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Spectrometer Instructions

The document provides safety and operational guidelines for using a full spectrum spectrometer, emphasizing the need for trained personnel, proper ventilation, and adherence to electrical safety measures. It details the instrument's features, installation requirements, and maintenance procedures, highlighting the importance of using high-purity argon gas and proper sample preparation. Additionally, it covers the principles of spectral analysis and the relationship between spectral line intensity and sample concentration for accurate quantitative analysis.

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0% found this document useful (0 votes)
12 views26 pages

Spectrometer Instructions

The document provides safety and operational guidelines for using a full spectrum spectrometer, emphasizing the need for trained personnel, proper ventilation, and adherence to electrical safety measures. It details the instrument's features, installation requirements, and maintenance procedures, highlighting the importance of using high-purity argon gas and proper sample preparation. Additionally, it covers the principles of spectral analysis and the relationship between spectral line intensity and sample concentration for accurate quantitative analysis.

Uploaded by

jcandy0530
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOC, PDF, TXT or read online on Scribd

Note for the safe use of the spectrometer

Before using the instrument, you should carefully read the relevant service
instructions to understand the service conditions of the equipment (such as voltage,
frequency, rated output power and other parameters), installation methods, test methods and
parameter range.
1、 The personnel operating the equipment need to be trained and assessed, and can
obtain the certificate before using it;
2、 Avoid other objects blocking the cooling sink of the instrument to ensure its
ventilation; avoid putting the instrument together to avoid scratching the surface of
the instrument;
3、 When the instrument is used for the first time, the manufacturer's installation
engineer (or video connection) must be requested to confirm that the connection is
correct, so as to avoid the operator's damage or damage to the instrument due to the
connection problems;
4、 The circuit part of the instrument should be protected by the grounding wire, the
external power supply must have a real grounding wire, the grounding wire is
installed on the back of the instrument, there is an obvious grounding mark, to
avoid the instrument to damage to personnel and cause damage to the electronic
system;
5、 This instrument has a high voltage system, the normal work of the voltage can reach
1000V, so in the use of the instrument, it is forbidden to open the front cover of the
instrument, prohibit any part of the human body to touch the spark platform and
high voltage module, the instrument has obvious high voltage prompt sign, if
touched will cause harm to the human body;
6、 The test samples of this instrument should be provided with high purity argon gas.
The argon bottle should be fitted with a safety cap and placed vertically on the fixed
support; the window should be opened regularly for ventilation. A certain
concentration of argon will cause suffocation risk.
7、 There are parts in the instrument that require strong electricity. When you check the
circuit parts, if you are not careful, there will be a risk of being shocked or even
dying. So in the maintenance of the circuit, we must turn off the total power supply
of the instrument, do not use liquid or leakage liquid near the circuit components;
8、 When the instrument maintains the spark table, it must turn off the power supply of
the excitation light source. When the maintenance equipment opens the shell, it
must turn off the power supply of the instrument.
9、 Instrument maintenance must ask the manufacturer maintenance engineer or the
manufacturer recognized with the maintenance qualification of personnel
maintenance, otherwise the dangerous instrument manufacturer will not assume any
responsibility.
10、 The instrument shell has an obvious electricity safety mark.

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introduction
Full spectrum spectrometer is a straight reading spectrometer capable of element
analysis of metal and its alloys. The overall stability is easy to change and increase
channels, and even adding an analysis matrix is very simple.
The spectrometer adopts modern photoelectric technology and automation technology,
such as the application of automatic spectral line correction technology, which greatly
improves the automation degree of the instrument, making it simple and flexible.
The spectrometer uses an optical chamber vacuum technique to minimize the
absorption of O2 to the wavelength <200nm line. The stability and detection limit of C, P, S
and other elements of the instrument are well improved, and the high vacuum stop valve is
used to avoid the pollution of vacuum oil to the optical components in the optical room.
The spectrometer uses a constant temperature system (constant temperature of 34℃).
Make the instrument to the environmental temperature requirements is not big, long-term
stability.
The spectrometer uses a digital light source with high integration and maintenance
free, which is a composite light source that can produce spark, arc, arc, arc and other
combined parameters. It can analyze constant, high content, trace elements and even trace
elements and ultra-high content elements.
The software of the spectrometer adopts Windows interface, display in all Chinese,
perfect function and simple operation.
Each instrument is specially manufactured according to the requirements of users,
carefully installed and adjusted, comprehensive calibration, aging. Therefore spectrometer
is the quality assurance of metal smelting process control, is the preferred, ideal analytical
instrument.
This manual aims to make a comprehensive introduction of the spectrometer and
matters needing attention. All the employees of the company are willing to answer your
questions and provide quality and efficient service in various ways.
Due to the hasty preparation of this manual, it is inevitable that there are any mistakes
or omissions. Please criticize and correct us. We will change it in time to meet the
requirements of users. My heartfelt thanks to you for your valuable suggestions!
Finally, we sincerely hope that the spectrometer can bring you good economic and social benefits.

