JP3001169B2 - Fly incense stick - Google Patents

Fly incense stick

Info

Publication number
JP3001169B2
JP3001169B2 JP4117889A JP11788992A JP3001169B2 JP 3001169 B2 JP3001169 B2 JP 3001169B2 JP 4117889 A JP4117889 A JP 4117889A JP 11788992 A JP11788992 A JP 11788992A JP 3001169 B2 JP3001169 B2 JP 3001169B2
Authority
JP
Japan
Prior art keywords
fly
stabilizer
empentrin
incense stick
tert
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.)
Expired - Lifetime
Application number
JP4117889A
Other languages
Japanese (ja)
Other versions
JPH05271018A (en
Inventor
純郎 勝田
良裕 南手
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dainihon Jochugiku Co Ltd
Original Assignee
Dainihon Jochugiku Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Dainihon Jochugiku Co Ltd filed Critical Dainihon Jochugiku Co Ltd
Priority to JP4117889A priority Critical patent/JP3001169B2/en
Priority to CN93101771A priority patent/CN1044660C/en
Publication of JPH05271018A publication Critical patent/JPH05271018A/en
Application granted granted Critical
Publication of JP3001169B2 publication Critical patent/JP3001169B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Agricultural Chemicals And Associated Chemicals (AREA)

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、有効成分としてエムペ
ントリンを含有するハエ取線香に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fly incense stick containing empentrin as an active ingredient.

【0002】[0002]

【従来の技術】蚊取線香は、蚊の成虫駆除用殺虫剤とし
て100年以上も前から親しまれているもので、その有
効成分としては、その加熱蒸散性と熱安定性ゆえに
(±)−2−アリル−3−メチル−シクロペント−2−
エン−1−オン−4−イル (+)−シス,トランス−
クリサンテマート(以降、ピナミンフォルテと称す)が
広く使用されている。一方、ハエについては、都市部で
は発生が減っているものの、ゴミ処理場や畜舎、鶏舎な
どの周辺では従来以上に悩まされる機会が多くなってい
る。ハエの発生源対策用として乳剤、油剤、粉剤などの
殺虫剤が使用されるほか、一般家庭で成虫駆除用に空間
エアゾールが汎用されているが一過性で効果の持続性に
乏しいという欠点がある。そこで、空間処理剤であっ
て、かつ効果が数時間持続し、更に拡散性がよく開放的
な場面でも有効なハエ防除剤の開発が望まれている。
2. Description of the Related Art Mosquito coils have been used for more than 100 years as an insecticide for controlling mosquitoes, and their active ingredients are due to their heat transpiration and thermal stability.
(±) -2-allyl-3-methyl-cyclopent-2-
En-1-one-4-yl (+)-cis, trans-
Chrysanthemato (hereinafter referred to as pinamin forte) is widely used. On the other hand, flies are less common in urban areas, but are more likely to be troubled around garbage dumps, livestock stalls, and poultry houses. Insects such as emulsions, oils and powders are used to control the source of flies.Furthermore, space aerosols are widely used in general households to control adults, but they have the disadvantage of being transient and of poor sustainability. is there. Therefore, development of a fly control agent which is a space treatment agent, has an effect lasting for several hours, has a good diffusibility, and is effective even in an open scene is desired.

【0003】[0003]

