Quality inspection method for chemical liquid

Abstract

A quality inspection method for a chemical liquid used for manufacturing a semiconductor substrate includes: a step W of preparing a first container and washing at least a portion of a liquid contact portion by using a portion of the chemical liquid, a step A of performing concentration of a portion of the chemical liquid by using the washed first container so as to obtain c liquid, a step B of performing measurement of a content of a specific component in c liquid, and a step C of comparing the content of the specific component with a preset standard value. At least the step W and the step A are performed in a clean room having cleanliness equal to or higher than class 4 specified in ISO14644-1:2015, the concentration is performed in inert gas or under reduced pressure, and the measurement is performed by a predetermined measurement method.

Claims

1. A quality inspection method for a chemical liquid used for manufacturing a semiconductor substrate, comprising: a step W of preparing a first container having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from a group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, adopting a portion of the chemical liquid as a liquid, and washing at least a portion of the liquid contact portion by using a liquid; a step A of adopting a portion of the chemical liquid as b liquid and performing concentration of b liquid by using the washed first container so as to obtain c liquid; a step B of performing measurement of a content of a specific component in c liquid; and a step C of comparing the content of the specific component with a preset standard value, wherein the step W, the step A, the step B, and the step C are performed in this order, at least the step W and the step A are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1:2015 established by the International Organization for Standardization, the concentration is performed under at least one kind of inert gas selected from a group consisting of an Ar gas, a He gas, and a N.sub.2 gas or under reduced pressure, and the measurement is performed by at least one kind of measurement method selected from a group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, gas chromatography atomic emission detection, gas chromatography quadrupole time-of-flight type mass spectrometry, direct sample introduction-type mass spectrometry, high-performance liquid chromatography mass spectrometry, high-performance liquid chromatography tandem mass spectrometry, high-performance liquid chromatography time-of-flight type mass spectrometry, inductively coupled plasma mass spectrometry, inductively coupled plasma emission spectrometry, temperature programmed desorption mass spectrometry, ion chromatography, nuclear magnetic resonance spectrometry, and atomic absorption spectrometry.

2. The quality inspection method for the chemical liquid according to claim 1, further comprising: a step D of determining the chemical liquid as being inadequate and discarding the chemical liquid in a case where the content of the specific component is greater than the standard value in the step C; or a step E of purifying the chemical liquid in a case where the content of the specific component is greater than the standard value in the step C and then performing again the step W, the step A, the step B, and the step C.

3. The quality inspection method for the chemical liquid according to claim 1, wherein the step B is also performed in the clean room.

4. The quality inspection method for the chemical liquid according to claim 1, wherein the step W further has at least one kind of step selected from a group consisting of a step of performing acid washing on at least the liquid contact portion of the first container, a step of performing ultrasonic washing on at least the liquid contact portion of the first container, and a step of drying at least the liquid contact portion of the first container.

5. The quality inspection method for the chemical liquid according to claim 1, wherein a factor of concentration in the step A is 2 to 1,000,000.

6. The quality inspection method for the chemical liquid according to claim 1, wherein a factor of concentration in the step A is 10 to 10,000.

7. The quality inspection method for the chemical liquid according to claim 1, wherein the specific component contains at least one kind of compound selected from a group consisting of Formulae (1) to (7) ##STR00003##

8. The quality inspection method for the chemical liquid according to claim 1, wherein a temperature condition of the concentration in the step A is 10° C. to 250° C.

9. The quality inspection method for the chemical liquid according to claim 1, wherein a volume of b liquid in the step A is equal to or smaller than 5 L.

10. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the first container is a fluorine-containing polymer container in which at least a portion of the liquid contact portion is formed of a fluorine-containing polymer, the fluorine-containing polymer container satisfies a condition 1 or a condition 2 in the following test, test: a portion of the chemical liquid is adopted as d liquid, the liquid contact portion is washed using d liquid, a portion of the chemical liquid is adopted as e liquid, and under the condition that a ratio of a mass of the washed fluorine-containing polymer container to a mass of e liquid becomes 1.0 provided that a liquid temperature of e liquid is 25° C., the washed fluorine-containing polymer container is immersed for 24 hours in e liquid having a liquid temperature of 25° C., condition 1: in a case where e liquid having been used for the immersion contains one kind of fluoride ion, an increase of one kind of the fluoride ion before and after the immersion is equal to or smaller than 1 mass ppm, condition 2: in a case where e liquid having been used for the immersion contains two or more kinds of fluoride ions, a total increase of two or more kinds of the fluoride ions before and after the immersion is equal to or smaller than 1 mass ppm.

11. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the first container is a fluorine-containing polymer container in which at least a portion of the liquid contact portion is formed of a fluorine-containing polymer, within a surface of at least a portion of the liquid contact portion, provided that an atom number ratio of the number of fluorine atoms contained in the surface to the number of carbon atoms contained in the surface is M.sub.1, and an atom number ratio of the number of fluorine atoms contained in a position, which is 10 nm below the surface in a thickness direction of the fluorine-containing polymer container, to the number of carbon atoms contained in the position is M.sub.2, a ratio of M.sub.1 to M.sub.2 is higher than 1.0.

12. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, the electropolished stainless steel container satisfies a condition 3 or a condition 4 in the following test, test: a portion of the chemical liquid is adopted as f liquid, the liquid contact portion is washed using f liquid, a portion of the chemical liquid is adopted as g liquid, and under the condition that a ratio of a mass of the washed electropolished stainless steel container to a mass of g liquid becomes 0.25 provided that a liquid temperature of g liquid is 25° C., the washed electropolished stainless steel container is immersed for 24 hours in g liquid having a liquid temperature of 25° C., condition 3: in a case where g liquid having been used for the immersion contains one kind of metal component, an increase of one kind of the metal component before and after the immersion is equal to or smaller than 1 mass ppm, condition 4: in a case where g liquid having been used for the immersion contains two or more kinds of metal components, a total increase of two or more kinds of the metal components before and after the immersion is equal to or smaller than 1 mass ppm.

13. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, within a surface of at least a portion of the liquid contact portion, provided that an atom number ratio of the number of chromium atoms contained in the surface to the number of iron atoms contained in the surface is P.sub.1, and an atom number ratio of the number of chromium atoms contained in a position, which is 10 nm below the surface in a thickness direction of the electropolished stainless steel container, to the number of iron atoms contained in the position is P.sub.2, a ratio of P.sub.1 to P.sub.2 is higher than 1.0.

14. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, within a surface of at least a portion of the liquid contact portion, an atom number ratio of the number of chromium atoms contained in a position, which is 1 nm below the surface in a thickness direction of the electropolished stainless steel container, to the number of iron atoms contained in the position is equal to or higher than 1.0.

15. The quality inspection method for the chemical liquid according to claim 1, wherein the chemical liquid contains at least one kind of organic solvent selected from a group consisting of propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, methoxymethyl propionate, cyclopentanone, cyclohexanone, γ-butyrolactone, diisoamyl ether, butyl acetate, isoamyl acetate, isopropanol, and 4-methyl-2-pentanol.

16. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement includes organic analysis for measuring a content of an organic component in c liquid and inorganic analysis for measuring a content of an inorganic component in c liquid.

17. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, high-performance liquid chromatography mass spectrometry, high-performance liquid chromatography tandem mass spectrometry, and inductively coupled plasma mass spectrometry.

18. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and high-performance liquid chromatography tandem mass spectrometry.

19. The quality inspection method for the chemical liquid according to claim 1, wherein each of the content of the specific component measured in the step B and the standard value compared in the step C is an absolute quantity.

20. The quality inspection method for the chemical liquid according to claim 1, wherein each of the content of the specific component measured in the step B and the standard value compared in the step C is a relative quantity.

21. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, high-performance liquid chromatography mass spectrometry, and high-performance liquid chromatography tandem mass spectrometry, and the specific component contains an organic substance in which m/Z is 300 to 1,000.

22. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement includes inorganic analysis for analyzing a content of an inorganic component in c liquid, and provided that the content of the specific component measured in the step B is an absolute quantity, the absolute quantity is determined by a standard addition method.

23. The quality inspection method for the chemical liquid according to claim 1, wherein in a case where the content of the specific component is be equal to or smaller than the standard value in the step C, the chemical liquid is determined as being adequate.

24. The quality inspection method for the chemical liquid according to claim 1, wherein the specific component contains an organic substance having a boiling point equal to or higher than 200° C.

25. The quality inspection method for the chemical liquid according to claim 24, wherein the specific component contains an organic substance having a boiling point of 300° C. to 800° C.

26. The quality inspection method for the chemical liquid according to claim 1, wherein the specific component contains an organic substance having a molecular weight equal to or greater than 200.

27. The quality inspection method for the chemical liquid according to claim 26, wherein the specific component contains an organic substance having a molecular weight of 300 to 1,000.

28. The quality inspection method for the chemical liquid according to claim 1, further comprising: a specific component determination step that is performed before the step W or between the step W and the step A, wherein the specific component determination step includes a step W3 of preparing a third container having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from the group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, adopting a portion of the chemical liquid as h liquid, and washing at least a portion of the liquid contact portion of the third container by using h liquid, a step A3 of adopting a portion of the chemical liquid as i liquid and concentrating i liquid by using the washed third container so as to obtain three or more kinds of j liquids having different factors of concentration, a step B3 of performing measurement of a content of an organic substance, in which m/Z is 300 to 1,000, in j liquids by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and gas chromatography mass spectrometry, and a step C3 in which in a case where one kind of organic substance is commonly detected from all of three or more kinds of j liquids, one kind of the organic substance is determined as a specific component, and in a case where two or more kinds of organic substances are commonly detected from all of three or more kinds of j liquids, from a coefficient of correlation obtained by performing linear regression on the factors of concentration and the content of each of two or more kinds of the organic substances and a coefficient of correlation obtained by performing linear regression on the factors of concentration and the total content of organic substances in a combination of two or more kinds of the organic substances, a maximum coefficient of correlation is selected, and an organic substance or a combination of organic substances from which the maximum coefficient of correlation is obtained is determined as a specific component, the step W3, the step A3, the step B3, and the step C3 are performed in this order, at least the step W3 and the step A3 are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1:2015 established by the International Organization for Standardization, and the concentration of i liquid is performed under at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N.sub.2 gas or under reduced pressure.

