Standard impregnated columns for the determination of the concentration of acid or base components in gases and their use

Abstract

To provide a standard impregnated column that can be used in a quantitative determination method that can easily determine the concentration of an acid component or a base component contained in a gas through a simplified operation. [Solution] One embodiment of the present invention is a standard impregnated column for quantifying the concentration of an acid component or a base component in a gas, in which a known amount of acid component is impregnated into an acid component collection column for collecting acid components in the gas, or a known amount of base component is impregnated into a base component collection column for collecting base components in the gas.

Description

[Technical Field]

[0001] The present invention relates to a standard impregnated column for quantifying the concentration of an acid or base component in a gas, and uses thereof, specifically, a kit for quantifying the concentration of an acid or base component in a gas, a method for quantifying the concentration of an acid or base component in a gas, and a method for controlling the cleanliness of an air space. [Background technology]

[0002] In environments where electronic substrates (hereinafter referred to as substrates), such as semiconductor wafers, liquid crystal substrates, and magnetic disks, are manufactured, contaminants, such as acidic substances (acidic components) and basic substances (basic components), in the manufacturing space can adsorb onto the substrates, resulting in reduced product yield and quality. To prevent this, the manufacturing process of such substrates is carried out in a clean room. It is necessary to evaluate the contamination level of the clean room caused by the acidic substances, basic substances, etc., during each manufacturing process, i.e., the cleanliness level, and to manage the cleanliness of the clean room by, for example, removing the cause of contamination if the cleanliness level deteriorates. Furthermore, in recent years, clean rooms have been required to ensure highly clean spaces. Accordingly, there has been a demand for methods for evaluating the contamination level of acidic or basic components, i.e., the cleanliness level, with higher sensitivity. Furthermore, in recent years, there has been a demand for shortening the time required for the evaluation in order to simplify clean room cleanliness management.

[0003] Examples of methods for evaluating the cleanliness level with high sensitivity and in a short time include a method for quantifying contaminants using a gas adsorption column described in Patent Documents 1 and 2, or a liquid-free trap described in Patent Document 3. Here, the contaminants refer to acidic and / or basic components in the air. Specifically, the method for quantifying contaminants involves passing air in a clean room through the gas adsorption column or liquid-free trap to adsorb the contaminants in the air, and then quantifying the amount of the adsorbed contaminants.

[0004] When quantifying trace amounts of acidic and / or basic components in a gas sample, standard solutions containing trace amounts of acidic and / or basic components are typically used, and these standard solutions are prepared by specially trained experts. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Japanese Patent Application Laid-Open No. 2009-14522 [Patent Document 2] International Publication No. 2010 / 067464 [Patent Document 3] Patent No. 6563396 Summary of the Invention [Problem to be solved by the invention]

[0006] As described above, in the conventional quantitative determination methods described above, the work of preparing standard solutions, particularly when highly sensitive quantitative determination is performed, requires the preparation of standard solutions by specially trained experts, which is extremely cumbersome.

[0007] Therefore, an object of the present invention is to provide a method for easily quantifying the concentration of an acid or base component contained in a gas, as well as a standard-loaded column and a kit for use in the method. Another object of the present invention is to provide a method for controlling the cleanliness of a space, which allows a clean space to be easily maintained. [Means for solving the problem]

[0008] In order to achieve the above object, a standard impregnation column according to one embodiment of the present invention is a standard impregnation column for quantifying the concentration of an acid component or a base component in a gas, comprising: The standard impregnation column is a standard impregnation column in which a known amount of acid component is impregnated onto an acid component collection column for collecting acid components in a gas, or a standard impregnation column in which a known amount of base component is impregnated onto a base component collection column for collecting base components in a gas.

[0009] In order to achieve the above object, a quantitative determination kit according to one embodiment of the present invention is a kit for quantifying the concentration of an acid component and / or a base component in a gas, which satisfies one or more of the following (a) and (b): (a) one or more standard impregnation columns impregnated with the known amounts of acid components, and one or more acid component collection columns for collecting acid components in gas; (b) A kit for quantifying the concentration of acid and / or base components in a gas, comprising one or more standard impregnated columns to which known amounts of the base components are impregnated, and one or more base component trapping columns for trapping the base components in the gas.

[0010] In order to achieve the above object, a quantification method according to one embodiment of the present invention is a method for quantifying the concentration of an acid component and / or a base component in a gas using the above quantification kit, comprising: Step A, in which a solvent is passed through the standard-loaded column to elute the known amount of the acid component or the known amount of the base component into the solvent, thereby obtaining an eluate A; Step B1, in which the gas is passed through an acid component collection column for collecting acid components in the gas or a base component collection column for collecting base components in the gas, thereby collecting acid components or base components in the gas; Step B2, after step B1, of passing a solvent through the acid component collection column that has collected the acid components in the gas in step B1 or the base component collection column that has collected the base components in the gas in step B1, thereby eluting the collected acid components or base components into the solvent to obtain an eluate B; and and step C of analyzing the eluate A and the eluate B and comparing the analysis results of the two to quantify the concentration of the acid component or the base component in the gas.

[0011] In order to achieve the above object, a management method according to one embodiment of the present invention includes a quantification step of quantifying the concentration of an acid component or a base component in a gas in a space using the quantification method; This is a method for managing the cleanliness of a space, which includes a step of identifying and eliminating a source of the acid component or base component in the gas inside the space when the concentration of the acid component or base component quantified in the quantification step exceeds a threshold value. [Effects of the Invention]

[0012] According to one aspect of the present invention, there are provided a method for easily quantifying the concentration of an acid or base component contained in a gas, a standard impregnation column that can be used in the method, and a kit for the method. Furthermore, according to another aspect of the present invention, there is provided a method for controlling the cleanliness of a space that can easily ensure a clean space. DETAILED DESCRIPTION OF THE INVENTION

[0013] Although one embodiment of the present invention will be described below, the present invention is not limited to the following embodiments. Various modifications of the present invention are possible within the scope of the claims, and embodiments obtained by appropriately combining the technical means disclosed in different embodiments are also included in the technical scope of the present invention.

[0014] [Embodiment 1: Standard impregnated column] A standard impregnation column according to one embodiment of the present invention (hereinafter also referred to as "this standard impregnation column") is a standard impregnation column for quantifying the concentration of an acid component or a base component in a gas. The standard impregnation column is a standard impregnation column in which a known amount of acid component is impregnated into an acid component collection column for collecting acid components in a gas, or a known amount of base component is impregnated into a base component collection column for collecting base components in a gas. Here, "a known amount of acid component (base component) is impregnated into the acid component collection column (base component collection column)" means "a known amount of acid component (base component) is impregnated into the adsorbent packed in the column constituting the acid component collection column (base component collection column)."

[0015] Examples of the "collection column" described in this specification include "acid component collection column A," "base component collection column A," "collection column A," "acid component collection column B," "base component collection column B," and "collection column B," which will be described later.

[0016] In this specification, among the standard impregnated columns, a standard impregnated column in which a known amount of acid component is impregnated onto an acid component collection column for capturing acid components in a gas is also referred to as an "acid standard impregnated column." An acid standard impregnated column is a standard impregnated column used to quantify the concentration of acid components in a gas. On the other hand, in this specification, among the standard impregnated columns, a standard impregnated column in which a known amount of base component is impregnated onto a base component collection column for capturing base components in a gas is also referred to as a "base standard impregnated column." A base standard impregnated column is a standard impregnated column used to quantify the concentration of base components in a gas.

