Liquid sample analysis method, liquid sample analysis program, and liquid sample analysis system

Abstract

Even for a liquid sample in which particle elements forming solid particles partially overlap compound elements forming a compound dissolved in a solution, the present invention quantifies only the solid particles. The present invention involves: measuring the concentration of elements (hereinafter referred to as non-overlapping elements) in the liquid not overlapping particle elements; calculating the concentration of elements (hereinafter referred to as overlapping elements) in the liquid overlapping the particle elements; measuring the total concentration of the overlapping elements and the particle elements included in the liquid sample; and calculating the concentration of the particle elements by subtracting the concentration of the overlapping elements from the total concentration.

Description

Liquid sample analysis method, liquid sample analysis program, and liquid sample analysis system

[0001] The present invention relates to a liquid sample analysis method, a liquid sample analysis program, and a liquid sample analysis system.

[0002] Conventionally, as a device for measuring the concentration of solid particles in a liquid, there is an X-ray fluorescence analyzer that irradiates the liquid with X-rays and detects the fluorescent X-rays generated thereby, as disclosed in Patent Document 1.

[0003] However, there are cases where the components of solid particles and the components of the liquid in which the solid particles are dispersed contain the same components, and the above-mentioned X-ray fluorescence analyzer measures the components of solid particles without distinguishing between them and the components in the liquid that are the same as the components of solid particles, making it difficult to quantify the concentration of solid particles.

[0004] Patent Application No. 2000-241522

[0005] Therefore, the present invention has been made in consideration of the above-mentioned problems, and its main object is to quantify only solid particles in a liquid sample in which particle elements constituting solid particles and elements present in the liquid overlap.

[0006] That is, the liquid sample analysis method according to the present invention is a liquid sample analysis method in which solid particles are dispersed in a liquid, and in which the particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, and is characterized by measuring the concentrations of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements), calculating the concentrations of elements in the liquid that overlap with the particle elements (hereinafter referred to as overlapping elements), measuring the total concentration of the particle elements and the overlapping elements contained in the liquid sample, and calculating the concentration of the particle elements by subtracting the concentration of the overlapping elements from the total concentration.

[0007] This liquid sample analysis method makes it possible to calculate the concentration of particle elements in a liquid sample in which the particle elements constituting the solid particles overlap with some of the liquid elements present in the liquid, thereby making it possible to quantify only the solid particles dispersed in the liquid sample.

[0008] Furthermore, the liquid sample analyzing method according to the present invention preferably includes measuring the particle size distribution of the solid particles contained in the liquid sample, calculating the volume ratio of the solid particles from the particle size distribution of the solid particles, and calculating the number concentration of the solid particles from the concentration of the particle element, the density per unit volume of the solid particles, and the volume ratio. With this configuration, by calculating the number concentration of the solid particles, it is possible to quantify only the solid particles dispersed in the liquid sample.

[0009] If impurities other than the solid particles are contained in a liquid (particle dispersion) in which solid particles are dispersed in a solution, the impurities will become a source of error. Therefore, in the liquid sample analyzing method according to the present invention, it is desirable to separate the particle size distribution of the solid particles from the particle size distribution measurement result of the liquid sample obtained by the particle size distribution measuring device.

[0010] A specific example of measuring the concentration of non-overlapping elements is to measure the ion concentration of the non-overlapping elements, which can be measured using an ion concentration meter, an X-ray fluorescence analyzer, an inductively coupled plasma emission analyzer, or the like.

[0011] As a specific embodiment for measuring the total concentration of particle elements and overlapping elements, it is considered that the total concentration is measured using an X-ray fluorescence analyzer.

[0012] In addition, the liquid sample analysis program of the present invention is a liquid sample analysis program for analyzing a liquid sample in which solid particles are dispersed in a liquid and particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, and is characterized in that the program has a computer equipped with a function for acquiring the concentration of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements), a function for calculating the concentration of elements in the liquid that overlap with the particle elements (hereinafter referred to as overlapping elements), a function for acquiring the total concentration of the particle elements and the overlapping elements contained in the liquid sample, and a function for calculating the concentration of the particle elements by subtracting the concentration of the overlapping elements from the total concentration.

[0013] The liquid sample analysis program may be distributed electronically, or may be recorded on a program recording medium such as a CD, DVD, or flash memory.

