技术领域Technical Field
本发明涉及一种元素分析技术，尤其涉及一种脉冲火花气溶胶直接进样ICP光谱仪器与方法。The invention relates to an element analysis technology, in particular to a pulse spark aerosol direct sampling ICP spectrometer and a method.
背景技术Background technique
电感耦合等离子体原子发射光谱法(ICP-AES)具有检出限低、精密度高、基体效应干扰小、分析线性范围宽、可对元素周期表中的众多元素同时进行测定等优点。但是试样的引入却始终限制着ICP-AES的灵敏度。因此进样方式始终是一个热点问题和极为活跃的研究方向。Inductively coupled plasma atomic emission spectrometry (ICP-AES) has the advantages of low detection limit, high precision, small matrix effect interference, wide analytical linear range, and the ability to simultaneously determine many elements in the periodic table. However, the introduction of samples has always limited the sensitivity of ICP-AES. Therefore, the sampling method has always been a hot issue and an extremely active research direction.
目前，试样引入的方法主要有溶液进样法和固体进样法两种。溶液进样形式最为常见，具体方法是将待测样品以溶液形式经过气动雾化器雾化以后，形成稳定而均匀的气溶胶后送入ICP。这种进样技术的发展已经较为成熟。利用溶液进样法检测物质成分以前，必须先将待测样品制备成清晰透明的溶液，否则易堵塞雾化器。当待测物质为固体样品时，要先利用无机酸将其溶解成溶液，必要时还须借助微波消解系统等装置进行处理。这务必会造成样品的污染与损失。为保证产品的质量常常需要快速准确的分析技术以实时提供产品在生产过程中的信息快速甄别材料中掺杂的物质以及分布信息等。但是，溶液分析方法无法满足上述的分析需求。At present, there are two main methods for sample introduction: solution injection and solid injection. Solution injection is the most common form. The specific method is to atomize the sample to be tested in the form of a solution through a pneumatic nebulizer, and then send it into the ICP to form a stable and uniform aerosol. The development of this injection technology has been relatively mature. Before using the solution injection method to detect the composition of the substance, the sample to be tested must be prepared into a clear and transparent solution, otherwise it is easy to clog the nebulizer. When the substance to be tested is a solid sample, it must first be dissolved into a solution using inorganic acid, and if necessary, it must be processed with the help of a microwave digestion system and other devices. This will inevitably cause contamination and loss of the sample. In order to ensure the quality of the product, fast and accurate analysis technology is often required to provide real-time information on the product during the production process, quickly identify the substances doped in the material and distribution information, etc. However, the solution analysis method cannot meet the above analysis needs.
有鉴于此，特提出本发明。In view of this, the present invention is proposed.
发明内容Summary of the invention
本发明的目的是提供了一种脉冲火花气溶胶直接进样ICP光谱仪器与方法，以解决现有技术中存在的上述技术问题。The purpose of the present invention is to provide a pulse spark aerosol direct sampling ICP spectrometer and method to solve the above technical problems existing in the prior art.
本发明的目的是通过以下技术方案实现的：The objective of the present invention is achieved through the following technical solutions:
本发明的脉冲火花气溶胶直接进样ICP光谱仪器，包括底座、样品台、压条、侧板、载气接口、导电座、绝缘座、放电室、电极、脉冲火花源、三通阀、电感耦合等离子体、光谱仪；The pulse spark aerosol direct sampling ICP spectrometer of the present invention comprises a base, a sample stage, a pressure strip, a side plate, a carrier gas interface, a conductive seat, an insulating seat, a discharge chamber, an electrode, a pulse spark source, a three-way valve, an inductively coupled plasma, and a spectrometer;
所述底座接脉冲火花源的负极，电极接脉冲火花源正极，所述电极嵌入导电座内并与导电座紧密配合，绝缘座位于导电座与底座之间；The base is connected to the negative electrode of the pulse spark source, the electrode is connected to the positive electrode of the pulse spark source, the electrode is embedded in the conductive seat and closely matches the conductive seat, and the insulating seat is located between the conductive seat and the base;
底座、绝缘座与样品台围成放电室，且在样品台中部开有小孔，样品置于样品台上部的小孔处并紧密贴合，使放电室形成密闭空间；The base, the insulating seat and the sample stage form a discharge chamber, and a small hole is opened in the middle of the sample stage. The sample is placed in the small hole on the upper part of the sample stage and fits tightly, so that the discharge chamber forms a closed space;
所述放电室为碗状，其进气口和出气口保持在同一水平线并位于外壳两侧，进气口通过所述三通阀与所述电感耦合等离子体连接，所述电感耦合等离子体与光谱仪连接。The discharge chamber is bowl-shaped, with an air inlet and an air outlet maintained at the same horizontal line and located on both sides of the shell, the air inlet is connected to the inductively coupled plasma through the three-way valve, and the inductively coupled plasma is connected to the spectrometer.
