JP3198945B2 - High-purity water production equipment - Google Patents
High-purity water production equipmentInfo
- Publication number
- JP3198945B2 JP3198945B2 JP25866496A JP25866496A JP3198945B2 JP 3198945 B2 JP3198945 B2 JP 3198945B2 JP 25866496 A JP25866496 A JP 25866496A JP 25866496 A JP25866496 A JP 25866496A JP 3198945 B2 JP3198945 B2 JP 3198945B2
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- Prior art keywords
- water
- steam
- purity
- heating
- toc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Physical Water Treatments (AREA)
Description
【0001】[0001]
【発明の属する技術分野】本発明は高純度水製造装置に
係り、特に、有機物を実質的に含有しない高純度水を製
造するための装置に関する。The present invention relates to an apparatus for producing high-purity water, and more particularly, to an apparatus for producing high-purity water containing substantially no organic matter.
【0002】[0002]
【従来の技術】近年、半導体製造分野、生化学分野或い
は医薬分野で使用される超純水の純度向上が重要な課題
となっている。2. Description of the Related Art In recent years, it has become an important issue to improve the purity of ultrapure water used in the field of semiconductor manufacturing, biochemistry or medicine.
【0003】超純水の製造に際しては、製造された超純
水の有機物濃度を測定して、これを管理する必要があ
る。この有機物濃度の測定には、一般に、有機物濃度を
有機物中の炭素量で求めるTOC(全有機炭素)計が用
いられ、このTOC計についても、より高感度であるこ
とが求められている。[0003] When producing ultrapure water, it is necessary to measure the concentration of organic substances in the produced ultrapure water and to control this. In measuring the organic substance concentration, a TOC (total organic carbon) meter for measuring the organic substance concentration by the amount of carbon in the organic substance is generally used, and the TOC meter is also required to have higher sensitivity.
【0004】ところで、TOC計による超純水のTOC
濃度の測定に当っては、零校正液と称される有機物を実
質的に含まない水と有機物濃度既知の水とを用いて、T
OC計の校正を行う必要がある。Incidentally, TOC of ultrapure water by TOC meter
In the measurement of the concentration, water containing substantially no organic substance called a zero calibration solution and water having a known organic substance concentration are used to measure T
It is necessary to calibrate the OC meter.
【0005】従来、TOC計の校正に使用される零校正
液の製造装置として、蒸留法と高温燃焼法とを組み合せ
たもの、即ち、水蒸気を酸素と共に高温の触媒層中に通
過させることで、水蒸気中の有機物を燃焼させて除去す
る装置が提案されている(特開昭63−287590号
公報)。Conventionally, as an apparatus for producing a zero-calibration liquid used for calibration of a TOC meter, a combination of a distillation method and a high-temperature combustion method, that is, by passing steam together with oxygen through a high-temperature catalyst layer, An apparatus for burning and removing organic substances in water vapor has been proposed (JP-A-63-287590).
【0006】[0006]
【発明が解決しようとする課題】特開昭63−2875
90号公報記載の装置であれば、有機物濃度をTOC2
ppb程度にまで低減することができるが、零校正液と
しての使用目的のためには、より一層のTOCの低減が
必要とされる。特に、TOC計にて1ppb以下のTO
Cを精度良く測定するためには、零校正液としては、少
なくともTOC1ppb以下、好ましくはTOC0.3
ppb以下のものが必要となる。SUMMARY OF THE INVENTION Japanese Patent Application Laid-Open No. 63-2875
No. 90, the organic matter concentration is set to TOC2.
Although it can be reduced to about ppb, further reduction of TOC is required for the purpose of use as a zero calibration solution. In particular, TOC of 1 ppb or less
In order to measure C with high accuracy, the zero calibration solution should be at least TOC 1 ppb or less, preferably TOC 0.3 ppb.
What is less than ppb is required.
