Verification of the Reporting Limit and Validation

依风1986

2012/10/20

私聊

ICP光谱

Verification of the Reporting Limit and Validation for Soluble Cadmium in small part metal sample

1. Scope

The study is to examine the validation of reporting limit of heavy metal soluble element (Cadmium) in small part metal as sample in accordance with test method CPSC-CH-E1004-11(GC051.TP).

2. Reagent and Apparatus

2.1 Inductively Coupled Argon Plasma Spectrometer.

2.2 Electronic balance 1 Div. = 0.001 g.

2.3 Metal Scissors, stainless steel

2.4 Shaking water bath, 37 ± 2°C

2.7 Conc. Hydrochloric acid (A.R.).

2.8 Deionized water..

2.9 General laboratory apparatus.

3. Experimental

In this study of the reporting limit, one trial was performed on non spike metal sample (free of soluble Cd in metal material) and ten trials were performed on spiked metal sample (free of soluble Cd metal material).

For small part metal materials by soluble extraction according to CPSC-CH-E1004-11(GC051.TP)

0.2g of the sample was weighed in 50 mL conical flask. Add 50 times the mass of sample ,10ml, of 0.07N hydrochloric acid in conical flask and spike with 0.5mg/l of Cd in sample at 37 ± 2°C and shake continuously for 24 hours.The shaking frequency of the shaker was set to 60 rpm. The bath was cover with lid to avoid light during shaking. After 24 hours, decant an aliquot of acid solution from the flask and save for analysis.The percentage recovery, the mean value and the relative standard deviation for studied sample were reported.

4. Result

Validation record of reporting limit of soluble Cadmium in small part metal sample according to GC051.TP
4.1 Spike 0.5 mg/l of Cd into metal sample with 10 replicates and analyzed by ICP
Item description	Soluble Cadnium Content (mg/l in solution)
Item description	Cd (final concentration in solution)	Recovery( %)
A1	0.4971	99.4
A2	0.5015	100.3
A3	0.5165	103.3
A4	0.4876	97.5
A5	0.5062	101.2
A6	0.4840	96.8
A7	0.5259	105.2
A8	0.5251	105.0
A9	0.4814	96.3
A10	0.4949	99.0
Mean	0.5020	100.4
Std. deviation	0.01620	--
RSD (%)	3.23	--

5. Conclusion

The recovery data of the spiked samples were summarsied in the table 1. The relative standard deviations of the spiked metal samples for reporting limit were found to be within 5%. It could be concluded that it is acceptable for the test process and result of reporting limit (0.5mg/l or 5ug of Cd) is satisfactory.

Prepared by : ___________________ Date : ___________________

Checked by : ___________________ Date : ___________________

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