29. The quality inspection method for the chemical liquid according to claim 28, further comprising: a standard value determination step of determining the standard value at a point in time when the specific component determination step has finished but the step C is not yet started, wherein the standard value determination step includes a step W4 of preparing n pieces of fourth containers each having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from the group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, preparing n kinds of chemical liquids manufactured by different manufacturing methods, obtaining twice a portion of each of n kinds of the chemical liquids, naming the obtained chemical liquids as p.sub.1 liquid and p.sub.2 liquid respectively, and washing at least a portion of the liquid contact portion of each of the fourth containers by using each of p.sub.1 liquids, a step A4 of performing concentration of each of the corresponding liquids p.sub.2 by using each of the fourth containers washed with each of the liquids p.sub.1 so as to obtain n kinds of liquids q, a step B4 of performing measurement of a content of a specific component in each of q liquids by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and gas chromatography mass spectrometry, a step S of evaluating a defect inhibition performance of each of n kinds of the chemical liquids by using a defect inspection device, a step T of creating a calibration curve by performing linear regression on the content of the specific component and the defect inhibition performance, and a step U of determining the content of the specific component corresponding to a predetermined defect inhibition performance as a standard value by using the calibration curve, the step W4, the step A4, the step B4, the step S, the step T, and the step U are performed in this order, at least the step W4 and the step A4 are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1:2015 established by the International Organization for Standardization, the concentration of p.sub.2 liquid is performed under at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N.sub.2 gas or under reduced pressure, and n represents an integer equal to or greater than 3.

30. The quality inspection method for the chemical liquid according to claim 1, wherein the measurement includes inorganic analysis for measuring a content of an inorganic substance in c liquid, and the inorganic analysis is measurement of a content of at least 5 or more kinds of atoms selected from a group consisting of Ag, Al, As, Au, Ba, Ca, Cd, Co, Cr, Cu, Fe, Ga, Ge, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Pb, Sb, Sn, Sr, Ta, Th, Ti, Tl, V, W, Zn, and Zr in c liquid.

31. The quality inspection method for the chemical liquid according to claim 30, wherein 5 or more kinds of the atoms contain at least two or more kinds of atoms selected from a group consisting of Al, Fe, and Ti.

Description

EXAMPLES

(1) Hereinafter, the present invention will be more specifically described based on examples. The materials, the amount and proportion of the materials used, the details of treatments, the procedure of treatments, and the like shown in the following examples can be appropriately modified as long as the gist of the present invention is maintained. Accordingly, the scope of the present invention is not limited to the following examples.

Test Example 1: Preparation of Chemical Liquid

(2) By the following method, chemical liquids 1-1 to 1-4 which contained an organic solvent shown in Table 1 and purified by different methods were prepared.

(3) [Chemical Liquid 1-1]

(4) A substance to be purified containing an organic solvent described in Table 1 was distilled and then purified by passing through the following filters in the following order, thereby obtaining a chemical liquid 1-1. That is, the substance to be purified was subjected to multistage filtration using a first filter: filter made of polytetrafluoroethylene (PTFE) having a pore size of 15 nm, a second filter: 12 nm PTFE manufactured by Entegris, Inc. (filter made of PTFE having a pore size of 12 nm), and a third filter: 10 nm IEX PTFE manufactured by Entegris, Inc. (filter having a pore size of 10 nm constituted with a base material made of PTFE having a sulfo group on the surface thereof), thereby manufacturing the chemical liquid. This method is called purification method “A”.

(5) [Chemical Liquid 1-2]

(6) A substance to be purified containing an organic solvent was distilled and then subjected to multistage filtration using a first filter: 12 nm PTFE manufactured by Entegris, Inc. (filter having a pore size of 12 nm made of PTFE) and a second filter: 10 nm IEX PTFE manufactured by Entegris, Inc. (filter having a pore size of 10 nm constituted with a base material made of PTFE having a sulfo group on the surface thereof), thereby manufacturing a chemical liquid 1-2. This method is called purification method “B”.

(7) [Chemical Liquid 1-3]

(8) A substance to be purified containing an organic solvent was distilled and then filtered using only 10 nm IEX PTFE manufactured by Entegris, Inc. (filter having a pore size of 10 nm constituted with a base material made of PTFE having a sulfo group on the surface thereof), thereby manufacturing a chemical liquid 1-3. This method is called purification method “C”.

(9) [Chemical Liquid 1-4]

(10) A substance to be purified containing nBA was distilled and then filtered using only PTFE (filter having a pore size of 15 nm made of PTFE), thereby manufacturing a chemical liquid 1-4. This method is called purification method “D”.

(11) Each of the substances to be purified was purified in a clean room (class 1) by using a “high-purity grade” organic solvent described in Table 1 having purity equal to or higher than 99% by mass.

(12) The organic solvent contained in the used substances to be purified and the second container storing the manufactured chemical liquid are shown in Table 1.

Test Example 1: Determination of Specific Component

(13) A chemical liquid prepared by the same method as that used for preparing the chemical liquid 1-1 was stored in a clean bottle made of perfluoroalkoxyalkane (PFA), and the bottle was sealed by putting a lid thereon, thereby obtaining a chemical liquid storage body.

(14) Then, the chemical liquid storage body was opened in a clean room of class 1, and the chemical liquid was concentrated under reduced pressure by using a Soxhlet extractor. At a point in time when the factor of concentration became 100×, 300×, 500×, and 1,000×, the chemical liquid was extracted, thereby preparing measurement samples.

(15) For the concentration of the chemical liquid, a glass container was used which was subjected to acid washing by using diluted HF and HNO.sub.3, then washed with ultrapure water and with the chemical liquid, and then dried.

(16) Thereafter, for each of the measurement samples, by using LC/MS and GC/MS, the content of all the compounds in which m/Z was 300 to 1,000 (value of integral of signal intensity in a mass chromatogram) was analyzed. As the measurement results, the contents of detected components (value of integral of signal intensity: relative quantity) and the total content of a combination of the components (sum of the values of integral of signal intensity: relative quantity) were plotted on the ordinate, and the factors of concentration were plotted on the abscissa.

(17) Subsequently, a component or a combination thereof from which a maximum coefficient of correlation was obtained through linear regression was searched for, and the combination of components described in Table 1 was determined as a specific component in each example.

(18) Specific component A: a combination of compounds in which m/Z=300 to 1,000 including the compounds of Formulae (1) to (7) (“Content of specific component A” is the total content of the above compounds)

(19) Specific component B: a combination of compounds of Formulae (1) to (7) (“Content of specific component B” is the total content of the compounds of Formulae (1) to (7))

Test Example 1: Preparation of Concentrated Liquid

(20) By using a Soxhlet extractor, the chemical liquids 1-1 to 1-4 were concentrated under reduced pressure such that the factor of concentration set for each of the measurement methods, which will be described later, was achieved, and the concentrated liquids were collected in a nitrogen atmosphere. This operation was performed in a class 1 clean room.

(21) (Washing of Container)

(22) The fourth container used for the concentration of the chemical liquid was made of glass. The fourth container was subjected to acid washing by using diluted HF and HNO.sub.3, then washed with ultrapure water and then with each of the chemical liquids 1-1 to 1-4 (specific washing solutions), and then dried.

(23) <Measurement of P.sub.1 and P.sub.2>

(24) By using a time-of-flight secondary ion mass spectrometer (manufactured by IONTOF GmbH, trade name: “TOF-SIMS5”), P.sub.1 and P.sub.2 were measured under the following conditions.

(25) Primary ion: Bi.sub.3.sup.2+

(26) Primary ion acceleration voltage: 25 kV

(27) Measurement area: 500 μm×500 μm

(28) Measurement temperature: equal to or lower than −100° C.

(29) For etching, Ar-GCIB (Ar gas cluster ion beam) was radiated. Furthermore, as a primary ion source, Bi.sup.3+ was radiated, and the obtained secondary ion was analyzed using time-of-flight type mass spectrometer, thereby obtaining a spectrum.

(30) Ar-GCIB injection pressure: 3 MPa

(31) Measurement surface: 150 μm×150 μm

(32) Measurement mode: high mass resolution

(33) <Elution Test>

(34) A portion of each of the chemical liquids was adopted as an immersion liquid, and the washed first container was immersed for 24 hours in each of the immersion liquids at a liquid temperature of 25° C., under the condition that a mass ratio (g/g) of the mass of the washed first container to the mass of the immersion liquid became 1.0. The increase in the content of fluoride ions contained in the immersion liquid before and after the immersion was measured by the following method. The results are shown in Table 1. In Table 1, “<” means that the measurement result is less than the numerical value described in the table. Furthermore, in Table 1, “ppm” in the columns of “Fluoride ion” and “Metal component” means “mass ppm”.

(35) (Fluoride Ion)

(36) For the measurement, HIC-SP suppressor ion chromatograph manufactured by Shimadzu Corporation was used. The measurement conditions are as below.

(37) Measurement Conditions

(38) Used column: ion exchange resin (inner diameter: 4.0 mm, length: 25 cm)

(39) Mobile phase: sodium hydrogen carbonate solution (1.7 mmol/L)-sodium carbonate solution (1.8 mmol/L), flow rate: 1.5 mL/min

(40) Amount of sample injected: 25 μL

(41) Column temperature: 40° C.

(42) Suppressor: electrodialysis type detector: electric conductivity detector (30° C.)

(43) (Metal Component)

(44) For the measurement, Agilent 8800 triple quadrupole ICP-MS (for semiconductor analysis, option #200) was used. Based on the measurement results, the content of the metal particles and the content of the metal ions were determined.

(45) Measurement Conditions

(46) As a sample introduction system, a quartz torch, a coaxial perfluoroalkoxyalkane (PFA) nebulizer (for self-suction), and a platinum interface cone were used. The measurement parameters of cool plasma conditions are as below.

(47) Output of Radio Frequency (RF) (W): 600

(48) Flow rate of carrier gas (L/min): 0.7

(49) Flow rate of makeup gas (L/min): 1

(50) Sampling depth (mm): 18

Test Example 1: Measurement

(51) By the following method, the content of the specific component in each of the obtained concentrated liquids was measured.

(52) [LC/MS]

(53) As samples, 1,000× concentrated liquids were used. The content of the specific component was measured using a liquid chromatography mass spectrometer (trade name: “UPLC-H-Class, Xevo G2-XS QTof”, manufactured by Thermo Fisher Scientific K. K., adopting the following measurement conditions) as LC/MS. As the specific component, compounds in which m/XZ was 300 to 1,000 (including the compounds represented by Formulae (1) to (7)) measured by the method described above were adopted. The results were expressed as an exponent (relative quantity) determined on the premise that the signal intensity of the concentrated liquid of the chemical liquid 1-1 is 1.0.

(54) (Measurement Conditions)

(55) LC Conditions

(56) Device: UPLC-H-Class

(57) Column: ACQUITY UPLC C8 1.7 μm, 2.1×100 mm

(58) Column temperature: 40° C.

