JPH11192401A - Oil component recovery device - Google Patents
Oil component recovery deviceInfo
- Publication number
- JPH11192401A JPH11192401A JP9321619A JP32161997A JPH11192401A JP H11192401 A JPH11192401 A JP H11192401A JP 9321619 A JP9321619 A JP 9321619A JP 32161997 A JP32161997 A JP 32161997A JP H11192401 A JPH11192401 A JP H11192401A
- Authority
- JP
- Japan
- Prior art keywords
- steam
- volatile oil
- oil
- waste liquid
- distillation
- 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.)
- Granted
Links
- 238000011084 recovery Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 239000000341 volatile oil Substances 0.000 claims abstract description 33
- 239000003921 oil Substances 0.000 claims abstract description 26
- 239000002699 waste material Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000001256 steam distillation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims 1
- 238000009877 rendering Methods 0.000 claims 1
- 238000011109 contamination Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229950011008 tetrachloroethylene Drugs 0.000 description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004045 organic chlorine compounds Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Landscapes
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Accessory Of Washing/Drying Machine, Commercial Washing/Drying Machine, Other Washing/Drying Machine (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、工場等で生じた揮
発性油分を含有する廃液を処理して、蒸留残渣を無害化
すると共に、回収原料揮発性油を再利用し、さらに揮発
性油分を含む水溶液を系外に出さない油分回収装置に関
する。[0001] The present invention relates to a method for treating a waste liquid containing a volatile oil produced in a factory or the like to render the distillation residue harmless, reusing the recovered raw volatile oil, and further removing the volatile oil. TECHNICAL FIELD The present invention relates to an oil recovery device that does not discharge an aqueous solution containing urea.
【０００２】[0002]
【従来の技術および発明が解決しようとする課題】従
来、揮発性油分含有廃液において油分含量が少量の場
合、産業廃棄物業者に委託し、燃焼によって処理してい
るが、有機塩素系化合物からはダイオキシン等の有害性
物質が生成し世界的に問題となっている。不法投棄はあ
とをたたず、地下水を汚染したりオゾン層を破壊し、社
会問題としても取り上げられている。又、大量の廃液で
比較的油分の含有量の高い水系のものは分液し、油分は
減圧もしくは常圧による蒸留によって処理されている
が、法的規制の厳しい有害性物質の処理については、規
則値内での処理において、残渣中の有害性物質の残存と
いう問題を常に残している。最終的には有害物質を含有
したまま産業廃棄物として燃焼処理されている。これは
蒸留終盤において蒸留釜空間に揮発性油分が残存してい
ることによる。2. Description of the Related Art Conventionally, when the oil content of a volatile oil-containing waste liquid is small, it is entrusted to an industrial waste contractor and treated by combustion. Toxic substances such as dioxin are generated and have become a problem worldwide. Illegal dumping continues to pollute groundwater and destroy the ozone layer, and has been raised as a social issue. In addition, a large amount of waste liquid and a water-based substance having a relatively high oil content are separated, and the oil component is treated by distillation under reduced pressure or normal pressure. The problem of remaining harmful substances in the residue is always left in the processing within the regulation value. Finally, it is burnt and treated as industrial waste while containing harmful substances. This is because volatile oil remains in the still space at the end of distillation.
【０００３】なお、水蒸気蒸留を用いる手法は、例えば
植物等から精油を製造するために使用されているが、加
熱水蒸気を用いる方法は精油成分が変質するため使用さ
れていない。加熱水蒸気による廃液中の油分の回収も未
だ知られていない。[0003] A method using steam distillation is used for producing essential oils from plants and the like, but a method using heated steam is not used because the essential oil components are deteriorated. Recovery of oil content in waste liquid by heating steam has not yet been known.
【０００４】さらに、水層に溶存した揮発性油分の含有
率は高く、環境衛生上そのままでは廃棄できない場合が
あり、規制値の含有率までさらに希釈するか、吸着剤に
吸着させて規制値の含有率に落とすなどの煩雑な処理が
必要である。この水層を蒸気発生機に戻し再利用するこ
とはかって行われていなかった。[0004] Furthermore, the content of volatile oil dissolved in the water layer is high and may not be discarded as it is for environmental sanitation. Complicated treatment such as reducing the content is required. This water layer has never been returned to the steam generator for reuse.
