Classifications

• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D11/00—Solvent extraction
  • B01D11/04—Solvent extraction of solutions which are liquid
  • B01D11/0492—Applications, solvents used
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F9/00—Multistage treatment of water, waste water or sewage
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/26—Treatment of water, waste water, or sewage by extraction
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/28—Treatment of water, waste water, or sewage by sorption
  • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/28—Treatment of water, waste water, or sewage by sorption
  • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F2101/00—Nature of the contaminant
  • C02F2101/10—Inorganic compounds
  • C02F2101/12—Halogens or halogen-containing compounds
  • C02F2101/14—Fluorine or fluorine-containing compounds
• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
  • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
  • C02F2103/346—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from semiconductor processing, e.g. waste water from polishing of wafers

Definitions

• the present invention relates to a purification process of a mixed solution containing a fluorine -based solvent such as hydrofluorocarbon ether (HFE).
• a fluorine -based solvent such as hydrofluorocarbon ether (HFE).
• Fluorine -based solvents are used to clean workpieces such as electronic components or semiconductor wafers.
• workpieces such as electronic components or semiconductor wafers.
• the in-line purification typically consists of using a distillation regenerator, a particle removing filter or the like.
• Kokai Japanese Unexamined Patent Publication
• Kokai No. 2001-129302 each describes a distillation regenerator for a fluorine-based solvent.
• the particle number in the solution is difficult to reduce to a desired or necessary level by a particle removing filter in a typical cleaning apparatus.
• fluorine -based solvent such as hydrofluorocarbon ether (HFE)
• HFE hydrofluorocarbon ether
• An objective of the present invention is to provide a purification process where a fluorine-based solvent such as hydrofluorocarbon ether (HFE) can be obtained at a high purity by using relatively small equipment and without using a distillation apparatus.
• HFE hydrofluorocarbon ether
• a purification process of a mixed solution containing a fluorine-based solvent which is a process for purifying a fluorine-based solvent from a mixed solution containing a fluorine-based solvent such as hydrofluorocarbon ether (HFE) and/or hydrofluorocarbon (HFC), a water-soluble organic solvent contaminant, an organic contaminant and an ion contaminant, the process comprising: step (1): washing the mixed solution with water to obtain a first treated solution in which the water-soluble organic solvent contaminant concentration is reduced to 0.01 weight % (wt%) or less, step (2): treating the first treated solution with activated carbon to obtain a second treated solution in which the organic contaminant concentration is reduced to 20 parts per billion (ppb) or less, step (3): treating the second treated solution with activated alumina to obtain a third treated solution in which the fluoride ion contaminant being reduced to 10 ppb or less, and step (4): treating the third treated solution with a particle removing filter to obtain
• a purification process of a mixed solution containing a fluorine-based solvent which is a process for purifying a fluorine-based solvent from a mixed solution containing a fluorine-based solvent such as hydrofluorocarbon ether (HFE) and/or hydrofluorocarbon (HFC), a water-soluble organic solvent contaminant, an organic contaminant and an ion contaminant, the process comprising: step (1): washing the mixed solution with water to obtain a first treated solution in which the water-soluble organic solvent contaminant concentration is reduced to 0.01 wt% or less, step (2): treating the first treated solution with activated alumina to obtain a second treated solution in which the fluoride ion contaminant is reduced to 10 ppb or less, step (3): treating the second treated solution with activated carbon to obtain a third treated solution in which the organic contaminant concentration is reduced to 20 ppb or less, and step (4): treating the third treated solution with a particle removing filter to obtain a fluorine-based
• a purification apparatus which is a solution purifying apparatus used for the purification process described in any one of (i) to (vii) above, the apparatus comprising a water-soluble organic solvent removing device for performing the step (1), an activated carbon filter for performing the step (2), an activated alumina filter for performing the step (3), and a particle removing filter for performing the step (4).
• a cleaning apparatus for precision cleaning of electric/electronic components or a cleaning apparatus for cleaning a semiconductor wafer comprising the purification apparatus described in (viii) above together with a cleaning apparatus for cleaning an electric/electronic component or a semiconductor wafer.
• the above-described steps are combined, whereby a high- purity fluorine-based solvent such as hydrofluorocarbon ether can be obtained using small equipment within a short time. Also, regeneration by distillation is not used and therefore, an ion contaminant is not produced during the regeneration process.
• a fluorine-based solvent applicable to this usage can be obtained.
• High-purity fluorine-based solvent in this specification means that the solvent meets the following criteria: the water-soluble organic solvent contamination concentration is 10 ppb or less, the organic contamination concentration in a fluorine-based solvent is 20 ppb or less, the number of particles having a size of 0.1 ⁇ m or more in a fluorine-based solvent is 10 particles/mL or less.