(59) Mobile phase: A: 0.1% formic acid, B: 0.1% formic acid-containing MeOH

(60) Flow rate: 0.5 mL/min

(61) Injection amount: 2 μL

(62) MS Conditions

(63) Device: Xevo G2-XS Q-Tof

(64) Ionization mode: ESI positive/negative

(65) Capillary voltage: 1.0 kV/2.5 kV

(66) Desolvation gas: 1,000 L/hr, 500° C.

(67) Cone gas: 50 L/hr

(68) Cone voltage: 40 V (offset 80 V)

(69) Collision energy: 2 eV

(70) Measurement range: m/z 100 to 1,000

(71) Measurement mode: MS Sensitivity Mode (resolution/30,000)

(72) [GC/MS]

(73) As samples, 1,000× concentrated liquids were used. The content of an organic impurity having a boiling point equal to or higher than 200° C. in each of the measurement samples was measured using a gas chromatography mass spectrometer (trade name “GCMS-2020”, manufactured by Shimadzu Corporation, adopting the following measurement conditions). As the specific component, compounds in which m/Z was 300 to 1,000 (including the compounds represented by Formulae (1) to (7)) measured by the method described above were adopted. The results were expressed as an exponent (relative quantity) determined on the premise that the signal intensity of the concentrated liquid of the chemical liquid 1-1 is 1.0.

(74) (Measurement Conditions)

(75) Capillary column:

(76) InertCap 5MS/NP 0.25 mm I. D.×30 m df=0.25 μm

(77) Sample introduction method: split 75 kPa constant pressure

(78) Vaporizing chamber temperature: 250° C.

(79) Column oven temperature: 80° C. (2 min)−500° C. (13 min) heating rate 15° C./min

(80) Carrier gas: helium

(81) Septum purge flow rate: 5 mL/min

(82) Split ratio: 25:1

(83) Interface temperature: 250° C.

(84) Ion source temperature: 200° C.

(85) Measurement mode: Scan m/z=85 to 500

(86) Amount of sample introduced: 1 μL

(87) [DI-MS]

(88) As samples, 1,000,000× concentrated liquids were used. The content of an organic impurity having a boiling point equal to or higher than 200° C. in each of the measurement samples was measured using a gas chromatography mass spectrometer (trade name “GCMS-QP2010 Ultra”, manufactured by Shimadzu Corporation, adopting the following measurement conditions). As the specific component, compounds represented by Formulae (1) to (7) were adopted, and the total amount thereof was measured. The results were expressed as an exponent (relative quantity) determined on the premise that the signal intensity of the concentrated liquid of the chemical liquid 1-1 is 1.0.

(89) (Measurement Conditions)

(90) Sample introduction method: direct introduction (DI without using GC portion)

(91) Ion source temperature: 230° C.

(92) Interface temperature: 240° C.

(93) Ionization mode: SEI

(94) Measurement mode: Scan m/z=30 to 1,000

(95) [NMR]

(96) As samples, 10,000× concentrated liquids were used. As the specific component, the compounds represented by Formulae (1) to (7) were adopted, and the total amount thereof was measured. The results are expressed as an absolute quantity (mass ppb).

(97) (Measurement Conditions)

(98) Device: AL400 model manufactured by JEOL Ltd.

(99) Nucleus for measurement: .sup.1H

(100) Solvent: CDCl3

(101) [ICP-MS]

(102) As samples, 100× concentrated liquids were used. The content of metal atoms in each of the measurement samples was measured using an ICP-MS mass spectrometer (trade name: “Agilent 8800”, manufactured by Agilent Technologies, Inc, adopting the following measurement conditions). As the specific component, the total content of Ag, Al, As, Au, Ba, Ca, Cd, Co, Cr, Cu, Fe, Ga, Ge, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Pb, Sb, Sn, Sr, Ta, Th, Ti, Tl, V, W, Zn, Zr, and Mo were adopted, and the total amount thereof was measured. The result was expressed as an absolute quantity (mass ppt).

(103) (Measurement conditions)

(104) Measurement device: Agilent 8800

(105) RF output (W): 600

(106) Flow rate of carrier gas (L/min): 0.7

(107) Flow rate of makeup gas (L/min): 1

(108) Sampling position (mm): 18

(109) [Evaluation of Defect Inhibition Performance]

(110) First, a silicon oxide film substrate having a diameter of about 300 mm (12 inches) was prepared.

(111) Then, by using a wafer surface inspection device (SP-5; manufactured by KLA-Tencor Corporation), the number of defects having a diameter equal to or greater than 17 nm present on the substrate was counted (the counted number was adopted as an initial value).

(112) Thereafter, by using “CLEAN TRACK LITHIUS (trade name)” manufactured by Tokyo Electron Limited, the substrate was spin-coated with each of the chemical liquids at 1,500 rpm and then spin-dried.

(113) Subsequently, by using the device (SP-5), the number of defects present on the substrate coated with the chemical liquid was counted (the counted number was adopted as a counted value). Then, a difference between the initial value and the counted value (initial value-counted value) was calculated and adopted as total number of defects. The total number of defects represents the defect inhibition performance of a chemical liquid. It is determined that the smaller the total number of defects, the better the defect inhibition performance.

(114) Furthermore, the coordinates of the defects were read using a full automatic defect review device “SEMVision G6” manufactured by Applied Materials, Inc., the composition of each of the defects was analyzed by energy dispersive X-ray spectroscopy, and the number of defects containing metal atoms was counted as the number of metal defects. The number of metal defects represents the defect inhibition performance of a chemical liquid. It is determined that the smaller the number of metal defects, the better the defect inhibition performance. In Table 1, the unit of the total number of defects and the number of metal defects is number/12 inchWf (number of defects on a 12-inch wafer, 12 inches approximately equal 300 mm).

Test Example 1: Checking results

(115) For the chemical liquids 1-1 to 1-4 among which the content of the specific component varied, a coefficient of correlation was determined by performing linear regression on the measured content of the specific component (LC/MS, GC/MS, DI-MS, and NMR) and the total number of defects, and another coefficient of correlation was determined by performing linear regression on the measured content of the specific component (ICP-MS) and the number of metal defects. The results are shown in Table 1. The results show that the closer the coefficient of correlation to 1, the higher the obtained positive coefficient of correlation.

Test Examples 2 to 22

(116) In each of Test Examples 2 to 22, each of substances to be purified containing an organic solvent described in Table 1 was purified by the purification methods A to D described above and then stored in the second container described in Table 1, thereby manufacturing a chemical liquid storage body. In Table 1, regarding the chemical liquid denoted by “(first number)-(second number)”, “(first number)” corresponds to the number of the test example, and “(second number)” corresponds to the purification method. That is, regarding (second number), 1 corresponds to A, 2 corresponds to B, 3 corresponds to C, and 4 corresponds to D.

(117) Then, the chemical liquid storage body was opened in a class 1 clean room, and the chemical liquid was concentrated by the method described in Table 1 by using the fourth container having a liquid contact portion formed of a material described in Table 1.

(118) The physical properties of the liquid contact portion of the fourth container used and the results of the elution test are described in Table 1.

(119) In Table 1, “Electropolished SUS” means that the container had a liquid contact portion formed of electropolished stainless steel, “PTFE container” means that the container had a liquid contact portion formed of polytetrafluoroethylene, “Washed with water” means that the container was washed with ultrapure water without being subjected to acid washing, “-” means that the corresponding treatment was not performed, “In the atmosphere” means that the treatment was not performed in a clean room, “Heating concentration N2” means that the chemical liquid was concentrated by heating in a N.sub.2 gas environment, and “Heating concentration Ar” means that the chemical liquid was concentrated by heating in an Ar gas environment.

(120) For the concentrated liquid, the content of the specific component was measured by the same method as in Test Example 1 and compared with the defect inhibition performance measured by the same method as in Test Example 1. In a case where the content of the specific component was expressed as a relative value, the value was expressed as an exponent determined on the premise that the specific signal intensity of the concentrated liquid purified by the purification method A (chemical liquid denoted by “(first number)−1”) is 1.0.

(121) From the above results, it was understood that in Test Examples 1 to 22, there is a strong correlation between the measured content of the specific component and the number of defects (defect inhibition performance) measured by the defect inspection device.

(122) From the results shown in Table 1, it was understood that in a case where linear regression was performed on the content of the specific component and the number of defects (defect inhibition performance) measured by the defect inspection device, the obtained coefficient of correlation was higher in Test Example 1 performed in a predetermined clean room than in Test Example 2.

(123) From the results shown in Table 1, it was understood that in a case where PGME, PGEE, PGMEA, EL, MPM, CyPe, CyHe, γBL, DIAE, MIBC, or a mixture of PGMEA and PGME (volume ratio=7:3) was used as an organic solvent, by the linear regression performed on the content of the specific component and the number of defects (defect inhibition performance) measured by the defect inspection device, a higher coefficient of correlation was obtained.

(124) From the results shown in Table 1, it was understood that in a case where linear regression was performed on the content of the specific component (particularly, the specific organic substance) and the number of defects (defect inhibition performance) measured by the defect inspection device, the obtained coefficient of correlation was higher in Test Example 10, in which the liquid contact portion of the fourth container was formed of glass, than in Test Example 17 in which the liquid contact portion of the fourth container was formed of PTFE.

(125) It was understood that in a case where linear regression was performed on the content of the specific component (particularly, the specific organic substance) and the number of defects (defect inhibition performance) measured by the defect inspection device, the obtained coefficient of correlation was higher in Test Example 10, in which the liquid contact portion of the second container in the chemical liquid storage body was formed of a fluorine-containing polymer, than in Test Example 18 in which the liquid contact portion of the second container was formed of electropolished stainless steel.

(126) From the results shown in Table 1, it was understood that in a case where linear regression was performed on the content of the specific component (particularly, the specific organic substance) and the number of defects (defect inhibition performance) measured by the defect inspection device, the obtained coefficient of correlation was higher in Test Example 10, in which acid washing was performed, than in Test Example 21 in which acid washing was not performed.

(127) From the results shown in Table 1, it was understood that in a case where linear regression was performed on the content of the specific component (particularly, the specific organic substance) and the number of defects (defect inhibition performance) measured by the defect inspection device, the obtained coefficient of correlation was higher in Test Example 10, in which ultrasonic washing was performed, than in Test Example 22 in which ultrasonic washing was not performed.