【０００５】[0005]
【課題を解決するための手段】本発明は、揮発性油分を
含有する廃液に加熱水蒸気を送りつつ、揮発性油分を水
蒸気蒸留して除去し蒸留残渣を無害化することを特徴と
する油分回収装置を提供するものである。すなわち、揮
発性廃液を加熱蒸気を用いることによって、廃液の温度
を１００℃以上に上げ、揮発性油分を蒸留され易くし、
なおかつ温度が上がりすぎて廃液の樹脂化が進む程に温
度が上がることもなく、廃液を効率よく処理することが
できる。有毒な揮発性油分を除去し蒸留残渣を無害化す
ると共に、回収揮発性油を再利用することができる。SUMMARY OF THE INVENTION The present invention is directed to an oil recovery system in which heated steam is sent to a waste liquid containing volatile oil, and the volatile oil is removed by steam distillation to render the distillation residue harmless. An apparatus is provided. That is, by using a volatile waste liquid by heating steam, the temperature of the waste liquid is raised to 100 ° C. or higher, and the volatile oil is easily distilled.
In addition, the waste liquid can be efficiently treated without increasing the temperature as the temperature of the waste liquid rises to the extent that the waste liquid is converted into resin. The toxic volatile oil can be removed to make the distillation residue harmless, and the recovered volatile oil can be reused.
【０００６】さらに、本発明は上記装置の水蒸気蒸留に
より得られた揮発性油層と水層を分液し、油層は系外に
除き、揮発性油分を含む水層は蒸気発生機に戻して揮発
性油分を含む水層を系外に出さないことを特徴とする油
分回収装置を提供する。この装置を用いることによっ
て、揮発性油分が系外に出ないため揮発性油分が毒性の
強いものである場合は環境汚染などの危険を防ぐことが
可能である。Further, the present invention separates a volatile oil layer and an aqueous layer obtained by steam distillation in the above apparatus, removes the oil layer outside the system, and returns the aqueous layer containing volatile oil to a steam generator for volatilization. Provided is an oil recovery device characterized in that an aqueous layer containing a volatile oil is not discharged out of the system. By using this apparatus, it is possible to prevent the risk of environmental pollution and the like when the volatile oil is highly toxic because the volatile oil does not go out of the system.
【０００７】構成要素として、蒸留釜、蒸気発生機、冷
却器、分液器、温度計、蒸気調整弁、液面レベルセンサ
ー、吸着槽、廃液送液ポンプ、留出液抜き取りポンプを
含むことができる。上記構成要素は廃液中の油分の種
類、量によって適宜選択される。本発明の装置は、バッ
チ式もしくは連続式のいずれの場合でもよい。さらに、
上記の構成要素に水層を蒸気発生機に返送するための水
層循環ポンプを含むことができる。しかし、揮発性油分
を含む水層の蒸気発生機への返送は落差で戻すことも可
能である。The components include a distillation still, a steam generator, a cooler, a liquid separator, a thermometer, a steam regulating valve, a liquid level sensor, an adsorption tank, a waste liquid feed pump, and a distillate discharge pump. it can. The above components are appropriately selected depending on the type and amount of the oil component in the waste liquid. The apparatus of the present invention may be either a batch type or a continuous type. further,
The above components may include a water layer circulation pump for returning the water layer to the steam generator. However, the return of the water layer containing volatile oil to the steam generator can be returned by head.
【０００８】[0008]
【発明の実施の形態】本発明の装置に適用し得る廃液は
含まれる油分が揮発性であれば、あらゆる種類の廃液に
適応し得る。蒸留釜は、ガラス製、金属製と種々の容器
が知られ市販されている。特別な仕様の容器の製作も可
能であるし、入手も可能である。蒸気発生機は、市販で
容易に入手することも出来る。工場等においては余剰の
蒸気を利用することも可能である。加熱水蒸気は絶対圧
で１〜５kg／cm2であり、好ましくは約１〜３kg／cm2で
あり、このとき、蒸留釜中の温度は約１００〜約１０３
℃にまで上昇している。蒸留に付す時間は処理量による
規模により異なる。DETAILED DESCRIPTION OF THE INVENTION The waste liquid applicable to the apparatus of the present invention can be applied to all kinds of waste liquid as long as the oil contained therein is volatile. Distillation pots are known and are commercially available in various containers such as glass and metal. Containers with special specifications are available and available. Steam generators are also readily available commercially. In a factory or the like, surplus steam can be used. The heating steam has an absolute pressure of 1 to 5 kg / cm 2 , preferably about 1 to 3 kg / cm 2 , and at this time, the temperature in the distillation still is about 100 to about 103.
