JP2006204398A - Liquid for detecting fingerprint, its manufacturing method, and method for detecting fingerprint by using it - Google Patents
Liquid for detecting fingerprint, its manufacturing method, and method for detecting fingerprint by using it Download PDFInfo
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本発明は、鑑識技術分野において指紋を含む検体から潜在指紋を検出するための、ニンヒドリンを含有する指紋検出用液、前記指紋検出用液の製造方法および前記指紋検出用液を用いた指紋検出方法に関する。 The present invention relates to a fingerprint detection liquid containing ninhydrin, a method for manufacturing the fingerprint detection liquid, and a fingerprint detection method using the fingerprint detection liquid for detecting a latent fingerprint from a specimen containing a fingerprint in the field of identification technology. About.
従来、指紋検出方法としては、（１）アルミニウム系の銀色粉末、銅系の金色粉末、カーボン系の黒色粉末、またはその他の白色粉末もしくは有色粉末を用いて、検体に付着した分泌物中の水分および脂肪分に前記粉末を付着させ、検体の背景色と粉末の色との色相差を利用して検出する方法、（２）検体を乾燥させた後に分泌物中の脂肪分をヨウ素ガスと反応させ、呈色させて検出する方法等が知られている。 Conventional fingerprint detection methods include: (1) moisture in the secretions attached to the specimen using aluminum-based silver powder, copper-based gold powder, carbon-based black powder, or other white or colored powder. And the method of detecting by utilizing the hue difference between the background color of the specimen and the color of the powder, and (2) reacting the fat in the secretion with iodine gas after the specimen is dried And a method for detecting the color and the like is known.
また、紙等に付着した指紋を検出するための従来の方法として、（３）ニンヒドリンを用いる方法が一般に用いられている。この方法は、人体の汗に含まれるアミノ酸がニンヒドリンと反応して紫色に発色することを利用したものである。
新聞紙、リポート用紙、上質紙等の普通紙に付着した指紋を検出する場合には、従来、ケトン類、アルコール類等の有機溶剤を溶媒とするニンヒドリン溶液に指紋の付着した普通紙を浸せきさせる方法、普通紙に前記ニンヒドリン溶液をハケ等で塗布する方法、普通紙に前記ニンヒドリン溶液を噴霧して均一に塗布する方法等により、普通紙に十分な量の溶液を染み込ませ、その後、加熱処理を施すことによって発色反応を促進させていた。
Further, as a conventional method for detecting a fingerprint attached to paper or the like, (3) a method using ninhydrin is generally used. This method utilizes the fact that an amino acid contained in human sweat reacts with ninhydrin and develops a purple color.
When detecting fingerprints adhering to plain paper such as newspaper, report paper, fine paper, etc., a conventional method of immersing plain paper with fingerprints in a ninhydrin solution using an organic solvent such as ketones or alcohols as a solvent. A method of applying the ninhydrin solution on plain paper with a brush or the like, or spraying the ninhydrin solution on plain paper and applying it uniformly, etc., soaks a sufficient amount of the solution into plain paper, and then heat treatment. The coloring reaction was promoted by applying.
上記（３）のニンヒドリンを用いる方法によれば、指紋がにじまずにくっきりと検出できるが、以下のような問題があった。
即ち、ニンヒドリンは、アルコール類、ケトン類等の極性溶剤には溶解するが、通常のハイドロカーボン等の無極性溶剤には溶解しない。そのため、ニンヒドリンを用いる方法においては、極性を有する有機溶剤にニンヒドリンを溶解させ、それをもとに調製した指紋検出用液を使用することになる。
その結果、普通紙に油性ボールペン等で文字が書かれていた場合には、ニンヒドリン溶液に含有される有機溶剤によって指紋の検出に悪影響が出るばかりでなく、筆跡鑑定等の指紋以外に得られるべき有力な情報にも損傷を与えることになる。また、感熱紙等の紙に対して用いる場合、極性有機溶媒や熱による変質が生じ、表面がすぐに黒っぽく変色してしまうことから、指紋の検出が困難となってしまう。
According to the method (3) using ninhydrin, fingerprints can be clearly detected without blurring, but there are the following problems.
That is, ninhydrin dissolves in polar solvents such as alcohols and ketones, but does not dissolve in nonpolar solvents such as ordinary hydrocarbons. Therefore, in the method using ninhydrin, a ninhydrin is dissolved in a polar organic solvent, and a fingerprint detection solution prepared based on the ninhydrin is used.
As a result, when characters are written on plain paper with an oil-based ballpoint pen, etc., the organic solvent contained in the ninhydrin solution not only adversely affects fingerprint detection, but should be obtained in addition to fingerprints such as handwriting appraisal. It will also damage valuable information. In addition, when used on paper such as thermal paper, alteration due to a polar organic solvent or heat occurs, and the surface immediately changes to blackish color, which makes fingerprint detection difficult.
これらの問題を解決することを目的とした手法として、ハイドロフルオロエーテルとニンヒドリンと水とを含む指紋検出用溶液を用いることが知られている（特許文献１参照。）。
特許文献１には、ハイドロフルオロエーテルの具体例として、（パーフルオロブトキシ）メタン、（パーフルオロブトキシ）エタン、および１−エトキシ−１，１，２，２−テトラフルオロエタンが記載されており、これらのハイドロフルオロエーテルに溶解する水によりニンヒドリンを溶解して指紋検出用溶剤とするという手法が記載されている。
As a technique for solving these problems, it is known to use a fingerprint detection solution containing hydrofluoroether, ninhydrin, and water (see Patent Document 1).
Patent Document 1 describes (perfluorobutoxy) methane, (perfluorobutoxy) ethane, and 1-ethoxy-1,1,2,2-tetrafluoroethane as specific examples of hydrofluoroethers, A technique is described in which ninhydrin is dissolved with water dissolved in these hydrofluoroethers to form a solvent for fingerprint detection.