(128) TABLE-US-00001 TABLE 1 Step W4 Fourth container Material Step Liquid Result of Chemical liquid of liquid Specific contact elution test Organic Second contact Acid Ultrasonic washing portion Fluoride Metal TABLE 1-1-1 No. solvent container portion washing washing solution Drying P.sub.1 P.sub.2 ion component Test Example 1  1-1 nBA PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  1-2 bottle HNO3 .fwdarw.  1-3 washed  1-4 with water Test Example 2  2-1 nBA PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  2-2 bottle HNO3 .fwdarw.  2-3 washed  2-4 with water Test Example 3  3-1 PGME PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  3-2 bottle HNO3 .fwdarw.  3-3 washed  3-4 with water Test Example 4  4-1 PGEE PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  4-2 bottle HNO3 .fwdarw.  4-3 washed  4-4 with water Test Example 5  5-1 PGPE PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  5-2 bottle HNO3 .fwdarw.  5-3 washed  5-4 with water Test Example 6  6-1 PGMEA PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  6-2 bottle HNO3 .fwdarw.  6-3 washed  6-4 with water Test Example 7  7-1 EL PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  7-2 bottle HNO3 .fwdarw.  7-3 washed  7-4 with water Test Example 8  8-1 MPM PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  8-2 bottle HNO3 .fwdarw.  8-3 washed  8-4 with water Test Example 9  9-1 CyPe PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm  9-2 bottle HNO3 .fwdarw.  9-3 washed  9-4 with water Test Example 10 10-1 CyHe PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm 10-2 bottle HNO3 .fwdarw. 10-3 washed 10-4 with water Test Example 11 11-1 γBL PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm 11-2 bottle HNO3 .fwdarw. 11-3 washed 11-4 with water Test Example 12 12-1 DIAE PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm 12-2 bottle HNO3 .fwdarw. 12-3 washed 12-4 with water Test Example 13 13-1 iAA PFA clean Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm 13-2 bottle HNO3 .fwdarw. 13-3 washed 13-4 with water

(129) TABLE-US-00002 TABLE 2 Step A4 Step B4 Concentration Concentration Measurement LC/MS GC/MS DI-MS NMR Table 1-1- 2 environment condition environment (relative quantity) (relative quantity) (relative quantity) (mass ppb) Test Class 1 Pressure reduction Class 1 1.0 Specific 1.0 Specific 1.0 Specific 3.0 Specific Example 1  in vacuum 1.5 component 1.3 component 2.1 component 9.0 component 2.0 A 2.1 A 3.5 B 10.0 B 3.0 3.2 3.6 20.0 Test Class 1 Pressure reduction In the 1.0 1.0 1.0 3.0 Example 2  in vacuum atmosphere 2.7 2.4 3.9 16.6 3.0 2.5 4.0 17.3 3.7 2.6 4.2 17.0 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 2.0 Example 3  in vacuum 1.2 1.5 2.5 10.5 1.4 2.1 3.4 11.0 1.6 2.6 4.2 18.2 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 5.0 Example 4  in vacuum 1.4 1.6 2.6 11.3 1.8 2.4 3.8 16.4 2.2 3.6 5.8 17.1 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 6.0 Example 5  in vacuum 1.5 2.9 4.7 20.0 2.0 3.6 5.7 24.6 3.0 4.4 7.1 26.4 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 5.0 Example 6  in vacuum 1.8 1.9 3.1 13.4 2.6 2.6 4.2 18.2 3.4 3.1 5.0 19.4 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 4.0 Example 7  in vacuum 1.7 1.6 2.6 11.0 2.4 2.0 3.2 16.0 3.1 2.2 3.5 15.2 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 4.0 Example 8  in vacuum 1.6 1.4 2.2 10.0 2.2 1.7 2.8 10.2 2.8 2.0 3.3 14.1 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 3.0 Example 9  in vacuum 1.3 1.2 2.0 8.4 1.6 1.4 2.3 10.0 1.9 1.4 2.6 10.6 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 1.0 Example 10 in vacuum 1.4 1.2 1.9 2.9 1.8 1.4 2.8 9.6 2.2 1.9 3.4 10.5 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 8.0 Example 11 in vacuum 1.8 1.9 3.1 10.2 2.6 2.8 4.6 19.5 3.4 3.7 6.0 21.3 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 4.0 Example 12 in vacuum 1.2 1.5 2.5 10.5 1.4 2.1 3.4 11.4 1.6 2.6 4.2 18.2 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 3.0 Example 13 in vacuum 1.5 1.4 2.3 9.8 3.0 1.9 3.1 13.3 3.8 1.9 3.1 13.4

(130) TABLE-US-00003 TABLE 3 Step B4 Table ICP-MS (mass ppt) 1-1-3 Ag Al As Au Ba Ca Cd Test 0.010 0.030 0.001 0.001 0.002 0.050 0.001 Example 0.014 0.042 0.001 0.001 0.003 0.070 0.001  1 0.020 0.059 0.002 0.002 0.004 0.098 0.002 0.027 0.082 0.003 0.003 0.005 0.137 0.003 Test 0.048 0.144 0.005 0.005 0.010 0.240 0.005 Example 0.067 0.202 0.007 0.007 0.013 0.336 0.007  2 0.094 0.282 0.009 0.009 0.019 0.470 0.009 0.132 0.395 0.013 0.013 0.026 0.659 0.013 Test 0.008 0.024 0.001 0.001 0.002 0.040 0.001 Example 0.011 0.034 0.001 0.001 0.002 0.056 0.001  3 0.016 0.047 0.002 0.002 0.003 0.078 0.002 0.022 0.066 0.002 0.002 0.004 0.110 0.002 Test 0.012 0.036 0.001 0.001 0.002 0.060 0.001 Example 0.017 0.050 0.002 0.002 0.003 0.084 0.002  4 0.024 0.071 0.002 0.002 0.005 0.118 0.002 0.033 0.099 0.003 0.003 0.007 0.165 0.003 Test 0.014 0.043 0.001 0.001 0.003 0.072 0.001 Example 0.020 0.060 0.002 0.002 0.004 0.101 0.002  5 0.028 0.085 0.003 0.003 0.006 0.141 0.003 0.040 0.119 0.004 0.004 0.008 0.198 0.004 Test 0.013 0.039 0.001 0.001 0.003 0.065 0.001 Example 0.018 0.054 0.002 0.002 0.004 0.091 0.002  6 0.025 0.076 0.003 0.003 0.005 0.127 0.003 0.036 0.107 0.004 0.004 0.007 0.178 0.004 Test 0.022 0.066 0.002 0.002 0.004 0.110 0.002 Example 0.031 0.093 0.003 0.003 0.006 0.154 0.003  7 0.043 0.130 0.004 0.004 0.009 0.216 0.004 0.060 0.181 0.006 0.006 0.012 0.302 0.006 Test 0.011 0.033 0.001 0.001 0.002 0.055 0.001 Example 0.015 0.046 0.002 0.002 0.003 0.077 0.002  8 0.022 0.065 0.002 0.002 0.004 0.108 0.002 0.030 0.091 0.003 0.003 0.006 0.151 0.003 Test 0.012 0.036 0.001 0.001 0.002 0.061 0.001 Example 0.017 0.051 0.002 0.002 0.003 0.085 0.002  9 0.024 0.071 0.002 0.002 0.005 0.119 0.002 0.033 0.100 0.003 0.003 0.007 0.166 0.003 Test 0.017 0.051 0.002 0.002 0.003 0.085 0.002 Example 0.024 0.071 0.002 0.002 0.005 0.119 0.002 10 0.033 0.100 0.003 0.003 0.007 0.166 0.003 0.047 0.140 0.005 0.005 0.009 0.233 0.005 Test 0.022 0.066 0.002 0.002 0.004 0.110 0.002 Example 0.031 0.093 0.003 0.003 0.006 0.154 0.003 11 0.043 0.130 0.004 0.004 0.009 0.216 0.004 0.061 0.182 0.006 0.006 0.012 0.303 0.006 Test 0.020 0.060 0.002 0.002 0.004 0.099 0.002 Example 0.028 0.083 0.003 0.003 0.006 0.139 0.003 12 0.039 0.117 0.004 0.004 0.008 0.195 0.004 0.054 0.163 0.005 0.005 0.011 0.272 0.005 Test 0.015 0.045 0.001 0.001 0.003 0.074 0.001 Example 0.021 0.063 0.002 0.002 0.004 0.104 0.002 13 0.029 0.088 0.003 0.003 0.006 0.146 0.003 0.041 0.123 0.004 0.004 0.008 0.204 0.004

(131) TABLE-US-00004 TABLE 4 Step B4 Table ICP-MS (mass ppt) 1-1-4 Co Cr Cu Fe Ga K Li Test 0.020 0.001 0.003 0.080 0.001 0.030 0.020 Example 0.028 0.001 0.004 0.112 0.001 0.042 0.028  1 0.039 0.002 0.006 0.157 0.002 0.059 0.039 0.055 0.003 0.008 0.220 0.003 0.082 0.055 Test 0.096 0.005 0.014 0.384 0.005 0.144 0.096 Example 0.134 0.007 0.020 0.538 0.007 0.202 0.134  2 0.188 0.009 0.028 0.753 0.009 0.282 0.188 0.263 0.013 0.040 1.054 0.013 0.395 0.263 Test 0.016 0.001 0.002 0.064 0.001 0.024 0.016 Example 0.022 0.001 0.003 0.090 0.001 0.034 0.022  3 0.031 0.002 0.005 0.125 0.002 0.047 0.031 0.044 0.002 0.007 0.176 0.002 0.066 0.044 Test 0.024 0.001 0.004 0.096 0.001 0.036 0.024 Example 0.034 0.002 0.005 0.134 0.002 0.050 0.034  4 0.047 0.002 0.007 0.188 0.002 0.071 0.047 0.066 0.003 0.010 0.263 0.003 0.099 0.066 Test 0.029 0.001 0.004 0.115 0.001 0.043 0.029 Example 0.040 0.002 0.006 0.161 0.002 0.060 0.040  5 0.056 0.003 0.008 0.226 0.003 0.085 0.056 0.079 0.004 0.012 0.316 0.004 0.119 0.079 Test 0.026 0.001 0.004 0.104 0.001 0.039 0.026 Example 0.036 0.002 0.005 0.145 0.002 0.054 0.036  6 0.051 0.003 0.008 0.203 0.003 0.076 0.051 0.071 0.004 0.011 0.284 0.004 0.107 0.071 Test 0.044 0.002 0.007 0.176 0.002 0.066 0.044 Example 0.062 0.003 0.009 0.247 0.003 0.093 0.062  7 0.086 0.004 0.013 0.345 0.004 0.130 0.086 0.121 0.006 0.018 0.484 0.006 0.181 0.121 Test 0.022 0.001 0.003 0.088 0.001 0.033 0.022 Example 0.031 0.002 0.005 0.123 0.002 0.046 0.031  8 0.043 0.002 0.006 0.173 0.002 0.065 0.043 0.060 0.003 0.009 0.242 0.003 0.091 0.060 Test 0.024 0.001 0.004 0.097 0.001 0.036 0.024 Example 0.034 0.002 0.005 0.136 0.002 0.051 0.034  9 0.048 0.002 0.007 0.190 0.002 0.071 0.048 0.067 0.003 0.010 0.266 0.003 0.100 0.067 Test 0.034 0.002 0.005 0.136 0.002 0.051 0.034 Example 0.048 0.002 0.007 0.190 0.002 0.071 0.048 10 0.067 0.003 0.010 0.266 0.003 0.100 0.067 0.093 0.005 0.014 0.372 0.005 0.140 0.093 Test 0.044 0.002 0.007 0.176 0.002 0.066 0.044 Example 0.062 0.003 0.009 0.247 0.003 0.093 0.062 11 0.086 0.004 0.013 0.346 0.004 0.130 0.086 0.121 0.006 0.018 0.484 0.006 0.182 0.121 Test 0.040 0.002 0.006 0.159 0.002 0.060 0.040 Example 0.056 0.003 0.008 0.222 0.003 0.083 0.056 12 0.078 0.004 0.012 0.311 0.004 0.117 0.078 0.109 0.005 0.016 0.436 0.005 0.163 0.109 Test 0.030 0.001 0.004 0.119 0.001 0.045 0.030 Example 0.042 0.002 0.006 0.167 0.002 0.063 0.042 13 0.058 0.003 0.009 0.233 0.003 0.088 0.058 0.082 0.004 0.012 0.327 0.004 0.123 0.082