℃. The time required for distillation depends on the scale depending on the throughput.
【０００９】冷却器は、種々の種類の冷却器が市場に存
在する。分液器は、市場で容易に入手出来る。温度計
は、アナログ、デジタルと種々な型式のものが市販され
ている。液面レベルセンサーは市場で容易に入手可能で
ある。蒸気調整弁は、手動から自動まで種々のものの入
手が可能である。吸着槽において、容器はガラス製、金
属製いずれも市場で容易に入手が可能で、それに充填す
る吸着剤も活性炭等多数市販されている。廃液送液・留
出液抜き取り、水層循環ポンプは、種々の能力を有した
ポンプを入手することができる。本発明の油分回収装置
の上記の各構成要素は廃液中の油分の種類、量によって
適宜選択される。[0009] There are various types of coolers on the market. Separators are readily available on the market. Various types of thermometers such as analog and digital are commercially available. Level sensors are readily available on the market. Various types of steam regulating valves are available from manual to automatic. In the adsorption tank, both containers made of glass and metal are easily available on the market, and a large number of adsorbents, such as activated carbon, for filling the containers are commercially available. Pumps having various capabilities can be obtained for the waste liquid feeding / distillate removal and water layer circulation pumps. The above components of the oil recovery apparatus of the present invention are appropriately selected depending on the type and amount of the oil in the waste liquid.
【００１０】本発明の油分回収装置を概念図により説明
すると、図１において、蒸気発生機（）の加熱水蒸気
は蒸気調整弁（）を経て、廃液を入れた蒸留釜（）
に導入され、加熱水蒸気蒸留される。揮発性油分は水蒸
気と共に揮発し、冷却部（）で冷却され液化し、分液
部（）に至る。分液部では油層と水層が分離され、例
えば、比重の大きい水に対して難溶性の油分は下層に、
比重の小さい油分は上層に分液される。分液された油分
は、必要に応じて適宜精製され再利用される。これらの
液の移動に送液ポンプが使用され、水層部に溶解した油
分は吸着槽（）にて除去される。温度計（）は内温
の確認に用いる。The oil recovery apparatus of the present invention will be described with reference to a conceptual diagram. In FIG. 1, heated steam of a steam generator () passes through a steam regulating valve () and passes through a distillation still () containing waste liquid.
And heated and distilled by steam. The volatile oil evaporates together with the water vapor, is cooled and liquefied in the cooling section (), and reaches the liquid separating section (). In the liquid separation part, the oil layer and the water layer are separated, for example, the oil that is hardly soluble in water having a large specific gravity is placed in the lower layer,
The oil having a small specific gravity is separated into an upper layer. The separated oil is appropriately purified and reused as necessary. A liquid feed pump is used to move these liquids, and the oil dissolved in the aqueous layer is removed in the adsorption tank (). The thermometer () is used to check the internal temperature.
【００１１】図２において、図１の吸着槽に替えて水層
循環ポンプを用いて揮発性油分を含む水層を蒸気発生機
に返送し再利用する。この時各所に液面レベルセンサー
を採用することによって自動的に水層の搬送が可能であ
る。In FIG. 2, an aqueous layer containing volatile oil is returned to a steam generator for reuse by using an aqueous layer circulation pump instead of the adsorption tank of FIG. At this time, the water layer can be automatically conveyed by adopting the liquid level sensors in various places.