しかしながら、特許文献１に記載されている、（パーフルオロブトキシ）メタンおよび（パーフルオロブトキシ）エタンは、飽和水分濃度がそれぞれ９５ｐｐｍおよび９２ｐｐｍと低い（（パーフルオロブトキシ）メタンの例である米国３Ｍ社製のＨＦＥ−７１００および（パーフルオロブトキシ）エタンの例である米国３Ｍ社製のＨＦＥ−７２００についての米国３Ｍ社商品カタログ（１９９８年）参照。）。したがって、水分が飽和したそれぞれの溶剤にニンヒドリンを混合しても、混合した溶剤に含まれるニンヒドリンの濃度が低くなってしまう。その結果、はっきりした指紋を検出するためには、指紋が付着した普通紙、感熱紙等の検体と前記指紋検出用溶液との接触時間を長くする必要があった。また、接触時間が長くなるため、指紋のにじみ、感熱紙の変色、指紋以外の文字等の情報のにじみや消失等が発生しうるという問題があった。 However, (perfluorobutoxy) methane and (perfluorobutoxy) ethane described in Patent Document 1 have a low saturated water concentration of 95 ppm and 92 ppm, respectively, which is an example of ((perfluorobutoxy) methane. (See US 3M product catalog (1998) for HFE-7100 made by 3M USA, which is an example of HFE-7100 and (perfluorobutoxy) ethane).) Therefore, even if ninhydrin is mixed with each solvent saturated with water, the concentration of ninhydrin contained in the mixed solvent is lowered. As a result, in order to detect a clear fingerprint, it is necessary to lengthen the contact time between a specimen such as plain paper or thermal paper to which the fingerprint is attached and the fingerprint detection solution. In addition, since the contact time becomes longer, there are problems such as fingerprint bleeding, discoloration of thermal paper, and bleeding or disappearance of information such as characters other than fingerprints.
また、特許文献１に記載されている、１−エトキシ−１，１，２，２−テトラフルオロエタンは、タグ密閉式の引火点測定法において−１４℃という低い引火性を有するため、発色の促進のための加温などに特別な注意が必要で、取扱いが煩雑であった。 In addition, 1-ethoxy-1,1,2,2-tetrafluoroethane described in Patent Document 1 has a low flammability of −14 ° C. in a tag-sealed flash point measurement method, and therefore has a color development. Special care was required for warming for promotion and the handling was complicated.
そこで、本発明は、普通紙や感熱紙の潜在指紋の検出に使用することができるニンヒドリンを含有する指紋検出用液であって、検体との接触時間が短く、指紋のにじみ、感熱紙の変色、指紋以外の文字等の情報のにじみや消失等が発生せず、取扱いが容易な、指紋検出用液を提供することを目的とする。
また、本発明は、前記指紋検出用液を効率的に製造する方法および前記指紋検出用液を用いた指紋検出方法を提供することを更なる目的とする。
Therefore, the present invention is a fingerprint detection liquid containing ninhydrin that can be used for detection of latent fingerprints on plain paper and thermal paper, has a short contact time with a specimen, smears fingerprints, and discolors thermal paper. Another object of the present invention is to provide a fingerprint detection liquid that is easy to handle without causing bleeding or disappearance of information such as characters other than fingerprints.
Another object of the present invention is to provide a method for efficiently producing the fingerprint detection liquid and a fingerprint detection method using the fingerprint detection liquid.
本発明者は、上記目的を達成すべく鋭意研究した結果、ハイドロフルオロエーテルの１種である１−（２，２，２−トリフルオロエトキシ）−１，１，２，２−テトラフルオロエタン（以下、便宜上、別名の「ＨＦＥ−３４７」を用いる場合がある。）が、以下の性質を有することを見出した。
即ち、（ａ）ＨＦＥ−３４７は、比較的小さい極性を有するため、インク等を溶解させないので、普通紙に書かれた文字に影響を与えない。（ｂ）ＨＦＥ−３４７は、単独ではニンヒドリンをほとんど溶解させないが、水を含有する場合には十分な濃度で溶解させる。（ｃ）その場合、含有される水が、ＨＦＥ−３４７から遊離しない限り、即ち、ＨＦＥ−３４７の飽和水分濃度を超えない限り、水を含有するＨＦＥ−３４７（以下「含水ＨＦＥ−３４７」ともいう。）は、感熱紙に影響せず、また、普通紙について指紋以外の有力情報に損傷を与えない。（ｄ）ＨＦＥ−３４７は、引火点を持たない不燃性であり、また、飽和水分濃度が比較的高い。
本発明者は、上記知見に基づき、本発明を完成させた。
As a result of earnest research to achieve the above object, the present inventor has found that 1- (2,2,2-trifluoroethoxy) -1,1,2,2-tetrafluoroethane (which is a kind of hydrofluoroether) Hereinafter, for the sake of convenience, the alias “HFE-347” may be used.)) Has the following properties.
That is, (a) HFE-347 has a relatively small polarity and does not dissolve ink or the like, so that it does not affect characters written on plain paper. (B) HFE-347 alone hardly dissolves ninhydrin, but dissolves it at a sufficient concentration when it contains water. (C) In that case, unless the contained water is liberated from HFE-347, that is, unless the saturated water concentration of HFE-347 is exceeded, HFE-347 containing water (hereinafter also referred to as “hydrous HFE-347”) Does not affect the thermal paper and does not damage the leading information other than fingerprints on plain paper. (D) HFE-347 is nonflammable without a flash point and has a relatively high saturated water concentration.
The present inventor completed the present invention based on the above findings.
即ち、本発明は、以下の（１）〜（１０）を提供する。 That is, the present invention provides the following (1) to (10).
