Standard pre-attached material tubular column for quantifying concentration of acid component or alkali component in gas and application of standard pre-attached material tubular column

Abstract

Provided are: a standard pre-charge string for use in a quantification method that can simply quantify the concentration of an acid component or an alkali component contained in a gas by supplying energy with a simple operation; a known amount of an acid component is pre-added to an acid component trapping string for trapping the acid component in the gas of the standard pre-charge string, or a known amount of an alkali component is pre-added to an alkali component trapping string for trapping the alkali component in the gas of the standard pre-charge string.

Description

Technical Field

[0001] This invention relates to quantitative standard pre-attached tubing for quantifying the concentration of acidic or alkaline components in gases, and its applications. Specifically, these applications include quantitative reagent kits for quantifying the concentration of acidic and / or alkaline components in gases, quantitative methods for quantifying the concentration of acidic or alkaline components in gases, and methods for managing cleanroom conditions. Background Technology

[0002] In environments where electronic substrates (hereinafter referred to as substrates) such as semiconductor wafers, liquid crystal substrates, and hard disks are manufactured, contaminants such as acids (acidic components) and alkalis (alkaline components) in the manufacturing space can sometimes adhere to the substrates, leading to reduced product yield and quality. To prevent this reduction in yield and quality, the substrate manufacturing process is carried out in a cleanroom. Furthermore, it is necessary to evaluate the cleanroom's cleanliness level (i.e., the level of contamination caused by acids and alkalis during each manufacturing process) and to eliminate the cause of contamination if the cleanliness level deteriorates, thereby managing the cleanroom's cleanliness. In recent years, with cleanrooms being required to maintain a high level of cleanliness, there is a growing demand for methods to evaluate the cleanliness level caused by acids or alkalis within the cleanroom with higher sensitivity. Moreover, in recent years, there has been a demand to simplify cleanroom cleanliness management and shorten the evaluation time.

[0003] Regarding methods for evaluating cleanliness with high sensitivity and short time, examples include the methods described in Patent Documents 1 and 2 for quantifying contaminants using a gas adsorption column, and the method described in Patent Document 3 for quantifying contaminants using a liquid-free trap. Here, the contaminants refer to acidic and / or alkaline components in the air. Specifically, the method for quantifying the contaminants involves passing air from the cleanroom through the gas adsorption column or the 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 acid and / or alkali in a gas sample, standard solutions containing trace amounts of acid and / or alkali are typically used. These standard solutions are prepared by specially trained professionals.

[0005] [Existing Technical Documents]

[0006] Patent Document 1: Japanese Patent Application Publication No. 2009-14522

[0007] Patent Document 2: International Publication No. 2010 / 067464

[0008] Patent Literature 3: Japanese Patent No. 6563396 SUMMARY

[0009] (PROBLEMS TO BE SOLVED BY THE INVENTION)

[0010] As described above, in the conventional quantitative method described above, the preparation operation of the standard solution, particularly the operation of preparing the standard solution by a specially trained professional in the case where high sensitivity quantification is required, is very complicated.

[0011] Therefore, an object of the present application is to provide a quantitative method capable of easily quantifying the concentration of an acid component or a base component contained in a gas, and a standard pre-adsorption column and a quantitative kit for use in the quantitative method. In addition, another object of the present application is to provide a space cleanliness management method capable of easily ensuring a clean space.

[0012] (Technical Means for Solving the Problems)

[0013] To achieve the object, a standard pre-adsorption column according to an embodiment of the present application is a standard pre-adsorption column for quantifying the concentration of an acid component or a base component in a gas,

[0014] The acid component trapping column for trapping an acid component in a gas is pre-adsorbed with a known amount of the acid component, or the base component trapping column for trapping a base component in a gas is pre-adsorbed with a known amount of the base component.

[0015] To achieve the object, a quantitative kit according to an embodiment of the present application is a quantitative kit for quantifying the concentration of an acid component and / or a base component in a gas, which satisfies the following requirements (a) and / or (b):

[0016] (a) contains one or more standard pre-adsorption columns pre-adsorbed with a known amount of an acid component as described in claim 1 or 2, and one or more acid component trapping columns for trapping an acid component in a gas,

[0017] (b) contains one or more standard pre-adsorption columns pre-adsorbed with a known amount of a base component as described in claim 1 or 2, and one or more base component trapping columns for trapping a base component in a gas.

[0018] To achieve the object, a quantitative method according to an embodiment of the present application quantifies the concentration of an acid component and / or a base component in a gas using the quantitative kit, and the quantitative method includes:

[0019] Step A, flowing a solvent through the standard preconcentration column to elute the known amount of the acid component or the known amount of the base component into the solvent to obtain eluate A;

[0020] Step B1, flowing a gas through a column for capturing an acid component in the gas or a column for capturing a base component in the gas to capture the acid component or the base component in the gas;

[0021] Step B2, after the step B1, flowing a solvent through the column for capturing the acid component in the gas in the step B1 or the column for capturing the base component in the gas in the step B1 to elute the captured acid component or the captured base component into the solvent to obtain eluate B; and

[0022] Step C, 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 results of the analysis.

[0023] To achieve the object, an embodiment of the present application relates to a management method for managing cleanliness of a space, comprising:

[0024] a quantification step of quantifying the concentration of the acid component or the base component in the gas in the space using the aforementioned quantification method; and

[0025] an exclusion step of determining and excluding a source of the acid component or the base component in the gas in the interior of the space when the concentration of the acid component or the base component quantified in the quantification step exceeds a threshold value.

[0026] (EFFECT OF INVENTION)

[0027] According to one aspect of the present application, a quantification method capable of easily quantifying the concentration of an acid component or a base component contained in a gas, and a standard preconcentration column and a quantification kit for use in the quantification method can be provided. In addition, according to one aspect of the present application, a space cleanliness management method capable of easily ensuring cleanliness of a clean space can be provided. DETAILED DESCRIPTION

[0028] An embodiment of the present application will be described below, but the present application is not limited to the following described embodiments. The present application can be variously changed within the technical concept described in the specification, and embodiments obtained by appropriately combining the technical means disclosed in each of the embodiments are also included in the technical scope of the present application.

[0029] [Embodiment 1: Standard Preconcentration Column]

[0030] The standard pre-adsorption column (hereinafter, also referred to as "the present standard pre-adsorption column") according to an embodiment of the present application is a standard pre-adsorption column used for quantifying the concentration of an acid component or a base component in a gas. As for the standard pre-adsorption column, an acid component trapping column for trapping an acid component in a gas is pre-adsorbed with a known amount of the acid component, or a base component trapping column for trapping a base component in a gas is pre-adsorbed with a known amount of the base component. Here, the "acid component trapping column / base component trapping column pre-adsorbed with a known amount of the acid component / base component" means that an adsorbent material filled in the acid component trapping column / base component trapping column is pre-adsorbed with a known amount of the acid component / base component.

[0031] As the "trapping column" described in the present specification, the "acid component trapping column A", "base component trapping column A", "trapping column A", "acid component trapping column B", "base component trapping column B", and "trapping column B" described later can be given.

[0032] In the present specification, as for the present standard pre-adsorption column, the standard pre-adsorption column in which the acid component trapping column for trapping an acid component in a gas is pre-adsorbed with a known amount of the acid component is also referred to as a "standard pre-adsorption acid column". The standard pre-adsorption acid column is a standard pre-adsorption column used for quantifying the concentration of an acid component in a gas. On the other hand, in the present specification, as for various present standard pre-adsorption columns, the standard pre-adsorption column in which the base component trapping column for trapping a base component in a gas is pre-adsorbed with a known amount of the base component is also referred to as a "standard pre-adsorption base column". The standard pre-adsorption base column is a standard pre-adsorption column used for quantifying the concentration of a base component in a gas.

[0033] In the present specification, the "acid component trapping column for trapping an acid component in a gas" used to constitute the standard pre-adsorption acid column is also referred to as an "acid component trapping column A". In addition, in the present specification, the "base component trapping column for trapping a base component in a gas" used to constitute the standard pre-adsorption base column is also referred to as a "base component trapping column A". In the present specification, the acid component trapping column A and the base component trapping column A are also simply referred to as a "trapping column A".

