CN115639265A - A kind of plasma mass spectrometric determination method of arsenic content in cobalt - Google Patents

A kind of plasma mass spectrometric determination method of arsenic content in cobalt Download PDF

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CN115639265A
CN115639265A CN202110816174.5A CN202110816174A CN115639265A CN 115639265 A CN115639265 A CN 115639265A CN 202110816174 A CN202110816174 A CN 202110816174A CN 115639265 A CN115639265 A CN 115639265A
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cobalt
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solution
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arsenic
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杨利春
杨永明
李歆
葛宁
崔靖
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China North Nuclear Fuel Co Ltd
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Abstract

The invention belongs to the technical field of chemical detection, and particularly relates to a plasma mass spectrometry method for determining arsenic content in cobalt, which comprises the steps of sample treatment, sample dissolving acid selection, solution acidity selection, precipitant dosage selection, precipitation time selection and determination; the method successfully establishes the method for detecting the content of the arsenic impurity element in the cobalt, can accurately determine the content of the arsenic element in the cobalt by using the experimental conditions listed in the invention content to be 0.5-20 mu g/g, solves the determination work of the content of the arsenic impurity element in the cobalt required in the production, and meets the requirement of detecting the content of the arsenic element in the cobalt material. By adopting the method, the linear correlation coefficient of the element to be detected is more than or equal to 0.999, the recovery rate of the added standard is between 94 and 106 percent, and the precision is better than 5 percent. The method is simple, convenient, rapid and accurate to operate and is suitable for analyzing and detecting the cobalt material.

Description

一种钴中砷含量的等离子体质谱测定方法A kind of plasma mass spectrometric determination method of arsenic content in cobalt

技术领域technical field

本发明属于化学检测技术领域,具体涉及一种钴中砷含量的等离子体质谱测定方法。The invention belongs to the technical field of chemical detection, and in particular relates to a plasma mass spectrometry method for determining the content of arsenic in cobalt.

背景技术Background technique

常见的砷含量测定方法主要是原子荧光光谱技术,该技术是专属性很强,成熟度很高的测定方法,已应用到各个行业中砷含量的检测。但国外现在很少采用这种检测技术,而是采用电感耦合等离子体原子发射技术光谱法(ICP-AES)。电感耦合等离子体原子发射技术以其具有的高灵敏度、高准确度、多元素同时测定等特点在各个行业得到了广泛应用,在元素分析领域得到迅速发展,已慢慢取代原子吸收光谱技术(AAS)、原子荧光光谱技术(AFS)和紫外分光光谱技术(UV)等传统元素分析技术成为主要的检测技术。The common determination method of arsenic content is mainly atomic fluorescence spectroscopy, which is a highly specific and mature determination method, and has been applied to the detection of arsenic content in various industries. However, this detection technology is rarely used in foreign countries, but inductively coupled plasma atomic emission spectrometry (ICP-AES). Inductively coupled plasma atomic emission technology has been widely used in various industries due to its high sensitivity, high accuracy, and simultaneous determination of multiple elements. It has developed rapidly in the field of elemental analysis and has gradually replaced atomic absorption spectroscopy (AAS ), atomic fluorescence spectroscopy (AFS) and ultraviolet spectroscopy (UV) and other traditional element analysis techniques have become the main detection techniques.

钴-60放射源项目作为高技术产业项目,国内需求量较大,钴源用钴调节棒组件中砷含量高低,会直接影响组件性能,采用等离子体质谱法检测砷含量,钴基体对其测定有严重干扰,目前国内并未查阅到相关钴中砷含量的检测方法。As a high-tech industrial project, the cobalt-60 radioactive source project has a large domestic demand. The content of arsenic in the cobalt adjustment rod assembly for cobalt source will directly affect the performance of the assembly. The arsenic content is detected by plasma mass spectrometry, and the cobalt matrix is used for its determination There is serious interference. At present, there is no relevant detection method for arsenic content in cobalt in China.

发明内容Contents of the invention

针对以上不足,本发明的目的是提供一种钴中砷含量的等离子体质谱测定方法,采用酸溶,再加入沉淀剂,使砷与钴基体分离,保障了检测结果准确度与稳定性,步骤简便易操作,且精密度高。In view of the above deficiencies, the purpose of the present invention is to provide a plasma mass spectrometry method for the determination of arsenic content in cobalt, which uses acid dissolution and then adds a precipitant to separate the arsenic from the cobalt matrix, ensuring the accuracy and stability of the detection results. It is easy to operate and has high precision.

