JP7153921B2 - A method for preserving a training sample for a guard dog that can be used for training a guard dog to remember the smell of TATP - Google Patents
A method for preserving a training sample for a guard dog that can be used for training a guard dog to remember the smell of TATP Download PDFInfo
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Description
本発明は、昇華性を有する過酸化物であるトリアセトントリパーオキサイド（Triacetone triperoxide、以下、TATPという）の安定な保存方法に関する。 The present invention relates to a method for stably preserving triacetone triperoxide (hereinafter referred to as TATP), which is a sublimable peroxide.
TATPは、アセトン、過酸化水素、酸を混合・撹拌することで容易に合成できる過酸化物で、下記非特許文献1には、TATPに関する論文が開示されている。その概要は次の通りである。 TATP is a peroxide that can be easily synthesized by mixing and stirring acetone, hydrogen peroxide, and an acid, and Non-Patent Document 1 below discloses a paper on TATP. The outline is as follows.
論文の245頁の2.2. Sample preparationの9行目以降には、試料の調製手順が記載されている。以下にその概要を示す。 On page 245 of the article, 2.2. Sample preparation, line 9 onwards, the sample preparation procedure is described. The outline is shown below.
何も付着していないアルコールワイプを透明なガラス瓶に入れ、1mlの60％メタノール／水混合溶液を加えたのちに蓋をし、フィルムで封をした。その透明ガラス瓶に超音波洗浄機で10分間、超音波を印加し抽出を行った。抽出後透明ガラス瓶を室温に冷却した。ワイプをガラスパスツールピペットの先で叩き、ワイプから抽出液を取出し、溶液を透明ガラス瓶或いは褐色ガラス瓶に移した。その抽出液に30μgのTATPが溶解した溶液30μｌを加えて試料溶液とした。透明ガラス瓶中の試料溶液は20℃（室温）、10℃（冷蔵庫）及び－20℃（冷凍庫）で保存し、褐色ガラス瓶中に保存した試料溶液は20℃で保存したこと等が記載されている。 The free alcohol wipe was placed in a transparent glass bottle, 1 ml of 60% methanol/water mixed solution was added, and the bottle was capped and sealed with a film. Extraction was performed by applying ultrasonic waves to the transparent glass bottle for 10 minutes using an ultrasonic cleaner. After extraction, the clear vial was cooled to room temperature. The wipe was tapped with the tip of a glass Pasteur pipette, the extract was removed from the wipe, and the solution was transferred to a clear or amber glass bottle. A sample solution was prepared by adding 30 µl of a solution in which 30 µg of TATP was dissolved to the extract. It states that the sample solution in the transparent glass bottle was stored at 20°C (room temperature), 10°C (refrigerator), and -20°C (freezer), and that the sample solution in the brown glass bottle was stored at 20°C. .
また252頁左欄、下から4行目以降には、前記〔０００３〕で調製したTATP溶液の安定性について記載されている。以下にその概要を示す。 Further, the stability of the TATP solution prepared in [0003] above is described in the left column on page 252, from the fourth line onwards. The outline is shown below.
TATPは抽出液中とワイプ上では全ての保存条件下で比較的安定である（論文の図9及び図10）。一方でTATPを付着させたスライドガラスをナイロン袋に封入し、ヒートシールしたうえで冷蔵庫内に保存した試料であっても、6日以内にTATPが大きく消失した(論文の図11)。このTATPの急速な消失は、容器内で昇華したTATPが、スライドガラス以外の箇所に沈着したためと推定される。付着したTATPの昇華・沈着による消失を最少に抑える方法は、－80℃のような極低温で保管することである(論文の図12)。これらの結果から、TATPは溶液中又は湿らせた綿棒・ワイプ上での保存が望ましいこと、等が記載されている。 TATP is relatively stable in extracts and on wipes under all storage conditions (Figs. 9 and 10 of the paper). On the other hand, even when the slide glass to which TATP was attached was enclosed in a nylon bag, heat-sealed, and stored in a refrigerator, TATP largely disappeared within 6 days (Fig. 11 of the paper). This rapid disappearance of TATP is presumed to be due to the deposition of TATP sublimed in the container on sites other than the slide glass. A method for minimizing the loss of attached TATP due to sublimation and deposition is to store it at an extremely low temperature such as -80°C (Fig. 12 of the paper). Based on these results, it is described that TATP should preferably be stored in a solution or on a moist cotton swab/wipe.