(132) TABLE-US-00005 TABLE 5 Step B4 Table ICP-MS (mass ppt) 1-1-5 Mg Mn Mo Na Nb Ni Pb Test 0.010 0.002 0.001 0.030 0.001 0.001 0.001 Example 0.014 0.003 0.001 0.042 0.001 0.001 0.001  1 0.020 0.004 0.002 0.059 0.002 0.002 0.002 0.027 0.005 0.003 0.082 0.003 0.003 0.003 Test 0.048 0.010 0.005 0.144 0.005 0.005 0.005 Example 0.067 0.013 0.007 0.202 0.007 0.007 0.007  2 0.094 0.019 0.009 0.282 0.009 0.009 0.009 0.132 0.026 0.013 0.395 0.013 0.013 0.013 Test 0.008 0.002 0.001 0.024 0.001 0.001 0.001 Example 0.011 0.002 0.001 0.034 0.001 0.001 0.001  3 0.016 0.003 0.002 0.047 0.002 0.002 0.002 0.022 0.004 0.002 0.066 0.002 0.002 0.002 Test 0.012 0.002 0.001 0.036 0.001 0.001 0.001 Example 0.017 0.003 0.002 0.050 0.002 0.002 0.002  4 0.024 0.005 0.002 0.071 0.002 0.002 0.002 0.033 0.007 0.003 0.099 0.003 0.003 0.003 Test 0.014 0.003 0.001 0.043 0.001 0.001 0.001 Example 0.020 0.004 0.002 0.060 0.002 0.002 0.002  5 0.028 0.006 0.003 0.085 0.003 0.003 0.003 0.040 0.008 0.004 0.119 0.004 0.004 0.004 Test 0.013 0.003 0.001 0.039 0.001 0.001 0.001 Example 0.018 0.004 0.002 0.054 0.002 0.002 0.002  6 0.025 0.005 0.003 0.076 0.003 0.003 0.003 0.036 0.007 0.004 0.107 0.004 0.004 0.004 Test 0.022 0.004 0.002 0.066 0.002 0.002 0.002 Example 0.031 0.006 0.003 0.093 0.003 0.003 0.003  7 0.043 0.009 0.004 0.130 0.004 0.004 0.004 0.060 0.012 0.006 0.181 0.006 0.006 0.006 Test 0.011 0.002 0.001 0.033 0.001 0.001 0.001 Example 0.015 0.003 0.002 0.046 0.002 0.002 0.002  8 0.022 0.004 0.002 0.065 0.002 0.002 0.002 0.030 0.006 0.003 0.091 0.003 0.003 0.003 Test 0.012 0.002 0.001 0.036 0.001 0.001 0.001 Example 0.017 0.003 0.002 0.051 0.002 0.002 0.002  9 0.024 0.005 0.002 0.071 0.002 0.002 0.002 0.033 0.007 0.003 0.100 0.003 0.003 0.003 Test 0.017 0.003 0.002 0.051 0.002 0.002 0.002 Example 0.024 0.005 0.002 0.071 0.002 0.002 0.002 10 0.033 0.007 0.003 0.100 0.003 0.003 0.003 0.047 0.009 0.005 0.140 0.005 0.005 0.005 Test 0.022 0.004 0.002 0.066 0.002 0.002 0.002 Example 0.031 0.006 0.003 0.093 0.003 0.003 0.003 11 0.043 0.009 0.004 0.130 0.004 0.004 0.004 0.061 0.012 0.006 0.182 0.006 0.006 0.006 Test 0.020 0.004 0.002 0.060 0.002 0.002 0.002 Example 0.028 0.006 0.003 0.083 0.003 0.003 0.003 12 0.039 0.008 0.004 0.117 0.004 0.004 0.004 0.054 0.011 0.005 0.163 0.005 0.005 0.005 Test 0.015 0.003 0.001 0.045 0.001 0.001 0.001 Example 0.021 0.004 0.002 0.063 0.002 0.002 0.002 13 0.029 0.006 0.003 0.088 0.003 0.003 0.003 0.041 0.008 0.004 0.123 0.004 0.004 0.004

(133) TABLE-US-00006 TABLE 6 Step B4 Table ICP-MS (mass ppt) 1-1-6 Sb Sn Sr Ta Th Ti Tl Test 0.001 0.001 0.009 0.001 0.001 0.040 0.001 Example 0.001 0.001 0.013 0.001 0.001 0.056 0.001  1 0.002 0.002 0.018 0.002 0.002 0.078 0.002 0.003 0.003 0.025 0.003 0.003 0.110 0.003 Test 0.005 0.005 0.043 0.005 0.005 0.192 0.005 Example 0.007 0.007 0.060 0.007 0.007 0.269 0.007  2 0.009 0.009 0.085 0.009 0.009 0.376 0.009 0.013 0.013 0.119 0.013 0.013 0.527 0.013 Test 0.001 0.001 0.007 0.001 0.001 0.032 0.001 Example 0.001 0.001 0.010 0.001 0.001 0.045 0.001  3 0.002 0.002 0.014 0.002 0.002 0.063 0.002 0.002 0.002 0.020 0.002 0.002 0.088 0.002 Test 0.001 0.001 0.011 0.001 0.001 0.048 0.001 Example 0.002 0.002 0.015 0.002 0.002 0.067 0.002  4 0.002 0.002 0.021 0.002 0.002 0.094 0.002 0.003 0.003 0.030 0.003 0.003 0.132 0.003 Test 0.001 0.001 0.013 0.001 0.001 0.058 0.001 Example 0.002 0.002 0.018 0.002 0.002 0.081 0.002  5 0.003 0.003 0.025 0.003 0.003 0.113 0.003 0.004 0.004 0.036 0.004 0.004 0.158 0.004 Test 0.001 0.001 0.012 0.001 0.001 0.052 0.001 Example 0.002 0.002 0.016 0.002 0.002 0.073 0.002  6 0.003 0.003 0.023 0.003 0.003 0.102 0.003 0.004 0.004 0.032 0.004 0.004 0.142 0.004 Test 0.002 0.002 0.020 0.002 0.002 0.088 0.002 Example 0.003 0.003 0.028 0.003 0.003 0.123 0.003  7 0.004 0.004 0.039 0.004 0.004 0.173 0.004 0.006 0.006 0.054 0.006 0.006 0.242 0.006 Test 0.001 0.001 0.010 0.001 0.001 0.044 0.001 Example 0.002 0.002 0.014 0.002 0.002 0.062 0.002  8 0.002 0.002 0.019 0.002 0.002 0.086 0.002 0.003 0.003 0.027 0.003 0.003 0.121 0.003 Test 0.001 0.001 0.011 0.001 0.001 0.048 0.001 Example 0.002 0.002 0.015 0.002 0.002 0.068 0.002  9 0.002 0.002 0.021 0.002 0.002 0.095 0.002 0.003 0.003 0.030 0.003 0.003 0.133 0.003 Test 0.002 0.002 0.015 0.002 0.002 0.068 0.002 Example 0.002 0.002 0.021 0.002 0.002 0.095 0.002 10 0.003 0.003 0.030 0.003 0.003 0.133 0.003 0.005 0.005 0.042 0.005 0.005 0.186 0.005 Test 0.002 0.002 0.020 0.002 0.002 0.088 0.002 Example 0.003 0.003 0.028 0.003 0.003 0.124 0.003 11 0.004 0.004 0.039 0.004 0.004 0.173 0.004 0.006 0.006 0.054 0.006 0.006 0.242 0.006 Test 0.002 0.002 0.018 0.002 0.002 0.079 0.002 Example 0.003 0.003 0.025 0.003 0.003 0.111 0.003 12 0.004 0.004 0.035 0.004 0.004 0.156 0.004 0.005 0.005 0.049 0.005 0.005 0.218 0.005 Test 0.001 0.001 0.013 0.001 0.001 0.060 0.001 Example 0.002 0.002 0.019 0.002 0.002 0.083 0.002 13 0.003 0.003 0.026 0.003 0.003 0.117 0.003 0.004 0.004 0.037 0.004 0.004 0.163 0.004

