JP2020105089A - Triacetone triperoxide storage method - Google Patents
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Abstract
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 stable storage method of 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 paper, the ninth and subsequent lines of 2.2. Sample preparation describe the sample preparation procedure. 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。 An alcohol wipe with nothing attached was put in a transparent glass bottle, 1 ml of a 60% methanol/water mixed solution was added thereto, and the lid was capped and sealed with a film. Ultrasonic waves were applied to the transparent glass bottle with an ultrasonic cleaner for 10 minutes to perform extraction. After extraction, the transparent glass bottle 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 transparent glass bottle or a brown glass bottle. 30 μl of a solution in which 30 μg of TATP was dissolved was added to the extract to prepare a sample solution. It is stated that the sample solution in a transparent glass bottle was stored at 20°C (room temperature), 10°C (refrigerator) and -20°C (freezer), and the sample solution stored in a 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 the above [0003] is described in the left column on page 252, the fourth line from the bottom. 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 extract and on wipes under all storage conditions (Figs. 9 and 10 of the article). On the other hand, even in a sample in which a slide glass with TATP attached was sealed 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 because TATP sublimated in the container was deposited on a place other than the slide glass. The method of minimizing the disappearance of the attached TATP due to sublimation/deposition is to store it at an extremely low temperature such as -80°C (Fig. 12 of the paper). From these results, it is described that TATP is preferably stored in a solution or on a moistened cotton swab or 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 used as an explosive substance in recent world terrorist incidents and has been attracting attention. In order to prevent terrorism using TATP, it is effective to detect explosives using guard dogs. In order for guard dogs to detect explosives, training is required to make them smell the substance. TATP must be prepared as a sample in order to train guard dogs to remember the smell of TATP. TATP has a subliming property and begins to decompose at 40 to 50°C.
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 a very sensitive substance in the dry state, with a drop sensitivity of JIS 1 class, a friction sensitivity of JIS 1 class, and an electrostatic sensitivity of 40 to 100 mJ. Due to these properties, it is inappropriate to use TATP itself or a medium with a small amount of TATP attached to train guard dogs, in terms of TATP stability and safety, and handle TATP in a stable and safe state. There is a need for training samples that can It is also desirable that the training sample should have no odor other than the intended product so as not to hinder the 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 the above points, and an object thereof 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の保存方法は、TATPを水に溶解させ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に係る発明において、TATP水溶液を5〜20℃で保存することを特徴とする。
The method for preserving TATP of the invention according to claim 1 is characterized in that TATP is dissolved in water and stored.
The invention according to claim 2 is characterized in that, in the method for preserving TATP of the invention according to claim 1, TATP is dissolved in water at a concentration of 50 to 170 ppm.
The invention according to claim 3 is characterized in that, in the invention according to claim 1 or 2, the TATP aqueous solution is stored at 5 to 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 it becomes difficult for sublimation and decomposition of TATP to maintain stability for a long period of time. In addition, compared to a solution of methanol, which is a deleterious substance as described in Non-Patent Document 1, the aqueous solution is safe, methanol is easily vaporized, and TATP is excessively dissolved. On the other hand, the aqueous solution has the effects of being less likely to vaporize and causing such problems, and being able to retain the odor of TATP alone in the aqueous solution.
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 added to a container, and after proper shaking, the mixture was placed in a refrigerator and allowed to stand overnight. Then, the TATP aqueous solution was filtered to remove undissolved TATP to prepare a TATP aqueous solution. Since TATP has low solubility in water and the concentration of TATP in the solution is low, the TATP aqueous solution can be handled more safely by removing the undissolved portion of TATP by filtration.
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 for several months at a constant temperature, for example, 5° C. within a concentration range of 50 to 170 ppm. Then, the remaining rate of TATP was measured during the storage period.
When preparing a training sample using the TATP aqueous solution obtained as described above, apply it to medical gauze as it is, store it in a plastic bag in a wet state, heat seal and store 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
A flask was charged with 10 mg of TATP and 200 ml of water, and the 50 ppm TATP aqueous solution prepared by the method shown in FIG. 1 was stored in a refrigerator at 5°C. With respect to this stored TATP aqueous solution, the amount of TATP remaining in the aqueous solution was measured every week for 12 weeks. This measurement was performed using 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 could be retained 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 similar to that of Example 1 was prepared except that the TATP aqueous solution had a concentration of 129 ppm and was stored in a refrigerator at 5°C. Then, in the same manner as in Example 1, the remaining amount of TATP was measured every week for 12 weeks by the same measurement method as in Example 1. 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 similar to that of Example 1 was prepared except that the concentration of the TATP aqueous solution was set to 168 ppm and stored in a refrigerator at 5°C. Then, in the same manner as in Example 1, the remaining amount of TATP was measured every week for 12 weeks by the same measurement method as in Example 1. 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 similar to that in Example 1 was prepared except that the TATP aqueous solution had a concentration of 167 ppm, and was stored in a constant temperature bath at 10°C. Then, in the same manner as in Example 1, the remaining amount of TATP was measured every week for 12 weeks by the same measurement method as in Example 1. 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 similar to that of Example 1 was prepared except that the TATP aqueous solution had a concentration of 167 ppm, and was stored in a constant temperature bath at 20°C. Then, in the same manner as in Example 1, the remaining amount of TATP was measured every week for 12 weeks by the same measurement method as in Example 1. 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 similar to that of Example 1 was prepared except that the TATP aqueous solution had a concentration of 129 ppm and was stored in a constant temperature bath at 30°C. Then, in the same manner as in Example 1, the remaining amount of TATP was measured every week for 12 weeks by the same measurement method as in Example 1. 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 shown in Table 1 and FIG. 2, Examples 1-5 stored at 5 to 20° C. had a markedly improved TATP residual rate as compared with 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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| JP2011021145A (en) * | 2009-07-17 | 2011-02-03 | Nec Corp | Treating material for explosive and method for removing the explosive |
Non-Patent Citations (3)
| Title |
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| ANIKO KENDE ET AL: "Trace level triacetone-triperoxide identification with SPME-GC-MS in model systems", MICROCHIM ACTA, vol. 163,, JPN6022023342, 2008, pages 335 - 338, ISSN: 0004792252 * |
| GAMBLE, SALLY C. ET AL: "Detection of trace peroxide explosives in environmental samples using solid phase extraction and liq", ENVIRONMENTAL FORENSICS, vol. 18(1),, JPN6022023343, 2017, pages 50 - 61, ISSN: 0004792253 * |
| RAPP-WRIGHT ET AL: "Suspect screening and quantification of trace organic explosives in wastewater using solid phase ext", JOURNAL OF HAZARDOUS MATERIALS, vol. 329,, JPN6022023344, 2017, pages 11 - 21, ISSN: 0004792254 * |
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