[0034] The standard pre-attached column is a column to which a known amount of an acid component or a known amount of a base component is pre-attached to column A for trapping an acid component or column A for trapping a base component. In this case, when the amount of the known amount of the acid component or the known amount of the base component pre-attached to the standard pre-attached column is measured by a predetermined method, a predetermined value corresponding to the amount of the known amount of the acid component or the known amount of the base component can be obtained as a result of the measurement. Hereinafter, the obtained predetermined value is referred to as a "standard result". In addition, a correspondence relationship between the known amount and the standard result can be derived. Hereinafter, the correspondence relationship is also referred to as a "correspondence relationship A".

[0035] In this case, the unknown amount of the acid component or the base component trapped by the acid component trapping column or the base component trapping column for trapping an acid component or a base component in a gas other than column A for trapping can also be quantified by the same method as that employed when the correspondence relationship is derived. In this case, a value corresponding to the unknown amount can be obtained.

[0036] In the present specification, the acid component trapping column for trapping an acid component in a gas other than column A for trapping is also referred to as "acid component trapping column B". In addition, in the present specification, the base component trapping column for trapping a base component in a gas other than column A for trapping is also referred to as "base component trapping column B". Furthermore, in the present specification, the acid component trapping column B and the base component trapping column B are also collectively referred to as "trapping column B". In addition, in the present specification, the correspondence relationship between the unknown amount and the value corresponding to the unknown amount obtained in the case where the unknown amount of the acid component or the base component trapped by the trapping column B is quantified is also referred to as a "correspondence relationship B".

[0037] In this case, if the amount of the acid component or the base component trapped by the standard pre-attached column and the trapping column B and the like is measured, an eluent containing almost the entire amount of the trapped acid component or base component is generally required to be prepared, and the eluent is analyzed. In this case, "almost the entire amount" means that the amount of the acid component or the base component remaining after elution is an amount that can be ignored for quantification. Through the analysis, a value corresponding to almost the entire amount of the trapped acid component or base component can be obtained. Therefore, the correspondence relationship A and the correspondence relationship B both involve a value corresponding to almost the entire amount of the acid component or the base component measured by the same method with the almost the entire amount of the acid component or the base component and the eluent containing almost the entire amount of the trapped acid component or base component as the subject. Therefore, it can be considered that the correspondence relationship A and the correspondence relationship B are substantially identical.

[0038] Here, for example, let the known quantity be α1, the value of the standard result be β1, the unknown quantity be α2, and the value corresponding to the unknown quantity be β2. In this case, the correspondence A is "α1 / β1", the correspondence B is "α2 / β2", and we can consider "α1 / β1=α2 / β2". At this time, we can obtain the relationship "α2=β2×(α1 / β1)". For example, if we take the volume of gas supplied to the collection column B associated with the measurement result of α2 as V, we can consider the concentration of the acid or base component in the gas as "α2 / V".

[0039] Using the pre-attached tubing of this standard, the amount and concentration of the acid or alkali component captured by the collection tubing B can be calculated.

[0040] As an example of the specified method, an eluent may be prepared by eluting the acidic or alkaline component, and the acidic or alkaline component in the eluent may be quantified using a known method. Here, the known method is not particularly limited; for example, it may be liquid chromatography. Regarding liquid chromatography, examples include anion exchange and cation exchange methods using ion exchange columns, and suppressor-type ion chromatography using suppressors. Furthermore, if the eluent is prepared and the acidic or alkaline component in the eluent is quantified using liquid chromatography, the obtained value may be the peak area. Additionally, as a method for preparing the eluent, an example may be preparing the eluent by passing a solvent through a standard pre-added column to elute the acidic or alkaline component pre-added to the solvent.

[0041] (Acid-containing trapping column, alkali-containing trapping column)

[0042] This standard pre-attached feed column includes a collection column A. In one embodiment of the invention, the collection column A is not particularly limited as long as it is capable of collecting a known amount of acid or alkali components, or acid or alkali components in a gas.

[0043] Here, it is envisioned that the standard pre-attached column and the trapping column B are used to quantify the concentration of acid or alkali components in a gas. If the trapping column A of the standard pre-attached column has the same configuration as the trapping column B, then the difference between the amount of acid or alkali components remaining in the standard pre-attached column after elution and the amount of acid or alkali components remaining in the trapping column B will be small. Therefore, the consistency between correspondence A and correspondence B is improved, and the accuracy of the quantification is increased. Therefore, in the quantification, it is preferable that the trapping column A and the trapping column B have similar structures, and more preferably, they have the same structure.

[0044] In particular, when the amount of the acid component or the base component trapped by the trapping column B is extremely small, the effect of the residual acid component or the residual base component is relatively large. Therefore, when the amount of the acid component or the base component is quantified, that is, when the quantification is performed with high sensitivity, it is particularly preferable that the trapping column A provided in the standard pre-packed column has the same configuration as the trapping column B.

[0045] Here, when the trapping column A and the trapping column B have the same configuration, for example, the trapping column A and the trapping column B can both have the adsorbent material A described later. In addition, when the trapping column A and the trapping column B have the same configuration, for example, the trapping column A and the trapping column B can both have the adsorbent material A, and the type, the content, the size, and the void volume of the non-porous base material described later and the basic adsorbent or the acidic adsorbent described later can be the same.

[0046] In summary, as the preferable configuration of the trapping column A provided in the standard pre-packed column, it is preferable that the trapping column A has the same configuration as the trapping column B, and specifically, it is preferable that the trapping column A has the preferable configuration described in the "(trapping column B)" column in the "[Embodiment 2: Quantification kit]" column described later.

[0047] (Acid component, base component)

[0048] The standard pre-packed column contains a known amount of an acid component or a known amount of a base component. In the standard pre-packed column, the acid component or the base component is in a state of being pre-added to the trapping column A. The acid component or the base component in the standard pre-packed column is not particularly limited as long as it is an acid component or a base component that can be pre-added to the trapping column A.

[0049] In one embodiment of the present application, the acid component is not particularly limited. As the acid component, for example, hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, hydrofluoric acid, formic acid, acetic acid, bromic acid, iodine, lactic acid, propionic acid, butyric acid, valeric acid, and the like can be exemplified as the acid itself, and ammonium fluoride, ammonium formate, ammonium acetate, and the like can be exemplified. In addition, in one embodiment of the present application, the base component is not particularly limited. As the base component, for example, ammonia, trimethylamine, triethylamine, alkanolamine, dimethylamine, diethylamine, and the like can be exemplified as the base itself, and ammonium fluoride, ammonium formate, ammonium acetate, and the like can be exemplified.

[0050] The standard pre-packed column is a column in which a known amount of the acid component or a known amount of the base component is pre-added to the trapping column A. In one embodiment of the present application, the method of pre-adding a known amount of the acid component or a predetermined amount of the base component to the trapping column A is not particularly limited, and a standard solution addition method and the like can be exemplified.

[0051] The known amount is not particularly limited as long as it is an amount that is below the limit amount that can be trapped by the trapping column A and that enables the correspondence to be obtained by the standard pre-attached column.

[0052] Regarding the limit amount that can be trapped by the trapping column A, if the trapping column A is provided with the adsorbent material A, the limit amount depends on the amount (equivalent amount) of the basic adsorbent or the acidic adsorbent held by the adsorbent material A, and the limit value increases as the equivalent amount is larger. Therefore, in the case where the trapping column A is provided with the adsorbent material A, the limit value can be controlled by adjusting the equivalent amount of the basic adsorbent or the acidic adsorbent held by the adsorbent material A.

[0053] In addition, from the viewpoint of the accuracy of the quantitative method using the standard pre-attached column, it is preferable that the value of the known amount be close to (for example, be of the same order of magnitude as) the expected trapping amount of the acidic component or the basic component that is trapped by the trapping column B in the quantitative method using the standard pre-attached column. The reason for this is that the identity between the correspondence A and the correspondence B in this case can be improved.