matters need attention

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 Welcome to choose our company direct reading spectrometer, in order to you
better use this instrument, please read the first "Installation instructions" chapter
carefully before the instrument installation.
 This instrument must be used strictly according to the operating instructions.
 The maintenance and repair of the instruments can only be carried out by the
professional and technical personnel trained by the company, and all safety
measures shall be taken.
 Only authentic parts. The damage to the instrument caused by the use of other
accessories is not covered by the company's warranty.
 When maintaining the light source, cleaning the excitation table, and replacing the
electrode, the power supply of the light source system must be cut off.
 For reliable use, back up data regularly.
 If there is any problem that I do not understand, I can call for consultation, and it
is absolutely not allowed to dismantle and repair the instrument by themselves.
Otherwise, the consequences shall be borne by oneself.

direction for use


This manual contains the complete information of the full spectrum spectrometer
required by the user, including technical instructions and operation guidelines for the
hardware and software.
` Daily operation instructions to the function keys, menu, step by step, so that the user
to have a comprehensive understanding and introduction of the function of the
instrument.
Sample analysis includes the preparation of the instrument before the work. Such as:
sampling, sample preparation, etc., and finally is how to obtain accurate analysis data
through the operation of the instrument.
The chapter of instrument calibration gives a detailed description of what corrections
should be made on the daily basis, which is the key technology that the user must master.
The chapter of making the working curve introduces the drawing of the working curve and
some adjustment and calibration of the instrument before making the curve.
Finally, some simple fault phenomena and elimination methods of the instrument are
briefly introduced, and the maintenance of the instrument is a common sense explanation.
The technical data of the instrument is the unique data of the instrument ordered by
the user, which is particularly important for the maintenance personnel. Please keep it
properly. The electrical arrangement of the instrument is described in detail in the hardware
manual, which is very important for the maintenance of the instrument.

installation notice

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1. Transportation and movement
The spectrometer is made of wooden standard packing boxes, which can be removed
directly into the laboratory.
Note: After the instrument arrives at the user site, the Company is only responsible for
guiding the user site to move the instrument to the installation site, and is not responsible
for moving the instrument to the installation space in the user site.
For convenient repair and maintenance, there should be some space on all sides of the
instrument (at least 0.8m away from the wall). The size of the instrument itself is 700mm
560mm 300mm, which can be placed on the table. In addition, leave space for the printer,
computer, and argon bottle near the instrument, so that the working space is at least 10m2,
and all interfaces to the instrument are located behind the instrument.
Note: The instrument must absolutely avoid one side heat (e. g. direct sunlight, close to
the heating device, etc.).
2. Environmental requirements
There is a constant temperature system inside the instrument, so the operating
environment temperature of the instrument is between 10℃ and 30℃. It is recommended
to install air conditioning to avoid the continuous working of the internal constant
temperature affecting the service life of the instrument. The relative humidity at the
working site of the instrument shall be less than 70%. Otherwise, the optical system, high
voltage system or other electronic system will have unpredictable failure due to low
temperature or high humidity.
3. Electrical connection
The power supply requirements of the spectrometer are: 220V ± 10%, 50Hz, 10A fuse.
It is suggested that the user distribution system should have power off protection (with AC
contactor and reset switch) and overvoltage protection (with 3 ~ 5 KVA stabilized power
supply). The main power supply, computer serial port and argon line are behind the
instrument.
4. Argon requirements
Relying on the analytical material, using a spectrometer-dedicated argon gas. The
purity was over 99.9995%.
argon
Purity was 99.9995%
N2 <1PPm
O2 <3PPm
H2O <3PPm
When installing the instrument, qualified argon should be prepared, which is
responsible by the user. If the argon can not reach the subpurity, please use the argon
purification device.
When installing the instrument, the argon bottle shall be equipped with argon meter
(or oxygen meter) and copper pipe or ferrofluorine tube connected to the meter, and the
argon pressure provided to the instrument shall be 0.42MPa.
5. Sample processing
Sample preparation is extremely important when analyzed by spectrometer. The
preparation method depends on the analytical material, steel and other hard materials are

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usually prepared with a tray grinding prototype or belt mill. It is recommended to use 40-60
purpose iron oxide sandpaper or sand plate (cutting plate). The cast iron specimen must be
ground with a rotary-hanging grinder and select the appropriate grinding wheel. For
example: the standby iron sample uses aluminum oxide (palm steel jade) grinding wheel,
and can not use silicon carbide grinding wheel.
Non-ferrous metal materials, such as copper and aluminum, should be prepared using
a high-speed lathe or grinder.
6, and prepared the samples
Steel plant sampling can be taken in a
specific shape; cylindrical samples are cut at 1 /
3~1 / 2; cast iron samples are generally in the
shape of "seal", so that the excitation parts can be
completely "white".

