ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">1ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">峰拖尾 portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
1、篩板阻塞
a、反沖色譜柱
portant; word-wrap: break-word !important; font-size: 14px;">b、更換進口篩板
portant; word-wrap: break-word !important; font-size: 14px;">c、更換色譜柱
2、色譜柱塌陷
填充色譜柱
3、干擾峰
a、使用更長的色譜柱
b、改變流動相或更換色譜柱
4、流動相PH選擇錯誤
調整PH值。對于堿性化合物,低PH值更有利于得到對稱峰
5、樣品與填料表面的溶化點發生反應
portant; word-wrap: break-word !important; font-size: 14px;">a、加入離子對試劑或堿性揮發性修飾劑
b、更改色譜柱
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">2ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">峰前延portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、柱溫低portant; word-wrap: break-word !important; font-size: 14px;">
升高柱溫
2、樣品溶劑選擇不恰當
使用流動相作為樣品溶劑
3、樣品過載
降低樣品含量
4、色譜柱損壞
更換色譜柱
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">3ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">峰分叉portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、 保護柱或分析柱污染portant; word-wrap: break-word !important; font-size: 14px;">
取下保護柱再進行分析。如果必要更換保護柱。如果分析柱阻塞,拆下來清洗。如果問題仍然存在,可能是柱子被強保留物質污染,運用適當的再生措施。如果問題仍然存在,入口可能被阻塞,更換篩板或更換色譜柱。
2、樣品溶劑不溶于流動相
改變樣品溶劑。如果可能采取流動相作為樣品溶劑。
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">4ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">峰變形portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、樣品過載portant; word-wrap: break-word !important; font-size: 14px;">
減少樣品載量
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">5ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">早出的峰變形portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、樣品溶劑選擇不恰當portant; word-wrap: break-word !important; font-size: 14px;">
a、減少進樣體積
b、運用低極性樣品溶劑
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">6ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">早出峰拖尾程度大于晚出峰portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、柱外效應portant; word-wrap: break-word !important; font-size: 14px;">
a、調整系統連接(使用更短、內徑更小的管路)
b、使用小體積的流通池
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">7ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">K’增加時,脫尾更嚴重portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、二級保留效應,反相模式portant; word-wrap: break-word !important; font-size: 14px;">
a、加入三乙胺(或堿性樣品)
b、加入乙酸(或酸性樣品)
c、加入鹽或緩沖劑(或離子化樣品)
d、更換一支柱子
portant; word-wrap: break-word !important; font-size: 14px;">
2、二級保留效應,正相模式
a、加入三乙胺(或堿性樣品)
b、加入乙酸(或酸性樣品)
c、加入水(或多官能團化合物)
d、試用另一種方法
3、二級保留效應,離子對
加入三乙胺(或堿性樣品)
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">8ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">酸性或堿性化合物的峰拖尾portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、緩沖不合適portant; word-wrap: break-word !important; font-size: 14px;">
a、使用濃度50-100mM的緩沖液
b、使用Pka等于流動相PH值的緩沖液
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">9ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">額外的峰portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、樣品中有其他組份portant; word-wrap: break-word !important; font-size: 14px;">
2、前一次進樣的洗脫峰
a、增加運行時間或梯度斜率
b、提高流速
portant; word-wrap: break-word !important; font-size: 14px;">
3、空位或鬼峰
a、檢查流動相是否純凈
b、使用流動相作為樣品溶劑
c、減少進樣體積
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">10ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">保留時間波動portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、溫控不當portant; word-wrap: break-word !important; font-size: 14px;">
調好柱溫
2、流動相組分變化
防止變化(蒸發、反應等)
3、色譜柱沒有平衡
在每一次運行之前給予足夠的時間平衡色譜柱
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">11ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">保留時間不斷變化portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、流速變化portant; word-wrap: break-word !important; font-size: 14px;">
重新設定流速
2、泵中有氣泡
從泵中除去氣泡
3、流動相選擇不恰當
a、更換合適的流動相
b、選擇合適的混合流動相
portant; word-wrap: break-word !important; font-size: 14px;">
