JPH0228540A - Sensitizing diluent for infrared ray spectrum - Google Patents
Sensitizing diluent for infrared ray spectrumInfo
- Publication number
- JPH0228540A JPH0228540A JP63178136A JP17813688A JPH0228540A JP H0228540 A JPH0228540 A JP H0228540A JP 63178136 A JP63178136 A JP 63178136A JP 17813688 A JP17813688 A JP 17813688A JP H0228540 A JPH0228540 A JP H0228540A
- Authority
- JP
- Japan
- Prior art keywords
- diluent
- sample
- weight
- sensitizing
- infrared ray
- 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.)
- Pending
Links
Landscapes
- Spectrometry And Color Measurement (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は赤外吸収スペクトルを例えば錠剤法で測定する
場合に試料の錠剤化に際して混合される希釈剤に関し、
特に光散乱性の強い試料に対して有効な希釈剤に関する
ものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a diluent that is mixed when tabletting a sample when measuring an infrared absorption spectrum by, for example, a tablet method.
This invention relates to a diluent that is particularly effective for samples with strong light scattering properties.
赤外吸収スペクトルを測定する際には一般に試料の希釈
が行なわれ、その希釈法に応じて、溶液法、ペースト法
、錠剤法などに分類されている。When measuring an infrared absorption spectrum, a sample is generally diluted, and the method is classified into solution method, paste method, tablet method, etc. depending on the dilution method.
これらのなかで錠剤法は試料が少量ですむこと、吸収ス
ペクトルがシャープであること、溶媒の吸収に煩わされ
ることがないこと、操作が容易であることなどの利点が
認められて広く利用されている０錠剤法においては、赤
外領域に吸収がなくまた加圧により可塑性を帯びる材料
である臭化カリウム、塩化カリウム、塩化ナトリウム、
ヨウ化カリウムなどがこの希釈剤として使用されてきた
。Among these, the tablet method is widely used because of its advantages such as requiring a small amount of sample, sharp absorption spectrum, no problem with solvent absorption, and ease of operation. In the 0-tablet method, potassium bromide, potassium chloride, sodium chloride, which has no absorption in the infrared region and becomes plastic under pressure, is used.
Potassium iodide and the like have been used as this diluent.
各種試料のなかで、特に石炭粉末などの光散乱性の強い
不均一系試料の場合には試料に当った赤外光が散乱され
一方相当量の赤外光が試料を素通りするためバックグラ
ウンドが高く吸収ピークの小さなスペクトルになる。従
来は、この得られたスペクトルから直線とか曲線を用い
てベースラインを差し引くことによりバックグラウンド
を消去していた（大沢祥拡、松村秀彦、藤井修治、燃協
誌、４８．７０３（１９６９）、 Ｐｅｔｅｒ Ｒ，５
ｏｌｏｓ＋ｏｎ ａｎｄ ＲｏｂｅｒｔＭ、Ｃａｒａｎ
ｇｅｌｏ、 Ｆｕｅｌ、 ６１．６６３（１９８２））
。Among various samples, especially in the case of heterogeneous samples with strong light scattering properties such as coal powder, infrared light that hits the sample is scattered, while a considerable amount of infrared light passes through the sample, resulting in background noise. The spectrum will have a high absorption peak and a small one. Conventionally, the background was removed by subtracting the baseline from the obtained spectrum using a straight line or curve (Yoshihiro Osawa, Hidehiko Matsumura, Shuji Fujii, Nenkoo Shi, 48.703 (1969), Peter R, 5
olos+on and Robert M, Caran
gelo, Fuel, 61.663 (1982))
.