[0014] Furthermore, the liquid sample analysis system of the present invention is a liquid sample analysis system for analyzing a liquid sample in which solid particles are dispersed in a liquid and particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, and is characterized by comprising a non-overlapping element concentration measurement unit that measures the concentration of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements), a duplicated element concentration calculation unit that calculates the concentration of elements in the liquid that overlap with the particle elements (hereinafter referred to as duplicated elements), a total concentration calculation unit that measures the total concentration of the particle elements and the duplicated elements contained in the liquid sample, and a particle element concentration calculation unit that calculates the concentration of the particle elements by subtracting the concentration of the duplicated elements from the total concentration.

[0015] According to the present invention as described above, it is possible to quantify only solid particles in a liquid sample in which particle elements constituting solid particles and some of the liquid elements, which are elements present in the liquid, overlap.

[0016] While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments.

[0017] One embodiment of the present invention will now be described with reference to the drawings. For clarity, all of the drawings shown below are drawn in a schematic manner, with appropriate omissions or exaggerations. Identical components are designated by the same reference numerals, and their descriptions will be omitted where appropriate.

[0018] <Configuration of liquid sample analyzing system 100> Liquid sample analyzing system 100 of this embodiment measures the concentration or number of solid particles contained in a liquid sample in which solid particles are dispersed in a liquid, as shown in Figure 1. The concentration or number of solid particles obtained by liquid sample analyzing system 100 can be used to manage the liquid sample.

[0019] Here, as shown in Figure 2, the liquid sample is one in which part of the particle elements that make up the solid particles overlap with part of the compound elements that make up the compounds dissolved in the liquid (liquid elements that are elements present in the liquid).

[0020] In this liquid sample, the solid particles are, for example, copper oxide (CuO), and the solution is, for example, an aqueous solution of copper sulfate (CuSO ４ Specifically, in a liquid sample, the particle element (Cu) constituting the solid particles and the compound (CuSO 4 ) dissolved in the solution can be used. ４ ) overlaps with the compound element (Cu) that constitutes it.

[0021] In the following, the compound element (CuSO ４ In the liquid phase, elements that do not overlap with the particle element (Cu) are called "non-overlapping elements (A)," and in this case, it is sulfur (S). Also, the compound element (CuSO ４ In the liquid sample, an element that overlaps with a particle element (Cu) is called a "duplicate element (B)," which is copper (Cu) in this example. Solid particles are represented as B0 and compound elements as AB. In a liquid sample, a duplicate element does not have three or more sources, and a non-duplicate element does not have any source other than the compound element.

[0022] Specifically, as shown in FIG. 1, the liquid sample analyzing system 100 has the following components (a) to (g).

[0023] (a) Concentration C of non-overlapping element (A) Ａ (b) A non-overlapping element concentration measuring unit 2 for measuring the overlapping element (B) from the mass ratio of the chemical formula of the compound (AB). （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） (c) A particle element (B) contained in the liquid sample. （Ｐａｒｔｉｃｌｅ） ) and overlapping elements of the solution (B （ｓｏｌｖｅｎｔ） ) total concentration C Ｂ（Ａｌｌ） (d) Total concentration C Ｂ（Ａｌｌ） and the concentration of overlapping elements C Ｂ（ｓｏｌｖｅｎｔ） Using the concentration of solid particles (BO) C ＢＯ(e) a particle concentration calculation unit 5 that calculates the particle size distribution of the solid particles (BO) contained in the liquid sample; (f) a particle size distribution measurement unit 6 that calculates the volume ratio V of the solid particles (BO) from the particle size distribution of the solid particles (BO); ＢＯ (g) Concentration C of solid particles (BO) ＢＯ , density per unit volume of solid particles (BO) ρ ＢＯ and the volume ratio V of the solid particles (BO) ＢＯ From the number concentration C of solid particles (BO) Ｎ A number concentration calculation unit 8 calculates the number concentration.

[0024] The overlapping element concentration calculation unit 3, the particle concentration calculation unit 5, the volume ratio calculation unit 7, and the number concentration calculation unit 8 are configured by a calculation device 10.