[0054] The known amount is not particularly limited, but specifically, it is preferably greater than 1 ng, more preferably 5 ng or greater, and further preferably 10 ng or greater. In the case where the quantitative method is used to quantify a trace amount of an acidic component or a trace amount of a basic component in a gas, from the viewpoint of the accuracy of the quantitative method, the known amount is preferably 1000 μg or less, more preferably 100 μg or less, and further preferably 10 μg or less.

[0055] Furthermore, from the viewpoint of the accuracy of the quantitative method, the kind of the acidic component or the basic component in the standard pre-attached column is preferably the same as the kind of the acidic component or the basic component that is expected to be trapped by the trapping column B in the quantitative method. For example, if it is expected that ammonia in a gas will be trapped in the trapping column B and its concentration will be measured in the quantitative method, it is preferable that ammonia (ammonium ion) be used as the basic component in the standard pre-attached column.

[0056] [Embodiment 2: Quantitative kit]

[0057] The quantitative kit of one embodiment of the present application (hereinafter also referred to as "the present quantitative kit") is a quantitative kit for quantifying an acidic component and / or a basic component in a gas, and includes one or more standard pre-attached columns to which a known amount of an acidic component has been pre-attached and one or more acidic component trapping columns for trapping an acidic component in a gas, and / or one or more standard pre-attached columns to which a known amount of a basic component has been pre-attached and one or more basic component trapping columns for trapping a basic component in a gas.

[0058] In summary, the present quantitative kit is a quantitative kit comprising a combination of one or more of the present standard pre-column and one or more of the trapping column B. Here, the quantitative method for the acid component or the base component in the gas using the present standard pre-column is a method for quantifying the acid component or the base component in the gas using the present standard pre-column and the trapping column B. Therefore, the quantitative method for the acid component or the base component in the gas using the present standard pre-column can be equivalent to the quantitative method for the acid component or the base component in the gas using the present quantitative kit. As described above, the quantitative method for the acid component or the base component in the gas using the present standard pre-column can easily quantify the concentration of the acid component or the base component contained in the gas. Therefore, according to the present quantitative kit, a quantitative method that can easily quantify the concentration of the acid component or the base component contained in the gas can be implemented by a simple operation.

[0059] (The present standard pre-column)

[0060] As for the constitution of the present standard pre-column constituting the present quantitative kit and the like, the constitution of the present standard pre-column described in the aforementioned "[Embodiment 1: Standard pre-column]" column can be cited.

[0061] (The trapping column B)

[0062] As the trapping column B, as with the trapping column A, there is no particular limitation as long as it can trap the acid component or the base component in the gas. In addition, for the reason described later, it is preferable that the trapping column B is filled with a non-porous base material that holds a basic adsorbent for adsorbing the acid component or an acidic adsorbent for adsorbing the base component. Hereinafter, the non-porous base material that holds a basic adsorbent for adsorbing the acid component or an acidic adsorbent for adsorbing the base component will be simply referred to as "adsorption material A".

[0063] Even in the case where the non-porous base material has a weak adsorption force for the adsorption target substance and adsorbs a very small amount of the substance, the adsorbed substance can be easily desorbed into the solvent. Therefore, by the quantitative method using the trapping column having the adsorption material A, the amount of the acid component or the base component remaining in the trapping column after elution can be reduced, and thus a value that corresponds better to the total amount of the trapped acid component or the base component can be obtained. Therefore, in the trapping column B, particularly in the trapping column B constituting the present quantitative kit for quantifying a very small amount of the acid component or the base component, it is preferable that the non-porous base material is filled. In this case, the precision of the quantification of the acid component or the base component in the gas using the present quantitative kit can be improved.

[0064] In addition, the trapping column provided with the adsorbent A has a non-porous base material filled therein, and the non-porous base material does not adsorb other substances. Therefore, it is possible to prevent the precision of the quantification of the acid component or the base component in the gas using the present quantification kit from being reduced due to the presence of the other substances as noise.

[0065] In the above, in the case where the trapping column B is the trapping column provided with the adsorbent A, it is possible to improve the precision of the quantification of the acid component or the base component in the gas using the present quantification kit. In addition, in the case of the quantification, it is possible to trap and quantify the acid component or the base component in the gas with high sensitivity. In addition, in the present specification, the trapping and quantification with high sensitivity means, for example, the trapping and quantification of the concentration of the acid component or the base component in the gas in the order of about 10 -2 μg / m 3 In other words, in the case where the trapping column B is the trapping column provided with the adsorbent A, it is possible to trap and quantify a trace amount of the acid component or a trace amount of the base component by using the present quantification kit in the quantification of the acid component or the base component in the gas.

[0066] Therefore, in the case where the trapping column B is the trapping column provided with the adsorbent A, it is possible to simply and easily quantitate the acid component or the base component in the gas with high precision by using the present quantification kit by a simple operation. In addition, in the case where the trapping column B is the trapping column provided with the adsorbent A, it is possible to simply quantitate a trace amount of the acid component or a trace amount of the base component in the gas by using the present quantification kit.

[0067] Hereinafter, the detailed structure of the trapping column B provided with the adsorbent A will be described.

[0068] The non-porous base material is not particularly limited as long as it is in a state of not having a hole. As the material of the non-porous base material, for example, quartz, glass, polycarbonate resin, polystyrene resin, polyamide resin, silicon carbide (SiC), aluminum oxide (AI2O3), silicon nitride (SiN), or the like can be given. From the viewpoint of more preferably preventing the non-porous base material from being contaminated when the acid component or the base component in the gas is quantified using the present quantification kit, the material of the non-porous base material is preferably quartz or glass, and particularly preferably quartz.

[0069] The shape of the non-porous base material is not particularly limited, and a shape having a large surface area is preferable from the viewpoint of more preferably trapping the acid component or the base component in the gas when the acid component or the base component in the gas is quantified using the present quantification kit. As the shape having a large surface area, for example, a granular shape, a fibrous shape, or the like can be given. The shape of the non-porous base material is more preferably a granular shape.

[0070] From the viewpoint of improving the efficiency of the passage of the gas to be collected to the column B for collection when the acid component or the base component in the gas is quantified using the present quantitative kit, the lower limit of the average particle diameter or the cross-sectional average diameter of the non-porous base material is preferably 300 μm, more preferably 400 μm, further preferably 450 μm, still further preferably 500 μm, and particularly preferably 600 μm. From the viewpoint of improving the efficiency of the collection of the acid component or the base component when the acid component or the base component in the gas is quantified using the present quantitative kit, the upper limit of the average particle diameter or the cross-sectional average diameter of the non-porous base material is preferably 1200 μm, more preferably 1100 μm, further preferably 1050 μm, still further preferably 1000 μm, and particularly preferably 850 μm. Note that the average particle diameter and the cross-sectional average diameter herein are measured according to JIS K0069 "Chemical Products: Sieving Test Method".

[0071] The basic adsorbent is an adsorbent for adsorbing an acid component, and specifically can be an adsorbent composed of a basic substance, or can be an adsorbent containing a basic substance. In addition, the acid adsorbent is an adsorbent for adsorbing a base component, and specifically can be an adsorbent composed of an acid substance, or can be an adsorbent containing an acid substance.

[0072] The amount of the basic adsorbent or the acid adsorbent in the column for collection provided with the adsorption material A is preferably 0.4 μeq or more, more preferably 0.7 μeq or more, and further preferably 0.8 μeq or more. From the viewpoint of exerting the effect of preventing column breakthrough when collecting a gas at a high concentration, the amount of the basic adsorbent or the acid adsorbent is preferably adjusted to 0.4 μeq or more. On the other hand, the amount of the basic adsorbent or the acid adsorbent is preferably 50 μeq or less, more preferably 30 μeq or less, and further preferably 20 μeq or less. From the viewpoint of exerting the effect of preventing an excessive adsorbent component from interfering with the measurement, the amount of the basic adsorbent or the acid adsorbent is preferably adjusted to 50 μeq or less. The amount of the basic adsorbent or the acid adsorbent is a value expressed in equivalents, and can be measured by the method described in the examples.