上述述的脉冲火花气溶胶直接进样ICP光谱仪器实现光谱分析的方法，其特征在于：The method for implementing spectral analysis by direct injection of pulse spark aerosol into an ICP spectrometer is characterized by:
脉冲火花烧蚀待测样品，通过改变频率、电流、气流，调节气溶胶颗粒的尺寸使得气溶胶颗粒在ICP中充分离子化，能检测样品中的Mn、Cr、Ni、Ti合金元素及C、P、S元素，定量曲线的线性相关系数R2大于0.99。Pulse spark ablation of the sample to be tested, by changing the frequency, current, airflow, adjusting the size of the aerosol particles so that the aerosol particles are fully ionized in the ICP, can detect the Mn, Cr, Ni, Ti alloy elements and C, P, S elements in the sample, the linear correlation coefficient R2 of the quantitative curve is greater than 0.99.
与现有技术相比，本发明所提供的脉冲火花气溶胶直接进样ICP光谱仪器与方法，采用脉冲火花在氩气环境中烧蚀待测样品生成气溶胶，并由氩气将气溶胶直接导入电感耦合等离子体原子发射光谱(ICP-AES)分析元素，与传统的液体进样法相比火花烧蚀直接进样可以避免常规湿法化学消解过程中存在的操作繁琐、加热蒸酸耗时长、挥发性元素易损失和容易造成污染等缺点，并具有制样过程简单、分析速度快等优点，数据准确度更高。此方法不仅能检测样品中的Mn、Cr、Ni、Ti等合金元素对样品中C、P、S都有很好的检出效果。Compared with the prior art, the pulse spark aerosol direct sampling ICP spectrometer instrument and method provided by the present invention uses pulse spark to ablate the sample to be tested in an argon environment to generate aerosol, and the argon gas directly introduces the aerosol into the inductively coupled plasma atomic emission spectrometer (ICP-AES) to analyze the elements. Compared with the traditional liquid sampling method, the spark ablation direct sampling can avoid the shortcomings of the conventional wet chemical digestion process, such as cumbersome operation, long heating and acid evaporation time, easy loss of volatile elements and easy pollution, and has the advantages of simple sample preparation process, fast analysis speed, and higher data accuracy. This method can not only detect alloy elements such as Mn, Cr, Ni, and Ti in the sample, but also has a good detection effect on C, P, and S in the sample.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本发明实施例提供的脉冲火花气溶胶直接进样ICP光谱仪器结构示意图；FIG1 is a schematic diagram of the structure of a pulsed spark aerosol direct injection ICP spectrometer provided in an embodiment of the present invention;
图2为本发明实施例标钢激发形貌特征图；FIG2 is a graph showing the morphological characteristics of the standard steel excited by the embodiment of the present invention;
图3为本发明实施例气溶胶粒径检测图；FIG3 is a graph showing aerosol particle size detection according to an embodiment of the present invention;
图4为本发明实施例采用火花烧蚀—ICP光谱对标钢样品定量分析C元素的标准曲线。FIG. 4 is a standard curve for quantitative analysis of the C element in a steel sample using spark ablation-ICP spectroscopy in an embodiment of the present invention.