(134) TABLE-US-00007 TABLE 7 Step B4 Table ICP-MS (mass ppt) 1-1-7 V W Zn Zr Mo Total Test 0.001 0.001 0.006 0.001 0.001 0.360 Example 0.001 0.001 0.008 0.001 0.001 0.497  1 0.002 0.002 0.012 0.002 0.002 0.708 0.003 0.003 0.016 0.003 0.003 0.990 Test 0.005 0.005 0.029 0.005 0.005 1.732 Example 0.007 0.007 0.040 0.007 0.007 2.423  2 0.009 0.009 0.056 0.009 0.009 3.378 0.013 0.013 0.079 0.013 0.013 4.739 Test 0.001 0.001 0.005 0.001 0.001 0.292 Example 0.001 0.001 0.007 0.001 0.001 0.401  3 0.002 0.002 0.009 0.002 0.002 0.571 0.002 0.002 0.013 0.002 0.002 0.788 Test 0.001 0.001 0.007 0.001 0.001 0.428 Example 0.002 0.002 0.010 0.002 0.002 0.609  4 0.002 0.002 0.014 0.002 0.002 0.843 0.003 0.003 0.020 0.003 0.003 1.183 Test 0.001 0.001 0.009 0.001 0.001 0.510 Example 0.002 0.002 0.012 0.002 0.002 0.723  5 0.003 0.003 0.017 0.003 0.003 1.019 0.004 0.004 0.024 0.004 0.004 1.427 Test 0.001 0.001 0.008 0.001 0.001 0.464 Example 0.002 0.002 0.011 0.002 0.002 0.655  6 0.003 0.003 0.015 0.003 0.003 0.922 0.004 0.004 0.021 0.004 0.004 1.289 Test 0.002 0.002 0.013 0.002 0.002 0.788 Example 0.003 0.003 0.019 0.003 0.003 1.111  7 0.004 0.004 0.026 0.004 0.004 1.550 0.006 0.006 0.036 0.006 0.006 2.173 Test 0.001 0.001 0.007 0.001 0.001 0.394 Example 0.002 0.002 0.009 0.002 0.002 0.562  8 0.002 0.002 0.013 0.002 0.002 0.774 0.003 0.003 0.018 0.003 0.003 1.087 Test 0.001 0.001 0.007 0.001 0.001 0.430 Example 0.002 0.002 0.010 0.002 0.002 0.616  9 0.002 0.002 0.014 0.002 0.002 0.849 0.003 0.003 0.020 0.003 0.003 1.193 Test 0.002 0.002 0.010 0.002 0.002 0.616 Example 0.002 0.002 0.014 0.002 0.002 0.849 10 0.003 0.003 0.020 0.003 0.003 1.193 0.005 0.005 0.028 0.005 0.005 1.683 Test 0.002 0.002 0.013 0.002 0.002 0.788 Example 0.003 0.003 0.019 0.003 0.003 1.112 11 0.004 0.004 0.026 0.004 0.004 1.551 0.006 0.006 0.036 0.006 0.006 2.179 Test 0.002 0.002 0.012 0.002 0.002 0.717 Example 0.003 0.003 0.017 0.003 0.003 1.005 12 0.004 0.004 0.023 0.004 0.004 1.405 0.005 0.005 0.033 0.005 0.005 1.951 Test 0.001 0.001 0.009 0.001 0.001 0.528 Example 0.002 0.002 0.013 0.002 0.002 0.751 13 0.003 0.003 0.018 0.003 0.003 1.053 0.004 0.004 0.025 0.004 0.004 1.471

(135) TABLE-US-00008 TABLE 8 Evaluation Coefficient of correlation ICP- GC/ MS LC/MS MS DI-MS NMR and and and and and num- Total Num- total total total total ber num- ber of number number number number of Table ber of metal of of of of metal 1-1-8 defects defects defects defects defects defects defects Test 123 2 0.982 0.969 0.959 0.953 0.987 Example 250 5  1 370 7 492 9 Test 123 2 0.952 0.845 0.833 0.796 0.977 Example 250 5  2 370 7 492 9 Test 246 4 1.000 0.999 0.992 0.959 0.991 Example 500 9  3 740 12 984 18 Test 98.4 1 1.000 0.986 0.996 0.958 0.972 Example 200 4  4 296 5 393.6 7 Test 147.6 3 0.982 0.972 0.959 0.923 0.967 Example 300 5  5 444 9 590.4 11 Test 184.5 3 1.000 0.990 0.975 0.950 0.973 Example 375 7  6 555 11 738 13 Test 369 7 1.000 0.981 0.950 0.910 0.992 Example 750 12  7 1110 20 1476 27 Test 307.5 6 1.000 1.000 0.978 0.948 0.994 Example 625 11  8 925 15 1230 22 Test 172.2 2 1.000 0.910 0.958 0.915 0.976 Example 350 6  9 518 9 688.8 12 Test 246 3 1.000 0.955 0.996 0.955 0.972 Example 500 9 10 740 13 984 18 Test 147.6 3 1.000 1.000 0.997 0.956 0.965 Example 300 5 11 444 9 590.4 11 Test 233.7 2 1.000 0.999 0.992 0.967 0.968 Example 475 9 12 703 13 934.8 17 Test 369 5 0.981 0.952 0.931 0.920 0.980 Example 750 14 13 1110 20 1476 27

(136) TABLE-US-00009 TABLE 9 Step W4 Fourth container Material Step Liquid Result of elution Chemical liquid of liquid Specific contact Test Table Organic Second contact Ultrasonic washing portion Fluoride Metal 1-2-1 No. solvent container portion Acid washing washing solution Drying P.sub.1 P.sub.2 ion component Test 14-1 MIBC PFA Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 14-2 clean HNO3 .fwdarw. washed 14 14-3 bottle with water 14-4 Test 15-1 PGMEA/ PFA Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 15-2 PGME clean HNO3 .fwdarw. washed 15 15-3 (7:3) bottle with water 15-4 Test 16-1 CyHe PFA Electro- Diluted HF, Performed Performed Performed 1.2 0.6 <1 ppm <1 ppm Example 16-2 clean polished HNO3 .fwdarw. washed 16 16-3 bottle SUS with water 16-4 Test 17-1 CyHe PFA PTFE Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 17-2 clean container HNO3 .fwdarw. washed 17 17-3 bottle with water 17-4 Test 18-1 CyHe Electro- Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 18-2 polished HNO3 .fwdarw. washed 18 18-3 SUS with water 18-4 Test 19-1 CyHe PFA Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 19-2 clean HNO3 .fwdarw. washed 19 19-3 bottle with water 19-4 Test 20-1 CyHe PFA Glass Diluted HF, Performed Performed Performed <1 ppm <1 ppm Example 20-2 clean HNO3 .fwdarw. washed 20 20-3 bottle with water 20-4 Test 21-1 CyHe PFA Glass Washed with Performed Performed Performed <1 ppm <1 ppm Example 21-2 clean water 21 21-3 bottle 21-4 Test 22-1 CyHe PFA Glass Diluted HF, — Performed Performed <1 ppm <1 ppm Example 22-2 clean HNO3 .fwdarw. washed 22 22-3 bottle with water 22-4

(137) TABLE-US-00010 TABLE 10 Step A4 Step B4 Table Concentration Concentration Measurement LC/MS GC/MS DI-MS NMR 1-2- 2 environment condition environment (relative quantity) (relative quantity) (relative quantity) (mass ppb) Test Class 1 Pressure reduction Class 1 1.0 Specific 1.0 Specific 1.0 Specific 5.0 Specific Example in vacuum 1.6 component 1.6 component 2.6 component 11.0 component 14 2.2 A 2.3 A 3.7 B 15.7 B 2.8 2.3 3.8 16.2 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 3.0 Example in vacuum 1.9 1.0 3.6 3.6 15 2.8 2.6 4.2 4.8 3.7 3.1 4.3 19.1 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 6.0 Example in vacuum 2.1 1.1 1.2 6.4 16 2.3 1.9 3.0 7.0 3.8 2.0 3.0 13.6 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 2.0 Example in vacuum 1.5 1.6 2.6 13.0 17 3.0 2.1 3.4 14.5 4.0 2.3 3.5 16.2 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 9.0 Example in vacuum 1.8 1.7 2.7 11.7 18 3.5 2.9 4.7 12.0 3.8 3.2 5.1 21.1 Test Class 1 Heating Class 1 1.0 1.0 1.0 2.0 Example concentration 2.2 1.9 4.0 4.0 19 N2 3.5 2.8 4.4 19.0 4.1 3.1 5.0 21.5 Test Class 1 Heating Class 1 1.0 1.0 1.0 4.0 Example concentration 2.4 2.2 3.5 15.2 20 Ar 3.0 3.0 4.8 16.1 4.5 3.4 5.6 23.8 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 4.0 Example in vacuum 4.0 1.9 4.0 2.0 21 5.5 2.8 4.4 4.0 5.2 2.5 4.0 25.0 Test Class 1 Pressure reduction Class 1 1.0 1.0 1.0 8.0 Example in vacuum 2.0 2.2 3.5 7.0 22 4.0 3.0 4.8 11.0 3.8 2.8 4.5 23.8

(138) TABLE-US-00011 TABLE 11 Step B4 Table ICP-MS (mass ppt) 1-2-3 Ag Al As Au Ba Ca Cd Test 0.013 0.040 0.001 0.001 0.003 0.067 0.001 Example 0.019 0.056 0.002 0.002 0.004 0.094 0.002 14 0.026 0.079 0.003 0.003 0.005 0.131 0.003 0.037 0.110 0.004 0.004 0.007 0.184 0.004 Test 0.015 0.044 0.001 0.001 0.003 0.074 0.001 Example 0.021 0.062 0.002 0.002 0.004 0.103 0.002 15 0.029 0.087 0.003 0.003 0.006 0.144 0.003 0.040 0.121 0.004 0.004 0.008 0.202 0.004 Test 0.016 0.049 0.002 0.002 0.003 0.081 0.002 Example 0.023 0.068 0.002 0.002 0.005 0.113 0.002 16 0.032 0.095 0.003 0.003 0.006 0.159 0.003 0.044 0.133 0.004 0.004 0.009 0.222 0.004 Test 0.018 0.053 0.002 0.002 0.004 0.089 0.002 Example 0.025 0.075 0.002 0.002 0.005 0.125 0.002 17 0.035 0.105 0.003 0.003 0.007 0.175 0.003 0.049 0.147 0.005 0.005 0.010 0.245 0.005 Test 0.020 0.059 0.002 0.002 0.004 0.098 0.002 Example 0.027 0.082 0.003 0.003 0.005 0.137 0.003 18 0.038 0.115 0.004 0.004 0.008 0.192 0.004 0.054 0.161 0.005 0.005 0.011 0.269 0.005 Test 0.022 0.065 0.002 0.002 0.004 0.108 0.002 Example 0.030 0.091 0.003 0.003 0.006 0.151 0.003 19 0.042 0.127 0.004 0.004 0.008 0.211 0.004 0.059 0.178 0.006 0.006 0.012 0.296 0.006 Test 0.024 0.071 0.002 0.002 0.005 0.119 0.002 Example 0.033 0.100 0.003 0.003 0.007 0.166 0.003 20 0.047 0.140 0.005 0.005 0.009 0.233 0.005 0.065 0.195 0.007 0.007 0.013 0.326 0.007 Test 0.019 0.057 0.002 0.002 0.004 0.095 0.002 Example 0.021 0.063 0.002 0.002 0.004 0.105 0.002 21 0.042 0.126 0.004 0.004 0.008 0.209 0.004 0.078 0.234 0.008 0.008 0.016 0.391 0.008 Test 0.021 0.063 0.002 0.002 0.004 0.105 0.002 Example 0.023 0.069 0.002 0.002 0.005 0.116 0.002 22 0.046 0.138 0.005 0.005 0.009 0.230 0.005 0.086 0.258 0.009 0.009 0.017 0.430 0.009

