JPH0413967A - Quartz capillary column - Google Patents
Quartz capillary columnInfo
- Publication number
- JPH0413967A JPH0413967A JP11798890A JP11798890A JPH0413967A JP H0413967 A JPH0413967 A JP H0413967A JP 11798890 A JP11798890 A JP 11798890A JP 11798890 A JP11798890 A JP 11798890A JP H0413967 A JPH0413967 A JP H0413967A
- Authority
- JP
- Japan
- Prior art keywords
- quartz capillary
- polyethylene glycol
- layer
- capillary column
- stationary phase
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000010453 quartz Substances 0.000 title claims abstract description 37
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 25
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 25
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 10
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 8
- -1 methyl siloxane Chemical class 0.000 claims abstract description 8
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 6
- 230000005526 G1 to G0 transition Effects 0.000 claims description 18
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract 3
- 239000007790 solid phase Substances 0.000 abstract 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052710 silicon Inorganic materials 0.000 abstract 2
- 239000010703 silicon Substances 0.000 abstract 2
- 229920006389 polyphenyl polymer Polymers 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 17
- 238000004817 gas chromatography Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 6
- 239000011241 protective layer Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- NXXYKOUNUYWIHA-UHFFFAOYSA-N 2,6-Dimethylphenol Chemical compound CC1=CC=CC(C)=C1O NXXYKOUNUYWIHA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- QWBBPBRQALCEIZ-UHFFFAOYSA-N 2,3-dimethylphenol Chemical compound CC1=CC=CC(O)=C1C QWBBPBRQALCEIZ-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は石英キャピラリカラム、特に極性化合物の分析
に適する石英キャピラリカラムに関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a quartz capillary column, particularly a quartz capillary column suitable for analyzing polar compounds.
ガスクロマトグラフィ用カラムのうち石英キャピラリカ
ラムは、従来の充填カラム、あるいはＳＵＳステンレス
鋼や多成分ガラスを用いたキャピラリカラムに比べて高
り分解能を示し、微量分析に不可欠である。石英キャピ
ラリカラムのうち、キャピラリの内面にポリエチレング
リコールを固定相として有するものは、フェノール類、
アミン類、アルコール類、各種香料等の極性化合物の分
析に有用である。ポリエチレングリコールを固定相とす
る石英キャピラリカラムは通常、第２図に示すように、
石英キャピラリ１の内面に固定相となるポリエチレング
リコール層２、外側に耐熱保護層４を具える。Among columns for gas chromatography, quartz capillary columns exhibit higher resolution than conventional packed columns or capillary columns using SUS stainless steel or multi-component glass, and are essential for trace analysis. Among quartz capillary columns, those with polyethylene glycol as a stationary phase on the inner surface of the capillary contain phenols,
It is useful for analyzing polar compounds such as amines, alcohols, and various fragrances. A quartz capillary column with polyethylene glycol as the stationary phase usually has the following characteristics as shown in Figure 2.
A polyethylene glycol layer 2 serving as a stationary phase is provided on the inner surface of the quartz capillary 1, and a heat-resistant protective layer 4 is provided on the outer surface.
しかし、ポリエチレングリコールを固定相とする石英キ
ャピラリカラムは最高使用温度が２５０°Ｃ程度である
ため、高沸点物質の分離、分析ができない。もう一つの
欠点は、他の固定相を用いた場合に比べて、カラムの寿
命が短いことである。However, since the maximum operating temperature of a quartz capillary column using polyethylene glycol as a stationary phase is approximately 250°C, it is not possible to separate or analyze high-boiling substances. Another drawback is the short lifetime of the column compared to other stationary phases.
その原因は、キャリアガス中に含まれる微量の酸素によ
る酸化である。The cause of this is oxidation caused by a trace amount of oxygen contained in the carrier gas.
それ故本発明の目的は、ポリエチレングリコールから成
る固定相を有する石英キャピラリカラムの耐熱性と耐久
性を向上させることにある。Therefore, it is an object of the present invention to improve the heat resistance and durability of a quartz capillary column having a stationary phase made of polyethylene glycol.
本発明では、ポリエチレングリコールから成る固定相を
有する石英キャピラリカラムの耐熱性と耐久性を向上さ
せるため、アルキル基を有するシリコーンの層でポリエ
チレングリコール層の表面を被覆して、固定相とした。In the present invention, in order to improve the heat resistance and durability of a quartz capillary column having a stationary phase made of polyethylene glycol, the surface of the polyethylene glycol layer was coated with a layer of silicone having an alkyl group to form the stationary phase.