一方、本発明者らはこのバックグラウンドを軽減するべ
く鋭意検討の結果、ＫＢｒとＣｓ１等屈折率の異なる２
種以上の無機物よりなる光散乱フィルターを開発するに
至り、この光散乱フィルターを錠開化試料の後方に配置
することによってバックグラウンドを軽減できることを
見出してその内容を既に発表した（第３５回分析化学会
、特開昭６３−１１８６３７号公報）。On the other hand, as a result of intensive studies to reduce this background, the present inventors found that two materials with different refractive indexes, such as KBr and Cs1,
We have developed a light-scattering filter made of inorganic substances of more than 100% species, and have already published our findings on the discovery that the background can be reduced by placing this light-scattering filter behind the unlocked sample (35th Analytical Chemistry Society, Japanese Patent Publication No. 118637/1983).
従来の直線とか曲線を用いてベースラインを想定して差
し引（方法では真のバックグラウンドは不明確であり、
バックグラウンドとしての直線や曲線の決定を人間の勘
に頷らざるをえないところから分析精度に問題があった
。Traditional straight or curved lines are used to assume a baseline and then subtracted (in this method, the true background is unclear,
There was a problem with the accuracy of the analysis because humans had to rely on their intuition to determine the straight lines and curves in the background.
また、前記の新たな光散乱フィルターを利用する方法に
ついてはさらにバックグラウンドを減少させて強くてシ
ャープな吸収スペクトルが得られる方法の開発が望まれ
ていた。Furthermore, regarding the method using the above-mentioned new light scattering filter, it has been desired to develop a method that can further reduce the background and obtain a strong and sharp absorption spectrum.
本発明はこれらの問題点を解決する手段を提供するもの
であり、平均粒径が２０μ以下のヨウ化セシウム５〜９
５重量％と平均粒径が２０．以下の臭化カリウム９５〜
５重量％の均一混合物よりなる赤外線スペクトルの増感
希釈剤によってこの目的を達成したものである。The present invention provides a means to solve these problems, and uses 5 to 9 cesium iodide with an average particle size of 20μ or less.
5% by weight and an average particle size of 20. Potassium bromide below 95~
This objective was achieved with a 5% by weight homogeneous mixture of sensitizing diluents in the infrared spectrum.
ヨウ化セシウム及び臭化カリウムはいずれも粒径２Ｏｎ
以下であり、３〜２０ｎ程度のものが好ましい、混合比
はＣｓｌ ： ＫＢｒの重量比で５：９５〜９５：５で
あり、３０ ： ７０〜８０ ： ２０程度が好ましい
。Both cesium iodide and potassium bromide have a particle size of 2On.
The weight ratio of Csl:KBr is preferably 5:95 to 95:5, preferably about 30:70 to 80:20.
この粉末を試料の錠剤化用に使用する方法は従来のＫＢ
ｒ等の単品の場合と同様でよく、試料と均一に混合後所
定の形状に真空プレス成型すればよい、試料との混合比
率も従来と同様でよい。The method of using this powder for tabletting samples is the conventional KB method.
It may be the same as in the case of a single item such as r, and it is sufficient to vacuum press mold it into a predetermined shape after uniformly mixing it with the sample.The mixing ratio with the sample may also be the same as in the conventional case.
光散乱性の強い不均一系試料の場合には試料に当った赤
外光が散乱されるため試料の情報を含む赤外光の検出器
への入射量が少なくなる。一方、試料を素通りする赤外
光が相当あってこれがバックグラウンドを上昇させる。In the case of a heterogeneous sample with strong light scattering properties, the infrared light that hits the sample is scattered, so the amount of infrared light containing information about the sample that is incident on the detector is reduced. On the other hand, there is a considerable amount of infrared light that passes through the sample, which increases the background.
