JPS59222763A - Column for high-speed liquid chromatography - Google Patents
Column for high-speed liquid chromatographyInfo
- Publication number
- JPS59222763A JPS59222763A JP9765083A JP9765083A JPS59222763A JP S59222763 A JPS59222763 A JP S59222763A JP 9765083 A JP9765083 A JP 9765083A JP 9765083 A JP9765083 A JP 9765083A JP S59222763 A JPS59222763 A JP S59222763A
- Authority
- JP
- Japan
- Prior art keywords
- filter
- column
- filling agent
- inner diameter
- particle size
- 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
- 238000004811 liquid chromatography Methods 0.000 title 1
- 239000011148 porous material Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000012856 packing Methods 0.000 claims abstract description 10
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000011368 organic material Substances 0.000 abstract description 2
- 230000002542 deteriorative effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000012156 elution solvent Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6004—Construction of the column end pieces
- G01N30/603—Construction of the column end pieces retaining the stationary phase, e.g. Frits
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はカラムクロマトグラフィー用カラム特に高速液
体クロマトグラフィー用カラムに関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to columns for column chromatography, particularly columns for high performance liquid chromatography.
近年、高速液体クロマトグラフィーの進歩は目覚しく種
々の混合物の分離定量や分析に多く用いられている。こ
のクロマトグラフィーに用いられるカラムは両端にフィ
ルターを有しているが、フィルターの孔径以上の粒径を
持つ硬質充填剤をバッキングして使用する場合には適当
であるが、軟質な充填剤や粒径が不均一な場合にはフィ
ルターの孔に充填剤がつまるために、カラム内の圧力が
上昇し使用できなくなることがあった。In recent years, high performance liquid chromatography has made remarkable progress and is now widely used for the separation, quantification and analysis of various mixtures. The column used for this chromatography has filters at both ends, but it is suitable when used with a backing of hard packing material with a particle size larger than the pore size of the filter. If the diameters are non-uniform, the pores of the filter may be clogged with filler, which may increase the pressure inside the column and make it unusable.
又、充填剤によってはスラリ一式充填法では充填できず
、乾式充填法でしか充填できない場合があった。例えば
、Ｇ、Ｇ１１ｂｉ１；ｚらは、Ｔ Ｏｕ ｒ ｎ ａ、
１ｏｆ Ｈｌｇｈ Ｒｅ５ｏｌｕｔｉｏｎ Ｃｈｒｏ
ｍａｔｏｇｒａｐｈｙ ＆Ｃｈｒｏｍａｔｏｇｒａｐ
ｈｙ Ｏｏｍｕｎｉｃａｔｉｏｎ 、 ｖｏ１３ 、１
９８０年のＰ、１０３１に粒径７ａｍのセルロース（Ｂ
・Ｍｅｒｃｋ社製）を充填するのに、スラリ一式充填法
では圧力が上昇してうまく充填できず、乾式充填法でし
か行なえないことを報告している。Furthermore, depending on the filler, it may not be possible to fill it using the slurry complete filling method, and it may only be possible to fill it using the dry filling method. For example, G, G11bi1;z et al.
1 of Hlgh Re5solution Chro
matography & chromatography
hy Ocommunication, vo13, 1
P in 980, cellulose with a particle size of 7 am in 1031 (B
・Merck) has been reported to be unable to be filled successfully using the slurry complete filling method due to increased pressure, and that only the dry filling method can be used.
充填剤がフィルターにつまるのは充填剤の径に対してフ
ィルターの孔径が比較的太きいためであジ、フィルター
の孔径を小さくすれば、充填剤はつまらなくなるが、孔
径が小さくなるとカラム内の圧力が増加し、充填剤を圧
力で押しつぶしてしまうという二律背反がおこる。The reason why the packing material gets clogged in the filter is because the pore size of the filter is relatively large compared to the diameter of the packing material.If the pore size of the filter is made small, the packing material becomes boring, but if the pore size is made small, the inside of the column becomes clogged. A trade-off occurs in that the pressure increases and the filler is crushed by the pressure.
本発明者らは、上記の問題を克服すべく鋭意研究の結果
、本発明に至ったのである。The present inventors conducted extensive research to overcome the above-mentioned problems, and as a result, they arrived at the present invention.
すなわち、本発明はカラムの両端又は片端に二層構造を
持つフィルターを有し、内側のフィルターが充填剤よシ
小さな孔径を持ち、外側のフィルターがカラム内径の１
１５〜１／１０００００１７）孔径を持つことを特徴と
する高速液体クロマトグラフィー用カラムに係るもので
ある。That is, the present invention has a filter with a two-layer structure at both ends or one end of the column, the inner filter has a smaller pore size than the packing material, and the outer filter has a pore size that is 1 part of the inner diameter of the column.
The present invention relates to a column for high performance liquid chromatography characterized by having a pore size of 15 to 1/10000017).