• Fig. 1 A schematic view of a purification apparatus usable in the present invention.
• Fig. 1 shows a schematic view of a purification apparatus usable in the present invention.
• the purification apparatus 100 comprises, as main constituent devices, a water- soluble organic solvent removing device 1, an activated carbon filter 2, an activated alumina filter 3 and a particle removing filter (particulate filter) 4.
• the activated carbon filter 2 and the activated alumina filter 3 may be in separate columns but, as shown in Fig. 1 , these filters may be combined in the same column. Additionally, the activated carbon filter and the activated alumina filter order may be switched (i.e. the activated alumina filter may be before the activated carbon filter) in keeping with the spirit of this invention.
• the purification apparatus 100 may comprise, if desired, an auxiliary device such as a mixed solution (used cleaning solution) feed tank 11, a feed pump 12, a circulation pump 13, a circulation line 14 and a solution delivery pump 15.
• the water-soluble organic solvent removing device 1 comprises a water washing tank 5 and a water eliminator 6.
• a used cleaning solution (U) in the mixed solution (used cleaning solution) feed tank 11 is introduced into the water washing tank 5 by the feed pump 12.
• the water washing tank 5 is previously filled with a certain amount of water.
• the used cleaning solution (U) introduced into the water washing tank 5 is introduced into the water as mist or relatively small liquid droplets by a dispersion means such as a sprayer 7.
• a dispersion means such as a sprayer 7.
• the water-soluble organic solvent contaminants contained in the used cleaning solution (U) dissolves in the water and the fluorine-based solvent (HFE) is separated as a separate phase from the water. More specifically, in this water washing step, the fluorine-based solvent and the water-soluble organic solvent contaminants are separated based on the difference between the low solubility of the fluorine -based solvent in water and the high solubility of the water-soluble organic solvent contaminants in water. Accordingly, the fluorine-based solvent to be purified is preferably water-insoluble. Even if the fluorine -based solvent is water-soluble, it can be purified by the process of this invention.
• the fluorine-based solvent must be incompatible with water and less soluble in water than the water- soluble organic solvent contaminents. Only a portion of the fluorine-based solvent that is not dissolved in the water can be purified. The fluorine-based solvent dissolved in the water is not recovered because of the difficulty in extracting dissolved fluorine-based solvent from the water by the process of the invention. Therefore, the larger difference in solubility of the fluorine-based solvent in water and water-soluble organic solvent in water, the easier to extract the water soluble organic contaminants from the fluorine-based solvent.
• the water-soluble organic solvent contaminants include: water- soluble alcohols such as methanol, ethanol and isopropanol, and short carbon number ketones such as acetone.
• the separated fluorine-based solvent preferably contains only a trace (0.01 wt% or less) amount of the water-soluble organic solvent contaminant and a trace (1 ppm or less, preferably 30ppb or less) amount of ionic component.
• the separated fluorine -based solvent is usually accompanied by a small amount of free water. Therefore, the fluorine-based solvent is further treated by a water eliminator 6 and separated into a fluroine-based solvent containing solution (HFE Liq. 1) and a water- soluble organic solvent contaminant-containing waste water (WW).
• HFE Liq. 1 fluroine-based solvent containing solution
• WW water-soluble organic solvent contaminant-containing waste water
• an oil-water separator such as the Eutec filter produced by
• Asahi Kasei can be used.
• the concentration of water- soluble organic solvent contaminant in the fluorine -based solvent containing solution (HFE Liq. 1) is 0.01 wt% or less and the water content is not more than the saturated water content
• the HFE Liq. 1 is delivered to the activated carbon filter 2.
• fluid pressure necessary for the water eliminator 6 or activated carbon filter 2 and subsequent steps may be obtained by the circulation pump 13 and/or the solution delivery pump 15. If the concentration of water-soluble organic solvent contaminant in the HFE Liq. 1 is 0.01 wt% or more, the HFE Liq.
• the water-soluble organic solvent contaminant concentration can be easily reduced to the concentration specified above even by using a smaller water washing tank 5.
• a similar effect can be obtained by connecting two or more water-soluble organic solvent removing devices 1 in series instead of circulating the HFE Liq. 1 solution.
• the size of one water washing tank 5 is preferably 6 liters or more, that is, a residence time of 3 minutes or more, per feed of 1 liter/min.
• the water-soluble organic solvent contaminant concentration in the HFE Liq. 1 can be measured by gas chromatography (GC).