【００１２】本発明の装置は、従来の装置あるいは方法
に比較して次のような利点を有している。 １）処理によって新たな有害物質を生じない（有機塩素
系化合物処理によるダイオキシンの生成は社会問題とな
っている。）。 ２）ランニングコストが極めて低い（冷却水、加熱蒸
気、人件費）。 ３）回収油分の再利用が可能である。 ４）操作が極めて容易である。 ５）安全性が極めて高い。 ６）自動化が容易である。 ７）水層が循環することにより、揮発性油分を含む水層
が系外に出ないことになり、有害物質による環境汚染を
防ぐことが可能である。The apparatus of the present invention has the following advantages over the conventional apparatus or method. 1) No new harmful substances are generated by the treatment (the generation of dioxin by the treatment with organochlorine compounds is a social problem). 2) Extremely low running costs (cooling water, heating steam, labor costs). 3) Recovered oil can be reused. 4) Operation is extremely easy. 5) Extremely high safety. 6) Automation is easy. 7) By circulating the water layer, the water layer containing volatile oil does not go out of the system, and it is possible to prevent environmental pollution by harmful substances.
【００１３】[0013]
【実施例】次にテトラクロロエチレン（ＴＣＥと略記す
る）を含有する排出規制の厳しいクリーニング分野の廃
液を用いて本発明を更に具体的に説明する。 実施例１ 丸底フラスコ３ｌにテトラクロロエチレンを含有するク
リーニング店廃液（ＴＣＥ蒸留残渣）１.０ｋｇを秤量
し、電気蒸気発生機（大阪電気工業株式会社製ＯＳＧ−
４０型）より０.８〜０.９kg/cm2（絶対圧０.５〜４.５
kg/cm2）の水蒸気を導入して、約２０分間蒸留に付した
（内温１００〜１０３℃）。ＴＣＥの定性定量にはガス
クロマトグラフィー・質量分析計（島津製作所製ＧＣＭ
Ｓ−ＱＰ２０００Ａ）を用いて定性定量した。留出物は
分液ロート中に受け、上層（水層）と下層（ＴＣＥ層）
に分け、蒸留残渣及び蒸留容器空間のＴＣＥについても
常法に従って分析した。上層は活性炭槽を通したものに
ついても同様に分析した。Next, the present invention will be described in more detail by using a waste liquid containing tetrachloroethylene (abbreviated as TCE) in the field of cleaning in which discharge regulations are strict. Example 1 In a 3 l round-bottom flask, 1.0 kg of a cleaning solution waste liquid (TCE distillation residue) containing tetrachloroethylene was weighed, and an electric steam generator (OSG- manufactured by Osaka Electric Industry Co., Ltd.) was used.
0.8-0.9 kg / cm 2 (absolute pressure 0.5-4.5)
kg / cm 2 ), and the mixture was subjected to distillation for about 20 minutes (internal temperature: 100 to 103 ° C.). For qualitative determination of TCE, use a gas chromatography / mass spectrometer (GCM manufactured by Shimadzu Corporation).
S-QP2000A). Distillate is collected in a separating funnel, and the upper layer (water layer) and the lower layer (TCE layer)
And TCE in the distillation residue and the space in the distillation vessel were also analyzed according to a conventional method. The upper layer passed through an activated carbon tank was analyzed in the same manner.
【００１４】 結果 各分取物中のＴＣＥ含有量（３回の平均値） 原料廃液 １ｋｇ中 ３１３.１０ｇ 分液上層 １.５１ｋｇ中 １５８.４５ｍｇ 活性炭通過水 検出されず（排出規制：０.１ppm以下） 分液下層 ３５４.９ｇ中 ２９７.０７g 残渣 検出されず（排出規制：０.１ppm以下） 容器空間 ４.８１ppm（作業環境評価基準 ５０ppm以下）Results TCE content in each fraction (average value of 3 times) 313.10 g / kg of raw material waste liquid 158.45 mg / 1.51 kg of liquid separation upper layer Activated carbon passing water Not detected (discharge regulation: 0.1 ppm) Lower) Separation lower layer 297.007 g in 354.9 g Residue Not detected (Emission regulation: 0.1 ppm or less) Container space 4.81 ppm (Working environment evaluation standard 50 ppm or less)
【００１５】実施例２ 実施例１において、分液器より流出する上層部（水層
部）を蒸気発生機に付属するストレージタンクに導入
した。ストレージタンクには液面レベルセンサー（上部
および下部の２カ所）が取り付けられ、水層循環ポンプ
に電気的に連動している。ストレージタンク内の揮発
性油分を含む水層部は、蒸気発生機内の液面レベルセン
サーの指示により逐次蒸気発生機に導入され、水蒸気蒸
留に用いられた。数バッチを連続的に行った結果、分液
器から系外に排出された油分以外に本来水層として系外
に排出されるべきテトラクロロエチレンが、水層部１.