TATPは、近年世界で発生するテロ事件で爆発性物質として使用され注目されている。TATPを使用したテロを防ぐためには、警備犬を活用した爆発物の探知が有効である。警備犬に爆発物を探知させるには、該当物質の臭いを覚えさせるための訓練が必要である。TATPの臭いを警備犬に覚えさせる訓練をするためには、TATPを試料として用意しなければならないが、TATPは昇華性を有し、40～50℃で分解を開始する。 TATP has been attracting attention as it has been used as an explosive substance in terrorist incidents that have occurred around the world in recent years. In order to prevent terrorism using TATP, it is effective to detect explosives using guard dogs. In order for guard dogs to detect explosives, they must be trained to smell the substance. In order to train a guard dog to remember the smell of TATP, TATP must be prepared as a sample.
TATPはまた、乾燥状態では落槌感度JIS 1級、摩擦感度 JIS 1級、静電気感度40～100mJという極めて鋭敏な物質である。これらの性質から、警備犬の訓練にTATPそのものやTATPを少量付着させた媒体を使用することはTATPの安定性及び安全性の点で不適当であり、TATPを安定かつ安全な状態で取り扱うことができる訓練用試料が求められている。訓練用試料にはまた、訓練に支障をきたさないように、目的物以外の臭いがないことが望まれる。 TATP is also an extremely sensitive substance with JIS class 1 drop sensitivity, JIS class 1 friction sensitivity, and 40-100 mJ static electricity sensitivity in a dry state. Due to these properties, it is inappropriate to use TATP itself or a medium to which a small amount of TATP is attached for the training of guard dogs in terms of the stability and safety of TATP. There is a need for training samples that can Training samples are also desired to be free of extraneous odors so as not to interfere with training.
本発明は、かかる点に鑑みてなされたもので、TATPを安定かつ安全な状態で取り扱う方法を提供することを目的とする。 The present invention has been made in view of this point, and an object of the present invention is to provide a method for handling TATP in a stable and safe state.
請求項１に係る発明のTATPの臭いを警備犬に覚えさせる訓練に用いることが可能な警備犬の訓練用試料の保存方法は、TATPを水に溶解させて得たTATP水溶液を保存し、ガーゼに前記TATP水溶液を塗布して作成した警備犬の訓練用試料を前記TATP水溶液で湿った状態のままビニール袋に収納するとともに該ビニール袋をヒートシールして保存することを特徴とし、
請求項２に係る発明は、請求項１に係る発明のTATPの臭いを警備犬に覚えさせる訓練に用いることが可能な警備犬の訓練用試料の保存方法において、TATPを水に50～170ppmの濃度に溶解させることを特徴とする。
請求項３に係る発明は、請求項１または２に係る発明のTATPの臭いを警備犬に覚えさせる訓練に用いることが可能な警備犬の訓練用試料の保存方法において、前記TATP水溶液を5～20℃で保存することを特徴とする。
The method for preserving a sample for training a guard dog that can be used for training a guard dog to remember the smell of TATP according to the invention according to claim 1 comprises preserving an aqueous solution of TATP obtained by dissolving TATP in water and gauze. The guard dog training sample prepared by applying the TATP aqueous solution to the above is placed in a plastic bag while it is moistened with the TATP aqueous solution, and the plastic bag is heat-sealed and stored.
The invention according to claim 2 is a method for preserving a sample for training a guard dog that can be used for training a guard dog to remember the smell of TATP according to the invention according to claim 1, wherein TATP is added to water at a concentration of 50 to 170 ppm. It is characterized by dissolving in concentration.
The invention according to claim 3 is a method for preserving a sample for training a guard dog that can be used for training a guard dog to remember the smell of TATP according to the invention according to claim 1 or 2, wherein It is characterized by being stored at 20°C.