【0007】しかしながら、従来の蒸留法と高温燃焼法
とを併用した装置では、有機物の燃焼用の酸素ガス又は
過酸化剤に含まれる不純物の混入や、酸化触媒層を通過
することによる汚染が避けられず、このため、有機物を
極低濃度にまで低減することができなかった。[0007] However, the conventional apparatus using both the distillation method and the high-temperature combustion method avoids contamination of impurities contained in oxygen gas for combustion of organic substances or a peroxide, and contamination caused by passing through the oxidation catalyst layer. Therefore, the organic matter could not be reduced to an extremely low concentration.
【0008】本発明は上記従来の問題点を解決し、TO
C1ppb以下の測定に使用する、TOC0.3ppb
程度以下の、実質的に有機物を含有しない高純度水を製
造することができる高純度水製造装置を提供することを
目的とする。[0008] The present invention solves the above conventional problems and provides a TO
TOC 0.3ppb used for measurement below C1ppb
It is an object of the present invention to provide a high-purity water production apparatus capable of producing high-purity water containing substantially no organic matter and having a purity of about or less.
【0009】[0009]
【課題を解決するための手段】本発明の高純度水製造装
置は、TOC濃度が2〜3ppbの純水からなる原料水
を加熱して水蒸気を発生させる水蒸気発生手段と、該水
蒸気発生手段で発生した水蒸気を、酸素の非供給下であ
って、かつ触媒層不存在の条件下に、加熱して該水蒸気
中の微量有機物を熱分解する水蒸気加熱手段と、該水蒸
気加熱手段からの水蒸気を冷却して凝縮水を得る冷却凝
縮手段と、得られた凝縮水が導入される処理水貯留容器
とを備え、TOC濃度0.3ppb以下の高純度水を製
造することを特徴とする。A high-purity water producing apparatus according to the present invention comprises: a steam generating means for heating raw water consisting of pure water having a TOC concentration of 2 to 3 ppb to generate steam; the generated steam, non-supply under der oxygen
Steam heating means for heating and thermally decomposing trace organic substances in the steam under the absence of the catalyst layer, and cooling and condensing means for cooling the steam from the steam heating means to obtain condensed water. And a treated water storage container into which the obtained condensed water is introduced, and produces high-purity water having a TOC concentration of 0.3 ppb or less.
It is characterized by being manufactured .
【0010】かかる本発明の高純度水製造装置では、水
蒸気中の有機物を高温加熱して熱分解するため、酸素や
酸化触媒を必要としない。従って、酸素供給物質中の不
純物の混入や酸化触媒を通過することによる汚染がな
く、TOC0.3ppb以下の高純度水を得ることがで
きる。In the high-purity water producing apparatus of the present invention, the organic matter in the steam is heated at a high temperature and thermally decomposed, so that oxygen and an oxidation catalyst are not required. Therefore, high purity water having a TOC of 0.3 ppb or less can be obtained without contamination by impurities in the oxygen supply material or contamination caused by passing through the oxidation catalyst.
【0011】本発明において、水蒸気発生手段、水蒸気
加熱手段及び冷却凝縮手段は、少なくとも水蒸気との接
触面を白金で構成することにより、装置構成部材からの
有機物汚染が防止されるようになり、より一層極低TO
C濃度の高純度水を得ることが可能となる。In the present invention, the steam generation means, the steam heating means, and the cooling and condensing means are configured so that at least the contact surface with the steam is made of platinum, so that organic matter contamination from the components of the apparatus can be prevented. Extremely low TO
High-purity water having a C concentration can be obtained.
【0012】また、処理水貯留容器に、貯留された処理
水に紫外線(UV)を照射するUV照射手段を設けるこ
とにより、貯留中においても処理水中の極微量の有機物
を分解してTOCの低減を図ることができる。更に、処
理水貯留容器に空気中の汚染物の混入を防止する汚染防
止手段を設けることにより、貯留中の汚染を防止し、純
度を維持することができる。Further, by providing a UV irradiation means for irradiating the stored treated water with ultraviolet rays (UV) in the treated water storage container, a trace amount of organic substances in the treated water can be decomposed even during storage to reduce the TOC. Can be achieved. Further, by providing the treated water storage container with a pollution prevention means for preventing contamination of air with contaminants, contamination during storage can be prevented and purity can be maintained.