アルキル基を有するシリコーンとしては、例えばポリジ
メチルシロキサン、ポリフェニルメチルシロキサン等を
用いることができる。As the silicone having an alkyl group, for example, polydimethylsiloxane, polyphenylmethylsiloxane, etc. can be used.
ポリエチレングリコール層の厚さは、ポリエチレングリ
コール層を単独で固定相として用いる場合と同様でよい
。アルキル基を有するシリコーンの層の厚さは、０．１
μｍ以下とすることが好ましい。The thickness of the polyethylene glycol layer may be the same as when the polyethylene glycol layer is used alone as a stationary phase. The thickness of the silicone layer with alkyl groups is 0.1
It is preferable to set it to below micrometer.
石英キャピラリ内面には、ガラス表面に存在する水酸基
を不活性化するため、固定相を設ける前に不活性化処理
を施すことが好ましい。不活性化処理はシランカプリン
グ剤の存在下に高温（例えば４００°Ｃ）で十数時間処
理することにより行うことができる。In order to inactivate the hydroxyl groups present on the glass surface, it is preferable to perform an inactivation treatment on the inner surface of the quartz capillary before providing the stationary phase. The inactivation treatment can be carried out by treatment at a high temperature (for example, 400° C.) for more than ten hours in the presence of a silane coupling agent.
ポリエチレングリコール層とその表面を覆うポリジメチ
ルシロキサン等の層から成る固定相を用いることにより
、石英キャピラリカラムの最高使用温度が２５０°Ｃか
ら約３５０°Ｃまで上昇する。By using a stationary phase consisting of a layer of polyethylene glycol and a layer of polydimethylsiloxane or the like covering the surface, the maximum operating temperature of the quartz capillary column is increased from 250°C to about 350°C.
また、ガスクロマトグラフィに使用したときの寿命が約
３倍に延びる。これは、キャリアガス中に含まれる微量
の酸素等による劣化が防止されるためと考えられる。Furthermore, the lifespan when used in gas chromatography is approximately three times longer. This is thought to be because deterioration due to trace amounts of oxygen contained in the carrier gas is prevented.
以下、実施例により本発明をさらに詳細に説明する。Hereinafter, the present invention will be explained in more detail with reference to Examples.
第１図のような断面を持つ石英キャピラリカラムを製作
した。石英キャピラリカラムは石英キャピラリ１の一内
面に固定相となるポリエチレングリコール層２およびポ
リジメチルシロキサン層３、外側にポリイミドから成る
耐熱保護層４を具える。A quartz capillary column with a cross section as shown in Figure 1 was fabricated. The quartz capillary column includes a polyethylene glycol layer 2 and a polydimethylsiloxane layer 3 serving as a stationary phase on one inner surface of a quartz capillary 1, and a heat-resistant protective layer 4 made of polyimide on the outside.
この石英キャピラリカラムを製造するには、ポリイミド
耐熱保護層４で被覆された石英キャピラリ１を長さ５０
ｍに切断し、常法により石英キャピラリ１の内面をシリ
ル化し、内面に厚さ０．３μｍのポリエチレングリコー
ル層２をスタティック法により形成させ、常法によりポ
リエチレングリコールを架橋させた。さらにその内表面
に、厚さ０．０５μｍのポリジメチルシロキサンの膜３
をスタティック法により形成させ、固定相とした。In order to manufacture this quartz capillary column, a quartz capillary 1 coated with a polyimide heat-resistant protective layer 4 has a length of 50 mm.
The inner surface of the quartz capillary 1 was silylated by a conventional method, a polyethylene glycol layer 2 having a thickness of 0.3 μm was formed on the inner surface by a static method, and the polyethylene glycol was crosslinked by a conventional method. Furthermore, on the inner surface, a polydimethylsiloxane film 3 with a thickness of 0.05 μm is applied.
was formed by a static method and used as a stationary phase.
ポリジメチルシロキサン膜３の厚さは、溶液の濃度によ
り調整した。The thickness of the polydimethylsiloxane film 3 was adjusted by the concentration of the solution.
