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Microwave Solutions for Metals Prep
UltraWAVE Ethos UP
MILESTONE
Microwave Digestion Mercury | Clean Chemistry | Ashing | Extraction | Synthesis milestonesci.com | 866.995.5100
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ith increased state regu- reaction chamber (SRC) technology potential matrix-suppression effects
lations, cannabis growers (1). So, how do you go about select- in the plasma should be taken into
are required to conduct ing the optimum technology for your consideration. It is therefore well-rec-
trace metals testing to ensure a safe samples? What types of mineral ac- ognized that the most plasma spec-
and high-quality product. This test- ids will be best suited for your ele- trochemical-friendly reagents are
ing encompasses a wide variety of ments of interest, and what temper- typically strong oxidizing agents
samples from growers and the pro- ature and pressure will be required such as nitric acid (HNO3) and hydro-
cessing industry including soils, fer- for the digestion process of your gen peroxide (H2O2), which are ex-
tilizers, plant material, edible prod- sample matrices? It’s only when you tremely efficient, but tend to gener-
ucts, concentrates, and topicals. have a good understanding of these ate large amounts of carbon dioxide
Obtaining analytical data required issues, that you can begin to look (CO2) and various oxides of nitrogen
to ensure quality products starts more closely at the pros and cons of (NOx) when they react with the sam-
with the crucial step of preparing the different commercially-available ples. The microwave system and its
the sample for analysis. Reducing microwave technology. So first, let’s components will therefore not only
handling steps, eliminating outside take a closer look at the fundamen- need to accommodate the high tem-
contamination, and minimizing rea- tal principles of both designs. perature required to digest all the dif-
gent blank contribution are all nec- ferent organic sample types, but also
essary for good sample preparation. Principles of Microwave be able to handle the subsequent in-
It is well recognized that closed-ves- Digestion Technology crease in pressure produced by the
sel microwave digestion offers the First it should be emphasized that generation of large volumes of these
best approach for getting your sam- sample digestion of organic matrices gases. For some samples, the addi-
ples into solution for analysis by in- such as cannabis products should be tion of small amounts of hydrochloric
ductively coupled plasma–optical carried out using reagents compati- acid will also help to stabilize some el-
emission spectrometry (ICP-OES) or ble with ICP-OES and ICP-MS instru- ements particularly mercury (Hg) and
inductively coupled plasma–mass mentation. For example, the chemical the platinum group elements. How-
spectrometry (ICP-MS). However, or physical properties and concentra- ever, it should be noted that if ICP-MS
there are basically two very differ- tion of the mineral acids used and is being used as the analytical tech-
ent commercially available designs: how they affect the sample introduc- nique the 40Ar35Cl polyatomic spe-
rotor-based systems and single tion nebulization processes and the cies could potentially interfere with
Rotor-Based Technology
With rotor-based technology, micro-
waves are directed onto vessels con-
taining the sample and the digestion
reagents, which are placed in a rotat-
ing carousel. The digestion process
is accomplished by raising the pres-
sure and temperature through micro- Figure 1: Principles of the “vent-and-reseal” approach.
wave irradiation, as the carousel is ro-
tating. This increase in temperature
and pressure, together with the op- 40
timum reagent, increases both the
speed of thermal decomposition of 30
Pressure (bar)
Microwave
Single Reaction
Chamber Technology
So let’s take a more detailed look
Figure 3: Single reaction chamber microwave digestion technology. at the principles of single reaction
chamber (SRC) technology, and how
it differs from the rotor-based sys-
tem. Instead of a rotor with a dis-
crete sample vessel, the samples are
Hg (ppt)
put into vials with loose-fitting caps,
Bk position 01 0.020
which are sitting in a rack that is low-
Bk position 03 0.032
ered into a larger vessel containing a
Bk position 05 0.001
base load of acidified water. It’s this
Bk position 07 0.002
baseload that absorbs the micro-
Bk position 09 -0.003
wave energy and transfers it to the
Bk position 11 -0.007
vial. This design allows every vial to
Bk position 13 -0.007
(15 Position) White vials: blanks. react independently within the base
Red vials: 110 ppm Hg Bk position 15 -0.006
load and ensures that all samples
achieve maximum temperature with
pressures contained up to 200 bar.
No batching of samples is neces-
Figure 4: Study of sealing capability of nitrogen gas shows no sign of contamination sary, and any combination of sample
from mercury. type and acid chemistry can be run
simultaneously in the same chamber.
corrosion of internal components will in high-throughput rotors, which were A schematic of the SRC is shown in
occur. This is exemplified in Figure 2, developed to address the needs of Figure 3.
which compares the burst disk ap- laboratories that process larger sam- As previously mentioned, loose-
proach with vent-and-reseal: the red ple volumes on a routine basis. Self- fitting caps are used to seal the vi-
line shows the complete loss of pres- regulating vessels are very easy to as- als. This is possible because they are
sure when a burst disk fails, and the semble and disassemble and rely on pre-pressurized with 40 bar of nitro-
whole run is stopped. Whereas, the the PTFE sealing plug inside the cap gen before the start of the micro-
blue line shows that with the vent- deforming to release pressure. Their wave program, which acts as a gas
and-reseal technology, excess pres- compact design results in more mod- cap and keeps all the vials indepen-
sure is gently released at the vessel’s erate temperature and pressure ca- dently closed. As the pressure builds,
pressure limit (f.i. 30 bar), and the di- pabilities, but allows for a large num- equilibrium is achieved both inside
gestion continues to completion, with ber of vessels to fit onto the rotor. and outside the vial. As a result, a va-
no loss of sample. These characteristics make self-reg- riety of vial types including dispos-
ulating rotors ideal for high workload able glass, quartz, and PTFE or any
Self-Regulating Rotors laboratories with relatively straight combination of these materials can
This third approach is typically used forward applications such as clinical, be used (4).
