CN111579349A - Method for preparing ICP-MS sample by concentration - Google Patents
Method for preparing ICP-MS sample by concentration Download PDFInfo
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- CN111579349A CN111579349A CN202010518378.6A CN202010518378A CN111579349A CN 111579349 A CN111579349 A CN 111579349A CN 202010518378 A CN202010518378 A CN 202010518378A CN 111579349 A CN111579349 A CN 111579349A
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- Prior art keywords
- concentration
- icp
- sample
- pfa
- bottle
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- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 20
- 238000004458 analytical method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012468 concentrated sample Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a concentration preparation method of an ICP-MS sample, which comprises the following steps: s1, providing a cleaned PFA concentration bottle, and putting the PFA concentration bottle into an analytical balance for zeroing; s2, adding the tape test sample into the PFA concentration bottle and weighing to obtain the actual weight T0(ii) a S3, putting the PFA concentration bottle into a concentrator, controlling the temperature to be 170-200 ℃, and concentrating until the water is evaporated to dryness; s4, adding 1% of HNO3 with the same amount, and continuing to concentrate in a concentrator, wherein the heating temperature is 70-90 ℃, and the heating time is 5-30 minutes; s5, weighing again after the concentration to obtain the weight T after the concentration1And obtaining an ICP-MS sample, and testing on a machine.
Description
Technical Field
The invention relates to a chemical sample preparation method, in particular to a concentration preparation method of an ICP-MS sample.
Background
At present, the ICP-MS sample pretreatment is one of important steps of sample analysis and detection, and has important influence on the accuracy of analysis and detection results. Generally, ICP-MS only needs a few minutes to a few tens of minutes to analyze a sample, and sample pretreatment takes a few hours to a few tens of hours. Therefore, the research on the sample pretreatment method and technology has been a great concern for the analysts. Conventional methods for sample treatment include dilution, extraction, and pressure analysis, but these methods are too complicated and take a long time.
Disclosure of Invention
The invention provides a concentration preparation method of an ICP-MS sample, which can effectively solve the problems.
The invention is realized by the following steps:
a method for preparing an ICP-MS sample in a concentration mode comprises the following steps:
s1, providing a cleaned PFA concentration bottle, and putting the PFA concentration bottle into an analytical balance for zeroing;
s2, adding the tape test sample into the PFA concentration bottle and weighing to obtain the actual weight T0；
S3, putting the PFA concentration bottle into a concentrator, controlling the temperature to be 170-200 ℃, and concentrating until the water is evaporated to dryness;
s4, adding 1% of HNO3 with the same amount, and continuing to concentrate in a concentrator, wherein the heating temperature is 70-90 ℃, and the heating time is 5-30 minutes;
s5, weighing again after the concentration to obtain the weight T after the concentration1And obtaining an ICP-MS sample, and testing on a machine.
The invention has the beneficial effects that: compared with other methods in the prior art, the ICP-MS sample concentration preparation method is simple and feasible, consumes short time (2.5-3 hours), and can be used for accurately and quickly preparing the ICP-MS sample; in addition, the ICP-MS sample concentration preparation method provided by the invention also comprises the following steps: the anti-interference performance is high, and the method is suitable for preparing a test sample of a high-oxidizing substance.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of a method for preparing a concentrated sample for ICP-MS, provided by an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, the method for preparing a concentrated ICP-MS sample according to an embodiment of the present invention includes the following steps:
s1, providing a cleaned PFA concentration bottle, and putting the PFA concentration bottle into an analytical balance for zeroing;
s2, adding the tape test sample into the PFA concentration bottle and weighing to obtain the actual weight T0；
S3, putting the PFA concentration bottle into a concentrator, controlling the temperature to be 170-200 ℃, and concentrating until the water is evaporated to dryness, so that possible anti-interference substances can be removed;
s4, adding 1% of HNO3 with the same quantity, and continuing to concentrate in a concentrator, wherein the heating temperature is 70-90 ℃, and the heating time is 5-30 minutes, so that residual metal oxide organic matter ash on the wall pipe can be removed, and the deterioration of PFA materials is avoided;
s5, weighing again after the concentration to obtain the weight T after the concentration1And obtaining an ICP-MS sample, and testing on a machine.
As a further modification, in step S1, the step of washing the PFA concentrate bottle includes:
and adding 5% HNO3 into a PFA concentration bottle, heating to 180 ℃, and heating for 5-30 minutes.
As a further improvement, in step S2, the actual weight T of the test specimen08 to 15 g. In this example, the actual weight T of the test specimen0About 10 g. The test sample is preferably a strongly oxidizing substance.
In a further improvement, in step S3, the temperature is controlled to be 175-185 ℃. In this embodiment, the temperature is controlled to be about 180 ℃.
In a further improvement, in step S4, the heating temperature is 75 to 85 ℃, and the heating time is 10 minutes. In this embodiment, the heating temperature is about 80 ℃, and the heating time is about 10 minutes.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for preparing an ICP-MS sample in a concentration manner is characterized by comprising the following steps:
s1, providing a cleaned PFA concentration bottle, and putting the PFA concentration bottle into an analytical balance for zeroing;
s2, adding the tape test sample into the PFA concentration bottleAnd weighing to obtain the actual weight T0；
S3, putting the PFA concentration bottle into a concentrator, controlling the temperature to be 170-200 ℃, and concentrating until the water is evaporated to dryness;
s4, adding 1% of HNO3 with the same amount, and continuing to concentrate in a concentrator, wherein the heating temperature is 70-90 ℃, and the heating time is 5-30 minutes;
s5, weighing again after the concentration to obtain the weight T after the concentration1And obtaining an ICP-MS sample, and testing on a machine.
