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Studiul spectrofotometric al mediilor active laser

Scopul lucrării:

• Analiza transmisiei şi absorbţiei pentru un mediul activ laser solid (sticlă dopată cu Nd);

• Analiza transmisiei şi absorbţiei pentru un mediu activ laser lichid (Rodamina G6);

• Analiza transmisiei şi absorbţiei pentru determinarea coeficientului de reflexie spectral al unor


componente optice laser (două oglinzi laser). Coeficientul de reflexie = 1- (coef.absorbţie+coef.transmisie).

Determinările se fac cu ajutorul unui spectrofotometru cuplat cu un calculator.

-capacul de acoperire a locaşului de introducere a probelor -comutator de pornit/oprit;


investigate; -cablul de alimentare la reţeaua electrică (220V);
-tamburul de variaţie a lungimii de undă (de la 335 nm până -cablul de transmisie a datelor la calculator;
la 1000 nm);
-buton de setare 0%;
-buton de setare 100%;
-buton de setare a funcţiei de măsurare;
-buton de setare „mode” (transmitere la calculator a datelor
pentru lungimea de undă stabilită);
-afişajul lungimii de undă (733nm);
-afişajul valorii numerice a funcţiei de măsurare (35,2%);
-afişajul funcţiei de măsurare (transmisie);

-suportul de probă ce conţine o placă plan paralelă din sticlă -fereastra de dialog a softului de achiziţie şi prelucrare a
dopată cu Nd; datelor.
-suportul de probă ce conţine un paralelipiped cu două
oglinzi laser diferite (se poziţionează pe rând în dreptul
fantei suportului prin rotire cu 180o;
-suportul de probă ce conţine o cuvă cu mediul activ laser
lichid – colorant: Rodamina G6;
INSTRUCTION MANUAL
The instruction manual is for the spectrophotometer. To ensure the safety and obtain optimum performance and familiarize yourself
fully with the use of this spectrophotometer, we recommend that you read this manual thoroughly before operating the
spectrophotometer.Retain this instruction manual in an easily accessible place near spectrophotometer for further reference.
1 1 PRINCIPLE, APPLICATION AND CHARACTERISTICS
1.1 Principle
The series spectrophotometer is a single beam spectrophotometer with simple structure and fine properties. It is
conventional to use for qualitative and quantitative analysis of various sample based on optical absorption law of
substances and principle of comparative measurement. It is to say, in the wavelength that can be absorbed by tested sample,
setting the transmittance up to 100% for selected standard sample of impregnate or air, the transmittance value of tested
sample will be get correspond to standard sample. In a certain concentration range, every parameter follows:

A-absorbance
T-transmittance in relation to standard sample
I-intensity that light irradiate detector through measuring sample
I0-intensity that light irradiate detector through standard sample
K-extinction coefficient of sample liquor
L-length of optical path in sample liquor
C-concentration
1. 2 Application
It is widely used in biochemistry, petrochemistry, environment monitoring, education, medical and sanitary examination,
etc. for qualitative and quantitative analysis of various substance.
1. 3 Main Character
1. Wide spectrum range (335nm~1000nm), the entire numerical displays of the wavelength and the reading of measurement
2. Automatic on replacement “0” and “100%T”
3. The functions of setting concentration factor and setting concentration.
4. The sample chamber obturated wholly for operating
5. RS232C connector that can connect with personal computer
2 SPECIFICATIONS AND STANDARD ACCESSORIES
·Optical system, C—T monochromator, 1200 line/mm holographic grating
·Wavelength range: 335nm - 1000nm
·Light Source: Halogen Tungsten Lamp- 20W / 12V
·Wavelength Accuracy:±2nm
·Wavelength Repeatability: 1nm
·Photometric Accuracy:±1.0%(T)
·Photometric Repeatability:0.3%(T)
·Spectral Bandwidth :10nm (model 1), 6nm (model 2)
·Stray Light:≤ 0.2%(T) (360nm, NaNO2)
·Display: T-0 - 199.9%
A--0.3 - 2.5
F-1 - 9999
C-0 - 9999
·Power:(220V10% 50Hz) / (110V±10% 60Hz)
·Dimensions:385 W×310 D×190 H-mm
·Net Weight: 5.5Kg
Standard Specification:
Item Specification Quantity
1 Spectrophotometer 1
2 Square sample cell 2
3 1cm Colorimetric frame 2
4 Colorimetric frame with Didymium Filter 1
5 Power cable 1
6 Manual 1
7 Inspective eligible card 1
8 Fuse (1A) 2
·Optional accessory :
1. Fuse: 1A
2. Power lamp with adjustable holder
3. 1cm, 2cm, 3cm sample cell
4. 1cm, 2cm (3cm) colorimetric frame
5. 1cm sample chamber subassembly
6. 2cm (3cm) sample chamber subassembly
7. 2cm (3cm)colorimetric frame with Didymium Filter
8. Spectrophotometer’s software (set)
9. RS232C cable
3 NAME AND FUNCTION OF COMPONENTES AND OPERATIONAL KEYS
1 MODE key: Select running mode. When pressing the key repeatedly the pilot lamp of TRANSMITTANCE, ABSORBANCE,
FACTOR and CONCENTRATION will be lighted in circulation it indicates the current running mode.
2 FUNC key: Preconcerted function-extending key. The key is used to shift the setting bit of the FACTOR data when the pilot
lamp of FACTOR is lighted and to shift the setting bit of the CONCENTRATION data when the pilot lamp of
CONCENTRATION is lighted. The readings of display can be transmitted to personal computer through RS232 port under the
mode of TRANSMITTANCE, ABSORBANCE, FACTOR and CONCENTRATION.
3 100%ADJ key: When the pilot lamp of TRANSMITTANCE is light-press the key once to adjust 100%(T) automatically (if
not, press it again); When the pilot lamp of ABSORBANCE is light, pressing the key the absorbance display value is 0.000.
When the pilot lamp of FACTOR is light, it is used to reduce FACTOR setting value. When the pilot lamp of
CONCENTRATION is light, it is used to reduce the setting value of concentration.
4 0%ADJ key: When the pilot lamp of TREANSMITTANCE is light, the key is used to adjust 0%(T) automatically (if not,
press it again). When the pilot lamp of ABSORBANCE is light, the key is useless. When the pilot lamp of FACTOR is light, it
is used to increase FACTOR setting value. When the pilot lamp of CONCENTRATION is light, it is used to increase the
setting value of concentration.
5 CONCENTRATION and pilot lamp: Displays tested data or set concentration on the numerical display
6 FACTOR and pilot lamp: Displays data of concentration factor on the numerical display
7 ABSORBANCE and pilot lamp: Displays data of absorbance on the numerical display
8 TRANSMITTANCE and pilot lamp: Displays data of transmission on the numerical display
9 Numerical display window: 4 bit LED number- Displays the testing data and the wrong or overflow information.
10 Wavelength display window(4 bit LED number): Displays current wavelength data.
11 Sample chamber: It is used for installing colorimetric frame.
12 Wavelength adjustive knob: It is used for adjusting wavelength.
13 RS232C port: Can be connected with personal computer through RS232C interface cable.
14 Elaborate adjustive hole of wavelength: It is used for accurate adjusting the display of the wavelength.
15 Electrical outlet: Connect power cable.
16 Fuse cable: Install fuse.
17 Power switch: Turn on or off power.
