Metallurgical Industry

Determination of Pb, Ca, Ti and Al Content in Iron Powder and Tin-based Alloy Welding Powder

1 Sample solution preparation:
0.2g sample (precision to 0.0001g) was weighed and placed in a 250mL high neck beaker, 10mL aqua regia (HCl: HNO3 = 3:1) was added, covered with glass lid, heated on hot plate until the sample digests.  Then, it was removed for cooling, transferred to a 25 mL volumetric flask, rinsed and made up to the volume with deionized water, shaken well, spared for later use.

2 Experimental equipment and reagents 
AA7000 series atomic absorption spectrophotometer (with Pb, Ca, Ti, Al hollow cathode lamp, EWAI Inc.)
Temperature-controlled hot plate
Nitric acid (HNO3): excellent grade purity
Hydrochloric acid (HCl): excellent grade purity
Lead standard solution (National Reference Materials Research Center)
Calcium standard solution (National Reference Materials Research Center)
Titanium standard solution (National Reference Materials Research Center)
Aluminium standard solution (National Reference Materials Research Center)
 
3 Instrument conditions
Parameter Wavelength
(nm)
Slit width(nm) Burner height(mm) Fuel gas flow rate(L/min) Lamp current(mA) Flame type
Pb 283.3 0.2 10 1.5 3.0 Air – acetylene
Ca 422.7 0.2 10 1.5 3.0 Air – acetylene
Ti 364.2 0.2 8 3.0 3.0 Air – acetylene
Al 309.3 0.2 8 3.0 3.0 Air - acetylene

4 Standard solution preparation
Element Concentration(μg/mL)
Pb 0 0.5 1.0 2.0 3.0
Ca 0 0.5 1.0 2.0 3.0
Ti 0 5.0 10.0 15.0  
Al 0 2.0 4.0 8.0 10.0

5 Standard curve
\
Pb Curve equation:y=0.02379*x+0.00086
Linearity coefficient:1.00000
\ 
Ca Curve equation:Y=0.08469*X+0.00431
Linearity coefficient:0.99970
\
 Ti Curve equation:Y=0.00076*X+0.00107
 Linearity coefficient:0.99990
\ 
Al Curve equation:Y=0.00323*X-0.00051
Linearity coefficient:0.99960

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