图中：In the figure:
1.底座、2.样品台、3.压块、4.侧板、5.载气接口、6.导电座、7.绝缘座、8.放电室、9.电极、10.脉冲火花源、11.三通阀、12.电感耦合等离子体(ICP)、13.光谱仪、M.固体样品1. Base, 2. Sample stage, 3. Press block, 4. Side plate, 5. Carrier gas interface, 6. Conductive seat, 7. Insulating seat, 8. Discharge chamber, 9. Electrode, 10. Pulse spark source, 11. Three-way valve, 12. Inductively coupled plasma (ICP), 13. Spectrometer, M. Solid sample
具体实施方式Detailed ways
下面结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述；显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例，这并不构成对本发明的限制。基于本发明的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明的保护范围。The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, not all of the embodiments, which does not constitute a limitation of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the protection scope of the present invention.
首先对本文中可能使用的术语进行如下说明：First, the terms that may be used in this article are explained as follows:
术语“和/或”是表示两者任一或两者同时均可实现，例如，X和/或Y表示既包括“X”或“Y”的情况也包括“X和Y”的三种情况。The term “and/or” means that either or both of them can be realized at the same time. For example, X and/or Y means both “X” or “Y” and “X and Y”.
术语“包括”、“包含”、“含有”、“具有”或其它类似语义的描述，应被解释为非排它性的包括。例如：包括某技术特征要素(如原料、组分、成分、载体、剂型、材料、尺寸、零件、部件、机构、装置、步骤、工序、方法、反应条件、加工条件、参数、算法、信号、数据、产品或制品等)，应被解释为不仅包括明确列出的某技术特征要素，还可以包括未明确列出的本领域公知的其它技术特征要素。The terms "include", "comprises", "contains", "has" or other descriptions with similar semantics should be interpreted as non-exclusive inclusion. For example, "including certain technical feature elements (such as raw materials, components, ingredients, carriers, dosage forms, materials, dimensions, parts, components, mechanisms, devices, steps, procedures, methods, reaction conditions, processing conditions, parameters, algorithms, signals, data, products or products, etc.) should be interpreted as including not only certain technical feature elements explicitly listed, but also other technical feature elements known in the art that are not explicitly listed.
术语“由……组成”表示排除任何未明确列出的技术特征要素。若将该术语用于权利要求中，则该术语将使权利要求成为封闭式，使其不包含除明确列出的技术特征要素以外的技术特征要素，但与其相关的常规杂质除外。如果该术语只是出现在权利要求的某子句中，那么其仅限定在该子句中明确列出的要素，其他子句中所记载的要素并不被排除在整体权利要求之外。The term "consisting of..." means excluding any technical feature elements not explicitly listed. If this term is used in a claim, it will make the claim closed, so that it does not contain technical feature elements other than the technical feature elements explicitly listed, except for the conventional impurities related to them. If this term only appears in a clause of a claim, it only limits the elements explicitly listed in the clause, and the elements recorded in other clauses are not excluded from the overall claim.
除另有明确的规定或限定外，术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解，例如：可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以根据具体情况理解上述术语在本文中的具体含义。Unless otherwise specified or limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example: it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in this article can be understood according to specific circumstances.
术语“中心”、“纵向”、“横向”、“长度”、“宽度”、“厚度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”“内”、“外”、“顺时针”、“逆时针”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述和简化描述，而不是明示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本文的限制。The orientation or position relationship indicated by terms such as "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", etc. are based on the orientation or position relationship shown in the drawings and are only for the convenience and simplification of description, and do not explicitly or implicitly indicate that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore should not be understood as a limitation of this document.
本发明实施例中未作详细描述的内容属于本领域专业技术人员公知的现有技术。本发明实施例中未注明具体条件者，按照本领域常规条件或制造商建议的条件进行。本发明实施例中所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。The contents not described in detail in the examples of the present invention belong to the prior art known to professionals in the field. If no specific conditions are specified in the examples of the present invention, the conditions are carried out according to the conventional conditions in the field or the conditions recommended by the manufacturer. If the manufacturers of the reagents or instruments used in the examples of the present invention are not specified, they are all conventional products that can be purchased commercially.