[0017] Herein, the "acid component collection column for collecting acid components in a gas" that constitutes the acid standard impregnated column is also referred to as "acid component collection column A." Herein, the "base component collection column for collecting base components in a gas" that constitutes the base standard impregnated column is also referred to as "base component collection column A." Herein, acid component collection column A and base component collection column A are collectively referred to simply as "collection column A."

[0018] In this standard impregnation column, a known amount of acid component is impregnated to the acid component collection column A, or a known amount of base component is impregnated to the base component collection column A. When the amount of the known amount of acid component or known amount of base component impregnated to the standard impregnation column is measured using a predetermined method, a predetermined numerical value corresponding to the amount of the known amount of acid component or known amount of base component is obtained as the measurement result. Hereinafter, the obtained predetermined numerical value is referred to as the "standard result." Then, a correspondence relationship between the known amount and the standard result is derived. Hereinafter, the correspondence relationship is also referred to as "correspondence relationship A."

[0019] Here, consider quantifying an unknown amount of acid or base components trapped in an acid component trapping column or base component trapping column separate from trapping column A by the same method as used to derive the correspondence relationship. In this case, a numerical value corresponding to the unknown amount is obtained.

[0020] Herein, an acid component collection column for collecting acid components in a gas, separate from acid component collection column A, is also referred to as "acid component collection column B." Herein, a base component collection column for collecting base components in a gas, separate from base component collection column A, is also referred to as "base component collection column B." Herein, acid component collection column B and base component collection column B are collectively referred to simply as "collection column B." In addition, herein, when quantifying an unknown amount of acid or base component collected in the aforementioned collection column B, the correspondence relationship between the unknown amount and the obtained numerical value corresponding to the unknown amount is also referred to as "correspondence relationship B."

[0021] Here, when measuring the amount of acid or base components trapped in a column such as the standard impregnation column or collection column B, an eluate containing almost the entire amount of the trapped acid or base components is typically prepared and analyzed. Here, "almost the entire amount" means that the amount of acid or base component remaining after elution is negligible at the time of quantification. The analysis then yields a value corresponding to almost the entire amount of the trapped acid or base component. Therefore, both Correspondence Relationship A and Correspondence Relationship B can be considered to be values ​​corresponding to almost the entire amount of the trapped acid or base component, measured by the same method using an eluate containing almost the entire amount of the trapped acid or base component. Therefore, Correspondence Relationship A and Correspondence Relationship B can be considered to be sufficiently identical.

[0022] Here, for example, the known quantity is α1, the numerical value that is the standard result is β1, the unknown quantity is α2, and the numerical value corresponding to the unknown quantity is β2. In this case, correspondence relationship A is "α1 / β1", correspondence relationship B is "α2 / β2", and it can be considered that "α1 / β1 = α2 / β2". In this case, the relational equation "α2 = β2 × (α1 / β1)" is obtained. For example, if the volume of gas supplied to collection column B when the measurement result of α2 is obtained is V, the concentration of the acid component or base component in the gas can be considered as "α2 / V".

[0023] As described above, by using this standard impregnation column, the amount and concentration of the acid component or base component trapped in the trapping column B can be calculated.

[0024] The predetermined method may include, for example, preparing an eluate containing the eluted acid or base component, and quantifying the acid or base component in the eluate using a known method. The known method is not particularly limited and may be, for example, liquid chromatography. Examples of the liquid chromatography include anion exchange and cation exchange methods using an ion exchange column, and suppressor ion chromatography using a suppressor. Furthermore, when the eluate is prepared and the acid or base component in the eluate is quantified by liquid chromatography, the resulting value may be the peak area. Furthermore, the method for preparing the eluate may include, for example, passing a solvent through a standard-loaded column to elute the acid or base component captured on the standard-loaded column into the solvent, thereby preparing the eluate.

[0025] (Columns for collecting acid components, columns for collecting base components) This standard impregnation column includes a collection column A. In one embodiment of the present invention, the configuration of the collection column A is not particularly limited as long as it can collect a known amount of an acid component or a base component, or an acid component or a base component in a gas.

[0026] Consider the case where the concentration of an acid or base component in a gas is quantified using the standard impregnated column and collection column B. If the configurations of collection columns A and B included in the standard impregnated column are similar, the difference in the amount of acid or base component remaining in the standard impregnated column and collection column B after elution of the acid or base component will be small. This will improve the identity of correspondence relationship A and correspondence relationship B, and improve the accuracy of the quantification. For this reason, in the quantification, collection columns A and B preferably have similar configurations, and more preferably have identical configurations.

[0027] In particular, when the amount of acid or base component captured in collection column B is extremely small, the influence of the remaining acid or base component becomes relatively large. Therefore, when quantifying extremely small amounts of acid or base components, i.e., when performing highly sensitive quantification, it is particularly preferable that collection column A and collection column B included in this standard impregnation column have the same configuration.

[0028] Here, collection column A and collection column B having the same configuration may mean, for example, that both collection column A and collection column B are equipped with adsorbent A, which will be described later. Furthermore, collection column A and collection column B having the same configuration may mean, for example, that both collection column A and collection column B are equipped with adsorbent A, and that the types and contents of the non-porous substrate and the basic adsorbent or acidic adsorbent, which will be described later, as well as the size, pore volume, etc., are the same.

[0029] In view of the above, it is preferable that the collection column A included in this standard attachment column has the same configuration as that of collection column B, specifically, the same configuration as the preferred configuration listed in the section (collection column B) of [Embodiment 2: Quantitative kit] described below.

[0030] (acid component, base component) This standard impregnated column contains a known amount of an acid component or a base component. In this standard impregnated column, the acid component or the base component is impregnated onto collection column A. The acid component or the base component in this standard impregnated column is not particularly limited as long as it is an acid component or a base component that can be impregnated onto collection column A.

[0031] In one embodiment of the present invention, the acid component is not particularly limited. Examples of the acid component include acids such as hydrogen chloride, nitric acid, sulfuric acid, phosphoric acid, hydrofluoric acid, formic acid, acetic acid, bromic acid, iodine, lactic acid, propionic acid, butyric acid, and valeric acid, as well as ammonium fluoride, ammonium formate, and ammonium acetate. In addition, in one embodiment of the present invention, the base component is not particularly limited. Examples of the base component include bases such as ammonia, trimethylamine, triethylamine, alkanolamine, dimethylamine, and diethylamine, as well as ammonium fluoride, ammonium formate, and ammonium acetate.

[0032] The standard impregnated column is prepared by impregnating a known amount of the acid component or a known amount of the base component to collection column A. In one embodiment of the present invention, the method for impregnating a known amount of the acid component or a predetermined amount of the base component to collection column A is not particularly limited, and examples thereof include a standard solution addition method.

[0033] The known amount is not particularly limited as long as it is equal to or less than the limit amount that can be collected by collection column A and is an amount that allows the above-mentioned correspondence to be obtained from the standard impregnated column.

[0034] When the collection column A is equipped with adsorbent A, the limit amount that can be collected by the collection column A depends on the amount (equivalent) of the basic adsorbent or acidic adsorbent held by the adsorbent A, and the limit value increases as the equivalent amount increases. Therefore, when the collection column A is equipped with adsorbent A, the limit value can be controlled by adjusting the equivalent amount of the basic adsorbent or the acidic adsorbent held by the adsorbent A.

[0035] Furthermore, from the viewpoint of the accuracy of the quantitative determination method using the present standard-loaded column, it is preferable that the known amount is close to (e.g., on the same order of magnitude as) the predicted amount of the acid component or base component to be trapped on trapping column B in the quantitative determination method using the present standard-loaded column, because in this case, the identity between correspondence relationship A and correspondence relationship B is improved.

