparatus of prior art.
Fig. 2 schematically shows the process flow diagram according to the inductivity coupled plasma mass spectrometry method of testing of the embodiment of the invention.
Need to prove that accompanying drawing is used to illustrate the present invention, and unrestricted the present invention.Notice that the accompanying drawing of expression structure may not be to draw in proportion.And in the accompanying drawing, identical or similar elements indicates identical or similar label.
Embodiment
In order to make content of the present invention clear and understandable more, content of the present invention is described in detail below in conjunction with specific embodiments and the drawings.
Fig. 2 schematically shows the process flow diagram according to the inductivity coupled plasma mass spectrometry method of testing of the embodiment of the invention.
In conjunction with Fig. 1 and Fig. 2, can be used for testing ion concentration to be measured in the solution to be measured according to the inductivity coupled plasma mass spectrometry method of testing of the embodiment of the invention, for example in current specific embodiment, be used for detecting phosphorus (P) ion of diluted hydrofluoric acid DHF.
Inductivity coupled plasma mass spectrometry method of testing according to the embodiment of the invention comprises:
Multi-atomic ion integrating step S1 to be measured in ICP, treats that measured ion combines to form multi-atomic ion to be measured with other element.For example, phosphorus combines formation " P+O " ion with oxygen.
Multi-atomic ion separating step S2 to be measured, specifically, by the mass separation system, the ion that respectively has the different quality charge ratio is separated respectively.
Multi-atomic ion strength detection step S3 to be measured measures the caused electronic signal intensity of separating of multi-atomic ion impingement of electrons multiplier to be measured.
Standard items testing procedure S4, the standard items (element to be measured) of preparation variable concentrations utilize said method to measure each electronic signal intensity respectively, and manufacture typical curve.
Handle calculation procedure S5, being used for per sample, signal intensity and typical curve calculate ion concentration to be measured.
Need to prove, it will be appreciated by persons skilled in the art that standard items testing procedure S4 not necessarily carries out after multi-atomic ion testing procedure S3 to be measured, but can for example before ions binding step S1 to be measured, carry out etc.
From top specific embodiment as can be known, the embodiment of the invention effectively utilizes the multi-atomic ion effect.For example, can there be bigger interference (N+O), this multi-atomic ion that combines not as the test P that in ICP, also can form and O, P and N, P and Ar etc. since directly test the P ion.So just avoided big multi-atomic ion and disturbed (as N+0).Certainly also have new interference and exist, but for the interference of independent P ion, new interference is weakened greatly, and some can also thoroughly be eliminated by other means with respect to " N+O (combination of N atom and O atom) ".
The preferred embodiments of the present invention preferably adopt standard addition method, this is the method for making of a kind of typical curve in the analytical chemistry, its advantage is to add a small amount of high concentration standard items to prepare standard items on the ordinary meaning in a large amount of samples, add so later standard items and sample relatively except that concentration of element height to be measured, other physical property, chemical property can be thought no change.That is the standard items (except that concentration of element to be tested is different) of solution example physical property chemical property basically identical a kind of and to be measured, have been prepared.This is significant in the present invention because the stability of multi-atomic ion combination own is not very strong, so must sample and the physical property chemical property basically identical of standard items just meaningful.Otherwise the very large deviation that can cause the result.
In a word, the present invention can characterize object ion (promptly treating measured ion) (for example P) concentration by the mensuration (for example multi-atomic ion of P and O composition) of utilizing multi-atomic ion, thereby measures object ion concentration more accurately than conventional means.And this method is very simple, operation easily, and very strong practical application meaning is arranged.Particularly at semicon industry, high-purity chemical reagent industry, whether qualified grade has very strong actual application prospect to judge certain chemicals.For apparatus manufacturer, perhaps also can increase this function, not need HardwareUpgring, increase the software function corresponding and just can.
And for whole the present invention, though exemplified above-mentioned element, the present invention is not limited to above-mentioned some specific element.The inventor all obtains good effect by multiple element is tested.
Be understandable that though the present invention with the preferred embodiment disclosure as above, yet the foregoing description is not in order to limit the present invention.For any those of ordinary skill in the art, do not breaking away under the technical solution of the present invention scope situation, all can utilize the technology contents of above-mentioned announcement that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical solution of the present invention, all still belongs in the scope of technical solution of the present invention protection any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (3)
1. inductivity coupled plasma mass spectrometry method of testing, the ion concentration to be measured that is used for testing solution to be measured is characterized in that comprising:
Selection treats that measured ion combines the multi-atomic ion of formation as tested object with other element;
Manufacture typical curve; And
Select this multi-atomic ion to handle so that do final data equally for the test of standard items as tested object.
2. inductivity coupled plasma mass spectrometry method of testing according to claim 1 is characterized in that, selects to treat measured ion combines formation with other element multi-atomic ion as tested object, and does not adopt and treat that measured ion itself is as tested object.
3. inductivity coupled plasma mass spectrometry method of testing according to claim 1 and 2 is characterized in that, utilizes standard addition method but not external standard method is manufactured typical curve.
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| CN201110176492A CN102279219A (en) | 2011-06-28 | 2011-06-28 | Inductively coupled plasma mass spectrometry method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102830155A (en) * | 2012-08-16 | 2012-12-19 | 四川鑫龙碲业科技开发有限责任公司 | Method for determining content of trace impurity element in cadmium telluride |
Citations (4)
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| US20020070338A1 (en) * | 2000-12-08 | 2002-06-13 | Loboda Alexander V. | Ion mobility spectrometer incorporating an ion guide in combination with an MS device |
| JP2004327243A (en) * | 2003-04-24 | 2004-11-18 | Tdk Corp | Inductively coupled plasma mass spectrometer and mass spectrometry method |
| CN1635366A (en) * | 2003-12-26 | 2005-07-06 | 上海贝岭股份有限公司 | Process for detecting phosphorus utilizing low resolution inductively coupled plasma mass spectrograph |
| CN101532929A (en) * | 2009-04-21 | 2009-09-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for clearing and detecting vanadic oxide |
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2011
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020070338A1 (en) * | 2000-12-08 | 2002-06-13 | Loboda Alexander V. | Ion mobility spectrometer incorporating an ion guide in combination with an MS device |
| JP2004327243A (en) * | 2003-04-24 | 2004-11-18 | Tdk Corp | Inductively coupled plasma mass spectrometer and mass spectrometry method |
| CN1635366A (en) * | 2003-12-26 | 2005-07-06 | 上海贝岭股份有限公司 | Process for detecting phosphorus utilizing low resolution inductively coupled plasma mass spectrograph |
| CN101532929A (en) * | 2009-04-21 | 2009-09-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for clearing and detecting vanadic oxide |
Non-Patent Citations (2)
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| 刘世毅等: "电感耦合等离子体质谱法测定钽粉中的磷", 《稀有金属与硬质合金》, vol. 33, no. 4, 31 December 2005 (2005-12-31) * |
| 胡圣虹等: "等离子体质谱法测定地质样品中痕量稀土元素的基体效应及多原子离子干扰的校正研究", 《高等学校化学学报》, vol. 21, no. 3, 31 March 2000 (2000-03-31), pages 368 - 372 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102830155A (en) * | 2012-08-16 | 2012-12-19 | 四川鑫龙碲业科技开发有限责任公司 | Method for determining content of trace impurity element in cadmium telluride |
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Owner name: SHANGHAI HUAHONG GRACE SEMICONDUCTOR MANUFACTURING Free format text: FORMER OWNER: HONGLI SEMICONDUCTOR MANUFACTURE CO LTD, SHANGHAI Effective date: 20140425 |
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