（１）１−（２，２，２−トリフルオロエトキシ）−１，１，２，２−テトラフルオロエタンと、ニンヒドリンと、水とを含有する指紋検出用液。 (1) A fingerprint detection liquid containing 1- (2,2,2-trifluoroethoxy) -1,1,2,2-tetrafluoroethane, ninhydrin, and water.
（２）前記水の含有量が３００ｐｐｍ以上である上記（１）に記載の指紋検出用液。 (2) The fingerprint detection liquid according to (1), wherein the water content is 300 ppm or more.
（３）前記ニンヒドリンの含有量が２０ｐｐｍ以上である上記（１）または（２）に記載の指紋検出用液。 (3) The liquid for fingerprint detection according to (1) or (2), wherein the content of the ninhydrin is 20 ppm or more.
（４）水を含有する１−（２，２，２−トリフルオロエトキシ）−１，１，２，２−テトラフルオロエタンに、ニンヒドリンを溶解させて、上記（１）〜（３）のいずれかに記載の指紋検出用液を得る、指紋検出用液の製造方法。 (4) Any one of (1) to (3) above, wherein ninhydrin is dissolved in 1- (2,2,2-trifluoroethoxy) -1,1,2,2-tetrafluoroethane containing water. A method for producing a fingerprint detection liquid, wherein the fingerprint detection liquid is obtained.
（５）上記（１）〜（３）のいずれかに記載の指紋検出用液を被検体に接触させる接触工程と、その後、前記被検体を乾燥させる乾燥工程とを具備する、指紋検出方法。 (5) A fingerprint detection method comprising: a contact step of bringing the fingerprint detection liquid according to any one of (1) to (3) above into contact with a subject; and a drying step of drying the subject.
（６）前記接触工程おいて、前記指紋検出用液に前記被検体を浸せきさせることにより接触させる、上記（５）に記載の指紋検出方法。 (6) The fingerprint detection method according to (5), wherein in the contacting step, the subject is contacted by immersing the subject in the fingerprint detection liquid.
（７）前記接触工程および前記乾燥工程を繰り返し行う上記（５）または（６）に記載の指紋検出方法。 (7) The fingerprint detection method according to (5) or (6), wherein the contact step and the drying step are repeated.
（８）繰り返し回数が３回以上である上記（７）に記載の指紋検出方法。 (8) The fingerprint detection method according to (7), wherein the number of repetitions is three or more.
（９）前記被検体を前記指紋検出用液に浸せきさせる時間が１回あたり０．５〜５秒である上記（７）または（８）に記載の指紋検出方法。 (9) The fingerprint detection method according to (7) or (8), wherein the time for immersing the subject in the fingerprint detection liquid is 0.5 to 5 seconds per time.
（１０）前記指紋検出用液の温度が４０℃以上である上記（７）〜（９）のいずれかに記載の指紋検出方法。 (10) The fingerprint detection method according to any one of (7) to (9), wherein the temperature of the fingerprint detection liquid is 40 ° C. or higher.
本発明の指紋検出用液は、普通紙や感熱紙の潜在指紋の検出に際し、検体との接触時間が短く、指紋のにじみ、感熱紙の変色、指紋以外の文字等の情報のにじみや消失等が発生しない。また、本発明の指紋検出用液は、原料として用いられるＨＦＥ−３４７が不燃性であるため、取扱いが容易である。 The liquid for detecting a fingerprint of the present invention has a short contact time with a specimen when detecting a latent fingerprint on plain paper or thermal paper, and blots of fingerprints, discoloration of thermal paper, blurring or disappearance of information such as characters other than fingerprints, etc. Does not occur. Further, the fingerprint detection liquid of the present invention is easy to handle because HFE-347 used as a raw material is nonflammable.
以下、本発明を詳細に説明する。
本発明の指紋検出用液は、ＨＦＥ−３４７と、ニンヒドリンと、水とを含有する。
ＨＦＥ−３４７は、水素原子、フッ素原子、炭素原子および酸素原子を含むハイドロフルオロエーテルの１種である。ＨＦＥ−３４７は、沸点が５６℃、凝固点が−９４℃であり、２５℃における水分飽和濃度が質量基準で９００ｐｐｍであり、引火点や空気との混合ガスが爆発範囲を持たない不燃性の溶剤である。
Hereinafter, the present invention will be described in detail.
The fingerprint detection liquid of the present invention contains HFE-347, ninhydrin, and water.
HFE-347 is one type of hydrofluoroether containing a hydrogen atom, a fluorine atom, a carbon atom, and an oxygen atom. HFE-347 has a boiling point of 56 ° C., a freezing point of −94 ° C., a water saturation concentration at 25 ° C. of 900 ppm on a mass basis, and a nonflammable solvent whose flash point or mixed gas with air does not have an explosion range. It is.
本発明の指紋検出用液においては、水の含有量が１００ｐｐｍ以上であるのが好ましく、３００ｐｐｍ以上であるのがより好ましい。
ニンヒドリンは、ＨＦＥ−３４７自体にはほとんど溶解しないが、含水ＨＦＥ−３４７には溶解する。また、ニンヒドリンの溶解しうる量は、ＨＦＥ−３４７中の水の含有量が高いほど、多くなる。
本発明の指紋検出用液における水の含有量が上記範囲であると、後述するニンヒドリンの含有量を十分に多くすることができる。
水の含有量は、上限を特に限定されないが、ＨＦＥ−３４７の飽和濃度以下であるのが好ましい。即ち、含有される水が、ＨＦＥ−３４７から遊離しないのが好ましい。
In the fingerprint detection liquid of the present invention, the water content is preferably 100 ppm or more, and more preferably 300 ppm or more.
Ninhydrin hardly dissolves in HFE-347 itself, but dissolves in hydrous HFE-347. The amount of ninhydrin that can be dissolved increases as the water content in HFE-347 increases.
When the content of water in the fingerprint detection liquid of the present invention is in the above range, the content of ninhydrin described later can be sufficiently increased.