[0025] The calculation device 10 is configured as a computer having a CPU, memory, an input / output interface, an AD converter, a display device such as a display, etc. The calculation device 10 performs the functions of each of the above-mentioned parts by the CPU and peripheral devices working together based on a liquid sample analysis program stored in the memory.

[0026] The calculation device 10 also receives the concentration C of the non-overlapping element (A) from the non-overlapping element concentration measurement unit 2. Ａ the non-overlapping element concentration acquisition unit 11 that acquires the total concentration C Ｂ（Ａｌｌ） a particle size distribution acquisition unit 13 that acquires the particle size distribution of the solid particles from the particle size distribution measurement unit 6, and the like.

[0027] The calculation device 10 may be configured as a physically integrated computer, or may be configured as physically separate computers. Furthermore, the functions of the calculation device 10 may be provided in a calculation device (not shown) provided in each of the measurement units 2, 4, and 6.

[0028] The non-overlapping element concentration measurement unit 2 measures the ion concentration C of the non-overlapping element (A). ＡThe total concentration measurement unit 4 is configured using, for example, an ion concentration meter, an X-ray fluorescence analyzer, an inductively coupled plasma optical emission analyzer, or the like. The total concentration measurement unit 4 is configured using, for example, an X-ray fluorescence analyzer. The particle size distribution measurement unit 6 is configured using, for example, a laser diffraction / scattering particle size distribution measurement device or a particle size distribution measurement device using a dynamic light scattering method. Liquid samples are often colored, making it difficult to measure the particle size distribution with an image analysis particle size distribution measurement device, but the above two particle size distribution measurement devices make it easy to measure the particle size distribution by, for example, selecting the wavelength of the laser to be irradiated.

[0029] The overlapping element concentration calculation unit 3 calculates the ion concentration C of the non-overlapping element (A) measured by the non-overlapping element concentration measurement unit 2. Ａ and the mass ratio of the chemical formula of the compound (AB), the overlapping element (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） This is to calculate the following.

[0030] Here, copper sulfate solution (CuSO ４ ), the mass ratio of the non-overlapping element (A) in the compound (AB) is k1, and the mass ratio of the overlapping element (B （ｓｏｌｖｅｎｔ） ) is k2. Therefore, the overlap element concentration calculation unit 3 calculates the overlap element (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） Calculate.

[0031]

[0032] The particle concentration calculation unit 5 calculates the total concentration C measured by the total concentration measurement unit 4. Ｂ（Ａｌｌ） From the above, the overlapping element concentration calculated by the overlapping element concentration calculation unit 3 (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） Subtracting this, the concentration of particle element (B) C Ｂ（Ｐａｒｔｉｃｌｅ） Specifically, the particle concentration calculation unit 5 calculates the concentration C of the particle element (B) using the following formula: Ｂ（Ｐａｒｔｉｃｌｅ） Calculate.

[0033]

[0034] In the case of copper oxide (CuO), the particle concentration calculation unit 5 calculates the concentration C of the solid particles (BO) using the mass ratio (k3) of the particle element (M) in the solid particles (BO) according to the following formula: ＢＯ Calculate.

[0035]

[0036] The volume ratio calculation unit 7 calculates the volume ratio V of the solid particles (BO) from the particle size distribution of the solid particles (BO) measured by the particle size distribution measurement unit 6. ＢＯ Calculate.

[0037] Here, the volume ratio calculation unit 7 separates the particle size distribution of the solid particles (BO) from the particle size distribution measurement result obtained from the particle size distribution measurement unit 6. At this time, since the approximate particle size distribution of the solid particles (BO) is known in advance, the particle size distribution of the solid particles (BO) can be separated by peak separation or the like. Note that the volume ratio (V ＢＯ ), it is assumed that the solid particles (BO) are spherical and that the solid particles (BO) are uniformly dispersed in the solution.

[0038] Specifically, the volume ratio calculation unit 7 calculates the volume ratio V of the solid particles (BO) using the following formula: ＢＯ Calculate.

[0039]

[0040] where h is the upper end of the particle size distribution of the solid particles, ll is the lower end of the particle size distribution of the solid particles, and R ＢＯ (i) is the radius of the solid particle, Count ＢＯ (i) shows the particle size distribution measurement results (abundance ratio (%)).

