Item 7. Instalación de equipos, uso y mantenimiento – buenas prácticas

Instalación de equipos, uso y
mantenimiento – buenas prácticas
Estefania Perez-Fernandez
Leonardo Ramirez-Lopez
BUCHI, Switzerland

Sobre nosotros…
Dr. Leonardo Ramirez-Lopez
NIR Data Analytics Manager
Büchi Labortechnik
Dr. Estefania Perez-Fernandez
NIR Chemometrics Specialist
Büchi Labortechnik

Presentación Buchi
❖ More than 700 employees worldwide
❖ Development and manufacturing in Flawil – Switzerland
❖ Own affiliates in 16 countries and distribution partners in over
70 countries
81 years as a leading solution provider in
different systems
• Pharmaceutical industry
•Chemical industry
• Food and beverage, feed industry
•Environmental laboratories
• Academia

BUCHI en el mundo
Headquarters
⚫ Affiliates
⚫ Support Centers
⚫ Distributors

Líneas de Productos
Conceived solutions
whether you operate
in R&D or quality
control (QC) for a
wide range of
industries
Laboratory
Evaporation
Rotatory evaporator
solutions for R&D or
production
Industrial
Evaporation
Convenient
solutions for the
evaporation in the
parallel format
Parallel
Evaporation
Spray drying of
solutions, emulsions,
suspensions and
spray chilling with
smart bench-top
instruments
Spray Drying &
Encapsulation

Freeze Drying
Determination of
melting and boiling
point in high
accuracy
Melting Point
Continuous Freeze
Drying available to a
broad spectrum of
applications from R&D
to quality control
Preparative
Chromatography
Convincing solutions
in the preparative
chromatography up to
50 bar
Kjeldahl
Integrated workflow
packages for the
determination of
nitrogen and protein as
well as volatile
compounds

NIR
Solutions
Comprehensive
solutions for qualitative
and quantitative Near-
infrared analysis
NIR - Online
Analysis across the
entire value chain from
incoming goods
inspection, production
and control of the
finished product.
Extraction
Solutions
Versatile solutions
for solid-liquid
extractions

Equipamiento habitual en un
laboratorio de suelos…
• Balanza
• Horno
• Titulador
• pH meter
• Higrómetro
• Analizador elemental
• Espetroscopía
• …

Equipos que describiremos
• Determinación de nitrógeno- Kjeldahl
• Analizador Elemental
• Espectrómetro de Absorción Atómica
• Espectroscopía NIR
• Espectroscopía MIR

Kjeldahl
Atomic Absorption
Spectrophotometer
Elemental Analyzers/Dumas
Near-Infrared
Spectrometer
Mid-Infrared
Spectrometer
K, Mg, Ca, Na
Al, Fe and Mn
C
N
S
pH (water)
% Sand, % Clay, % Silt
Análisis de suelos e instrumentos
relevantes

Recomendaciones
generales
Para la instalación/operación/mantenimiento de
instrumentos

Recomendaciones generales
• Los equipos deberían siempre ser instalados por un
especialista de la compañía a la que se compra el
instrumento
• Si los equipos son usados de una manera no
especificada por el fabricante, la protección que
ofrece el equipo puede verse afectada
• Pida una lista de verificación por adelantado para
asegurar que puede cumplir los requisitos para la
instalación (computadores, enchufes, condiciones
ambientales, etc.)

• Es recomendable crear una rutina de mantenimiento con una lista
de tareas para cada instrumento
• Si planea hacer todo el mantenimiento por sí mismo/a, es muy
recomendable asistir a cursos preparatorios ofrecidos por el
fabricante
• Periféricos: Compruebe qué accesorios y periféricos no incluidos
en el pedido puede necesitar
• Los botones de encendido/apagado DEBEN siempre estar en la
posición de apagado antes de conectar a la fuente de alimentación
Recomendaciones generales

Análisis Kjeldahl
Para la determinación de nitrógeno

EL proceso Kjeldahl incluye 3 pasos:
- Digestión de la muestra
- Alcalinización y destilación
- Titulación
Análisis Kjeldahl

• Configuración clásica
Análisis Kjeldahl

Uso del sistema automático de
análisis Kjeldahl
El siguiente video muestra los pasos de una rutina de
análisis Kjeldahl
https://www.youtube.com/watch?time_continue=15
&v=r0CYLxkNglo