[0036] Specifically, the known amount is not particularly limited, but is preferably more than 1 ng, more preferably 5 ng or more, and even more preferably 10 ng or more. When the purpose of the quantification method is to quantify a trace amount of an acid component or a trace amount of a base component in a gas, from the viewpoint of the accuracy of the quantification method, the known amount may be preferably 1000 μg or less, more preferably 100 μg or less, and even more preferably 10 μg or less.

[0037] In addition, from the viewpoint of the accuracy of the quantification method, it is preferable that the type of the acid component or base component in the standard impregnated column be the same as the type of the acid component or base component expected to be trapped in trapping column B in the quantification method. For example, if it is expected that the quantification method will trap ammonia in gas in trapping column B and quantify its concentration, it is preferable to use ammonia (ammonium ion) as the base component in the standard impregnated column.

[0038] [Embodiment 2: Quantitation kit] A quantitative kit according to one embodiment of the present invention (hereinafter also referred to as "the quantitative kit") is a kit for quantifying acid and / or base components in a gas, which includes one or more standard-loaded columns to which known amounts of acid components are loaded and one or more acid component-collecting columns for capturing acid components in the gas, and / or one or more standard-loaded columns to which known amounts of base components are loaded and one or more base component-collecting columns for capturing base components in the gas.

[0039] In essence, this quantification kit is a quantification kit comprising a combination of one or more of the present standard-loaded columns and one or more collection columns B. Here, the method for quantifying acid or base components in a gas using the present standard-loaded columns is, more specifically, a method for quantifying acid or base components in a gas using the present standard-loaded columns and collection columns B. Therefore, the method for quantifying acid or base components in a gas using the present standard-loaded columns can also be considered as a method for quantifying acid or base components in a gas using the present quantification kit. As described above, the method for quantifying acid or base components in a gas using the present standard-loaded columns can easily quantify the concentrations of acid or base components contained in a gas. Therefore, the present quantification kit allows for the implementation of a quantification method that can easily quantify the concentrations of acid or base components contained in a gas through simplified procedures.

[0040] (Standard column) Regarding the configuration of the standard impregnated column constituting the present quantification kit, the description of the configuration of the standard impregnated column in the above [Embodiment 1: Standard impregnated column] can be used.

[0041] (Collection column B) Like the collection column A, the collection column B is not particularly limited as long as it can collect acidic or basic components in the gas. For reasons described below, the collection column B is preferably filled with a non-porous substrate that holds a basic adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing basic components. Hereinafter, the non-porous substrate that holds a basic adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing basic components will also be referred to simply as "adsorbent A."

[0042] The non-porous substrate has a weak adsorption force for the substance to be adsorbed, and even when adsorbing a very small amount of substance, the adsorbed substance can be easily desorbed into the solvent. Therefore, in a quantification method using a collection column equipped with the adsorbent A, by reducing the amount of acid or base components remaining in the collection column after elution, a value more appropriately corresponding to the total amount of acid or base components captured can be obtained. Therefore, it is preferable that the collection column B, particularly the collection column B constituting the present quantification kit used for quantifying very small amounts of acid or base components, be filled with the non-porous substrate. In this case, the accuracy of the quantification of acid or base components in gas using the present quantification kit can be improved.

[0043] Furthermore, the collection column containing the adsorbent A is packed with a non-porous substrate, and the other substances are not incorporated into the non-porous substrate. Therefore, the presence of the other substances can be prevented from becoming noise in the quantification of acid or base components in gas using this quantitative determination kit, thereby preventing a decrease in the accuracy of the quantification.

[0044] As described above, when the collection column B is a collection column equipped with the adsorbent A, the accuracy of the quantification of the acid or base component in the gas using this quantification kit can be improved. Furthermore, in the quantification, the acid or base component in the gas can be collected and quantified with high sensitivity. In this specification, the term "collecting and quantifying with high sensitivity" means, for example, measuring the concentration of the acid or base component in the gas at a level of about 10 -2 μg / m 3 In other words, when the collection column B is a collection column equipped with the adsorbent A, trace amounts of acid components or base components can be collected and quantified by quantifying the acid components or base components in a gas using this quantification kit.

[0045] Therefore, when collection column B is a collection column equipped with adsorbent A, the use of this quantification kit allows for easy and highly accurate quantification of acid or base components in gas through simplified operations. Also, when collection column B is a collection column equipped with adsorbent A, the use of this quantification kit allows for easy quantification of trace amounts of acid or base components in gas.

[0046] Hereinafter, assuming that the collection column B is a collection column equipped with the adsorbent A, the detailed configuration thereof will be described.

[0047] The non-porous substrate may be of any material, as long as it has no pores. Examples of the material for the non-porous substrate include quartz, glass, polycarbonate resin, polystyrene resin, polyamide resin, silicon carbide (SiC), alumina (Al2O3), and silicon nitride (SiN). In order to effectively prevent contamination of the non-porous substrate when quantifying acid or base components in a gas using this quantification kit, the material for the non-porous substrate is preferably quartz or glass, and particularly preferably quartz.

[0048] The shape of the non-porous substrate is not particularly limited, and from the viewpoint of suitably capturing the acid or base components in the gas when quantifying the acid or base components in the gas using this quantification kit, a shape with a large surface area is preferred. Examples of shapes with a large surface area include particulate and fibrous shapes. The shape of the non-porous substrate is more preferably particulate.

[0049] The lower limit of the average particle size or average cross-sectional diameter of the non-porous substrate is preferably 300 μm or more, more preferably 400 μm or more, even more preferably 450 μm or more, even more preferably 500 μm or more, and particularly preferably 600 μm or more, from the viewpoint of increasing the efficiency of aeration into the collection column B when quantifying acid or base components in a gas using this quantification kit. The upper limit of the average particle size or average cross-sectional diameter of the non-porous substrate is preferably 1200 μm or less, more preferably 1100 μm or less, even more preferably 1050 μm or less, even more preferably 1000 μm or less, and particularly preferably 850 μm or less, from the viewpoint of increasing the efficiency of capturing the acid or base components when quantifying acid or base components in a gas using this quantification kit. The method for measuring the average particle size and average cross-sectional diameter is in accordance with JIS K0069 "Sieving test method for chemical products."

[0050] The basic adsorbent is an adsorbent for adsorbing acid components, and specifically may be made of or contain a basic substance, while the acidic adsorbent is an adsorbent for adsorbing base components, and specifically may be made of or contain an acidic substance.

[0051] The amount of the basic adsorbent or the acidic adsorbent in the collection column containing adsorbent A is preferably 0.4 μeq or more, more preferably 0.7 μeq or more, and even more preferably 0.8 μeq or more. Adjusting the amount of the basic adsorbent or the acidic adsorbent to 0.4 μeq or more is preferable in terms of preventing breakthrough of the column when collecting high-concentration gases. On the other hand, the amount of the basic adsorbent or the acidic adsorbent is preferably 50 μeq or less, more preferably 30 μeq or less, and even more preferably 20 μeq or less. Adjusting the amount of the basic adsorbent or the acidic adsorbent to 50 μeq or less is preferable in terms of preventing measurement inhibition by excess adsorbent components. The amount of the basic adsorbent or the acidic adsorbent is a value expressed in equivalents and can be measured by the method described in the Examples.

[0052] The basic adsorbent may be an inorganic base or an organic base. The inorganic base may be an alkali metal carbonate or an alkali metal hydroxide. The organic base may be an amine or an ammonium compound.

