Pet food analysis

XRF SALES AND CONSULTING
PET FOOD ANALYSIS USING EDXRF

Whats in Pet
Food ?
5/19/2021 XRF SALES AND CONSULTING 2
In order to be considered a “complete food,”
pet foods do not require mineral
supplements. However, when analyzed, dry
foods will generally consist of 5-8% macro
and trace minerals, each serving different
purposes for your pet’s body.
Source: 2012 Royal Canin Nutrient Guide

14 kinds of
Minerals -
Source: 2012
Royal Canin
Nutrient Guide
Mineral Form Chemical Formula
Calcium Bone meal
Calcium carbonate (chalk)
Calcium phosphate
CaCO3
Ca3(PO4)2
Phosphorus Meat
Wheat
Gluten
Potassium dried fruits, avocado,
meat and smoked fish.
Potassium Citrate K3C6H5O7
Sodium sodium chloride, Sodium
phosphates
NaCl, Na2HPO4
Magnesium Bone Meal, Magnesia Mg(OH)2

+ Chelated Trace
Elements
Element Form Chemical Formula
•Iron Liver
Meat
Fish
Green vegetables
Mineral salts
•Zinc zinc gluconate or
zinc plush methionine
ZnC12H22O14
ZnC10H20N2O4S2
•Copper Lamb
Pork
Duck
Peas
Lentils
Soy
•Manganese Cereals
Grain
Fruits
Mineral salts
•Iodine Sea salt
Fish
•Selenium Mineral salts
Fish
Meats

Assumptions
in XRF
Analysis
-The elements of interest are all in the same physical and
chemical form
The material is homogenous, and the particle size is less
than 80 microns
The moisture content of the material is fairly consistent
.from sample to sample
BASED ON THESE REQUIREMENTS YOU CAN IMAGINE
THAT ANALYSIS OF PET FOOD IN THE “AS RECEIVED
FORM” IS PROBABLY NOT GOING TO BE ACCURATE AND
PRECISION WILL ALSO BE PROBLEMATIC

Steps to take
to prepare
Pet Food for
XRF analysis
Pre -Dry the Dog Food to constant weight using an Infra Red
balance
Homogenize and reduce particle size in a rotary mill/ might need a
cutting mill to prevent smearing of softer minerals during the
sample reduction process.
Analyze a set of dog foods using ICP – you can then attempt to
measure the dog foods as pressed pellets using a hydraulic press or
an arbor press to achieve uniform packing and remove air voids.
The XRF can be calibrated for the desired elements using the ICP
data for secondary reference materials

/
Pros and Cons to the Pressed Powder Method
Pros Cons
Quick , easy sample prep method Subject to inaccuracies once the compounds change
either in concentration or in chemical formula
Lose Powder Method – the easiest prep Also a source of the greatest inaccuracies since air
voids are not reproducible from sample to sample.
It adversely affects Na, Mg analysis to a greater
extent than Ca – Se
Pressed Powders using a hydraulic press Better Na, Mg, K, Ca analysis, still suffers from
Mineralogical Effects

Ideal Method
Dry the material @ 110
degrees C
Ash at 960 degrees for 2 hrs
Weigh 1g of sample ash and
add 5g of LiT flux. Fuse until all
sample particles are dissolved
in the flux
Measure glass bead on XRF
unit.
XRF SALES AND CONSULTING 5/19/2021 8
Pros Cons
Guaranteed
accurate results
More tedious and
costly to prepare

What the
ideal XRF is
going to have
Light element analysis capability (Low kV 4-6kV and high mA
preferably > 1000uA)
◦ You need low excitation voltage just above the Absorption
Edges of the EOI and you need maximum flux to maximize the
number of fluorescent x-rays produced that escape to the
detector
◦ Close coupling for maximized x-ray flux from the sample
reaching the detector
◦ Helium or Vacuum pathway to reduce air absorption of low
energy x-rays of Na and Mg
◦ Thin windowed XRF Silicon Drift Detector to allow maximum
low energy x-rays to be counted.
Intermediate Z analysis – 60kV nice to have , 50kV would be fine
X-ray Tube anode choice probably Rh or Pd – Air analysis mode,

What the Elva X PRO offers
Meet the professional XRF
 ElvaX Pro is the next-generation benchtop X-ray
fluorescence analyzer.
 It offers a new level of analysis accuracy, speed and
detection limits for a wide range of elements from Na(11)
to U(92) due to the new 60kV, 1000 μA X-ray tube and the
ultra large area Fast SDD detector.
 Powerful hardware combined with unique software
algorithms make ElvaX Pro a multipurpose lab instrument
for elemental analysis of various materials including
solids, powders, liquids etc.