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">12ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">基線漂移portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、柱溫波動portant; word-wrap: break-word !important; font-size: 14px;">
控制好柱子和流動相的溫度,在檢測器之前使用熱交換器
2、流動相不均勻。(流動相條件變化引起的基線漂移大于溫度導致的漂移。)
使用HPLC級的溶劑,高純度的鹽和添加劑。流動相在使用前進行脫氣,使用中使用氦氣。
3、流通池被污染或有氣體
用甲醇或其他強極性溶劑沖洗流通池。如有需要,可以用1N的硝酸。(不要用鹽酸)
4、檢測器出口阻塞。(高壓造成流通池窗口破裂,產生噪音基線)
取出阻塞物或更換管子。參考檢測器手冊更換流通池窗。
5、流動相配比不當或流速變化
更改配比或流速。為避免這個問題可定期檢查流動相組成及流速。
6、柱平衡慢,特別是流動相發生變化時
用中等強度的溶劑進行沖洗,更改流動相時,在分析前用10-20倍體積的新流動相對柱子進行沖洗。
7、流動相污染、變質或由低品質溶劑配成
檢查流動相的組成。使用高品質的化學試劑及HPLC級的溶劑
8、樣品中有強保留的物質(高K’值)以饅頭峰樣被洗脫出,從而表現出一個逐步升高的基線。
使用保護柱,如有必要,在進樣之間或在分析過程中,定期用強溶劑沖洗柱子。
9、使用循環溶劑,但檢測器未調整。
重新設定基線。當檢測器動力學范圍發生變化時,使用新的流動相。
10、檢測器沒有設定在最大吸收波長處。
將波長調整至最大吸收波長處
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">13ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">基線噪音(規則的)portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、在流動相、檢測器或泵中有空氣portant; word-wrap: break-word !important; font-size: 14px;">
流動相脫氣。沖洗系統以除去檢測器或泵中的空氣。
2、漏液
檢查管路接頭是否松動,泵是否漏液,是否有鹽析出和不正常的噪音。如有必要,更換泵密封。
3、流動相混合不完全
用手搖動使混合均勻或使用低粘度的溶劑
4、溫度影響(柱溫過高,檢測器未加熱)
減少差異或加上熱交換器
5、在同一條線上有其他電子設備
斷開LC、檢測器和記錄儀,檢查干擾是否來自于外部,加以更正。
6、泵振動
在系統中加入脈沖阻尼器
ntnet="t" style="margin: 0px; padding: 0px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; float: left; width: 40px; height: 40px; text-align: center; color: rgb(255, 255, 255); font-size: 24px; line-height: 40px; background-color: rgb(13, 12, 12);">14ntent="t" style="margin: 0px; padding: 0px 15px; max-width: 100%; box-sizing: border-box !important; word-wrap: break-word !important; width: auto; display: inline-block; float: left; height: 40px; font-size: 18px; line-height: 35px; border-bottom-width: 2px; border-bottom-style: solid; border-bottom-color: rgb(13, 12, 12); border-top-width: 2px; border-top-style: solid; border-top-color: rgb(13, 12, 12);">基線噪音portant; word-wrap: break-word !important; font-size: 14px;">
portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、 漏液portant; word-wrap: break-word !important; font-size: 14px;">
檢查接頭是否松動,泵是否漏液,是否有鹽析出和不正常的噪音。如有必要,更換密封。檢查流通池是否漏液。
2、流動相污染、變質或由低質溶劑配成
檢查流動相的組成。
3、流動相各溶劑不相溶
選擇互溶的流動相
4、檢測器/記錄儀電子元件的問題
斷開檢測器和記錄儀的電源,檢查并更正。
5、系統內有氣泡
用強極性溶液清洗系統
6、檢測器內有氣泡
清洗檢測器,在檢測器后面安裝背景壓力調節器
7、流通池污染(即使是極少的污染物也會產生噪音。)
用1N的硝酸(不能用磷酸)清洗流通池
8、檢測器燈能量不足
更換燈
9、色譜柱填料流失或阻塞
更換色譜柱
10、流動相混合不均勻或混合器工作不正常
維修或更換混合器,在流動相不走梯度時,建議不使用泵的混合裝置
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portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、流動相組成變化portant; word-wrap: break-word !important; font-size: 14px;">
重新制備新的流動相
2、流動相流速太低
調節流速
3、漏液(特別是在柱子和檢測器之間)
檢查接頭是否松動、泵是否漏液、是否有鹽析出以及不正常的噪音。如果必要更換密封。
4、檢測器設定不正確
調整設定
5、柱外效應影響
a、柱子過載
b、檢測器對反應時間或池體積響應過大
c、柱子與檢測器之間的管路太長或管路內徑太大
d、記錄儀響應時間太長
6、緩沖液濃度太低
增加濃度
7、保護柱污染或失效
更換保護柱
8、色譜柱污染或失效,塔板數較低
更換同樣類型的色譜柱。如果新柱子可以提供對稱的色譜峰,則用強溶劑沖洗舊柱子。
9、柱入口塌陷
打開柱入口,填補塌陷或更換柱子
10、呈現兩個或多個未被完全分離的物質的峰
選擇其它類型的色譜柱以改善分離效果
11、柱溫過低
提高柱溫。除非特殊情況,溫度不宜超過75℃
12、檢測器時間常數太大
使用較小的時間常數
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portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、流動相污染或變質(引起保留時間變化)portant; word-wrap: break-word !important; font-size: 14px;">
重新配置流動相
2、保護柱或分析柱阻塞
去掉保護柱進行分析。如果必要則更換保護柱。如果分析柱阻塞,可進行反沖。如果問題仍然存在色譜柱可能被強保留的污染物損壞,建議使用恰當的再生程序。如果問題仍然存在,進口可能阻塞了,更換入口處的篩板或更換色譜柱。
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portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、檢測器衰減設定過高portant; word-wrap: break-word !important; font-size: 14px;">
減少衰減的設定
2、檢測器時間常數設定太大
設定較小的時間常數
3、進樣量太少
增大進樣量
4、記錄儀連接不當
使用正確的連接
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portant; word-wrap: break-word !important; font-size: 14px;">原因和解決方法
portant; word-wrap: break-word !important; font-size: 14px;">1、檢測器衰減設定過低portant; word-wrap: break-word !important; font-size: 14px;">
采取較大的衰減
2、進樣過多
減少進樣量
3、記錄儀連接不正確
正確連接記錄儀