【0013】[0013]
【発明の実施の形態】以下、図面を参照して本発明の実
施の形態を説明する。Embodiments of the present invention will be described below with reference to the drawings.
【0014】図1は本発明の高純度水製造装置の実施の
形態を示す模式的な断面図である。1は純水タンクであ
り、水蒸気発生の原料水としての純水が貯留されてい
る。FIG. 1 is a schematic sectional view showing an embodiment of the high-purity water producing apparatus of the present invention. Reference numeral 1 denotes a pure water tank which stores pure water as raw water for generating steam.
【0015】本発明においては、極低TOC濃度の高純
度水を製造することから、原料水としてもTOCの低い
ものが好ましい。原料水としてはTOC2〜3ppbの
低TOC濃度の純水を用いる。 In the present invention, since high-purity water having an extremely low TOC concentration is produced, it is preferable that the raw material water has a low TOC. As the raw material water Ru using pure water of low TOC concentration of TOC2~3ppb.
【0016】2は原料水を加熱して水蒸気を発生させる
ための、加熱容器部分が白金製の水蒸気発生器であり、
マントルヒータとカートリッジヒータを装備する。Reference numeral 2 denotes a steam generator whose heating vessel portion is made of platinum for heating the raw water to generate steam.
Equipped with mantle heater and cartridge heater.
【0017】3は水蒸気を高温加熱して有機物を熱分解
させる加熱炉である。この加熱炉3は、白金製の炉本体
に直接通電して炉本体を発熱体とするものであり、これ
により炉内部を900℃以上、好ましくは1000℃以
上に保持して水蒸気を加熱し、有機物を熱分解させる。Reference numeral 3 denotes a heating furnace for heating steam at a high temperature to thermally decompose organic substances. The heating furnace 3 is configured to directly energize a furnace body made of platinum to make the furnace body a heating element, thereby heating the inside of the furnace at 900 ° C. or higher, preferably 1000 ° C. or higher to heat steam, Thermal decomposition of organic matter.
【0018】4,5は、それぞれ水蒸気を冷却凝縮する
ための空冷フィン付き空冷管、リービーヒ型の水冷ジャ
ケット付き水冷管であり、いずれも白金製とされてい
る。Reference numerals 4 and 5 denote air-cooled tubes with air-cooled fins for cooling and condensing water vapor, and water-cooled tubes with a Liebeich type water-cooled jacket, both of which are made of platinum.
【0019】6は処理水貯留タンクであり、内部にUV
ランプ7が設けられている。また、外気からの汚染防止
のためにトラップ8が設けられている。Reference numeral 6 denotes a treated water storage tank in which UV is stored.
A lamp 7 is provided. Further, a trap 8 is provided to prevent contamination from outside air.
【0020】本実施例の装置においては、水蒸気発生器
2の加熱容器、加熱炉3の炉本体、空冷管4及び水冷管
5をいずれも白金製として、加熱された水蒸気が凝縮さ
れるまでの間に、水蒸気は白金とのみ接触するように構
成されている。In the apparatus of the present embodiment, the heating vessel of the steam generator 2, the furnace main body of the heating furnace 3, the air cooling pipe 4 and the water cooling pipe 5 are all made of platinum, and are used until the heated steam is condensed. In between, the steam is configured to only contact the platinum.