[0053] Of the compounds listed above, the basic adsorbent is preferably at least one compound selected from the group consisting of alkali metal carbonates, alkali metal hydroxides, amines, and ammonium compounds.

[0054] Examples of the alkali metal carbonates include sodium carbonate, potassium carbonate, and potassium hydrogen carbonate. Examples of the alkali metal hydroxides include strontium hydroxide, potassium hydroxide, and sodium hydroxide. Examples of the amines include triethanolamine. Examples of the ammonium compounds include tetramethylammonium hydroxide and tetrabutylammonium hydroxide.

[0055] The basic adsorbent is more preferably at least one compound selected from the group consisting of sodium carbonate, sodium hydroxide, and triethanolamine.

[0056] The acidic adsorbent may include inorganic acids and organic acids.

[0057] Examples of the inorganic acid include sulfuric acid, phosphoric acid, etc. Examples of the organic acid include methanesulfonic acid, maleic acid, malonic acid, etc.

[0058] Of the compounds listed above, the acidic adsorbent is preferably at least one compound selected from the group consisting of sulfuric acid, phosphoric acid, and methanesulfonic acid.

[0059] In a collection column including the adsorbent A, the form in which the nonporous substrate holds the basic adsorbent or the acidic adsorbent is not particularly limited. For example, the form may be such that the solid basic adsorbent or the acidic adsorbent is attached to the surface of the nonporous substrate, or such that the nonporous substrate is covered with a liquid phase containing the basic adsorbent or the acidic adsorbent.

[0060] The liquid phase is a liquid containing the basic adsorbent or the acidic adsorbent, and optionally contains a solvent. In other words, if the basic adsorbent or the acidic adsorbent is solid, the liquid phase can be prepared by dissolving the basic adsorbent or the acidic adsorbent in a solvent. The solvent is not particularly limited and can be any solvent that can dissolve the basic adsorbent or the acidic adsorbent and does not adversely affect the non-porous substrate. Specific examples of the solvent include water; polyhydric alcohols such as ethylene glycol, propylene glycol, and glycerin; polyalkylene glycols such as polyethylene glycol and polypropylene glycol; hydrogen peroxide; ethanol; acetonitrile; or mixtures thereof. The solvent is preferably a water-containing solvent, such as a mixture of water and a solvent other than water from the specific examples of the solvents listed above, and more preferably a solvent consisting solely of water. On the other hand, if the basic adsorbent or the acidic adsorbent is liquid, the basic adsorbent or the acidic adsorbent can be used directly as the liquid phase.

[0061] In a collection column equipped with adsorbent A, the method for coating the nonporous substrate with the liquid phase is not particularly limited. Examples of such methods include applying the liquid phase to the nonporous substrate, and immersing the nonporous substrate in the liquid phase, then lifting it out and drying it. A specific example of a method for applying the liquid phase to the nonporous substrate is a method in which the liquid phase is passed through the porous substrate. Here, the term "passing through" refers to passing the liquid phase through a container, such as a column, filled with the porous substrate. Note that if the drying conditions are high temperature and long time, the solvent in the liquid phase may evaporate, resulting in the precipitation of the basic adsorbent or the acidic adsorbent in solid form on the surface of the nonporous substrate. In such a case, the nonporous substrate can be obtained in a form in which the solid basic adsorbent or the acidic adsorbent is attached to the surface.

[0062] In a collection column equipped with adsorbent A, the nonporous substrate may further hold a humectant. When the basic adsorbent or the acidic adsorbent is held in the liquid phase in the nonporous substrate further holding a humectant, the liquid phase further contains the humectant. Examples of the humectant include polyhydric alcohols such as ethylene glycol, propylene glycol, and glycerin; and polyalkylene glycols such as polyethylene glycol and polypropylene glycol. The content of the humectant may be 0.01 wt % or more and 1.0 wt % or less, and preferably 0.1 wt % or more and 0.5 wt % or less, based on the total weight of the nonporous substrate covered with the liquid phase.

[0063] A collection column equipped with adsorbent A may be composed of a housing (i.e., an exterior part) and a frit, which is a filter disposed inside the housing and prevents the nonporous substrate from leaking out. The materials for the housing and the frit are not particularly limited, as long as they do not affect the acid or base components to be collected and are not adversely affected, such as by corrosion, by the basic adsorbent or the acidic adsorbent. Examples of materials for the housing include polypropylene, glass, polyethylene (PE), polyether ether ketone (PEEK), polyvinyl chloride (PVC), polystyrene (PS), ABS resin (ABS), methacrylic resin, acrylic resin (PMMA), polyamide (PA), polyacetal (POM), polycarbonate (PC), modified polyphenylene ether (mPPE), polybutylene terephthalate (PBT), polyethylene terephthalate (PET), polyphenylene sulfide (PPS), polysulfone (PSU), polyarylate (PAR), fluororesin (PFA), and mixtures thereof. Examples of materials for the frit include polyethylene, polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), polyethersulfone (PES), cellulose, glass fiber, carbon fiber, diatomaceous earth, cellulose, polyethylene terephthalate (PET), nylon, and mixtures thereof. The materials of the housing and the frit may be the same or different.

[0064] The shape of the collection column equipped with adsorbent A is not particularly limited, and a cylindrical column can usually be used. The collection column equipped with adsorbent A is preferably a column consisting of a column body, a frit, a sleeve, and an end fitting, and examples thereof include those described in JP-A-2001-249120.

[0065] The internal volume of the collection column equipped with the adsorbent A (the internal volume of the housing) can be an appropriate size depending on the amount of analysis to be processed. The volume is, for example, 0.6 ml to 5 ml, 0.6 ml to 3 ml, or 0.7 ml to 2 ml.

[0066] The void volume of a collection column comprising adsorbent A refers to the volume of the gaps in the collection column comprising adsorbent A that are not filled with the non-porous substrate covered with the liquid phase. The void volume can be measured, for example, by the method described in the Examples.

[0067] The larger the void volume is, i.e., the greater the amount of gas passing through collection column B, which is a collection column equipped with adsorbent A, per unit time when quantifying acid or base components in gas using this quantification kit, i.e., the greater the airflow rate. Here, when quantifying acid or base components in gas using the quantification kit, a predetermined amount of gas is collected in collection column B, and the gas is allowed to pass through, thereby capturing the acid or base components contained in the predetermined amount of gas. Therefore, the larger the void volume is, the shorter the time required to pass a predetermined amount of gas through collection column B.

[0068] Therefore, when quantifying an acid or base component in a gas using this quantification kit, the larger the void volume, the faster the acid or base component in the gas can be collected and quantified. From this perspective, the lower limit of the void volume may be preferably 200 μL or more, more preferably 300 μL or more, and even more preferably 400 μL or more.

[0069] On the other hand, when the void volume is equal to or less than a predetermined value, the amount of non-porous substrate carrying the basic adsorbent or acidic adsorbent in collection column B, which is a collection column equipped with adsorbent A, is sufficiently large, and the ability to capture acid or base components in the gas can be sufficiently ensured. Therefore, when quantifying acid or base components in a gas using this quantification kit, the acid or base components in the gas can be captured and quantified with high sensitivity. From the viewpoint of being able to capture and quantify acid or base components in the gas with high sensitivity, the void volume is preferably equal to or less than 5000 μL, more preferably equal to or less than 3000 μL, even more preferably equal to or less than 600 μL, and particularly preferably equal to or less than 500 μL.