• a fluorine-based solvent containing solution (HFE Liq. 1) in which the concentration of the water-soluble organic solvent contaminant is reduced to a concentration of about 0.01 wt% or less is obtained as a first treated solution.
• This first treated solution is delivered to the activated carbon filter 2.
• the activated carbon filter 2 removes the organic contaminant. Since the water-soluble organic solvent contaminant is mostly removed by the water washing in the water-soluble organic solvent removing device 1 before passing through the activated carbon filter 2, the load for the activated carbon filter 2 is reduced.
• the organic contaminant include: hydrocarbons, esters, and silicones.
• the kind of the activated carbon in the activated carbon filter 2 can be appropriately selected according to the accompanying organic contaminant component.
• a granular activated carbon having a particle size of 1 to 2 mm is used in Examples, but a powder activated carbon or a fibrous activated carbon may also be used.
• a powder activated carbon has a possibility of dusting and needs to be used carefully.
• useful commercially available activated carbon include Kuraray Coal, activated carbon for liquid phase, produced by Kuraray Chemical Co., Ltd. (Osaka, Japan); Shirosagi produced by Japan EnviroChemicals, Ltd. (Osaka, Japan); and Calgon and Diahope produced by Calgon Mitsubishi Chemical Corp (Tokyo, Japan).
• the activated carbon may be packed in an appropriate column such as cylindrical column for use.
• the size of the activated carbon filter 2 is appropriately determined according to the treating rate and the concentration of organic contaminant in the fluorine-based solvent containing solution (HFE Liq. 1).
• the organic contaminant concentration can be reduced to 10 ppb or less by an activated carbon filter of 10 liters, that is, a residence time of 10 minutes per feed at 1 liter/min.
• the organic contaminant concentration can be measured by a Fourier transformation infrared spectrometer (FT-IR).
• the fluorine -based solvent containing solution (HFE Liq. 1) solution passed through the activated carbon filter 2 is obtained as a second treated solution, and the second treated solution is delivered to the activated alumina filter 3. Since most of the ionic components in the fluorine-based solvent are removed by water washing, the load on the activated alumina is lowered.
• the activated alumina filter 3 removes the ion contaminant in the fluorine-based solvent containing solution.
• the size of the activated alumina is not particularly limited, but a granular alumina having a particle diameter of 1 to 2 mm or more is easy to use. A powdered alumina has a possibility of dusting and needs to be used carefully.
• KH Series produced by Sumitomo Chemical Co. Ltd.(Tokyo, Japan), and activated alumina produced by Showa Denko K.K. (Tokyo, Japan) can be used.
• the size of the activated alumina filter 3 is appropriately determined according to the treating rate and the concentration of ion contaminant in the fluorine-based solvent.
• the ion contaminant concentration can be reduced to about 1 ppb or less by an activated alumina filter of 5 liters, that is, a residence time of 5 minutes per feed at 1 liter/min.
• the fluoride ion concentration can be measured by using an ion meter or a fluoride ion electrode.
• the fluorine -based solvent containing solution passed through the activated alumina filter 3 is obtained as a third treated solution, and the third treated solution is delivered to the particle removing filter 4.
• the fluorine- based solvent containing solution is treated until the number of particles of about 0.1 ⁇ m or more are reduced to 10 particles/mL or less, whereby a regenerated cleaning solution (R) can be finally obtained.
• the particle removing filter 4 may be a filter using a polymer membrane as the filter element and, for example, a polytetrafluoroethylene (PTFE) membrane and a tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA) housing filter such as the UltiKleen filter (for 0.05 to 0.2 ⁇ m) produced by Pall Corp. (East Hills, NY, USA).
• PTFE polytetrafluoroethylene
• PFA tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer
• Other filters may be used if the filter is capable of removing particles of appropriate size.
• contamination may be generated from the filter depending on the kind of the polymer or vendor.
• a filter comprising polytetrafluoroethylene (PTFE) and a tetafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA) is preferably used.
• the size of the particle removing filter 4 is generally about 4 inches (101.6 mm), 10 inches (254 mm), 20 inches (508 mm) or 30 inches (762 mm) in length, but may be appropriately selected according to the desired flow rate.
• a disposable-type filter may also be used.
• the number of particles in the solution can be measured by an in-liquid particle counter.
• molecular sieve and ion exchange resin produced by Union Showa K.K. (Tokyo, Japan) are also effective.
• the molecular sieve and ion exchange resins are preferably selected and used depending on the required characteristics.
• the above-described activated carbon filter or activated alumina filter also has an ability of removing water, but in order to reduce the load, an additional water eliminator 6 is preferably used.
• a stainless steel (SUS), a polytetrafluoroethylene (PTFE) or a tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA) is preferably used.
