Metallurgical Industry

Detection of Thallium Content in Wastewater Lead Block

1 Sample solution preparation
1.1 Water sample could be introduced into the machine directly.
1.2About 1.0g sample (precision to one-ten-thousandth) was weighed and placed in a conical flask, 15mL 10% nitric acid was added, covered with lid, heated at lower temperature on hot place to digest the sample.  After digestion, it was removed for cooling, then the cup wall was rinsed with deionized water, heated on the hot plate to reduce the acid to about 5mL, transferred into a 25mL volumetric flask, rinsed at least 3 times with deionized water.  Then, it was diluted and made up to the volume to volume, spared for later use.

2 Experimental equipment and reagents
AA7000 series atomic absorption spectrophotometer (with Tl hollow cathode lamp, EWAI Inc.)
Temperature-controlled hot plate
Conical beaker
Nitric acid (HNO3): excellent grade purity
Thallium standard solution (National Reference Materials Research Center)

3 Instrument conditions
Element Wavelength
(λ/nm)
Lamp current
(I/mA)
D2 lamp current(I/mA) Spectral Bandpass width(△λ/nm) Background correction technique
Tl 276.8 2 100 0.2 氘灯
D2 lamp
 
[Graphite furnace  temperature curve]  
No Step Start temp (℃) End temp(℃) Heating time (s) Inner gas path Auxiliary gas path Mode Alarm
1 Drying 40 100 30 Open Off Power Open
2 Drying 100 120 10 Open Off Power Open
3 Ashing 120 600 10 Open Off Power Open
4 Ashing 600 600 8 Open Off Power Open
5 Ashing 600 600 6 Off Off Power Open
6 Atomization 2700 2700 3 Off Off Power Open
7 Cleaning 2700 2700 3 Open Off Power Open
8 Cooling 0 0 22 Open Off Power Open
9 Cooling 0 0 1 Off Off Power Open
 
4 Standard solution preparation
Element   Concentration
Tl(μg/L)  0 2.0 6.0 10.0 20.0
5 Standard curve
 
\ 
Curve equation : Y=0.00737*X+0.00292
Linearity coefficient : 0.99980
 

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