[0073] As the basic adsorbent, inorganic bases and organic bases can be given. As the inorganic bases, carbonates of alkali metals, hydroxides of alkali metals, and the like can be given. As the organic bases, amines, ammonium compounds, and the like can be given.

[0074] The basic adsorbent is preferably at least one compound selected from among the above-listed compounds, among which alkali metal carbonates, alkali metal hydroxides, amines, and ammonium compounds are given.

[0075] As the alkali metal carbonate, sodium carbonate, potassium carbonate, potassium hydrogen carbonate, and the like can be given. As the alkali metal hydroxide, strontium hydroxide, potassium hydroxide, sodium hydroxide, and the like can be given. As the amine, triethanolamine, and the like can be given. As the ammonium compound, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, and the like can be given.

[0076] The basic adsorbent is more preferably at least one compound selected from the group consisting of sodium carbonate, sodium hydroxide, and triethanolamine.

[0077] As the acidic adsorbent, inorganic acids and organic acids can be given.

[0078] As the inorganic acid, sulfuric acid, phosphoric acid, and the like can be given. As the organic acid, methanesulfonic acid, maleic acid, malonic acid, and the like can be given.

[0079] The acidic adsorbent is preferably at least one compound selected from the group consisting of sulfuric acid, phosphoric acid, and methanesulfonic acid among the above-listed compounds.

[0080] In the trapping column provided with the adsorbent A, the form in which the non-porous base material holds the basic adsorbent or the acidic adsorbent is not particularly limited. The form can be, for example, a form in which a solid form of the basic adsorbent or the acidic adsorbent is attached to the surface of the non-porous base material, or a form in which the non-porous base material is coated with a liquid phase containing the basic adsorbent or the acidic adsorbent.

[0081] The liquid phase is a liquid containing the basic adsorbent or the acidic adsorbent, and contains a solvent as necessary. In other words, in the case where 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. As the solvent, a solvent capable of dissolving the basic adsorbent or the acidic adsorbent without causing adverse effects on the non-porous base material can be used, and is not particularly limited. As specific examples of the solvent, water, glycols such as ethylene glycol and propylene glycol, glycerol, polyhydric alcohols, polyalkylene glycols such as polyethylene glycol and polypropylene glycol, hydrogen peroxide, ethanol, acetonitrile, or a mixture liquid thereof, and the like can be given. The solvent is preferably a solvent containing water, for example, a mixture of water and a solvent other than water among the above-listed specific examples of the solvent, and more preferably a solvent consisting only of water. On the other hand, in the case where the basic adsorbent or the acidic adsorbent is a liquid, the basic adsorbent or the acidic adsorbent can be used directly as the liquid phase.

[0082] The method of coating the non-porous substrate with the liquid phase is not particularly limited with respect to the trapping column having the adsorbent A. As the method, there can be mentioned a method of applying the liquid phase to the non-porous substrate, and a method of dipping the non-porous substrate in the liquid phase and then taking up the non-porous substrate and drying it. As a specific example of the method of applying the liquid phase to the non-porous substrate, there can be mentioned a method of applying by flowing the liquid phase through the porous substrate. Here, the "flowing through" means flowing the liquid phase through a container such as a column packed with the porous substrate. Note that in the case where the drying conditions are set to high temperature and long time, sometimes the solvent in the liquid phase evaporates to cause precipitation of a solid of the basic adsorbent or the acidic adsorbent on the surface of the non-porous substrate. At this time, the non-porous substrate of this form in which the basic adsorbent or the acidic adsorbent in a solid state is attached to the surface can be obtained.

[0083] In the trapping column having the adsorbent A, the non-porous substrate can further hold a humectant. Note that in the case where the non-porous substrate further holds a humectant and the basic adsorbent or the acidic adsorbent is held in the form of the liquid phase, the liquid phase further contains the humectant. As the humectant, there can be mentioned polyhydric alcohols such as ethylene glycol, propylene glycol, and glycerol; and polyalkylene glycols such as polyethylene glycol and polypropylene glycol. In addition, the content of the humectant can be 0.01% by weight or more and 1.0% by weight or less, preferably 0.1% by weight or more and 0.5% by weight or less, with respect to the total weight of the non-porous substrate coated with the liquid phase.

[0084] The trapping column having the adsorbent A can be composed of a housing (i.e., a jacket portion) and a filter (i.e., a grid) for preventing the outflow of the non-porous substrate disposed inside the housing. As for the materials of the housing and the grid, there are no particular limitations as long as the materials do not affect the acid component or the base component as a trapping target and are not adversely affected by corrosion of the basic adsorbent or the acidic adsorbent. As for the material of the housing, for example, 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 can be mentioned. In addition, as for the material of the grid, for example, polyethylene, polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), polyethersulfone (PES), cellulose, glass fiber, carbon fiber, diatomite, cellulose, polyethylene terephthalate (PET), nylon, and mixtures thereof, and the like can be mentioned. The materials of the housing and the grid can be the same or different.

[0085] The shape of the trapping column having the adsorbent A is not particularly limited, and a cylindrical shape can be generally employed. As the trapping column having the adsorbent A, a column composed of a column main body, a grid, a sleeve, and a tip fitting, for example, the column described in Japanese Patent Application Publication No. 2001-249120 can be mentioned.

[0086] The inner volume of the trapping column having the adsorbent A (the inner volume of the housing) can be appropriately set in accordance with 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.

[0087] The void volume of the trapping column having the adsorbent A refers to the volume of the void not occupied by the non-porous substrate coated with the liquid phase in the trapping column having the adsorbent A. The void volume can be measured, for example, by the method described in the examples.

[0088] The larger the void volume is above the prescribed value, the more the amount of the gas per unit time flowing through the trapping column B provided with the adsorbent A, i.e., the ventilation amount, increases when the acid component or the base component in the gas is quantified using the present quantitative test kit. Here, when the acid component or the base component in the gas is quantified using the quantitative test kit, a prescribed amount of the gas is caused to flow through the trapping column B to trap the acid component or the base component contained in the prescribed amount of the gas. Therefore, the larger the void volume is, the shorter the time required for causing the prescribed amount of the gas to flow through the trapping column B.

[0089] Therefore, the larger the void volume is when the acid component or the base component in the gas is quantified using the present quantitative test kit, the shorter the time required for trapping and quantifying the acid component or the base component in the gas. From this viewpoint, the lower limit value of the void volume is preferably 200 μL, more preferably 300 μL, and further preferably 400 μL.

[0090] On the other hand, if the void volume is below the prescribed value, the amount of the non-porous base material holding the basic adsorbent or the acidic adsorbent filled in the trapping column B provided with the adsorbent A, i.e., the trapping column B, is sufficient, and the ability to trap the acid component or the base component in the gas can be sufficiently ensured. Thus, by quantifying the acid component or the base component in the gas using the present quantitative test kit, the acid component or the base component in the gas can be trapped and quantified with high sensitivity. From the viewpoint of being able to trap and quantify the acid component or the base component in the gas with high sensitivity, the void volume is preferably 5,000 μL or less, more preferably 3,000 μL or less, further preferably 600 μL or less, and particularly preferably 500 μL or less.

[0091] With respect to the trapping column provided with the adsorbent A, the upper limit value of the pressure loss when the gas in the trapping column is sucked at a suction rate of 2.0 L / min is preferably 10 kPa. Hereinafter, the pressure loss when sucked at a suction rate of 2.0 L / min will be referred to as "pressure loss A". By making the pressure loss A 10 kPa or less, the gas can be sucked at high speed without imposing a load on the suction pump for gas collection when the measurement target gas is collected in the trapping column B provided with the adsorbent A and ventilated. Therefore, a prescribed amount of the gas can be collected and caused to flow through the trapping column B provided with the adsorbent A in a short time. Thus, by quantifying the acid component or the base component in the gas using the present quantitative test kit, the acid component or the base component in the gas can be trapped and quantified in a short time. From this viewpoint, the upper limit value of the pressure loss A of the trapping column provided with the adsorbent A is preferably 7 kPa, and more preferably 5 kPa.