(139) TABLE-US-00012 TABLE 12 Step B4 Table ICP-MS (mass ppt) 1-2-4 Co Cr Cu Fe Ga K Li Test 0.027 0.001 0.004 0.107 0.001 0.040 0.027 Example 0.038 0.002 0.006 0.150 0.002 0.056 0.038 14 0.053 0.003 0.008 0.210 0.003 0.079 0.053 0.074 0.004 0.011 0.294 0.004 0.110 0.074 Test 0.029 0.001 0.004 0.118 0.001 0.044 0.029 Example 0.041 0.002 0.006 0.165 0.002 0.062 0.041 15 0.058 0.003 0.009 0.231 0.003 0.087 0.058 0.081 0.004 0.012 0.324 0.004 0.121 0.081 Test 0.032 0.002 0.005 0.130 0.002 0.049 0.032 Example 0.045 0.002 0.007 0.182 0.002 0.068 0.045 16 0.064 0.003 0.010 0.254 0.003 0.095 0.064 0.089 0.004 0.013 0.356 0.004 0.133 0.089 Test 0.036 0.002 0.005 0.143 0.002 0.053 0.036 Example 0.050 0.002 0.007 0.200 0.002 0.075 0.050 17 0.070 0.003 0.010 0.280 0.003 0.105 0.070 0.098 0.005 0.015 0.391 0.005 0.147 0.098 Test 0.039 0.002 0.006 0.157 0.002 0.059 0.039 Example 0.055 0.003 0.008 0.220 0.003 0.082 0.055 18 0.077 0.004 0.012 0.308 0.004 0.115 0.077 0.108 0.005 0.016 0.431 0.005 0.161 0.108 Test 0.043 0.002 0.006 0.173 0.002 0.065 0.043 Example 0.060 0.003 0.009 0.242 0.003 0.091 0.060 19 0.085 0.004 0.013 0.338 0.004 0.127 0.085 0.118 0.006 0.018 0.474 0.006 0.178 0.118 Test 0.047 0.002 0.007 0.190 0.002 0.071 0.047 Example 0.066 0.003 0.010 0.266 0.003 0.100 0.066 20 0.093 0.005 0.014 0.372 0.005 0.140 0.093 0.130 0.007 0.020 0.521 0.007 0.195 0.130 Test 0.038 0.002 0.006 0.152 0.002 0.057 0.038 Example 0.042 0.002 0.006 0.168 0.002 0.063 0.042 21 0.084 0.004 0.013 0.335 0.004 0.126 0.084 0.156 0.008 0.023 0.625 0.008 0.234 0.156 Test 0.042 0.002 0.006 0.167 0.002 0.063 0.042 Example 0.046 0.002 0.007 0.185 0.002 0.069 0.046 22 0.092 0.005 0.014 0.368 0.005 0.138 0.092 0.172 0.009 0.026 0.688 0.009 0.258 0.172

(140) TABLE-US-00013 TABLE 13 Step B4 Table ICP-MS (mass ppt) 1-2-5 Mg Mn Mo Na Nb Ni Pb Test 0.013 0.003 0.001 0.040 0.001 0.001 0.001 Example 0.019 0.004 0.002 0.056 0.002 0.002 0.002 14 0.026 0.005 0.003 0.079 0.003 0.003 0.003 0.037 0.007 0.004 0.110 0.004 0.004 0.004 Test 0.015 0.003 0.001 0.044 0.001 0.001 0.001 Example 0.021 0.004 0.002 0.062 0.002 0.002 0.002 15 0.029 0.006 0.003 0.087 0.003 0.003 0.003 0.040 0.008 0.004 0.121 0.004 0.004 0.004 Test 0.016 0.003 0.002 0.049 0.002 0.002 0.002 Example 0.023 0.005 0.002 0.068 0.002 0.002 0.002 16 0.032 0.006 0.003 0.095 0.003 0.003 0.003 0.044 0.009 0.004 0.133 0.004 0.004 0.004 Test 0.018 0.004 0.002 0.053 0.002 0.002 0.002 Example 0.025 0.005 0.002 0.075 0.002 0.002 0.002 17 0.035 0.007 0.003 0.105 0.003 0.003 0.003 0.049 0.010 0.005 0.147 0.005 0.005 0.005 Test 0.020 0.004 0.002 0.059 0.002 0.002 0.002 Example 0.027 0.005 0.003 0.082 0.003 0.003 0.003 18 0.038 0.008 0.004 0.115 0.004 0.004 0.004 0.054 0.011 0.005 0.161 0.005 0.005 0.005 Test 0.022 0.004 0.002 0.065 0.002 0.002 0.002 Example 0.030 0.006 0.003 0.091 0.003 0.003 0.003 19 0.042 0.008 0.004 0.127 0.004 0.004 0.004 0.059 0.012 0.006 0.178 0.006 0.006 0.006 Test 0.024 0.005 0.002 0.071 0.002 0.002 0.002 Example 0.033 0.007 0.003 0.100 0.003 0.003 0.003 20 0.047 0.009 0.005 0.140 0.005 0.005 0.005 0.065 0.013 0.007 0.195 0.007 0.007 0.007 Test 0.019 0.004 0.002 0.057 0.002 0.002 0.002 Example 0.021 0.004 0.002 0.063 0.002 0.002 0.002 21 0.042 0.008 0.004 0.126 0.004 0.004 0.004 0.078 0.016 0.008 0.234 0.008 0.008 0.008 Test 0.021 0.004 0.002 0.063 0.002 0.002 0.002 Example 0.023 0.005 0.002 0.069 0.002 0.002 0.002 22 0.046 0.009 0.005 0.138 0.005 0.005 0.005 0.086 0.017 0.009 0.258 0.009 0.009 0.009

(141) TABLE-US-00014 TABLE 14 Step B4 Table ICP-MS (mass ppt) 1-2-6 Sb Sn Sr Ta Th Ti Tl Test 0.001 0.001 0.012 0.001 0.001 0.054 0.001 Example 0.002 0.002 0.017 0.002 0.002 0.075 0.002 14 0.003 0.003 0.024 0.003 0.003 0.105 0.003 0.004 0.004 0.033 0.004 0.004 0.147 0.004 Test 0.001 0.001 0.013 0.001 0.001 0.059 0.001 Example 0.002 0.002 0.019 0.002 0.002 0.083 0.002 15 0.003 0.003 0.026 0.003 0.003 0.116 0.003 0.004 0.004 0.036 0.004 0.004 0.162 0.004 Test 0.002 0.002 0.015 0.002 0.002 0.065 0.002 Example 0.002 0.002 0.020 0.002 0.002 0.091 0.002 16 0.003 0.003 0.029 0.003 0.003 0.127 0.003 0.004 0.004 0.040 0.004 0.004 0.178 0.004 Test 0.002 0.002 0.016 0.002 0.002 0.071 0.002 Example 0.002 0.002 0.022 0.002 0.002 0.100 0.002 17 0.003 0.003 0.031 0.003 0.003 0.140 0.003 0.005 0.005 0.044 0.005 0.005 0.196 0.005 Test 0.002 0.002 0.018 0.002 0.002 0.078 0.002 Example 0.003 0.003 0.025 0.003 0.003 0.110 0.003 18 0.004 0.004 0.035 0.004 0.004 0.154 0.004 0.005 0.005 0.048 0.005 0.005 0.215 0.005 Test 0.002 0.002 0.019 0.002 0.002 0.086 0.002 Example 0.003 0.003 0.027 0.003 0.003 0.121 0.003 19 0.004 0.004 0.038 0.004 0.004 0.169 0.004 0.006 0.006 0.053 0.006 0.006 0.237 0.006 Test 0.002 0.002 0.021 0.002 0.002 0.095 0.002 Example 0.003 0.003 0.030 0.003 0.003 0.133 0.003 20 0.005 0.005 0.042 0.005 0.005 0.186 0.005 0.007 0.007 0.059 0.007 0.007 0.261 0.007 Test 0.002 0.002 0.017 0.002 0.002 0.076 0.002 Example 0.002 0.002 0.019 0.002 0.002 0.084 0.002 21 0.004 0.004 0.038 0.004 0.004 0.167 0.004 0.008 0.008 0.070 0.008 0.008 0.313 0.008 Test 0.002 0.002 0.019 0.002 0.002 0.084 0.002 Example 0.002 0.002 0.021 0.002 0.002 0.093 0.002 22 0.005 0.005 0.041 0.005 0.005 0.184 0.005 0.009 0.009 0.077 0.009 0.009 0.344 0.009

(142) TABLE-US-00015 TABLE 15 Step B4 Table ICP-MS (mass ppt) 1-2-7 V W Zn Zr Mo Total Test 0.001 0.001 0.008 0.001 0.001 0.476 Example 0.002 0.002 0.011 0.002 0.002 0.679 14 0.003 0.003 0.016 0.003 0.003 0.953 0.004 0.004 0.022 0.004 0.004 1.329 Test 0.001 0.001 0.009 0.001 0.001 0.521 Example 0.002 0.002 0.012 0.002 0.002 0.742 15 0.003 0.003 0.017 0.003 0.003 1.044 0.004 0.004 0.024 0.004 0.004 1.453 Test 0.002 0.002 0.010 0.002 0.002 0.591 Example 0.002 0.002 0.014 0.002 0.002 0.813 16 0.003 0.003 0.019 0.003 0.003 1.141 0.004 0.004 0.027 0.004 0.004 1.591 Test 0.002 0.002 0.011 0.002 0.002 0.646 Example 0.002 0.002 0.015 0.002 0.002 0.890 17 0.003 0.003 0.021 0.003 0.003 1.250 0.005 0.005 0.029 0.005 0.005 1.765 Test 0.002 0.002 0.012 0.002 0.002 0.708 Example 0.003 0.003 0.016 0.003 0.003 0.990 18 0.004 0.004 0.023 0.004 0.004 1.387 0.005 0.005 0.032 0.005 0.005 1.930 Test 0.002 0.002 0.013 0.002 0.002 0.774 Example 0.003 0.003 0.018 0.003 0.003 1.087 19 0.004 0.004 0.025 0.004 0.004 1.517 0.006 0.006 0.036 0.006 0.006 2.134 Test 0.002 0.002 0.014 0.002 0.002 0.847 Example 0.003 0.003 0.020 0.003 0.003 1.191 20 0.005 0.005 0.028 0.005 0.005 1.683 0.007 0.007 0.039 0.007 0.007 2.353 Test 0.002 0.002 0.011 0.002 0.002 0.686 Example 0.002 0.002 0.013 0.002 0.002 0.754 21 0.004 0.004 0.025 0.004 0.004 1.505 0.008 0.008 0.047 0.008 0.008 2.815 Test 0.002 0.002 0.013 0.002 0.002 0.753 Example 0.002 0.002 0.014 0.002 0.002 0.827 22 0.005 0.005 0.028 0.005 0.005 1.663 0.009 0.009 0.052 0.009 0.009 3.103

