CN105628782A - ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) analysis method - Google Patents
ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) analysis method Download PDFInfo
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Abstract
The invention relates to an ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) analysis method. The ICP-MS analysis method comprises the following steps: (A1) extracting current samples and starting data collection; (A2) judging the stability of signals by virtue of a judging module, wherein the data collection time after the signals are stable is preset quantitative data collection time; (A3) finishing data collection of the current samples. The ICP-MS analysis method has the advantages of continuous data collection, high analysis flux, accurate data and the like.
Description
Technical field
The present invention relates to ultimate analysis field, in particular to the ICP-MS analytical procedure of data continuous acquisition.
Background technology
ICP-MS, taking inductively coupled plasma body as ion source, screens the ion of specific mass-to-charge ratio with mass analyzer, is analyzed by multiple element finally by detector. The influence factor of sample analysis flux comprises: sample wash time, sample extraction time and data acquisition time, in existing ICP-MS sample analysis, sample wash time, sample extraction time and quantitative data acquisition time is set in advance when quantivative approach editor, as shown in Figure 1, within sample wash time and sample extraction time, do not carry out data gathering, no signal response value, in quantitative data acquisition time, only carry out data gathering, therefore there is following defect:
1, there is difference in the signal stabilization time of different sample, sample wash time, sample extraction time and data acquisition time is set in advance, makes to there is error in quantitative analysis process;
2, in order to guarantee accuracy and the reliability of quantitative analytical data, the long time (as sample wash and sample extraction time arrange 1 minute altogether) was set, and data acquisition time usually all at Millisecond to second level, seriously have impact on the analysis throughput of sample; In addition, when sample size is little, the long sample extraction time was set, also easily occurs data also not start to gather, but the situation that sample has consumed.
4, in sample extraction process, sample may be caused not extract smoothly owing to sample hose is not in place, when the default sample extraction time does not also arrive, operator may directly adjust sample hose position and do not re-start sample extraction in order to lazy, thus cause analytical error, fail this kind of violation operation is carried out quality control in existing analytical procedure.
Summary of the invention
In order to the deficiency solved in above-mentioned prior art, the present invention provides data continuous acquisition in a kind of sample analysis process, and sample analysis flux height, analytical data is ICP-MS analytical procedure accurately and reliably.
Data continuous acquisition, analysis throughput height, data are accurate
It is an object of the invention to be achieved through the following technical solutions:
A kind of ICP-MS analytical procedure, described ICP-MS analytical procedure comprises the following steps:
(A1) extract when time sample, start data gathering;
(A2) judging that module judges that signal is stablized, the data acquisition time after signal is stable is default quantitative data acquisition time;
(A3) when secondary sample data collection terminates.
According to above-mentioned ICP-MS analytical procedure, can selection of land, described ICP-MS analytical procedure comprises further: when secondary sample data collection terminates, and repeats (A1) step, enters the data gathering of next sample.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that when the data gathering of secondary sample data collection with next sample carries out continuously, middle uninterrupted.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that described ICP-MS analytical procedure comprises further:
(B1) rinse previous sample, start data gathering;
(B2) judge that module judges to respond without previous sample signal, extract when time sample.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that utilize washing fluid to rinse previous sample.
According to above-mentioned ICP-MS analytical procedure, can selection of land, described washing fluid is pure water and/or salpeter solution.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that described ICP-MS analytical procedure comprises further:
(C1) judge module is according to whether the diversity judgement signal of adjacent signals response value is stablized:
If difference exceeds threshold range, judge that signal is not stablized;
If difference is in threshold range, judge that signal is stablized.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that described ICP-MS analytical procedure comprises further:
(D1) module reception channel A is judged1��A2����AnSignal response value, judge the time point that each channel signal is stable, wherein n is positive integer, and n >=1;
(D2) signal of all passages is stablized, and judges that module judges that signal is stablized.
According to above-mentioned ICP-MS analytical procedure, can selection of land, the data acquisition time after signal is stable is judged by described judgement module.
