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布鲁克Bruker---X射线荧光光谱分析备样技术.ppt


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布鲁克Bruker---X射线荧光光谱分析备样技术
分析层的厚度:无限厚
X-ray tube
to soller slit
(collimator)
analysed layer
(saturation depth)
Sam布鲁克Bruker---X射线荧光光谱分析备样技术
分析层的厚度:无限厚
X-ray tube
to soller slit
(collimator)
analysed layer
(saturation depth)
Sample
分析层的厚度:无限厚
Sample
B KA1 (0,18 keV)
Sn LA1 (3,4 keV)
Cr KA1 (5,4 keV)
Sn KA1 (25,2 keV)
tube
to soller slit
Is your sample homogeneous ?
Analysed layer on the sample surface
no excitation within the inner (upper) part of the sample
the lower parts (layers) of the sample can be excited (by short wavelengths) but emmitted radiation will be absorbed within the sample
fluorescence radiation to be measured comes from a layer near the sample (specimen) surface
分析层的厚度:无限厚
0,01 mm = 10 nm = 100 A
atom radius: 0,5 - 3 A
tube
分析层的厚度:对于轻基体(如液体)
Light matrix
颗粒效应: 不均匀的颗粒样品
CaCO3
SiO2
压片样品
松散样品
颗粒效应:不均匀的颗粒样品
分析层 !!
analysed layer
颗粒效应:不均匀的颗粒样品
松散样品
Na to U
absorption in foil
He flushing required ?
for qualitative and semiquantitative analysis
for quantitative analysis in special cases only(一般是压不成片的时候)
压片制样
press
as pure pellet
on a support of boric acid
in steel rings
in aluminium cups
add binder if necessary
wax ( C and H)
boric acid ( B, H and O)
压片制样的精密度
熔融制样
熔融设备
马弗炉
燃气炉
inductively heated
熔剂
lithiumtetraborate Li2B4O7
lithiummetaborate LiBO2
mixtures of Li2B4O7 and LiBO2
白金坩埚 (crucibles and moulds)
Analysis of Raw Meal Samples Pressed pellets versus fused beads
Samples
six certified reference materials (Holderbank)
Two different preparation methods
fused beads
g of material
g of flux
pressed pellets with 20% of wax
Analysis of Raw Meal Samples Pressed pellets versus fused beads
压片制样和熔融制样的分析结果的比较
压片制样和熔融制样的分析结果的比较
The comparison of the two different preparation methods clearly shows:
sensitivities and LLD´s are better for pressed pellets
the accuracy is much better for fused beads
up to a factor of 10 for SiO2
液体样品
水,油, 溶液,泥浆, ...
尽量不要分析对仪器有腐蚀或

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  • 页数32
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  • 时间2022-04-22