(143) TABLE-US-00016 TABLE 16 Evaluation Coefficient of correlation ICP- GC/ MS LC/MS MS DI-MS NMR and and and and and num- Total Num- total total total total ber num- ber of number number number number of Table ber of metal of of of of metal 1-2-8 defects defects defects defects defects defects defects Test 430.5 6 1.000 0.963 0.947 0.952 0.982 Example 875 16 14 1295 23 1722 31 Test 258.3 4 1.000 0.933 0.872 0.828 0.985 Example 525 9 15 777 14 1033.2 19 Test 246 3 0.970 0.936 0.914 0.838 0.974 Example 500 9 16 740 13 984 18 Test 246 3 0.982 0.980 0.935 0.892 0.972 Example 500 9 17 740 13 984 18 Test 246 3 0.969 0.975 0.972 0.895 0.976 Example 500 9 18 740 13 984 18 Test 246 3 0.990 0.986 0.905 0.941 0.975 Example 500 9 19 740 13 984 18 Test 246 3 0.989 0.983 0.968 0.959 0.976 Example 500 9 20 740 13 984 18 Test 246 3 0.890 0.894 0.776 0.767 0.901 Example 500 9 21 740 13 984 18 Test 246 3 0.928 0.899 0.885 0.851 0.902 Example 500 9 22 740 13 984 18

Example 1

(144) By performing linear regression on the content of the specific component in the concentrated liquid of each of the chemical liquids 1-1 to 1-4 obtained in Test Example 1 and the number of defects of each of the chemical liquids, a calibration curve was created. Then, based on the calibration curve, “400/12 inchWf” was determined as the total number of defects for determining whether a chemical liquid is adequate or inadequate (in other words, the desired defect inhibition performance was set to be “400/12 inchWf”), and the content of the specific component measured by each of LC/MS and GC/MS corresponding thereto was calculated from the calibration curve and determined as a standard value.

(145) Then, by the same method as that used for manufacturing the chemical liquids 1-1 and 1-4, chemical liquids 1-1(2) and 1-4(2) were manufactured on a day different from the day on which the chemical liquids 1-1 and 1-4 were manufactured.

(146) Subsequently, by using the chemical liquids 1-1(2) and 1-4(2), concentrated liquids were prepared by the same method as in Test Example 1, and the content of the specific component was measured by the same method as in Test Example 1.

(147) The obtained measurement results were compared with the standard value determined as described above. As a result, the content of the specific component in the chemical liquid 1-1(2) was equal to or smaller than the standard value. Therefore, the chemical liquid 1-1(2) was determined as being adequate. In contrast, the content of the specific component in the chemical liquid 1-4(2) was greater than the standard value. Therefore, the chemical liquid 1-4(2) was determined as being inadequate.

(148) Subsequently, the defect inhibition performance of the chemical liquids 1-1(2) and 1-4(2) was evaluated by the same method as in Test Example 1. As a result, the total number of defects of the chemical liquid 1-1(2) was 121/12 inchWf, and the total number of defects of the chemical liquid 1-4(2) was 490/12 inchWf.

(149) From the above results, it was understood that by the present quality inspection method for a chemical liquid, the defect inhibition performance of a chemical liquid can be simply evaluated.

Example 2

(150) By performing linear regression on the content of the specific component in each of the concentrated liquids of the chemical liquids 2-1 to 2-4 obtained in Test Example 2 and the number of defects of each of the chemical liquids, a calibration curve was created. Then, based on the calibration curve, the content of the specific component (relative quantity) which corresponded to the total number of defects of 400/12 inchWf and was measured by each of LC/MS and GC/MS was determined as a standard value.

(151) Thereafter, by the same method as that used for manufacturing the chemical liquids 2-1 and 2-4, chemical liquids 2-1(2) and 2-4(2) were manufactured on a day different from the day on which the chemical liquids 2-1 and 2-4 were manufactured.

(152) Subsequently, by using the chemical liquids 2-1(2) and 2-4(2), concentrated liquids were prepared by the same method as in Test Example 2, and the content of the specific component was measured by the same method as in Test Example 2.

(153) The obtained measurement results were compared with the standard value determined as described above. As a result, the content of the specific component in the chemical liquid 2-1(2) was equal to or smaller than the standard value. Therefore, the chemical liquid 2-1(2) was determined as being adequate. In contrast, the content of the specific component in the chemical liquid 2-4(2) was greater than the standard value. Therefore, the chemical liquid 2-4(2) was determined as being inadequate.

(154) Then, the defect inhibition performance of the chemical liquids 2-1(2) and 2-4(2) was evaluated by the same method as in Test Example 1. As a result, the total number of defects of the chemical liquid 2-1(2) was 122/12 inchWf, and the total number of defects of the chemical liquid 2-4(2) was 491/12 inchWf.

Examples 3 to 22

(155) A chemical liquid denoted by (first number)-1 and a chemical liquid denoted by (first number)-4 corresponding to a test example denoted by (first number) were manufactured in the same manner as described above on another day. Then, the chemical liquids were concentrated by a method corresponding to each test example denoted by (first number), the content of the specific component was analyzed and compared with the predetermined standard value, and whether the chemical liquid was adequate or inadequate was determined. For each of the chemical liquids, the defect inhibition performance was evaluated. As a result, the predicted defect inhibition performance calculated from the calibration curve based on the content of the specific component substantially coincided with the actually measured defect inhibition performance. Therefore, it was understood that by the above method, the defect inhibition performance of a chemical liquid can be simply evaluated.

Comparative Example 1

(156) By performing linear regression on the content of the specific component in the concentrated liquids of the chemical liquids 1-1 to 1-4 obtained in Test Example 1 and the number of defects of each of the chemical liquids, a calibration curve was created. Then, based on the calibration curve, the content of the specific component which corresponded to the total number of defects of 400/12 inchWf and was measured by each of LC/MS and GC/MS was determined as a standard value.

(157) Then, by the same method as that used for manufacturing the chemical liquids 1-1 and 1-4, chemical liquids 1-1(2) and 1-4(2) were manufactured on a day different from the day on which the chemical liquids 1-1 and 1-4 were manufactured.

(158) Thereafter, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was measured by the same method as in Example 1, except that each of the chemical liquids was concentrated not in a clean room but in the atmosphere.

(159) The obtained measurement results were compared with the standard value determined as above. As a result, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was greater than the standard value. Therefore, both the chemical liquids were determined as being inadequate.

(160) Subsequently, the defect inhibition performance of the chemical liquids 1-1(2) and 1-4(2) was evaluated by the same method as in Test Example 1. As a result, the total number of defects of the chemical liquid 1-1(2) was 121/12 inchWf, and the total number of defects of the chemical liquid 1-4(2) was 490/12 inchWf.

(161) From the above results, it was understood that unless the chemical liquid is concentrated in a predetermined clean room, the defect inhibition performance of the chemical liquid cannot be accurately evaluated.

Comparative Example 2

(162) By performing linear regression on the content of the specific component in the concentrated liquids of the chemical liquids 1-1 to 1-4 obtained in Test Example 1 and the number of defects of each of the chemical liquids, a calibration curve was created. Then, based on the calibration curve, the content of the specific component which corresponded to the total number of defects of 400/12 inchWf and was measured by each of LC/MS and GC/MS was determined as a standard value.

(163) Then, by the same method as that used for manufacturing the chemical liquids 1-1 and 1-4, chemical liquids 1-1(2) and 1-4(2) were manufactured on a day different from the day on which the chemical liquids 1-1 and 1-4 were manufactured.

(164) Thereafter, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was measured by the same method as in Example 1, except that the first container was used without being washed.

(165) The obtained measurement results were compared with the standard value determined as above. As a result, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was greater than the standard value. Therefore, both the chemical liquids were determined as being inadequate.

(166) Subsequently, the defect inhibition performance of the chemical liquids 1-1(2) and 1-4(2) was evaluated by the same method as in Test Example 1. As a result, the total number of defects of the chemical liquid 1-1(2) was 121/12 inchWf, and the total number of defects of the chemical liquid 1-4(2) was 490/12 inchWf.

(167) From the above results, it was understood that unless the first container is washed by a predetermined method, the defect inhibition performance cannot be accurately evaluated.

Comparative Example 3

(168) By performing linear regression on the content of the specific component in the concentrated liquids of the chemical liquids 1-1 to 1-4 obtained in Test Example 1 and the number of defects of each of the chemical liquids, a calibration curve was created. Then, based on the calibration curve, the content of the specific component which corresponded to the total number of defects of 400/12 inchWf and was measured by each of LC/MS and GC/MS was determined as a standard value.

(169) Then, by the same method as that used for manufacturing the chemical liquids 1-1 and 1-4, chemical liquids 1-1(2) and 1-4(2) were manufactured on a day different from the day on which the chemical liquids 1-1 and 1-4 were manufactured.

(170) Thereafter, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was measured by the same method as in Example 1, except that the chemical liquid was concentrated in the air by means of heating concentration.

(171) Subsequently, the obtained measurement results were compared with the standard value determined as above. As a result, the content of the specific component in the chemical liquids 1-1(2) and 1-4(2) was greater than the standard value. Therefore, both the chemical liquids were determined as being inadequate.

(172) Then, the defect inhibition performance of the chemical liquids 1-1(2) and 1-4(2) was evaluated by the same method as in Test Example 1. As a result, the total number of defects of the chemical liquid 1-1(2) was 121/12 inchWf, and the total number of defects of the chemical liquid 1-4(2) was 490/12 inchWf.

(173) From the above results, it was understood that unless the chemical liquid is concentrated under predetermined conditions, the defect inhibition performance cannot be accurately evaluated.