According to above-mentioned ICP-MS analytical procedure, it may be preferred that judge the terminal that module gathers according to the diversity judgement quantitative data of adjacent signals response value:
If difference is in threshold range, judge that not arriving quantitative data gathers terminal;
If difference exceeds threshold range, it is judged to that quantitative data gathers terminal.
Compared with prior art, the useful effect that the present invention has is:
1, the signal response value in monitor in real time sample handoff procedure of the present invention, realize the data continuous acquisition in sample wash, sample extraction and quantitative data gatherer process, by judging that module judges the time point that signal is stable, ensure quantitative data accurately and reliably, shorten the analysis time of single sample.
2, the present invention is without the need to setting in advance sample wash time and sample extraction time, it is to increase the ratio of quantitative data acquisition time in single sample analysis; Meanwhile, analysis throughput is improved when ensureing that quantitative analysis requires.
3, sample analysis is carried out quality control by the present invention, eliminates the possibility that may bring artificial violation operation because presetting the sample extraction time, and then avoids analytical error.
4, the present invention is directed to the analysis of low dose of sample, adopt and judge that module judges the terminal that quantitative data gathers, carry out data gathering when avoiding there is no sample ions, it is ensured that the accuracy of analytical data.
Accompanying drawing explanation
With reference to accompanying drawing, the disclosure of the present invention will become to be more readily understood. Those skilled in the art it is easily understood that: these accompanying drawings are only for illustrating the technical scheme of the present invention, and and are not intended to protection scope of the present invention be construed as limiting. In figure:
Fig. 1 is the data acquisition time of the ICP-MS analytical procedure of background technology and the schematic diagram of response value relation;
Fig. 2 is the schematic flow sheet of the ICP-MS analytical procedure of the embodiment of the present invention 1;
Fig. 3 is the standard model data acquisition time of the ICP-MS analytical procedure of the embodiment of the present invention 2 and the schematic diagram of response value relation;
Fig. 4 is the sample data acquisition time of the ICP-MS analytical procedure of the embodiment of the present invention 4 and the schematic diagram of response value relation.
Embodiment
Fig. 1-4 and following description describe the present invention optional enforcement mode to instruct how those skilled in the art implement and reproduce the present invention. In order to instruct technical solution of the present invention, simplify or eliminated some conventional aspects. Those skilled in the art should understand that the modification being derived from these enforcement modes or replace will within the scope of the invention. Those skilled in the art should understand that following characteristics can combine the multiple modification forming the present invention in various mode. Thus, the present invention is not limited to following embodiment, and only limits by claim and their jljl such as grade.
Embodiment 1
Fig. 2 schematically illustrates the schematic flow sheet of the ICP-MS analytical procedure of the present embodiment, and as shown in Figure 2, described ICP-MS analytical procedure comprises the following steps:
(A1) extract when time sample, start data gathering;
(A2) judging that module judges that signal is stablized, the data acquisition time after signal is stable is default quantitative data acquisition time;
(A3) when secondary sample data collection terminates.
When there being multiple sample to analyze, setting quantitative data acquisition time in advance when quantivative approach editor, namely the quantitative data acquisition time of each sample immobilizes, and then successively each sample is carried out data collection and analysis, therefore:
Further, when secondary sample data collection terminates, repeat (A1) step, enter the data gathering of next sample. As preferably, when the data gathering of secondary sample data collection with next sample carries out continuously, middle uninterrupted.
In order to avoid the crossed contamination of sample room, therefore:
Further, described ICP-MS analytical procedure also comprises:
(B1) rinse previous sample, start data gathering;
(B2) judge that module judges to respond without previous sample signal, extract when time sample.
Further, utilizing washing fluid to rinse previous sample, described washing fluid can be pure water and/or salpeter solution.