[0070] The upper limit of the pressure drop when gas is aspirated into the collection column comprising the adsorbent A at a suction rate of 2.0 L / min is preferably 10 kPa or less. Hereinafter, the pressure drop when aspirating at a suction rate of 2.0 L / min is referred to as "pressure drop A." Having a pressure drop A of 10 kPa or less enables high-speed gas sampling without placing a load on the gas sampling suction pump when the gas to be measured is sampled and passed through collection column B, which is a collection column comprising adsorbent A. This allows a predetermined amount of gas to be sampled and passed through collection column B, which is a collection column comprising adsorbent A, in a short period of time. Therefore, when quantifying acid or base components in a gas using this quantification kit, the acid or base components in the gas can be captured and quantified in a short period of time. From this perspective, the upper limit of the pressure drop A of the collection column comprising the adsorbent A is preferably 7 KPa or less, and more preferably 5 KPa or less.

[0071] [Embodiment 3: Quantitation method] A quantitative determination method according to one embodiment of the present invention (hereinafter also referred to as "the present quantitative determination method") comprises: Step A, in which a solvent is passed through the standard-loaded column to elute the known amount of the acid component or the known amount of the base component into the solvent, thereby obtaining an eluate A; Step B1: passing the gas through an acid component collection column for collecting acid components in the gas or a base component collection column for collecting base components in the gas, thereby collecting acid components or base components in the gas; Step B2, after step B1, of passing a solvent through the acid component collection column that has collected the acid components in the gas in step B1 or the base component collection column that has collected the base components in the gas in step B1, thereby eluting the collected acid components or base components into the solvent to obtain an eluate B; and and step C of analyzing the eluate A and the eluate B and comparing the analysis results of the two to quantify the concentration of the acid component or the base component in the gas.

[0072] In short, this quantitative method is a method for quantifying acid or base components in a gas using the standard-loaded column and collection column B, and allows for easy quantification of the acid or base components in the gas.

[0073] Hereinafter, the method for quantifying the concentration of acid components in a gas using a column impregnated with the standard for acid components and column B for collecting acid components will also be referred to as the "method for quantifying acid components." Additionally, the method for quantifying the concentration of base components in a gas using a column impregnated with the standard for base components and column B for collecting base components will also be referred to as the "method for quantifying base components."

[0074] Each step constituting this quantitative method will be described in detail below.

[0075] (Process A) This quantitative method includes step A of passing a solvent through the standard-loaded column to elute the known amount of acid component or the known amount of base component into the solvent, thereby obtaining eluate A.

[0076] For the configuration etc. of the standard impregnated column used in step A, the description of the configuration etc. of the standard impregnated column in the above [Embodiment 1: Standard impregnated column] can be used.

[0077] In step A, a known amount of the acid or base component trapped in the standard-loaded column containing the trapping column A is eluted into the solvent, resulting in an eluate A containing the known amount of the acid or base component. Thus, the known amount of the acid or base component trapped in the standard-loaded column is dissolved in eluate A. The solvent is not particularly limited as long as it can elute the acid or base component. From the perspective of the sensitivity of the present quantification method, it is preferable to use a solvent that does not contain impurities that could cause a decrease in sensitivity, or that contains only minimal amounts of such impurities. From this perspective, it is particularly preferable to use pure water as the solvent. Here, pure water refers to water with an electrical resistivity in the range of 0.1 MΩ·cm to 18 MΩ·cm.

[0078] (Process B1) This quantification method includes step B1 of passing a gas through an acid component collection column for collecting acid components in the gas, or through a base component collection column for collecting base components in the gas, to collect acid components or base components in the gas.

[0079] In short, step B1 is a step of passing a gas through a collection column B and collecting acid components or base components in the gas. Hereinafter, step B1, a step of collecting acid components in a gas using an acid component collection column B, will also be referred to as an "acid component collection step." Furthermore, step B1, a step of collecting base components in a gas using a base component collection column B, will also be referred to as a "base component collection step." Step B1 is an acid component collection step or a base component collection step.

[0080] The configuration of the trapping column B used in step B1 can be referenced to the description of the configuration of the trapping column B in the section [Embodiment 2: Quantitative Kit] above. Furthermore, the effects of the present quantitation kit in quantifying acid or base components in gas, as described in the section [Embodiment 2: Quantitative Kit] above, can be referenced as the effects of the present quantitation method. Furthermore, the acid or base components to be trapped in step B1 are not particularly limited and may be the acid or base components exemplified in the section [Embodiment 1: Standard Impregnated Column] above. From the viewpoint of the accuracy of the present quantitation method, it is preferable that the acid or base components to be trapped in step B1 are the same as the acid or base components trapped in the present standard impregnated column used in step A.

[0081] Here, both the acid component collection step and the base component collection step can be carried out on the same gas at the same time, so that the acid component and the base component in the gas can be collected together.

[0082] In step B1, the gas to be collected is passed through a collection column B, whereby acidic or basic components in the gas are collected inside the collection column B. The aeration is usually carried out using a suction pump.

[0083] In step B1, by passing the gas through the acid component trapping column B or the base component trapping column B at a higher flow rate, the time required to capture the acid component or the base component in step B1 can be shortened. As a result, step B1 allows the acid component or base component in the gas to be collected in a short time, enabling it to be quantified in a short time by the present quantification method. From the viewpoint of collecting the acid component or base component in the gas in a short time and quantifying it in a short time by the present quantification method, the flow rate is preferably 2.0 L / min or more, more preferably 3.0 L / min or more. On the other hand, if the flow rate is excessively high, the pressure applied to trapping column B when passing the gas through it increases, which may damage trapping column B. From the viewpoint of effectively preventing damage to trapping column B, the flow rate is preferably 10 L / min or less, more preferably 7 L / min or less. From the viewpoint of achieving excellent results in both the ability to perform quantification in a shorter time and the prevention of breakage in the present quantification method, it is particularly preferable that the aeration flow rate is 5 L / min.

[0084] The ventilation of the collection column B is usually carried out in the space to be evaluated, such as a clean room or clean booth. The collection column B is transported by sealing the opening of the collection column B with a plug that is not contaminated by the analyte and / or by storing the collection column B in a sealed container that is not contaminated by the analyte.

[0085] When the acid component collection step and the base component collection step are performed together, the acid component collection step and the base component collection step may be performed continuously using an apparatus having an acid component collection column B and a base component collection column B arranged in series. That is, the air may be sucked into the apparatus and continuously passed through both the acid component collection column B and the base component collection column B that constitute the apparatus. More specifically, (i) air that has passed through the acid component collection column B may be passed through the base component collection column B, or (ii) air that has passed through the base component collection column B may be passed through the acid component collection column B. In this case, the acid component collection column B and the base component collection column B may be connected directly or via a connecting pipe.

[0086] By simultaneously carrying out the acid component collection step and the base component collection step, the method for quantifying acid components and the method for quantifying base components can be carried out. In this case, for example, the air may be sucked into an apparatus having a configuration in which an acid component collection column B and a base component collection column B are arranged in series, and the air may be simultaneously passed through both the acid component collection column B and the base component collection column B that make up the apparatus. Thereafter, the acid component collection column B and the base component collection column B are separated from the apparatus, and the below-described steps B2 and C are carried out for each.

[0087] (Process B2) This quantification method includes, after step B1, step B2 of passing a solvent through the acid component collection column that has collected the acid components in the gas in step B1 or the base component collection column that has collected the base components in the gas in step B1, thereby eluting the collected acid components or base components into the solvent to obtain eluate B.