Consejos de seguridad
Dada la naturaleza del proceso, los principales aspectos de
seguridad a tener en cuenta son:
• Altas temperaturas: digestión alcanza 580°C
• Vapores tóxicos: trabajar en campana de extracción, usar
colector y neutralizador de vapores (scrubber)
• Quemaduras a causa del uso de químicos corrosivos (ácidos y
bases)
• Rotura de vidrios
• Electricidad

Instalación
Lugar de instalación
• Colocar el dispositivo en una campana de extracción
(especialmente para el paso de digestión)
• El dispositivo debe colocarse sobre una superficie
estable, limpia y nivelada
• Mantener distancia de al menos 30 cm desde la parte
trasera del dispositivo y cualquier otro objeto
• Mantener el área libre de objetos innecesarios,
compuestos químicos, contenedores, etc…
• Todos los instrumentos deben instalarse de forma de
las tomas de corriente e interruptores sean accesibles
en todo momento

El scrubber debe colocarse a la izquierda de la
unidad de digestión.
El auto-muestreador debe situarse en la parte izquierda de la unidad de
destilación con un espacio entre ellos de aprox. de 10 cm. y dejando espacio
libre en la parte trasera
Instalación

Connections required
• Electrical connections
• Data connection between different parts of the
system
• Reagent/water and waste connections
• Storage tank connection
• Level sensors
• Connections to peripheral devices (e.g. balance,
printer, bar code reader…)
Instalación

Mantenimiento – recomendaciones
generales
• All maintenance and repair work may only be carried
out by trained personnel and with the tools provided
for this purpose.
• Prior to all maintenance work on the device switch off
the power supply and remove all sources of flammable
vapor. Let the device cool down for at least 30 minutes
after switching off.
• The device may not be reconnected to the power
supply before the housing has been closed properly.
• Always wear personal protective equipment such as
protective eye goggles, protective clothing and gloves
when maintaining the instrument!!!

Mantenimiento
Daily:
• Cleaning and calibrating pH electrode
• Refilling boric acid into receiving vessel
• Sample tube cleaning
• Etc…
Weekly:
• Cleaning the housing and glass parts
• Cleaning the titrator
• Cleaning the dip tube of the Sampler
• Cleaning colorimetric sensor

Mantenimiento
Monthly:
• Calibrating the pump
• Checking the distillate amount
• Inspecting the buret
• Inspecting the titrator
• Inspecting the sample tubes

Mantenimiento
Half year maintenance
• Sealing of all tubes and pipes
• Replacing the splash protector
• Replacing the pH probe
Yearly
• Replacement of wear parts
• Decalcification of the steam generator
• Replacement of the sodium hydroxide pump

Elemental Analyzers for (soil)
C and N
Principle:
Weight the
sample

C and N
Principle:
Weight the
sample
Press the
sample

C and N
Principle:
Weight the
sample
Press the
sample
Burn the
sample
960 °C + O2 → Combustion

C and N
Principle:
Weight the
sample
Press the
sample
Burn the
sample
960~1600°C + O2 → Combustion
Analyze the resulting
gas (after water
removal) for
CO2 and N2

Furnace
Autosampler
Thermo conductivity
detector
5 tubes
C and N

Samples can be packed in tin foil
C and N

Functional principle – Gas flow
Autosampler
Ball valve
Ash finger
Post combustion
Reductor
Drying stages
Detector (TCD)
CombustionSeparationDetection
Elemental Analyzers for (soil) C and N

Paso 1 – Inserción de la muestra
Carrier gas:
PC-Software:
detector signal
during the
determination

Paso 2 – Combustión
Combustion
tube:
Temperature
> 950°C
Controlled
at-the-spot
oxygen dosing

Typical mixture
of gases:
Paso 3 – Gases típicos de combustión

Post combustion
tube:
Paso 4 – Eliminación de metano

3 drying stages:
• Condenser
• Membrane
gas drying
• Chemical
drying agent
Paso 5 – Pasos de secado

Reductor
tube:
Paso 6 - Regainer-Reductor technology

Thermal
Conductivity
Detector
Paso 7 – Detección

Software
related peak
integration and
quantification
Paso 8 – Integrción del área del pico
Result:
%N
%C
Approx. 4 min per
analysis

Calibration of the instrument
The instrument needs to be calibrated with certified reference materials (e.g.
Aspartic acid, EDTA or others specified by the device provider).