The ICP-MS of different mass analyzer is quite fast to the ion breakneck acceleration of different nucleo plasmic relation, judges that whether institute's image data is stablized by the difference of adjacent signals response value, therefore:
Further, described ICP-MS analytical procedure comprises:
(C1) judge module is according to whether the diversity judgement signal of adjacent signals response value is stablized:
If difference exceeds threshold range, judge that signal is not stablized;
If difference is in threshold range, judge that signal is stablized.
Multielement can be analyzed by ICP-MS simultaneously, when entering sample multielement sample analysis, it is necessary to gathers the signal response value of each element respective channel, therefore:
Further, described ICP-MS analytical procedure also comprises:
(D1) module reception channel A is judged1��A2����AnSignal response value, judge the time point that each channel signal is stable, wherein n is positive integer, and n >=1;
(D2) signal of all passages is stablized, and judges that module judges that signal is stablized.
The benefit of the present embodiment is: the data continuous acquisition realizing whole analysis process, by judging that module judges the time point that signal is stable automatically, without the need to arranging long sample wash time and sample extraction time, while ensureing quantitative data accuracy, shorten sample analysis time, it is to increase analysis throughput.
Embodiment 2
The application examples of the ICP-MS analytical procedure of the embodiment of the present invention 1 in Criterion curve. When adopting external standard method or marker method to carry out full quantitative analysis on ICP-MS instrument, it is necessary to configure the mark liquid of some concentration gradients, the mark liquid of all different concns is analyzed, according to the response value matching Criterion curve of each mark liquid concentration and correspondence thereof. Only concentration is different for each mark liquid, and contained element is all identical, therefore after adopting, a high density mark liquid carries out sample wash as washing fluid.
Fig. 3 schematically illustrates the standard model data acquisition time of the present embodiment and the graph of a relation (eliminating the exception shake of signal during data blank stage and the sample switching that first sample starts extraction but do not arrive in data acquisition components process in figure) of response value, as shown in Figure 3, data continuous acquisition between all standard models, after adopting, a high density mark liquid then eliminates the sample wash time as washing fluid. The step of the ICP-MS analytical procedure of the present embodiment is as follows:
S1. extract when time sample, start data gathering;
S2. module reception channel A is judged1��A2����AnThe signal response value of (n is positive integer, and n >=1), compares the difference of adjacent signals response value in each passage and the threshold value (such as setting threshold value 3%) of setting:
A1In passage, the response value of adjacent signals is ai��ai+1If, the difference (a of adjacent signals response valuei+1-ai)/aiThe threshold value being less than setting is also (ai+1-ai)/ai< 3%, then judge that module judges A1Channel signal is stablized;
Passage A2����AnThe same A of the decision method whether signal is stablized1Passage, does not repeat them here;
The signal of all passages is stablized, and judges that module judges that signal is stablized, starts quantitative data collection, and quantitative data acquisition time sets (such as 30ms) in advance;
S3. when secondary sample data collection terminates, repeat S1 step, enter the data gathering of next sample.
Embodiment 3
The present invention provides a kind of ICP-MS analytical procedure, as different from Example 2, and passage A in described ICP-MS analytical procedure1��A2����AnThe decision method whether (n is positive integer, and n >=1) signal is stablized is different, and in the present embodiment, the difference of adjacent signals response value is the relative standard deviation of one group of adjacent signals response value, is specially:
A1Selected one group (such as 3,5,7,9 etc.) adjacent signals in passage, the response value of described adjacent signals is respectively ai��ai+1����ai+m(m is positive integer, and m >=2), calculate relative standard deviation RSD, if RSD is (ai��ai+1����ai+m) be less than the threshold value of setting, then judge that module judges A1Channel signal is stablized;
Passage A2��AnThe same A of the decision method whether signal is stablized1Passage, does not repeat them here.