The upper limit of the water content is not particularly limited, but it is preferably not higher than the saturation concentration of HFE-347. That is, it is preferable that the contained water is not liberated from HFE-347.
本発明の指紋検出用液においては、ニンヒドリンの含有量が１０ｐｐｍ以上であるのが好ましく、２０ｐｐｍ以上であるのがより好ましい。
本発明の指紋検出用液におけるニンヒドリンの含有量が上記範囲であると、検体との接触時間を短くすることができ、指紋のにじみ、感熱紙の変色、指紋以外の文字等の情報のにじみや消失等が発生を防止することができ、潜在指紋を鮮明に発色させることができる。
ニンヒドリンの含有量は、上限を特に限定されないが、含水ＨＦＥ−３４７の飽和濃度以下であるのが好ましい。即ち、含有されるニンヒドリンが、含水ＨＦＥ−３４７から遊離しないのが好ましい。
In the fingerprint detection liquid of the present invention, the ninhydrin content is preferably 10 ppm or more, and more preferably 20 ppm or more.
When the content of ninhydrin in the fingerprint detection liquid of the present invention is in the above range, the contact time with the specimen can be shortened, and fingerprint bleeding, thermal paper discoloration, information bleeding such as characters other than fingerprints, The disappearance can be prevented and the latent fingerprint can be clearly colored.
The upper limit of the content of ninhydrin is not particularly limited, but is preferably equal to or lower than the saturated concentration of hydrous HFE-347. That is, it is preferable that the contained ninhydrin is not released from the hydrous HFE-347.
本発明の指紋検出用液は、通常は、他の極性有機溶剤を含有しないのが好ましいが、ニンヒドリンの溶解度を更に高めるために、感熱紙を変色させずインク等で書かれた筆跡に影響を与えない濃度で、他の極性有機溶剤を含有することもできる。
他の極性有機溶剤としては、例えば、ケトン類、アルコール類が挙げられる。その含有量は、５０００ｐｐｍ以下であるのが好ましく、５００ｐｐｍ以下であるのがより好ましい。
In general, the fingerprint detection liquid of the present invention preferably contains no other polar organic solvent, but in order to further increase the solubility of ninhydrin, it does not discolor the thermal paper and affects the handwriting written with ink or the like. Other polar organic solvents can also be included at concentrations not given.
Examples of other polar organic solvents include ketones and alcohols. The content is preferably 5000 ppm or less, and more preferably 500 ppm or less.
本発明の指紋検出用液は、製造方法を特に限定されないが、本発明の指紋検出用液の製造方法により好適に製造される。即ち、含水ＨＦＥ−３４７に、ニンヒドリンを溶解させて、指紋検出用液を得る方法が好ましい。以下、より詳細に説明する。
含水ＨＦＥ−３４７は、ＨＦＥ−３４７に水を添加することにより得ることができる。添加される水は、特に限定されないが、有機溶剤、酸、アルカリ等を含有しないものが好ましく、蒸留水または限外ろ過等の処理を施した純水がより好ましい。
また、水の添加後にかくはん、振とうなどを行うのが好ましい。それにより、ＨＦＥ−３４７の水分濃度を高めることができる。
The manufacturing method of the fingerprint detection liquid of the present invention is not particularly limited, but is preferably manufactured by the fingerprint detection liquid manufacturing method of the present invention. That is, a method for obtaining a fingerprint detection liquid by dissolving ninhydrin in hydrous HFE-347 is preferable. This will be described in more detail below.
The hydrous HFE-347 can be obtained by adding water to HFE-347. The water to be added is not particularly limited, but preferably does not contain an organic solvent, acid, alkali or the like, and more preferably distilled water or pure water subjected to treatment such as ultrafiltration.
Moreover, it is preferable to perform stirring, shaking, etc. after addition of water. Thereby, the water concentration of HFE-347 can be increased.
ＨＦＥ−３４７の飽和水分濃度は、温度を調節することにより制御することができる。ＨＦＥ−３４７の飽和水分濃度は、高温であるほど高くなるが、指紋検出用液を使用する際の温度が低いと、含有されている水が遊離する場合があるため、使用温度に近い温度でＨＦＥ−３４７に水を添加して溶解させるのが好ましい。 The saturated water concentration of HFE-347 can be controlled by adjusting the temperature. The saturated water concentration of HFE-347 increases as the temperature increases. However, if the temperature when using the fingerprint detection liquid is low, the contained water may be liberated. It is preferable to dissolve HFE-347 by adding water.
上述した含水ＨＦＥ−３４７に、ニンヒドリンを溶解させて、指紋検出用液が得られる。この際、含水ＨＦＥ−３４７の沸点以下の温度に加温することにより、ニンヒドリンの溶解速度を高めることができる。
溶解の時間は、長いほど（例えば、一晩）ニンヒドリンの溶解量を多くすることができるが、通常、３０分程度で、指紋の検出に十分な溶解量にすることができる。
また、ニンヒドリンを過剰に添加し、溶解せずに残った固形のニンヒドリンをろ過等により除去することもできる。
Ninhydrin is dissolved in the above-mentioned hydrous HFE-347 to obtain a fingerprint detection liquid. At this time, the dissolution rate of ninhydrin can be increased by heating to a temperature not higher than the boiling point of hydrous HFE-347.
The longer the dissolution time (for example, overnight), the greater the amount of ninhydrin dissolved. However, in general, the amount of dissolution can be sufficient for fingerprint detection in about 30 minutes.
Further, ninhydrin can be added excessively, and solid ninhydrin remaining without being dissolved can be removed by filtration or the like.
本発明の指紋検出用液は、例えば、以下の指紋検出方法に用いることができる。即ち、本発明の指紋検出用液を被検体に接触させる接触工程と、その後、前記被検体を乾燥させる乾燥工程とを具備する、指紋検出方法である。 The fingerprint detection liquid of the present invention can be used, for example, in the following fingerprint detection method. That is, it is a fingerprint detection method comprising a contact step of bringing the fingerprint detection liquid of the present invention into contact with a subject, and then a drying step of drying the subject.