【0021】なお、水蒸気の加熱から凝縮に到るまでの
間で水蒸気が有機性材料と接触すると、有機性材料から
の汚染が生起するが、水蒸気発生器2、加熱炉3、空冷
管4及び水冷管5の少なくとも水蒸気と接触する面を白
金とすることにより、かかる汚染が防止される。また、
加熱炉3は、炉本体自体を発熱体とした構成が好まし
く、この場合、通電による加熱が可能であり、また10
00℃以上の耐熱性を有する材料として、白金が好適で
ある。If the steam comes into contact with the organic material during the period from the heating to the condensation of the steam, contamination from the organic material occurs, but the steam generator 2, the heating furnace 3, the air cooling tube 4, By making at least the surface of the water cooling tube 5 that is in contact with the water vapor with platinum, such contamination is prevented. Also,
The heating furnace 3 preferably has a structure in which the furnace body itself is a heating element. In this case, heating by energization is possible.
Platinum is preferred as a material having a heat resistance of at least 00 ° C.
【0022】この高純度水製造装置により極低TOC濃
度の高純度水を製造するには、まず、バルブV1 を開け
て純水タンク1内の純水を水蒸気発生器2に入れ、水蒸
気発生器2のヒータに通電してこの純水を加熱して水蒸
気を発生させる。[0022] To produce the high-purity water of ultralow TOC concentration by the high-purity water producing apparatus, firstly, it puts the pure water in the pure water tank 1 by opening the valve V 1 to the steam generator 2, steam generator The heater of the vessel 2 is energized to heat the pure water to generate steam.
【0023】発生した水蒸気を加熱炉3に送給し、水蒸
気を900℃以上、好ましくは1000〜1500℃に
加熱する。The generated steam is sent to the heating furnace 3 and the steam is heated to 900 ° C. or higher, preferably 1000 to 1500 ° C.
【0024】なお、水蒸気の加熱炉3の滞留時間は、加
熱温度や原料水として用いた純水のTOC濃度によって
も異なるが、通常の場合、0.1秒〜数秒程度とするの
が好ましい。The residence time of the steam in the heating furnace 3 varies depending on the heating temperature and the TOC concentration of the pure water used as the raw water, but is usually preferably about 0.1 second to several seconds.
【0025】この水蒸気が900℃以上に加熱されるこ
とにより、含有される有機物が水(水蒸気)と炭酸ガス
とに熱分解する。When this water vapor is heated to 900 ° C. or higher, the contained organic matter is thermally decomposed into water (water vapor) and carbon dioxide.
【0026】加熱炉3で有機物が分解された水蒸気は、
空冷管4で冷却された後、水冷管5で更に冷却されて凝
縮し、凝縮水(処理水)は処理水貯留タンク6に貯留さ
れる。The water vapor from which the organic matter is decomposed in the heating furnace 3 is
After being cooled by the air cooling pipe 4, it is further cooled and condensed by the water cooling pipe 5, and condensed water (treated water) is stored in a treated water storage tank 6.
【0027】この処理水貯留タンク6にはUVランプ7
が設けられている。処理水にUV照射することにより、
極微量残留する有機物が分解される。The treated water storage tank 6 has a UV lamp 7
Is provided. By irradiating the treated water with UV,
Very small amount of remaining organic matter is decomposed.
【0028】この処理水貯留タンク6には、有機物の熱
分解で発生した炭酸ガス等のガスを排出するためにトラ
ップ8を設けている。このトラップ8を設けたことによ
り、タンク6内への大気(汚染物質を含んだ空気)の流
入が防止され、貯留中の処理水の水質低下が防止され
た。The treated water storage tank 6 is provided with a trap 8 for discharging gas such as carbon dioxide gas generated by thermal decomposition of organic matter. By providing the trap 8, the inflow of the atmosphere (air containing pollutants) into the tank 6 was prevented, and the water quality of the stored treated water was prevented from lowering.
