啊啊啊
第2楼2014/07/23
工程师建议的这个方法不见得好,目标物出峰完毕后,我们通常会切到高浓度的淋洗液冲洗色谱柱,此时如果想完全抑制住背景电导,需要很大的电流,比如按照GB 5009.33做亚硝酸盐检测,最高是1mL/min,70mM,按工程师的建议是需要到174mA,而这是完全没有必要的。
抑制器某种程度上来说也是个消耗品,过高的电流会明显降低使用寿命,因此,仍然以GB 5009.33做亚硝酸盐为例,我给你两个建议的方法:
1.淋洗液6mM时抑制器电流设定为50mA就足够,淋洗液70mM阶段,可延迟2分钟将抑制器电流设定为174mA,淋洗液切回6mM后,延迟1分钟将抑制器电流设为50mA;
2.全程抑制器电流设定为50mA,淋洗液70mM冲洗后切回6mM再平衡阶段,加长2分钟。
yfytap
第3楼2014/07/23
同意!
zangfukun
第4楼2014/08/07
很专业的建议!
不过小弟还有一点疑问:在建仪器方法时,抑制器电流好像只能设一个值,您的建议1难道是在仪器界面手动改变电流吗?如果序列中有很多样品,那岂不是要一直守在仪器旁?
啊啊啊
第5楼2014/08/30
变色龙工作站中,仪器方法是有脚本编辑器的,可以在里面直接修改,贴个给你看看,是6.8版本的。
Wait Sampler.Ready
Column_TC.AcquireExclusiveAccess
Compartment_TC.AcquireExclusiveAccess
Pressure.LowerLimit = 200 [psi]
Pressure.UpperLimit = 3000 [psi]
MaximumFlowRamp = 3.00 [ml/min2]
%A.Equate = "%A"
%B.Equate = "%B"
%C.Equate = "%C"
%D.Equate = "%D"
CR_TC = On
InjectMode = PushPartial
CycleTime = 0 [min]
DrawSpeed = 5.0 [μl/s]
DrawDelay = 2.0
DispSpeed = 5.0 [μl/s]
WashDispSpeed = 20.0 [μl/s]
DispenseDelay = 2.0
WasteSpeed = 20.0 [μl/s]
WashSpeed = 20.0 [μl/s]
DilutionMixSpeed = 30.0 [μl/s]
DilutionMixDispenseSpeed = 60.0 [μl/s]
DilutionMixIterations = 3
PunctureOffset = 3.0 [mm]
BufferWashFactor = 2.000
SampleHeight = 2.000 [mm]
WashVolume = 1000.0 [μl]
SyncWithPump = On
InjectWash = AfterInj
Pump_1_Pressure.Step = Auto
Pump_1_Pressure.Average = On
PartialCutVolume = 10.0 [μl]
UV.Data_Collection_Rate = 2.5 [Hz]
TimeConstant = 0.60
CDet1.Data_Collection_Rate = 5.0 [Hz]
Temperature_Compensation = 1.7 [%/°C]
CellHeater.Mode = On
CellHeater.TemperatureSet = 35.00 [°C]
Column_TC.Mode = On
Column_TC.TemperatureSet = 30.00 [°C]
Compartment_TC.Mode = On
Compartment_TC.TemperatureSet = 30.00 [°C]
Suppressor1.Type = ASRS_4mm
CurrentSet = 50 [mA]
; Suppressor1.Carbonate = 0.0
; Suppressor1.Bicarbonate = 0.0
; Suppressor1.Hydroxide = 70.0
; Suppressor1.Tetraborate = 0.0
; Suppressor1.Other eluent = 0.0
; Suppressor1.Recommended Current = 174
UV_VIS_1.Wavelength = 225 [nm]
Flow = 1.000 [ml/min]
%B = 0.0 [%]
%C = 0.0 [%]
%D = 0.0 [%]
Pump_1.Curve = 5
0.000 UV.Autozero
CDet1.Autozero
Concentration = 8.00 [mM]
EGC_1.Curve = 5
Wait UV.Ready and Sampler.Ready
Wait CycleTimeState
Inject
Pump_1_Pressure.AcqOn
CD_1.AcqOn
UV_VIS_1.AcqOn
Concentration = 8.00 [mM]
EGC_1.Curve = 5
25.00 Concentration = 8.00 [mM]
EGC_1.Curve = 5
25.10 Concentration = 70.00 [mM]
EGC_1.Curve = 5
30.00 Concentration = 70.00 [mM]
EGC_1.Curve = 5
30.10 Concentration = 8.00 [mM]
EGC_1.Curve = 5
37.00 Concentration = 8.00 [mM]
EGC_1.Curve = 5
Pump_1_Pressure.AcqOff
CD_1.AcqOff
UV_VIS_1.AcqOff
Compartment_TC.ReleaseExclusiveAccess
Column_TC.ReleaseExclusiveAccess
End
zangfukun
第10楼2014/11/17
按上述方法设置后,当抑制器电流改变时,基线会出现一个较明显的波动,看上去就像一个小峰,这种情况下,抑制器电流是不是要比仪器方法中推荐值稍大一些比较合适?