[0088] In short, step B2 is a step performed after step B1, in which a solvent is passed through the collection column B that has collected the acid component or base component in the gas in step B1, thereby eluting the acid component or base component into the solvent to obtain an eluate B. Thus, the eluate B contains dissolved therein the amount of the acid component or base component collected in step B1.

[0089] As in step A, the solvent used in step B2 is not particularly limited as long as it is a solvent that can elute the acid component or the base component. As in step A, from the viewpoint of the sensitivity of the present quantification method, it is preferable to use a solvent that does not contain impurities that may cause a decrease in sensitivity or that contains only a minimal amount of such impurities as the solvent used in step B2. From this viewpoint, it is particularly preferable to use pure water as the solvent used in step B2. Furthermore, from the viewpoint of the accuracy of the present quantification method, it is preferable to use the same type of solvent in step B2 as in step A.

[0090] (Process C) This quantitative method includes a step C of analyzing the eluate A and the eluate B and comparing the analytical results of both to quantify the concentration of the acid component or the base component in the gas.

[0091] The step C can be, for example, the following steps (1) to (4). (1) By analyzing an eluate A containing a known amount of an acid component or a base component using a method for quantifying the acid component or the base component, the "standard result" can be obtained, and a correspondence relationship A can be obtained from the standard result. (2) For the eluate B containing the acid or base components in the collected gas, a numerical value corresponding to the amount of the acid or base components contained in the eluate B is obtained using the same method as the method for quantifying the acid or base components in (1) above. (3) The numerical value obtained in (2) is converted into the amount of acid or base components contained in eluate B based on the correspondence relationship A obtained in (1) above, and the amount of acid or base components contained in eluate B is calculated. (4) The amount of the acid component or base component obtained in (3) is divided by the amount of gas passed through the collection column B in step B1 to calculate the concentration of the acid component or base component in the gas.

[0092] The acid component or the base component in the eluate B is the same as the acid component or the base component in the gas collected in step B1. Therefore, the amount of the acid component or the base component in the eluate B calculated in step (3) of step C corresponds to the amount of the acid component or the base component in the gas passed through the collection column B. Therefore, the amount of the acid component or the base component in the gas can be quantified by the measurement step.

[0093] In (1) and (2), the method for quantifying the acid component or the base component in the eluate A and the eluate B (hereinafter also referred to as the "measurement method") can be a known method and is not particularly limited. The measurement method can be, for example, a liquid chromatography method. Examples of the liquid chromatography method include an anion exchange method using an ion exchange column, a cation exchange method, and a suppressor-type ion chromatography method using a suppressor.

[0094] The acid components are present as anions in the eluate A and the eluate B, and the base components are present as cations in the eluate A and the eluate B. Therefore, in (1), the "standard result" and correspondence relationship A are obtained for the total amount of anions or cations in the eluate A, and these are used as the "standard result" and correspondence relationship A for the known amount of acid components or base components. Similarly, in (2), a numerical value corresponding to the total amount of anions or cations in the eluate B is obtained, and this numerical value is used as the numerical value corresponding to the amount of acid components or base components collected in step B1.

[0095] [Embodiment 4: Method for managing the cleanliness of a space] A method for managing the cleanliness of a space according to one embodiment of the present invention (hereinafter also referred to as "this management method") is a method for managing the cleanliness of a space, comprising: a quantification step of quantifying the concentration of an acid component or a base component in a gas in a space using this quantification method; and a step of identifying and excluding a source of the acid component or base component in the gas inside the space when the concentration of the acid component or base component quantified in the quantification step exceeds a threshold value.

[0096] As described above, this quantification method allows the amount of acid or base contained in a gas to be easily quantified through simplified operations. Therefore, this control method can be easily implemented, and therefore, this control method allows a clean space to be easily secured.

[0097] (Quantitative process) This control method includes a quantification step of quantifying the concentrations of acidic and basic components in the gas in the space using this quantification method. By carrying out the quantification step, the concentrations of acidic and basic components, which are contaminants in the space, can be easily (simple) determined.

[0098] The space in this specification refers to a space that is the subject of evaluation using this quantification method, and may be, for example, a space in which the concentrations of the acid component and the base component as contaminants are required to be below a specific threshold value for the purpose of performing operations such as the manufacture of electronic substrates. The space in this management method may typically be a space having a predetermined volume formed by walls, a floor, etc. The space is not particularly limited, and examples thereof include a clean room, a clean booth, and the space inside a manufacturing device.

[0099] The configuration and the like of the quantification method in the quantification step are the same as those described in [Embodiment 3: Quantification method] above.

[0100] In this control method, to easily ensure a clean space, the amount (concentration) of the acid component and / or the base component, which are contaminants in the space, is simply quantified, and the source of contamination is identified and eliminated based on the quantified concentration. Therefore, in the quantification step, either the acid component quantification method or the base component quantification method may be performed, or both the acid component quantification method and the base component quantification method may be performed simultaneously. However, it is preferable to perform both the acid component quantification method and the base component quantification method simultaneously. To perform these simultaneously, it is preferable to use an apparatus having the aforementioned acid component collection column B and base component collection column B arranged in series. When using this apparatus, a single suction operation into the apparatus can ventilate both the acid component collection column B and the base component collection column B, making the quantification step and this control method easier to perform.

[0101] (Process of identifying and eliminating the source of contamination) This management method includes a step of identifying and eliminating a source of the acid component or base component in the gas inside the space when the concentration of the acid component or base component quantified in the quantification step exceeds a threshold value. In this specification, the "source of the acid component or base component in the gas inside the space" is also referred to as the "contamination source." Therefore, the "step of identifying and eliminating a source of the acid component or base component in the gas inside the space" is the "step of identifying and eliminating a contamination source." By performing the step of identifying and eliminating the contamination source, the concentration of the acid component or base component, which is a contaminant, inside the space can be controlled to a threshold value or below, thereby easily ensuring a clean space.

[0102] The threshold value in the process can be appropriately determined depending on the type of operation performed in the space and the quality required for the product manufactured by the operation, and is not particularly limited. For example, when manufacturing high-quality electronic substrates in the space, the threshold value is 1.0 μg / m 3 , 0.1 μg / m 3 or 0.01 μg / m 3 etc.

[0103] Identifying and eliminating the source of contamination means grasping the concentrations of the acid components and base components, which are contaminants inside the space, and taking appropriate measures. The specific method for this is not particularly limited, and any known method can be used.

[0104] One embodiment of the present invention may be any of the inventions shown in [1] to

[11] below. [1] A standard impregnated column for determining the concentration of an acid or base component in a gas, The standard impregnation column is a standard impregnation column in which a known amount of acid component is impregnated into an acid component collection column for collecting acid components in a gas, or a standard impregnation column in which a known amount of base component is impregnated into a base component collection column for collecting base components in a gas. [2] The standard loaded column according to [1], wherein the amount of the known amount of acid component or the known amount of base component is more than 1 ng and 1000 μg or less. [3] The column for collecting the acid component or the base component is The non-porous substrate is filled, the non-porous substrate holds a basic adsorbent for adsorbing an acid component or an acidic adsorbent for adsorbing a base component; The pressure loss when the gas in the column for collecting acid or base components is sucked at a suction rate of 2.0 L / min is 10 kPa or less. Standard loaded column described in [1] or [2]. [4] The standard loading column according to [3], wherein the void volume of the collection column is 200 μL or more and 3000 μL or less. [5] The standard loading column according to [3] or [4], wherein the amount of the basic adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less. [6] A kit for quantifying the concentration of an acid component and / or a base component in a gas, which satisfies one or more of the following (a) and (b): (a) One or more standard impregnation columns impregnated with a known amount of the acid component described in [1] or [2], and one or more acid component collection columns for collecting the acid component in the gas, (b) A kit for quantifying the concentration of acid and / or base components in a gas, comprising one or more standard impregnated columns impregnated with a known amount of base component described in [1] or [2], and one or more base component trapping columns for trapping base components in the gas. [7] The column for collecting the acid component or the base component is The non-porous substrate is filled, the non-porous substrate holds a basic adsorbent for adsorbing an acid component or an acidic adsorbent for adsorbing a base component; The pressure loss when the gas in the column for collecting acid or base components is sucked at a suction rate of 2.0 L / min is 10 kPa or less. A kit for quantifying the concentration of an acid component and / or a base component in a gas according to [6]. [8] The kit for quantifying the concentration of acidic and / or basic components in a gas according to [7], wherein the void volume of the collection column is 200 μL or more and 3000 μL or less. [9] A kit for quantifying the concentration of acidic and / or basic components in a gas according to [7] or [8], wherein the amount of the basic adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less.