本发明的脉冲火花气溶胶直接进样ICP光谱仪器，包括底座、样品台、压条、侧板、载气接口、导电座、绝缘座、放电室、电极、脉冲火花源、三通阀、电感耦合等离子体、光谱仪；The pulse spark aerosol direct sampling ICP spectrometer of the present invention comprises a base, a sample stage, a pressure strip, a side plate, a carrier gas interface, a conductive seat, an insulating seat, a discharge chamber, an electrode, a pulse spark source, a three-way valve, an inductively coupled plasma, and a spectrometer;
所述底座接脉冲火花源的负极，电极接脉冲火花源正极，所述电极嵌入导电座内并与导电座紧密配合，绝缘座位于导电座与底座之间；The base is connected to the negative electrode of the pulse spark source, the electrode is connected to the positive electrode of the pulse spark source, the electrode is embedded in the conductive seat and closely matches the conductive seat, and the insulating seat is located between the conductive seat and the base;
底座、绝缘座与样品台围成放电室，且在样品台中部开有小孔，样品置于样品台上部的小孔处并紧密贴合，使放电室形成密闭空间；The base, the insulating seat and the sample stage form a discharge chamber, and a small hole is opened in the middle of the sample stage. The sample is placed in the small hole on the upper part of the sample stage and fits tightly, so that the discharge chamber forms a closed space;
所述放电室为碗状，其进气口和出气口保持在同一水平线并位于外壳两侧，进气口通过所述三通阀与所述电感耦合等离子体连接，所述电感耦合等离子体与光谱仪连接。The discharge chamber is bowl-shaped, with an air inlet and an air outlet maintained at the same horizontal line and located on both sides of the shell, the air inlet is connected to the inductively coupled plasma through the three-way valve, and the inductively coupled plasma is connected to the spectrometer.
所述放电室在进气口4cm处做一个下切30度气路相切于碗底。The discharge chamber is cut 30 degrees downward at 4 cm from the air inlet, and the air path is tangent to the bottom of the bowl.
上述的脉冲火花气溶胶直接进样ICP光谱仪器实现光谱分析的方法，包括：The method for implementing spectral analysis by the pulse spark aerosol direct sampling ICP spectrometer comprises:
脉冲火花烧蚀待测样品，通过改变频率、电流、气流，调节气溶胶颗粒的尺寸使得气溶胶颗粒在ICP中充分离子化，能检测样品中的Mn、Cr、Ni、Ti合金元素及C、P、S元素，定量曲线的线性相关系数R2大于0.99。Pulse spark ablation of the sample to be tested, by changing the frequency, current, airflow, adjusting the size of the aerosol particles so that the aerosol particles are fully ionized in the ICP, can detect the Mn, Cr, Ni, Ti alloy elements and C, P, S elements in the sample, the linear correlation coefficient R2 of the quantitative curve is greater than 0.99.
所述ICP的载气气氛为氩气，所述脉冲火花烧蚀的载气气氛为氩气；The carrier gas atmosphere of the ICP is argon, and the carrier gas atmosphere of the pulse spark ablation is argon;
生成的气溶胶颗粒大小在20nm-200nm或团聚的颗粒簇小于1.5um。The size of the generated aerosol particles is between 20nm and 200nm or the agglomerated particle clusters are less than 1.5um.
所述脉冲火花源采用电感为储能元件，频率为500～1000Hz，放电电流为30A～140A，脉冲放电时长为50us～150us。The pulse spark source uses inductance as an energy storage element, the frequency is 500-1000 Hz, the discharge current is 30A-140A, and the pulse discharge time is 50us-150us.
所述脉冲火花烧蚀氩气载气流量在激发前保持7～10L/Min冲洗火花腔体，进样时脉冲火花烧蚀氩气载气流量在0.5～1L/Min，ICP-AES的载气流量在0.5～1L/Min。The pulse spark ablation argon carrier gas flow rate is maintained at 7-10 L/Min to flush the spark cavity before excitation, the pulse spark ablation argon carrier gas flow rate is 0.5-1 L/Min during sampling, and the carrier gas flow rate of ICP-AES is 0.5-1 L/Min.
所述放电室的出气口连接一个三通阀一分为二，一路保证火花腔体冲洗阶段不吹灭ICP火炬以废气形式排入水中避免污染环境，一路连接ICP，当冲洗阶段结束后打开此通道使得样品气溶胶顺利进样。The gas outlet of the discharge chamber is connected to a three-way valve and divided into two parts. One way ensures that the ICP torch is not blown out during the spark cavity flushing stage and discharged into the water in the form of exhaust gas to avoid polluting the environment. The other way is connected to the ICP. When the flushing stage is completed, this channel is opened to allow the sample aerosol to be smoothly injected.