* Sampling should be representative;


* There shall be no inclusions, cracks, and
pores in the sample;
* The surface after preparation shall be
free of oil pollution (note: it is strictly
prohibited to contact the grinding surface by hand after grinding);
* The analysis shall be conducted according to the sampling site specified in the
"National Standard". Seal-shaped cast iron sample

Install the checklist


 Power distribution is complete
 Argon is ready
 Special ground wire matching for the instrument (less than 4 ohm)
 Sample processing equipment (selected according to analytical materials)
 Rotary grinder (grinding wheel sheet (palm steel jade))
 Lathes (nonferrous metal)
 replacement tool
 Sampling equipment and ingot mold

Chapter 1: Principles of spectral analysis


1, the basic knowledge of the spectral analysis
The spectrum is the electromagnetic radiation arranged in the order of wavelength (or
frequency). In a broad sense, all kinds of electromagnetic radiation belong to the spectrum,
which can be divided according to its wavelength:
γ ray 0.00005~0.14nm
x ray 0.01~10nm
Microwave spectra range from 0.3 to 1 nm
The spectral regions can be divided into:

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10 to 200 nm
And 200 – 380 nm near the UV zone
Visible spectral region of 380 nm – 780nm
The NIR spectrum is 780 – – 3 µ m
Far-infrared spectrum of 3- -300 µ m
Note: 1 m (m) =103 mm (mm) =106 microns (µ m) =109 nm (nm)
UV, visible, and infrared are collectively known as optical spectra. The optical direct
read spectrometer analyzed the applied element wavelength, mostly in the vacuum and
near-UV regions.
The general so-called "spectrum" is only refers to the optical spectrum. The spectra
emitted from matter (solid, liquid, gas,) heating or electric excitation are divided into three
types of spectra. Line spectrum is usually obtained by the excitation of atoms or ions in the
gas state, so it is called line spectrum. In terms of its production mode, it can be divided
into emission spectrum (bright line) and absorption spectrum (dark line), so spectral
analysis is divided into emission spectrum analysis and atomic absorption spectrum
analysis. If the spectrum is generated by atomic excitation, it is called atomic spectrum; if
the spectrum generated by ionic excitation is called ion spectrum. We usually talk about the
spectral analysis, generally refers to the "atomic emission spectral analysis", the
photoelectric spectral analysis of the element wavelength is the atomic spectrum and ion
spectrum of the elements.
Now the photoelectric spectrometers are mainly divided into two categories. The non-
vacuum photoelectric spectrometer works with a wavelength range in the near-ultraviolet
and visible regions. The working wavelength of vacuum photoelectric spectrometer extends
to vacuum ultraviolet 120.0nm, so the sensitivity of carbon, phosphorus, sulfur and other
spectral lines in this band is used to analyze the important elements in steel.

2. Basic principles of qualitative and quantitative analysis of the

spectrometer
2.1 Relationship between spectral line intensity and sample concentration
Quantitative spectral analysis, mainly based on the analysis of the concentration of
the spectral line intensity of the elements. The relationship between the line strength of the
element and the concentration of the element in the specimen can be expressed by the
following empirical formula, namely the Seber-Roman Gold formula:

Where I is the intensity of the spectral line, C is the concentration of the analyzed
element, A is A parameter related to the evaporation, excitation process and sample
composition of the sample, and the size of the constant b is related to the self-absorption of
the spectral line.
2.2 Internal standard method and analysis line pair
Due to the evaporation of the sample, excitation conditions and any change of the
sample composition, make the parameter A change, will directly affect the line strength,
this change often is difficult to avoid, so in the actual spectral analysis, often choose a
comparison line, spectral quantitative analysis with analysis line intensity ratio, to offset the

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influence of these uncontrollable factors A, the comparison line used inside line, provide
the comparison line elements called internal standard elements.
In the spectral quantitative analysis, the content of internal standard elements does not
change much. It can be the basic component in the sample, or it can be added to the
additional elements in the sample with a certain content. This method of quantitative
spectral analysis by analytical intensity ratio is called as the internal standard method. The
combination of the analysis line and the inner line line chosen is called the analysis line
pair.
If a and r represent the analysis line and the internal line marking,
respectively, then:
Analyze line intensity

Internal line marking strength

When the internal standard element Cr is fixed, i. e., the intensity ratio of the
analysis line pair is:

Make K = Aa / A0, C = Ca, and b=ba then

In a certain concentration range, k and b are independent of the concentration, and this
formula is the basic formula for the quantitative analysis of the internal standard method.
However, not any element can be used as internal standard, and any pair of spectral lines
can be used as analysis line pair. In order to make K value a constant, the following
conditions must be met for the selection of internal standard elements, internal line marking
and analysis line:
A) The analysis line corresponds to the same or similar excitation potential and ionization
potential, so as to reduce the influence of the change of discharge temperature (excitation
temperature) on the change of the analysis line on the dissociation degree, excitation
efficiency and ionization degree;
B) The internal standard element and the analytical element shall have close melting point,
boiling point, chemical activity and similar atomic weight, so as to reduce the impact of the
change of the electrode temperature (evaporation temperature) on the relative strength of
the analytical line caused by remelting, sputtering, evaporation, diffusion and other
changes;
C) The content of internal standard elements does not change with the content of the
analytical elements. The matrix element iron is often used as the internal standard in steel
analysis; in the standard sample design, the content of internal standard elements is
basically consistent to reduce the influence of matrix effect;
D) The self-absorption of analysis line and internal line should be small. Generally, the
resonance line with the self-absorption coefficient b=1, the choice of resonance line in low
content; in high content, the non-resonance line with self-absorption coefficient b close to 1
can be selected;
E) The background near the analysis line and the inner line should be as small as possible

