Estimation of measurement uncertainty in chemical analysis

Self-test 10.5 A

Description

In a steelworks chemical laboratory the nickel content of steel is determined using flame atomic absorption spectrometry (FAAS). For the estimation of the within lab reproducibility they use a steel control sample with nickel content of around 8%. An X control chart is maintained with control sample (data are below). The laboratory has participated in 5 interlaboratory comparisons (data are below).

Data

X control chart:

Date Ni content (%)
01.08.2015 7.96
02.08.2015 7.77
05.08.2015 8.03
06.08.2015 7.92
07.08.2015 8.21
08.08.2015 8.27
09.08.2015 8.17
12.08.2015 8.10
11.08.2015 8.27
13.08.2015 8.16
14.08.2015 8.00
15.08.2015 8.04
16.08.2015 7.79
19.08.2015 8.08
20.08.2015 7.76
21.08.2015 8.20
22.08.2015 7.72
23.08.2015 7.82
26.08.2015 7.68
27.08.2015 7.96

 

Proficiency tests data:

No Consensus value (%) Standard deviation
of participants (%) 
Result of the
laboratory (%)
No of participants
1 7.72 0.19 8.06 30
2 8.49 0.20 8.67 29
3 9.23 0.30 9.66 35
4 7.89 0.21 8.11 30
5 10.25 0.16 10.01 32

 

From the control chart the random component u(Rw) can be calculated. That is actually the standard deviation.

Using the proficiency tests data, calculate the biasiu(Crefi), RMSbias and u(Cref). Combine RMSbias and the u(Cref). Consensus values can be considered as the Cref  values in the Nordtest approach.

Combine the u(Rw) and the u(bias). Calculate the expanded uncertainty from the standard uncertainty (via multiplying with coverage factor).

 

Task 1

Please calculate the expanded uncertainty of this analysis (at k = 2 level) for a sample with nickel content 10.2% using absolute uncertainties.

 

Task 2

Please calculate the expanded uncertainty of this analysis (at k = 2 level) for a sample with nickel content 10.2% using relative uncertainties.

Task 3
Which uncertainty estimation would you rather use?

Task 4
Laboratory has participated in two consecutive years in interlaboratory comparisons (ILCs)of waste water and has obtained the following results for fluoride ion content: 0.99 mg/l and 3.92 mg/l. The reference values of the ILCs for fluoride (obtained by independent expert labs) were 1.14 mg/l and 3.77 mg/l, respectively. The laboratory routinely analyses only drinking water, not waste water (drinking water is a matrix of much simpler composition than waste water). Within-lab long-term reproducibility sRW of the laboratory’s procedure for fluoride determination at roughly 2 mg/l level as found from the X control chart is 0.04 mg/l. The procedure used at laboratory does not have detectable bias. Which of the following statements are necessarily true?


 

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