被検体としては、例えば、普通紙、感熱紙が挙げられる。 Examples of the subject include plain paper and thermal paper.
接触工程おいて、本発明の指紋検出用液を被検体に接触させる方法は、特に限定されない。例えば、本発明の指紋検出用液に被検体を浸せきさせる方法、本発明の指紋検出用液を被検体に刷毛等で塗布する方法、本発明の指紋検出用液をスプレー等により噴霧して被検体に塗布する方法が挙げられる。
中でも、本発明の指紋検出用液に被検体を浸せきさせる方法が、最も一般的な操作であり、好ましい。この方法において、被検体を本発明の指紋検出用液に浸せきさせる時間は、５秒〜１分であるのが好ましい。なお、後述する浸せきを繰り返し行う場合においては、浸せき時間の合計が上記範囲になるのが好ましい。
In the contacting step, the method for bringing the fingerprint detection liquid of the present invention into contact with the subject is not particularly limited. For example, a method of immersing the subject in the fingerprint detection liquid of the present invention, a method of applying the fingerprint detection liquid of the present invention to the subject with a brush or the like, and spraying the fingerprint detection liquid of the present invention by a spray or the like. The method of apply | coating to a test substance is mentioned.
Among them, the method of immersing the subject in the fingerprint detection liquid of the present invention is the most common operation and is preferable. In this method, the time for immersing the subject in the fingerprint detection liquid of the present invention is preferably 5 seconds to 1 minute. In the case where immersion described later is repeated, the total immersion time is preferably in the above range.
接触工程の後、湿潤状態になった被検体を乾燥させる乾燥工程を行う。例えば、本発明の指紋検出用液に被検体を浸せきさせる方法においては、浸せき後、引き上げて乾燥させる。
本発明に用いられる含水ＨＦＥ−３４７は、揮散しやすいため、湿潤状態になった被検体は、室温でも容易に乾燥させることができる。
After the contacting step, a drying step is performed for drying the wet specimen. For example, in the method of immersing a subject in the fingerprint detection liquid of the present invention, the specimen is lifted and dried after immersion.
Since the hydrous HFE-347 used in the present invention is easily volatilized, the wet specimen can be easily dried even at room temperature.
更に、乾燥工程の後、被検体を加温する加温工程を具備するのが好ましい態様の一つである。これにより、指紋が発色するまでの時間を短縮することができる。加温温度は、特に限定されないが、被検体が感熱紙である場合は、変色を防止するために４０〜６０℃程度に調整するのが好ましい。 Furthermore, it is one of the preferable embodiments that a heating step for heating the subject is provided after the drying step. Thereby, it is possible to shorten the time until the fingerprint is colored. The heating temperature is not particularly limited, but when the subject is thermal paper, it is preferably adjusted to about 40 to 60 ° C. in order to prevent discoloration.
本発明においては、上述した接触工程および乾燥工程を含む手順を繰り返し行うのが好ましい態様の一つである。その場合、上記手順の繰り返し後に、加温工程を行うのが好ましい。また、上述した接触工程、乾燥工程および加温工程を含む手順を繰り返し行うのも好ましい態様の一つである。
中でも、本発明の指紋検出用液に被検体を浸せきさせ、その後、引き上げて乾燥させる手順を繰り返し行うのが好ましい。この際、指紋の発色の程度を観察しながら、繰り返し回数を決定することができる。
上記手順を繰り返し行うことにより、本発明の指紋検出用液に含有されるニンヒドリンが被検体の指紋と繰り返し接触し、その結果、指紋の発色が促進され、また、発色の鮮明度が向上する。本発明の指紋検出用液は、指紋の発色が短時間に起こるので、このような手順を繰り返しても、指紋検出にかかる時間は十分に短くなる。
In the present invention, it is one of the preferred embodiments that the procedure including the contact step and the drying step described above is repeated. In that case, it is preferable to perform the heating step after repeating the above procedure. Moreover, it is also one of the preferable aspects to repeat the procedure including the contact process, the drying process, and the heating process described above.
In particular, it is preferable to repeat the procedure of immersing the subject in the fingerprint detection liquid of the present invention and then pulling it up and drying. At this time, the number of repetitions can be determined while observing the degree of color development of the fingerprint.
By repeating the above procedure, the ninhydrin contained in the fingerprint detection liquid of the present invention repeatedly comes into contact with the fingerprint of the subject, and as a result, the color development of the fingerprint is promoted and the color sharpness is improved. Since the fingerprint detection liquid of the present invention develops fingerprints in a short time, the time required for fingerprint detection is sufficiently short even if such a procedure is repeated.
繰り返し回数は、３回以上であるのが好ましく、５回以上であるのがより好ましい。繰り返し回数が多くなると、発色した指紋がより鮮明になる。 The number of repetitions is preferably 3 times or more, and more preferably 5 times or more. As the number of repetitions increases, the colored fingerprint becomes clearer.
接触工程において、本発明の指紋検出用液に被検体を浸せきさせる方法を用いる場合、浸せきさせる時間は、１回あたり０．５〜５秒であるのが好ましい。上記範囲であると、浸せきの効果が十分に発現し、また、繰り返しの回数を増やして、短時間の発色および鮮明な発色を効果的に実現することができる。 In the contacting step, when the method of immersing the subject in the fingerprint detection liquid of the present invention is used, the time for immersing is preferably 0.5 to 5 seconds per time. If it is within the above range, the effect of immersion can be sufficiently exhibited, and the number of repetitions can be increased to effectively realize short-time color development and clear color development.