【発明が解決しようとする課題】蚊取線香は、マッチ一
本で空間処理を時間的にも保持し、燃え尽きるまで効力
は一定なので非常に合理的な殺虫形態であり、蚊取線香
の有効成分は燃焼部から数mm離れた200〜250℃
付近の部位から揮散する。従来のピナミンフォルテ含有
線香では安定剤を添加しなくても、有効成分の揮散率が
70〜80%に達することが知られているが、ハエに対
する効力は弱く、ハエ取線香への適用は困難であった。
ところで、エムペントリンは、特公昭55−42045
号公報に記載の殺虫性化合物で、各種害虫に高い殺虫効
力を示し、かつ常温揮散性を有することから特に衣料害
虫防除用分野で実用化に至っている。本発明者らは、エ
ムペントリンのハエに対する効力と揮散性に着目し、ハ
エ取線香の開発に着手したが、従来線香のピナミンフォ
ルテをエムペントリンに置き換えただけでは揮散率がお
よそ50%に低下するという問題に直面した。これは、
エムペントリンがピナミンフォルテに比べて熱安定性に
劣り、加熱による薬剤の分解、重合等に起因したものと
考えられる。従って熱安定性の改善は、エムペントリン
ハエ取線香の重要な課題であった。
A mosquito coil is a very rational insecticidal form since a single match maintains spatial processing over time and its efficacy is constant until it is burned out. Is 200 to 250 ° C, several mm away from the combustion part
Volatilizes from nearby parts. It is known that the volatilization rate of the active ingredient reaches 70 to 80% without adding a stabilizer in the conventional pinamin forte-containing incense, but the effect on fly is weak, and application to the fly incense is difficult. It was difficult.
By the way, empentrin is
The insecticidal compound described in Japanese Patent Application Publication No. JP-A-2003-133873 has a high insecticidal effect on various pests and has a normal-temperature volatilization property, and thus has been put to practical use particularly in the field of controlling insect pests on clothing. The present inventors have focused on the efficacy and volatility of empentrin against flies, and have started the development of fly incense sticks. Faced the problem. this is,
It is considered that empentrin is inferior in thermal stability to pinamine forte and is caused by decomposition of the drug by heating, polymerization and the like. Therefore, improvement of thermal stability has been an important issue for empentrin fly incense sticks.

【0004】[0004]

【課題を解決するための手段】上記課題を解決するた
め、本発明は、有効成分として、エムペントリンを0.
3〜2.0重量%含有し、かつ、沸点が250℃以上の
ジ−ターシャリーブチル−フェノール系安定剤の1種又
は2種以上を、エムペントリンに対して0.05〜2.
0倍量配合したことを特徴とするハエ取線香に係る。
Means for Solving the Problems In order to solve the above-mentioned problems, the present invention comprises empentrin as an active ingredient in an amount of 0.1 to 0.1%.
One or two or more di-tert-butyl-phenol-based stabilizers containing 3 to 2.0% by weight and having a boiling point of 250 ° C. or more are used in an amount of 0.05 to 2.
The present invention relates to a fly incense stick, which is blended in an amount of 0 times.

【0005】すなわち、エムペントリンハエ取線香の熱
安定性を改善するために、種々の安定剤を検討したとこ
ろ、沸点が250℃以上のジ−ターシャリーブチル−フ
ェノール系安定剤の1種又は2種以上をエムペントリン
に対して0.05〜2.0倍量配合することによって、
経時的安定性のみならず、燻煙時の安定性も著しく増強
させ、揮散率を70〜80%にまで高め得ることを見い
出し本発明を完成した。
That is, when various stabilizers were studied to improve the thermal stability of the empentrin fly incense stick, one of di-tertiary butyl-phenol-based stabilizers having a boiling point of 250 ° C. or higher or By blending two or more types in an amount of 0.05 to 2.0 times with respect to empentrin,
The inventors have found that not only the stability over time but also the stability during smoking can be significantly enhanced, and the volatilization rate can be increased to 70 to 80%, thus completing the present invention.

【0006】[0006]