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with no interference elements to improve the signal to noise ratio. In fact, the above
conditions is difficult to meet at the same time, and in most cases also need not meet at the
same time, such as in steel and pure material composition, because it is easier to achieve
stable excitation conditions, so in the analysis line, even if the excitation potential and
ionization potential difference is larger, still can get satisfactory effect.
2.3 Quantitative relation of the full spectrum
In the whole spectrum spectrum analysis, the sample after the light of the light, the
incident slit to the dispersion system grating, after concentrating the monochromatic
light is focused on the focal surface form spectrum, placed on the focal surface several
outgoing slit, the analysis element specific wavelength, analysis line to photomultiplier
tube receiver, the light energy into electrical signal, stored by the integral capacitance,
when the exposure is terminated, by the measurement system individually detection on
the integral capacitor voltage, according to the size of the measured voltage value to
determine the content of the elements.
During the excitation process of the sample, the intensity of the spectral line is
unstable, so the instantaneous value of the photocurrent output from the receiver will
fluctuate. Therefore, the output is often transferred to the integral capacitor charging
method to measure the average intensity of the spectral line.
If the integral capacitor is C, the photocurrent is I, and V is the voltage reached on
the integral capacitor after the integration time T, then

Where i is the average photocurrent, it can be seen that the voltage V on the integrated
capacitor is proportional to the average photocurrent i and the exposure time T, and
inversely proportional to the capacitance of the integrated capacitor. In the practical
work. C and T are constants, where the average photocurrent i is proportional to the
line intensity, for which the voltage of the integrated capacitor is measured to find the
content of the elements in the sample.

3, Methods for full-spectrum quantitative analysis


In spectral quantitative analysis, due to the influence of analysis conditions, the k
value and b value in the formula are only applicable to the same type of samples, different
types of samples, their k value and b value will change, so the experimental calibration
curve must be made to determine the content of the elements in the sample C.
3.1 Standard test sample method
This method is to stimulate a series of standard samples before each sample analysis.
(strictly speaking, standard samples with the same smelting process and crystal structure
should be used. In fact, this match is hard to do.) Make the calibration curve. The
relationship between line intensity and analyte concentration can be expanded as a power
function:

Store after successful curve fitting. Then the samples to be tested are analyzed, and the

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intensity value I of each element is inserted into the above formula to calculate the content
of the elements to be measured.
Although the standard sample method can maintain the completely consistent analysis
conditions and the analysis results are accurate and reliable, each analysis needs to
stimulate a series of standard samples and redraw the calibration curve, which is not only
time-consuming and laborious, but also large standard sample loss. Therefore, the
persistent curve method is commonly used in photoelectric spectral analysis.
3.2 Persistent curve method
The persistent curve method is to make the persistent calibration curve with the
standard sample method in advance, and only stimulate the analysis sample in each
analysis, and the content is obtained from the persistent curve.
Due to the changes of temperature, humidity, argon pressure, vibration and so on, the
spectrum line will produce displacement, lens pollution, electrode pollution, power supply
fluctuation will make the calibration curve shift or move. Therefore, in the actual analysis
process, every day (each shift) must be used for correcting the drift of the standard curve,
which is called the standardization of the calibration curve.
There are two-point standardization and single-point standardization: two-point
standardization is to select two standard samples near the upper and lower limit of the
calibration curve, and find the light intensity Rv and Rl respectively:

Two types of phase reduction

Where Lu 0 and Rl 0 are the light intensity values corresponding to the upper and lower
content of the original persistent curve, respectively. α and β are the drift coefficient of the
curve, α represents the change of the slope of the curve, and β represents the translation of
the curve.
For single point standardization, select only one standard sample with content near the
upper limit, the light intensity R measured at excitation, the original reference on the
original calibration curve is R0, and the correction factor is:

This normalization method can only correct the translation of the original calibration curve.
In practical work, due to the difference between the metallurgical process of the test sample
and the standard sample and the state of some substances, the analysis results often have
some deviations, which needs to be corrected by control samples.
3.3 Control the test sample method
Control sample is a standard sample consistent with the metallurgical process and
some physical states of the analytical test samples. The content of each element should be
accurate and reliable, evenly distributed, without pores, trachoma, and cracks, and the

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content of each element should be within the content range of the calibration curve, which
may be close to the content of the analytical samples.
In daily analysis, analyze the control sample and the sample to test with the same
working conditions as the sample to be tested. Set the reading of the control sample as R
control, the corresponding content is C control, the reading of the test sample is R control,
and the corresponding content is:

From this, we obtained the actual content of the samples to be tested.