本発明の指紋検出用液の温度は、特に限定されないが、上記手順を繰り返し行う場合には、４０℃以上であるのが好ましい。
繰り返しの手順を行う環境が、高温で高湿度であるときには、乾燥の際にＨＦＥ−３４７が蒸発して被検体から熱（蒸発潜熱）を奪い、その結果、被検体の温度が周囲の環境よりも低くなって、空気中の水分が被検体の表面で凝縮して付着する可能性がある。このような被検体への水分の付着が起こると、発色した指紋が不鮮明になることがある。
本発明の指紋検出用液が４０℃以上であると、このような被検体への水分の付着を防止することができる。
The temperature of the fingerprint detection liquid of the present invention is not particularly limited, but is preferably 40 ° C. or higher when the above procedure is repeated.
When the environment in which the repetitive procedure is performed is high temperature and high humidity, HFE-347 evaporates at the time of drying and takes heat (evaporation latent heat) from the subject. As a result, the temperature of the subject is higher than that of the surrounding environment. And the moisture in the air may condense and adhere on the surface of the subject. When such moisture adheres to the subject, the colored fingerprint may become unclear.
When the fingerprint detection liquid of the present invention is 40 ° C. or higher, it is possible to prevent such moisture from adhering to the subject.
本発明の指紋検出用液によれば、従来、潜在指紋の検出が困難であったレシート等の感熱紙に付着した指紋を検出することができる。これは、本発明の指紋検出用液には極性を有する水が含有されているが、含有量が極めて低いためである。
また、検出される指紋は肉眼で観察することができるほどに鮮明である。
更に、普指紋以外の有力情報に損傷を与えるおそれが低く、印字の変色による妨害や、印字の消失による警察捜査の証拠物件の消滅が起こりにくい。
According to the fingerprint detection liquid of the present invention, it is possible to detect a fingerprint attached to a thermal paper such as a receipt, which has been difficult to detect a latent fingerprint. This is because the fingerprint detection liquid of the present invention contains polar water, but its content is extremely low.
Also, the detected fingerprint is so clear that it can be observed with the naked eye.
Furthermore, there is a low possibility of damaging leading information other than the common fingerprint, and it is difficult for the obstruction due to the discoloration of the print or the disappearance of the evidence of the police investigation due to the loss of the print.
以下に実施例を示して本発明を具体的に説明する。ただし、本発明はこれらに限られるものではない。
１．指紋検出用液の調製
（実施例１）
ガラス製分液漏斗中の１０００ｍＬのＨＦＥ−３４７に、１０ｍＬの純水を添加して、よくかくはんした後に室温で３０分間静置した。その結果、少量の水が液面に浮上し、上層となった。ついで、下層より５００ｍＬの含水ＨＦＥ−３４７を採取した。
更に、１００ｇの上記で得られた含水ＨＦＥ−３４７に、１ｇのニンヒドリンを添加して５０℃で３０分間保温し、その後、ろ紙を用いてろ過を行い、ろ液を指紋検出用液とした。
The present invention will be specifically described below with reference to examples. However, the present invention is not limited to these.
1. Preparation of fingerprint detection liquid (Example 1)
10 mL of pure water was added to 1000 mL of HFE-347 in a glass separatory funnel, and after stirring well, the mixture was allowed to stand at room temperature for 30 minutes. As a result, a small amount of water floated on the liquid surface and became an upper layer. Next, 500 mL of hydrous HFE-347 was collected from the lower layer.
Furthermore, 1 g of ninhydrin was added to 100 g of the hydrous HFE-347 obtained above and kept at 50 ° C. for 30 minutes, followed by filtration using filter paper, and the filtrate was used as a fingerprint detection solution.
（実施例２〜８）
上記で得られた含水ＨＦＥ−３４７に、水を添加していないＨＦＥ−３４７を添加して、水の濃度を低下させた後に、ニンヒドリンを添加した以外は、実施例１と同様の方法により、指紋検出用液を得た。
(Examples 2 to 8)
To the water-containing HFE-347 obtained above, HFE-347 not added with water was added, the concentration of water was lowered, and then ninhydrin was added in the same manner as in Example 1, A liquid for fingerprint detection was obtained.
（比較例１）
ガラス製分液漏斗中の１０００ｍＬの１−エトキシ−１，１，２，２−テトラフルオロエタンに、１０ｍＬの純水を添加して、よくかくはんした後に室温で３０分間静置した。その結果、少量の水が液面に浮上し、上層となった。
ついで、下層より５００ｍＬの含水１−エトキシ−１，１，２，２−テトラフルオロエタンを採取した。
更に、１００ｇの上記で得られた含水１−エトキシ−１，１，２，２−テトラフルオロエタンに、１ｇのニンヒドリンを添加して５０℃で３０分間保温し、その後、ろ紙を用いてろ過を行い、ろ液を指紋検出用液とした。
(Comparative Example 1)
10 mL of pure water was added to 1000 mL of 1-ethoxy-1,1,2,2-tetrafluoroethane in a glass separatory funnel, and after stirring well, the mixture was allowed to stand at room temperature for 30 minutes. As a result, a small amount of water floated on the liquid surface and became an upper layer.
Next, 500 mL of hydrous 1-ethoxy-1,1,2,2-tetrafluoroethane was collected from the lower layer.
Further, 1 g of ninhydrin was added to 100 g of the water-containing 1-ethoxy-1,1,2,2-tetrafluoroethane obtained above and kept at 50 ° C. for 30 minutes, and then filtered using a filter paper. The filtrate was used as a fingerprint detection solution.