本発明によると、TATPを水に溶解させることにより、安全性に富み、TATPが昇華・分解し難くなって安定性を長期間にわたって持続させることができる。また非特許文献１に記載されるような劇物であるメタノールの溶液と比べても、水溶液は安全であること、メタノールは気化し易いうえ、TATPが溶け過ぎるため、TATPが析出し易く危険であるのに対し、水溶液は気化し難く、こうした問題を生じ難いこと、水溶液ではTATPのみの臭いを保持させることができること、等の効果を有する。 According to the present invention, by dissolving TATP in water, it is highly safe and TATP is less likely to sublimate and decompose, and stability can be maintained over a long period of time. In addition, compared to the solution of methanol, which is a deleterious substance as described in Non-Patent Document 1, the aqueous solution is safe, methanol is easy to vaporize, and TATP is too dissolved, so TATP is easy to precipitate and dangerous. On the other hand, the aqueous solution is difficult to evaporate, so it is difficult to cause such a problem, and the aqueous solution can retain the odor of TATP alone.
図１に示すように、容器にTATPと、水を入れ、適度に振り混ぜたのち、冷蔵庫に入れ一晩静置させた。その後TATP水溶液をろ過し、未溶解のTATPを除去してTATP水溶液を作成した。TATPは水への溶解度が低く、溶液のTATP濃度は低いため、TATPの未溶解分をろ過して取り除くことにより、TATP水溶液をより安全に取り扱うことができる。 As shown in FIG. 1, TATP and water were placed in a container, shaken moderately, and then placed in a refrigerator and allowed to stand overnight. After that, the TATP aqueous solution was filtered to remove undissolved TATP to prepare a TATP aqueous solution. Since TATP has a low solubility in water and the concentration of TATP in the solution is low, removing the undissolved TATP by filtration makes it possible to handle the TATP aqueous solution more safely.
図１に示すようにして作成したTATP水溶液は、濃度50～170ppmの範囲内で、一定温度、例えば5℃で数か月間保存した。そして保存期間中、TATPの残存率を測定した。
以上のようにして得たTATP水溶液を用い、訓練用試料を作成するときは、そのまま医療用ガーゼに塗布し、湿った状態のままビニール袋に収納し、ヒートシールして使用時まで保存される。
The TATP aqueous solution prepared as shown in FIG. 1 was stored at a constant temperature, eg, 5° C., for several months within a concentration range of 50 to 170 ppm. Then, the residual rate of TATP was measured during the storage period.
When preparing a training sample using the TATP aqueous solution obtained as described above, it is applied to medical gauze as it is, placed in a wet plastic bag, heat-sealed, and stored until use. .
実施例１
フラスコにTATP10mgと、水200mｌを入れ、図1に示す方法で作成した50ppmのTATP水溶液を5℃の冷蔵庫で保存した。この保存したTATP水溶液について、各週ごとに12週間にわたって水溶液中のTATP残存量を測定した。この測定は、株式会社島津製作所の高速液体クロマトグラフィー（UHPLC/HPLC System）を用いて行った。測定結果を表1及び図２に示す。表1及び図２に示されるように、12週間経過後もTATPを90.9％残存させることができた。
Example 1
10 mg of TATP and 200 ml of water were placed in a flask, and the 50 ppm TATP aqueous solution prepared by the method shown in Fig. 1 was stored in a refrigerator at 5°C. For this preserved TATP aqueous solution, the amount of TATP remaining in the aqueous solution was measured every week for 12 weeks. This measurement was performed using a high-performance liquid chromatography (UHPLC/HPLC System) manufactured by Shimadzu Corporation. The measurement results are shown in Table 1 and FIG. As shown in Table 1 and FIG. 2, 90.9% of TATP was able to remain even after 12 weeks.