Chapter 2: Basic composition of the instrument


2.1 Instrument appearance diagram

picture

Chapter 3: Characteristics of the instrument

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1. Instrument technical features

1,300mm focal length grating design, Pa-longge device, high vacuum, high resolution, high
sensitivity characteristics; because the machine engraving grating can produce more
advanced spectrum, so the line selection is more flexible, so as to avoid spectral interference;
2、The instrument structure design is reasonable, the electronic system adopts the
international standard machine cage, high integrated circuit design, low failure rate;
3、Fast analysis speed, good repeatability, good stability;
4、It can be used for multiple matrix analysis: Fe, Co, Cu, Ni, Al, Pb, Mg, Zn, Sn, etc.;
5、Using the operation software under the pure Chinese Windows system, the operation is
simple and easy to understand;
6、Computer software has a database system, convenient for the query and printing of
measurement data, but also through the network remote transmission of data, convenient
and fast;
7、Each system is independent power supply, composed of units, easy to use, simple
maintenance;
8、Using the optical part of the constant temperature measures, to ensure the normal
operation of the instrument, thus reducing the requirements of the environment;
9、Add, change the element channel, through the software Settings can be, do not need to
add any hardware, save worry, save time, save money
10、The analysis speed is fast, after testing the elements of all channels within 30 seconds.
For different analysis materials, by setting the precombustion time and line marking, so that
the instrument with the shortest time to achieve the optimal analysis effect;
11、The optical system of the spectrometer adopts vacuum and constant temperature light
chamber, and the arc flame generated during excitation is directly imported into the
vacuum light chamber by the lens to realize the light path direct connection, eliminate the
light path loss, improve the detection limit, the measurement results are accurate, the
reproducibility and long-term stability are excellent;
12、Automatic optical path calibration, optical system automatically for spectral line
scanning, to ensure the correctness of receiving, avoid tedious peak scanning work. The
instrument automatically identifies the specific spectral line, compares it with the original
storage line, determines the drift position, and finds out the current pixel position of the
analysis line for determination;
13、Open electrode frame design, can adjust the sample clip, facilitate the sample analysis
of various shapes and sizes;
14、The working curve adopts international standard samples, and the pre-made working
curve can be extended and expanded according to the needs, and the excitation of each
curve is generated by dozens of standard samples, which will automatically deduct
interference;
15、Excitation energy, frequency continuous adjustable full digital solid-state light source,
adapt to a variety of different materials;
16、Solid state adsorption trap, prevent the pollution of oil and gas to the light chamber,
improve the long-term operation stability;

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17、Reasonable argon gas circuit design, shorten the argon flushing time, for the user to
save argon, argon consumption less than half of the ordinary spectrometer;
18、High-performance DSP and ARM processor, with ultra-high-speed data acquisition
and control function and automatic real-time monitoring of light chamber temperature,
vacuum, argon pressure, light source, excitation chamber and other modules.

2. instrument parameter
2.1 Optical system
Optical structure: Full spectrum optical system of Pxing-Longge structure (vacuum)
Length range: 165-589nm
Grating focal length: 300nm
Grating engraving line: 2400 / mm
First-level spectral line dispersion rate: 1.1 nm / mm
Photoelectric detector: multiple high-performance line array CMOS
2.2, and the excitation table
This excitation stage adopts punching argon type, jet type click structure, with automatic
purge function. The platform opening size is 13mm.

2.3 Inspire the light source


Type: fully digital spark excitation light source
Frequency: 100-1000Hz
Discharge current: pulse 1-100A
2.4 Data acquisition system
High-end ARM processor, high-speed data synchronous acquisition and processing,
DM9000A-based Ethernet data transmission.

Note: this instrument is through the network port and computer


communication, it is forbidden to change this IP address to

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access the Internet, if you need to access the Internet, you can
connect to the external network through the wireless network!!!
2.5 External size of the instrument
Dimensions: 700mm 560mm 300mm
Weight: about 98 Kg

Chapter 4: Operation method of the


spectrometer
1. Open the machine machine
1、 The startup sequence is to turn on the main power switch behind the instrument,
then open the light source switch in front, and then turn on the computer host,
display and printer in turn. Open the main valve of argon bottle and adjust the
pressure gauge to about 0.42 Mpa.
2、 Shutdown order is just the opposite, the first close peripheral after the host.
3、 The instrument is in standby mode:
The temperature and humidity meet the requirements, the temperature is between 10 and
30℃ (best controlled at about 25℃), and the relative humidity is <70% (best
controlled at 60%);
Note: If the instrument needs to analyze samples every day, it is recommended that the
main power supply is always turned on to ensure the constant temperature and high
vacuum, and the CMos detector are stable, so that the instrument can enter the standby
analysis state at any time; for more than two days, all the instruments can be turned off, but
the main power supply is turned on 2-4 hours before using the instrument.

