Standard impregnation column for quantitative determination of the concentration of acidic or basic components in a gas, and its application.

Abstract

To provide a standard impregnation column that can be used in a quantitative method that allows for the simple quantification of the concentration of acidic or basic components contained in a gas through a simplified procedure. [Solution] 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, wherein a known amount of an acid component is impregnated onto an acid component collection column for collecting acid components in a gas, or a known amount of a base component is impregnated onto a base component collection column for collecting base components in a gas.

Description

[Technical Field]

[0001] The present invention relates to a standard impregnation column for the quantitative determination of the concentration of acidic or basic components in a gas, and its uses. Specifically, these uses include a kit for the quantitative determination of the concentration of acidic and / or basic components in a gas, a method for the quantitative determination of the concentration of acidic or basic components in a gas, and a method for controlling the cleanliness of a space. [Background technology]

[0002] In environments where electronic substrates such as semiconductor wafers, liquid crystal substrates, and magnetic disks (hereinafter referred to as "substrates") are manufactured, contaminants such as acidic substances (acidic components) and basic substances (basic components) in the manufacturing space can be adsorbed onto the substrates, sometimes resulting in reduced product yield and quality. Therefore, to prevent such reductions in yield and quality, the manufacturing process for these substrates is carried out in a cleanroom. It is necessary to evaluate the level of contamination by the aforementioned acidic and basic substances in the cleanroom during each manufacturing process, in other words, the cleanliness level, and to manage the cleanliness of the cleanroom by removing the cause of contamination if the cleanliness level deteriorates. Furthermore, in recent years, there has been a demand for cleanrooms to provide a highly clean environment, and consequently, there is a need for methods to evaluate the level of contamination by acidic or basic components within the cleanroom, i.e., the cleanliness level, with higher sensitivity. Moreover, in recent years, there has been a demand to shorten the time required for the evaluation in order to simplify the management of cleanroom cleanliness.

[0003] As a method for evaluating the cleanliness with high sensitivity and in a short time, for example, a method of 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 of quantifying the contaminants involves passing air from a cleanroom through the gas adsorption column or liquid-free trap to adsorb the contaminants in the air, and then quantifying the amount of adsorbed contaminants.

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

[0005] [Patent Document 1] Japanese Patent Publication No. 2009-14522 [Patent Document 2] International Publication No. 2010 / 067464 [Patent Document 3] Patent No. 6563396 [Overview of the Initiative] [Problems that the invention aims to solve]

[0006] As mentioned above, the conventional quantitative methods described earlier required the preparation of standard solutions, and in particular, the preparation of standard solutions by specially trained specialists was extremely cumbersome when performing highly sensitive quantitative analysis.

[0007] Therefore, an object of the present invention is to provide a quantitative method that can easily quantify the concentration of acidic or basic components contained in a gas, as well as a standard impregnation column and a quantitative kit that can be used in said quantitative method. Another object of the present invention is to provide a method for managing the cleanliness of a space that can easily ensure a clean space. [Means for solving the problem]

[0008] To achieve the above objective, a standard impregnation column according to one embodiment of the present invention is a standard impregnation column for determining the concentration of an acidic or basic component in a gas, The aforementioned 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 known amount of base component is impregnated onto a base component collection column for collecting base components in a gas.

[0009] To achieve the above objective, a quantitative kit according to one embodiment of the present invention is a kit for quantifying the concentration of acidic and / or basic components in a gas, and satisfies one or more of the following (a) and (b): (a) comprising one or more standard impregnation columns impregnated with the aforementioned known amount of acid component, and one or more acid component collection columns for collecting acid component in gas, (b) A kit for quantifying the concentration of acidic and / or basic components in a gas, comprising one or more standard impregnation columns impregnated with the known amount of basic component described above, and one or more basic component collection columns for collecting basic components in a gas.

[0010] To achieve the above objective, a quantitative method according to one embodiment of the present invention is a method for quantifying the concentration of acidic and / or basic components in a gas using the quantitative kit described above, Step A involves passing a solvent through the standard impregnation column to elute the known amount of acid or the known amount of base into the solvent, thereby obtaining eluate A. Step B1 involves 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, to collect the acid component or base component in the gas. Step B2 is performed after step B1, by passing a solvent through the acid component collection column that collected the acid component in the gas in step B1 or the base component collection column that collected the base component in the gas in step B1, thereby eluting the collected acid component or base component into the solvent to obtain eluate B, and The quantitative method includes step C, which involves analyzing eluent A and eluent B and comparing the analysis results of both 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 an 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 above quantification method, and a step of identifying and excluding a generation source of an acid component or a base component in the gas inside the space when the concentration of the acid component or the base component quantified in the quantification step exceeds a threshold value. It is a method for managing the cleanliness of a space. [Advantages of the Invention]

[0012] According to one aspect of the present invention, it is possible to provide a quantification method for easily quantifying the concentration of an acid component or a base component contained in a gas, and a standard attachment column and a quantification kit that can be used in the quantification method. Further, according to one aspect of the present invention, it is possible to provide a method for managing the cleanliness of a space that can easily secure a clean space. [Modes for Carrying Out the Invention]

[0013] An embodiment of the present invention will be described below, but the present invention is not limited to the embodiments described later. The present invention can be variously modified within the scope shown in the claims, and embodiments obtained by appropriately combining technical means disclosed in different embodiments are also included in the technical scope of the present invention.

[0014] [Embodiment 1: Standard Attachment Column] A standard attachment column according to an embodiment of the present invention (hereinafter also referred to as "this standard attachment column") is a standard attachment column for quantifying the concentration of an acid component or a base component in a gas. In the standard attachment column, a known amount of an acid component is attached to an acid component collection column for collecting an acid component in the gas, or a known amount of a base component is collected in a base component collection column for collecting a base component in the gas. Here, "a known amount of an acid component (base component) is attached to an acid component collection column (base component collection column)" means that "a known amount of an acid component (base component) is attached to an adsorbent filled in a column constituting the acid component collection column (base component collection column)".