Benefit of Nitrogen Table I: Range of cannabis products tested, their sample weights, and digestion
Pressurized Caps reagents using the rotor-based microwave system
To exemplify that 40 bar of nitrogen Sample Weight Used in Ethos UP – SK15
is sufficient to seal the vials, an ex- Sample
8 mL Conc. HNO3, 1 mL Conc. HCl, 1 mL H2O2
periment was carried out where vials Cannabis plant material (flowers) 1g
containing 110 ppm of mercury were
CBD oil (cannabidiol) 0.5 g
placed right next to blank solutions
Cannabis vape cartridge 0.5 g
in a 15-rack sample holder. In other
words, every alternate sample vial in Cannabis salve (ointment) 0.5 g
Table III: Recovery of 20 ppb Pb, As, Cd, and 10 ppb Hg spiked into cannabis products, digested by rotor-based microwave technology,
and analyzed by ICP-MS
rotor-based systems and SRC tech- normal plant metabolism. Some of metals. Depending on their work-
nology. The main drawback of ro- these metals are naturally occurring load and the diversity of the products
tor-based technology is that they and leach into the groundwater. Oth- and testing protocols used will clear-
require batching of similar matrices ers precipitate in rainwater or may ly impact the optimum type of mi-
and chemistries, because control of be introduced into the plant’s envi- crowave system they choose for this
the power is based on the reaction ronment as constituents of fertiliz- task. To get a better understanding
of one vessel at a time. Regardless ers, pesticides, herbicides, and fun- of this, we took a representative sam-
of how temperature is being meas- gicides used to increase crop yield. pling of different commercially availa-
ured, it’s still measuring the pow- Regardless of their prevalence, when ble cannabis products and digested
er level based on one sample. By metabolized, metals are absorbed them by both rotor-based technolo-
batching similar samples, under-di- and transported through the plant gy (Ethos UP- SK-15 high pressure sys-
gestion of some samples can be roots into plant tissue, leaves, and tem, Milestone Inc.) and a single re-
minimized because of the pressure flowers. Cannabis is so effective at action chamber system (UltraWAVE,
and temperature required by oth- absorbing metals from its environ- Milestone Inc.) and analyzed them
ers. Additionally, in rotor-based sys- ment that it has been referred to as using ICP-MS (Model 7900, Agilent
tems, the vessels are typically made a hyper-accumulator of trace met- Technologies).
from PTFE, which limits the temper- als, including many of the tradition-
ature and pressure because of the al heavy metals. This characteristic of Rotor-Based Analytical Procedure
type of material used. The multiple cannabis leads to concern that these Table I shows the cannabis products
components of vessels also require elements may occur in high concen- tested, their sample weights, and re-
additional handling before and after trations in cannabis plants. State gov- agents used to digest them using
digestion, which could impact pro- ernments and private laboratories are the rotor-based microwave system,
ductivity. Depending on detection therefore focusing on product safety and Table II exemplifies the micro-
limit requirements, the vessel liners testing with special emphasis on As, wave program that was used to di-
may also require extra cleaning be- Cd, Hg, and Pb because they are ex- gest the samples. The resulting solu-
tween runs. tremely hazardous to human health, tions produced were then made up to
even at low levels. 50 mL with deionized water and pre-
Heavy Metals Testing of The combination of closed-vessel sented to the ICP-MS instrument for
Cannabis Plants, Concentrates, microwave digestion and ICP-MS has analysis. Note: only Pb, Cd, As, and
and Edibles by ICP-MS become the preferred approach of Hg will be presented here, but a to-
Like all plants, cannabis absorbs met- cannabis testing laboratories to carry tal of 14 elements (As, Cd, Pb, Hg, Ag,
als from its environment, a result of out the measurement of these heavy Ba, Co, Cr, Cu, Mn, Ni, Se, V, and Zn)
Simultaneous Mixed-Batch simultaneously without sample-to- point out that higher sample weights
Sample Preparation for Metals sample cross contamination. Addi- are typically used with SRC technol-
Testing of Cannabis Samples tionally, a soil sample was digested ogy and there is no minimum sample
Using SRC Technology in the same analytical run as the can- volume that has to be used. In addi-
The combination of SRC technolo- nabis products, to exemplify the ca- tion, because of the higher temper-
gy with ICP-MS allows cannabis an- pability of SRC technology to digest ature and pressure capability of the
alytical testing laboratories to an- widely different matrices simultane- SRC technology, digestion times are
alyze a broad variety of sample ously in the same chamber. This ap- usually much shorter.