[0092] [Embodiment 3: Quantitative method]

[0093] The quantitative method of one embodiment of the present application (hereinafter, also referred to as "the present quantitative method") is a quantitative method of the concentration of an acid component and / or a base component in a gas, comprising:

[0094] Step A: flowing a solvent through the standard pre-column to elute the known amount of the acid component or the known amount of the base component into the solvent to obtain an eluate A;

[0095] Step B1: flowing a gas through an acid component trapping column for trapping an acid component in a gas or a base component trapping column for trapping a base component in a gas to trap the acid component or the base component in the gas;

[0096] After the step B1, flowing a solvent through the acid component trapping column in which the acid component in the gas is trapped in the step B1 or the base component trapping column in which the base component in the gas is trapped in the step B1, thereby eluting the trapped acid component or the base component into the solvent to obtain an eluate B; and

[0097] Step B2, after the step B1, flowing a solvent through the acid component trapping column in which the acid component in the gas is trapped in the step B1 or the base component trapping column in which the base component in the gas is trapped in the step B1, thereby eluting the trapped acid component or the base component into the solvent to obtain an eluate B; and

[0098] Step C, 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 results of the analysis.

[0099] In summary, the present quantitative method is a method of quantifying an acid component or a base component in a gas using the standard pre-column and the trapping column B, and can simply and easily quantify the acid component or the base component in the gas.

[0100] Hereinafter, the method of quantifying the concentration of an acid component in a gas using the acid component standard pre-column and the acid component trapping column B among the present quantitative method is also referred to as "the acid component quantitative method". In addition, the method of quantifying the concentration of a base component in a gas using the base component standard pre-column and the base component trapping column B among the present quantitative method is also referred to as "the base component quantitative method".

[0101] Each step constituting the present quantitative method is described in detail below.

[0102] (Step A)

[0103] The present quantitative method includes: Step A, flowing a solvent through the present standard pre-column, thereby eluting the known amount of the acid component or the known amount of the base component into the solvent to obtain an eluate A.

[0104] As for the constitution of the present standard pre-column used in Step A, the constitution of the present standard pre-column described in the aforementioned "[Embodiment 1: Standard pre-column]" column can be cited.

[0105] In Step A, the known amount of the acid component or the base component which has been pre-attached in the present standard pre-column provided with the trapping column A is eluted into the solvent, as a result of which the eluate A containing the known amount of the acid component or the base component can be obtained. Therefore, the known amount of the acid component or the base component which has been pre-attached in the present standard pre-column is dissolved in the eluate A. The solvent is not particularly limited as long as it is a solvent capable of eluting the acid component or the base component. From the viewpoint of the sensitivity of the present quantitative method, a solvent not containing an impurity which can cause a decrease in the sensitivity, or a solvent in which the content of the impurity is extremely small, is preferably used as the solvent. From this viewpoint, the use of pure water is particularly preferable as the solvent. Here, pure water refers to water having a specific resistance in the range of 0.1 MΩ-cm or more and 18 MΩ-cm or less.

[0106] (Step B1)

[0107] The present quantitative method includes: Step B1, flowing a gas through an acid component trapping column for trapping an acid component in a gas or a base component trapping column for trapping a base component in a gas, thereby trapping the acid component or the base component in the gas.

[0108] In summary, Step B1 is a step of flowing a gas through a trapping column B, thereby trapping an acid component or a base component in the gas. Hereinafter, Step B1 in the case where an acid component trapping column B is used to trap an acid component in a gas will be referred to as an "acid component trapping step". In addition, Step B1 in the case where a base component trapping column B is used to trap a base component in a gas will also be referred to as a "base component trapping step". Step B1 is either an acid component trapping step or a base component trapping step.

[0109] The constitution of the trapping column B used in Step B1, etc. can be cited as described in the aforementioned "[Embodiment 2: Quantitative kit]" column regarding the constitution of the trapping column B. Also, the effects of the present quantitative method can be cited as described in the aforementioned "[Embodiment 2: Quantitative kit]" column regarding the effects in the case of quantifying the acid component or the base component in the gas using the present quantitative kit. Furthermore, the acid component or the base component that becomes the trapping target in Step B1 is not particularly limited and can be the acid component or the base component exemplified in the aforementioned "[Embodiment 1: Standard pre-attached column]" column. Here, from the viewpoint of the accuracy of the present quantitative method, the acid component or the base component that becomes the trapping target in Step B1 is preferably the same as the acid component or the base component that is pre-attached in the present standard pre-attached column used in Step A.

[0110] Here, it is also possible to simultaneously perform both the acid component trapping step and the base component trapping step on the same gas, thereby trapping both the acid component and the base component in the gas.

[0111] In Step B1, the acid component or the base component in the gas that becomes the trapping target is trapped inside the trapping column B by flowing the gas through the trapping column B. The flowing can be performed using a suction pump, for example.

[0112] In Step B1, the time required for trapping the acid component or the base component in the gas by Step B1 can be shortened by flowing the gas through the acid component trapping column B or the base component trapping column B at a higher flow rate. As a result, the acid component or the base component in the gas can be trapped in a short time by Step B1, and the quantification can be performed in a shorter time by the present quantitative method. From the viewpoint of trapping the acid component or the base component in the gas in a short time and performing the quantification in a shorter time by the present quantitative method, the flow rate is preferably 2.0 L / min or higher, and more preferably 3.0 L / min or higher. On the other hand, if the flow rate is too high, the pressure that the trapping column B receives when the gas flows through it can increase, and the trapping column B can be damaged. From the viewpoint of better preventing the trapping column B from being damaged, the flow rate is preferably 10 L / min or lower, and more preferably 7 L / min or lower. From the viewpoint of being able to perform the quantification in a shorter time by the present quantitative method and better preventing the damage, the flow rate is particularly preferably 5 L / min.

[0113] The flowing in the trapping column B can generally be performed in an evaluation target space such as a clean room or a dust-free room. The transportation of the trapping column B can be performed by sealing the port of the trapping column B with a plug that is not contaminated with the analysis target substance, and / or by housing the trapping column B in a closed container that is not contaminated with the analysis target substance.

[0114] If the acid component capturing step and the base component capturing step are performed together, the device having the structure in which the acid component capturing column B and the base component capturing column B are connected in series can be used to continuously perform the acid component capturing step and the base component capturing step. That is, the device can be caused to draw the air so that the air continuously flows through both the acid component capturing column B and the base component capturing column B formed in the device. More specifically, the air that has flowed through the acid component capturing column B can be caused to flow through the base component capturing column B (i), or the air that has flowed through the base component capturing column B can be caused to flow through the acid component capturing column B (ii). In these cases, the acid component capturing column B and the base component capturing column B can be directly connected or connected via a connection pipe.

[0115] By performing the acid component capturing step and the base component capturing step together, the acid component quantification method and the base component quantification method can be performed together. In this case, for example, the device having the structure in which the acid component capturing column B and the base component capturing column B are connected in series can be caused to draw the air so that the air simultaneously flows through both the acid component capturing column B and the base component capturing column B formed in the device. Then, the acid component capturing column B and the base component capturing column B are separated from the device, and the steps B2 and C described below are performed for each of them.

[0116] (Step B2)

[0117] The present quantification method includes: a step B2 of, after the step B1, causing a solvent to flow through the acid component capturing column B in which the acid component in the gas has been captured in the step B1 or the base component capturing column B in which the base component in the gas has been captured in the step B1, to thereby elute the captured acid component or base component into the solvent to obtain an eluate B.

[0118] In summary, the step B2 is a step of eluting the acid component or the base component captured in the capturing column B in the step B1 into a solvent to obtain an eluate B by causing the solvent to flow through the capturing column B in which the acid component or the base component in the gas has been captured in the step B1 after the step B1. Therefore, the eluate B has the acid component or the base component captured in the step B1 dissolved in an amount.

