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E400 User Guide
E400 User Guide
User Guide
Rapid, Accurate, and Simple Element Concentration Measurement
By T U R B O S P E C LLC
User Guide
Table of Contents
Overview of the TURBOSPEC e400 .................................................................................................. 2
The Instrument ..........................................................................................................................................3
Safety, Installation and Service ............................................................................................................4
Operation ................................................................................................................................................... 7
Data Reporting ......................................................................................................................................... 11
Operational Details ................................................................................................................................ 13
Element Concentration ......................................................................................................................... 14
The Science behind TURBOSPEC e400 ......................................................................................... 17
Troubleshooting ..................................................................................................................................... 19
Instrument Specifications ..................................................................................................................... 19
Contact TURBOSPEC LLC .................................................................................................................. 20
Among the attributes of the instrument are ease of calibration, quick results, and high precision over an
extended range. Samples require minimal or no preparation, distinguishing the TURBOSPEC e400 from other
labor-intensive, consumable-rich methods such as Titration and Atomic Absorption.
This User Guide describes the TURBOSPEC e400 operation. The guide also includes the system specifications
and an explanation of the principles behind the analysis.
The TURBOSPEC e400 is a tabletop Magnetic Resonance (MR) analyzer equipped with a touch screen and an
intuitive Graphical User Interface. Data reports are presented to the user on the screen and may be
transferred to an external USB device.
Front Side
The instrument requires minimal maintenance by the user. The enclosure should be periodically cleaned
with a cloth slightly dampened with water only; no solvents or cleansers should be used.
WARNING: To reduce the risk of fire, electric shock or injury when using the TURBOSPEC e400, follow
these basic precautions:
• Place the analyzer on a table or platform that can safely support the weight of the unit.
Grounding
• Use only the external power supply included by the manufacturer.
• Do not defeat the safety purpose of the three-contact, grounding-type AC plug. If the provided plug does
not fit into your outlet, consult an electrician to have a suitable outlet installed.
• Before performing any type of installation or cleaning, turn the unit OFF and then disconnect it from the
electrical source.
Cleaning
Before cleaning, turn the unit OFF and unplug the power cord.
• Wipe the screen gently with a soft cloth.
• Clean the exterior surfaces of the TURBOSPEC e400 using a damp cloth and mild soap.
• Never use solvent, thinner, benzene, alcohol or any other chemicals to clean the unit. Such chemicals may
discolor the surface or damage the unit.
Screen
• To avoid damaging the LCD screen, do not expose it to direct sunlight.
• Do not scratch the screen or place objects on top of it.
• Avoid using chemicals to clean the screen.
• If the surface of the screen is cracked or otherwise damaged, unplug the AC Power Cord and contact the
manufacturer. Do not attempt to repair.
Installation
• The TURBOSPEC e400 should be installed near an easily accessible AC power outlet.
• If multiple units are installed, they must be separated by a minimum of 4 feet.
• Do not allow anything to rest on or roll over the power cord.
• Never install the unit on unstable and/or uneven surfaces.
• Do not install the unit in places subject to extreme temperature variations, such as in direct sunlight, or
near a radiator or heating vent.
• Do not install the unit where it may be exposed to mechanical vibrations.
Servicing
• Do not attempt to service the TURBOSPEC e400. Refer all servicing to the manufacturer’s qualified service
personnel only. Contact information is located on the last page of this User Guide.
• If replacement parts are required, contact the manufacturer. Improper substitution of parts may result in
a fire, electric shock or other hazards.
• Unauthorized repairs or part substitutions will void the manufacturer’s warranty.
Disposal
For information about disposing of the TURBOSPEC e400, contact the manufacturer.
2. Positioning: Select a location that is convenient to your samples but is also free of rapid temperature
variations - away from direct sun exposure or drafty air if possible.
3. Power: Insert the power cord into the back of the TURBOSPEC e400 and secure it in place by screwing in the
nut. Plug the power cord into a standard 110-240 V outlet.
4. Starting up: Turn on the power switch on the back of the TURBOSPEC e400. The instrument will be ready
for use in about one minute.
Do not switch the instrument off during startup. Initializing the instrument takes about one minute
and the screen is dark during part of the process.
If your instrument is already plugged in and the switch is in the off position, but the monitor is off, turn
the power switch off and then back on in order to start the TURBOSPEC e400.