本発明の二層構造を有するフィルターのうち、充填剤に
接触する内側のフィルターは孔が充填剤の粒径よシも小
さな多孔質フィルターであり、フィルターの厚さはカラ
ムの内径の１／１０〜１／１００００が好ましく、更に
好ましくは１／１００〜１／１００００である。１／１
０より厚くなると空隙容量が大きくなシ好ましくな’＜
％ １／１００００未満であると強度が弱くなシ好ま
□しくない。内側フィルターの材質は、溶出溶媒や溶出
化合物によって劣化しない有機材又は無機材が使用され
る。Among the filters having a two-layer structure of the present invention, the inner filter that comes into contact with the packing material is a porous filter whose pores are smaller than the particle size of the packing material, and the thickness of the filter is 1/10 of the inner diameter of the column. It is preferably from 1/10000 to 1/10000, and more preferably from 1/100 to 1/10000. 1/1
If it is thicker than 0, the void volume will be large, which is preferable.
% less than 1/10000 is not preferable because the strength is weak. The material for the inner filter is an organic or inorganic material that does not deteriorate due to the elution solvent or the elution compound.
特に繊維状のものが好ましく、例えばガラス繊維、シリ
カ繊維、Ｆ紙、４−弗化エチレン繊維等が好ましい。In particular, fibrous materials are preferred, such as glass fibers, silica fibers, F paper, and 4-fluorinated ethylene fibers.
又、外側のフィルターの孔径、厚さ及び材質は内側のフ
ィルターを補強できる程良のものであればよいＯフィル
ターの孔径は、カラム内径の′ｉ１５〜１／１００００
０が好ましく、厚さはカラムの内径に対して１／２〜１
／１００００であって、１／２よす厚くなると空隙容量
が大きくなり好ましくなく、１／１００００未満である
と強度が弱くなシ好ましくない。材質は有機材又は無機
材の多孔質のものが好ましく、金属又はプラスチック、
セラミック等が使用できるが、溶出溶媒や溶出化合物に
侵されるものであってはならない。The pore size, thickness, and material of the outer filter should be good enough to reinforce the inner filter.The pore size of the O filter should be 15 to 1/10,000 of the column inner diameter.
0 is preferable, and the thickness is 1/2 to 1 with respect to the inner diameter of the column.
/10,000, and if it is thicker by 1/2, the void volume will increase, which is undesirable, and if it is less than 1/10,000, the strength will be weak, which is not preferable. The material is preferably an organic or inorganic porous material, such as metal or plastic,
Ceramic or the like can be used, but it must not be attacked by the elution solvent or the elution compound.
上記の如き二層構造フィルターを有する本発明のカラム
は、内側フィルターの孔が比較的小さいために充填剤が
つまらず、しかも厚みが薄いためにカラム管内に圧力が
かからない。さらに、比較約０の粗い外側のフィルター
で内側のフィルターを補強した二層構造にすることによ
って軟質充填剤や粒径分布の広い充填剤を容易にバッキ
ングでき、しかも長期間使用できる利点を有する。In the column of the present invention having a double-layered filter as described above, the pores of the inner filter are relatively small, so that the packing material does not become clogged, and the thickness is small, so no pressure is applied inside the column tube. Furthermore, by having a two-layer structure in which the inner filter is reinforced with an outer filter having a roughness of about 0, it is possible to easily back a soft filler or a filler with a wide particle size distribution, and it has the advantage of being usable for a long period of time.
以下図面によシ本発明を更に詳述する。The present invention will be explained in more detail below with reference to the drawings.
第１図は本発明のカラムの一例を示す断面図であるが、
本発明の特徴は二層構造を有するフィルターにあるので
あって、カラム本体の形状は、いかなるものでもよい。FIG. 1 is a sectional view showing an example of the column of the present invention.
The feature of the present invention is a filter having a two-layer structure, and the column body may have any shape.
例えば日本分光工業タイプのカラムであれば、カラムの
片端は第１図に示すようになシ、二層構造フィルタ一部
分を拡大すると第２図に示すようになる。ここで、１は
内側フィルター、２は外側フィルター、３はクロマト管
、４はフィルターホールダーである。For example, in the case of a JASCO Corporation type column, one end of the column is blank as shown in FIG. 1, and if a part of the two-layer structure filter is enlarged, it becomes as shown in FIG. 2. Here, 1 is an inner filter, 2 is an outer filter, 3 is a chromato tube, and 4 is a filter holder.
実施例１及び比較例１
長さ２５ｃＩｎ、内径０．４６αのステンレスカラムに
孔径３〜５ｔｚｍのフィルターを使用した一層フイルタ
ー付空カラムー１と、このフィルターの上にｒ紙Ａ５
Ａ （東洋Ｆ ａｍ ） ’ｅ Ｏ，４６ｏｎ ＣＤ直
径の円形に切ったものを置いて二層構造にした空力ラム
−２を用意した。これに粒径７μｍ〜２５μｍの破砕形
三酢酸セルロースをエタノールに懸濁させ、高速液体ク
ロマトグラフを用いて流速１． Ｊｍｌ／ｍｉｎでスラ
リーバッキングを行なつた。カラム−１（比較例１）は
圧力が上昇し、５００１ｖ／Ｊ以上になシ使用できなか
ったが、カラム−２（実施例１）は圧力が２７ ’ｙ／
ａｉで三酢酸セルロース充填カラムとして使用できた０Example 1 and Comparative Example 1 An empty column 1 with a single layer filter using a stainless steel column with a length of 25 cIn and an inner diameter of 0.46α and a filter with a pore size of 3 to 5 tzm, and an A5 r paper on top of this filter.