[0119] 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, like in Step A. As the solvent used in Step B2, like in Step A, a solvent containing no impurities that can cause a decrease in sensitivity, or a solvent containing a very small amount of such impurities, is preferably used from the viewpoint of the sensitivity of the present quantitative method. From this viewpoint, pure water is particularly preferably used as the solvent used in Step B2. In addition, in Step B2, a solvent of the same kind as in Step A is preferably used from the viewpoint of the accuracy of the present quantitative method.

[0120] (Step C)

[0121] The present quantitative method includes Step C, which quantifies 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 results of the analysis.

[0122] The Step C can be, for example, the steps shown in (1) to (4) below.

[0123] (1) The eluate A containing a known amount of the acid component or the base component is subjected to analysis by a method for quantifying the acid component or the base component, and a "standard result" is obtained. From this standard result, a correlation A is obtained.

[0124] (2) The eluate B containing the acid component or the base component captured from the gas is subjected to analysis by the same method as the method for quantifying the acid component or the base component described in the Step (1), and a value corresponding to the amount of the acid component or the base component contained in the eluate B is obtained.

[0125] (3) The value obtained in the Step (2) is converted into the amount of the acid component or the base component contained in the eluate B based on the correlation A obtained in the Step (1), and the amount of the acid component or the base component contained in the eluate B is calculated.

[0126] (4) The amount of the acid component or the base component obtained in the Step (3) is divided by the amount of the gas that has flowed through the trapping column B in the Step B1, and the concentration of the acid component or the base component in the gas is calculated.

[0127] The acid component or the base component in the eluate B is the acid component or the base component in the gas that has been captured by the Step B1. Therefore, the amount of the acid component or the base component in the eluate B calculated in the Step (3) in the Step C substantially corresponds to the amount of the acid component or the base component in the gas that has flowed through the trapping column B. Thus, the amount of the acid component or the base component in the gas can be quantified by the Step C.

[0128] As the method for quantifying the acid component or the base component in the eluent A and the eluent B in the above-mentioned steps (1) and (2) (hereinafter also referred to as "the present determination method"), a publicly known method can be employed without particular limitation. The present determination method can be, for example, a liquid chromatography method. As the liquid chromatography method, for example, an anion exchange method using an ion exchange column, a cation exchange method using an ion exchange column, and an ion chromatography method using a suppressor can be mentioned.

[0129] In addition, the acid component exists in the eluent A and the eluent B in an anionic manner, and the base component exists in the eluent A and the eluent B in a cationic manner. Therefore, by the step (1), the "standard result" and the correlation A with respect to the total amount of anions or cations in the eluent A, that is, the "standard result" and the correlation A with respect to the known amount of the acid component or the base component can be obtained. Similarly, by the step (2), a value corresponding to the total amount of anions or cations in the eluent B is obtained, and this value is used as a value corresponding to the amount of the acid component or the base component captured in the step B1.

[0130] [Embodiment 4: Management method of space cleanliness]

[0131] The management method of space cleanliness according to one embodiment of the present application (hereinafter also referred to as "the present management method") is a management method including a quantification step of quantifying the concentration of an acid component or a base component in a gas in a space by the present quantification method, and an exclusion step of determining and excluding a source of the acid component or the base component in the gas in the interior of the space when the concentration of the acid component or the base component quantified in the quantification step exceeds a threshold value.

[0132] According to the present quantification method, as described above, the acid component or the base component contained in a gas can be simply quantified by a simple operation. Therefore, the present management method can be easily implemented, and thus a clean space can be easily ensured by the present management method.

[0133] (Quantification step)

[0134] The present management method includes a quantification step of quantifying the concentration of an acid component and a base component in a gas in a space by the present quantification method. By implementing the quantification step, the concentration of a contaminant, that is, the acid component and the base component in a space can be easily (simply) quantified.

[0135] The space described in the present specification is an object space of the evaluation by the present quantitative method, an object space of the quantification, and the like, and can be, for example, a space in which the concentration of the contaminant, that is, the acid component and the base component, is required to be below a certain threshold value in order to perform an operation in electronic substrate manufacturing or the like. In addition, the space described in the present management method can generally be a space having a prescribed volume formed by walls, floors, and the like. The space is not particularly limited, and can be, for example, a clean room, a clean booth, or a space inside a manufacturing device.

[0136] As for the configuration and the like of the quantitative method employed in the quantification step, the configuration and the like described in the aforementioned "[Embodiment 3: Quantitative method]" can be cited.

[0137] In the present management method, in order to easily secure a clean space, the amount (concentration) of the contaminant, that is, the acid component and / or the base component, in the space is quantified, and on this basis, a contamination source is also determined and excluded in accordance with the quantified concentration. Therefore, in the quantification step, either the acid component quantitative method or the base component quantitative method can be implemented, both the acid component quantitative method and the base component quantitative method can be implemented, and preferably both the acid component quantitative method and the base component quantitative method are implemented. In order to implement both the quantitative methods at the same time, a device having a structure in which the acid component trapping column B and the base component trapping column B are arranged in series is preferably used. In the case of using this device, by performing a single suction of the device, both the acid component trapping column B and the base component trapping column B formed in the device can be aerated, and thus the quantification step and the present management method can be easily implemented.

[0138] (Determining and excluding a contamination source step)

[0139] The present management method includes a step of determining and excluding a source of the acid component or the base component in the gas inside the space in the case where the concentration of the acid component or the base component quantified in the quantification step exceeds a threshold value. Herein, the "source of the acid component or the base component in the gas inside the space" is also referred to as a "contamination source" in the present specification. Therefore, the "step of determining and excluding a source of the acid component or the base component in the gas inside the space" is a "step of determining and excluding a contamination source". By implementing the step of determining and excluding the contamination source, the concentration of the contaminant, that is, the acid component or the base component, can be controlled to be below the threshold value inside the space, and thus a clean space can be easily secured.

[0140] The threshold value involved in the step can be appropriately decided in accordance with the kind of the operation performed in the space, the required quality of the product manufactured by the operation, and the like, and is not particularly limited. For example, if a high-quality electronic substrate is manufactured in the space, the threshold value can be 1.0 pg / m3 0.1 μg / m 3 or 0.01 μg / m 3 and the like.

[0141] The determination and elimination of the contamination source means an operation of grasping the concentration of the contaminant, i.e., the acid component and the base component, inside the space and taking appropriate measures, and the specific method is not particularly limited and can be a publicly known method.

[0142] One embodiment of the present application can be the inventions shown in the following [1] to

[11] .

[0143] [1] A standard preconcentration column for quantifying the concentration of an acid component or a base component in a gas, wherein an acid component trapping column of the standard preconcentration column for trapping the acid component in the gas is preconcentrated with a known amount of the acid component, or a base component trapping column of the standard preconcentration column for trapping the base component in the gas is preconcentrated with a known amount of the base component.

[0144] [2] The standard preconcentration column according to [1], wherein the amount of the known amount of the acid component or the known amount of the base component is greater than 1 ng and 1000 μg or less.

[0145] [3] The standard preconcentration column according to [1] or [2], wherein

[0146] the acid component trapping column or the base component trapping column is filled with a non-porous substrate,

[0147] the non-porous substrate retains a basic adsorbent for adsorbing the acid component or an acid adsorbent for adsorbing the base component,

[0148] the pressure loss of the acid component trapping column or the base component trapping column when the gas in the trapping column is sucked at a suction rate of 2.0 L / min is 10 kPa or less.

[0149] [4] The standard preconcentration column according to [1], wherein the void volume of the trapping column is 200 μL or more and 3000 μL or less.

[0150] [5] The standard preconcentration column according to [3] or [4], wherein the amount of the basic adsorbent or the acid adsorbent is 0.4 μeq or more and 50 μeq or less.