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2. Analysis software
1. Open the analysis program
Double-click the desktop shortcut icon "Spectrometer", and the screen displays the login interface, as
follows:

&quot;User name&quot; is to prompt what mode login analysis software, optional project
have operator and administrator, the operator only the right to use the software, any
analysis parameters in the software is not allowed to modify, administrator mode login
interface, can modify some parameters in the analysis, such as: excitation time, frequency,
etc.
"Password" is to enter the correct password and log in to the analysis interface. The
password is in the case of letters. Generally, the operator password is 123456, and the
administrator password is 123.
Click "OK" to enter the software, click "Exit" and leave the software.
After entering the analysis main interface, the display is as follows:

The main interface is divided into analysis window, menu bar and Settings bar
"Analysis window" is used to display the content of analysis elements, each row displays
10 elements, extra elements to the second column display, up to three columns elements,
each time per screen display 11 columns, extra columns need to be pulled down scroll bar
display, analysis times more than 2 times automatically display SD and RSD values.
The Menu Bar displays File, Data, Performance, Operations, Instrument, Format, and Help,

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respectively, describing the functions of each submenu bar:
1. Documents:

" Exit" means the exit from the software.


2、data:

" Query analysis data": query saved data, saved data must be
edited for the sample name of the data, otherwise it can not confirm what data, query data
can be queried according to the date and sample name, the query data can be printed in
batches;
"Report Information Settings": set the report format of the printed data, and can set the
printed items, such as: the name of the sample sending unit, etc
3、function:

"Analysis window": the interface of the analysis element display;


"Curve call": select the appropriate analysis curve of different materials, such as iron
matrix and aluminum matrix, etc. Iron matrix can be divided into alloy steel, stainless steel,
cast iron, aluminum alloy can be divided into ordinary aluminum and cast aluminum alloy,
etc. Select the appropriate analysis curve according to the material when analyzed.
"Recall the current analysis curve": after recalling the secondary analysis curve to refresh
the secondary analysis curve, the element content displayed on the last interface is cleared.
"Control sample correction": used to select the standard sample selected for this calibration
analysis sample. Divided into "new" and "view", the new is to establish a new control
sample, control sample correction, need to stimulate the control sample 2-3 times, take
repetitive good data saved, general requirements of relative standard deviation RSD less
than 3, "view" is to view all the correction coefficient of the control sample, not modified
and to control sample.;
"Light intensity standardization": when the parameters of the instrument are offset, the
instrument needs to be corrected, and at this time, the instrument needs to be corrected
through the high and low standard. It can be divided into "new construction" and "view".
The new construction is to stimulate the standardized sample. Each sample should be
stimulated 2-3 times, and select the data with good repetition to save. Generally, the
relative standard deviation RSD is less than 3.

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"Spectral line correction": when the analysis accuracy of the instrument deviates with the
change of temperature and vacuum, the optical path of the equipment should be corrected.
At this time, a factory sample should be stimulated, stimulated 5-8 times, click all the
optical paths after correction, and then click save to put the correction into effect.
Element Display Settings: the order of elements in the analysis interface and the number of
decimal points.
4、operate:

"Open Argon": open the argon solenoid valve, test whether there is argon through the instrument, can be
observed through the flowmeter, and the general main argon is 5-6L, the auxiliary argon is 1.5L;
"Argon gas": close the argon solenoid valve;
"Vacuum pump analysis status": display the setting state of the vacuum pump;
"Vacuum pump standby state": display the setting state of the vacuum pump;
"Instrument reset": when the power switch of the light source needs to be restarted, click
this command to reset the light source (or press the R key on the keyboard), and the reset
light source can stimulate the sample.
5、instrument:
This menu is displayed after administrator login, and is mainly used to set the hardware of
the instrument.
6、forms:

The style used to display the form.


7、help:

The shortcut keys and instructions for copyright, and analysis.


8. The "Setting Bar" is mainly used to set the data processing mode before and after
analysis:

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8.1 "Excitation": it is the excitation of this analytical sample;
8.2 "Content correction": in the analysis of samples, call the control sample, the
control sample needs to be stimulated, and effective, when click the control sample
correction, select the required control sample to correct the sample to be
stimulated, generally need the control sample of the same material to correct, when
the appropriate control sample, the name of the control sample will be displayed;
8.3 "Sample Name": the name of the stimulated sample;
8.4 "Storage data": save the stimulated data in the database, and the
name of the sample should be filled in when saving the storage data for
later viewing and printing;
8.5 "Generation report": it is the way to guide the WORD2003
spreadsheet, divided into exported average and all analysis data;
8.6 "Print data": print the data in the form of the average;
8.7 "Import spectra": reimport the previously exported spectral excitation data to the
analysis interface for display;
8.8 "Export spectra": the results of this analysis can be exported in different formats to
facilitate the import of this analysis data to the analysis interface later;

9. Status Bar: In this column, Sample Name shows the name of the current excitation
sample; The &quot;Content correction&quot; shows whether the control sample correction
is enabled for this excitation; &quot;Analysis curve&quot; shows the analysis curve
selected for the excitation sample; The &quot;Light chamber temperature&quot; shows the
light chamber temperature of the instrument, Generally changes within the range of 34 ±
0.5℃; &quot;Vacuum degree&quot; shows the vacuum state of the instrument, Generally,
&lt;20Pa; &quot;Sufficient flow&quot; indicates that argon is on, The input pressure
detected by the pressure switch on the gas circuit module is 0.5MPa, If the
&quot;insufficient pressure&quot; shown here indicates that argon is not open or the output
pressure of argon is less than 0.5MPa; The Alert Status shows the online status of the
instrument and the communication status of the light source, The presence of green
indicates the normal, If red appears, It means that the excitation light source switch is not
on or the instrument and the computer are not connected, Can double-click here, An error
message will appear.