Embodiment 4
The application examples of the ICP-MS analytical procedure of the embodiment of the present invention 1. In this application examples, being analyzed by different sample, in extraction when utilizing washing fluid that previous sample is carried out sample wash before time sample, washing fluid is pure water and/or massfraction is the salpeter solution of 2%;
Fig. 4 schematically illustrates the sample data acquisition time of the present embodiment and the graph of a relation (eliminating the exception shake of signal during data blank stage and the sample switching that first sample starts extraction but do not arrive in data acquisition components process in figure) of response value, as shown in Figure 4, data continuous acquisition between all samples, whole analysis process data gathers free of discontinuities, the quantitative data acquisition time of different sample identical (setting in advance), and the sample wash time different from the sample extraction time (determination module judges automatically) of different sample room.
Embodiment 5
The present embodiment also provides a kind of ICP-MS analytical procedure, and as different from Example 1, in the present embodiment, by judging, module judges the data acquisition time after signal is stable.
Utilize and judge that module is to judge the terminal that quantitative data gathers, it is particularly useful for the situation to a small amount of sample analysis, such as precious metal element analysis, still carrying out data gathering when avoiding quantitative data acquisition time to cross length and cause there is no sample ions, thus affecting the accuracy of data.
As preferably, judging the terminal that module gathers according to the diversity judgement quantitative data of adjacent signals response value:
If difference is in threshold range, judge that not arriving quantitative data gathers terminal;
If difference exceeds threshold range, it is judged to that quantitative data gathers terminal.
Concrete decision method is identical with judging the stable mode of signal, does not repeat them here.
Above-mentioned enforcement mode should not be construed as limiting the scope of the invention. The present invention's it is crucial that: whole analysis process data continuous acquisition, and adopt and judge that module judges the stable time point of signal, ensures quantitative data accurately and reliably, shortens the analysis time of single secondary sample, it is to increase sample analysis flux. Without departing from the spirit of the invention, any type of change the present invention made all should fall within protection scope of the present invention.
Claims (10)
1. an ICP-MS analytical procedure, described ICP-MS analytical procedure comprises the following steps:
(A1) extract when time sample, start data gathering;
(A2) judging that module judges that signal is stablized, the data acquisition time after signal is stable is default quantitative data acquisition time;
(A3) when secondary sample data collection terminates.
2. ICP-MS analytical procedure according to claim 1, it is characterised in that: described ICP-MS analytical procedure comprises further:
When secondary sample data collection terminates, repeat (A1) step, enter the data gathering of next sample.
3. ICP-MS analytical procedure according to claim 2, it is characterised in that: when the data gathering of secondary sample data collection with next sample carries out continuously.
4. ICP-MS analytical procedure according to claim 1, it is characterised in that: described ICP-MS analytical procedure comprises further:
(B1) rinse previous sample, start data gathering;
(B2) judge that module judges to respond without previous sample signal, extract when time sample.
5. ICP-MS analytical procedure according to claim 4, it is characterised in that: utilize washing fluid to rinse previous sample.
6. ICP-MS analytical procedure according to claim 5, it is characterised in that: described washing fluid is pure water and/or salpeter solution.
7. ICP-MS analytical procedure according to claim 1, it is characterised in that: described ICP-MS analytical procedure comprises further:
(C1) judge module is according to whether the diversity judgement signal of adjacent signals response value is stablized:
If difference exceeds threshold range, judge that signal is not stablized;
If difference is in threshold range, judge that signal is stablized.
8. ICP-MS analytical procedure according to claim 1, it is characterised in that: described ICP-MS analytical procedure comprises further:
(D1) module reception channel A is judged1��A2����AnSignal response value, judge the time point that each channel signal is stable, wherein n is positive integer, and n >=1;
(D2) signal of all passages is stablized, and judges that module judges that signal is stablized.
9. ICP-MS analytical procedure according to claim 1, it is characterised in that: the data acquisition time after signal is stable is judged by described judgement module.
10. ICP-MS analytical procedure according to claim 9, it is characterised in that: judge the terminal that module gathers according to the diversity judgement quantitative data of adjacent signals response value:
If difference is in threshold range, judge that not arriving quantitative data gathers terminal;
If difference exceeds threshold range, it is judged to that quantitative data gathers terminal.
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101551357A (en) * | 2009-02-26 | 2009-10-07 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
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