4 INSTALLATION
4. 1 Environment for installation
The instruments are suitable to work in room such as analysis lab. It can be connected with computer. Working
environment condition as below:
0 0
· Temperature: 5 C - 35 C
· Humidity:≤ 85%
· Avoid exposure to sunlight, high temperature and humidity, dust and vibration.
· Power voltage: (110V / 220V) 10%, 50Hz/60Hz ±
·Clean surface of the instrument gently by gauze with clean water, avoid with ethanol, ether and acetone and so on. If
necessary, move with original pack, and spot working environment accord requirement, if especial requirement, explain
as order, it is convenient to supply.
4. 2 Open and check
4.2.1 Please check packing is in good condition before open the box, if package is broken or damaged, please connect
transportation insurance.
4.2.2 Unseal box along adhesive tape (save packing box for move). Check the amount spectrophotometer, standard fittings and
accessories for choose refer to list, if wrong, please connect district agent or our company.
4. 3 Install
Wipe off every adhesive tape fixed and clean surface, mount spectrophotometer on the steady desk, the distance is more
than 10cm between wall and back-end, turn on power, enter working condition.
5 OPERATION
5. 1 Basic operation of instrument
5.1.1 Pre-heating
Turn on power of the spectrophotometer for 30 minutes in order for the balance of inside heat. If urgent to use, when
the warm-up time less 30 minutes, pay attention to adjust 0%(T) and 100%(T) in time to insure the result of testing effect.
5.1.2 Adjust 0
Objective: Adjust two end of essential reading staff ( 0%-T-and100%-T- ): also adjust 100%(T) to entering correct test
status
Adjustive opportunity:Turn on the power of the spectrophotometer for pre-heating 30 minutes; Change testing wavelength
or after testing for a longer time; Before high precise testing.
Operation: Check the pilot lamp of TRANSMITTANCE if it is light. If not, press MODE key to let the pilot lamp of
TRANSMISSION in lighting. Close shell of sample chamber without any sample in the chamber, press
0%ADJ key to adjust “0” automatically, “0.0” is displayed on the numerical display window. (If not, press
again)
5.1.3 Adjust 100%-T:
Objective:Adjust two ends of essential readings staff, also adjusting 0% (T) to entering correct test.
Adjustive opportunity:Turn on power of the spectrophotometer for pre-heating 30 minutes; Change testing wavelength or after
testing for a longer time; Before high precise testing.
Operation: Turn on shell of sample chamber, put empty colorimetric cell into its frame. Insert the frame into the sample
chamber (the instrument will turn on optical gate automatically) then cover the top of chamber. Press 100%(T)
key, adjust 100%(T) automatically. (If not, press the key once again)
Attention:Effecting of auto. gain system in instrument will affect 0%(T) after adjusted 100%(T), please check 0%(T). if
have some change, adjust 0%(T) repeatedly.
5.1.4 Adjust wavelength
It is convenient to adjust current testing wavelength with wavelength adjustive knob (12 of instrument figure). The steps of
wavelength adjustment for accurate display are shown as following:
1. Cover shell of sample chamber, press MODE key, the pilot lamp of TRANSMITTANCE is light.
2. Turn the wavelength adjustive knob until 800nm is displayed on the numerical display window, insert empty colorimetric
frame to sample chamber, set 0%(T) and 100%(T) following step 5.1.2 and 5.1.3, then move empty colorimetric frame, and
insert colorimetric frame with Pr-Nd glass, cover shell of sample chamber. Shift display of wavelength 1nm by 1nm until
807nm is displayed. Use air as reference, test each transmittance value at the different wavelength and find out the
wavelength value that corresponding to the minimal value of transmittance is displayed.
3. If the wavelength value is 807nm2nm-also between 805nm—809nm-it means that the value display is accurate, needn’t
adjust. If the wavelength value is over ±2nm, it need adjust accurately by next step.
4. Insert two-inch screwdrivers into the wavelength accurate adjusting hole (14 of figure), turn screwdriver CW or CCW,
change wavelength value until 807nm is displayed.
Attention: The optical filter is changed by mechanical linkage when the adjustive knob is turning at the wavelength of
380nm and 560nm, so when the knob is turning between 380nm-335nm and 560-1000nm, there is a slight frictional sound
and it is normal.