本発明の希釈剤を用いると試料部内に屈折率の異なる無
機物がランダムに寄り集まった状態になるため赤外光が
無機物の境界面で屈折する。その結果、再散乱回数が増
して同じ光が何回も試料に繰返し衝突してその情報量が
増し、測定感度を上昇させる。希釈剤の微粒子の粒径分
布を赤外光の波長程度（〜２０ｎ）としたことにより、
より完全な赤外光の散乱効果が得られ、著しく良質なス
ペクトルが得られる。一方、この高散乱性によって試料
部を素通りする光はほとんどなくなりバックグラウンド
が低下する。When the diluent of the present invention is used, inorganic substances having different refractive indexes are randomly gathered in the sample portion, so that infrared light is refracted at the interface between the inorganic substances. As a result, the number of rescattering increases, and the same light repeatedly collides with the sample many times, increasing the amount of information and increasing measurement sensitivity. By setting the particle size distribution of the fine particles of the diluent to about the wavelength of infrared light (~20n),
A more complete infrared light scattering effect is obtained, resulting in a significantly better quality spectrum. On the other hand, due to this high scattering property, almost no light passes through the sample portion, reducing the background.
Ｃｓｌの微粉末（２０ｎアンダー）６０重量％とＫＢｒ
の微粉末（２０ｎアンダー）４０重量％を均一に混合し
て赤外吸収スペクトルの増感希釈剤を得た。60% by weight of Csl fine powder (under 20n) and KBr
A sensitizing diluent for infrared absorption spectrum was obtained by uniformly mixing 40% by weight of fine powder (20n under).
石炭試料粉末（１４９ミクロンアンダー）１．０重量％
と希釈剤を均一に混合し、直径１０ａｍディスク状に真
空プレス成型した。Coal sample powder (under 149 microns) 1.0% by weight
and a diluent were uniformly mixed and vacuum press molded into a disk shape with a diameter of 10 am.
一方、比較のために同じ石炭試料粉末と従来の希釈剤で
あるＫＢｒ単品の粉末（１４９−アンダー）を均一に混
合し、同形のディスク状に真空プレス成型した。On the other hand, for comparison, the same coal sample powder and the conventional diluent KBr single powder (149-under) were mixed uniformly and vacuum press-molded into the same disk shape.
こうして得られた錠剤化試料の赤外吸収スペクトルを測
定した結果を第１図に示す。図中、Ａは本発明の希釈剤
を用いて調製した錠剤化試料を測定した場合のそして、
Ｂは従来のＫＢｒ単品の希釈剤を用いて調製した錠剤化
試料を測定した場合のそれぞれ赤外線吸収スペクトルを
表わしている。FIG. 1 shows the results of measuring the infrared absorption spectrum of the tableted sample thus obtained. In the figure, A is the result when a tableted sample prepared using the diluent of the present invention was measured.
B represents the infrared absorption spectra obtained when tableting samples prepared using a conventional KBr single diluent were measured.
次に、Ｃｓｌの微粉末（２０ｎアンダー）とＫＢｒの微
粉末（２０ｎアンダー）の混合比を変えて上記の例と同
様にして石炭試料粉末の赤外線吸収スペクトルを測定し
た結果を第２図に示す。図中ＣはＣｓ１２０重量％ＫＢ
ｒ ８０重量％の、ＤはＣｓ１４０重量％ＫＢｒ ６０
重量％の、ＥはＣｓｌ ６０重重量ＫＢｒ ４０重量％
の、そしてＦはＣｓＩ ８０重量％ＫＢｒ ２０重量％
の場合をそれぞれ示している。Next, the infrared absorption spectrum of the coal sample powder was measured in the same manner as in the above example by changing the mixing ratio of Csl fine powder (under 20n) and KBr fine powder (under 20n). The results are shown in Figure 2. . C in the figure is Cs120wt%KB
r 80% by weight, D is Cs140% by weight KBr 60
Weight%, E is Csl 60wt KBr 40wt%
and F is CsI 80% by weight KBr 20% by weight
Each case is shown.
本発明の希釈剤を用いることにより吸収スペクトルのピ
ークを著しく増大させ、またバックグラウンドを減少さ
せてベースラインの歪みを少な（することができる。そ
の結果、従来法では見つからなかった新しい吸収を判別
でき、また吸収の強度も強くシャープになっている。そ
のため、スペクトルの解析精度は著しく向上した。By using the diluent of the present invention, it is possible to significantly increase the peak of the absorption spectrum, reduce the background, and reduce the distortion of the baseline.As a result, it is possible to distinguish new absorptions that were not found using conventional methods. In addition, the absorption intensity is strong and sharp.As a result, the accuracy of spectrum analysis has been significantly improved.