[0151] [6] A quantification kit for quantifying the concentration of an acid component and / or a base component in a gas, which satisfies the following requirements (a) and / or (b):

[0152] (a) one or more standard pre-attachment column to which a known amount of an acid component is pre-attached, and one or more column for trapping an acid component in a gas, as described in [1] or [2];

[0153] (b) one or more standard pre-attachment column to which a known amount of a base component is pre-attached, and one or more column for trapping a base component in a gas, as described in [1] or [2];

[0154] [7] The quantitative kit for quantifying the concentration of an acid component and / or a base component in a gas according to [6], wherein

[0155] the column for trapping an acid component or the column for trapping a base component is filled with a non-porous substrate,

[0156] the non-porous substrate holds a basic adsorbent for adsorbing an acid component or an acid adsorbent for adsorbing a base component,

[0157] the pressure loss of the column for trapping an acid component or the column for trapping a base component is 10 kPa or less when a gas in the column is sucked at a suction rate of 2.0 L / min.

[0158] [8] The quantitative kit for quantifying the concentration of an acid component and / or a base component in a gas according to [7], wherein the void volume of the column for trapping is 200 μL or more and 3000 μL or less.

[0159] [9] The quantitative kit for quantifying the concentration of an acid component and / or a base component in a gas according to [7] or [8], wherein the amount of the basic adsorbent or the acid adsorbent is 0.4 μeq or more and 50 μeq or less.

[0160]

[10] A method for quantifying the concentration of an acid component and / or a base component in a gas, using the quantitative kit for quantifying the concentration of an acid component and / or a base component in a gas according to [6], the method comprising:

[0161] Step A, flowing a solvent through the standard pre-attachment column, thereby eluting the known amount of the acid component or the known amount of the base component into the solvent to obtain an eluate A;

[0162] Step B1, flowing a gas through the column for trapping an acid component in the gas or the column for trapping a base component in the gas, thereby trapping an acid component or a base component in the gas;

[0163] Step B2, after the step Bl, flowing a solvent through the acid component trapping column that traps the acid component in the gas in the step Bl or the base component trapping column that traps the base component in the gas in the step Bl, thereby eluting the trapped acid component or the base component into the solvent to obtain an eluate B; and

[0164] Step C, 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 results of the analysis.

[0165]

[11] A management method for managing cleanliness of a space, comprising:

[0166] 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 of

[10] ; and

[0167] an exclusion step of determining and excluding a source of the acid component or the base component in the gas in the interior of the space in a case where the concentration of the acid component or the base component quantified in the quantification step exceeds a threshold value.

[0168] <Embodiments>

[0169] The present application is described in more detail below by way of examples, but the present application is not limited to these examples.

[0170] [Measurement method]

[0171] The method of measuring a value corresponding to the amount of a base component or an acid component contained in an eluate obtained from a standard pre-column and a trapping column in the examples is as follows.

[0172] (Ion chromatography)

[0173] In the examples, the eluate A or the eluate B was analyzed by the method shown below using an ion chromatograph, and a value corresponding to the amount of an acid component or a base component contained in the eluate A or the eluate B was measured.

[0174] The eluate A and the eluate B were analyzed using a two-channel ion chromatography system having conductivity detection function. The anion channel of the ion chromatography system used a potassium hydroxide gradient eluent, an anion analysis column, and a suppressor. The cation channel of the ion chromatography system used a methanesulfonic acid gradient eluent, a cation analysis column, and a suppressor.

[0175] [Production Example 1: Preparation of base component trapping column A and base component trapping column B]

[0176] A quartz particle having a particle size of 0.5 mm to 1.0 mm was packed into a polypropylene cylindrical column housing having an inner volume of 0.92 mL. After flowing methanol, purified water (resistivity of 0.1 MΩ-cm or more) was flowed through the inside of the column to perform cleaning.

[0177] A mixed aqueous solution of sulfuric acid and glycerin was flowed through the cleaned column, and then clean air was introduced to dry, thereby producing an alkali component trapping column A.

[0178] Further, the same method as the above was repeatedly performed five times, thereby producing five alkali component trapping columns B having the same constitution as the alkali component trapping column A.

[0179] [Example 1: Production of an alkali component standard pre-packed column]

[0180] To the alkali component trapping column A produced in Production Example 1, 5 μL of an ammonium ion standard solution having an ammonium ion concentration of 10 μg / mL was added by a method of adding a standard solution, and then clean nitrogen gas was introduced to dry, thereby producing an alkali component standard pre-packed column to which 50 ng of ammonium ions (NH4 + ) had been pre-packed. Specifically, using a micropipette, 5 μL of an ammonium ion standard solution having an ammonium ion concentration of 10 μg / mL was added to the alkali component trapping column A, and then clean nitrogen gas was introduced to dry. As a result, an alkali component standard pre-packed column to which 50 ng of ammonium ions (NH4 + ) had been pre-packed was produced.

[0181] Pure water 10 mL was flowed through the produced alkali component standard pre-packed column, thereby producing an eluate A in which the alkali component, i.e., ammonium ions, pre-packed in the alkali component standard pre-packed column was eluted. To the produced eluate A, the ion chromatograph was used to obtain a value corresponding to the amount of the alkali component, i.e., a peak area. The obtained peak area was referred to as "peak area A". The specific value of the peak area A is shown in Table 1 below.

[0182] [Examples 2 to 6]

[0183] A single simple room in which a part of the room was configured as a clean room was prepared. In the single simple room, the base component trapping column B prepared in Production Example 1 was aerated from the air flow introduction side at a flow rate of 2 L / min for 125 minutes at any one of the outside of the clean room and any four of the inside of the clean room. Then, in the same manner as in Example 1, 10 mL of pure water was caused to flow through each of the aerated base component trapping columns B, whereby each eluate B was prepared. For each of the prepared eluates B, a value corresponding to the amount of the base component, i.e., a peak area, was obtained using the ion chromatograph. The obtained peak area was referred to as "peak area B". Here, the example in which the aerating was performed at one place outside the clean room was Example 2, and the examples in which the aerating was performed at four places inside the clean room were Examples 3 to 6, respectively.

[0184] 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 of the aerated gas was calculated based on the following formula (I), respectively.

[0185] Concentration of base component in gas = (0.2 x area B) / area A [μg / m 3 ] Formula (I)

[0186] With respect to Examples 2 to 6, the concentration of the base component in the gas calculated by the formula (I) is shown in Table 1 below, respectively.

[0187] [Table 1]

[0188]

[0189] [Production Example 2: Preparation of acid component trapping column A and acid component trapping column B]

[0190] A quartz particle having a particle size of 0.5 mm to 1.0 mm was packed into a polypropylene cylindrical column housing having an inner volume of 0.92 mL. After flowing methanol, pure water (resistivity of 0.1 MΩ-cm or more) was caused to flow inside the column to perform cleaning.

[0191] A mixed aqueous solution of sodium carbonate and glycerin was caused to flow through the cleaned column, and then clean air was introduced to dry, whereby an acid component trapping column A was prepared.

[0192] In addition, the same method as the above method was repeatedly performed five times, whereby five acid component trapping columns B having the same configuration as the acid component trapping column A were prepared.

[0193] [Example 7: Production of acid component trapping column using commercially available column]

[0194] To the acid component trapping column A prepared in Production Example 2, an acid component mixture composed of 50 ng or 100 ng each 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 additionally preattached by adding a standard solution, thereby producing an acid component standard preattachment column. Specifically, 5 μL of an acid component standard solution having a concentration of 10 μg / mL or 20 μg / mL of each acid component of the acid component mixture was added to the acid component trapping column A using a micropipette, and then, clean nitrogen gas was passed to perform drying. As a result, an acid component standard preattachment column to which 50 ng or 100 ng of each of the above acid components was additionally preattached was produced. Here, the amount of each acid component contained in 5 μL of the acid component standard solution is shown in Table 2 below. In addition, the amount of each acid component contained in 5 μL of the acid component standard solution is also the amount of each acid component that is additionally preattached in the acid component standard preattachment column.