2. Preparation work before measuring the samples


Before the sample analysis, you need to call the appropriate working curve, please click the
curve call within the performance on the menu:

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Then enter the main interface and stimulate the waste sample. When analyzing the
sample, check whether the pressure of the stator on the gas path module is 0.42MPa
until the data stabilizes. After stabilization, then stimulate the sample whose
component content was determined.
The following figure shows the image excited by different materials, the steel
sample is the central point, around the black circle; cast iron sample central point,
surrounded by a circle of white, the higher the silicon content, the larger the white
circle;

Steel samples
Iron samples
(1) If the results are consistent with the nominal value, the daily analysis can be
performed.
(2) If the result is not much different from the nominal value, the control sample shall be
done (type standardization)
(3) If the result diffgreatly from the nominal value, it should be standardized.
3, the calibration method of the spectrometer
The instrument is in use due to changes in environmental conditions. For example, the change of
temperature and humidity, the fluctuation of power supply voltage, the replacement of argon, cleaning
the spark table and other factors will cause slight changes in instrument parameters, so various
calibration should be carried out frequently.
3.1 for spectral line correction
Correction is the calibration of the optical system, due to the thermal expansion of the
material, may cause a small deviation of the instrument seam. We adjusted the effect of this
shift on the results of the analysis by moving the position of the entry seam.
When the indoor temperature change is obvious or the downtime is long, the general

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temperature fluctuation is more than ± 5℃, the data drift of the instrument is large after the
control sample analysis. If the indoor temperature is constant, it can be corrected about
once every three months (or longer).(See Appendix 1 for the specific operation method.)
3.2 Instrument standardization
Standardization is a method of correcting the working curve of element features by high
and low standard. Since the condition of the instrument work is a relatively stable state
composed of many factors. Instrument working environment (temperature and humidity)
change, change the purity of argon, argon pressure (the size of the flow), the sample
grinding surface and operator operators and a series of external factors, can cause the
instrument working curve drift, in different periods of the test results of the same sample is
different, so the instrument should be standardized according to the usage at any time;
In addition, some factors that can change slowly in the instrument work with time,
such as: pollution of lens, aging of electronic system, energy attenuation of optical system,
etc., will cause the slow drift of the working curve.
In short, the drift of these working curves can be corrected by standardized means, so that
being relatively stable for a period of time is enough to meet the work needs.
The standardization process can be realized through the drop-down menu. Click
"Light intensity Standardization" in the "Performance" menu to enter the standardization
procedure.

Click AS1 sample, but AS1 display effective, then click "stimulate" to analyze the sample,
generally the sample analysis 2-3 times, select good repetitive data; the first sample
analysis, click AS2, make AS2 effective, click "stimulate", the second sample analysis
process, select the second data in the first piece, when all samples are analyzed, click the
next step to save the standardized analysis data.
pour:
A) For each excitation, pay attention to observe the quality of the excitation point, and
listen carefully to whether there is a leakage sound.
Bb) After stimulating two- - - - -three points, carefully check the reproducibility of the
calibrated channel. When meeting the requirements (specific requirements are <5%
depending on the content), you can directly press the F3 key to measure the next sample.
And c) if poor reproducibility, it can be continuously excited until sample reproducibility is

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required.
D) The reproducibility is directly related to the purity of the grinding samples, the argon
gas, and the homogeneity of the samples. The calibration of the channel elements
shall be of good precision.
Carefully check the standardization coefficient, the normal coefficient is generally
around 1. When the deviation of this coefficient is large, especially the results beyond the
range of 0.5-2.5, the correction of the normal measurement result is large, and the
measurement deviation is also large. Find out the reason or perform instrument
maintenance operations (wipe the incident window opening, generally clean the spark table
first, and then wipe the incident window opening).
3.3 Type standardization
If the channel analysis range of an analysis program is relatively large or there is
interference (such as, superposition interference, matrix effect, etc.), the control sample
analysis still deviates after standardization, the type standardization should be conducted.
Type standardization can effectively calibrate the impact of various disturbances on the
analysis results. It is especially suitable for multi-sample analysis of metals and their alloys
with the same sample content or the same grade. Type normalization is a method of making
local correction of the working curves of the elemental analysis channels.

Input of type controlled concentration


1. Click the "Concentration Library" menu and input the content of the secondary control
sample into the standard concentration library. The secondary concentration library is in the
file menu and only visible after logging in the administrator mode;
2. Enter the content value of each element in turn according to the content table, and click
Save.