5.1.5 Change sample chamber


The wholly obturation designed sample chamber insures that the instrument has lower stray light. Two kinds of sample chambers are
suited to the colorimetric cell of 1cm, 2cm and 3cm light length. They can be interchanged as test demanded. The interchanging step
is: Open the sample chamber cover, insert a two-inch screwdriver at 45°inclined angle into the little hole, which have 10mm distance
from up surface of the sample chamber. Release the tight screw of the chamber and pull out whole sample chamber in vertical
direction. Then insert a demanded sample chamber and mount it following the contrary step.

5.1.6 Set sample


1. Select colorimetric frame for test (1cm colorimetric frame or 2cm (3cm) colorimetric frame).
2. Put cell with sample in colorimetric frame.
3. Open the shell of sample chamber and insert colorimetric frame with cell to the chamber, the optical gate will open
automatically, and then cover the shell of sample chamber.
5.1.7 Change staff
There are four kinds of staffs on the panel of the instrument:
1. TRASMITTANCE : Reading of transmittance
2. ABSORBANCE : Reading of absorbance
3. FACTOR : Setting concentration factor
4. CONCENTRATION: Setting and reading concentration
Among these staffs, they can be converted by pressing MODE key. The pilot lamp of TRANSMITTANCE is lighted when
the power is turned on. At that time the instrument is preparing to measure transmittance of sample, and the numerical
display shows the value of transmittance. Press MODE key continuously, The pilot lamp of ABSORBANCE, FACTOR,
CONCENTRATION, TRANSMITTANCE will be lighted sequentially, it shows the current mode of instrument, and the
readers of the current mode is shown on the numerical display window.
5.1.8 Setting of concentration factor and concentration
1. Setting of concentration factor.
When the pilot lamp of FACTOR is light, press the MODE key till the right bit of the data in numerical display is
blinking, which means the setting mode is entered. Go on to press the FUNC key continuously; each bit of the data will
blink in turn from right to left. Each bit of the data can be set by pressing UP or DOWN (0%ADJ key or 100%ADJ) key
when it is blinking. When the four bits of the data is set by FUNC key, 0%ADJ key and 100%ADJ key, press MODE key
again, 4-bit concentration factor value will be shown on the numerical display.
2. Setting concentration.
When the pilot lamp of CONCENTRATION is light, press the MODE key till the right bit of the data in numerical display
is blinking, which means the setting mode is entered. Just like the operation steps to setting concentration factor, Press
FUNC key to select the demand bit of the data, then press 0%ADJ and 100%ADJ key to set the concentration data, when
the four bits of the data is set, press MODE key again, the concentration value will be shown on numerical display.
5.1.9 RS232C cable for spectrophotometer
The instrument can be connected with personal computer though RS232C interface cable and the data format of the
RS232C output interface is defined as following:
baud rate: 9600 bps
data bit: 8 bit
stop bit: 1 bit 7
5.2 Application and operation 0
5.2.1 Measure transmission of transparent material

5.2.2 Measure transmission curve of transparent material


Following 1-7 steps of 5.2.1, measure the sample repeatedly in the demanded interval of wavelength at tested wavelength.
Record the corresponding readers of transmittance and write them on the section paper, these data will form the
transmission curve of tested sample. Other way to get the transmission curve is that connect the instrument to personal
computer though the RS232C interface cable, and the transmission curve will be done and shown by PC or printing by
printer.
5.2.3 Measure absorbance of transparent liquor

5.2.4 Measure concentration with method of standard curve 1


5.2.5 Application of concentration
It is unnecessary for user to test the sample quantitatively with the method of complex standard curve when the sample is
stable and its standard curve is nearly passed zero. The method of concentration direct reading can be used. The
concentration of the standard sample is set at the 2/3 places of whole the quantificational concentration ranges which user
demand to test.
The operation steps are shown below:

5.2.6 Application of concentration factor


Set FACTOR staff following first three steps of 5.2.5, a concentration factor of standard sample will be shown on the
numerical display. Record this value, which can help you to get the concentration value of same tested sample through the
method of concentration direct reading. You needn’t to test the concentration factor of standard sample when you need to
test the same sample next time.
The operation steps are shown below:

6 GENERAL MAINTENANCE AND TROUBLESHOOTING GUIDE


6.1 Periodic Maintenance
6.1.1 Precautions on use
1. Environment for instrument daily using accord with 4.1.demands.
2. The surface of the instrument can be cleaned with warm water by gently gauze and be avoided with ethanol, ether,
acetone and so on. The surface spots can be wiped with neutral detergent if necessary. Be sure to cover the instrument with
the dust cover when it is not in using.
3. The colorimetric cell should be washed with petroleum-ether and be cleaned with gently paper then be put into the
colorimetric box after every using.
4. The effective measuring wavelength range is limited by the position fixed frame. Avoid to using great force in case of
breaking the frame when turn the circular adjustive knob near to the wavelength of 335nm and 1000nm. (Though the
wavelength can be adjusted within 332nm to 1003nm)
6.1.2 Open the shell and inspect
The shell of the instrument should be opened in order to check the frame, the optical system and the electro-circuit or if the
light source needs to be changed.
The particular operation steps are shown as following:
1. Cut off the power.
2. Take off the sample chamber as 5.1.5 step shown.
3. Release two tight screws at the side of the adjustive knob with two- inch screwdriver and demount adjustive knob up vertically
4. Demount two M3 screws on the front of the instrument base then turn up the shell of the instrument, every section of the
instrument can be checked now.
6.1.3 Change the light source
A long-life pre-regulated light source, which is produced by our company, is used in the instrument. It can be replaced very
conveniently when the lamp is damaged. The pre-regulated light source is allowed to change by the following steps:
1. Open the shell of the instrument (6.1.2)
2. Demount the old light source package:
-1-Pull out the power cord of the light source on the monochromator cover, wrest out the fixed screws of the light
source holder, take out the light source package carefully.
-2-Mount a new light source package follow the contrary step of (1).
-3-Insert the power cord of new light source package on the monochromator cover.
-4-Turn on main power switch, select the wavelength at 560nm place, pull out the observational cover, inspect the
filament whether aim at the incident slit, otherwise, release the fixed screws of the light source holder, move the light
source package to right and left, let filament aim at incident slit, then tight the fixed screws.
6.2 Check the function of spectrophotometer
Check and adjust as following to approve the eligibility of the instruments before they are leaving factory or after their
being repaired.
6.2.1 Check the range of wavelength
1. Turn on the spectrophotometer and let it pre-heating for 30 minutes, press MODE key letting the instrument to be
worked under the mode of TRANSMITTANCE.
2. Run the adjustive knob of wavelength from short wavelength position to long wavelength position, the displays of the
wavelength can show every wavelength at the range of 335nm-1000nm.
3. Whether at the short wave band or at the long wave band, setting blank, press 100%ADJ key to adjust 100%(T),
numerical display shows 100.0. Not setting colorimetric frame, press 0%ADJ key to adjust 0%(T), now numerical
display shows 0.0.
6.2.2 Check photometric repeatability
1. Set wavelength at 560nm place.
2. Set the sample (generally select neutral filter) which has even absorbance with transmittance about 40%, check the
readings of display three times, the maximum difference≤0.3%.
6.2.4 Wavelength repeatability
1. Set the staff for TRANSMITTANCE.
2. Adjust 0%(T) at the background state, then insert blank colorimetric frame to sample chamber, Adjust 100%(T). Insert
colorimetric frame with Pr-Nd glass to sample chamber, test the transmittance at the range of wavelength from 800nm to
815nm, and record the wavelength readings when the minimum readings of transmittance is observed.
3. Repeat step 2 several times(at least three times), put down the readings of wavelength every time, the error of the
readings of wavelength should≤1nm.
6.3 Troubleshooting guide
Symptom Cause Check point & correction
1.The instrument have 1. Power cord is not connected. 1. Check the power supply is normal; check that the
no response by turning 2.Power fuse is blown. cable is connected correctly; check the power switch is in
on the POWER switch 3.Connected accessory inside the well.
instrument is released. 2.Change the fuse.
3.Open the shell of instrument-insert the accessory again.
2. Numerical displays 1.The pre-heating time of the 1.Time of pre-heating should≥30 min.
of wavelength and instrument is insufficient. 2. No mutation power supply (110V/220V)±10% is
readings are unstable 2.Power supply is unstable. required.
in measuring 3.Environmental vibrations are 3.Change environment that can accord with 4.1
excessive. requirements.
4.Electric circuit is defective. 4.Open the shell of instrument-6.1.2--insert the accessory
again.
3.No signal is 1.Light source is not ignited. 1.Lamp is broken, change the lamp.-6.1.3-
inspected in 2.Optical gate is not turned on. 2.Check that the optical gate can be opened.
measuring 3.There is no signal output from the 3.Input or output plug of the detector is not well contact
detector. with the jack; insert it again.If detector is broken, contact
with service department of our company.
4. Can not adjust 1.Light energy is insufficiency. 1.Check if the light is focused on the incident slit or not;
100%-T- 2.Colorimetric frame is incorrect; see (6.1.3.4) adjust again; If the voltage is over lower,
and the optical gate is closed. adjust it suitably.
2.Insert the colorimetric frame to the end.
5. Can not adjust 0%- A blank colorimetric frame is Draw out the colorimetric frame, the optical gate will be
T- inserted in sample chamber; the closed automatically, cover the sample chamber shell
optical gate is opened. again.
6. Test data is 1. Sample is wrong processed. 1.Process the sample correctly.
abnormal 2. Sample cell is imparity. 2.Deduct comparative error.
3.Great errors of the wavelength 3.Adjust the wavelength again according to-5.1.4-
between display value and actual.
7.Numerical displays 1.The work wavelength of the 1. Adjust 100%(T) firstly by inserting the comparative
show OVER instrument is changed from short to chamber when wavelength is changed, then measure the
long directly during measuring. sample again.
2.The transmittance of sample is 2. Limit the sample in dynamic range which can be
over the dynamic range of the tested by the instrument
instrument under the
ABSORBANCE mode.

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