[0195] [Table 2]

[0196]

[0197] Pure water 10 mL was passed through the acid component standard preattachment column thus produced, thereby producing an eluate A in which the acid component mixture that was additionally preattached in the acid component standard preattachment column was eluted. To the produced eluate A, the ion chromatograph was used to obtain a value corresponding to the amount of each acid component that constitutes the acid component mixture, i.e., a peak area. The obtained peak area is referred to as "peak area A".

[0198] [Examples 8 to 12]

[0199] A single simple room partially composed of a clean room was prepared. In the single simple room, the acid component trapping column B produced in Production Example 2 was ventilated from the air flow introduction side at a flow rate of 2 L / min for 125 minutes at any one place outside the clean room and at any four places inside the clean room. Then, in the same manner as in Example 1, pure water 10 mL was passed through each acid component trapping column B after the ventilation, thereby producing each eluate B. To each produced eluate B, the ion chromatograph was used to obtain a value corresponding to the amount of each acid component, i.e., a peak area. The obtained peak area is referred to as "peak area B".

[0200] The concentration of each acid component in the gas was calculated from the peak area B corresponding to the amount of each acid component obtained in Examples 8 to 12 and the peak area A corresponding to the amount of each acid component obtained in Example 7, based on the following formula (II), for each of the 250 L of the gas passed.

[0201] Concentration of acid component in gas = (0.2 x area B) / area A [μg / m 3 ] Formula (II)

[0202] The concentration of each acid component in the gas calculated by the formula (II) for Examples 8 to 12 is shown in Table 3 below.

[0203] [Reference Examples 1 to 5]

[0204] Five calibration curves for each acid component were prepared, which represented the correspondence between the peak area corresponding to the amount of each acid component obtained by the ion chromatograph in Examples 8 to 12 and the amount (mass) of each acid component in the eluent. Specifically, first, the following five kinds of standard solutions were prepared using pure water as a solvent: a standard solution having a concentration of 0.5 ng / mL or 1 ng / mL of each acid component; a standard solution having a concentration of 1 ng / mL or 2 ng / mL of each acid component; a standard solution having a concentration of 5 ng / mL or 10 ng / mL of each acid component; a standard solution having a concentration of 10 ng / mL or 20 ng / mL of each acid component; and a standard solution having a concentration of 50 ng / mL or 100 ng / mL of each acid component. Next, for each of the five kinds of standard solutions, the peak area corresponding to the amount of each acid component in each standard solution was obtained using the ion chromatograph, and five kinds of peak areas were obtained. The obtained five kinds of peak areas and the amount of each acid component corresponding to the peak areas were plotted, and thus the five calibration curves were prepared.

[0205] The concentration of each acid component in the eluent was calculated from the peak area B corresponding to the amount of each acid component obtained in Examples 8 to 12 by the five calibration curves. In addition, based on the calculated concentration of each acid component in the eluent, the product of the concentration of each acid component in the eluent and the amount of the eluent, and the amount of the gas passed (i.e., 2 L min x 125 minutes = 250 L = 250 x 10 -3 m 3 ), the concentration of each acid component in the gas was calculated. Here, each of Examples 8 to 12 using the peak area B corresponding to the amount of each acid component obtained in each of Examples 8 to 12 and calculating the mass and concentration of each acid component in the gas by the calibration curves was used as Reference Examples 1 to 5, respectively, and the concentration of each acid component in the gas obtained is shown in Table 3 below. In Table 3 below, the unit of the concentration of each acid component is noted as [ng / L = μg / m 3 ].

[0206] [Table 3]

[0207]

[0208] As shown in Table 1 and Table 3, it was found that the concentration of the component in the gas could be quantitatively determined by the quantitative method described in Examples 2 to 6 and 8 to 12. In addition, it was found that the results of Examples 8 to 12 were substantially the same as those of Reference Examples 1 to 5, and thus according to the present standard prep column, the present quantitative kit, and the present quantitative method, even without intentionally making a calibration curve, the concentration of the acid component or the base component contained in the gas could be simply quantitatively determined.

[0209] [Industrial applicability]

[0210] According to the present standard prep column, the present quantitative kit, and the present quantitative method, the concentration of the acid component or the base component in the gas can be simply quantitatively determined. Thus, according to the present management method using the present quantitative method, a clean room can be simply ensured. Therefore, the present standard prep column, the present quantitative kit, the present quantitative method, and the present management method can be used for managing a work space in which a clean area is required in electronic substrate manufacturing or the like.

Claims

1. A standard pre-attached column for quantitatively determining the concentration of acidic or alkaline components in a gas, characterized in that... The standard pre-filled column for capturing acid components in a gas is pre-filled with a known amount of acid components, or the standard pre-filled column for capturing alkaline components in a gas is pre-filled with a known amount of alkaline components.

2. The standard pre-attached tubular column according to claim 1, wherein, The known amount of acid or alkali is greater than 1 ng and less than 1000 μg.

3. The standard pre-attached tubular column according to claim 1 or 2, wherein, The acid or alkali component trapping column is filled with a non-porous substrate. The non-porous substrate contains an alkaline adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing alkaline components. When the gas in the acid component trapping column or the alkali component trapping column is attracted at an attraction rate of 2.0 L / min, the pressure loss of the trapping column is less than 10 kPa.

4. The standard pre-attached tubular column according to claim 3, wherein, The pore volume of the collection tubing is 200 μL or more and 3000 μL or less.

5. The standard pre-attached tubular column according to claim 3, wherein, The amount of the alkaline adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less.

6. A quantitative reagent kit for quantifying the concentration of acidic and / or alkaline components in a gas, characterized in that... The following requirements (a) and / or (b) must be met: (a) comprising one or more standard pre-filled feed columns as described in claim 1 or 2, which are pre-filled with a known amount of acid components, and one or more acid component capture columns for capturing acid components in gases; (b) comprising one or more standard pre-filled feed columns as described in claim 1 or 2, which are pre-filled with a known amount of alkaline components, and one or more alkaline component capture columns for capturing alkaline components in gases.

7. The quantitative reagent kit for quantifying the concentration of acidic and / or alkaline components in a gas according to claim 6, wherein, The acid or alkali component trapping column is filled with a non-porous substrate. The non-porous substrate contains an alkaline adsorbent for adsorbing acidic components or an acidic adsorbent for adsorbing alkaline components. When the gas in the acid component trapping column or the alkali component trapping column is attracted at an attraction rate of 2.0 L / min, the pressure loss of the trapping column is less than 10 kPa.

8. The quantitative reagent kit for quantifying the concentration of acidic and / or alkaline components in a gas according to claim 7, wherein, The pore volume of the collection tubing is 200 μL or more and 3000 μL or less.

9. The quantitative reagent kit for quantifying the concentration of acidic and / or alkaline components in a gas according to claim 7, wherein, The amount of the alkaline adsorbent or the acidic adsorbent is 0.4 μeq or more and 50 μeq or less.

10. A quantitative method, comprising using the quantitative kit of claim 6 for quantifying the concentration of acidic and / or alkaline components in a gas to quantify the concentration of acidic and / or alkaline components in a gas. This quantitative method is characterized by including: Step A involves passing the solvent through the standard pre-feed column to elute the known amount of acid or alkali into the solvent to obtain eluent A. Step B1 involves passing the gas through an acid component trapping column for trapping acid components in the gas or an alkaline component trapping column for trapping alkaline components in the gas, in order to trap the acid or alkaline components in the gas. Step B2: After step B1, the solvent is passed through the acid component trapping column that has captured the acid component in the gas in step B1 or the alkali component trapping column that has captured the alkali component in the gas in step B1, thereby eluting the captured acid component or the alkali component into the solvent to obtain eluent B. as well as Step C involves quantifying the concentration of the acidic or alkaline component in the gas by analyzing eluent A and eluent B and comparing their analytical results.

11. A management method for managing the cleanliness of a space, characterized in that... include: The quantitative step involves using the quantitative method described in claim 10 to quantify the concentration of acid or alkali components in the gas within the space. as well as The exclusion step involves identifying and excluding the source of the acid or alkali component in the gas inside the space if the concentration of the acid or alkali component quantified in the quantitative step exceeds a threshold.

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