综上可见，本发明实施例的脉冲火花气溶胶直接进样ICP光谱仪器与方法。属于固体样品元素分析领域。包括底座、样品台、压块、侧板、载气接口、导电座、绝缘座、放电室、电极、脉冲火花源(含控制板和点火板)、三通阀、电感耦合等离子体(ICP)、光谱仪。将待测样品放置于火花激发样品台上。采用脉冲火花在氩气环境中烧蚀待测样品生成气溶胶，并由氩气将气溶胶直接导入电感耦合等离子体原子发射光谱(ICP-AES)分析元素的方法。与传统的液体进样法相比火花烧蚀直接进样可以避免常规湿法化学消解过程中存在的操作繁琐、加热蒸酸耗时长、挥发性元素易损失和容易造成污染等缺点，并具有制样过程简单、分析速度快等优点，数据准确度更高。此方法不仅能检测样品中的Mn、Cr、Ni、Ti等合金元素对样品中C、P、S都有很好的检出效果，From the above, it can be seen that the pulse spark aerosol direct sampling ICP spectrometer instrument and method of the embodiment of the present invention belongs to the field of solid sample element analysis. It includes a base, a sample table, a pressing block, a side plate, a carrier gas interface, a conductive seat, an insulating seat, a discharge chamber, an electrode, a pulse spark source (including a control board and an ignition board), a three-way valve, an inductively coupled plasma (ICP), and a spectrometer. The sample to be tested is placed on the spark excitation sample table. A pulse spark is used to ablate the sample to be tested in an argon environment to generate an aerosol, and the argon gas is used to directly introduce the aerosol into the inductively coupled plasma atomic emission spectrometry (ICP-AES) method for element analysis. Compared with the traditional liquid sampling method, spark ablation direct sampling can avoid the shortcomings of conventional wet chemical digestion processes such as cumbersome operation, long heating and acid evaporation time, easy loss of volatile elements and easy pollution, and has the advantages of simple sample preparation process, fast analysis speed, and higher data accuracy. This method can not only detect alloy elements such as Mn, Cr, Ni, Ti in the sample, but also has a good detection effect on C, P, and S in the sample.
为了更加清晰地展现出本发明所提供的技术方案及所产生的技术效果，下面以具体实施例对本发明实施例所提供的进行详细描述。In order to more clearly demonstrate the technical solution and technical effects provided by the present invention, the embodiments of the present invention are described in detail with specific embodiments below.
实施例1Example 1
如图1所示：As shown in Figure 1:
本发明发明实施例包括底座1、样品台2、压块3、侧板4、载气接口5、导电座6、绝缘座7、放电室8、电极9、脉冲火花源10、三通阀11、电感耦合等离子体(ICP)12、光谱仪13、M样品。The embodiment of the present invention includes a base 1, a sample stage 2, a pressing block 3, a side plate 4, a carrier gas interface 5, a conductive seat 6, an insulating seat 7, a discharge chamber 8, an electrode 9, a pulse spark source 10, a three-way valve 11, an inductively coupled plasma (ICP) 12, a spectrometer 13, and an M sample.
脉冲火花源10的正极接导电座6上的正极接口，恒压火花源10负极接底座1上的的负极接口。电极9嵌入导电座6内部并与导电座6紧密配合。绝缘座7位于导电座6和底座1之间，样品M放于样品台2上位于电极9的正上方。载气接口5与电感耦合等离子体(ICP)The positive electrode of the pulse spark source 10 is connected to the positive electrode interface on the conductive seat 6, and the negative electrode of the constant voltage spark source 10 is connected to the negative electrode interface on the base 1. The electrode 9 is embedded in the conductive seat 6 and fits tightly with the conductive seat 6. The insulating seat 7 is located between the conductive seat 6 and the base 1, and the sample M is placed on the sample stage 2 directly above the electrode 9. The carrier gas interface 5 and the inductively coupled plasma (ICP)
12直接相连。利用等离子体激发光源使样品气溶胶进一步电离成离子状态，并由光谱仪13采集光谱强度经计算机进行数据处理来确定元素的含量分析检测。The sample aerosol is further ionized into an ion state by using a plasma excitation light source, and the spectrum intensity is collected by a spectrometer 13 and the data is processed by a computer to determine the content of the element for analysis and detection.