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Selection of type control samples

Click the "Control sample Correction" in the "Performance" menu, select New, the above
menu appears, in the menu, click the "New" button to establish a new control sample, and
then name the control sample, as shown in the figure:

After transmitting the name of the control sample, click OK, add the standard sample that
needs to be found from the concentration library. After finding the sample from the
concentration library, right click the sample, click "Select the node" and add the sample as
the control sample.
Type standardization

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Select the control sample to be stimulated, and analyze the sample after clicking
"stimulate" to excite each sample 2-3 times.
Note: Like standardization, the reproducibility, or precision, should be strictly
assessed.
Click "Save" to display the type-standardized measurement results. Under normal
circumstances, the proportion coefficient with proportion correction should be close to 1,
and the offset using translation correction should be relatively small. When the deviation
is large, find the reason:
A) Poor standardization.
And b) Poor excitation of type standardized samples (air leakage, segregation, etc.).
C) Less measurement measurements.
And d) Incorrect determination of the alloy procedure.
E) Samples were not correctly selected.
If the coefficient meets the requirements, click <Accept>.
Note: check the accuracy of the instrument analysis with the type of standardized
sample, and meet the indoor or room deviation required by the national standard,
the sample analysis can be carried out.
When the control sample is excited, the control sample to be used is selected through
the "content correction" on the main interface. After the control sample is selected, the data
for the next analysis is the analysis results measured using the control sample. If the control
sample is not used, "no correction" and the result of the next analysis is not the data of the
control sample.

appendix
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Appendix 1. Optical calibration
Calibration is the calibration of the optical system, which may contribute to the small
deviation of the instrument CCD because of the material. We adjusted the effect of this
offset on the analysis results by the location of the software.
When the indoor temperature change is obvious or the downtime is long, the general
temperature fluctuation is more than ± 5℃ or the shutdown time is long, the data drift is
large when the instrument is doing the control sample analysis should be calibrated first.

Put the spectral correction sample (with the sample attached when the instrument leaves the
factory), click "excitation", after 5-7 tests, get the average of the spectrum, click the
"correction" button, the software will automatically calculate the correction result, and then
click "after" exit, that is, to complete the spectral correction.

Appendix 2 for spectrometer maintenance


1. Check the discharge clearance of the spark table

1.1 Unscrew the screw at the adjustment hole in the drawing with a one-word screwdriver,

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and then release the screw fixing the tungsten electrode from this adjustment hole with
the inner hexagon wrench of M3;

1.2 Cover the


excitation hole (the
other end of the
pressing bar) with
a 3.4mm spacing
gauge, release the
electrode fixing
screw on the left
side of the
excitation table,
and then press the
electrode with the spacing gauge until the spacing gauge fits the surface of the excitation
table. The protruding part of the spacing gauge should be completely placed into the hole
on the excitation table plate, and then tighten the electrode fixing screw.
2、 Stimulation table cleaning
When the sample is analyzed more than 600 times, the excitation platform shall be
maintained as follows:
A)Release the panel of spark table with an agon wrench;
B)Wipe the excitation table panel with skim cotton dipped to pure alcohol;
C)Pull out the exhaust gas pipe, use a vacuum cleaner to clean up the dust in the excitation
cavity, and then further clean up with skim cotton, absolutely can not use the liquid other
than alcohol to clean up the spark table;
D)After the alcohol in the excitation chamber after the excitation table panel is completely
evaporated, cover the panel and fix the four screws with spacing
Re-measure the analysis spacing once.

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Note: When cleaning the spark table, the power switch
stimulating the light source must be closed, otherwise it may
cause electric shock. Remember!!!
3、 Filter bucket cleaning
Clean the is is when when samples exceeds 2500 times.
Remove the exhaust gas bucket from the pipe, unscrew
the exhaust gas bucket, take out the filter element inside,
and use a vacuum cleaner to clean the dust in the pipe
and the exhaust gas bucket. If the filter element is too
dirty to use, you need to replace the filter element, and
then use a vacuum cleaner to clean the dust in the dust
of the exhaust gas pipe.
4、Lensing cleaning
The condenser is the only channel for the light
emitted by the sample to enter the spectrometer, and the mirror must be kept clean. But the
long-term use of the concentrating mirror will be contaminated, its outer surface attached to
a layer of tea-brown material, the longer the time, the thicker the deposition. The metal
powder produced by excitation will also adhere to the outer surface of the lens, reducing
the transmittance of light, which can reduce the absolute light intensity of all the elements,
especially the far-UV elements C, P, and S. It can reduce the working curve slope of the
element, reduce the analytical sensitivity, and increase the analytical error. So it is
necessary to regularly clean up the system, how much time to clean up once, to see the
analysis of the work task, generally 10-30 days to clean up the best. The two following lens
cleaning methods are listed below:
Open the upper cover of the instrument, you can see the lens state shown in the picture.
First, prepare the ether and ethanol (1:1) mixture, skim cotton and lens paper, close the ball
valve, and then draw the lens plate outward, the lens fixing plate can be removed, and the
condenser is exposed. The exposed surface of the light condenser was wiped with skimmed
cotton, dipped in a little mixture of ether ethanol, and wiped outward from the center of the
light condenser. If the pollution is serious, you can wipe it several times until you wipe the
dirt and then erase the watermark with dry cotton balls. The cleaned lens can be placed in
the sun and can not see the dirty things.
Special attention should be noted that the concentrating mirror is made of quartz, can
not use hard objects (never use metal tweezers to clip cotton), so as not to scratch the lens
surface.

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Lensing analysis status Clean the lens state

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