Throughput (9h): ~120 samples
Analysis time: 4 – 6 min per sample

An air conditioned room (dry and well ventilated) is recommended as some parts of
the analyzer give off heat.
Installation
Carrieer Gas: Helium He (or in some cases CO2); purity 99.996
Combustion Gas: Oxygen O2 ; purity 99.995
Reagents: specified by the device manufacturer
Calibration standards: For the installation, make sure you have the calibration
standards you need for your soil analyses (these might not be provided by the
manufacturer).

Es muy recomendable que la instalación y primer encendido sean
hechos por un técnico de servicio capacitado. Para la mayoría de
fabricantes este es un requisito explícito. Por tanto, es
recomendable no abrir el embalaje de transporte del instrumento
por adelantado.

Consumedfilling
Newfilling
Remove out consumed filling from drying tubes
and refill the drying tubes with new Sicapent
according filling instruction!
Maintenance
Small Drying tube: ~800 samples
Large drying tube: ~100 samples
Mantenimiento

Ash crucible
Reductiontube
Combustiontube
Maintenance
Combustion tube: ~1000 samples
Reduction tube: ~210 samples
Post combustion: ~2000 Temp. resistant gloves
Mantenimiento

Maintenance
Combustion tube: ~1000 samples
Reduction tube: ~210 samples
Post combustion: ~2000
Refill the tubes with the
materials specified by
the manufacturer
Mantenimiento

Leak tests
Regular checks on the blank value determination
Mantenimiento
Other important checks:

Flame Atomic absorption spectrophotometer (AAS)

- Ion Exchange and Extractable Cations (Ca2+ > Mg2+ > K+ > Na+)
- Al, Fe and Mn
- As and Se
- Heavy metals
Can be used for the following soil properties:

- Ion Exchange and Extractable Cations (Ca2+ > Mg2+ > K+ > Na+)
- Al, Fe and Mn
- As and Se
- Heavy metals
Can be used for the following soil properties:
Detectable elements
by AAS
Undetectable
elements by AAS
Source: VAZ JR, S. Analytical Chemistry Applied to Emerging Pollutants. Springer, 2018.

For flame, it usually
operates with:
- Air
- Nitrous oxide, N₂O
- Acetylene, C2H2
NEVER use any other gas as
fuel unless the manufacturer
recommends something
else!
Source: https://chemistry.stackexchange.com/questions/115895

Example of light absorption by some elements at specific wavelengths:
UV VIS
200 400 600 800
nm
- Na: 588.9 nm
- K: 765.5 nm
- Ca: 422.7 nm
- Mg: 285.2 nm
- Fe: 284.4 nm
+ Element
Concentration
- Element
Concentration

Instalación
Atomic absorption spectrophotometer (AAS)
Make sure these three
rubber hoses are correctly
plugged!

Instalación
Make sure these three
rubber hoses are correctly
plugged!
Pay always special attention
to this one!
If you plan to do the
maintenance by yourself, it is
highly recommended to
attend training courses
provided by the device
supplier.

https://www.osha.gov/pls/imis/ac
cidentsearch.accident_detail?id=
171054760
Source:

Uso y Mantenimiento
- Lamp and burner optimization
- Method parameters
- Quality of the calibration standard solutions (and proper
keeping)
- Cleanliness

Uso y Mantenimiento
- Lamp and burner optimization
Lamps must be correctly aligned and burner position
must be optimized

Ion concentration
Lightabsorbancew
Use mixed calibration standard solutions (MCSS)
High, Medium, Low, Very Low, and Blank
High
Medium
Low
Very low
Blank
Ion concentration = m * Light absorbancew + b
Calibration is done for each element
Uso y Mantenimiento

Ion concentration
Lightabsorbancew
High
Medium
Low
Very low
Blank
Ion concentration = m * Light absorbancew + b
Calibration is done for each element
Uso y Mantenimiento
Your accuracy and precision
depends largely on the quality of the
MCSS

Ion concentration
Lightabsorbancew
High
Medium
Low
Very low
Blank
Ion concentration = f(Light absorbancew)
Find an adequate f
Uso y Mantenimiento

Mantenimiento
Lamps are specific to the ion
being analyzed, i.e. each metal
requires an specific lamp.
- Instruments usually can allocate multiple lamps
- Ideally your instrument should be able to allocate at least all the lamps for all
the elements you need to measure.
Mg Ca
K

Mantenimiento
Mg Ca
K
You should calibrate/align the lamps if:
- You have just installed a new lamp
- You need the best possible signal to noise ratio
- You are using a lamp different from the one
recommended by the device manufacturer
Each lamp emits light at specific wavelengths where the
target element absorbs it.