Sample Changer and Spinner
Benefits
• World’s fastest XRF analyzer (throughput above 500 000 cps) –
highest accuracy and excellent precision within the shortest
measurement time
• 60 kV X-ray tube voltage allows to analyze rare earth elements
using K-series and consistently improves sensitivity to the high-
energy elements from Pd (Z=46) to Ba (Z=56)
• Up to 1000 μA X-ray tube current improves accuracy and
detection limits for light elements (Na, Mg, Al, Si, P, S) and
allows to use small-size collimators (<1mm) for small spot
analysis
• Motorized collimator changer for small spot analysis of jewelry,
welds etc.
• Helium purge feature improves sensitivity to light elements (Na,
Mg, Al, Si, P, S) several times
• 16-position automatic sample changer increases the productivity
of your lab
• Sample spinner for analysis of inhomogeneous samples
• Excellent calibration stability, compensation of ambient
temperature and pressure influence
• High-resolution CCD camera for precise sample positioning
The automatic 16-positions sample changer coupled with the fast
measurement increases the productivity of your lab up to 1000 samples per
workday.

Digital X-Ray Source digiX-60
Anode: W, Rh, Ag
Voltage: 60 kV
Current: 1000 μA
Power: 12 W
8 position filter changer
5 position collimator
X-Ray Detector
Type: Fast SDD
Area: 40 mm2
Energy resolution: 130 eV at Mn Kα, 85 eV at Al Kα
Count rate: 500 000 cps
Electronics
DPP: proprietory DAS (Dynamically Adaptive
Shaping) type, 80 MHz sampling rate
MCA: 4096 channels
The Elva X PRO difference is in the excitation
source and the detection unit

What that means for the User
Higher count rates = faster
throughput
Large Area Detector +
better sensitivity for Low Z
elements like Na, Mg
Reasonable power rating –
good x-ray flux generation
for Low Z elements
Large Sample Changer –
larger batches of
unattended sample
analysis
8 selectable Primary Beam
Filters – a large number of
choices to optimize the
excitation conditions for
maximum sensitivity

Internal Optics
of XRF
X R F S A L E S A N D C O N S U L T I N G 5/19/2021 14

Software
Operating system: Windows
10
Analysis algorithms:
Fundamental parameters
(FPA), Empirical (regression)
calibrations, Manual spectra
comparison
5/19/2021
X R F S A L E S A N D C O N S U L T I N G 15
Quantitative
analysis

Case Study – Animal
Feeds and Nutritional
Additives
EDXRF FP RESULTS INCLUDING LOI
MEASUREMENTS