実施例２
TATP水溶液の濃度を129ppmとした以外は実施例１と同様の水溶液を作成し、5℃の冷蔵庫で保存した。そして実施例1と同様、各週ごとに12週間にわたってTATP残存量を実施例１と同様の測定方法により測定した。結果を表１及び図２に示す。この実施例においては、12週間経過後のTATP残存率は82.0％であった。
実施例３
TATP水溶液の濃度を168ppmとした以外は実施例１と同様の水溶液を作成し、5℃の冷蔵庫で保存した。そして実施例1と同様、各週ごとに12週間にわたってTATP残存量を実施例１と同様の測定方法により測定した。結果を表１及び図２に示す。この実施例においては、12週間経過後のTATP残存率は80.6％であった。
実施例４
TATP水溶液の濃度を167ppmとした以外は実施例１と同様の水溶液を作成し、10℃の恒温槽で保存した。そして実施例1と同様、各週ごとに12週間にわたってTATP残存量を実施例１と同様の測定方法により測定した。結果を表１及び図２に示す。この実施例においては、12週間経過後のTATP残存率は75.2％であった。
実施例５
TATP水溶液の濃度を167ppmとした以外は実施例１と同様の水溶液を作成し、20℃の恒温槽で保存した。そして実施例1と同様、各週ごとに12週間にわたってTATP残存量を実施例１と同様の測定方法により測定した。結果を表１及び図２に示す。この実施例においては、12週間経過後のTATP残存率は66.2％であった。
比較例
TATP水溶液の濃度を129ppmとした以外は実施例１と同様の水溶液を作成し、30℃の恒温槽で保存した。そして実施例1と同様、各週ごとに12週間にわたってTATP残存量を実施例１と同様の測定方法により測定した。結果を表１及び図２に示す。この比較例においては、12週間経過後のTATP残存率は31.7％となった。
Example 2
An aqueous solution was prepared in the same manner as in Example 1 except that the concentration of the TATP aqueous solution was 129 ppm, and stored in a refrigerator at 5°C. Then, as in Example 1, the residual TATP amount was measured by the same measurement method as in Example 1 every week for 12 weeks. The results are shown in Table 1 and FIG. In this example, the TATP residual rate after 12 weeks was 82.0%.
Example 3
An aqueous solution was prepared in the same manner as in Example 1, except that the concentration of the TATP aqueous solution was changed to 168 ppm, and stored in a refrigerator at 5°C. Then, as in Example 1, the residual TATP amount was measured by the same measurement method as in Example 1 every week for 12 weeks. The results are shown in Table 1 and FIG. In this example, the TATP residual rate after 12 weeks was 80.6%.
Example 4
An aqueous solution was prepared in the same manner as in Example 1, except that the concentration of the TATP aqueous solution was changed to 167 ppm, and stored in a constant temperature bath at 10°C. Then, as in Example 1, the residual TATP amount was measured by the same measurement method as in Example 1 every week for 12 weeks. The results are shown in Table 1 and FIG. In this example, the TATP residual rate after 12 weeks was 75.2%.
Example 5
An aqueous solution was prepared in the same manner as in Example 1 except that the concentration of the TATP aqueous solution was changed to 167 ppm, and stored in a constant temperature bath at 20°C. Then, as in Example 1, the residual TATP amount was measured by the same measurement method as in Example 1 every week for 12 weeks. The results are shown in Table 1 and FIG. In this example, the TATP residual rate after 12 weeks was 66.2%.
Comparative example
An aqueous solution was prepared in the same manner as in Example 1 except that the concentration of the TATP aqueous solution was changed to 129 ppm, and stored in a constant temperature bath at 30°C. Then, as in Example 1, the residual TATP amount was measured by the same measurement method as in Example 1 every week for 12 weeks. The results are shown in Table 1 and FIG. In this comparative example, the TATP residual rate after 12 weeks was 31.7%.
表1及び図２に見られるように、5～20℃で保存した実施例１－５は比較例に比べTATP残存率が格段に向上した。
As seen in Table 1 and FIG. 2, Examples 1-5 stored at 5 to 20° C. showed a markedly improved TATP retention rate compared to Comparative Examples.
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| JP2011021145A (en) | 2009-07-17 | 2011-02-03 | Nec Corp | Treating material for explosive and method for removing the explosive |
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| Aniko Kende et al，Trace level triacetone-triperoxide identification with SPME-GC-MS in model systems，Microchim Acta ，2008年，163,，335-338 |
| Gamble, Sally C. et al，Detection of trace peroxide explosives in environmental samples using solid phase extraction and liquid chromatography mass spectrometry，Environmental Forensics，2017年，18(1),，50-61 |
| Rapp-Wright et al，Suspect screening and quantification of trace organic explosives in wastewater using solid phase extraction and liquid chromatography-high resolution accurate mass spectrometry，Journal of Hazardous Materials ，2017年，329,，11-21 |
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