[0041] The number concentration calculation unit 8 calculates the concentration C of solid particles (BO) calculated by the particle concentration calculation unit 5. ＢＯ and the density per unit volume of the solid particles (BO) ρ ＢＯ and the volume ratio V of the solid particles (BO) calculated by the volume ratio calculation unit 7. ＢＯ Therefore, the number concentration of solid particles (BO) C Ｎ The density ρ ＢＯ is calculated in advance.

[0042] Specifically, the number concentration calculation unit 8 calculates the number concentration C of solid particles (BO) using the following formula: Ｎ Calculate.

[0043]

[0044] Furthermore, the number concentration calculation unit 8 calculates the number concentration C Ｎ From this, it is possible to calculate the total number of solid particles (BO) and also to calculate the number distribution by particle size.

[0045] <Liquid Sample Analysis Method> Next, a liquid sample analysis method according to this embodiment will be described with reference to FIG.

[0046] The non-overlapping element concentration measurement unit 2 measures the concentration C of the non-overlapping element (A) in the liquid sample. Ａ is measured (step S1).

[0047] Ion concentration C of non-overlapping element (A) measured by non-overlapping element concentration measurement unit 2 Ａ and the mass ratio of the chemical formula of the compound (AB), the overlapping element (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） (Step S2). Specifically, using the above (Equation 1), the overlapping element (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） Calculate.

[0048] In addition, the total concentration measurement unit 4 measures the particle elements (B （Ｐａｒｔｉｃｌｅ） ) and duplicate elements (B （ｓｏｌｖｅｎｔ） ) total concentration C Ｂ（Ａｌｌ） is measured (step S3).

[0049] The total concentration C measured by the total concentration measurement unit 4 Ｂ（Ａｌｌ） From the above, the overlapping element concentration calculated by the overlapping element concentration calculation unit 3 (B （ｓｏｌｖｅｎｔ） ) concentration C Ｂ（ｓｏｌｖｅｎｔ） Subtracting this, the concentration of particle element (B) C Ｂ（Ｐａｒｔｉｃｌｅ） (Step S4). Specifically, the concentration C of the particle element (B) is calculated using the above-mentioned (Equation 2). Ｂ（Ｐａｒｔｉｃｌｅ） Calculate.

[0050] Then, using the mass ratio (k3) of the particle element (B) in the solid particles (BO) and the above-mentioned (Equation 3), the concentration C of the solid particles (BO) is calculated. ＢＯ is calculated (step S5).

[0051] The particle size distribution of the solid particles (BO) contained in the liquid sample is measured by the particle size distribution measurement unit 6 (step S6). Here, if necessary, the particle size distribution of the solid particles (BO) is separated from the particle size distribution measurement results obtained by the particle size distribution measurement unit 6. At this time, since the approximate particle size distribution of the solid particles (BO) is known in advance, the particle size distribution of the solid particles (BO) can be separated by peak separation or the like.

[0052] The volume ratio V of the solid particles (BO) is calculated from the particle size distribution of the solid particles (BO) measured by the particle size distribution measuring unit 6. ＢＯ (Step S7). Specifically, the volume ratio V of the solid particles (BO) is calculated using the above-mentioned (Equation 4). ＢＯ Calculate.

[0053] The concentration C of solid particles (BO) obtained above ＢＯ and the density per unit volume of the solid particles (BO) ρ ＢＯ and the volume ratio V of the solid particles (BO) ＢＯ Therefore, the number concentration of solid particles (BO) C Ｎ (Step S8). Specifically, the number concentration C is calculated using the above-mentioned (Equation 5). Ｎ Also, calculate the number concentration C Ｎ From the above, the total particle number of the solid particles (BO) can be calculated, and the number distribution by particle size can also be calculated. In addition, the particle size distribution measuring unit 6 can calculate the number concentration of impurities, the particle size distribution of impurities, the total particle number of impurities, or the number distribution by particle size of impurities.

[0054] In the above liquid sample analysis method, the measurement steps S1, S3, and S6 are not limited to the above order and may be performed in any order.Furthermore, the calculation steps accompanying each measurement step are also not limited to the above order and may be performed in any order.

