Upload
doankhanh
View
223
Download
0
Embed Size (px)
Citation preview
1 Proprietary & Confidential
The world leader in serving science
Proprietary & Confidential
High performance
for milk powder analysis
ARL OPTIM’X Unique WDXRF system
2 Proprietary & Confidential
Application: Food industry
Food industry
• Nutritional Supplements • Multi-element capability:
Mg, K, Ca, Cr, Mn, Fe, Zn, Cu, Se, Mo, Iodine
• High Throughput
• Advanced quantitative algorithms for optimal accuracy
• Excellent repeatability
• When Na and Mg are required, WDX must be used to get the required performance
3 Proprietary & Confidential
Minerals in milk powders
Indications on the box of a milk powder for
baby
4 Proprietary & Confidential
Minerals in milk powders
Indications on the box of a milk powder for baby
Concentrations are expressed in milli grams per 100g
and micro grams per 100g
6 Proprietary & Confidential
Low Power WDXRF
WD-XRF SmartGonio™
Flexible, versatile, elemental analysis
WD-XRF __Multichromators™
Rapid, dedicated routine analysis
ARL Optim’X
7 Proprietary & Confidential
WDX low power
Mini X-ray tube (50W - air cooled)
Close coupling of optics for optimized sensitivity equivalent
to 200 W
Elemental coverage: F to U
X-ray tube
Vacuum tank
Scintillation
counter
Sample holder
Crystal(s)
SmartGonio Flow Proportional
counter
8 Proprietary & Confidential
ARL OPTIM’X Exclusive SmartGonioTM
Access to all elements from F to U
(3 crystals - 2 detectors fitted)
View of the Moiré fringe SmartGonioTM
9 Proprietary & Confidential
Limits of detection in milk powders
Milk powders prepared as pressed pellets - n.m.=not measured
Element Concentration
range
in milk powders
LoD
SmartGonio
t=60s
(ppm)
LoD
Fixed channel
t=120s
(ppm)
Ca 0 – 1.6 % 10 n.m
Cl 0 – 0.48 % 10 n.m.
Cu 0 – 0.012 % 0.6 n.m.
Fe 0 – 0.33 % 2.1 n.m
K 0 – 1 % 2 n.m
Mg 0 – 0.12 % n.m. 22
Mn 0 – 0.0023 % 1.2 n.m.
Na 0 – 0.03 % n.m. 42
P 0 – 1.1 % 4.4 n.m
Se 0 – 3.4 ppm 0.24 n.m.
Zn 0 – 0.2 % 2 n.m.
10 Proprietary & Confidential
Calibration curves for milk based products: Na, Mg
ARL Optim’X
29 milk based product samples
In this study Na and Mg have
been measured on fixed
channels using sealed detectors
Total Analysis time 10’
The new version of the
SmartGonio (3 crystals) allows
analysis of Na and Mg
Copyright 2004 John Wiley & sons – X-ray spectrom. 2004, 33: 128-135
11 Proprietary & Confidential
Calibration curves for milk based products: P, S, Cl
ARL Optim’X
29 milk based product samples
60s counting time per element
Correction with Rh Compton
ratio
Copyright 2004 John Wiley & sons – X-ray spectrom. 2004, 33: 128-135
12 Proprietary & Confidential
Calibration curves for milk based products: K, Ca, Fe, Zn
Co
pyri
gh
t 2004 J
oh
n W
iley &
so
ns –
X-r
ay s
pectr
om
. 2004, 33:
128
-135
13 Proprietary & Confidential
Milk-based products: Fe repeatability
Iron in milk powder
• Short term repeatability (120 s)
• Standard Deviation: 1.2 ppm at 94 ppm Fe level
9390
94 93 93 94 93 94 93 94
40
45
50
55
60
65
70
75
80
85
90
95
100
105
110
115
120
0 1 2 3 4 5 6 7 8 9 10 11
Run nr.
Co
nce
ntr
ati
on
Fe
(p
pm
)
14 Proprietary & Confidential
Milk-based products: Ca repeatability
Calcium in milk powder
• Short term repeatability (120 s)
• Standard Deviation: 0.026% at 0.75% level Ca
0.66
0.67
0.68
0.69
0.7
0.71
0.72
0.73
0.74
0.75
0.76
0.77
0.78
0.79
0.8
0 2 4 6 8 10
Run nr.
Co
nce
ntr
ati
on
(%
)
15 Proprietary & Confidential
Repeatability of analysis in milk powders
Milk powders prepared as pressed pellets
Element Analytical
Device
Concentration
level of sample
used for
precision test
Precision
(1 sigma)
in 6 runs of the
same pellet
Ca SmartGonio 3860 ppm 33 ppm in 60s
Cu SmartGonio 5 ppm 0.2 ppm in 60s
Fe SmartGonio 60 ppm 2 ppm in 60s
K SmartGonio 6000 ppm 44 ppm in 60s
Mg Fixed channel 500 ppm 11 ppm in 240s
Na Fixed channel 2400 ppm 28 ppm in 240s
P SmartGonio 2600 ppm 18 ppm in 60s
Zn SmartGonio 50 ppm 0.7 ppm in 60s
16 Proprietary & Confidential
Conclusions
• With ARL Optim’X, WDXRF is becoming a standard
technique for the analysis of various elements in milk-based
products
• Different analytical methods are used for optimum accuracy
• The new 200W version of ARL Optim’X can be a good
alternative
• to avoid fitting of Na and Mg fixed channels
• Or to increase the speed of analysis if Na and Mg fixed channels are
fitted
• Higher power instruments (ARL PERFORM’X series) are only
necessary for the most demanding cases