本发明的技术方案如下:Technical scheme of the present invention is as follows:

一种钴中砷含量的等离子体质谱测定方法,包括步骤一、样品处理,步骤二、溶样酸的选择,步骤三、溶液酸度的选择,步骤四、沉淀剂用量的选择,步骤五、沉淀时间的选择,步骤六、测定;A plasma mass spectrometry method for determining arsenic content in cobalt, comprising step 1, sample treatment, step 2, selection of sample-dissolving acid, step 3, selection of solution acidity, step 4, selection of precipitant dosage, step 5, precipitation The selection of time, step six, measure;

所述步骤二、溶样酸的选择,采用磷酸溶解样品;Said step 2, the selection of sample-dissolving acid, adopts phosphoric acid to dissolve the sample;

步骤四、沉淀剂用量的选择;Step 4, the selection of precipitating agent dosage;

硫化钠溶液用量为1.0~1.5mL;The dosage of sodium sulfide solution is 1.0-1.5mL;

步骤六、测定;采用砷国家标准溶液1000μg/mL按样品检测范围稀释成工作标准溶液。采用铑国家标准溶液1000μg/mL稀释成内标溶液,在电感耦合等离子体质谱仪上依次测定工作标准溶液、空白溶液、试料溶液,测定时持续引入内标溶液,用标准曲线法测定待测元素的含量,单位为纳克每毫升ng/mL。Step 6. Determination: use a national standard solution of arsenic at 1000 μg/mL to dilute into a working standard solution according to the detection range of the sample. Use rhodium national standard solution 1000μg/mL to dilute into an internal standard solution, measure the working standard solution, blank solution, and sample solution sequentially on an inductively coupled plasma mass spectrometer, continuously introduce the internal standard solution during the measurement, and use the standard curve method to determine the The content of the element, in nanograms per milliliter ng/mL.

所述步骤一、样品处理;Described step one, sample processing;

对砷含量在(0.5~20)μg/g范围的钴样品检测;Detection of cobalt samples with arsenic content in the range of (0.5-20) μg/g;

取一份车削状碎屑样品,精确到0.1mg,置于石英烧杯中,加入15~18mL的磷酸溶液,置于电热板上低温加热至完全溶解。Take a sample of turning chips, accurate to 0.1mg, put it in a quartz beaker, add 15-18mL of phosphoric acid solution, place it on an electric heating plate and heat it at low temperature until it is completely dissolved.

所述步骤一、样品处理,待完全溶解后,取下稍冷后,在摇动下加入1.0mL硫化钠溶液,使砷离子完全沉淀,静置3min。The first step is sample treatment. After it is completely dissolved, take it off and cool it slightly, then add 1.0 mL of sodium sulfide solution under shaking to completely precipitate the arsenic ions, and let it stand for 3 minutes.

所述步骤一、样品处理,静置后,用定量滤纸在漏斗上过滤,用去离子水洗涤烧杯3次,将洗涤液一同过滤,再将沉淀洗涤3~4次至粉色消失;The first step, sample processing, after standing still, filter on the funnel with quantitative filter paper, wash the beaker with deionized water 3 times, filter the washing liquid together, and then wash the precipitate 3 to 4 times until the pink color disappears;

弃去滤液,换上100mL容量瓶,加入适量硝酸溶解沉淀,接收液体于容量瓶中,继续用水洗涤滤纸3次,将滤液一并收集,然后用水定容至刻线,摇匀待测;Discard the filtrate, replace it with a 100mL volumetric flask, add an appropriate amount of nitric acid to dissolve the precipitate, receive the liquid in the volumetric flask, continue to wash the filter paper with water for 3 times, collect the filtrate together, then dilute to the mark line with water, shake well for testing;

随同试样作空白实验,作为空白溶液待测。Do a blank experiment together with the sample and serve as a blank solution to be tested.

所述步骤二、溶样酸的选择,磷酸用量选用15~18mL。Said step 2, the selection of sample-dissolving acid, the phosphoric acid consumption is selected as 15-18mL.

所述步骤三、溶液酸度的选择;磷酸溶液浓度为3mol/L。The third step, the choice of solution acidity; the concentration of phosphoric acid solution is 3mol/L.

所述步骤四、沉淀剂用量的选择;Described step 4, the selection of precipitating agent consumption;

硫化钠溶液用量为1.0~1.5mL。The dosage of sodium sulfide solution is 1.0-1.5mL.

