Excelet

What to do if the sample matrix interferes?

Standard Additions

Click tabs to navigate!!!

interferes?
Sample Matrix Interference
instrumental response
matrix of standards a= 7.3 b= 1.2 R= 0.87 87
simple complicated
c A A' slope = ab
1
0 0 0 A' Linear (A') 8.76
0.010 0.088 0.076 0.9 0 0.5
0.020 0.175 0.152 0.8 f(x) = 8.760.057078
x 0.5 slope = Rab
0.030 0.263 0.229 0.7 0.065606
f(x) = 7.6212 x 0.5 7.6212
0.040 0.350 0.305 0.065606 0
A 0.6
0.050 0.438 0.381 0.057078 0 unknown A
0.5
0.070 0.613 0.533 0.057078 0.5 0.5
0.100 0.876 0.762 0.4
0.3
0.2
The real problem can be that we
0.1
cannnot match the matrix to get
correct results! So, what are 0
0 0.01 0.02 0.03 concentration,
0.04 0.05 M
0.06 0.07 0.08 0.09 0.1
the possiblilities?

interpolation: c = 0.057 c' = 0.066 error = -13.0

Sinex 2009
slope = Rab
Making the Standards for Standard Additions
In standard additions the unknown is spiked with a varying known concentration of standard.
1 2 3 4 5 6

0
3 3 3 3 3 3
3 3 3 3 3 3
3 3 3 3 3 3
3 3 3 3 3 3
3 3 3 3 3 2
3 3 3 3 2 2
3 3 3 2 2 2
3 3 2 2 2 2
3 2 2 2 2 2
1 1 1 1 1 1

1 part unknown 1 part unknown 1 part unknown 1 part unknown 1 part unknown 1 part unknown
0 part standard 1 part standard 2 parts standard 3 parts standard 4 parts standard 5 parts standard

In this order - step 1: ✘ 1 of unknown

add aliquot this is a constant amount to all tubes

step 2: ✘ 1
add standard in increasing known amounts increasing known volume of standard

step 3: ✘ 1
fill remaining volume with water fill remaining volume with water to mark
and then mix the contents up and analzye!!!!

Sinex 2009
The Standard Additions Calibration Curve

✘ 1 for standards in distilled water

add comparison graph
Input parameters
C std = 1
Co= 0.1 0.5 0 0.076212
V unk = 50 0.45 0.0087 0.076212
f(x) = 7.6212 x + 0.076212
V flask = 500 slope - no interfer 0.4 f(x) = 8.76 x
0.0087 0
slope = 7.6212 8.76 0.35
0.3
A
V std C sa A sa A 0.25
0 0 0.076212 0 0.2
5 0.01 0.152424 0.0876
0.15
10 0.02 0.228636 0.1752
0.1
15 0.03 0.304848 0.2628
0.05
20 0.04 0.38106 0.3504
25 0.05 0.457272 0.438 0
-0.02 -0.01 0 concentration,
0.01 0.02 M0.03 0.04 0.05 0.06
-0.01 0
slope 7.6212 m
y-intercept 0.076212 b Co= 0.1 undiluted A= 0.076212 c= 0.0087
x-intercept -0.01 -b/m without standand additions
for the green line C diluted = 0.01 error = -13

The slope of this plot is controlled by the instrument response on the response change tab!

Sinex 2009
Influence of Random Error on Standard Additions
Random error
none 4 high small amount range
Input parameters
C std = 1 f(x) = NaN x + NaN
Co= 0.1 R² =12
0
V unk = 50
10
V flask = 250 slope - no interfer
slope = 7.6212 8.76
8
A
V std C sa A sa A6 random error
0 0 #ADDIN? 0 #ADDIN?
5 0.02 4
#ADDIN? #ADDIN? #ADDIN?
10 0.04 #ADDIN? #ADDIN? #ADDIN?
15 0.06 2
#ADDIN? #ADDIN? #ADDIN?
20 0.08 #ADDIN? #ADDIN? #ADDIN?
0
25 0.1 #ADDIN? #ADDIN? #ADDIN?
0 0.02 0.04 concentration,
0.06 M 0.08 0.1 0.12
#ADDIN? 0
slope #ADDIN?
y-intercept #ADDIN? C o = #ADDIN?
x-intercept #ADDIN? error = #ADDIN? Change the random error to see how the error in influenced.
(After setting a small random error, try alternately clicking
the terminal arrows of the slider and observe the orange point)

The slope (no error) of this plot is controlled by the instrument response on the response change tab!

Sinex 2009