【作用】本発明のハエ取線香で有効成分として用いられ
るエムペントリンは、ピナミンフォルテに比べてハエに
対して高い殺虫効力を有し、ハエ取線香中に0.3〜
2.0重量%配合されれば十分である。なお、これに従
来のピレスロイド、例えば、ピナミン、ピナミンフォル
テ、バイオアレスリン、エスビオール、エトックなどを
混合しても何らさしつかえない。本発明のハエ取線香
は、安定剤として沸点が250℃以上のジ−ターシャリ
ーブチル−フェノール系安定剤を配合したことに特徴を
有する。例えば、3−ターシャリーブチル−4−ヒドロ
キシアニソールや2−ターシャリーブチル−4−ヒドロ
キシアニソールのようなモノ−ターシャリーブチル−フ
ェノール系安定剤は効果がなく、また、N,N’−ジフ
ェニル−P−フェニレンジアミンやフェニル−β−ナフ
チルアミンのようなアミン系安定剤についても効果は低
かった。また、沸点が250℃以上のものが有効な理由
は、有効成分のピレスロイドが200〜250℃付近か
ら揮散するので、安定剤自身、この温度で揮散しないこ
とが必要なためである。
[Effect] Empentrin used as an active ingredient in the fly incense stick of the present invention has a higher insecticidal activity against flies than pinamine forte, and 0.3 to 10% is contained in the fly incense stick.
2.0% by weight is sufficient. It should be noted that even if a conventional pyrethroid such as pinamine, pinamine forte, bioarrestrin, esviol, ethoc, or the like is mixed with the mixture, there is no problem. The fly incense stick of the present invention is characterized in that a di-tert-butyl-phenol-based stabilizer having a boiling point of 250 ° C. or more is blended as a stabilizer. For example, mono-tert-butyl-phenol-based stabilizers such as 3-tert-butyl-4-hydroxyanisole and 2-tert-butyl-4-hydroxyanisole have no effect, and N, N'-diphenyl- Amine-based stabilizers such as P-phenylenediamine and phenyl-β-naphthylamine were also less effective. In addition, the reason why those having a boiling point of 250 ° C. or more is effective is that the stabilizer itself does not volatilize at this temperature because pyrethroid of the active ingredient volatilizes from around 200 to 250 ° C.

【0007】本発明で用いられる安定剤としては、次の
ようなものが挙げられるがもちろんこれらのみに限定さ
れるものではない。
[0007] Examples of the stabilizer used in the present invention include, but are not limited to, the following.

【0008】(1) 2,6−ジ−ターシャリーブチル
−4−メチルフェノール(BHT)
(1) 2,6-di-tert-butyl-4-methylphenol (BHT)

【安定剤A】(2) 2,2’−メチレンビス(4−メ
チル−6−ターシャリーブチルフェノール)
[Stabilizer A] (2) 2,2'-methylenebis (4-methyl-6-tert-butylphenol)

【安定剤B】(3) 2,2’−メチレンビス(4−エ
チル−6−ターシャリーブチルフェノール)
[Stabilizer B] (3) 2,2'-methylenebis (4-ethyl-6-tert-butylphenol)

【安定剤C】(4) 4,4’−ブチリデンビス(3−
メチル−6−ターシャリーブチルフェノール)
[Stabilizer C] (4) 4,4'-butylidenebis (3-
Methyl-6-tert-butylphenol)

【安定剤D】(5) 4,4’−チオビス(3−メチル
−6−ターシャリーブチルフェノール)
[Stabilizer D] (5) 4,4'-thiobis (3-methyl-6-tert-butylphenol)

【安定剤E】(6) 2−ターシャリーブチル−6−
(3−ターシャリーブチル−2−ヒドロキシ−5−メチ
ルベンジル)−4−メチルフェニル アクリレート
[Stabilizer E] (6) 2-tert-butyl-6-
(3-tert-butyl-2-hydroxy-5-methylbenzyl) -4-methylphenyl acrylate

【安定剤F】(7) 2,4−ジ−ターシャリーブチル
フェニル 3,5−ジ−ターシャリーブチル−4−ヒド
ロキシベンゾエート
[Stabilizer F] (7) 2,4-di-tert-butylphenyl 3,5-di-tert-butyl-4-hydroxybenzoate

【安定剤G】[Stabilizer G]

【0009】なお、本発明では上記安定剤の1種又は2
種以上がエムペントリンに対して0.05〜2.0倍量
配合されるが、もちろん、これにホスファイト系、アミ
ン系、有機イオウ系などの従来の種々の安定剤を混合し
てもかまわない。
In the present invention, one or two of the above stabilizers are used.
More than one kind is blended in an amount of 0.05 to 2.0 times the amount of empentrin, but of course, various conventional stabilizers such as phosphite-based, amine-based, and organic sulfur-based compounds may be mixed. .