[10] A method for quantifying the concentration of an acid component and / or a base component in a gas using the kit for quantifying the concentration of an acid component or a base component in a gas according to [6], Step A, in which a solvent is passed through the standard-loaded column to elute the known amount of the acid component or the known amount of the base component into the solvent, thereby obtaining an eluate A; Step B1, in which the gas is passed through an acid component collection column for collecting acid components in the gas or a base component collection column for collecting base components in the gas, thereby collecting acid components or base components in the gas; Step B2, after step B1, of passing a solvent through the acid component collection column that has collected the acid components in the gas in step B1 or the base component collection column that has collected the base components in the gas in step B1, thereby eluting the collected acid components or base components into the solvent to obtain an eluate B; and

[11] A quantitative determination method comprising: a step C of quantifying the concentration of the acid component or the base component in the gas by analyzing the eluate A and the eluate B and comparing the analysis results of both; a quantitative determination step of quantifying the concentration of the acid component or the base component in the gas in a space using the quantitative determination method according to

[10] ; A method for managing the cleanliness of a space, comprising a step of identifying and eliminating a source of the acid component or base component in the gas inside the space when the concentration of the acid component or base component quantified in the quantification step exceeds a threshold value. [Example]

[0105] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to these examples.

[0106] [Measurement method] In the examples, the methods for measuring the amounts of base components or acid components contained in the eluates obtained from the standard loading column and the collection column are shown below.

[0107] (ion chromatography) In the examples, eluent A or eluent B was analyzed using an ion chromatograph by the method described below, and the values ​​corresponding to the amounts of acid components or base components contained in eluent A or eluent B were measured.

[0108] A dual-channel ion chromatographic system with conductivity detection was used to analyze eluents A and B. The anion channel of the ion chromatographic system used a potassium hydroxide eluent gradient with an anion analytical column and suppressor. The cation channel of the ion chromatographic system used a methanesulfonic acid eluent gradient with a cation analytical column and suppressor.

[0109] [Production Example 1: Preparation of base component collection column A and base component collection column B] 0.9 g of quartz particles with particle diameters of 0.5 mm to 1.0 mm was packed into a cylindrical polypropylene column housing with an internal volume of 0.92 mL. After passing methanol through the column, the column was washed by passing ultrapure water (resistivity 0.1 MΩ cm or higher).

[0110] A mixed aqueous solution of sulfuric acid and glycerin was passed through the washed column, and then clean air was passed through to dry the column, thereby preparing column A for collecting base components.

[0111] Furthermore, the same method as above was repeated five times to prepare five columns B for collecting base components, each having the same configuration as the column A for collecting base components.

[0112] [Example 1: Preparation of a standard impregnated column for base components] 50 ng of ammonium ion (NH4 + ) was added to the column A for collecting base components, to prepare a standard column for base components. Specifically, 5 μL of an ammonium ion standard solution with an ammonium ion concentration of 10 μg / mL was added to the column A for base component collection using a micropipette, and then the column was dried by passing clean nitrogen gas through it. As a result, 50 ng of ammonium ion (NH + A standard impregnated column for the base component was prepared, impregnated with .

[0113] 10 mL of purified water was passed through the prepared standard base component impregnated column to prepare eluate A, in which ammonium ions, the base component impregnated in the standard base component impregnated column, were eluted. The peak area of ​​the prepared eluate A, which corresponds to the amount of the base component, was obtained using the ion chromatograph. The obtained peak area is referred to as "peak area A." Specific values ​​for peak area A are shown in Table 1 below.

[0114] [Examples 2 to 6] A room, part of which was a clean booth, was prepared. In the room, aeration was performed for 125 minutes on the airflow side of 2 L / min through each of the base component trapping columns B prepared in Production Example 1 at one arbitrary location outside the clean booth and at each of four arbitrary locations in the clean booth. Thereafter, 10 mL of pure water was passed through each of the aerated base component trapping columns B in the same manner as in Example 1 to prepare eluate B. The peak area, which is a numerical value corresponding to the amount of the base component, was obtained for each of the prepared eluate B using the ion chromatograph. The obtained peak area is referred to as "peak area B." The example in which aeration was performed at one location outside the clean booth was designated Example 2, and the examples in which aeration was performed at each of four locations in the clean booth were designated Examples 3 to 6, respectively.

[0115] Using the "peak area B" obtained in each of Examples 2 to 6 and the "peak area A" obtained in Example 1, the concentration of the base component in each of the 250 L aerated gases was calculated based on the following formula (I). Concentration of base component in gas = (0.2 × area B) / area A [μg / m 3 ]···Formula (I) The concentrations of the base components in the gas calculated by the formula (I) in each of Examples 2 to 6 are shown in Table 1 below.

[0116] [Table 1]

[0117] [Production Example 2: Preparation of Acid Component Collection Column A and Acid Component Collection Column B] 0.9 g of quartz particles with particle diameters of 0.5 mm to 1.0 mm was packed into a cylindrical polypropylene column housing with an internal volume of 0.92 mL. After passing methanol through the column, the column was washed by passing ultrapure water (resistivity 0.1 MΩ cm or higher).

[0118] After the washing, an aqueous solution of sodium carbonate and glycerin was passed through the column, and then clean air was passed through the column to dry it, thereby preparing column A for collecting acid components.

[0119] Furthermore, the same method as above was repeated five times to prepare five columns B for collecting acid components, each having the same configuration as the column A for collecting acid components.

[0120] [Example 7: Preparation of standard impregnated column for acid components] For the acid component collection column A prepared in Production Example 2, formic acid, acetic acid, and fluoride ions (F - ), chloride ions (Cl - ), bromide ion (Br - ), nitrite ion (NO2 - ), nitrate ions (NO3 - ), sulfate ions (SO4 2- ) and phosphate ions (PO4 3- ) was added to the column A for collecting acid components, and a standard impregnated column for acid components was prepared by adding 50 ng or 100 ng of an acid component mixture consisting of each acid component. Specifically, 5 μL of an acid component standard solution containing 10 μg / mL or 20 μg / mL of the acid component mixture was added to the column A for collecting acid components using a micropipette, followed by drying by passing clean nitrogen gas through the column. As a result, a standard impregnated column for acid components, with 50 ng or 100 ng of the acid component added, was prepared. The amount of each acid component contained in 5 μL of the acid component standard solution is shown in Table 2 below. The amount of each acid component contained in 5 μL of the acid component standard solution is also the amount of each acid component added to the standard impregnated column for acid components.