本希釈剤は光散乱性の強い不均一系試料の測定に対して
特に威力を発揮し、良好なスペクトルを得ることができ
る。This diluent is particularly effective in measuring heterogeneous samples with strong light scattering properties, and allows obtaining good spectra.
第１図は本発明の希釈剤を用いて錠剤化した不均一系試
料の赤外線吸収スペクトルを従来の希釈剤を用いて得ら
れた赤外線吸収スペクトルと比較して示したものである
。第２図はＣｓｌとＫＢｒの混合比を変えて赤外線吸収
スペクトルを測定した結果を示す図である。
特許出願人 日本鋼管株式会社
代 理 人 弁理士 日中 政浩
第
図
波数（ｃｉ’）
波数（ｃｊ）
波数（ｃｊ’）
波数（ｃｊ’）
波数（ｃｊ）FIG. 1 shows an infrared absorption spectrum of a heterogeneous sample tableted using the diluent of the present invention in comparison with an infrared absorption spectrum obtained using a conventional diluent. FIG. 2 is a diagram showing the results of measuring infrared absorption spectra with varying mixing ratios of Csl and KBr. Patent Applicant: Nippon Steel Tube Co., Ltd. Agent: Masahiro Japan, Patent Attorney Wavenumber (ci') Wavenumber (cj) Wavenumber (cj') Wavenumber (cj') Wavenumber (cj)
Claims (1)
％と平均粒径が２０μｍ以下の臭化カリウム９５〜５重
量％の混合物よりなる赤外線スペクトルの増感希釈剤An infrared spectral sensitizing diluent consisting of a mixture of 5 to 95% by weight of cesium iodide with an average particle size of 20 μm or less and 95 to 5% by weight of potassium bromide with an average particle size of 20 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63178136A JPH0228540A (en) | 1988-07-19 | 1988-07-19 | Sensitizing diluent for infrared ray spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63178136A JPH0228540A (en) | 1988-07-19 | 1988-07-19 | Sensitizing diluent for infrared ray spectrum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0228540A true JPH0228540A (en) | 1990-01-30 |
Family
ID=16043281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63178136A Pending JPH0228540A (en) | 1988-07-19 | 1988-07-19 | Sensitizing diluent for infrared ray spectrum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0228540A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057691A (en) * | 1989-06-28 | 1991-10-15 | Nkk Corporation | Dilution material, filter and accessory for measuring infrared spectra |
| WO2008129959A1 (en) * | 2007-04-13 | 2008-10-30 | Arkray, Inc. | Pellet for spectrometry, process for producing the pellet, and method for spectrometry using the pellet |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61184440A (en) * | 1985-02-13 | 1986-08-18 | Mitsubishi Heavy Ind Ltd | Method for preparing specimen for infrared spectroscopic analysis |
| JPS63118637A (en) * | 1986-06-27 | 1988-05-23 | Nkk Corp | Infrared scattering agent |
-
1988
- 1988-07-19 JP JP63178136A patent/JPH0228540A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61184440A (en) * | 1985-02-13 | 1986-08-18 | Mitsubishi Heavy Ind Ltd | Method for preparing specimen for infrared spectroscopic analysis |
| JPS63118637A (en) * | 1986-06-27 | 1988-05-23 | Nkk Corp | Infrared scattering agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057691A (en) * | 1989-06-28 | 1991-10-15 | Nkk Corporation | Dilution material, filter and accessory for measuring infrared spectra |
| WO2008129959A1 (en) * | 2007-04-13 | 2008-10-30 | Arkray, Inc. | Pellet for spectrometry, process for producing the pellet, and method for spectrometry using the pellet |
| JP5325097B2 (en) * | 2007-04-13 | 2013-10-23 | アークレイ株式会社 | Spectral measurement pellet and spectroscopic measurement method using the pellet |
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