【0010】本発明のハエ取線香は、上記有効成分組成
物に、必要ならば、ピペロニルブトキサイド、MGK−
264,MGK−5026,S−421,リーセン38
4などの共力剤を加えてもよい。更に、除虫菊抽出粕
粉、木粉などの支燃剤、たぶ粉、デキストリン、澱粉、
アラビアゴム、CMCなどの糊剤、着色剤としてのマラ
カイトグリーンや防黴剤としてのデヒドロ酢酸や2,4
−ジニトロフェノール、その他、鉱物性微粉末、ポリエ
チレングリコールなどを適宜加えて、常法に従い、ハエ
取線香を得ることができる。
[0010] The fly incense stick of the present invention may be added to the above-mentioned active ingredient composition, if necessary, with piperonyl butoxide, MGK-
264, MGK-5026, S-421, Reisen 38
A synergist such as 4 may be added. In addition, pyrethrum extract lees flour, flame retardants such as wood flour, soybean flour, dextrin, starch,
Sizing agents such as gum arabic and CMC, malachite green as a coloring agent, dehydroacetic acid as a fungicide and 2,4
Fly fly incense can be obtained in a conventional manner by appropriately adding dinitrophenol, other fine mineral powder, polyethylene glycol and the like.

【0011】本発明によれば、有効成分としてエムペン
トリンを用いるとともに、安定剤の効果で、従来のピナ
ミンフォルテ線香よりハエはもちろん、蚊に対しても高
い殺虫効果を奏し、極めて有用なハエ取線香を提供する
ものである。
According to the present invention, empentrin is used as an active ingredient, and the effect of a stabilizer is higher than that of conventional pinamin forte incense sticks. It provides incense.

【0012】次に、試験例及び実施例をあげて本発明を
より詳細に説明するが、本発明は、その要旨を越えない
限りこれらのみに限定されるものではない。
Next, the present invention will be described in more detail with reference to Test Examples and Examples, but the present invention is not limited only to these without departing from the gist thereof.

【0013】[0013]

【試験例】次表に示す処方にてハエ取線香を調製し、経
時安定性(40℃、6ヶ月保存)、燻煙時の有効成分の
揮散率、ハエ成虫に対する殺虫効力を調べた。なお、そ
の他の成分については、記載成分以外に、澱粉20重量
%、デヒドロ酢酸ナトリウム0.2重量%、除虫菊抽出
粕粉15重量%、ならびに木粉を加えて全量を100重
量%とした。また、経時安定性は以下の基準により評価
し、殺虫効力はピナミンフォルテ0.8重量%の線香を
1.0として相対効力で示した。 ○;40℃、6ヶ月保存後の有効成分の回収率が95%以上 △; 〃 90〜95% ×; 〃 90%以下
[Test Examples] Fly incense sticks were prepared according to the formulation shown in the following table, and the stability over time (preserved at 40 ° C. for 6 months), the volatilization rate of the active ingredient during smoking, and the insecticidal efficacy against flies were examined. In addition, about the other components, in addition to the components described, 20% by weight of starch, 0.2% by weight of sodium dehydroacetate, 15% by weight of fleas extracted from pyrethrum, and wood flour were added to make the total amount 100% by weight. The stability over time was evaluated according to the following criteria, and the insecticidal efficacy was indicated by relative efficacy with the incense stick of 0.8% by weight pinamine forte taken as 1.0. ;: Recovery rate of active ingredient after storage at 40 ° C. for 6 months is 95% or more △; 90 90 to 95% ×; 〃 90% or less

【0014】[0014]

【表1】 [Table 1]