步骤四、沉淀剂用量的选择;选用硫化钠的用量为1.0mL。Step 4, the selection of the dosage of precipitating agent; the dosage of sodium sulfide is selected as 1.0mL.

所述步骤五、沉淀时间的选择;The selection of step 5, precipitation time;

硫化钠加入到样品溶液中后,需静置数分钟,以保证溶液中的砷离子完全沉淀,静置2.0min~4.0min时,测定结果趋于稳定。After sodium sulfide is added to the sample solution, it needs to stand for a few minutes to ensure that the arsenic ions in the solution are completely precipitated. After standing for 2.0min to 4.0min, the measurement result tends to be stable.

所述步骤五、沉淀时间的选择;选用沉淀时间为3min。Said step five, the selection of precipitation time; the selection of precipitation time is 3 minutes.

本发明的有益效果在于:The beneficial effects of the present invention are:

成功建立了钴中砷杂质元素含量的检测方法,利用发明内容中列举的实验条件可以精确测定钴中砷元素含量0.5~20μg/g,解决了生产中所需的钴中砷杂质含量测定工作,满足了钴材料中砷含量检测的需求。Successfully established a detection method for the content of arsenic impurity elements in cobalt. Using the experimental conditions listed in the summary of the invention, the content of arsenic elements in cobalt can be accurately determined from 0.5 to 20 μg/g, which solves the determination of arsenic impurity content in cobalt required in production. It meets the demand for detection of arsenic content in cobalt materials.

采用本方法,待测元素线性相关系数≥0.999,加标回收率在94%~106%之间,精密度优于5%。方法操作简便、快速准确,适用于钴材料的分析检测。With this method, the linear correlation coefficient of the elements to be measured is ≥0.999, the standard addition recovery rate is between 94% and 106%, and the precision is better than 5%. The method is simple, fast and accurate, and is suitable for the analysis and detection of cobalt materials.

附图说明Description of drawings

图1为本发明所述的一种钴中砷含量的等离子体质谱测定方法检测流程图。Fig. 1 is a detection flowchart of a plasma mass spectrometry method for determining arsenic content in cobalt according to the present invention.

具体实施方式Detailed ways

下面将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。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention.

基于本发明中的实施例,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,都属于本发明保护的范围。Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

一种钴中砷含量的等离子体质谱测定方法,包括步骤一、样品处理,步骤二、溶样酸的选择,步骤三、溶液酸度的选择,步骤四、沉淀剂用量的选择,步骤五、沉淀时间的选择,步骤六、测定。A plasma mass spectrometry method for determining arsenic content in cobalt, comprising step 1, sample treatment, step 2, selection of sample-dissolving acid, step 3, selection of solution acidity, step 4, selection of precipitant dosage, step 5, precipitation The choice of time, step six, determination.

步骤一、样品处理;Step 1, sample processing;

对砷含量在(0.5~20)μg/g范围的钴样品检测。Detection of cobalt samples with arsenic content in the range of (0.5-20) μg/g.

取一份车削状碎屑样品,精确到0.1mg,置于石英烧杯中,加入15~18mL的磷酸溶液,置于电热板上低温加热至完全溶解。Take a sample of turning chips, accurate to 0.1mg, put it in a quartz beaker, add 15-18mL of phosphoric acid solution, place it on an electric heating plate and heat it at low temperature until it is completely dissolved.

取下稍冷后,在摇动下加入1.0mL硫化钠溶液,使砷离子完全沉淀,并且不会吸附钴基体,达到钴与砷分离的效果,静置3min。After taking it off and cooling slightly, add 1.0mL sodium sulfide solution under shaking to completely precipitate the arsenic ions without adsorbing the cobalt matrix to achieve the effect of separating cobalt and arsenic, and let it stand for 3 minutes.

然后用定量滤纸在漏斗上过滤,用去离子水洗涤烧杯3次,将洗涤液一同过滤,再将沉淀洗涤3~4次至粉色消失。Then use quantitative filter paper to filter on the funnel, wash the beaker 3 times with deionized water, filter the washing liquid together, and wash the precipitate 3 to 4 times until the pink color disappears.

弃去滤液,换上100mL容量瓶,加入适量硝酸溶解沉淀,接收液体于容量瓶中,继续用水洗涤滤纸3次,将滤液一并收集,然后用水定容至刻线,摇匀待测。Discard the filtrate, replace it with a 100mL volumetric flask, add an appropriate amount of nitric acid to dissolve the precipitate, receive the liquid in the volumetric flask, continue to wash the filter paper with water for 3 times, collect the filtrate together, then dilute to the mark with water, and shake well for testing.