Mantenimiento
Make sure the lamps compartment
is always properly closed (to prevent
exposure to hazardous UV radiation)
- Check your instrument manual for what types of lamps you can use
- When manipulating the lamps, hold them by their base
Mg Ca
K

Mantenimiento
- It is recommended
to have spare lamps.
Their lifetime varies
between 1000 –
8000 h, however, in
rare cases they may
start failing before
that.
- When acquiring new
lamps, check for the
lifetime
specifications of the
provider.

Mantenimiento
Deuterium (D2) Lamp
Some AAS instruments also come with a background
correction lamp which is usually a Deuterium (D2) lamp
Its lifetime is of aprox. 1000 h.
It requires alignment only when it is installed

Mantenimiento Diario
Check for leaks, exhaust system and empty the waste
Check N₂O and C2H2 levels
Clean spray chamber
Clean lamps and glass materials
After each day of use…
Use distilled water for cleaning

Mantenimiento Semanal
Deep cleaning of the spray chamber
Check air filters
Check the gas supply hoses

Determinación simultánea de
propiedades físicas y/o
químicas del suelo
Espectroscopía

Espectroscopía IR
Based on the interaction of matter and light in the mid or
near infrared range. Light is absorbed or reflected in
proportion to its physical and chemical characteristics.
Useful for estimation of organic compounds,
mineralogy, texture, pH…

Interaction of IR-Radiation and Matter
Molecules absorb IR light by
• Excitation of vibrations,
• that cause a change in the dipole momentum.
Absorbed IR frequency corresponds to natural frequency of
vibration

Alignedreflection
Diffusereflection
Adsorption
Transmission
Refraction
Dispersion
Principios básicos de medición con IR
Light Source
IR Detector

Spectra
FT
Chemometrics
QuantificationIdentification
Light Source
IR Detector
Interpretation
Principios básicos de medición con IR

Espectro MIR
Mid IR range 2500 – 25000 nm (4000 - 400 cm-1),
Fundamental vibration of functional groups: fingerprinting

NIR: 780 – 2500 nm (12800 – 4000 cm-1)
Consists of overtones and combinations of the fundamental vibrations in MIR
• Broad, overlapping peaks (10-100 cm-1 bandwith)
• Highly complex spectra – Chemometrics needed to extract information
Original Spectra
User Spectra
1/cm
5000 6000 7000 8000 9000
0.2
0.4
0.6
0.8
Nircal:Polymerdispersions.nirunnamed03/07/200201:28:57PMokrs
B
NIR MIR
Espectro NIR

Entonces…MIR o NIR?
• Fundamental vibrations of molecules that
absorb IR light
• Spectra interpretation provides fingerprint
of substances
• Great for soil mineralogy and identification
of more specific substances
• Requires more sample processing
• More expensive equiment
• Combination bands and overtones of MIR
fundamentals
• Broad, overlapping peaks. Chemometrics
required to extract information
• Great for more common soil parameters
(moisture, pH, C, N, texture…etc)
• Simpler sample processing
• Cheaper equipment
NIRMIR

Filter-based Spectrometer: the simplest design
Disandvantages: Measurements only at few determined wavelengths
Disandvantages: Reproducibility of wavelengths depending on the accuracy of the mechanical
components; low light intensity
Dispersive Spectrometer:
Light source
Filter Sample Detector Wavelength
Dispersive
element
Gap
Light source
Sample Detector
Intensity
Wavelength
Intensity
Filter based and dispersive NIR Spectrometer

Moving mirror
Fixed
mirror
Beam divider
Fourier Transformation IR Spectrometer
Michelson Interferometer
for Fourier Transformation (FT) NIRS
Detector
Sample

Moving mirror
Fixed
mirrow
Beam divider
Detector
Sample

Moving mirror
Fixed
mirror
Beam divider
Detector
Sample

 https://www.youtube.com/watch?v=UA1qG7Fjc2A
The interferogram can be converted into an electromagnetic spectra
 Fourier transformation needed
Interferogram
Moving mirror
Fixed
mirror
Beam divider
Detector
Sample

