毛细柱的安装
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Capillary Column Installation Quick Reference Guide
毛细柱安装快捷指南
Precolumn installation check list
预检查清单
1. Replace oxygen, moisture, and hydrocarbon traps as needed.
如有必要,替换掉除氧、除湿、除烃的捕集阱。
2. Check gas cylinder pressure to ensure that an adequate supply of carrier, makeup, and fuel gases is available. Minimum carrier gas purity percentages: helium 99.9995, hydrogen 99.9995.
检查气瓶压力,确认载气、补充气、可燃气合适。载气纯度百分比最小应达到:氦气,99.995;氢气,99.995。
3. Clean the injector port, replace critical injection port seals, replace injection port liners, and change septa as needed.
清洗进样口,如有必要,更换密封垫,衬管,隔垫。
4. Check detector seals, and replace as necessary. Clean or replace detector jets as necessary.
检查检测器密封垫,如有必要就替换。如有必要清洗或替换检测器喷嘴。
5. Carefully inspect the column for damage or breakage.
仔细检查柱是否破损。
6. Gather the necessary installation tools: you will need a column cutter, column nuts, ferrules, a magnifying loop, and typewriter correction fluid.
收集必要的安装工具:柱切割器、柱螺母、垫圈、放大镜、打字机改正液。
Installing the column
安装柱
1. Uncoil approximately 0.5m of tubing from the column basket at both ends of the column for injector and detector installation. Avoid sharp bends in the tubing.
从柱圈两端各解开约0.5米的柱,以便进样口和检测器安装。
2. Mount the column in the oven. Use the hanging bracket if available.
在柱箱中装柱。如果可能的话,用柱悬挂架。
3. Install the column nut and Vespel or graphite ferrule at each column end; pull the nut and ferrule down the tubing approximately 5 cm.
在柱两端按装螺母和Vespel或石墨垫。将螺母和垫圈顺着柱拉下约5厘米。
4. Score the column. Use a light touch to score the column about 4 to 5 cm from each end.
切割柱。距柱每个尾端约4-5cm处轻划一下。
5. Make a clean break. Grasp the column between the thumb and forefinger as close to the score point as possible. Gently pull and bend the column. The column should part easily. If the column doesn’t break easily, don’t force it! Score the column again in different place, and try for a clean break.
确保整齐的划口。用拇指和食指抓住柱,离划痕处越近越好。轻轻地弯曲柱。柱应该很容易地折断。如果柱不能折断,不能强行用力。在不同的地方再割一次柱,尝试获是整齐地划口。
6. Use a magnifying loop to inspect the cut. Make sure the cut is square across the tubing with no polyimide or glass fragments at the end of the tube.
用放大镜检查划口。确认划口正交于柱,柱端没有聚酰亚胺或石英碎片。
7. Install the column in the inlet. Check the GC manufacturer’s instrument manual for the correct insertion distance. Mark the correct distance on the column with typewriter correction fluid. Insert the column into the injector. Finger tighten the column nut until it starts to grab the column, and then tighten the nut an additional 1/4 to 1/2 turn so that the column can’t be pulled from the fitting when gentle pressure is applied.
在进样口装柱。查阅GC生产商的仪器说明书,以便获取正确的安装距离。用打字机改正液在柱子上标识正确地距离。将柱插入进样口。用手拧紧柱螺母直至其开始夹住柱子。再拧1/4-1/2圈,这样轻轻拉动时,柱子不会脱出来。
8. Turn on the carrier gas, and establish the proper flow rate. Set head pressure, split flow, and septum purge flow to appropriate levels. See Table B for nominal head pressure. If using a split/splitless inlet, check that the purge valve is ON.
接通载气,调至合适地流速。设置相应的柱头压、分流比、隔垫吹扫。常规地柱头压参考表B。如果使用分流/不分流进样口,检查分流阀是否打开。
9. Confirm carrier gas flow through the column. Immerse the end of the column in a vial of acetone and check bubbles.
确保载气通过了柱子。将柱尾端入丙酮中检查气泡。
10. Install the column into detector. Check the instrument maufacture’s manual for the proper insertion distance.
将柱子装进检测器。查阅仪器生产商的说明书,以便获取合适的安装距离。
11. Check for leaks. This if very important. Don’t enven think about heating the column without thoroughly checking for leaks.
检漏。这非常重要。不能不检漏就加热柱子。
12. Establish proper injector and detector temprature.
给进样口和检测器设定恰当的温度。
13. Establish proper makeup and detector gas flows. Ignite or turn on the detector.
设定恰当的补充气和检测气流量。点火或打开检测器。
14. Purge the column for a minimum of 10 minutes at ambient temperature(approximately six column volumes).
在室温下冷吹柱子至少10分钟(约6倍的柱体积)。
15. Inject a nonretained substance to check for proper injector installation. Examples: butane or methane(FID),headspace vapors from acetonitrile(NPD), methylene chloride(ECD),air(TCD),argon(mass spectrometer). Proper installation is indicated by a symmetrical peak. If tailing is observed, repeat the injector installation process.
进没有保留的物质检查进样口安装是否合适。如丁烷或甲烷(FID),乙腈顶空蒸汽(NPD),氯仿(ECD),空气(TCD),氩气(MSD)。安装合适会得到对称的峰形。如果峰拖尾,重新安装进样口。