• a construction material which is not a fluorine-based resin may be used as long as substantial elution of a plasticizer does not occur (for example, Ethylene Propylene Diene Monomer (EPDM) not using a plasticizer, and Arcury produced by Nippon Valqua Industries, Ltd.) (Tokyo, Japan).
• EPDM Ethylene Propylene Diene Monomer
• Step (1) a water-soluble organic solvent contaminant removing step using a water-soluble organic solvent removing device 1 (step (I)), an organic contaminant removing step using an activated carbon filter 2 (step (2)), an ion contaminant removing step using an activated alumina filter 3 (step (3)), and a particle removing step using a particle removing filter (particulate filter) 4 (step (4)).
• Step (1) should be performed in advance of steps (2) and (3) to increase the lifetime of the activated carbon or activated alumina columns.
• step (4) should be performed after steps (2) and (3), to remove any potential particulates that may be introduced during steps (2) and (3).
• the purification process of the present invention may be performed either in a separate stand-alone purification apparatus or in an in-line purification apparatus integrated with a cleaning apparatus. Incorporation as a part of the cleaning apparatus is preferred because the purification apparatus can be downsized.
• the cleaning solution regenerated by the process of the present invention capable of satisfactorily removing these contaminants can be advantageously used in such cleaning.
• an in-line arrangement of the cleaning solution regeneration process in a cleaning apparatus can be achieved by combining the apparatus for practicing the present invention with the cleaning apparatus, so that a high- purity fluorine-based solvent can be always provided to the cleaning apparatus.
• the fluorine -based solvent used in this invention includes a segregated hydrofluorocarbon ether (HFE), a non-segregated HFE, a hydrofluoropolyether, a hydrofluorocarbon or a hydrochlorofluorocarbon.
• HFE hydrofluorocarbon ether
• hydrofluoropolyether a hydrofluoropolyether
• hydrofluorocarbon a hydrofluorocarbon or a hydrochlorofluorocarbon.
• segments of HFE such as alkyl or alkylene segment linked via ether oxygen are either perfluorinated (for example, perfluorocarbon) or not fluorinated (for example, hydrocarbon), and thus they are not partially fluorinated.
• a non-segregated HFE at least one of segments linked via ether oxygen is not perfluorinated, not non-fluorinated, but partially fluorinated (i.e., containing a mixture of fluorine atoms and hydrogen atoms).
• the fluorine-based solvent used in the purification process of this invention includes 3M ⁇ Novec> 7100 containing 0.1 to 10 wt% of isopropanol. Further, the fluorine-based solvent used in the purification process of this invention may include methanol, ethanol, propanol or isopropanol in addition to a fluorine-based solvent.
• a fluorine-based solvent useful in the present invention includes the following solvents. Segregated HFE
• Water washing tank 5 a drum volume of 60 liters
• Water separator 6 Eutec Filter TH Series produced by Asahi Kasei
• Activated carbon filter 2 a stainless steel (SUS)-made cylindrical column having packed therein 2,600 cm 3 of WH2C (activated carbon having a particle size of 8 to 32 mesh and a specific surface area of 1,200 m 2 /g) produced by Takeda Chemical
• Activated alumina filter 3 a stainless steel (SUS)-made cylindrical column having packed therein 1,300 cm of KHO-12 (alumina having a particle diameter of 1 to 2 mm and a specific surface area of 140 to 190 m 2 /g) produced by Sumitomo Chemical Co., Ltd. (Tokyo, Japan)
• Particle removing filter 4 UltiKleen filters (for 0.05 ⁇ m and for 0.1 ⁇ m) produced by Pall Corp (East Hills, NY, USA). Emflon and IonKleen-SL (both from Pall Corp.) are also used in Example 4.
• the alcohol concentration in the fluorine-based solvent was measured by using Gas Chromatograph HP6890 manufactured by Hewlett Packard. Incidentally, in order to convert the concentration obtained by the gas chromatograph into a weight concentration, a calibration curve was prepared using a mixed solution of fluorine-based solvent and alcohol. The alcohol was the same as that added in the solution to be purified. In the Examples, only data on the alcohol concentration in the fluorine-based solvent are shown, but in practice, the alcohol concentration in the separated water phase was also measured in the same manner.
• the sample was put in a clean plastic bottle made of high-density polyethylene (HDPE) and after adding ultrapure water (purified by Milli-Q Ultrapure Water Purification System from Millipore Japan (Tokyo, Japan)) of the same weight, the plastic bottle was shaken using a shaker for 2 hours, thereby extracting the ions in the fluorine-based solvent to the aqueous layer. Subsequently, the aqueous layer (upper layer) was injected into an Ion Chromatograph DX320 manufactured by Dionex (Sunnyvale, CA) to determine the amount of ion in the solution.