matrices with widely different sam- proach would be very difficult to car-
ple weights and elemental require- ry out with a rotor-based system, Results and Discussion
ments. SRC microwave digestion is because of its batching limitations. The performance of the SRC system
a unique approach, incorporating all was evaluated through a recovery
the benefits of closed-vessel micro- Analytical Procedure study on samples of interest for the
wave digestion while making sample Using SRC Technology cannabis industry, from plant ma-
preparation fast, easy, and extreme- Table IV shows the cannabis prod- terial to edibles and concentrates.
ly efficient. SRC technology operates ucts tested, their sample weights All samples were fortified with a
at very high temperatures and pres- and reagents used to digest them spike solution containing 20 ppb of
sures (up to 300 °C and 200 bar, re- using SRC technology, and Table V all analytes, except for Hg, which
spectively), allowing for complete di- exemplifies the microwave program was 10 ppb. A soil reference mate-
gestion of even large sample sizes that was used to digest the sam- rial (SRM 2711a) was also included in
(up to 3–5 g) and difficult-to-digest ples. The resulting solutions pro- this study as a quality control sam-
matrices. Samples can be weighed duced were then made up to 50 mL ple and to show that a widely dif-
directly into disposable glass vials, with deionized water and presented ferent matrix to cannabis products
eliminating the need for acid clean- to the ICP-MS instrument for analy- could be digested in the same sam-
ing and vessel assembly. Further- sis. Note: As with the previous meth- ple run. It should be noted that the
more, SRC eliminates the need to od, only Pb, Cd, As, and Hg will be recoveries in the soil were calculat-
batch samples because mixed sam- shown here, but 14 elements (As, Cd, ed according to the total element
ple types, weights, and acid chemis- Pb, Hg, Ag, Ba, Co, Cr, Cu, Mn, Ni, content and represent the leacha-
tries can be successfully processed Se, V, and Zn) were evaluated. Please ble fraction, based on the acid used
in the same run. This application de- refer to the following reference for . . . refer to The National Institute of
scribes how a variety of samples from more information about the method- Standards and Technology (NIST)
the cannabis industry were digested ology used (6). It’s also important to Certificate of Analysis for SRM 2711a
Table VI: Recovery of 20 ppb Pb, As, Cd, and 10 ppb Hg spiked into cannabis products, digested by SRC technology, and analyzed by
ICP-MS
for further details (7). The analyti- found in cannabis plants and relat- if there is a need to digest many dif-
cal results for the cannabis prod- ed products. Highly reactive sam- fering sample matrices simultane-
ucts and soil reference sample are ples such as gummy bears, cookies, ously in the same run, an SRC system
shown in Table VI with recoveries of and cannabidiol (CBD) oil have been could be the best solution. Because
all analytes between 87.5–98.7% and completely digested even in large of its higher sample capacity, use
RSDs well below 3%, clearly demon- sample amounts, ensuring reliable of disposable vials, and faster cool
strating the robustness and repro- analysis. In addition to good ana- down times, sample throughput pro-
ducibility of microwave digestion lyte spike recoveries, this approach, cessing with SRC technology is up to
of different sample types using SRC using a high pressure, rotor-based 2–3 times higher than convention-
technology. Note: The full data set system with a 15 position carousel al closed-vessel digestion systems.
for all 14 analytes can be viewed at also provides a high level of repro- The ability to digest different sam-
the following reference (6). ducibility, even for volatile elements ple types together and larger sam-
such as As and Hg. And if higher ple weights with minimal acid vol-
Final Thoughts sample throughput is required for ume makes it the optimal technique
Modern plasma spectrochemical less demanding matrices, it should to perform sample preparation for
techniques will generate trace el- be noted that a 44-position option all cannabis related products, from
ement data of the highest quali- is available. the plant material to edibles, con-
ty. However, with any solution tech- However, for contract laboratories centrates, and even to get a better
nique, the data will only be as good that might be handling a more di- understanding of the soil chemistry
as the sample presented to the in- verse and complex range of samples where the plants are growing.
strument. For that reason, robust such as supplements, pharmaceu- There is no question that a new era
closed-vessel microwave diges- tical, or even soil samples, a rotor- of acceptance and legalization has
tion techniques are critically impor- based system might be somewhat opened new opportunities for can-
tant to the overall analytical proce- restrictive, because similar samples nabis testing laboratories, not only in
dure. The data in the first part of have to be batched together to en- heavy metals but also for an expand-
this study demonstrates full recov- sure they are being digested under ed list of analytes including poten-
ery of the most common elements the optimum conditions. Therefore, cy, terpenoids, pesticides, residual
LC-MS/MS Solutions
Pesticides, Potency & Terpenes
SCIEX instruments have been designed with the production laboratory in mind.
• California Class 1 and Class 2 pesticides by LC-MS/MS? No problem.
• Oregon pesticide list by LC-MS/MS? No problem.
• Potency, Pesticides & Terpenes by LC-MS/MS? No problem.
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