【0015】試験の結果、エムペントリンハエ取線香に
ジ−ターシャリーブチル−フェノール系安定剤をエムペ
ントリンに対して0.05倍量以上配合することによっ
て、経時的安定性、燻煙時の有効成分の揮散率が向上
し、ピナミンフォルテ線香(対照線香6)に比べて高い
殺虫効力を示すことが認められた。一方、安定剤とし
て、対照線香2のようにモノ−ターシャリーブチル−フ
ェノール系化合物を配合したものや、対照線香3のよう
にアミン系化合物を配合したものは、特に燻煙時の揮散
率に改善がみられず不適であった。また、本発明で用い
る安定剤の配合量は、対照線香4,5に示すように、エ
ムペントリンに対して0.05倍量以下では不十分で、
一方、2.0倍量を越えても効果は頭打ちとなることが
明らかとなった。ピナミンフォルテ線香では、安定剤配
合の効果がほとんどないのに対し、本発明のエムペント
リンハエ取線香は、特定の安定剤を配合することによっ
て高い殺虫活性の線香を実現し、その実用性は極めて高
い。
[0015] As a result of the test, the empertrin fly incense stick was added with a di-tertiary butyl-phenol-based stabilizer in an amount of 0.05 times or more of empentrin to provide stability over time and effective smoking. It was recognized that the volatilization rate of the component was improved, and the insecticidal effect was higher than that of the pinamine forte incense stick (control incense stick 6). On the other hand, as a stabilizer, a compound containing a mono-tertiary butyl-phenolic compound as in Control Incense 2 or a compound containing an amine compound as Control Incense 3, particularly the volatilization rate during smoking. No improvement was observed and it was unsuitable. Further, as shown in the control incense sticks 4 and 5, the compounding amount of the stabilizer used in the present invention is insufficient when the amount is 0.05 times or less of empentrin.
On the other hand, it became clear that the effect leveled off even if the amount exceeded 2.0 times. In the case of pinamine forte incense, there is almost no effect of compounding a stabilizer, while the empentrin fly incense stick of the present invention realizes a high insecticidal activity incense by adding a specific stabilizer, and its practicality Is extremely high.

【0016】[0016]

【実施例1】エムペントリン0.8部と安定剤A(2,
6−ジ−ターシャリーブチル−4−メチルフェノール)
0.15部を除虫菊抽出粕粉、木粉、澱粉などの線香用
基材99.05部と均一に混合し、公知の方法によって
ハエ取線香を得た。この一巻(13g)を6畳の部屋で
使用し、有効成分の揮散率を測定したところ75%で、
燻煙時間7時間半にわたり、ハエならびに蚊を完全に防
除できた。
Example 1 0.8 parts of empentrin and stabilizer A (2,
6-di-tert-butyl-4-methylphenol)
0.15 part was uniformly mixed with 99.05 parts of a base material for incense such as pyrethrum extract meal powder, wood flour, starch and the like, and a fly incense stick was obtained by a known method. When one volume (13 g) was used in a room of 6 tatami mats and the volatilization rate of the active ingredient was measured, it was 75%.
The flies and mosquitoes were completely controlled over a period of 7 and a half hours of smoking.

【0017】[0017]

【実施例2】エムペントリン0.6部、ピナミンフォル
テ0.15部と安定剤D〔4,4’−ブチリデンビス
(3−メチル−6−ターシャリーブチルフェノール)〕
0.3部を用い、実施例1に準じてハエ取線香を得た。
ハエ取線香を吊り下げ線香皿の中に入れ、腰に下げてハ
エの多数発生した畜舎内で作業に従事したが、約6時間
にわたりハエにわずらわされることはなかった。
Example 2 0.6 parts of empentrin, 0.15 parts of pinamine forte and stabilizer D [4,4'-butylidenebis (3-methyl-6-tert-butylphenol)]
Using 0.3 parts, a fly incense stick was obtained according to Example 1.
He placed the fly incense stick in the hanging incense dish, lowered it to his waist, and worked in a barn where a large number of flies had formed, but he did not bother him for about 6 hours.

【0018】[0018]

【発明の効果】本発明は、特定の安定剤を配合すること
により、経時安定性、燻煙時の揮散率、ならびに殺虫効
力にすぐれたエムペントリンハエ取線香を提供する。
The present invention provides an empentrin fly incense stick which is excellent in stability over time, volatilization rate during smoking, and insecticidal effect by blending a specific stabilizer.