[0015] Examples of the "collection column" described in this specification include the "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" described below.

[0016] In this specification, among this standard attachment column, a standard attachment column in which a known amount of an acid component is attached to an acid component collection column for collecting an acid component in the gas is also referred to as an "acid standard attachment column". The acid standard attachment column is a standard attachment column for quantifying the concentration of an acid component in the gas. On the other hand, in this specification, among this standard attachment column, a standard attachment column in which a known amount of a base component is attached to a base component collection column for collecting a base component in the gas is also referred to as a "base standard attachment column". The base standard attachment column is a standard attachment column for quantifying the concentration of a base component in the gas.

[0017] In this specification, the "acid component collection column for collecting an acid component in the gas" constituting the acid standard attachment column is also referred to as the "acid component collection column A". Also, in this specification, the "base component collection column for collecting a base component in the gas" constituting the base standard attachment column is referred to as the "base component collection column A". In this specification, the acid component collection column A and the base component collection column A are collectively also simply referred to as the "collection column A".

[0018] This standard impregnated column is either an acid component collection column A impregnated with a known amount of acid component, or a base component collection column A impregnated with a known amount of base component. When the amount of the known acid component or the known amount of base component impregnated in the standard impregnated column is measured by a predetermined method, the measurement result is a predetermined numerical value corresponding to the amount of the known acid component or the known amount of base component. Hereinafter, the predetermined numerical value obtained will be referred to as the "standard result." Then, a correspondence relationship between the known amount and the standard result is derived. Hereinafter, the correspondence relationship will also be referred to as "correspondence relationship A."

[0019] Here, we consider quantifying an unknown amount of acidic or basic component collected in an acidic or basic component collection column, separate from collection column A, using the same method as used to derive the correspondence. In this case, a numerical value corresponding to the unknown amount can be obtained.

[0020] In this specification, 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." Similarly, 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." Furthermore, in this specification, acid component collection column B and base component collection column B are collectively referred to simply as "collection column B." In addition, in this specification, when quantifying an unknown amount of acid or base component collected by the aforementioned collection column B, the correspondence between the unknown amount and the numerical value obtained that corresponds to the unknown amount is also referred to as "correspondence relationship B."

[0021] Here, when measuring the amount of acidic or basic components collected on columns such as this standard impregnated column and collection column B, an eluate containing almost the entire amount of the collected acidic or basic components is usually prepared and analyzed. Here, "almost the entire amount" means that the amount of acidic or basic components remaining after elution is negligible at the time of quantification. The analysis then yields a numerical value corresponding to almost the entire amount of the collected acidic or basic components. Therefore, correspondence A and correspondence B can both be considered to be numerical values ​​corresponding to almost the entire amount of acidic or basic components, measured using the same method on the eluate containing almost the entire amount of the collected acidic or basic components. Accordingly, correspondence A and correspondence B can be considered to be sufficiently identical.

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

[0023] As described above, by using this standard impregnated column, the amount and concentration of the acidic or basic component collected in collection column B can be calculated.

[0024] The aforementioned predetermined method may include, for example, a method of preparing an eluate from which the acid component or the base component has been eluted, and quantifying the acid component or the base component in the eluate using a known method. Here, the known method is not particularly limited and may include, for example, liquid chromatography. Examples of liquid chromatography include anion exchange methods using ion exchange columns, cation exchange methods, and suppressor-type ion chromatography using suppressors. Furthermore, for example, when preparing the eluate and quantifying the acid component or the base component in the eluate using liquid chromatography, the obtained value may be the peak area. In addition, as a method for preparing the eluate, for example, a method may be used in which a solvent is passed through the standard impregnation column to elute the acid component or base component collected on the standard impregnation column into the solvent, thereby preparing the eluate.

[0025] (Columns for collecting acidic components, columns for collecting basic components) This standard impregnated column includes collection column A. In one embodiment of the present invention, the composition of collection column A is not particularly limited, as long as it is capable of collecting a known amount of acidic or basic component, or acidic or basic component in a gas.

[0026] Here, we consider the case where the concentration of an acidic or basic component in a gas is quantified using the standard impregnated column and collection column B. If the composition of collection column A and collection column B included in the standard impregnated column are the same, the difference in the amount of acidic or basic component remaining in the standard impregnated column and collection column B after elution of the acidic or basic component will be small. As a result, the identity between correspondence A and correspondence B will be improved, and the accuracy of the quantification will be improved. For this reason, in the quantification, it is preferable that collection column A and collection column B have similar compositions, and more preferably that they have identical compositions.

[0027] In particular, when the amount of acidic or basic components collected in collection column B is extremely small, the influence of the residual acidic or basic components becomes relatively large. Therefore, when performing quantitative analysis of extremely small amounts of acidic or basic components, i.e., highly sensitive quantitative analysis, it is especially preferable that the composition of collection column A and collection column B included in this standard impregnated column are identical.

[0028] Here, the similarity of collection column A and collection column B could mean, for example, that both collection column A and collection column B are equipped with the adsorbent A described later. Alternatively, the identical configuration of collection column A and collection column B could mean, for example, that both collection column A and collection column B are equipped with the adsorbent A, and that the type and content of the non-porous substrate and the basic or acidic adsorbent described later, as well as their size and void volume, etc., are identical.

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

[0030] (Acid components, basic components) This standard impregnated column contains a known amount of an acidic or basic component. In this standard impregnated column, the acidic or basic component is impregnated onto collection column A. The acidic or basic component in this standard impregnated column may be any acidic or basic component that can be impregnated onto collection column A, and is not particularly limited.

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

[0032] This standard impregnated column is formed by impregnating a collection column A with a known amount of the acid component or a known amount of the base component. In one embodiment of the present invention, the method for impregnating the collection column A with a known amount of the acid component or a predetermined amount of the base component is not particularly limited and can include methods such as the addition of a standard solution.