０ｋｇ当たり、平均６５.０ｍｇ回収された。Example 2 In Example 1, the upper part (water layer) flowing out of the liquid separator was introduced into a storage tank attached to a steam generator. A liquid level sensor (upper and lower) is attached to the storage tank and is electrically linked to the water layer circulation pump. The aqueous layer containing volatile oil in the storage tank was successively introduced into the steam generator according to an instruction from a liquid level sensor in the steam generator, and used for steam distillation. As a result of performing several batches continuously, tetrachloroethylene which should be discharged outside the system as an aqueous layer in addition to the oil discharged from the separator from the system outside the system, the aqueous layer portion 1.
An average of 65.0 mg was recovered per 0 kg.
【図１】 本発明の請求項１記載の油分回収装置の概念
図である。FIG. 1 is a conceptual diagram of an oil recovery device according to claim 1 of the present invention.
【図２】 本発明の請求項２記載の油分回収装置の概念
図である。FIG. 2 is a conceptual diagram of an oil recovery apparatus according to a second embodiment of the present invention.
【符号の説明】 ・・蒸気発生機、・・蒸気調整弁、・・蒸留釜、
・・冷却部、・・分液部、・・吸着槽、・・温
度計 ・・水層循環ポンプ[Explanation of symbols] ・ ・ Steam generator, ・ ・ Steam regulating valve, ・ ・ Distillation pot,
..Cooling part, liquid separation part, adsorption tank, thermometer
Claims (4)
液に加熱水蒸気を送りつつ、揮発性油分を水蒸気蒸留し
て除去し蒸留残渣を無害化することを特徴とする油分回
収装置。An oil recovery apparatus characterized in that volatile oil is removed by steam distillation while heating steam is sent from a steam generator to a waste liquid containing volatile oil, thereby rendering the distillation residue harmless.
蒸気蒸留により得られた揮発性油層と水層を分液し、油
層は系外に除き、揮発性油分を含む水層は蒸気発生機に
戻して揮発性油分を含む水層を系外に出さないことを特
徴とする油分回収装置。2. The apparatus according to claim 1, wherein a volatile oil layer obtained by steam distillation and an aqueous layer are separated, the oil layer is removed outside the system, and the aqueous layer containing volatile oil is a steam generator. An oil recovery apparatus characterized by not returning an aqueous layer containing volatile oil to the system outside the system.
温度計、蒸気調整弁、液面レベルセンサー、廃液送液ポ
ンプ、留出液抜き取りポンプおよび、吸着槽または／お
よび水層循環ポンプを含む、請求項１または２記載の装
置。3. A distillation still, a steam generator, a cooler, a liquid separator,
The apparatus according to claim 1, further comprising a thermometer, a steam regulating valve, a liquid level sensor, a waste liquid feed pump, a distillate extraction pump, and an adsorption tank or / and a water layer circulation pump.
／cm2である、請求項１〜３のいずれか１項記載の装
置。4. The steam pressure of the heated steam is 1 to 5 kg in absolute pressure.
/ Cm is 2, apparatus according to any one of claims 1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32161997A JP3263351B2 (en) | 1997-10-29 | 1997-11-21 | Oil recovery device |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29691397 | 1997-10-29 | ||
| JP9-296913 | 1997-10-29 | ||
| JP32161997A JP3263351B2 (en) | 1997-10-29 | 1997-11-21 | Oil recovery device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11192401A true JPH11192401A (en) | 1999-07-21 |
| JP3263351B2 JP3263351B2 (en) | 2002-03-04 |
Family
ID=26560904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32161997A Expired - Fee Related JP3263351B2 (en) | 1997-10-29 | 1997-11-21 | Oil recovery device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3263351B2 (en) |
-
1997
- 1997-11-21 JP JP32161997A patent/JP3263351B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP3263351B2 (en) | 2002-03-04 |
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