As initial step, select the desired element on the graphical user interface. The appearance of the screen
and the list of elements may differ, based on the elements you selected when acquiring the TURBOSPEC e400.
3. Calibrating:
• Use the numerical keyboard that appears on the screen (see picture, below) to enter the concentration
value you associate with this calibration standard. Molarity is the recommended unit to be used for
calibration. You may use other units of concentration, e.g. mg/ml or ppm. Note that the units are not
entered into the instrument. For additional information regarding unit conversion, see the Element
Concentration section below.
• Press OK to begin the calibration. When the calibration process completes, the TURBOSPEC e400 will indicate
that it is ready for measurements.
4. Measuring a Sample: Insert the sample tube into the TURBOSPEC e400 and press the SCAN button. The
element concentration value will be displayed as soon as the scan is complete. The units are the same
ones used during calibration. See a thorough explanation in the Operational Details section.
5. Stopping a Measurement: It is possible to stop a measurement by pressing the ABORT button (see
figure above).
6. Recording Data: Every measurement is stored in a log file on the TURBOSPEC e400. Pressing on the
Previous Results button displays the log file. See below for more information about this log file.
7. Shutting Down: If you are done with your measurements, you may leave the system on or shut it down.
In either case, it is a good idea to remove the sample. To shut down, press the OFF button at the upper
right and confirm by pressing the OFF button on the next screen. Once the screen goes dark, switch the
instrument power off using the switch on the back panel.
Adding user Notes: After a measurement, the user can add a short notation in the results file by
selecting the ADD NOTES tab at the bottom of the screen. The note may be up to 30 characters long.
Notes can only be added for a measurement immediately after that measurement is made.
Deleting the Data Log File: The data log file may be deleted by pressing the DELETE button while
viewing the log file. Note: this operation deletes the entire data log file.
Exporting the Data Log File: The data file can be written to a USB memory stick. When a memory
stick is installed (see the back side panel diagram on p. 3), a SAVE TO FLASH button appears on the data
log file display (select PREVIOUS RESULTS to display the data log file). Pressing SAVE TO FLASH writes a
file to the main directory of the USB stick. A “Results Saved” message will pop up saying the data have
been written to the stick (see figure below). The file name begins with “ResultsLog” and contains the time
at which the file was written to the USB stick. The file is in comma separated value (CSV) format.
Re-calibrating: For routine use, calibration needs to be performed only once after start if the TURBOSPEC
e400 is maintained in a stable environment. Over time, the instrument may drift slightly out of calibration,
so recalibration is recommended every hour or so for high precision and accuracy. Recalibration should
also be performed if the instrument is moved, if the operating temperature has changed, or if large metal
objects near the instrument have been moved.
Loading Sample Tubes: The TURBOSPEC e400 is designed to work with 5 mm (outside diameter) sample
tubes. The sample fluids should fill the tubes to a height of at least 3 cm and no more than 5 cm. For
commonly available tubes, this will require about 400 µL (0.4 mL) of sample fluid. Cap the tube tightly.
Remove any air bubbles in or below the fluid. Wipe off any fluid on the outside of the sample tube.
Achieving the Highest Accuracy: The TURBOSPEC e400 makes high precision concentration
measurements. In order to achieve the best possible accuracy, special care is required. This care includes:
• Maintaining a stable thermal and mechanical environment for the TURBOSPEC e400 and
giving the instrument time to equilibrate thermally (sitting on for 30 minutes or more).
• Ensuring that all tubes used for samples and standard have the same inner diameter –
High precision MR tubes are recommended.
• Using a well characterized fluid for the calibration standard and sealing the standard tube,
preferably by flame sealing, if the same standard is to be kept and reused.
• Using a fluid nearly identical to the samples for the calibration standard.
• Repeating the calibration and measurement a few (four recommended) times to confirm
that nothing is amiss.
The TURBOSPEC e400 measures concentration in terms of numbers of atoms of an element located in the
sensitive volume of the device. There are subtleties involved in comparing such concentration units to
other units, such as weight percent and volume percent. The relationship between unit systems may not
be linear, and the precision of the TURBOSPEC e400 measurements may be high enough to make this an issue.