A (Toyo Fam) 'e O, 46 on An aerodynamic ram-2 having a two-layer structure was prepared by placing a circular cut piece with a diameter of CD. To this, crushed cellulose triacetate with a particle size of 7 μm to 25 μm was suspended in ethanol and analyzed using a high performance liquid chromatograph at a flow rate of 1. Slurry backing was performed at Jml/min. Column-1 (Comparative Example 1) had a pressure increase and could not be used above 5001v/J, but Column-2 (Example 1) had a pressure of 27'y/J.
0 that could be used as a cellulose triacetate packed column with ai
第１図は本発明のカラムの一例を示す断面図１第２図は
そのフィルタ一部分の断面拡大図である０
１・・・・・内側フィルター
２・・・・・・外側フィルター
出願人代理人 古 谷 馨
第１図
第２図
＝３６５−Figure 1 is a cross-sectional view showing an example of the column of the present invention. Figure 2 is an enlarged cross-sectional view of a portion of the filter. Kaoru Furuya Figure 1 Figure 2 = 365-
Claims (1)
し、内側のフィルターが充填剤より小さな孔径を持ち、
外側のフィルターがカラム内径の１１５〜１．／１００
０００の孔径を持つことを特徴とする高速液体クロマト
グラフィー用カラム。The column has a filter with a two-layer structure at both ends or one end, and the inner filter has a smaller pore size than the packing material.
The outer filter has a column inner diameter of 115 to 1. /100
A column for high performance liquid chromatography characterized by having a pore size of 0.000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9765083A JPS59222763A (en) | 1983-06-01 | 1983-06-01 | Column for high-speed liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9765083A JPS59222763A (en) | 1983-06-01 | 1983-06-01 | Column for high-speed liquid chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59222763A true JPS59222763A (en) | 1984-12-14 |
Family
ID=14197966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9765083A Pending JPS59222763A (en) | 1983-06-01 | 1983-06-01 | Column for high-speed liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59222763A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02262054A (en) * | 1989-03-31 | 1990-10-24 | Sekisui Chem Co Ltd | Filter for high-performance liquid chromatograph |
| JPH05203634A (en) * | 1991-11-27 | 1993-08-10 | Tosoh Corp | Usage of filter for liquid chromatograph |
| JPH06242094A (en) * | 1993-02-15 | 1994-09-02 | Tosoh Corp | Filter incorporating column for liquid |
| JP2006138724A (en) * | 2004-11-11 | 2006-06-01 | Sekisui Chem Co Ltd | Filter for liquid chromatography, column for liquid chromatography with which filter is integrated, liquid chromatography system using filter and measuring method by liquid chromatography using filter |
| JP2016206010A (en) * | 2015-04-23 | 2016-12-08 | 株式会社粧研 | Resin column body |
| WO2017033914A1 (en) * | 2015-08-25 | 2017-03-02 | 昭和電工株式会社 | Liquid chromatography column and liquid chromatography device equipped with same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55127140A (en) * | 1979-03-27 | 1980-10-01 | Nisshin Flour Milling Co Ltd | Packed tower |
-
1983
- 1983-06-01 JP JP9765083A patent/JPS59222763A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55127140A (en) * | 1979-03-27 | 1980-10-01 | Nisshin Flour Milling Co Ltd | Packed tower |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02262054A (en) * | 1989-03-31 | 1990-10-24 | Sekisui Chem Co Ltd | Filter for high-performance liquid chromatograph |
| JPH05203634A (en) * | 1991-11-27 | 1993-08-10 | Tosoh Corp | Usage of filter for liquid chromatograph |
| JPH06242094A (en) * | 1993-02-15 | 1994-09-02 | Tosoh Corp | Filter incorporating column for liquid |
| JP2006138724A (en) * | 2004-11-11 | 2006-06-01 | Sekisui Chem Co Ltd | Filter for liquid chromatography, column for liquid chromatography with which filter is integrated, liquid chromatography system using filter and measuring method by liquid chromatography using filter |
| JP2016206010A (en) * | 2015-04-23 | 2016-12-08 | 株式会社粧研 | Resin column body |
| WO2017033914A1 (en) * | 2015-08-25 | 2017-03-02 | 昭和電工株式会社 | Liquid chromatography column and liquid chromatography device equipped with same |
| CN107923884A (en) * | 2015-08-25 | 2018-04-17 | 昭和电工株式会社 | Phase chromatography-use column and the liquid-chromatography apparatus for possessing the phase chromatography-use column |
| JPWO2017033914A1 (en) * | 2015-08-25 | 2018-06-14 | 昭和電工株式会社 | Liquid chromatography column and liquid chromatograph apparatus provided with the same |
| EP3346266A4 (en) * | 2015-08-25 | 2019-05-01 | Showa Denko K.K. | Liquid chromatography column and liquid chromatography device equipped with same |
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