（比較例２）
ガラス製分液漏斗中の１０００ｍＬの（パーフルオロブトキシ）メタン（ＨＦＥ−７１００、米国３Ｍ社製）に、１０ｍＬの純水を添加して、よくかくはんした後に室温で３０分間静置した。その結果、少量の水が液面に浮上し、上層となった。
ついで、下層より５００ｍＬの含水（パーフルオロブトキシ）メタンを採取した。
更に、１００ｇの上記で得られた含水（パーフルオロブトキシ）メタンに、１ｇのニンヒドリンを添加して５０℃で３０分間保温し、その後、ろ紙を用いてろ過を行い、ろ液を指紋検出用液とした。
(Comparative Example 2)
10 mL of pure water was added to 1000 mL of (perfluorobutoxy) methane (HFE-7100, manufactured by 3M USA) in a glass separatory funnel, and after stirring well, the mixture was allowed to stand at room temperature for 30 minutes. As a result, a small amount of water floated on the liquid surface and became an upper layer.
Next, 500 mL of hydrous (perfluorobutoxy) methane was collected from the lower layer.
Further, 1 g of ninhydrin was added to 100 g of the water-containing (perfluorobutoxy) methane obtained above, and the mixture was kept at 50 ° C. for 30 minutes, followed by filtration using filter paper, and the filtrate was used as a fingerprint detection solution. It was.
（比較例３）
ガラス製分液漏斗中の１０００ｍＬの（パーフルオロブトキシ）エタン（ＨＦＥ−７２００、米国３Ｍ社製）に、１０ｍＬの純水を添加して、よくかくはんした後に室温で３０分間静置した。その結果、少量の水が液面に浮上し、上層となった。
ついで、下層より５００ｍＬの含水（パーフルオロブトキシ）エタンを採取した。
更に、１００ｇの上記で得られた含水（パーフルオロブトキシ）エタンに、１ｇのニンヒドリンを添加して５０℃で３０分間保温し、その後、ろ紙を用いてろ過を行い、ろ液を指紋検出用液とした。
(Comparative Example 3)
10 mL of pure water was added to 1000 mL of (perfluorobutoxy) ethane (HFE-7200, manufactured by 3M Corporation, USA) in a glass separatory funnel, and after stirring well, the mixture was allowed to stand at room temperature for 30 minutes. As a result, a small amount of water floated on the liquid surface and became an upper layer.
Subsequently, 500 mL of hydrous (perfluorobutoxy) ethane was collected from the lower layer.
Further, 1 g of ninhydrin was added to 100 g of the water-containing (perfluorobutoxy) ethane obtained above, and the mixture was kept at 50 ° C. for 30 minutes, followed by filtration using filter paper. It was.
２．指紋検出用液の水およびニンヒドリンの含有量
上記で得られた指紋検出用液の水およびニンヒドリンの含有量を以下のようにして求め、第１表に示した。
指紋検出用液の水の含有量は、カールフィッシャー水分計を用いて、電量滴定法により求めた。
指紋検出用液のニンヒドリンの含有量は、指紋検出用液を１０５℃で６０分間保温し、含水ＨＦＥ−３４７（実施例１〜８）、含水１−エトキシ−１，１，２，２−テトラフルオロエタン（比較例１）、含水（パーフルオロブトキシ）メタン（比較例２）または含水（パーフルオロブトキシ）エタン（比較例３）を蒸発させて、残留物の質量をニンヒドリンの質量とし、これを蒸発前の指紋検出用液の質量で除して、求めた。
2. Water and ninhydrin contents of the fingerprint detection liquid The water and ninhydrin contents of the fingerprint detection liquid obtained above were determined as follows and are shown in Table 1.
The water content of the fingerprint detection liquid was determined by a coulometric titration method using a Karl Fischer moisture meter.
The content of ninhydrin in the fingerprint detection liquid is such that the fingerprint detection liquid is kept warm at 105 ° C. for 60 minutes, hydrous HFE-347 (Examples 1 to 8), hydrous 1-ethoxy-1,1,2,2-tetra. Fluoroethane (Comparative Example 1), hydrous (perfluorobutoxy) methane (Comparative Example 2) or hydrous (perfluorobutoxy) ethane (Comparative Example 3) is evaporated to give the mass of the residue the mass of ninhydrin. It was obtained by dividing by the mass of the fingerprint detection liquid before evaporation.
３．指紋検出試験
上記で得られた指紋検出用液を用い、指で接触した食料品小売店のレジスターの感熱紙レシートを被検体として、指紋検出試験を行った。指紋検出試験は、以下の検出条件１〜３のそれぞれを行い、その後の被検体の指紋の発色の程度を目視で観察して評価した。また、印字の流れや溶出による不鮮明化および印字されていない部分の変色についても目視で観察した。
3. Fingerprint detection test Using the fingerprint detection liquid obtained above, a fingerprint detection test was conducted using a thermal paper receipt of a grocery retailer's register in contact with a finger as an object. In the fingerprint detection test, each of the following detection conditions 1 to 3 was performed, and the subsequent color development of the fingerprint of the subject was visually observed and evaluated. In addition, the flow of printing and smearing due to elution and discoloration of the unprinted portion were also visually observed.
＜検出条件＞
検出条件１：被検体を室温（２２〜２４℃）の指紋検出溶液に１５分間浸せきさせた後、恒温器中、５０℃で１５分間放置した。
検出条件２：被検体を室温（２２〜２４℃）の指紋検出溶液に５分間浸せきさせた後、恒温器中、５０℃で１５分間放置した。
検出条件３：被検体を室温（２２〜２４℃）の指紋検出溶液に１秒間浸せきさせた後、引き上げて５秒間放置するという操作を５回繰り返した後（合計浸せき時間：５秒間）、恒温器中、５０℃で１５分間放置した。
<Detection conditions>
Detection condition 1: The specimen was immersed in a fingerprint detection solution at room temperature (22-24 ° C.) for 15 minutes, and then left in a thermostat at 50 ° C. for 15 minutes.
Detection condition 2: The specimen was immersed in a fingerprint detection solution at room temperature (22-24 ° C.) for 5 minutes and then left in a thermostat at 50 ° C. for 15 minutes.