For instruments configured for Lithium measurements, the unit measures a signal that is proportional to
the number of 7Li nuclei that are in solution. It does not detect the nuclei of Li atoms that are in solid
particles or precipitates. It detects twice as much signal from a molecule containing 2 Li atoms than from
a molecule containing only one Li atom. Hence, it will report the concentration of Li, which may differ
from the concentration of the Li-bearing molecule or compound. 7Li accounts for 92.5% of naturally
occurring lithium atoms. The rest are 6Li. In the unlikely event you are working with isotopically enriched
samples, you will need to consider this enrichment to accurately calibrate your samples.
Calibration of the TURBOSPEC e400 is essentially the determination of a proportionality constant. This means
that any errors in the calibration process will directly and systematically affect the accuracy of all
subsequent measurements, until a new calibration is performed. Care should be taken to prepare the
calibration sample fluids so that their concentrations are known to a precision higher than the precision
desired in the subsequent measurements. For example, be aware that the final volumes of mixtures of
fluids may differ from the sum of the starting volumes, and that dissolving a solid into a liquid can cause
the total volume to increase. The TURBOSPEC e400 is accurate enough to detect these effects.
Like any high precision analysis device, the TURBOSPEC e400 will drift slowly out of calibration over time. For
measurements at the 5% accuracy level, this drift probably does not matter at all. If 1% accuracy is desired,
then the instrument should be re-calibrated every hour or so. If the lab environment of the instrument
changes (the device is moved, the room temperature changes, metal objects near the instrument are
moved, etc.) then the device should be allowed to re-equilibrate for 30 minutes or longer and then it
should be recalibrated. To achieve high accuracy, the device should be calibrated before each
measurement. If the device is in a very stable environment, the requirements for re-calibration are
relaxed.
The TURBOSPEC e400 is designed to be equally sensitive to all species of – for example - 7Li. That is, it should
not matter whether the solution contains lithium ions or organo-lithium molecules. Hence, for routine
measurements, the device is calibrated on one type of fluid and used to measure a different type of fluid.
However, it is always best to use calibration fluids that are similar to the fluids in the samples to be
measured. This is a requirement if the highest possible accuracy is needed.
Unit Conversion
Common solute concentration units used for elemental analysis are Molarity and parts per million.
Molarity is the preferred unit to be used when operating the TURBOSPEC e400.
As the concentration in ppm is the number of grams of solute per grams of solution times 106, a density
correction is necessary when converting units from ppm to M. This correction is not needed for dilute
solutions but is relevant when the density of the solution differs significantly from 1 gr/mL.
To convert from concentration in ppm (C[ppm]) to Molarity (C[M]) use the following formula:
For example, in an 8 M solution of LiCl with density of 1.15 gr/mL, the Lithium concentration in ppm is:
C[ppm] = 8 M x (6.941 gr/M /1.15 gr/mL) x 1000 = 48,285 (mg of Lithium per kg of solvent).
Example Dilution
If one adds 8.36 gr of LiCl to 39.9 gr H20, the result is a 4.48 M Lithium Chloride solution. The formula
weight of LiCl is 42.39 gr/mole, so there are 0.197 moles of LiCl in the water. Because each LiCl formula
unit contains one Li atom, there are also 0.197 moles of Li in the water. The volume of the water starts at
39.9 mL, but the total volume after adding the LiCl is 44.0 mL. Hence the molar concentration of Li is 0.197
mole/0.0440 L = 4.48 M. Note that the precision of the calibration standard is limited here by the precision
in the measurement of the final volume.
If this value (4.48) is entered into the analyzer during calibration, then the subsequent measurements will
give results in units of molar concentration of Li.
One might also choose to calibrate in terms of weight percent. The 0.197 moles of Li weigh 1.37 gr. Hence
the weight percent is 1.37 gr/(8.36 gr + 39.87 gr) = 2.84%. If 2.84 was entered into the analyzer during
calibration with this fluid, then the subsequent measurements would report results in units of weight
percent Li.
Note that as the TURBOSPEC e400 measures the element concentration in Moles, the percent weight or ppm
calibration will be slightly off for samples whose concentration differs substantially from the
concentration of the calibration standard. See previous section.
With the calibration entered in molar units, a measurement on a 1.00 M LiCl solution should yield a value
close to 1.00. However, if instead we take a measurement on 0.150 M Li2CO3 solution, we would read a
value close to 0.300. There are 0.300 M of Li ions in a 0.150 M Li2CO3 solution, because there are two
Lithium atoms in each formula unit.