该装置底座接脉冲火花源负极，电极接脉冲火花源正极，电极嵌入导电座内并与导电座紧密配合，绝缘座使用聚氟乙烯制作而成位于导电座和底座之间。The base of the device is connected to the negative electrode of the pulse spark source, the electrode is connected to the positive electrode of the pulse spark source, the electrode is embedded in the conductive seat and closely matched with the conductive seat, and the insulating seat is made of polyvinyl fluoride and is located between the conductive seat and the base.
进气口和出气口保持在同一水平线位于外壳两侧，样品置于电极正上方。并保证样品与样品台紧密贴合使得放电室形成密闭空间。The air inlet and the air outlet are kept at the same level and located on both sides of the shell, and the sample is placed directly above the electrode. It is ensured that the sample fits tightly with the sample stage so that the discharge chamber forms a closed space.
所述放电室为碗状结构，且体积大小在5cm3左右。在进气口4cm处做一个下切30度气路相切于碗底，保证样品气溶胶顺利导入ICP-AES并保证了大颗粒沉积在碗底减少基体干扰。The discharge chamber is a bowl-shaped structure with a volume of about 5 cm3. A 30-degree downward cut gas path is made tangent to the bottom of the bowl at 4 cm from the air inlet to ensure that the sample aerosol is smoothly introduced into the ICP-AES and that large particles are deposited at the bottom of the bowl to reduce matrix interference.
所述脉冲火花源以电感为储能元件其工作状态：频率为500～1000Hz，放电电流为30A～140A，脉冲放电时长为50us～150us。The pulse spark source uses inductance as an energy storage element and its working conditions are: frequency is 500-1000Hz, discharge current is 30A-140A, and pulse discharge duration is 50us-150us.
所述脉冲火花烧蚀氩气载气流量在激发前保持7～10L/Min冲洗火花腔体，进样时脉冲火花烧蚀氩气载气流量在0.5～1L/Min，ICP-AES的载气流量在0.5～1L/Min。The pulse spark ablation argon carrier gas flow rate is maintained at 7-10 L/Min to flush the spark cavity before excitation, the pulse spark ablation argon carrier gas flow rate is 0.5-1 L/Min during sampling, and the carrier gas flow rate of ICP-AES is 0.5-1 L/Min.
所述样品气溶胶通过改变频率、电流、气流等方式，可调节气溶胶颗粒的尺寸使得气溶胶颗粒在ICP中充分离子化。进入ICP源的颗粒尺寸尺寸在20nm-200nm或团聚的颗粒簇小于1.5um。The sample aerosol can adjust the size of aerosol particles by changing frequency, current, airflow, etc. so that the aerosol particles are fully ionized in the ICP. The size of the particles entering the ICP source is 20nm-200nm or the agglomerated particle cluster is less than 1.5um.