• HDPE high-density polyethylene
• ion concentration of ultrapure water is subtracted from the ion concentration of the sample.
• Detection limit of ion chromatography is about 0.01 ppb.
• the solution was transferred to a clean vessel and the particle number in the solution was measured using an in-liquid particle counter KS-40A manufactured by Rion Co., Ltd (Tokyo, Japan). The measured particle number was converted into the particle number per mL.
• the water volume in the sample was measured using a Karl-Fischer type water meter CA-21 manufactured by Mitsubishi Chemical Corp (Tokyo, Japan).
• Hydro fluorocarbon ether obtained under the trade name "3M NovecTM HFE-7100 " from Sumitomo 3M, (Tokyojapan)
• Hydrofluorocarbon ether obtained under the trade name "AE-3000” from Asahi Glass Company, Ltd. : HFE-347pc-f (CHF 2 CF 2 OCH 2 CF 3 )
• IPA isopropyl alcohol (purity 99.5% or more) from Wako Pure Chemical Industries, Ltd.
• EtOH ethanol (purity 99.5% or more) from Wako Pure Chemical Industries, Ltd [0035] Tests for confirming the performance of each device were performed.
• a simulated contaminated fluorine -based cleaning solution was made using 3M NovecTM 7100 and various concentrations of IPA.
• This simulated contaminated cleaning solution was treated using a water-soluble organic solvent removing device comprising a water washing tank and water eliminator to remove the IPA.
• the IPA concentration after treatment is shown in Table 1 below.
• the IPA concentration after treatment was measured using a gas chromatograph as described in "Measuring Method of Alcohol Concentration" above. Table 1
• N.D. means IPA was not detected (detection limit: 0.001 wt%)
• Another simulated contaminated fluorine-based cleaning solution was made 3M NovecTM 7100 and 5 wt% IPA. This simulated contaminated fluorine-based cleaning solution was passed through the water washing tank and water eliminator to remove IPA.
• N. D. means that IPA was not detected
• Example 2 (organic contaminant removing step using activated carbon filter) Test 1 :
• N.D. means that ester was not detected.
• Example 3 (ion contaminant removing step using activated alumina filter)
• N.D. means that the anion was not detected (detection limit of 0.01 ppb).
• a solution of HFE was passed through various particle filters and the organic contaminants were analyzed using a Fourier transformation infrared spectrometer (FT-IR) by the "Measuring Method of Organic Contaminant". Each filter was washed with 3M NovecTM 7100 before filtering the sample for organic contaminant analysis.
• FT-IR Fourier transformation infrared spectrometer
• Table 8 The HFE solution not passed through any filter was also tested and the amount of increase in organic contaminant due to the particle filters is reported in Table 8 below. Two trials were performed on each filter. Also shown is Table 8 are the materials for each filter type.
• Contaminant concentration of 3M NovecTM 7100 before treatment (not passed through filter) : 0.15 ⁇ g/lg-HFE of HC as Squalane, 0.07 ⁇ g/lg-HFE of Ester as DOP and no Silicone detected.
• HFE solutions derived from 3 lots of 3 M NovecTM 7100 solution treated as described above was also measured by the "Measuring Method of Organic Contaminant". The results are shown in Table 10 below.
• N.D. means that silicone was not detected.
• Example 5 It is seen from comparing the results in Table 10 and not filtered HFE contaminant level in test 1 of Example 4 that the particles can be removed without incurring organic contamination by an organic residue from the filter.
• a stimulate contaminated HFE cleaning solution containing about 5 wt% of isopropyl alcohol (IPA) was regenerated using the Device described above at the beginning of this Example section.
• the HFE used was NovecTM 7100 produced by 3M.
• the IPA concentration was measured on each treated solvents by the "Measuring Method of Alcohol Concentration". On these same samples, the fluoride ion contaminant, water content volume and pH were also measured by the methods described above. The results are shown in Table 11 below.
• N.D. means Not Detected
• the test was performed on the HFE-347-pcf (CHF 2 CF 2 OCH 2 CF 3 ) containing 10 wt% of ethanol.
• the solution containing fluorine-based solvent and ethanol was washed 5 minutes followed by another 5 minutes wash. Before the 2 nd 5 minute wash, the water in the water washing tank was replaced with the clean water. A part of the solution was taken from the tank at the time shown in the table 13 for analysis.
• N.D. means not detected.
• N.D. means that silicone was not detected.
• 0 anion or cation concentration means that the ion concentration of test sample was the same or fewer than that of ultra-pure water used for measurement.

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