Simultaneous information over all wavelengths  low noise
High spectral resolution
High precision of measurement
MIR devices usually have an FT spectrometer
Less common for NIR devices, but also used
Advantages of the FT Spectrometer
Rayleigh criteria
Fourier Transformation MIR or NIR Spectrometer

Instalación de dispositivos IR
The basic system consists of the spectrometer and a
side computer
• Installation is simple
• Connect the device to the PC
using the supplied Ethernet cable
• Plug the mains cable to the socket
• Switch on the device
• Start the PC, and install the
necessary software
• Set up the communication
between spectrometer and the PC

General site requirements
• Meet instrument space
requirements, plus
some surrounding space
• The spectrometer
should be placed on a
clean, stable and
horizontal base
(instruments are heavy!)

Environmental conditions:
Temperature and humidity variations can impair the
results of long-term measurements

Environmental conditions:
Installation in a controlled laboratory environment is
recommended
• Recommended ambient temperature range: 18°C -
35°C
• Relative humidity should not exceed 30%.
• Avoid vibration or rooms with intense floor
vibrations.
• Cleanliness

FTIR only
Supply of dust free purge gas
The presence of water and carbon dioxide in the path
of the mid infrared beam causes unwanted noise in
the spectrum. Purging the FTIR spectrometer with
clean, dry carbon dioxide-free gas will improve the
signal to noise ratio (SNR) by decreasing the level of
background noise

Additional recommendations
• Always follow manufacturer’s indications
• In FT devices, the scanning mechanism is usually
locked for transportation purposes. Always unlock
before operation
• Carry out instrument calibration and performance
tests prior operation

Simple device operation:
• Calibrate baseline using an external reference (reflectance
standard)
• Place sample in sample container as indicated by user guide
• Measure sample previously dried and homogenised
• Collect
Spectra
• Clean sample container and/or sampling window between
measurements
Interpret spectral features using library (mainly FTIR)
Obtain estimates using chemometrics (calibrations)
Uso de dispositivos IR

Importancia de las referencias
externas
• External references are usually made of a white
standard material (PMMA, Spectralon®…)
• External reference is a reflectance standard (99%
reflectance), used to calibrate reflectance baseline
• Frequent measurements may compensate for
environmental effects and ageing of the lamp,
which might influence the spectra.

Mantenimiento de referencias
externas
• Do not drop or touch the External Reference
• Do not scratch the surface
• Do not use any cleaning media with abrasive character which might scratch the
surface
• Do not use any compressed air for blowing off dirt from the External Reference,
as it often contains oil and is not sufficiently pure.
• If needed, clean with pure acetone
• Do not use item for reference measurement when damaged or scratched!!!

Mantenimiento de los instrumentos
• Regularly carry out system performance tests (as indicated
by manufacturer)
• In general, the following values are tested:
• Internal system temperatures (e.g. Laser, interferometer,
detectors)
• Linearity
• Signal-to-noise ratio
• Wavenumber stability

Mantenimiento de los instrumentos
Careful operation
For example the sample compartment window is a delicate component. Observe
the manufacturer’s handling instructions to ensure a long service life.
• The window is very fragile. Handle it with care because it can scratch easily. Avoid
any mechanical impact.
• Do not touch the window surface
• In FTIR most of the window materials are hygroscopic. Store them under dry
conditions.
Cleaning
• Housing (use dry or damp cloth)
• Optical surfaces and probes (optical tissue)
• Cleaning of the External Reference
Do not clean the spectrometer interior. This may lead to serious spectrometer
damage!

Mantenimiento
• Components replacement (stock spare parts!)
• Lamp module replacement
• Laser unit replacement
• Filter pad replacement
• Main fuse replacement
• Desiccant cartridge replacement

Unas observaciones
generales para concluir…

• Los instrumentos pueden variar entre fabricantes
• Los manuales son muy importantes y la información
que no esté presente en ellos debe ser aportada por
los fabricantes
• Solicite el apoyo necesario del fabricante o
distribuidor – es su derecho!
Observaciones

Agradecimientos
• Instituto Geográfico Agustin Codazzi (Colombia)

Item 7. Instalación de equipos, uso y mantenimiento – buenas prácticas

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