Detection condition 3: After immersing the subject in a fingerprint detection solution at room temperature (22 to 24 ° C.) for 1 second and then lifting it up and leaving it for 5 seconds (total immersion time: 5 seconds), constant temperature The vessel was left at 50 ° C. for 15 minutes.
被検体の指紋の発色の程度の結果を第１表に示す。第１表中の記号の意味は以下のとおりである。
◎：指紋の発色が濃く鮮明
○：指紋の発色が鮮明
△：指紋の発色が薄い
×：指紋の発色を認識することができない
The results of the degree of color development of the subject's fingerprint are shown in Table 1. The meanings of the symbols in Table 1 are as follows.
◎: Fingerprint color is dark and clear ○: Fingerprint color is clear △: Fingerprint color is light ×: Fingerprint color cannot be recognized
第１表から明らかなように、本発明の指紋検出用液（実施例１〜８）を用いた場合、検出条件を適宜選択することにより、指紋の検出を行うことができた。その際、発色の促進のための加温時に特別な注意は不要であった。なお、実施例８の指紋検出溶液を用いて、検出条件３の操作を３０回繰り返す試験（合計浸せき時間：３０秒間）を別途行った結果、被検体に付着していた指紋は鮮明に発色した。
また、水およびニンヒドリンの含有量が比較的高い本発明の指紋検出用液（実施例１〜６、特に実施例１〜４）を用いた場合、検体との接触時間を短くすることができ、発色性にも優れていた。特に、被検体との短時間の接触を繰り返す本発明の指紋検出方法（検出条件４）を用いた場合に、顕著であった。
更に、本発明の指紋検出用液（実施例１〜８）を用いた場合は、印字の流れや溶出による不鮮明化は見られず、また、印字されていない部分の変色が見られなかった。
これに対し、比較例１で得られた指紋検出用液を用いた場合は、印字されていない部分の一部が黒く変色していた。また、比較例２または３で得られた指紋検出用液を用いた場合は、上記検出条件で指紋の検出を行うことができなかった。
As is apparent from Table 1, when the fingerprint detection liquid of the present invention (Examples 1 to 8) was used, fingerprints could be detected by appropriately selecting the detection conditions. At that time, no special care was required during heating to promote color development. In addition, as a result of separately conducting a test (total immersion time: 30 seconds) in which the operation of detection condition 3 was repeated 30 times using the fingerprint detection solution of Example 8, the fingerprint attached to the subject was vividly colored. .
In addition, when using the fingerprint detection liquid of the present invention (Examples 1 to 6, especially Examples 1 to 4) having a relatively high content of water and ninhydrin, the contact time with the specimen can be shortened, Excellent color development. This was particularly noticeable when the fingerprint detection method (detection condition 4) of the present invention in which contact with a subject is repeated for a short time.
Furthermore, when the fingerprint detection liquid of the present invention (Examples 1 to 8) was used, no blurring due to the flow or elution of printing was observed, and no discoloration was observed in the unprinted portion.
On the other hand, when the fingerprint detection liquid obtained in Comparative Example 1 was used, a part of the unprinted portion was discolored black. Also, when the fingerprint detection liquid obtained in Comparative Example 2 or 3 was used, fingerprint detection could not be performed under the above detection conditions.
Claims (10)
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| JP2005017805A JP4609083B2 (en) | 2005-01-26 | 2005-01-26 | Liquid for fingerprint detection, manufacturing method thereof, and fingerprint detection method using the same |
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| JP2005017805A JP4609083B2 (en) | 2005-01-26 | 2005-01-26 | Liquid for fingerprint detection, manufacturing method thereof, and fingerprint detection method using the same |
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| JP4609083B2 JP4609083B2 (en) | 2011-01-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011516236A (en) * | 2008-04-14 | 2011-05-26 | ハネウェル・インターナショナル・インコーポレーテッド | Carrier solvent for fingerprint detection formulation |
| JP2011188969A (en) * | 2010-03-15 | 2011-09-29 | Nippon Menaade Keshohin Kk | Liquid for detecting fingerprint, and method of detecting fingerprint |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04124156A (en) * | 1990-09-14 | 1992-04-24 | Masahisa Takatsu | Reagent for detecting fingerprint and its production |
| JP2000186269A (en) * | 1998-10-13 | 2000-07-04 | Lintec Corp | Ninhydrin-containing pressure-sensitive adhesive composition and sheet for detecting amino compound |
| JP2003052670A (en) * | 2001-08-08 | 2003-02-25 | Asahi Glass Co Ltd | Finger print detecting solution and its preparing method |
| JP2003061937A (en) * | 2001-08-28 | 2003-03-04 | Asahi Glass Co Ltd | Fingerprints detecting liquid and preparing method for it |
-
2005
- 2005-01-26 JP JP2005017805A patent/JP4609083B2/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04124156A (en) * | 1990-09-14 | 1992-04-24 | Masahisa Takatsu | Reagent for detecting fingerprint and its production |
| JP2000186269A (en) * | 1998-10-13 | 2000-07-04 | Lintec Corp | Ninhydrin-containing pressure-sensitive adhesive composition and sheet for detecting amino compound |
| JP2003052670A (en) * | 2001-08-08 | 2003-02-25 | Asahi Glass Co Ltd | Finger print detecting solution and its preparing method |
| JP2003061937A (en) * | 2001-08-28 | 2003-03-04 | Asahi Glass Co Ltd | Fingerprints detecting liquid and preparing method for it |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011516236A (en) * | 2008-04-14 | 2011-05-26 | ハネウェル・インターナショナル・インコーポレーテッド | Carrier solvent for fingerprint detection formulation |
| JP2011188969A (en) * | 2010-03-15 | 2011-09-29 | Nippon Menaade Keshohin Kk | Liquid for detecting fingerprint, and method of detecting fingerprint |
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| JP4609083B2 (en) | 2011-01-12 |
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