It is always important to remember that the instrument measures the concentration of the element, not
the concentration of molecules that contain that element.
The TURBOSPEC e400 determines the number of atoms per unit of volume in solution; therefore, the
measurement is affected by the presence of solid particles. As the particles displace the liquid, the
measured concentration level is systematically lower when solids are present. A simple filtration process
reduces or eliminates the discrepancies.
Counting Atoms
At the core of every atom is the nucleus, consisting of a dense assembly of protons and neutrons. The
number of protons is the atomic number and determines what element it is; the sum of the number of
protons and neutrons is the mass number and determines the particular isotope of the element under
consideration.
Protons and neutrons are particles that have a quantum mechanical property called “spin” and an
associated magnetic moment. When protons and neutrons combine to make a nucleus, their individual
spins combine to form a net spin associated with this nucleus. The corresponding magnetic moment
makes the nucleus act like a small magnet.
In a liquid solution, all those small magnets are randomly oriented and therefore the sample has a zero
net magnetic moment. If the solution is placed in the field of a permanent magnet, however, nuclei tend
to align so that they are pointing in the direction of the external magnetic field generated by the magnet.
This orientation is their lowest energy state, so they are in equilibrium.
Randomly oriented nuclei in the absence of a magnetic field - left. Nuclear spins effectively oriented in the direction
of the strong magnetic field – right.
MR Measurement
If the right amount of energy is supplied to the sample, the nuclei can temporarily move from the low
energy state. This means they are out of equilibrium, rotated away from the magnetic field’s direction. In
the TURBOSPEC e400, the energy is supplied by applying a burst of oscillating magnetic field whose frequency
is tuned precisely to the resonance frequency of the element being measured. It is actually more specific
than that—it is tuned to one particular isotope of that element. The frequencies needed are similar to
those used to broadcast analog radio signals.
After the radio-frequency field has been applied to tip the nuclei away from their equilibrium orientation,
it is switched off rapidly, and the nuclei rotate around the magnetic field produced by the permanent
magnet in a process called “precession”. Eventually, the nuclei re-align with the magnetic field and
precession stops. However, while precession is occurring, the nuclei act like a rotating magnet, which can
be detected in a coil of wire wrapped around the sample. The signal detected is much smaller than the
radio-frequency pulse that was used to excite the nuclei, but it is highly amplified using low noise
electronics in order to be measured in the receiver. The more nuclei present in the sample, the larger the
signal detected, which is the fundamental measurement made by the TURBOSPEC e400.
The signal decreases with time as the nuclei return to equilibrium. The speed of this decrease depends on
the efficiency with which the nuclei can exchange energy amongst themselves and give up their excess
energy to their surroundings. Measuring the rates of decay of the signal provides further information
about the chemical and physical environment of the detected nuclei, enabling further characterization of
the material and its properties.
A radio-frequency pulse of the right length and frequency can rotate the orientation of the nuclei. Nuclei in the figure on the
left are oriented in the direction of the static field. After an RF pulse is applied, the nuclei are rotated – see the figure on the
right.
• If a sample is broken inside the TURBOSPEC e400, carefully clean the inside with a water-damp swab. Be
careful of glass fragments. After cleaning, run a scan with no sample. If the concentration the system
returns is not close to zero, the sample holder is contaminated. If this occurs or if there is any glass
visible in the sample holder, contact Turbospec LLC.
• If, after calibrating a reference sample, the results obtained are not precise or return unexpected
values, perform the following steps:
1. Rerun the calibration sample, and check that the results are consistent.
2. Make sure that there are no water drops on the sides of the tubes; if droplets are visible, make
sure to gently shake the sample or calibration standard so all solution is in the bottom of the tube.
4. Check sample tubes. If the inner diameter of the MR sample tubes being used is not very precise,
the sample volume may vary from tube to tube giving poor reproducibility in measurements. The
TURBOSPEC e400 is more precise than the ID tolerance for standard MR tubes.
Instrument Specifications
• Size: 48 cm width, 25 cm height, • Magnet: ultra-compact high
25 cm depth homogeneity permanent
magnet with passive shielding
• Weight: 8.3 Kg for stray fields
Web: turbospecllc.com
E-mail: info@turbospecllc.com