• Name of sample: Animal Feed
• Spectrum: 814 EDXRF FP Results
At. Numb Element Series Intensity Concentration
Unmeasured LE LOI 29.0000 ± 0.0000%
11 Na K 15979 6.7445 ± 0.1734%
12 MgO K 20923 2.7076 ± 0.0565%
13 Al2O3 K 9000 0.6101 ± 0.0284%
14 SiO2 K 46160 1.1376 ± 0.0181%
15 P2O5 K 979428 14.7856 ± 0.0474%
16 SO3 K 161486 1.6572 ± 0.0164%
17 Cl K 1698191 14.0317 ± 0.0370%
19 K K 90302 0.5119 ± 0.0052%
20 CaO K 3175107 25.9153 ± 0.0606%
22 TiO2 K 17915 0.1937 ± 0.0081%
24 Cr2O3 K 225 0.0013 ± 0.0041%
25 MnO K 93924 0.5062 ± 0.0058%
26 Fe2O3 K 233891 1.4333 ± 0.0095%
27 Co K 1509 0.0053 ± 0.0032%
28 NiO K 149 0.0028 ± 0.0024%
29 CuO K 14160 0.1807 ± 0.0036%
30 ZnO K 56791 0.5205 ± 0.0048%
33 As2O3 K 0 < 0.0005%
34 SeO2 K 681 0.0023 ± 0.0005%
35 Br K 642 0.0012 ± 0.0003%
37 Rb2O K 324 0.0004 ± 0.0002%
38 SrO K 15532 0.0122 ± 0.0002%
39 Y2O3 K 2308 0.0019 ± 0.0001%
40 ZrO2 K 1702 0.0016 ± 0.0002%
41 Nb2O5 K 1181 0.0011 ± 0.0002%
42 MoO3 K 1061 0.0009 ± 0.0001%
45 Rh K 478 < 0.0001%
53 I K 5553 0.0043 ± 0.0007%
56 BaO K 7371 0.0230 ± 0.0034%
82 PbO L 1576 0.0060 ± 0.0006%
Elements expected results Oxides unit
Ca 16.7-20 23 – 27.9 %
P 8.4 19.23 %
Na 5.1-6.1 %
Mg 1 1.65 %
K 0.6 %
Co 11 ppm
Cu 1450 1812 ppm
Mn 4320 5610 ppm
Se 18.7-22 26 - 30 ppm
Zn 5075 6288 ppm
Product Specification Sheets

Zinc Sulphate Additive
-------------------------------------------------------------
At. Numb | Element | Series | Intensity | Concentration
-------------------------------------------------------------
11 | Na | K | 0 | < 0.5788%
12 | MgO | K | 421 | 0.1821 ± 0.1029%
13 | Al2O3 | K | 577 | 0.1254 ± 0.0606%
14 | SiO2 | K | 0 | < 0.0107%
15 | P2O5 | K | 0 | < 0.0098%
16 | SO3 | K | 1671245 | 47.8430 ± 0.0758%
17 | Cl | K | 69464 | 1.5758 ± 0.0279%
19 | K | K | 19594 | 0.2074 ± 0.0055%
20 | CaO | K | 7877 | 0.1063 ± 0.0063%
22 | TiO2 | K | 799 | 0.0100 ± 0.0089%
24 | Cr2O3 | K | 1966 | 0.0129 ± 0.0045%
25 | MnO | K | 52787 | 0.3272 ± 0.0053%
26 | Fe2O3 | K | 167934 | 1.2015 ± 0.0086%
27 | Co | K | 0 | < 0.0044%
28 | NiO | K | 564 | 0.0063 ± 0.0052%
29 | CuO | K | 6058 | 0.0854 ± 0.0047%
30 | ZnO | K | 4193246 | 48.2931 ± 0.0345%
33 | As2O3 | K | 0 | < 0.0014%
34 | SeO2 | K | 0 | < 0.0012%
35 | Br | K | 1819 | 0.0150 ± 0.0011%
37 | Rb2O | K | 560 | 0.0028 ± 0.0006%
38 | SrO | K | 0 | < 0.0003%
39 | Y2O3 | K | 0 | < 0.0004%
40 | ZrO2 | K | 0 | < 0.0004%
42 | MoO3 | K | 0 | < 0.0008%
48 | CdO | K | 290 | 0.0012 ± 0.0010%
50 | SnO2 | K | 0 | < 0.0011%
53 | I | K | 253 | 0.0009 ± 0.0019%
56 | BaO | K | 0 | < 0.0082%
82 | PbO | L | 222 | 0.0036 ± 0.0019%