[0033] The known quantity is not particularly limited, as long as it is less than or equal to the maximum quantity that collection column A can collect, and as long as the correspondence can be obtained from this standard impregnated column.

[0034] The maximum amount that the collection column A can collect depends on the amount (equivalent) of the basic adsorbent or acidic adsorbent held in the adsorbent A, if the collection column A is equipped with an adsorbent A. If the equivalent amount is large, the limit value will also increase. Therefore, if the collection column A is equipped with an adsorbent A, the limit value can be controlled by adjusting the equivalent amount of the basic adsorbent or acidic adsorbent held in the adsorbent A.

[0035] Furthermore, it is preferable, from the viewpoint of accuracy of the quantitative method using this standard impregnation column, that the known amount is close to (for example, of the same order) the expected amount of the acid component or the base component collected in collection column B by the quantitative method using this standard impregnation column. This is because, in this case, the identity between correspondence A and correspondence B is improved.

[0036] Specifically, the known amount is not particularly limited, but is preferably greater than 1 ng, more preferably 5 ng or more, and even more preferably 10 ng or more. When the purpose of the quantitative method is to quantify trace amounts of acid or base components in a gas, from the viewpoint of the accuracy of the quantitative 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 accuracy of the quantitative analysis method, it is preferable that the type of acid component or base component in the standard impregnation column is the same as the type of acid component or base component expected to be collected in collection column B by the quantitative analysis method. For example, if the quantitative analysis method is expected to collect ammonia in a gas in collection column B and quantify its concentration, it is preferable to use ammonia (ammonium ions) as the base component in the standard impregnation column.

[0038] [Embodiment 2: Quantitative Kit] A quantitative analysis kit according to one embodiment of the present invention (hereinafter also referred to as "this quantitative analysis kit") comprises one or more standard impregnation columns impregnated with a known amount of acid component and one or more acid component collection columns for collecting acid component in a gas, and / or comprises one or more standard impregnation columns impregnated with a known amount of base component and one or more base component collection columns for collecting base component in a gas, and is a quantitative analysis kit for acid component and / or base component in a gas.

[0039] This quantitative analysis kit essentially includes a combination of one or more of these standard-impregnated columns and one or more collection columns B. Here, the method for quantifying acidic or basic components in a gas using this standard-impregnated column is, in detail, a method for quantifying acidic or basic components in a gas using this standard-impregnated column and collection column B. Therefore, the method for quantifying acidic or basic components in a gas using this standard-impregnated column can be considered equivalent to the method for quantifying acidic or basic components in a gas using this quantitative analysis kit. As mentioned above, the method for quantifying acidic or basic components in a gas using this standard-impregnated column allows for the simple quantification of the concentration of acidic or basic components contained in the gas. Therefore, this quantitative analysis kit allows for the simple quantification of the concentration of acidic or basic components contained in a gas through simplified procedures.

[0040] (This standard pre-attached column) Regarding the configuration of the standard impregnation column that constitutes this quantitative analysis kit, the description of the configuration of the standard impregnation column in [Embodiment 1: Standard Impregnation Column] above can be referenced.

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

[0042] The non-porous substrate has weak adsorption capacity to 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 quantitative method using a collection column equipped with the adsorbent A, by reducing the amount of acidic or basic components remaining in the collection column after elution, a more suitable numerical value can be obtained for the total amount of collected acidic or basic components. Accordingly, it is preferable that the collection column B, which constitutes this quantitative kit used for the quantitative determination of very small amounts of acidic or basic components, is filled with the non-porous substrate. In that case, the accuracy of quantitative determination of acidic or basic components in a gas using this quantitative kit can be improved.

[0043] Furthermore, in the collection column equipped with the adsorbent A, a non-porous substrate is packed, and the other substances are not incorporated into the non-porous substrate. Therefore, the presence of the other substances is prevented from becoming noise in the quantification of acidic or basic components in the gas using this quantification kit, thus preventing a decrease in the accuracy of the quantification.

[0044] As described above, when collection column B is a collection column equipped with the adsorbent A, the accuracy of quantitative determination of acidic or basic components in a gas using this quantitative kit can be improved. Furthermore, in this quantitative determination, acidic or basic components in the gas can be collected and quantified with high sensitivity. In this specification, "collecting and quantifying with high sensitivity" means, for example, determining the concentration of acidic or basic components in the gas at approximately 10 -2 μg / m 3 This means collecting and quantifying in that order. In other words, if collection column B is a collection column equipped with the adsorbent A, then when quantifying acidic or basic components in a gas using this quantification kit, trace amounts of acidic or basic components can be collected and quantified.

[0045] Therefore, if collection column B is a collection column equipped with the adsorbent A, this quantitative kit allows for the simple and highly accurate quantification of acidic or basic components in a gas through a simplified procedure.

[0046] The following describes the detailed configuration of the collection column B, assuming that it is a collection column equipped with adsorbent A.

[0047] The non-porous substrate can have any shape that does not have pores, and its material is not particularly limited. Examples of materials for the non-porous substrate include quartz, glass, polycarbonate resin, polystyrene resin, polyamide resin, silicon carbide (SiC), alumina (Al2O3), silicon nitride (SiN), etc. From the viewpoint of effectively preventing contamination of the non-porous substrate during the quantitative determination of acidic or basic components in a gas using this quantitative kit, the material of 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, but from the viewpoint of suitably capturing acidic or basic components in a gas when quantifying acidic or basic components in a gas using this quantitative 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 nonporous 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 improving the efficiency of aeration to collection column B when quantifying acidic or basic components in a gas using this quantitative kit. The upper limit of the average particle size or average cross-sectional diameter of the nonporous 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 improving the efficiency of collecting the acidic or basic components when quantifying acidic or basic components in a gas using this quantitative kit. The method for measuring the average particle size and average cross-sectional diameter in this case is in accordance with JIS K0069 "Test Method for Sieving Chemical Products".