【0029】本発明の高純度水製造装置によれば、水蒸
気の高温加熱系内から酸化触媒や酸化剤などの汚染物混
入の要因となるものを完全に排除し、高清浄に維持され
た系内で水蒸気を加熱して有機物を熱分解除去するた
め、極めて低TOC濃度の高純度水を得ることができ
る。According to the apparatus for producing high-purity water of the present invention, a system which keeps high purity is completely eliminated from the high-temperature heating system of water vapor, which is a cause of contaminants such as an oxidation catalyst and an oxidizing agent. Since the organic matter is thermally decomposed and removed by heating the water vapor in the inside, high-purity water having an extremely low TOC concentration can be obtained.
【0030】[0030]
【実施例】以下に実施例を挙げて本発明をより具体的に
説明する。The present invention will be described more specifically with reference to the following examples.
【0031】実施例1 図1に示す高純度水製造装置により高純度水の製造を行
った。Example 1 High-purity water was produced by the high-purity water producing apparatus shown in FIG.
【0032】原料水としては、通常の純水製造装置(イ
オン交換+限外濾過膜処理+UV照射)で製造されたT
OC2〜3ppbの純水を用いた。この純水を50ml
/minで供給し、水蒸気発生器2で発生した水蒸気
(110℃)を1050℃の加熱炉3で加熱し、空冷管
4及び水冷管5で冷却して処理水として5℃の凝縮水を
得た。As the raw water, T was produced by a conventional pure water production apparatus (ion exchange + ultrafiltration membrane treatment + UV irradiation).
Pure water of OC2 to 3 ppb was used. 50 ml of this pure water
/ Min, and the steam (110 ° C.) generated by the steam generator 2 is heated in the heating furnace 3 at 1050 ° C. and cooled by the air cooling pipe 4 and the water cooling pipe 5 to obtain condensed water at 5 ° C. as treated water. Was.
【0033】この処理水のTOCをTOC計(栗田工業
(株)製高感度型TOC計「クリマトック(KURIM
ATOC)」(湿式酸化方式))を用いて測定した。The TOC of the treated water was measured using a TOC meter (Kurita Kogyo Co., Ltd., high-sensitivity TOC meter "Kurimat").
ATOC) "(wet oxidation method)).
【0034】その結果、TOCは0.3ppb以下と著
しく低いことが確認された。As a result, it was confirmed that TOC was remarkably low at 0.3 ppb or less.
【0035】[0035]
【発明の効果】以上詳述した通り、本発明の高純度水製
造装置によれば、TOC0.3ppb以下という極低有
機物濃度の高純度水を製造することができる。本発明の
高純度水製造装置により製造された高純度水は、実質的
に有機物を含有しない極めて高純度のものであり、零校
正液としてTOC計を高精度に校正することができる。As described above in detail, according to the high-purity water producing apparatus of the present invention, high-purity water having an extremely low organic substance concentration of TOC of 0.3 ppb or less can be produced. The high-purity water produced by the high-purity water producing apparatus of the present invention is extremely high-purity water containing substantially no organic substances, and can highly accurately calibrate a TOC meter as a zero calibration liquid.
【図1】本発明の高純度水製造装置の実施の形態を示す
模式的な断面図である。FIG. 1 is a schematic cross-sectional view showing an embodiment of a high-purity water production apparatus of the present invention.
1 純水タンク 2 水蒸気発生器 3 加熱炉 4 空冷管 5 水冷管 6 処理水貯留タンク 7 UVランプ 8 トラップ DESCRIPTION OF SYMBOLS 1 Pure water tank 2 Steam generator 3 Heating furnace 4 Air cooling tube 5 Water cooling tube 6 Treated water storage tank 7 UV lamp 8 Trap
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) C02F 1/04 C02F 1/02 C02F 1/32 B01D 1/00 B01D 3/00 B01D 5/00 ──────────────────────────────────────────────────続 き Continued on the front page (58) Fields surveyed (Int. Cl. 7 , DB name) C02F 1/04 C02F 1/02 C02F 1/32 B01D 1/00 B01D 3/00 B01D 5/00
Claims (4)
る原料水を加熱して水蒸気を発生させる水蒸気発生手段
と、 該水蒸気発生手段で発生した水蒸気を、酸素の非供給下
であって、かつ触媒層不存在の条件下に、加熱して該水
蒸気中の微量有機物を熱分解する水蒸気加熱手段と、 該水蒸気加熱手段からの水蒸気を冷却して凝縮水を得る
冷却凝縮手段と、 得られた凝縮水が導入される処理水貯留容器とを備え、TOC濃度0.3ppb以下の高純度水を製造する 高純
度水製造装置。(1) Pure water having a TOC concentration of 2 to 3 ppb.