2. The method for concentrated preparation of an ICP-MS sample according to claim 1, wherein in step S1, the step of washing the PFA concentrate bottle comprises:
and adding 5% HNO3 into a PFA concentration bottle, heating to 180 ℃, and heating for 5-30 minutes.
3. The concentrated preparation method of an ICP-MS sample according to claim 1, characterized in that, in step S2, the actual weight T of the test sample08 to 15 g.
4. The concentrated preparation method of an ICP-MS sample according to claim 1, characterized in that, in step S3, the temperature is controlled to 175 to 185 ℃.
5. The concentrated preparation method of an ICP-MS sample according to claim 4, characterized in that, in step S3, the temperature is controlled to be 180 ℃.
6. The method for preparing a concentrated ICP-MS sample according to claim 1, wherein in step S4, the heating temperature is 75 to 85 ℃ and the heating time is 10 minutes.
7. The concentrated preparation method of an ICP-MS sample according to claim 6, characterized in that, in step S4, the heating temperature is 80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010518378.6A CN111579349A (en) | 2020-06-09 | 2020-06-09 | Method for preparing ICP-MS sample by concentration |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010518378.6A CN111579349A (en) | 2020-06-09 | 2020-06-09 | Method for preparing ICP-MS sample by concentration |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111579349A true CN111579349A (en) | 2020-08-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010518378.6A Pending CN111579349A (en) | 2020-06-09 | 2020-06-09 | Method for preparing ICP-MS sample by concentration |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1164318A (en) * | 1997-08-27 | 1999-03-05 | Sumitomo Chem Co Ltd | Method for determining element contained in liquid chemical |
| JPH1183704A (en) * | 1997-09-03 | 1999-03-26 | Nec Corp | Pretreatment method for surface analysis of semiconductor substrate and apparatus therefor |
| CN1740091A (en) * | 2004-05-13 | 2006-03-01 | 株式会社东芝 | Analyzing container and method for analyzing very small amount of element |
| CN102519939A (en) * | 2011-11-28 | 2012-06-27 | 沈阳工业大学 | Quantitative analytical method for determining trace cobalt in water by utilizing microwave digestion flame atomic absorption spectrometry (FAAS) method |
| CA2759252A1 (en) * | 2011-06-14 | 2012-12-14 | Korea Basic Science Institute | Analytical method on trace elements of rock sample by acid digestion method with fused glass beads |
| WO2014189123A1 (en) * | 2013-05-24 | 2014-11-27 | 関西電力株式会社 | Sample pre-treatment method for measuring the quantity of toxic elements in agricultural produce samples |
| CN104880341A (en) * | 2014-02-28 | 2015-09-02 | 中国科学院寒区旱区环境与工程研究所 | Sample pre-treatment method for determining total concentration of trace elements in polar ice and snow |
| US20170227517A1 (en) * | 2014-06-20 | 2017-08-10 | Atomic Energy Of Canada Limited / Énergie Atomique Du Canada Limitée | Chemical digestion methods of quantification for water and debris mixtures |
-
2020
- 2020-06-09 CN CN202010518378.6A patent/CN111579349A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1164318A (en) * | 1997-08-27 | 1999-03-05 | Sumitomo Chem Co Ltd | Method for determining element contained in liquid chemical |
| JPH1183704A (en) * | 1997-09-03 | 1999-03-26 | Nec Corp | Pretreatment method for surface analysis of semiconductor substrate and apparatus therefor |
| CN1740091A (en) * | 2004-05-13 | 2006-03-01 | 株式会社东芝 | Analyzing container and method for analyzing very small amount of element |
| CA2759252A1 (en) * | 2011-06-14 | 2012-12-14 | Korea Basic Science Institute | Analytical method on trace elements of rock sample by acid digestion method with fused glass beads |
| CN102519939A (en) * | 2011-11-28 | 2012-06-27 | 沈阳工业大学 | Quantitative analytical method for determining trace cobalt in water by utilizing microwave digestion flame atomic absorption spectrometry (FAAS) method |
| WO2014189123A1 (en) * | 2013-05-24 | 2014-11-27 | 関西電力株式会社 | Sample pre-treatment method for measuring the quantity of toxic elements in agricultural produce samples |
| CN104880341A (en) * | 2014-02-28 | 2015-09-02 | 中国科学院寒区旱区环境与工程研究所 | Sample pre-treatment method for determining total concentration of trace elements in polar ice and snow |
| US20170227517A1 (en) * | 2014-06-20 | 2017-08-10 | Atomic Energy Of Canada Limited / Énergie Atomique Du Canada Limitée | Chemical digestion methods of quantification for water and debris mixtures |
Non-Patent Citations (7)
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|---|
| 《土壤环境监测分析方法》编委会: "《安全风险物质高通量质谱检测技术》", 28 February 2019, 华南理工大学出版社 * |
| 乔胜英 等: "《武汉市湖泊中重金属污染状况》", 《水资源保护》 * |
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| 国家药典委员会: "《中华人民共和国药典四部》", 30 May 2020, 中国医药科技出版社 * |
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Application publication date: 20200825 |