[0121] [Table 2]

[0122] 10 mL of pure water was passed through the prepared standard acid component-imparted column to prepare eluate A, in which the acid component mixture impregnated on the standard acid component-imparted column was eluted. The prepared eluate A was analyzed by the ion chromatograph to obtain peak areas, which are values ​​corresponding to the amounts of each acid component constituting the acid component mixture. The obtained peak areas are referred to as "peak area A."

[0123] [Examples 8 to 12] A room, part of which was a clean booth, was prepared. In the room, each of the acid component trapping columns B prepared in Production Example 2 was aerated at an arbitrary location outside the clean booth and at each of four arbitrary locations within the clean booth at 2 L / min on the air flow side for 125 minutes. Thereafter, 10 mL of pure water was passed through each of the aerated acid component trapping columns B in the same manner as in Example 1 to prepare each eluate B. For each of the prepared eluates B, the peak area, which is a numerical value corresponding to the amount of each acid component, was obtained using the ion chromatograph. The obtained peak area is referred to as "peak area B."

[0124] Using the "peak area B" corresponding to the amount of each acid component obtained in each of Examples 8 to 12 and the "peak area A" corresponding to the amount of each acid component obtained in Example 7, the concentration of each acid component in each 250 L of gas aerated was calculated based on the following formula (II). Concentration of acid component in gas = (0.2 × area B) / area A [μg / m 3 ]...Formula (II) The concentrations of each acid component in the gas calculated by the formula (II) in each of Examples 8 to 12 are shown in Table 3 below.

[0125] [Reference examples 1~5] A five-point calibration curve was created for each acid component, showing the relationship between the peak area corresponding to the amount of each acid component obtained using the ion chromatograph used in Examples 8 to 12 and the amount (mass) of each acid component in the eluate. Specifically, five standard solutions were prepared for each acid component, with concentrations of 0.5 ng / mL, 1 ng / mL, 5 ng / mL, 10 ng / mL, and 50 ng / mL, or 1 ng / mL, 2 ng / mL, 10 ng / mL, 20 ng / mL, and 100 ng / mL, using pure water as the solvent. Next, five peak areas corresponding to the amount of each acid component in each standard solution were obtained using the ion chromatograph. The five peak areas obtained and the amount of each acid component corresponding to each peak area were plotted to create the five-point calibration curve.

[0126] Using the five-point calibration curve, the peak area B corresponding to the amount of each acid component obtained in Examples 8 to 12 was converted to calculate the concentration of each acid component in the obtained eluate. In addition, the product of the calculated concentration of each acid component in the eluate, the concentration of each acid component in the eluate, and the volume of the eluate was multiplied by the aeration volume: 2 L x 125 min = 250 L = 250 x 10 -3 m 3 The concentration of each acid component in the gas was calculated based on the above. Examples in which the mass and concentration of each acid component in the gas were calculated using the peak area B corresponding to the amount of each acid component obtained in each of Examples 8 to 12 and the calibration curve are designated as Reference Examples 1 to 5, respectively, and the concentrations of each acid component in the resulting gas are shown in Table 3 below. In Table 3 below, the unit of concentration of each acid component is [ng / L = μg / m 3 ].

[0127] [Table 3]

[0128] As shown in Tables 1 and 3, it was demonstrated that the concentrations of components in gas could be quantified without any problems by the quantification methods described in Examples 2 to 6 and 8 to 12. Furthermore, the results of Examples 8 to 12 were substantially identical to the results of Reference Examples 1 to 5, demonstrating that the standard-loaded column, quantification kit, and quantification method make it possible to easily quantitate the concentrations of acidic or basic components contained in gas without the need to prepare a calibration curve. [Industrial Applicability]

[0129] The standard impregnation column, the quantification kit, and the quantification method allow for easy quantification of the concentration of acid or base components in a gas. Furthermore, the control method using the quantification method allows for easy maintenance of a clean space. Therefore, the standard impregnation column, the quantification kit, the quantification method, and the control method can be used to control spaces where work requiring a clean space is performed, such as in the manufacture of electronic circuit boards.

Claims

1. A standard-loaded column for determining the concentration of an acid or base component in a gas, comprising: The standard impregnation column is a standard impregnation column in which a known amount of acid component is impregnated into an acid component collection column for collecting acid components in a gas, or a standard impregnation column in which a known amount of base component is impregnated into a base component collection column for collecting base components in a gas.

2. 2. The standard loaded column according to claim 1, wherein the amount of the known amount of acid component or the known amount of base component is more than 1 ng and not more than 1000 μg.

3. The column for collecting the acid component or the base component comprises: The non-porous substrate is filled, the non-porous substrate holds a basic adsorbent for adsorbing an acid component or an acidic adsorbent for adsorbing a base component; the pressure loss when the gas in the column for collecting acid or base components is sucked at a suction rate of 2.0 L / min is 10 kPa or less; 3. The standard loaded column according to claim 1 or 2.

4. 4. The standard loading column according to claim 3, wherein the void volume of the collection column is 200 μL or more and 3000 μL or less.

5. 4. The standard loading column according to claim 3, wherein the amount of the basic adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less.

6. A kit for quantifying the concentration of an acid component and / or a base component in a gas, which satisfies one or more of the following (a) and (b): (a) one or more standard impregnation columns impregnated with a known amount of the acid component according to claim 1 or 2, and one or more acid component collection columns for collecting the acid component in the gas; (b) A kit for quantifying the concentration of an acid component and / or a base component in a gas, comprising one or more standard impregnated columns impregnated with a known amount of the base component described in claim 1 or 2, and one or more base component trapping columns for trapping the base component in the gas.

7. The column for collecting the acid component or the base component comprises: The non-porous substrate is filled, the non-porous substrate holds a basic adsorbent for adsorbing an acid component or an acidic adsorbent for adsorbing a base component; the pressure loss when the gas in the column for collecting acid or base components is sucked at a suction rate of 2.0 L / min is 10 kPa or less; The kit for quantifying the concentration of an acid component and / or a base component in a gas according to claim 6.

8. 8. The kit for quantifying the concentration of an acid component and / or a base component in a gas according to claim 7, wherein the void volume of the collection column is 200 μL or more and 3000 μL or less.

9. 8. The kit for quantifying the concentration of an acid component and / or a base component in a gas according to claim 7, wherein the amount of the basic adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less.

10. A method for quantifying the concentration of an acid component and / or a base component in a gas, using the kit for quantifying the concentration of an acid component or a base component in a gas according to claim 6, Step A, in which a solvent is passed through the standard-loaded column to elute the known amount of the acid component or the known amount of the base component into the solvent, thereby obtaining an eluate A; Step B1, in which the gas is passed through an acid component collection column for collecting acid components in the gas or a base component collection column for collecting base components in the gas, thereby collecting acid components or base components in the gas; Step B2, after step B1, of passing a solvent through the acid component collection column that has collected the acid components in the gas in step B1 or the base component collection column that has collected the base components in the gas in step B1, thereby eluting the collected acid components or base components into the solvent to obtain an eluate B; and and step C of analyzing the eluate A and the eluate B and comparing the analysis results of the two to quantify the concentration of the acid component or the base component in the gas.

11. a quantifying step of quantifying the concentration of an acid component or a base component in a gas in a space using the quantifying method according to claim 10; A method for managing the cleanliness of a space, comprising a step of identifying and eliminating a source of the acid component or base component in the gas inside the space when the concentration of the acid component or base component quantified in the quantification step exceeds a threshold value.

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