同じ方法で製造した条長５０ｍの石英キャピラリカラム
４本を、日立Ｇ３０００形ガスクロマトグラフ装置（■
日立製作所商品）に装着し、２．６ジメチルフエノール
標準試料のガスクロマトグラフィを行い、分離特性を評
価した。カラムオーブンの温度は１２０°Ｃ１試料注入
口および検出部の温度は２２０°Ｃとした。５本のキャ
ピラリ試料のいずれも、検出ピークから求めた理論段数
は３７００段／ ｍ ’−，保持比は１３．５、保持指
標Ｒ１は１８９０であった。Four quartz capillary columns with a length of 50 m manufactured using the same method were installed on a Hitachi G3000 gas chromatograph system (■
(Hitachi, Ltd. product), gas chromatography was performed on a standard sample of 2.6 dimethylphenol, and the separation characteristics were evaluated. The temperature of the column oven was 120°C, and the temperature of the sample injection port and detection section was 220°C. For all of the five capillary samples, the number of theoretical plates determined from the detected peak was 3700 plates/m'-, the retention ratio was 13.5, and the retention index R1 was 1890.
上記の５本の石英キャピラリカラムを、ガスクロマトグ
ラフ装置中においてそれぞれ温度２５０”Ｃ，２７５°
Ｃ，３００°Ｃ，３２５°Ｃ，３５０°Ｃに保持して１
０時間ヘリウムガスをカラムに流した後、上記と同じ条
件で２，６−シメチルフエノール標準試料のガスクロマ
トグラフィを行い、分離特性を評価した。その結果を、
熱処理前の特性とともに第１表に示した。The above five quartz capillary columns were placed in a gas chromatograph at a temperature of 250"C and 275°C, respectively.
C, held at 300°C, 325°C, 350°C 1
After flowing helium gas through the column for 0 hours, a standard sample of 2,6-dimethylphenol was subjected to gas chromatography under the same conditions as above to evaluate the separation characteristics. The result is
Table 1 shows the characteristics before heat treatment.
第１表
第１表から明らかなように、本発明の石英ヰヤピラリカ
ラムは熱処理温度２５０″Ｃ〜３５０°Ｃの範囲におい
て、熱処理前のものと比べ、理論段数、保持比、保持指
標Ｒ１とも誤差の範囲以上には変化していない。すなわ
ち、３５０°Ｃまで使用できる耐熱性を有している。Table 1 As is clear from Table 1, in the heat treatment temperature range of 250″C to 350°C, the quartz fiber column of the present invention has fewer errors in the number of theoretical plates, retention ratio, and retention index R1 than the one before heat treatment. It does not change beyond the range.In other words, it has heat resistance that can be used up to 350°C.
上記と同じ方法で製造した条長５０ｍの石英キャピラリ
カラム３本を別に用意し、ガスクロマトグラフィに連続
使用したところ、３ケ月間使用できた。Three 50 m long quartz capillary columns manufactured in the same manner as above were separately prepared and used continuously for gas chromatography for 3 months.
本発明の効果を明らかにするため、従来のポリエチレン
グリコール層のみで構成された固定相について、ガスク
ロマトグラフィの分離特性を評価した。In order to clarify the effects of the present invention, the gas chromatography separation characteristics of a conventional stationary phase composed only of a polyethylene glycol layer were evaluated.
第２図のように、石英キャピラリ１の内面にポリエチレ
ングリコール層２、外側にポリイミドから成る耐熱保護
層４を具える石英キャピラリカラムを製作した。As shown in FIG. 2, a quartz capillary column was fabricated, comprising a polyethylene glycol layer 2 on the inner surface of a quartz capillary 1 and a heat-resistant protective layer 4 made of polyimide on the outer surface.
実施例と同様にポリイミド耐熱保護層４で被覆された石
英キャピラリ１を長さ５０ｍに切断し、内面をシリル化
し、内面に厚さ０．３５μｍのポリエチレングリコール
層２をスタティック法により形成させ、常法によりポリ
エチレングリコールを架橋させた。A quartz capillary 1 coated with a polyimide heat-resistant protective layer 4 was cut into a length of 50 m in the same manner as in the example, the inner surface was silylated, a polyethylene glycol layer 2 with a thickness of 0.35 μm was formed on the inner surface by a static method, and Polyethylene glycol was crosslinked by the method.