本发明的工作流程如下：The workflow of the present invention is as follows:
本次采用的样品为郑州机械研究所研制的中华人民共和国光谱标准样品，型号为JZG201-206B,6块标准样品的元素成分及含量如下图所示。标钢将样品在粒度为60目的氧化铝砂纸上磨制，去除标钢表面氧化物，使得激发面平整光滑。将样品放置在火花样品台上，使得样品激发表面与样品台平面紧密贴合。并用顶针压紧样品，保证放电腔体完全密封。在激发之前提前通入氩气，使载气以10L/Min流量冲洗20s火花腔体并以废气形式排入水中避免污染环境。调节脉冲火花的工作条件，使得火花源频率为500Hz，放电电流为140A，脉冲放电时长为120us，激发时保证载气流速在0.7L/Min的流量。使得产生的样品气溶胶颗粒为200nm完全小于1.5um。使得样品气溶胶顺利导入ICP火炬，并保证中心火炬温度最高使得样品完全离子化。由上述方法简单快捷的将标钢样品快速引入ICP-AES中，减少化学消蚀带来的样品污染。并且对样品中C、P、S、Si、Mn、Cr、Ni、Ti等均有很好的检出效果，定量曲线的线性相关系数R2均大于0.99。如下表：The samples used this time are the spectral standard samples of the People's Republic of China developed by Zhengzhou Mechanical Research Institute, model JZG201-206B. The elemental composition and content of the six standard samples are shown in the figure below. Standard steel grinds the sample on alumina sandpaper with a particle size of 60 mesh to remove the oxide on the surface of the standard steel, so that the excitation surface is flat and smooth. Place the sample on the spark sample table so that the sample excitation surface fits tightly with the sample table plane. And use a thimble to press the sample to ensure that the discharge cavity is completely sealed. Before excitation, argon gas is introduced in advance, so that the carrier gas flushes the spark cavity at a flow rate of 10L/Min for 20s and is discharged into the water in the form of exhaust gas to avoid polluting the environment. Adjust the working conditions of the pulse spark so that the spark source frequency is 500Hz, the discharge current is 140A, the pulse discharge duration is 120us, and the carrier gas flow rate is ensured to be 0.7L/Min during excitation. Make the sample aerosol particles generated 200nm completely less than 1.5um. Make the sample aerosol smoothly introduced into the ICP torch, and ensure that the central torch temperature is the highest so that the sample is completely ionized. The above method can simply and quickly introduce the standard steel sample into ICP-AES, reducing the sample contamination caused by chemical corrosion. It also has a good detection effect on C, P, S, Si, Mn, Cr, Ni, Ti, etc. in the sample, and the linear correlation coefficient R2 of the quantitative curve is greater than 0.99. As shown in the following table:
本发明突出优点在于：The outstanding advantages of the present invention are:
本发明简单快捷的将固体样品快速引入ICP-AES中，减少化学消蚀带来的样品污染。The present invention can simply and quickly introduce solid samples into ICP-AES, thereby reducing sample contamination caused by chemical ablation.
本发明不仅能检测样品中的Mn、Cr、Ni、Ti等合金元素对样品中C、P、S都有很好的检出效果,定量曲线的线性相关系数R2均大于0.99。The present invention can not only detect alloy elements such as Mn, Cr, Ni, Ti and the like in the sample, but also has a good detection effect on C, P and S in the sample, and the linear correlation coefficient R2 of the quantitative curve is greater than 0.99.
该系统简化了放电腔体结构，保证样品气溶胶顺利导入ICP-AES并保证了大颗粒沉积在碗底减少基体干扰。并且能连续稳定放电。The system simplifies the discharge chamber structure, ensures that the sample aerosol is smoothly introduced into the ICP-AES and that large particles are deposited at the bottom of the bowl to reduce matrix interference. It can also discharge continuously and stably.
本方案采用脉冲火花源储能元件为电感储能，能产生更大放电电流，提高对金属样品的烧蚀效率。This solution uses a pulse spark source energy storage element as inductive energy storage, which can generate a larger discharge current and improve the ablation efficiency of metal samples.
本发明可通过改变频率、电流、气流等方式改变气溶胶粒径大小尺寸在20nm-200nm或团聚的颗粒簇小于1.5um。使得气溶胶颗粒在电感耦合等离子体中充分离子化。The present invention can change the aerosol particle size to 20nm-200nm or agglomerated particle clusters to less than 1.5um by changing the frequency, current, airflow, etc., so that the aerosol particles are fully ionized in the inductively coupled plasma.
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。本文背景技术部分公开的信息仅仅旨在加深对本发明的总体背景技术的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域技术人员所公知的现有技术。The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed in the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims. The information disclosed in the background technology section of this article is only intended to deepen the understanding of the overall background technology of the present invention, and should not be regarded as an admission or in any form that the information constitutes prior art known to those skilled in the art.
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| CN202410249093.5ACN118090711A (en) | 2024-03-05 | 2024-03-05 | A pulsed spark aerosol direct sampling ICP spectrometer and method |
| Application Number | Priority Date | Filing Date | Title |
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| CN202410249093.5ACN118090711A (en) | 2024-03-05 | 2024-03-05 | A pulsed spark aerosol direct sampling ICP spectrometer and method |
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| CN (1) | CN118090711A (en) |
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