[0050] The basic adsorbent is an adsorbent for adsorbing acidic components, and specifically may consist of or contain a basic substance. The acidic adsorbent is an adsorbent for adsorbing basic components, and specifically may consist of or contain an acidic substance.

[0051] The amount of the basic adsorbent or the acidic adsorbent in the collection column equipped with 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 that it has the effect of preventing column breakthrough when collecting high concentrations of gas. 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 that it has the effect of preventing measurement interference due to excess adsorbent components. The amount of the basic adsorbent or the acidic adsorbent is expressed as an equivalent value and can be measured by the method described in the examples.

[0052] Examples of the basic adsorbent include inorganic bases and organic bases. Examples of the inorganic base include alkali metal carbonates and alkali metal hydroxides. Examples of the organic base include amines and ammonium compounds.

[0053] 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 among the compounds listed above.

[0054] Examples of alkali metal carbonates include sodium carbonate, potassium carbonate, and potassium bicarbonate. Examples of alkali metal hydroxides include strontium hydroxide, potassium hydroxide, and sodium hydroxide. Examples of amines include triethanolamine. Examples of 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] Examples of the aforementioned acidic adsorbent include inorganic acids and organic acids.

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

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

[0059] In a collection column equipped with adsorbent A, the form in which the non-porous substrate holds the basic adsorbent or the acidic adsorbent is not particularly limited. For example, this form may be one in which the solid basic adsorbent or the acidic adsorbent is attached to the surface of the non-porous substrate, or the non-porous substrate may be 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 a 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 only of water. On the other hand, if the basic adsorbent or the acidic adsorbent is a liquid, the basic adsorbent or the acidic adsorbent can be used as is as the liquid phase.

[0061] In a collection column equipped with adsorbent A, the method for covering the non-porous substrate with the liquid phase is not particularly limited. Examples of such methods include coating the non-porous substrate with the liquid phase, and immersing the non-porous substrate in the liquid phase, then removing and drying the non-porous substrate. A specific example of the method for coating the non-porous substrate with the liquid phase is coating it by passing the liquid phase through the porous substrate. Here, "passing through" means passing the liquid phase through a container, such as a column, in which the porous substrate is filled. If the drying conditions are high temperature and long duration, the solvent in the liquid phase may evaporate, and the solid basic adsorbent or acidic adsorbent may precipitate on the surface of the non-porous substrate. In that case, the non-porous substrate can be obtained in a form in which the solid basic adsorbent or acidic adsorbent is attached to the surface.

[0062] In a collection column equipped with adsorbent A, the non-porous substrate may further retain a humectant. If the basic adsorbent or the acidic adsorbent is retained in the liquid phase in the non-porous substrate that further retains the 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% by weight or more and 1.0% by weight or less, and preferably 0.1% by weight or more and 0.5% by weight or less, relative to the total weight of the non-porous substrate covered by the liquid phase.

[0063] A collection column equipped with adsorbent A may consist of a housing (i.e., an outer casing) and a frit, which is a filter placed inside the housing to prevent the non-porous substrate from flowing out. The materials of the housing and the frit are not particularly limited, as long as they do not affect the acidic or basic components to be collected and are not adversely affected by the basic adsorbent or the acidic adsorbent, such as corrosion. Examples of materials for the housing include polypropylene, glass, polyethylene (PE), polyetheretherketone (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 type or different types.

[0064] The shape of the collection column equipped with adsorbent A is not particularly limited, and a cylindrical shape is usually used. Preferably, the collection column equipped with adsorbent A is a column consisting of a column body, frit, sleeve and end fittings, for example, the one described in Japanese Patent Application Publication No. 2001-249120.

[0065] The internal volume of the collection column equipped with adsorbent A (the internal volume of the housing) can be of an appropriate size corresponding to the analytical processing volume. 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 equipped with adsorbent A refers to the volume of gaps in the collection column equipped with adsorbent A that are not filled with the non-porous substrate covered by the liquid phase. The void volume can be measured, for example, by the method described in the examples.

[0067] The larger the aforementioned void volume is above a predetermined value, the greater the amount of gas that passes through collection column B, which is a collection column equipped with adsorbent A, per unit time, i.e., the air permeability, when quantifying acidic or basic components in a gas using this quantitative kit. Here, when quantifying acidic or basic components in a gas using the quantitative kit, a predetermined amount of gas is collected in collection column B, passed through the gas, and the acidic or basic components contained in the predetermined amount of gas are collected. Therefore, the larger the aforementioned void volume, the shorter the time required to pass a predetermined amount of gas through collection column B.

[0068] Therefore, when quantifying acidic or basic components in a gas using this quantitative kit, a larger void volume allows for the rapid collection and quantification of acidic or basic components in the gas. From this viewpoint, the lower limit of the void volume is 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 less than or equal to a predetermined value, the collection column B, which is a collection column equipped with adsorbent A, has a sufficiently large amount of non-porous substrate holding the basic adsorbent or acidic adsorbent, and can adequately secure the ability to collect the acidic or basic components in the gas. Therefore, when quantifying the acidic or basic components in a gas using this quantitative kit, the acidic or basic components in the gas can be collected and quantified with high sensitivity. From the viewpoint of being able to collect and quantify the acidic or basic components in the gas with high sensitivity, the void volume is preferably 5000 μL or less, more preferably 3000 μL or less, even more preferably 600 μL or less, and particularly preferably 500 μL or less.

[0070] It is preferable that the upper limit of the pressure loss when gas is drawn from the collection column equipped with the adsorbent A at a suction rate of 2.0 L / min is 10 kPa or less. Hereinafter, the pressure loss when drawn at a suction rate of 2.0 L / min will be referred to as "pressure loss A". A pressure loss A of 10 kPa or less allows for high-speed collection of the gas to be measured into collection column B, which is equipped with the adsorbent A, without placing a load on the suction pump. Therefore, a predetermined amount of gas can be collected and passed through collection column B, which is equipped with the adsorbent A, in a short time. Consequently, when quantifying acidic or basic components in a gas using this quantitative kit, acidic or basic components in the gas can be collected and quantified in a short time. From this viewpoint, it is preferable that the upper limit of the pressure loss A of the collection column equipped with the adsorbent A is 7 kPa or less, and more preferably 5 kPa or less.