同じ方法で製造した条長５０ｍの石英キャピラリカラム
４本について、熱処理前および２５０°Ｃないし３２５
°Ｃの熱処理後に、上記実施例と同様の条件でガスクロ
マトグラフィを行い、分離特性を評価した。その結果は
第２表に示す通りである。Four quartz capillary columns with a length of 50 m manufactured by the same method were tested before heat treatment and at 250°C to 325°C.
After heat treatment at °C, gas chromatography was performed under the same conditions as in the above example to evaluate separation characteristics. The results are shown in Table 2.
第２表
第２表から明らかなように、従来のポリエチレングリコ
ール層のみで構成された固定相は、２５０°Ｃを超える
温度では時間とともに理論段数、保持指標、保持比がい
ずれも低下し、使用に耐えない。Table 2 As is clear from Table 2, the number of theoretical plates, retention index, and retention ratio of the conventional stationary phase composed only of a polyethylene glycol layer decreases with time at temperatures exceeding 250°C. I can't stand it.
同じ方法で製造した条長５０ｍの石英キャピラリカラム
３本を別に用意し、ガスクロマトグラフィに連続使用し
たところ、寿命は１ケ月であった。Three quartz capillary columns with a length of 50 m manufactured by the same method were separately prepared and used continuously for gas chromatography, and the lifespan was one month.
本発明によると、ポリエチレングリコールから成る固定
相を有する石英キャピラリカラムの耐熱性が向上し、石
英キャピラリカラムの最高使用温度が２５０°Ｃから約
３５０°Ｃまで上昇する。また耐久性が向上し、ガスク
ロマトグラフィに使用したときの寿命が約３倍に延びる
。According to the present invention, the heat resistance of a quartz capillary column having a stationary phase made of polyethylene glycol is improved, and the maximum operating temperature of the quartz capillary column is increased from 250°C to about 350°C. It also has improved durability, extending its lifespan by about three times when used in gas chromatography.
第１図は本発明による石英キャピラリカラムの一実施例
の断面図、第２図は従来の石英キャピラリカラムの断面
図である。
符号の説明
１−−−−−−−−−−石英キャピラリ２−−−−一・
−−−−−ポリエチレングリコール層３−−−−−・−
−一−−ポリジメチルシロキサン層４−−−一−−−−
耐熱保護層FIG. 1 is a sectional view of an embodiment of a quartz capillary column according to the present invention, and FIG. 2 is a sectional view of a conventional quartz capillary column. Explanation of symbols 1---------Quartz capillary 2---1・
------Polyethylene glycol layer 3-------・-
-1--Polydimethylsiloxane layer 4--1----
heat resistant protective layer
Claims (2)
スキャピラリカラムにおいて、 前記固定相がポリエチレングリコール層とその内表面に
被覆されたポリジメチルシロキサン等のアルキル基を有
するシリコーンの層から成ることを特徴とする石英キャ
ピラリカラム。(1) A quartz glass capillary column having a stationary phase on the inner surface of the quartz capillary, characterized in that the stationary phase consists of a polyethylene glycol layer and a layer of silicone having an alkyl group such as polydimethylsiloxane coated on the inner surface of the polyethylene glycol layer. quartz capillary column.
μｍ以下の厚さを有する、請求項第１項の石英キャピラ
リカラム。(2) The silicone layer having the alkyl group is 0.1
The quartz capillary column of claim 1, having a thickness of less than μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11798890A JPH0413967A (en) | 1990-05-07 | 1990-05-07 | Quartz capillary column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11798890A JPH0413967A (en) | 1990-05-07 | 1990-05-07 | Quartz capillary column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0413967A true JPH0413967A (en) | 1992-01-17 |
Family
ID=14725245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11798890A Pending JPH0413967A (en) | 1990-05-07 | 1990-05-07 | Quartz capillary column |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0413967A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0968522A (en) * | 1995-08-31 | 1997-03-11 | Toray Res Center:Kk | Decomposing product analyzing method in sf6 gas |
| CN100449310C (en) * | 2005-12-30 | 2009-01-07 | 中国石油化工股份有限公司 | Quartz capillary tube chromatographic column and method for making same |
-
1990
- 1990-05-07 JP JP11798890A patent/JPH0413967A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0968522A (en) * | 1995-08-31 | 1997-03-11 | Toray Res Center:Kk | Decomposing product analyzing method in sf6 gas |
| CN100449310C (en) * | 2005-12-30 | 2009-01-07 | 中国石油化工股份有限公司 | Quartz capillary tube chromatographic column and method for making same |
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