随同试样作空白实验,作为空白溶液待测。Do a blank experiment together with the sample and serve as a blank solution to be tested.

步骤二、溶样酸的选择;Step 2, the selection of sample-dissolving acid;

样品溶解常用的酸有硝酸、盐酸、硫酸、磷酸,实验对四种酸分别进行了考察,发现硫化砷沉淀只溶于硝酸,因此溶解样品不能采用硝酸,溶解沉淀时可采用硝酸;使用盐酸时,由于ICP-MS测定使用的载气为高纯氩气,溶样采用盐酸会使Ar+和Cl-结合对砷的测定产生严重干扰;对于硫酸而言,由于样品前处理产生的沉淀需要用滤纸过滤,而硫酸具有极强的氧化性和吸水性,会将滤纸烧穿;采用磷酸时以上三种情况均没有发生,并且可将样品完全溶解,所以方法采用磷酸溶解样品,并对磷酸用量进行考查。The commonly used acids for sample dissolution are nitric acid, hydrochloric acid, sulfuric acid, and phosphoric acid. The experiment investigated the four acids separately, and found that the arsenic sulfide precipitate is only soluble in nitric acid. Therefore, nitric acid cannot be used to dissolve the sample. Nitric acid can be used to dissolve the precipitate; , because the carrier gas used in ICP-MS determination is high-purity argon, the use of hydrochloric acid to dissolve the sample will cause serious interference to the determination of arsenic due to the combination of Ar + and Cl - ; for sulfuric acid, the precipitation due to sample pretreatment needs to be used filter paper, and sulfuric acid has strong oxidizing and water-absorbing properties, which will burn through the filter paper; when phosphoric acid is used, none of the above three situations occurs, and the sample can be completely dissolved, so the method uses phosphoric acid to dissolve the sample, and the amount of phosphoric acid To examine.

磷酸用量小于15mL时,样品溶解不完全,本方法选用15~18mL的磷酸用量。When the amount of phosphoric acid is less than 15mL, the sample will not be completely dissolved. This method uses 15-18mL of phosphoric acid.

步骤三、溶液酸度的选择;Step 3, the selection of solution acidity;

磷酸溶液浓度为3mol/L。The concentration of phosphoric acid solution is 3mol/L.

步骤四、沉淀剂用量的选择;Step 4, the selection of precipitating agent dosage;

硫化钠溶液用量为(1.0~1.5)mL,本方法选用硫化钠的用量为1.0mL即可满足测定需求。The amount of sodium sulfide solution is (1.0-1.5) mL, and the amount of sodium sulfide used in this method is 1.0 mL to meet the determination requirements.

步骤五、沉淀时间的选择;Step 5, the selection of precipitation time;

硫化钠加入到样品溶液中后,需静置数分钟,以保证溶液中的砷离子完全沉淀,静置2.0min~4.0min时,测定结果趋于稳定,证明在静置2.0min时已达到完全沉淀,本方法选用最佳沉淀时间为3min。After sodium sulfide is added to the sample solution, it needs to stand for a few minutes to ensure that the arsenic ions in the solution are completely precipitated. For precipitation, the optimum precipitation time for this method is 3 minutes.

步骤六、测定;Step six, measure;

采用砷国家标准溶液1000μg/mL按样品检测范围稀释成工作标准溶液。采用铑国家标准溶液1000μg/mL稀释成内标溶液。在电感耦合等离子体质谱仪上依次测定工作标准溶液、空白溶液、试料溶液,测定时持续引入内标溶液,用标准曲线法测定待测元素的含量,单位为纳克每毫升ng/mL。Use arsenic national standard solution 1000μg/mL to dilute into working standard solution according to the detection range of the sample. Rhodium national standard solution 1000μg/mL was used to dilute to an internal standard solution. The working standard solution, blank solution, and sample solution were sequentially measured on the inductively coupled plasma mass spectrometer, and the internal standard solution was continuously introduced during the measurement, and the content of the element to be tested was determined by the standard curve method, and the unit was nanogram per milliliter ng/mL.

需要说明的是,在本发明的描述中,术语“第一”、“第二”等仅用于描述目的,而不能理解为指示或暗示相对重要性。此外,在本发明的描述中,除非另有说明,“多个”的含义是指至少两个。It should be noted that, in the description of the present invention, the terms "first", "second" and so on are only used for description purposes, and should not be understood as indicating or implying relative importance. In addition, in the description of the present invention, unless otherwise specified, the meaning of "plurality" means at least two.