[0055] <Effects of this embodiment> With the liquid sample analyzing system 100 of this embodiment configured as described above, it is possible to calculate the concentration of particle elements in a liquid sample in which the particle elements that make up the solid particles overlap with some of the liquid elements that are present in the liquid, thereby making it possible to quantify only the solid particles dispersed in the liquid sample.

[0056] <Other Embodiments> In the liquid sample of the above-described embodiment, the solid particles are, for example, copper oxide (CuO), and the liquid is, for example, an aqueous solution of copper sulfate (CuSO ４ ), but other combinations are also possible. For example, the solid particles may be iron or iron oxide and the liquid may be an iron chloride solution, or the solid particles may be chromium or chromium oxide and the solution may be a potassium chromate solution. Alternatively, the liquid sample may be a melt such as a plating liquid in which solid particles are dispersed. In this case, the components of the melt itself will contain elements that overlap with the particle elements that make up the solid particles.

[0057] Furthermore, the present invention is applicable to the liquid sample of the above embodiment as long as it is a liquid sample in which solid particles are dispersed in a liquid, and part of the particle elements constituting the solid particles overlap with part of the liquid elements, which are elements present in the liquid.

[0058] In addition, various modifications and combinations of the embodiments may be made as long as they do not go against the spirit of the present invention.

[0059] According to the present invention, even in a liquid sample in which particulate elements constituting solid particles and part of compound elements constituting compounds dissolved in a solution overlap, it is possible to quantify only the solid particles.

[0060] REFERENCE SIGNS LIST 100: Solution analysis system 2: Non-overlapping element concentration measurement section 3: Overlapping element concentration calculation section 4: Total concentration measurement section 5: Particle concentration calculation section 6: Particle size distribution measurement section (particle size distribution measurement device) 7: Volume ratio calculation section 8: Number concentration calculation section 10: Arithmetic device

Claims

1. A liquid sample analysis method for analyzing a liquid sample in which solid particles are dispersed in a liquid, in which particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, the method comprising the steps of: measuring the concentrations of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements); calculating the concentrations of elements in the liquid that overlap with the particle elements (hereinafter referred to as overlapping elements); measuring the total concentration of the particle elements and the overlapping elements contained in the liquid sample; and calculating the concentration of the solid particles using the total concentration and the concentration of the overlapping elements.

2. The liquid sample analyzing method according to claim 1, further comprising the steps of: measuring the particle size distribution of the solid particles contained in the liquid sample; calculating the volume ratio of the solid particles from the particle size distribution of the solid particles; and calculating the number concentration of the solid particles from the concentration of the solid particles, the density per unit volume of the solid particles, and the volume ratio.

3. A liquid sample analyzing method according to claim 2, wherein the particle size distribution of the solid particles is separated from the particle size distribution measurement results of the liquid sample obtained by a particle size distribution measuring device.

4. A liquid sample analyzing method according to claim 1, 2 or 3, wherein the concentrations of the non-overlapping elements are measured as ion concentrations of the non-overlapping elements.

5. A liquid sample analysis method according to claim 1, 2, 3 or 4, wherein the concentration of the total elements is measured using an X-ray fluorescence analyzer.

6. A liquid sample analysis program for analyzing a liquid sample in which solid particles are dispersed in a liquid and in which particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, the liquid sample analysis program providing a computer with the following functions: acquiring the concentration of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements); calculating the concentration of elements in the liquid that overlap with the particle elements (hereinafter referred to as overlapping elements); acquiring the total concentration of the particle elements and the overlapping elements contained in the liquid sample; and calculating the concentration of the solid particles using the concentration of the total elements and the concentration of the overlapping elements.

7. A liquid sample analysis system for analyzing a liquid sample in which solid particles are dispersed in a liquid, in which particle elements constituting the solid particles overlap with some of the liquid elements that are elements present in the liquid, the liquid sample analysis system comprising: a non-overlapping element concentration measurement unit that measures the concentration of elements in the liquid that do not overlap with the particle elements (hereinafter referred to as non-overlapping elements); an overlapping element concentration calculation unit that calculates the concentration of elements in the liquid that overlap with the particle elements (hereinafter referred to as overlapping elements); a total concentration calculation unit that measures the total concentration of the particle elements and the overlapping elements contained in the liquid sample; and a particle element concentration calculation unit that calculates the concentration of the particle element using the total concentration and the concentration of the overlapping elements.

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