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) A01N 53/02 A01N 25/20 A01N 25/22 ──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) A01N 53/02 A01N 25/20 A01N 25/22

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 有効成分としてエムペントリンを0.3
〜2.0重量%含有し、かつ、沸点が250℃以上のジ
−ターシャリーブチル−フェノール系安定剤の1種又は
2種以上を、エムペントリンに対して0.05〜2.0
倍量配合したことを特徴とするハエ取線香。
(1) Empentrin is added as an active ingredient in an amount of 0.3.
One or two or more di-tert-butyl-phenol-based stabilizers having a boiling point of 250 ° C. or more and 0.05 to 2.0% by weight based on empentrin.
A fly incense stick characterized by being blended in twice the amount.
JP4117889A 1992-03-26 1992-03-26 Fly incense stick Expired - Lifetime JP3001169B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP4117889A JP3001169B2 (en) 1992-03-26 1992-03-26 Fly incense stick
CN93101771A CN1044660C (en) 1992-03-26 1993-02-19 A fly-repellent incense

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4117889A JP3001169B2 (en) 1992-03-26 1992-03-26 Fly incense stick

Publications (2)

Publication Number Publication Date
JPH05271018A JPH05271018A (en) 1993-10-19
JP3001169B2 true JP3001169B2 (en) 2000-01-24

Family

ID=14722736

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4117889A Expired - Lifetime JP3001169B2 (en) 1992-03-26 1992-03-26 Fly incense stick

Country Status (2)

Country Link
JP (1) JP3001169B2 (en)
CN (1) CN1044660C (en)

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5675411A (en) * 1979-11-22 1981-06-22 Yoshio Katsuta Method for killing insect
JP2816363B2 (en) * 1989-01-20 1998-10-27 大日本除蟲菊株式会社 Insect repellent

Also Published As

Publication number Publication date
CN1076586A (en) 1993-09-29
JPH05271018A (en) 1993-10-19
CN1044660C (en) 1999-08-18

Similar Documents

Publication Publication Date Title
JP2019147850A (en) Compositions for enhanced acaricidal activity
JP2018065880A5 (en)
JP3909717B1 (en) Flies and mosquito coils
JP2006028173A (en) Preventive/insecticidal composition against unpleasant vermin and preventive/insecticidal method
JP4127721B2 (en) Aedes aegypti or mosquito coils for controlling Aedes aegypti
JP3926836B1 (en) Mosquito coil for infectious disease control mosquito control
JP3001169B2 (en) Fly incense stick
JP3041709B2 (en) Pyrethroid-based compound stabilizer and pyrethroid-based compound stabilization method
JPS60139605A (en) Fumigation composition
KR100305561B1 (en) Smoke extinguishing and heat-insulating insecticides for flies and methods of erasing flies using them
JP4204009B2 (en) Incense stick
CN116076521A (en) Insecticide and method for exterminating pest using the same
JPS5926601B2 (en) Pyrethroid insecticidal composition
JPH05155724A (en) Mosquito-repellent incense
JP2004143151A5 (en)
JP3909716B2 (en) Flies and mosquito coils
JP3044479B2 (en) Sublimable insect repellent, insecticide composition
JPS60136504A (en) Insecticidal composition
JPH05271019A (en) Mosquito-repellent incense
JP2004143151A (en) Fly repellant incense
JPH05255026A (en) Repellent for blood-sucking insect pest
JP2019099519A (en) Pest repellent
JPH10203905A (en) Fly-repellent incense
JP2954965B2 (en) Smoke pest control agent
JPH10167903A (en) Mosquito-repellent incense

Legal Events

Date Code Title Description
R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20071112

Year of fee payment: 8

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20091112

Year of fee payment: 10

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20091112

Year of fee payment: 10

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20101112

Year of fee payment: 11

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20111112

Year of fee payment: 12

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20111112

Year of fee payment: 12

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20121112

Year of fee payment: 13

EXPY Cancellation because of completion of term
FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20121112

Year of fee payment: 13