[0071] [Embodiment 3: Quantitative Method] A quantitative method according to one embodiment of the present invention (hereinafter also referred to as "this quantitative method") is: Step A: By passing the solvent through this standard impregnated column, the known amount of acid component or the known amount of base component is eluted into the solvent to obtain eluate A; Step B1 involves passing a gas through an acid component collection column for collecting acidic components in a gas, or a base component collection column for collecting base components in a gas, to collect the acidic or base components in the gas; Step B2 is performed after step B1, by passing a solvent through the acid component collection column that collected the acid component in the gas in step B1 or the base component collection column that collected the base component in the gas in step B1, thereby eluting the collected acid component or base component into the solvent to obtain eluate B; and A method for quantifying the concentration of an acidic component or a basic component in a gas, comprising step C, which involves analyzing eluent A and eluent B and comparing the analysis results of both to quantify the concentration of the acidic component or the basic component in the gas.

[0072] This quantitative method, in essence, is a method for quantifying acidic or basic components in a gas using this standard impregnated column and collection column B, and allows for the simple quantification of the acidic or basic components in the gas.

[0073] In the following, the method for quantifying the concentration of acidic components in a gas using the standard impregnated column for acidic components and column B for acidic component collection will also be referred to as the "method for quantifying acidic components." Furthermore, the method for quantifying the concentration of basic components in a gas using the standard impregnated column for basic components and column B for basic component collection will also be referred to as the "method for quantifying basic components."

[0074] Each step in this quantitative method is described in detail below.

[0075] (Process A) This quantitative method includes step A, which involves passing a solvent through the standard impregnated column to elute a known amount of acidic component or a known amount of basic component into the solvent to obtain eluate A.

[0076] The configuration of the standard impregnation column used in process A can be described by referring to the description of the configuration of the standard impregnation column in [Embodiment 1: Standard Impregnation Column] above.

[0077] In step A, a known amount of the acid component or base component collected on the standard impregnation column, including collection column A, is eluted into the solvent, resulting in eluate A containing a known amount of the acid component or base component. Therefore, eluate A contains a known amount of the acid component or base component that was collected on the standard impregnation column. The solvent is not particularly limited as long as it is capable of eluting the acid component or base component. As the solvent, from the viewpoint of the sensitivity of this quantitative method, it is preferable to use a solvent that does not contain impurities that may cause a decrease in sensitivity, or has an extremely low content of such impurities. From this viewpoint, it is particularly preferable to use pure water as the solvent. Here, pure water means water whose electrical resistivity is in the range of 0.1 MΩ·cm or more and 18 MΩ·cm or less.

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

[0079] Step B1 is, in short, a step of passing a gas through collection column B to collect acidic or basic components in the gas. Hereinafter, step B1, which uses acidic component collection column B to collect acidic components in a gas, will also be referred to as the "acidic component collection step." Similarly, step B1, which uses basic component collection column B to collect basic components in a gas, will also be referred to as the "basic component collection step." Step B1 is either the acidic component collection step or the basic component collection step.

[0080] Regarding the configuration of collection column B used in step B1, the description of the configuration of collection column B described in the [Embodiment 2: Quantitative Kit] section above can be used by reference. Furthermore, the effects of using this quantitative kit in the quantitative determination of acidic or basic components in a gas, as described in the [Embodiment 2: Quantitative Kit] section above, can be used as effects in this quantitative method. Moreover, the acidic or basic components to be collected in step B1 are not particularly limited and may be the acidic or basic components exemplified in the [Embodiment 1: Standard Impregnation Column] section above. Here, from the viewpoint of accuracy of this quantitative method, it is preferable that the acidic or basic components to be collected in step B1 are the same as the acidic or basic components collected in this standard impregnation column used in step A.

[0081] Here, both the acid component collection step and the base component collection step can be carried out simultaneously on the same gas to collect both the acid and base components in the gas.

[0082] In step B1, the gas to be collected is passed through collection column B, thereby collecting acidic or basic components in the gas inside collection column B. This aeration is usually performed using a suction pump.

[0083] In step B1, by passing the gas through the acid component collection column B or the base component collection column B at a higher flow rate, the time required to collect the acid component or the base component in step B1 can be shortened. As a result, the acid component or base component in the gas can be collected in a short time by step B1, and quantification can be performed in a shorter time using this quantitative method. From the viewpoint of collecting the acid component or base component in the gas in a short time and quantifying it in a shorter time using this quantitative 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 the collection column B when passing the gas through will increase, and there is a risk of damage to the collection column B. From the viewpoint of suitably preventing damage to the collection column B, the flow rate is preferably 10 L / min or less, more preferably 7 L / min or less. From the viewpoint of being superior in both the ability to quantify in a shorter time and the ability to prevent damage, the airflow velocity is particularly preferably 5 L / min.

[0084] The ventilation of collection column B is typically performed in the space being evaluated, such as a cleanroom or clean booth. Collection column B is transported by sealing its opening with a stopper that is free from contamination of the analyte, and / or by placing collection column B in a sealed container that is free from contamination of the analyte.

[0085] When carrying out both the acid component collection process and the base component collection process, the acid component collection process and the base component collection process may be carried out continuously using an apparatus equipped with a configuration in which an acid component collection column B and a base component collection column B are arranged in series. That is, the apparatus may be used to draw in air and continuously pass the air through both the acid component collection column B and the base component collection column B that constitute the apparatus. More specifically, (i) the air that has passed through the acid component collection column B may be passed through the base component collection column B, or (ii) the 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 directly connected, or they may be connected via a connecting tube.

[0086] By carrying out the acid component collection step and the base component collection step together, the method for quantifying acid components and the method for quantifying base components can be carried out together. In this case, for example, the air may be drawn 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 constitute the apparatus. After that, the acid component collection column B and the base component collection column B may be separated from the apparatus, and steps B2 and C described below may be carried out for each.