在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。In the description of this specification, descriptions referring to the terms "one embodiment", "some embodiments", "example", "specific examples", or "some examples" mean that specific features described in connection with the embodiment or example , structure, material or characteristic is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are exemplary and should not be construed as limiting the present invention, those skilled in the art can make the above-mentioned The embodiments are subject to changes, modifications, substitutions and variations.

本发明公开实施例附图中,只涉及到与本公开实施例涉及到的方法,其他方法可参考通常设计,在不冲突情况下,本发明同一实施例及不同实施例可以相互组合;In the drawings of the disclosed embodiments of the present invention, only the methods related to the disclosed embodiments are involved, other methods can refer to the general design, and the same embodiment and different embodiments of the present invention can be combined with each other if there is no conflict;

以上所述仅为本发明的优选实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within range.

Claims (10)

1.一种钴中砷含量的等离子体质谱测定方法,包括步骤一、样品处理,步骤二、溶样酸的选择,步骤三、溶液酸度的选择,步骤四、沉淀剂用量的选择,步骤五、沉淀时间的选择,步骤六、测定;1. A plasma mass spectrometry method for arsenic content in cobalt, comprising step 1, sample treatment, step 2, the selection of sample-dissolving acid, step 3, the selection of solution acidity, step 4, the selection of precipitant consumption, step 5 , the selection of precipitation time, step six, measure; 其特征在于:It is characterized by: 所述步骤二、溶样酸的选择,采用磷酸溶解样品;Said step 2, the selection of sample-dissolving acid, adopts phosphoric acid to dissolve the sample; 步骤四、沉淀剂用量的选择;Step 4, the selection of precipitating agent dosage; 硫化钠溶液用量为1.0~1.5mL;The dosage of sodium sulfide solution is 1.0-1.5mL; 步骤六、测定;采用砷国家标准溶液1000μg/mL按样品检测范围稀释成工作标准溶液。采用铑国家标准溶液1000μg/mL稀释成内标溶液,在电感耦合等离子体质谱仪上依次测定工作标准溶液、空白溶液、试料溶液,测定时持续引入内标溶液,用标准曲线法测定待测元素的含量,单位为纳克每毫升ng/mL。Step 6. Determination: use a national standard solution of arsenic at 1000 μg/mL to dilute into a working standard solution according to the detection range of the sample. Use rhodium national standard solution 1000μg/mL to dilute into an internal standard solution, measure the working standard solution, blank solution, and sample solution sequentially on an inductively coupled plasma mass spectrometer, continuously introduce the internal standard solution during the measurement, and use the standard curve method to determine the The content of the element, in nanograms per milliliter ng/mL. 2.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤一、样品处理;2. the plasma mass spectrometry method of arsenic content in a kind of cobalt as claimed in claim 1, is characterized in that: described step 1, sample processing; 对砷含量在(0.5~20)μg/g范围的钴样品检测;Detection of cobalt samples with arsenic content in the range of (0.5-20) μg/g; 取一份车削状碎屑样品,精确到0.1mg,置于石英烧杯中,加入15~18mL的磷酸溶液,置于电热板上低温加热至完全溶解。Take a sample of turning chips, accurate to 0.1mg, put it in a quartz beaker, add 15-18mL of phosphoric acid solution, place it on an electric heating plate and heat it at low temperature until it is completely dissolved. 3.如权利要求2所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤一、样品处理,待完全溶解后,取下稍冷后,在摇动下加入1.0mL硫化钠溶液,使砷离子完全沉淀,静置3min。3. the plasma mass spectrometry method of arsenic content in a kind of cobalt as claimed in claim 2, it is characterized in that: described step 1, sample treatment, after dissolving completely, take off after cooling slightly, add 1.0 mL of sodium sulfide solution to completely precipitate the arsenic ions, and let stand for 3 minutes. 4.