D2102264#11At. Numb Element Series Intensity Concentration
LE 0 19.5000 ± 0.0000%
11 Na K 0 < 0.2857%
12 MgO K 879 0.2505 ± 0.0693%
13 Al2O3 K 23841 3.3964 ± 0.0604%
14 SiO2 K 53858 2.8021 ± 0.0327%
15 P2O5 K 4829 0.1506 ± 0.0197%
16 SO3 K 611502 11.1762 ± 0.0388%
17 Cl K 122146 1.6000 ± 0.0235%
19 K K 32734 0.2140 ± 0.0052%
20 CaO K 1486722 13.4542 ± 0.0238%
22 TiO2 K 9033 0.0988 ± 0.0102%
24 Cr2O3 K 848 0.0059 ± 0.0054%
25 MnO K 2984926 23.1563 ± 0.0286%
26 Fe2O3 K 906785 8.4020 ± 0.0286%
27 Co K 9814 0.0693 ± 0.0088%
28 NiO K 628 0.0205 ± 0.0061%
29 CuO K 71406 1.8133 ± 0.0145%
30 ZnO K 710703 13.3038 ± 0.0293%
33 As2O3 K 466 0.0046 ± 0.0015%
34 SeO2 K 0 < 0.0009%
35 Br K 743 0.0041 ± 0.0008%
37 Rb2O K 373 0.0012 ± 0.0004%
38 SrO K 11045 0.0255 ± 0.0006%
39 Y2O3 K 210 0.0005 ± 0.0004%
40 ZrO2 K 1625 0.0046 ± 0.0006%
41 Nb2O5 K 0 < 0.0002%
42 MoO3 K 674 0.0016 ± 0.0004%
45 Rh K 273 < 0.0001%
53 I K 144583 0.3482 ± 0.0023%
56 BaO K 19708 0.1884 ± 0.0090%
82 PbO L 673 0.0073 ± 0.0016%
Manganese Additive

At. Numb Element Series Intensity Concentration
LE 0 47.7000 ± 0.0000%
11 Na K 12759 4.4859 ± 0.1399%
12 MgO K 22779 2.4473 ± 0.0472%
13 Al2O3 K 10922 0.6227 ± 0.0258%
14 SiO2 K 58552 1.2236 ± 0.0158%
15 P2O5 K 726333 9.4146 ± 0.0336%
16 SO3 K 667410 5.8313 ± 0.0240%
17 Cl K 1385373 10.0115 ± 0.0291%
19 K K 253896 1.2254 ± 0.0068%
20 CaO K 2136389 14.7866 ± 0.0380%
22 TiO2 K 0 < 0.0038%
24 Cr2O3 K 3901 0.0175 ± 0.0036%
25 MnO K 115320 0.4867 ± 0.0050%
26 Fe2O3 K 172424 0.8266 ± 0.0067%
27 Co K 2444 0.0068 ± 0.0026%
28 NiO K 177 0.0028 ± 0.0022%
29 CuO K 21597 0.2329 ± 0.0037%
30 ZnO K 80137 0.6209 ± 0.0049%
33 As2O3 K 415 0.0012 ± 0.0005%
34 SeO2 K 2972 0.0089 ± 0.0006%
35 Br K 541 0.0009 ± 0.0002%
37 Rb2O K 810 0.0008 ± 0.0002%
38 SrO K 10323 0.0070 ± 0.0002%
39 Y2O3 K 2725 0.0020 ± 0.0001%
40 ZrO2 K 952 0.0008 ± 0.0002%
41 Nb2O5 K 0 < 0.0001%
42 MoO3 K 1758 0.0012 ± 0.0001%
53 I K 22818 0.0156 ± 0.0007%
56 BaO K 5780 0.0157 ± 0.0033%
82 PbO L 639 0.0021 ± 0.0005%
Sodium Chloride/Calcium Phosphate

Summary
For the Analysis of Animal Feed EDXRF
is a well-suited technique
Since the majority of the additive
ingredients are made from low z and
transition metal salts.
Lose powder preparation – tap
packing the sample into the cup is
sufficient to accurately measure
additives.
The feed itself which is mixture of
crude protein and fats with additives
blended in is a more complex analysis.
To ensure adequate mixing and
particle size reduction a milling step
would be necessary along with
rendering the sample into a pressed
pellet using 20 Tons of pressure.
We improved the accuracy of the FP
by including an experimental loss on
ignition data point.
Its possible to do this using the Xray
Tube Compton/Rayleigh Scatter
intensities which is how most vendors
compensate for unmeasured elements
but the correction is not sensitive
enough to values that are within 5% of
each other and this leads to the FP
estimation being off.

Thanks for your
attention

Pet food analysis

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