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

[0088] In short, step B2 is a step that, after step B1, involves passing a solvent through the collection column B, which collected the acidic or basic components in the gas in step B1, to elute the acidic or basic components into the solvent and obtain eluate B. Therefore, eluate B contains dissolved amounts of the acidic or basic components collected in step B1.

[0089] The solvent used in step B2 is not particularly limited, as long as it is a solvent capable of eluting the acid component or the base component, similar to step A. As with step A, it is preferable to use a solvent in step B2 that does not contain impurities that could reduce the sensitivity of this quantitative method, or has an extremely low content of such impurities, from this viewpoint. From this perspective, it is particularly preferable to use pure water as the solvent in step B2. Furthermore, from the viewpoint of accuracy, it is preferable to use the same type of solvent in step B2 as in step A.

[0090] (Process C) This quantitative method includes step C, which involves analyzing eluate A and eluate B and comparing the analysis results of both to quantify the concentration of the acidic component or the basic component in the gas.

[0091] The aforementioned step C may be, for example, one of the steps (1) to (4) below. (1) The "standard result" can be obtained by analyzing eluate A, which contains a known amount of acid or base component, using a method to quantify the acid or base component, and from the standard result, a correspondence A can be obtained. (2) Using the eluate B containing acidic or basic components in the collected gas, a numerical value corresponding to the amount of acidic or basic components contained in the eluate B is obtained using the same method as the method for quantifying the acidic or basic components in (1) above. (3) The numerical values ​​obtained in (2) above are converted to the amount of acidic or basic components contained in eluent B based on the correspondence relationship A obtained in (1) above, and the amount of acidic or basic components contained in eluent B is calculated. (4) The concentration of the acid component or base component in the gas is calculated by dividing the amount of the acid component or base component obtained in (3) by the amount of gas that was passed through the collection column B in step B1.

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

[0093] In (1) and (2) above, the method for quantifying the acid component or the base component in eluate A and eluate B (hereinafter also referred to as "the measurement method") can be a known method and is not particularly limited. The measurement method may 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 acidic component exists as anions in eluate A and eluate B, and the basic component exists as cations in eluate A and eluate B. Therefore, in (1), the "standard result" and correspondence A are obtained for the total amount of anions or cations in eluate A, and these can be used as the "standard result" and correspondence A for the known amount of acidic or basic component. Similarly, in (2), a numerical value corresponding to the total amount of anions or cations in eluate B is obtained, and this numerical value can be used as the numerical value corresponding to the amount of acidic or basic component collected in step B1.

[0095] [Embodiment 4: Method for controlling the cleanliness of a space] A method for controlling the cleanliness of a space according to one embodiment of the present invention (hereinafter also referred to as "this control method") is a method for controlling the cleanliness of a space, comprising: a quantitative step of quantifying the concentration of an acidic component or a basic component in a gas within a space using this quantitative method; and a step of identifying and removing the source of the acidic component or basic component in the gas inside the space when the concentration of the acidic component or basic component quantified in the quantitative step exceeds a threshold.

[0096] As described above, this quantitative method allows for the easy quantification of acidic or basic components contained in a gas through simplified procedures. Therefore, this control method can be easily implemented, and consequently, a clean environment can be easily secured using this method.

[0097] (Quantitative process) This control method includes a quantitative step of quantifying the concentrations of acidic and basic components in the gas within a space using this quantitative method. By performing the quantitative step, the concentrations of acidic and basic components, which are pollutants in the space, can be easily (simplely) quantified.

[0098] The space referred to in this specification is the space to be evaluated using this quantitative method, and may be, for example, a space where the concentrations of the acidic and basic components as contaminants must be below a specific threshold for use in operations such as the manufacture of electronic circuit boards. The space referred to in this control method may typically be a space with a predetermined volume formed by walls, floors, etc. The space is not particularly limited and may include, for example, a cleanroom, a clean booth, or the space inside a manufacturing apparatus.

[0099] The configuration of the quantitative method in the aforementioned quantitative process shall be based on the configuration described in [Embodiment 3: Quantitative Method] above.

[0100] In this management method, in order to easily secure a clean space, the amount (concentration) of the acid component and / or base component, which are contaminants in the space, is easily quantified, and the source of contamination is identified and excluded 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 the acid component quantification method and the base component quantification method may be performed simultaneously, but it is preferable to perform the acid component quantification method and the base component quantification method simultaneously. In order to perform these simultaneously, it is preferable to use an apparatus equipped with a configuration in which the acid component collection column B and the base component collection column B described above are arranged in series. When using such an apparatus, air can be passed through both the acid component collection column B and the base component collection column B that constitute the apparatus with a single suction to the apparatus, so the quantification step and this management method can be performed more easily.

[0101] (The process of identifying and eliminating the source of contamination) This control method includes a step of identifying and removing the source of the acidic or basic component in the gas inside the space when the concentration of the acidic or basic component quantified in the quantitative step exceeds a threshold. In this specification, "the source of the acidic or basic component in the gas inside the space" is also referred to as "the source of contamination." Therefore, "the step of identifying and removing the source of the acidic or basic component in the gas inside the space" is "the step of identifying and removing the source of contamination." By performing the step of identifying and removing the source of contamination, the concentration of the acidic or basic component, which is a pollutant, inside the space can be controlled to be below the threshold, and a clean space can be easily secured.

[0102] The threshold value in the aforementioned process can be appropriately determined based on the type of operation performed in the space and the quality required for the product manufactured by that 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 These are possible.

[0103] Identifying and eliminating the aforementioned source of contamination means determining the concentrations of the acidic and basic components, which are contaminants, within the space and taking corresponding actions. The specific method for doing so is not particularly limited, and known methods can be employed.