That raw water is heated to a steam generating means for generating steam, the steam generated in the water vapor generating means, non-supply of oxygen
Steam heating means for heating and thermally decomposing trace organic substances in the steam under the absence of the catalyst layer; and cooling and condensing means for cooling the steam from the steam heating means to obtain condensed water. And a treated water storage container into which the obtained condensed water is introduced, and a high-purity water producing apparatus for producing high-purity water having a TOC concentration of 0.3 ppb or less .
段、水蒸気加熱手段及び冷却凝縮手段は、少なくとも水
蒸気との接触面が白金で構成されていることを特徴とす
る高純度水製造装置。2. The high-purity water producing apparatus according to claim 1, wherein at least a contact surface of the steam generating means, the steam heating means, and the cooling / condensing means with the steam is made of platinum.
貯留容器は、貯留された処理水に紫外線を照射する紫外
線照射手段と、空気中の汚染物の混入を防止する汚染防
止手段とを備えることを特徴とする高純度水製造装置。3. The apparatus according to claim 1, wherein the treated water storage container comprises: an ultraviolet irradiation means for irradiating the stored treated water with ultraviolet light; and a pollution preventing means for preventing contaminants in the air from being mixed. An apparatus for producing high-purity water, comprising:
て、水蒸気加熱手段が白金製の炉本体に直接通電して炉
本体を発熱体とする加熱炉であることを特徴とする高純
度水製造装置。 4. The method according to claim 1, wherein:
The steam heating means directly energizes the platinum
High purity characterized by a heating furnace whose main body is a heating element
Dewatering equipment.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP25866496A JP3198945B2 (en) | 1996-09-30 | 1996-09-30 | High-purity water production equipment |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP25866496A JP3198945B2 (en) | 1996-09-30 | 1996-09-30 | High-purity water production equipment |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH1099846A JPH1099846A (en) | 1998-04-21 |
JP3198945B2 true JP3198945B2 (en) | 2001-08-13 |
Family
ID=17323393
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP25866496A Expired - Fee Related JP3198945B2 (en) | 1996-09-30 | 1996-09-30 | High-purity water production equipment |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3198945B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101899117B1 (en) * | 2017-02-15 | 2018-09-14 | 울산과학기술원 | INTEGRATED SYSTEM FOR MONITORING β-RAYS ON UNDERWATER FIELD AND METHOD THEREOF |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104390474A (en) * | 2014-11-12 | 2015-03-04 | 耒阳市焱鑫有色金属有限公司 | Natural-circulation hot-water vapor recovery tank of blast-furnace water jacket |
JP2018001061A (en) * | 2016-06-28 | 2018-01-11 | 合同会社トレスバイオ技研 | Method for decomposing or carbonizing organic material and device used in the method |
CN107673530A (en) * | 2017-10-17 | 2018-02-09 | 广州雅津水处理设备有限公司 | A kind of disinfection system for high purity water |
-
1996
- 1996-09-30 JP JP25866496A patent/JP3198945B2/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101899117B1 (en) * | 2017-02-15 | 2018-09-14 | 울산과학기술원 | INTEGRATED SYSTEM FOR MONITORING β-RAYS ON UNDERWATER FIELD AND METHOD THEREOF |
Also Published As
Publication number | Publication date |
---|---|
JPH1099846A (en) | 1998-04-21 |
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