如权利要求3所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤一、样品处理,静置后,用定量滤纸在漏斗上过滤,用去离子水洗涤烧杯3次,将洗涤液一同过滤,再将沉淀洗涤3~4次至粉色消失;4. the plasma mass spectrometry method of arsenic content in a kind of cobalt as claimed in claim 3, it is characterized in that: described step 1, sample processing, after leaving standstill, filter on funnel with quantitative filter paper, use deionized water Wash the beaker 3 times, filter the washing solution together, and then wash the precipitate 3 to 4 times until the pink color disappears; 弃去滤液,换上100mL容量瓶,加入适量硝酸溶解沉淀,接收液体于容量瓶中,继续用水洗涤滤纸3次,将滤液一并收集,然后用水定容至刻线,摇匀待测;Discard the filtrate, replace it with a 100mL volumetric flask, add an appropriate amount of nitric acid to dissolve the precipitate, receive the liquid in the volumetric flask, continue to wash the filter paper with water for 3 times, collect the filtrate together, then dilute to the mark line with water, shake well for testing; 随同试样作空白实验,作为空白溶液待测。Do a blank experiment together with the sample and serve as a blank solution to be tested. 5.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤二、溶样酸的选择,磷酸用量选用15~18mL。5. A plasma mass spectrometry method for determining arsenic content in cobalt as claimed in claim 1, characterized in that: said step 2, the selection of sample-dissolving acid, the phosphoric acid dosage is selected from 15 to 18 mL. 6.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤三、溶液酸度的选择;磷酸溶液浓度为3mol/L。6. The plasma mass spectrometry method for determining arsenic content in a kind of cobalt as claimed in claim 1, characterized in that: said step 3, the selection of solution acidity; the concentration of phosphoric acid solution is 3mol/L. 7.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤四、沉淀剂用量的选择;7. the plasma mass spectrometry method of arsenic content in a kind of cobalt as claimed in claim 1, is characterized in that: described step 4, the selection of precipitating agent consumption; 硫化钠溶液用量为1.0~1.5mL。The dosage of sodium sulfide solution is 1.0-1.5mL. 8.如权利要求7所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤四、沉淀剂用量的选择;选用硫化钠的用量为1.0mL。8. The plasma mass spectrometry method for determining arsenic content in a kind of cobalt as claimed in claim 7, characterized in that: said step 4, the selection of the dosage of precipitant; the dosage of sodium sulfide is 1.0mL. 9.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤五、沉淀时间的选择;9. the plasma mass spectrometry method of arsenic content in a kind of cobalt as claimed in claim 1, is characterized in that: described step 5, the selection of precipitation time; 硫化钠加入到样品溶液中后,需静置数分钟,以保证溶液中的砷离子完全沉淀,静置2.0min~4.0min时,测定结果趋于稳定。After sodium sulfide is added to the sample solution, it needs to stand for a few minutes to ensure that the arsenic ions in the solution are completely precipitated. After standing for 2.0min to 4.0min, the measurement result tends to be stable. 10.如权利要求1所述的一种钴中砷含量的等离子体质谱测定方法,其特征在于:所述步骤五、沉淀时间的选择;选用沉淀时间为3min。10. The method for determining arsenic content in cobalt by plasma mass spectrometry as claimed in claim 1, characterized in that: said step 5, the selection of the precipitation time; the precipitation time is 3 minutes.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2477326C2 (en) * 2011-04-25 2013-03-10 Учреждение Российской академии наук Тувинский институт комплексного освоения природных ресурсов СО РАН (ТувИКОПР СО РАН) Method for removing arsenic from cobalt production waste
CN105548330A (en) * 2015-12-04 2016-05-04 内蒙古包钢钢联股份有限公司 Determination method for content of arsenic, tin and zinc in steel
CN107340280A (en) * 2017-09-15 2017-11-10 赣州华兴钨制品有限公司 The method of arsenic in AFS DETERMINATION sodium tungstate solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2477326C2 (en) * 2011-04-25 2013-03-10 Учреждение Российской академии наук Тувинский институт комплексного освоения природных ресурсов СО РАН (ТувИКОПР СО РАН) Method for removing arsenic from cobalt production waste
CN105548330A (en) * 2015-12-04 2016-05-04 内蒙古包钢钢联股份有限公司 Determination method for content of arsenic, tin and zinc in steel
CN107340280A (en) * 2017-09-15 2017-11-10 赣州华兴钨制品有限公司 The method of arsenic in AFS DETERMINATION sodium tungstate solution

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
谢昊;郭持皓;王含渊;: "钴溶液硫化沉淀法除砷的热力学研究", 《中国有色冶金》, no. 6, 31 December 2013 (2013-12-31), pages 64 - 66 *
陈永欣 等: "氢氧化铁和氢氧化镧共沉淀分离电感耦合等离子体原子发射光谱法测定铜精矿中铅砷锑铋", 《冶金分析》, vol. 29, no. 5, 31 December 2009 (2009-12-31), pages 41 - 44 *

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