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

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

[10] [6], Step A involves passing a solvent through the standard impregnation column to elute the known amount of acid or the known amount of base into the solvent, thereby obtaining eluate A. Step B1 involves 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, to collect the acid component or base component in the gas. Step B2 is performed after step B1, by passing a solvent through the acid component collection column that collected the acid component in the gas in step B1 or the base component collection column that collected the base component in the gas in step B1, thereby eluting the collected acid component or base component into the solvent to obtain eluate B, and A quantitative method comprising step C, which involves analyzing eluate A and eluate B and comparing the analysis results of both to quantify the concentration of the acid component or the base component in the gas. A quantitative step of quantifying the concentration of the acid component or the base component in a gas in space using the quantitative method described in

[11]

[10] , and A method for controlling the cleanliness of a space, comprising the step of identifying and removing the source of the acidic or basic component in the gas inside the space when the concentration of the acidic or basic component quantified in the quantitative step exceeds a threshold. [Examples]

[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] The following describes the method used in the examples to measure the numerical values ​​corresponding to the amount of basic or acidic components contained in the eluate obtained from the standard impregnation column and the collection column.

[0107] (Ion chromatograph) In the examples, eluate A or eluate B was analyzed using an ion chromatograph in the manner described below, and a numerical value corresponding to the amount of acidic or basic component contained in eluate A or eluate B was measured.

[0108] Elutions A and B were analyzed using a dual-channel ion chromatography system equipped with electrical conductivity detection. The anion channel of the ion chromatography system used a potassium hydroxide eluent gradient, an anion analysis column, and a suppressor. The cation channel of the ion chromatography system used a methanesulfonic acid eluent gradient, a cation analysis column, and a suppressor.

[0109] [Manufacturing Example 1: Preparation of Basic Component Collection Column A and Basic Component Collection Column B] 0.9 g of quartz particles with a particle size 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, it was washed by passing ultrapure water (resistivity of 0.1 MΩ·cm or higher) through the inside of the column.

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

[0111] Furthermore, five basic component collection columns B, having the same configuration as the basic component collection column A, were prepared by repeating the same method five times.

[0112] [Example 1: Preparation of this standard impregnation column for basic components] To the basic component collection column A prepared in Production Example 1, 50 ng of ammonium ions (NH4) were added to the basic component collection column A by the method of adding a standard solution. + A standard impregnation column for basic components was prepared by impregnating it with ammonium ions (NH4). Specifically, 5 μL of an ammonium ion standard solution with an ammonium ion concentration of 10 μg / mL was added to the basic component collection column A using a micropipette, and then dried by passing clean nitrogen gas through it. As a result, 50 ng of ammonium ions (NH4) was obtained. + A standard pre-doped column for basic components was prepared with ) attached.

[0113] A standard impregnated column for the prepared basic component was passed through 10 mL of pure water to prepare eluate A, which contained ammonium ions, the basic component impregnated on the column. The peak area, a numerical value corresponding to the amount of the basic component, was obtained from the prepared eluate A using the ion chromatograph. The obtained peak area is referred to as "peak area A". Specific numerical values ​​for peak area A are shown in Table 1 below.

[0114] [Examples 2-6] A room was prepared, partly consisting of a clean booth. In this room, each of the basic component collection columns B prepared in Production Example 1 was aerated at a flow rate of 2 L / min for 125 minutes at any one location outside the clean booth and at any four locations inside the clean booth. Subsequently, 10 mL of pure water was passed through each of the aerated basic component collection columns B, as in Example 1, to prepare eluate B. For each prepared eluate B, the peak area, which is a numerical value corresponding to the amount of the basic component, was obtained using the ion chromatograph. The obtained peak area is referred to as "peak area B". The example where aeration was performed at one location outside the clean booth was designated as Example 2, and the examples where aeration was performed at each of the four locations inside the clean booth were designated as 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 basic component in the gas aerated at 250 L was calculated based on the following formula (I). Concentration of basic components in a gas = (0.2 × area B) / area A [μg / m²] 3 ]...Formula (I) Table 1 below shows the concentrations of the base component in the gas calculated using formula (I) in each of Examples 2 to 6.

[0116] [Table 1]

[0117] [Manufacturing Example 2: Preparation of Acid Component Collection Column A and Acid Component Collection Column B] 0.9 g of quartz particles with a particle size 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, it was washed by passing ultrapure water (resistivity of 0.1 MΩ·cm or higher) through the inside of the column.

[0118] After passing a mixed aqueous solution of sodium carbonate and glycerin through the column after washing, clean air was passed through to perform drying, and a column A for collecting acid components was prepared.

[0119] Also, the same method as the above method was repeated 5 times to prepare 5 columns B for collecting acid components having the same configuration as the column A for collecting acid components.

[0120] [Example 7: Production of the standard-attached column for acid components] For the column A for collecting acid components prepared in Production Example 2, by the method of adding a standard solution, 50 ng or 100 ng of an acid component mixture composed of each acid component of formic acid, acetic acid, fluoride ion (F - ), chloride ion (Cl - ), bromide ion (Br - ), nitrite ion (NO2 - ), nitrate ion (NO3 - ), sulfate ion (SO4 2- ) and phosphate ion (PO4 3- ) was attached, and a standard-attached column for acid components was manufactured. Specifically, 5 μL of an acid component standard solution in which each concentration of the acid component mixture was 10 μg / mL or 20 μg / mL was added to the column A for collecting acid components using a micropipette, and then clean nitrogen gas was passed through for drying. As a result, a standard-attached column for acid components to which 50 ng or 100 ng of the acid component was attached was manufactured. Here, the amounts of each acid component contained in 5 μL of the acid component standard solution are shown in Table 2 below. Also, the amounts of each acid component contained in 5 μL of the acid component standard solution are also the amounts of each acid component attached to the standard-attached column for acid components.

[0121]

Table 2

[0122] Ten milliliters of pure water were passed through a standard impregnated column for the prepared acid component to prepare eluate A, which contained the acid component mixture impregnated on the standard impregnated column. Using the ion chromatograph, peak areas corresponding to the amounts of each acid component constituting the acid component mixture were obtained from the prepared eluate A. The obtained peak area is referred to as "peak area A".

[0123] [Examples 8-12] A room was prepared, part of which was a clean booth. In this room, at any one location outside the clean booth and at any four locations inside the clean booth, each of the acid component collection columns B prepared in Production Example 2 was subjected to an airflow of 2 L / min for 125 minutes. After that, 10 mL of pure water was passed through each of the aerated acid component collection columns B, as in Example 1, to prepare eluate B. For each of the prepared eluate 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 the gas aerated at 250 L was calculated based on the following formula (II). Concentration of acid component in gas = (0.2 × area B) / area A [μg / m²] 3 ]...Formula (II) Table 3 below shows the concentrations of each acid component in the gas calculated using formula (II) in each of Examples 8 to 12.

[0125] [Reference examples 1~5] A five-point checkpoint curve was created for each acid component, showing the correspondence between the peak area corresponding to the amount of each acid component obtained using the ion chromatograph used in Examples 8-12 described above, and the amount (mass) of each acid component in the eluate. Specifically, first, five types of 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, prepared using pure water as the solvent. Next, for each of the five types of standard solutions, five peak areas corresponding to the amount of each acid component in each standard solution were obtained using the ion chromatograph. The five-point checkpoint curve was created by plotting the five obtained peak areas against the amount of each acid component corresponding to each peak area.

[0126] Using the aforementioned 5-point calibration curve, the concentration of each acid component in the eluate was calculated by converting the peak area B corresponding to the amount of each acid component obtained in Examples 8 to 12. Furthermore, the calculated concentration of each acid component in the eluate was used, and the product of the concentration of each acid component in the eluate and the volume of the eluate was used, along with the aeration rate: 2L × 125 min = 250L = 250 × 10 -3 m 3 Based on this, the concentrations of each acid component in the gas were calculated. Furthermore, using the peak area B corresponding to the amount of each acid component obtained in each of Examples 8 to 12, and using the calibration curve, examples of calculating the mass and concentration of each acid component in the gas are shown in Table 3 below, as Reference Examples 1 to 5. In Table 3 below, the units of the concentrations of each acid component are [ng / L = μg / m³]. 3 It is represented as ].

[0127] [Table 3]

[0128] As shown in Tables 1 and 3, the quantitative methods described in Examples 2-6 and 8-12 demonstrated that the concentrations of components in a gas could be quantified without any problems. Furthermore, since the results of Examples 8-12 and Reference Examples 1-5 were substantially identical, it was found that the concentrations of acidic or basic components contained in a gas can be easily quantified using this standard impregnation column, quantitative kit, and quantitative method, even without the need to create a calibration curve. [Industrial applicability]

[0129] This standard impregnation column, quantitative analysis kit, and quantitative analysis method allow for the simple determination of the concentration of acidic or basic components in a gas. Furthermore, this quantitative analysis method, along with the control method utilizing it, enables the simple creation of a clean environment. Therefore, this standard impregnation column, quantitative analysis kit, quantitative analysis method, and control method can be used for managing spaces required for tasks such as the manufacturing of electronic circuit boards, where a clean environment is necessary.

Claims

1. A standard impregnation column for the quantitative determination of the concentration of acidic or basic components in a gas, The standard impregnated column is a standard impregnated 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 known amount of base component is impregnated onto a base component collection column for collecting base components in a gas.

2. The standard impregnation column according to claim 1, wherein the amount of the known acid component or the known base component is greater than 1 ng and less than or equal to 1,000 μg.

3. The column for collecting the aforementioned acidic or basic components is: A non-porous substrate is filled in, The non-porous substrate holds a basic adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing basic components. The pressure loss when the gas in the collection column for the acidic or basic component is drawn out at a suction rate of 2.0 L / min is 10 kPa or less. A standard impregnated column according to claim 1 or 2.

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

5. The standard impregnation 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 determining the concentration of acidic and / or basic components in a gas, which satisfies one or more of the following conditions (a) and (b): (a) comprising one or more standard impregnation columns impregnated with a known amount of acid component as described in claim 1 or 2, and one or more acid component collection columns for collecting acid components in a gas, (b) A kit for determining the concentration of acidic and / or basic components in a gas, comprising one or more standard impregnation columns impregnated with a known amount of basic component as described in claim 1 or 2, and one or more basic component collection columns for collecting basic components in a gas.

7. The column for collecting the aforementioned acidic or basic components is: A non-porous substrate is filled in, The non-porous substrate holds a basic adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing basic components. The pressure loss when the gas in the collection column for the acidic or basic component is drawn out at a suction rate of 2.0 L / min is 10 kPa or less. A kit for determining the concentration of acidic and / or basic components in a gas, as described in claim 6.

8. The kit for determining the concentration of acidic and / or basic components 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. The kit for determining the concentration of acidic and / or basic components 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 determining the concentration of acidic and / or basic components in a gas, using the kit for determining the concentration of acidic or basic components in a gas as described in claim 6, Step A involves passing a solvent through the standard impregnation column to elute the known amount of acid component or the known amount of base component into the solvent, thereby obtaining eluate A. Step B1 involves 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, to collect the acid component or base component in the gas. Step B2 is performed after step B1, by passing a solvent through the acid component collection column that collected the acid component in the gas in step B1 or the base component collection column that collected the base component in the gas in step B1, thereby eluting the collected acid component or base component into the solvent to obtain eluate B, and A quantitative method comprising step C, which involves analyzing eluent A and eluent B and comparing the analysis results of both to quantify the concentration of the acid component or the base component in the gas.

11. A quantitative step of quantifying the concentration of an acidic or basic component in a gas in a space using the quantitative method described in claim 10, and A method for controlling the cleanliness of a space, comprising the step of identifying and removing the source of the acidic or basic component in the gas inside the space when the concentration of the acidic or basic component quantified in the quantitative step exceeds a threshold.

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